_publ_creation_date 2013-4-17 _publ_manuscript_number 'icXXXXXXX' _publ_creation_method 'SHELXL' _publ_contact_author 'James P. Donahue' _publ_contact_author_address ; James P. Donahue Department of Chemistry Tulane University Percival Stern Hall, Room 2015 6400 Freret Street New Orleans, Louisiana 70118-5698 ; _publ_contact_author_email 'donahue@tulane.edu' _publ_requested_journal ; 'Inorganic Chemistry' ; _publ_section_title ; A Structural and Spectroscopic Characterization of Octahedral Platinum Bis(dithiolene) Phosphine Complexes: Platinum-Dithiolene Internal Redox Chemistry Induced by Phosphine Association ; loop_ _publ_author_name _publ_author_address 'Chandrasekaran, Perumalreddy' ; Department of Chemistry and Biochemistry Lamar University Beaumont, Texas 77710 ; 'Greene, Angelique' ; Department of Chemistry Tulane University 6400 Freret Street New Orleans, Louisiana 70118-5698 ; 'Lillich, Karen' ; Department of Chemistry Tulane University 6400 Freret Street New Orleans, Louisiana 70118-5698 ; 'Capone, Stephen' ; Department of Chemistry Tulane University 6400 Freret Street New Orleans, Louisiana 70118-5698 ; 'Mague, Joel T.' ; Department of Chemistry Tulane University 6400 Freret Street New Orleans, Louisiana 70118-5698 ; 'DeBeer, Serena' ; Max-Planck Institut f\"ur Chemical Energy Conversion Stiftstrasse 34-36 D45470 M\"ulheim an der Ruhr, Germany ; 'Donahue, James P.' ; Department of Chemistry Tulane University 6400 Freret Street New Orleans, Louisiana 70118-5698 ; #===END # Dithiocarbonic acid S-[1,2-bis(4-methoxyphenyl)-2-oxoethyl] # ester O-isopropyl ester, Compound 1 data_jpd185a _audit_creation_method SHELXL-97 _chemical_name_systematic ; Dithiocarbonic acid S-[1,2-bis(4-methoxyphenyl)-2-oxoethyl] ester O-isopropyl ester ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H22 O4 S2' _chemical_formula_sum 'C20 H22 O4 S2' _chemical_formula_weight 390.50 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.527(1) _cell_length_b 16.947(2) _cell_length_c 10.322(1) _cell_angle_alpha 90.00 _cell_angle_beta 102.779(2) _cell_angle_gamma 90.00 _cell_volume 1966.5(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9933 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 27.17 _exptl_crystal_description Parallepiped _exptl_crystal_colour colourless _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.319 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 824 _exptl_absorpt_coefficient_mu 0.292 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9088 _exptl_absorpt_correction_T_max 0.9722 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2007)' _exptl_special_details ; The diffraction data were obtained from 3 sets of 400 frames, each of width 0.5 deg. in \w, collected at \f = 0.00, 90.00 and 180.00 deg. and 2 sets of 800 frames, each of width 0.45 deg in \f, collected at \w = -30.00 and 210.00 deg. The scan time was 45 sec/frame. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-AXS Smart APEX I CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31177 _diffrn_reflns_av_R_equivalents 0.0461 _diffrn_reflns_av_sigmaI/netI 0.0292 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 27.22 _reflns_number_total 4375 _reflns_number_gt 3769 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker APEX2 (Bruker-AXS, 2008)' _computing_cell_refinement 'Bruker APEX2 (Bruker-AXS, 2008)' _computing_data_reduction 'Bruker SAINT+ (Bruker-AXS, 2006a)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker APEX2 (Bruker-AXS, 2008)' _computing_publication_material 'Bruker APEX2 (Bruker-AXS, 2008)' _publ_section_references ; Bruker-AXS (2008). APEX2, Version 2.2.0, Madison, WI. Bruker-AXS (2006a). SAINT+, Version 7.34A, Madison, WI Sheldrick, G. M. (1997). SHELXS-97 and SHELXL-97. University of G\"ottingen, Germany. Sheldrick, G, M. (2007). SADABS, Version 2007/4. University of G\"ottingen, Germany. ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. H-atoms were placed in calculated positions (C---H = 0.95 - 0.98 \%A) and included as riding contributions with isotropic displacement parameters 1.2 - 1.5 times those of the attached carbon atoms. The isopropyl group is rotationally disordered about the O4---C18 bond over two essentially equally populated sites while there is about a 5% occupancy of an alternate site for each of the two sulfur atoms. Refinement was completed with restraints to approximately identical geometries for each of the disordered moieties. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0294P)^2^+4.3227P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4375 _refine_ls_number_parameters 251 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0824 _refine_ls_R_factor_gt 0.0710 _refine_ls_wR_factor_ref 0.1540 _refine_ls_wR_factor_gt 0.1492 _refine_ls_goodness_of_fit_ref 1.222 _refine_ls_restrained_S_all 1.231 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S1 S 0.67399(7) 0.22133(5) 0.12207(12) 0.0258(3) Uani 0.944(2) 1 d PD A 1 S2 S 0.65669(9) 0.04895(5) 0.11298(13) 0.0334(3) Uani 0.944(2) 1 d PD A 1 S1A S 0.6772(11) 0.2216(7) 0.196(2) 0.0258(3) Uani 0.056(2) 1 d PD A 2 S2A S 0.6505(15) 0.0549(9) 0.181(2) 0.0334(3) Uani 0.056(2) 1 d PD A 2 O1 O 1.3687(2) 0.35149(15) 0.3703(3) 0.0356(6) Uani 1 1 d . . . O2 O 0.8785(2) 0.25348(18) -0.0072(3) 0.0435(7) Uani 1 1 d . . . O3 O 0.6093(3) 0.59781(15) 0.0713(3) 0.0466(7) Uani 1 1 d . A . O4 O 0.85460(19) 0.13200(14) 0.2053(2) 0.0295(5) Uani 1 1 d . . . C1 C 1.4599(3) 0.3595(2) 0.2983(4) 0.0369(8) Uani 1 1 d . . . H1A H 1.4652 0.3109 0.2484 0.055 Uiso 1 1 calc R . . H1B H 1.5362 0.3691 0.3604 0.055 Uiso 1 1 calc R . . H1C H 1.4413 0.4039 0.2364 0.055 Uiso 1 1 calc R . . C2 C 1.2557(3) 0.33834(18) 0.2993(4) 0.0281(7) Uani 1 1 d . . . C3 C 1.2256(3) 0.3246(2) 0.1640(4) 0.0351(8) Uani 1 1 d . . . H3 H 1.2845 0.3275 0.1126 0.042 Uiso 1 1 calc R . . C4 C 1.1090(3) 0.3065(3) 0.1041(4) 0.0408(9) Uani 1 1 d . . . H4 H 1.0887 0.2955 0.0116 0.049 Uiso 1 1 calc R . . C5 C 1.0204(3) 0.30415(18) 0.1771(3) 0.0273(7) Uani 1 1 d . . . C6 C 1.0507(3) 0.3213(2) 0.3100(4) 0.0319(7) Uani 1 1 d . . . H6 H 0.9912 0.3213 0.3608 0.038 Uiso 1 1 calc R . . C7 C 1.1687(3) 0.3386(3) 0.3713(4) 0.0413(9) Uani 1 1 d . . . H7 H 1.1888 0.3507 0.4635 0.050 Uiso 1 1 calc R . . C8 C 0.8984(3) 0.2790(2) 0.1069(3) 0.0297(7) Uani 1 1 d . A . C9 C 0.7979(3) 0.28975(18) 0.1799(3) 0.0245(6) Uani 1 1 d D . . H9 H 0.8297 0.2822 0.2774 0.029 Uiso 1 1 calc R A 1 C10 C 0.7474(3) 0.37254(19) 0.1548(3) 0.0261(7) Uani 1 1 d . A . C11 C 0.7262(3) 0.4178(2) 0.2572(4) 0.0318(7) Uani 1 1 d . . . H11 H 0.7442 0.3974 0.3451 0.038 Uiso 1 1 calc R A . C12 C 0.6780(3) 0.4942(2) 0.2337(4) 0.0362(8) Uani 1 1 d . A . H12 H 0.6623 0.5249 0.3049 0.043 Uiso 1 1 calc R . . C13 C 0.6540(3) 0.5237(2) 0.1072(4) 0.0356(8) Uani 1 1 d . . . C14 C 0.6755(4) 0.4787(2) 0.0028(4) 0.0430(9) Uani 1 1 d . A . H14 H 0.6588 0.4995 -0.0848 0.052 Uiso 1 1 calc R . . C15 C 0.7214(4) 0.4034(2) 0.0269(4) 0.0382(8) Uani 1 1 d . . . H15 H 0.7353 0.3724 -0.0449 0.046 Uiso 1 1 calc R A . C16 C 0.5788(4) 0.6449(2) 0.1711(5) 0.0543(11) Uani 1 1 d . . . H16A H 0.5203 0.6170 0.2101 0.082 Uiso 1 1 calc R A . H16B H 0.5446 0.6948 0.1323 0.082 Uiso 1 1 calc R . . H16C H 0.6502 0.6557 0.2402 0.082 Uiso 1 1 calc R . . C17 C 0.7394(3) 0.12866(19) 0.1527(3) 0.0280(7) Uani 1 1 d D A . C18 C 0.9280(3) 0.0593(2) 0.2198(4) 0.0358(8) Uani 0.497(4) 1 d PD B 1 H18 H 0.8765 0.0161 0.2418 0.043 Uiso 0.497(4) 1 calc PR B 1 C19 C 0.9605(7) 0.0356(4) 0.0961(7) 0.0396(12) Uani 0.497(4) 1 d PD B 1 H19A H 0.8883 0.0295 0.0259 0.059 Uiso 0.497(4) 1 calc PR B 1 H19B H 1.0033 -0.0148 0.1096 0.059 Uiso 0.497(4) 1 calc PR B 1 H19C H 1.0116 0.0760 0.0699 0.059 Uiso 0.497(4) 1 calc PR B 1 C20 C 1.0250(7) 0.0697(4) 0.3389(7) 0.0379(12) Uani 0.497(4) 1 d PD B 1 H20A H 0.9912 0.0848 0.4145 0.057 Uiso 0.497(4) 1 calc PR B 1 H20B H 1.0791 0.1112 0.3222 0.057 Uiso 0.497(4) 1 calc PR B 1 H20C H 1.0689 0.0201 0.3589 0.057 Uiso 0.497(4) 1 calc PR B 1 C18A C 0.9280(3) 0.0593(2) 0.2198(4) 0.0358(8) Uani 0.503(4) 1 d PD B 2 H18A H 0.8942 0.0196 0.1499 0.043 Uiso 0.503(4) 1 calc PR B 2 C19A C 1.0488(6) 0.0959(4) 0.1957(8) 0.0396(12) Uani 0.503(4) 1 d PD B 2 H19D H 1.0362 0.1155 0.1044 0.059 Uiso 0.503(4) 1 calc PR B 2 H19E H 1.1106 0.0551 0.2101 0.059 Uiso 0.503(4) 1 calc PR B 2 H19F H 1.0740 0.1395 0.2579 0.059 Uiso 0.503(4) 1 calc PR B 2 C20A C 0.9378(7) 0.0279(4) 0.3491(7) 0.0379(12) Uani 0.503(4) 1 d PD B 2 H20D H 0.8609 0.0059 0.3567 0.057 Uiso 0.503(4) 1 calc PR B 2 H20E H 0.9611 0.0699 0.4150 0.057 Uiso 0.503(4) 1 calc PR B 2 H20F H 0.9981 -0.0139 0.3649 0.057 Uiso 0.503(4) 1 calc PR B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1 0.0172(4) 0.0207(4) 0.0373(7) 0.0065(4) 0.0013(3) -0.0013(3) S2 0.0349(5) 0.0219(4) 0.0427(7) 0.0048(4) 0.0066(4) -0.0028(4) S1A 0.0172(4) 0.0207(4) 0.0373(7) 0.0065(4) 0.0013(3) -0.0013(3) S2A 0.0349(5) 0.0219(4) 0.0427(7) 0.0048(4) 0.0066(4) -0.0028(4) O1 0.0195(11) 0.0402(14) 0.0463(15) 0.0005(12) 0.0058(10) -0.0050(10) O2 0.0318(13) 0.0660(19) 0.0331(14) 0.0010(13) 0.0077(11) -0.0090(13) O3 0.0536(17) 0.0221(13) 0.0662(19) 0.0048(13) 0.0175(14) 0.0004(12) O4 0.0229(11) 0.0267(12) 0.0380(13) 0.0005(10) 0.0048(9) 0.0066(9) C1 0.0221(16) 0.0324(19) 0.056(2) 0.0121(17) 0.0090(15) -0.0003(14) C2 0.0211(15) 0.0188(15) 0.044(2) 0.0021(14) 0.0060(13) -0.0004(11) C3 0.0297(17) 0.037(2) 0.041(2) 0.0025(16) 0.0125(15) -0.0048(15) C4 0.0331(19) 0.058(3) 0.0319(19) 0.0004(17) 0.0086(15) -0.0114(17) C5 0.0259(15) 0.0199(15) 0.0364(18) 0.0043(13) 0.0074(13) 0.0012(12) C6 0.0261(16) 0.0311(18) 0.0390(19) -0.0085(15) 0.0081(14) -0.0020(13) C7 0.0311(18) 0.056(2) 0.038(2) -0.0114(18) 0.0094(15) -0.0118(17) C8 0.0292(16) 0.0313(17) 0.0283(17) 0.0063(14) 0.0057(13) -0.0044(14) C9 0.0185(14) 0.0236(15) 0.0299(16) 0.0045(13) 0.0025(12) -0.0032(12) C10 0.0178(14) 0.0234(16) 0.0369(18) 0.0025(14) 0.0056(12) -0.0057(11) C11 0.0245(16) 0.0371(19) 0.0360(19) 0.0049(15) 0.0117(14) -0.0002(14) C12 0.0247(16) 0.037(2) 0.051(2) -0.0027(17) 0.0170(15) -0.0022(14) C13 0.0262(17) 0.0246(17) 0.055(2) 0.0057(16) 0.0077(16) -0.0051(13) C14 0.064(3) 0.0235(18) 0.037(2) 0.0052(16) 0.0028(18) -0.0001(17) C15 0.053(2) 0.0247(17) 0.0336(19) 0.0034(15) 0.0018(16) -0.0020(16) C16 0.054(3) 0.032(2) 0.079(3) -0.009(2) 0.018(2) -0.0030(19) C17 0.0259(16) 0.0253(16) 0.0333(17) 0.0063(14) 0.0074(13) 0.0021(13) C18 0.0356(18) 0.0276(18) 0.042(2) -0.0032(15) 0.0039(15) 0.0148(14) C19 0.044(3) 0.032(3) 0.043(3) 0.003(2) 0.011(2) 0.018(2) C20 0.039(3) 0.029(3) 0.042(3) -0.001(2) 0.003(2) 0.010(2) C18A 0.0356(18) 0.0276(18) 0.042(2) -0.0032(15) 0.0039(15) 0.0148(14) C19A 0.044(3) 0.032(3) 0.043(3) 0.003(2) 0.011(2) 0.018(2) C20A 0.039(3) 0.029(3) 0.042(3) -0.001(2) 0.003(2) 0.010(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 C17 1.741(3) . ? S1 C9 1.834(3) . ? S2 C17 1.652(3) . ? S1A C17 1.825(13) . ? S1A C9 1.843(12) . ? S2A C17 1.681(14) . ? O1 C2 1.364(4) . ? O1 C1 1.422(4) . ? O2 C8 1.228(4) . ? O3 C13 1.377(4) . ? O3 C16 1.407(5) . ? O4 C17 1.319(4) . ? O4 C18 1.483(4) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C7 1.374(5) . ? C2 C3 1.383(5) . ? C3 C4 1.384(5) . ? C3 H3 0.9500 . ? C4 C5 1.397(5) . ? C4 H4 0.9500 . ? C5 C6 1.369(5) . ? C5 C8 1.495(4) . ? C6 C7 1.399(5) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 C9 1.526(5) . ? C9 C10 1.519(4) . ? C9 H9 1.0000 . ? C10 C11 1.371(5) . ? C10 C15 1.390(5) . ? C11 C12 1.409(5) . ? C11 H11 0.9500 . ? C12 C13 1.368(5) . ? C12 H12 0.9500 . ? C13 C14 1.387(6) . ? C14 C15 1.384(5) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C18 C19 1.465(8) . ? C18 C20 1.478(7) . ? C18 H18 1.0000 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C19A H19D 0.9800 . ? C19A H19E 0.9800 . ? C19A H19F 0.9800 . ? C20A H20D 0.9800 . ? C20A H20E 0.9800 . ? C20A H20F 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C17 S1 C9 103.66(15) . . ? C17 S1A C9 100.1(7) . . ? C2 O1 C1 117.6(3) . . ? C13 O3 C16 117.3(3) . . ? C17 O4 C18 120.4(3) . . ? O1 C1 H1A 109.5 . . ? O1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? O1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 C7 115.7(3) . . ? O1 C2 C3 124.5(3) . . ? C7 C2 C3 119.8(3) . . ? C2 C3 C4 119.3(3) . . ? C2 C3 H3 120.3 . . ? C4 C3 H3 120.3 . . ? C3 C4 C5 121.3(4) . . ? C3 C4 H4 119.4 . . ? C5 C4 H4 119.4 . . ? C6 C5 C4 118.7(3) . . ? C6 C5 C8 123.3(3) . . ? C4 C5 C8 117.9(3) . . ? C5 C6 C7 120.3(3) . . ? C5 C6 H6 119.9 . . ? C7 C6 H6 119.9 . . ? C2 C7 C6 120.5(3) . . ? C2 C7 H7 119.7 . . ? C6 C7 H7 119.7 . . ? O2 C8 C5 121.4(3) . . ? O2 C8 C9 121.0(3) . . ? C5 C8 C9 117.5(3) . . ? C10 C9 C8 109.3(3) . . ? C10 C9 S1 106.7(2) . . ? C8 C9 S1 112.6(2) . . ? C10 C9 S1A 109.0(4) . . ? C8 C9 S1A 129.7(5) . . ? C10 C9 H9 109.4 . . ? C8 C9 H9 109.4 . . ? S1 C9 H9 109.4 . . ? S1A C9 H9 87.0 . . ? C11 C10 C15 119.0(3) . . ? C11 C10 C9 120.8(3) . . ? C15 C10 C9 120.2(3) . . ? C10 C11 C12 120.8(3) . . ? C10 C11 H11 119.6 . . ? C12 C11 H11 119.6 . . ? C13 C12 C11 119.3(4) . . ? C13 C12 H12 120.3 . . ? C11 C12 H12 120.3 . . ? C12 C13 O3 125.1(4) . . ? C12 C13 C14 120.5(3) . . ? O3 C13 C14 114.4(3) . . ? C15 C14 C13 119.7(4) . . ? C15 C14 H14 120.2 . . ? C13 C14 H14 120.2 . . ? C14 C15 C10 120.8(4) . . ? C14 C15 H15 119.6 . . ? C10 C15 H15 119.6 . . ? O3 C16 H16A 109.5 . . ? O3 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? O3 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O4 C17 S2 127.6(3) . . ? O4 C17 S2A 123.9(7) . . ? O4 C17 S1 113.1(2) . . ? S2 C17 S1 119.30(19) . . ? S2A C17 S1 116.5(6) . . ? O4 C17 S1A 106.1(5) . . ? S2 C17 S1A 122.0(4) . . ? S2A C17 S1A 108.2(9) . . ? C19 C18 C20 117.8(5) . . ? C19 C18 O4 113.0(4) . . ? C20 C18 O4 107.1(4) . . ? C19 C18 H18 106.1 . . ? C20 C18 H18 106.1 . . ? O4 C18 H18 106.1 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? H19D C19A H19E 109.5 . . ? H19D C19A H19F 109.5 . . ? H19E C19A H19F 109.5 . . ? H20D C20A H20E 109.5 . . ? H20D C20A H20F 109.5 . . ? H20E C20A H20F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.22 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.585 _refine_diff_density_min -0.297 _refine_diff_density_rms 0.070 #===END # [(MeO-p-C6H4)2C2S2C=O], Compound 2 data_jpd186_0m _audit_creation_method SHELXL-97 _chemical_name_systematic ; 4,5-Bis(4-methoxyphenyl)-[1,3]dithiol-2-one ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C17 H14 O3 S2' _chemical_formula_sum 'C17 H14 O3 S2' _chemical_formula_weight 330.40 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 5.4968(4) _cell_length_b 11.7792(9) _cell_length_c 12.5653(9) _cell_angle_alpha 113.3490(10) _cell_angle_beta 94.1080(10) _cell_angle_gamma 94.8570(10) _cell_volume 739.33(9) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9639 _cell_measurement_theta_min 3.082 _cell_measurement_theta_max 29.460 _exptl_crystal_description column _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.484 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 344 _exptl_absorpt_coefficient_mu 0.369 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9082 _exptl_absorpt_correction_T_max 0.9675 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2007)' _exptl_special_details ; The diffraction data were obtained from 3 sets of 400 frames, each of width 0.5 deg. in \w, collected at \f = 0.00, 90.00 and 180.00 deg. and 2 sets of 800 frames, each of width 0.45 deg in \f, collected at \w = -30.00 and 210.00 deg. The scan time was 25 sec/frame. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-AXS Smart APEX I CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12930 _diffrn_reflns_av_R_equivalents 0.0250 _diffrn_reflns_av_sigmaI/netI 0.0215 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 27.99 _reflns_number_total 3542 _reflns_number_gt 3234 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker APEX2 (Bruker-AXS, 2007)' _computing_cell_refinement 'Bruker APEX2 (Bruker-AXS, 2007)' _computing_data_reduction 'Bruker SAINT+ (Bruker-AXS, 2006)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker APEX2 (Bruker-AXS, 2006)' _computing_publication_material 'Bruker APEX2 (Bruker-AXS, 2006)' _publ_section_references ; Bruker-AXS (2006). APEX2, Version 2.2.0, Madison, WI. Bruker-AXS (2006). SAINT+, Version 7.34A, Madison, WI Sheldrick, G. M. (1997). SHELXS-97 and SHELXL-97. University of G\"ottingen, Germany. Sheldrick, G, M. (2007). SADABS, Version 2007/4. University of G\"ottingen, Germany. ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. H-atoms were placed in calculated positions (C---H = 0.95 - 0.98 \%A) and included as riding contributions with isotropic displacement parameters 1.2 - 1.5 times those of the attached carbon atoms. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0401P)^2^+0.2898P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3542 _refine_ls_number_parameters 201 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0319 _refine_ls_R_factor_gt 0.0288 _refine_ls_wR_factor_ref 0.0775 _refine_ls_wR_factor_gt 0.0749 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S1 S 1.27592(5) 0.37253(3) 0.49290(3) 0.01644(9) Uani 1 1 d . . . S2 S 1.52779(5) 0.16965(3) 0.50849(3) 0.01616(9) Uani 1 1 d . . . O1 O 1.65047(19) 0.40769(9) 0.65045(9) 0.0263(2) Uani 1 1 d . . . O2 O 1.06591(16) -0.38871(8) 0.13043(8) 0.01812(19) Uani 1 1 d . . . O3 O 0.41062(16) 0.20226(9) 0.04979(8) 0.01999(19) Uani 1 1 d . . . C1 C 1.1669(2) 0.22183(11) 0.38865(10) 0.0139(2) Uani 1 1 d . . . C2 C 1.2830(2) 0.12891(11) 0.39730(10) 0.0141(2) Uani 1 1 d . . . C3 C 1.5147(2) 0.33223(12) 0.56812(11) 0.0182(2) Uani 1 1 d . . . C4 C 1.2213(2) -0.00708(11) 0.32651(10) 0.0139(2) Uani 1 1 d . . . C5 C 1.3744(2) -0.07347(12) 0.24537(11) 0.0162(2) Uani 1 1 d . . . H5 H 1.5182 -0.0310 0.2339 0.019 Uiso 1 1 calc R . . C6 C 1.3172(2) -0.20052(12) 0.18181(10) 0.0166(2) Uani 1 1 d . . . H6 H 1.4208 -0.2447 0.1262 0.020 Uiso 1 1 calc R . . C7 C 1.1082(2) -0.26412(11) 0.19904(10) 0.0148(2) Uani 1 1 d . . . C8 C 0.9547(2) -0.19927(11) 0.27976(10) 0.0159(2) Uani 1 1 d . . . H8 H 0.8124 -0.2421 0.2921 0.019 Uiso 1 1 calc R . . C9 C 1.0119(2) -0.07106(11) 0.34215(10) 0.0154(2) Uani 1 1 d . . . H9 H 0.9060 -0.0265 0.3963 0.018 Uiso 1 1 calc R . . C10 C 0.8643(2) -0.45844(12) 0.15224(12) 0.0224(3) Uani 1 1 d . . . H10A H 0.8917 -0.4527 0.2322 0.034 Uiso 1 1 calc R . . H10B H 0.8514 -0.5459 0.0972 0.034 Uiso 1 1 calc R . . H10C H 0.7118 -0.4245 0.1422 0.034 Uiso 1 1 calc R . . C11 C 0.9654(2) 0.21436(11) 0.30063(10) 0.0138(2) Uani 1 1 d . . . C12 C 0.8111(2) 0.30788(11) 0.32716(10) 0.0163(2) Uani 1 1 d . . . H12 H 0.8347 0.3736 0.4029 0.020 Uiso 1 1 calc R . . C13 C 0.6240(2) 0.30808(12) 0.24653(11) 0.0169(2) Uani 1 1 d . . . H13 H 0.5216 0.3728 0.2670 0.020 Uiso 1 1 calc R . . C14 C 0.5890(2) 0.21215(12) 0.13558(10) 0.0154(2) Uani 1 1 d . . . C15 C 0.7418(2) 0.11783(12) 0.10663(11) 0.0166(2) Uani 1 1 d . . . H15 H 0.7181 0.0525 0.0307 0.020 Uiso 1 1 calc R . . C16 C 0.9276(2) 0.11890(11) 0.18782(10) 0.0151(2) Uani 1 1 d . . . H16 H 1.0304 0.0543 0.1669 0.018 Uiso 1 1 calc R . . C17 C 0.2629(2) 0.30256(13) 0.07441(12) 0.0217(3) Uani 1 1 d . . . H17A H 0.1763 0.3108 0.1422 0.032 Uiso 1 1 calc R . . H17B H 0.1428 0.2850 0.0066 0.032 Uiso 1 1 calc R . . H17C H 0.3686 0.3803 0.0913 0.032 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1 0.01897(15) 0.01137(15) 0.01665(15) 0.00380(11) -0.00227(11) 0.00265(11) S2 0.01677(15) 0.01449(15) 0.01731(15) 0.00699(12) -0.00187(11) 0.00276(11) O1 0.0296(5) 0.0187(5) 0.0239(5) 0.0041(4) -0.0096(4) 0.0014(4) O2 0.0219(4) 0.0120(4) 0.0178(4) 0.0035(3) 0.0025(3) 0.0011(3) O3 0.0183(4) 0.0239(5) 0.0181(4) 0.0091(4) -0.0024(3) 0.0048(4) C1 0.0151(5) 0.0115(5) 0.0142(5) 0.0044(4) 0.0011(4) 0.0012(4) C2 0.0142(5) 0.0138(6) 0.0143(5) 0.0062(4) 0.0007(4) 0.0009(4) C3 0.0203(6) 0.0165(6) 0.0176(6) 0.0068(5) -0.0006(5) 0.0032(5) C4 0.0153(5) 0.0125(5) 0.0150(5) 0.0070(4) -0.0005(4) 0.0031(4) C5 0.0152(5) 0.0166(6) 0.0189(6) 0.0092(5) 0.0034(4) 0.0025(4) C6 0.0170(6) 0.0170(6) 0.0165(6) 0.0064(5) 0.0045(4) 0.0052(5) C7 0.0184(6) 0.0122(5) 0.0135(5) 0.0051(4) -0.0008(4) 0.0030(4) C8 0.0146(5) 0.0152(6) 0.0180(6) 0.0070(5) 0.0020(4) 0.0008(4) C9 0.0152(5) 0.0152(6) 0.0166(5) 0.0066(5) 0.0030(4) 0.0044(4) C10 0.0238(6) 0.0142(6) 0.0263(6) 0.0064(5) 0.0014(5) -0.0025(5) C11 0.0149(5) 0.0125(5) 0.0152(5) 0.0074(4) 0.0003(4) 0.0009(4) C12 0.0194(6) 0.0133(6) 0.0155(5) 0.0050(4) 0.0009(4) 0.0028(5) C13 0.0175(6) 0.0151(6) 0.0199(6) 0.0084(5) 0.0019(5) 0.0052(5) C14 0.0139(5) 0.0178(6) 0.0167(5) 0.0101(5) -0.0003(4) 0.0000(4) C15 0.0174(6) 0.0155(6) 0.0156(5) 0.0055(4) 0.0008(4) 0.0006(5) C16 0.0163(5) 0.0123(5) 0.0163(5) 0.0052(4) 0.0020(4) 0.0026(4) C17 0.0186(6) 0.0257(7) 0.0255(6) 0.0157(5) -0.0013(5) 0.0044(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 C1 1.7580(12) . ? S1 C3 1.7677(13) . ? S2 C2 1.7557(12) . ? S2 C3 1.7685(13) . ? O1 C3 1.2105(16) . ? O2 C7 1.3645(14) . ? O2 C10 1.4301(15) . ? O3 C14 1.3663(14) . ? O3 C17 1.4353(16) . ? C1 C2 1.3489(16) . ? C1 C11 1.4794(16) . ? C2 C4 1.4858(16) . ? C4 C9 1.3909(16) . ? C4 C5 1.4005(16) . ? C5 C6 1.3832(17) . ? C5 H5 0.9500 . ? C6 C7 1.3954(17) . ? C6 H6 0.9500 . ? C7 C8 1.3934(17) . ? C8 C9 1.3929(17) . ? C8 H8 0.9500 . ? C9 H9 0.9500 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.3971(17) . ? C11 C16 1.4042(16) . ? C12 C13 1.3918(17) . ? C12 H12 0.9500 . ? C13 C14 1.3905(17) . ? C13 H13 0.9500 . ? C14 C15 1.3976(17) . ? C15 C16 1.3865(16) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 S1 C3 97.89(6) . . ? C2 S2 C3 97.14(6) . . ? C7 O2 C10 117.06(10) . . ? C14 O3 C17 117.10(10) . . ? C2 C1 C11 128.62(11) . . ? C2 C1 S1 115.78(9) . . ? C11 C1 S1 115.57(9) . . ? C1 C2 C4 127.55(11) . . ? C1 C2 S2 117.54(9) . . ? C4 C2 S2 114.84(8) . . ? O1 C3 S1 123.47(10) . . ? O1 C3 S2 124.88(10) . . ? S1 C3 S2 111.64(7) . . ? C9 C4 C5 118.90(11) . . ? C9 C4 C2 120.08(11) . . ? C5 C4 C2 121.00(11) . . ? C6 C5 C4 120.36(11) . . ? C6 C5 H5 119.8 . . ? C4 C5 H5 119.8 . . ? C5 C6 C7 120.31(11) . . ? C5 C6 H6 119.8 . . ? C7 C6 H6 119.8 . . ? O2 C7 C8 124.38(11) . . ? O2 C7 C6 115.67(11) . . ? C8 C7 C6 119.92(11) . . ? C9 C8 C7 119.35(11) . . ? C9 C8 H8 120.3 . . ? C7 C8 H8 120.3 . . ? C4 C9 C8 121.15(11) . . ? C4 C9 H9 119.4 . . ? C8 C9 H9 119.4 . . ? O2 C10 H10A 109.5 . . ? O2 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? O2 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 C16 117.63(11) . . ? C12 C11 C1 119.72(11) . . ? C16 C11 C1 122.58(11) . . ? C13 C12 C11 122.28(11) . . ? C13 C12 H12 118.9 . . ? C11 C12 H12 118.9 . . ? C14 C13 C12 119.06(11) . . ? C14 C13 H13 120.5 . . ? C12 C13 H13 120.5 . . ? O3 C14 C13 124.19(11) . . ? O3 C14 C15 116.03(11) . . ? C13 C14 C15 119.79(11) . . ? C16 C15 C14 120.52(11) . . ? C16 C15 H15 119.7 . . ? C14 C15 H15 119.7 . . ? C15 C16 C11 120.72(11) . . ? C15 C16 H16 119.6 . . ? C11 C16 H16 119.6 . . ? O3 C17 H17A 109.5 . . ? O3 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? O3 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C3 S1 C1 C2 1.10(11) . . . . ? C3 S1 C1 C11 -176.92(9) . . . . ? C11 C1 C2 C4 -6.4(2) . . . . ? S1 C1 C2 C4 175.94(10) . . . . ? C11 C1 C2 S2 176.77(9) . . . . ? S1 C1 C2 S2 -0.93(13) . . . . ? C3 S2 C2 C1 0.27(11) . . . . ? C3 S2 C2 C4 -177.00(9) . . . . ? C1 S1 C3 O1 179.39(12) . . . . ? C1 S1 C3 S2 -0.87(8) . . . . ? C2 S2 C3 O1 -179.79(12) . . . . ? C2 S2 C3 S1 0.47(8) . . . . ? C1 C2 C4 C9 -71.43(17) . . . . ? S2 C2 C4 C9 105.51(11) . . . . ? C1 C2 C4 C5 110.09(15) . . . . ? S2 C2 C4 C5 -72.97(13) . . . . ? C9 C4 C5 C6 0.16(17) . . . . ? C2 C4 C5 C6 178.65(11) . . . . ? C4 C5 C6 C7 -0.86(18) . . . . ? C10 O2 C7 C8 -6.77(17) . . . . ? C10 O2 C7 C6 175.18(11) . . . . ? C5 C6 C7 O2 178.80(10) . . . . ? C5 C6 C7 C8 0.65(18) . . . . ? O2 C7 C8 C9 -177.72(11) . . . . ? C6 C7 C8 C9 0.25(17) . . . . ? C5 C4 C9 C8 0.77(17) . . . . ? C2 C4 C9 C8 -177.75(11) . . . . ? C7 C8 C9 C4 -0.97(18) . . . . ? C2 C1 C11 C12 157.01(13) . . . . ? S1 C1 C11 C12 -25.27(14) . . . . ? C2 C1 C11 C16 -25.88(19) . . . . ? S1 C1 C11 C16 151.84(10) . . . . ? C16 C11 C12 C13 0.48(18) . . . . ? C1 C11 C12 C13 177.73(11) . . . . ? C11 C12 C13 C14 -0.09(19) . . . . ? C17 O3 C14 C13 4.60(17) . . . . ? C17 O3 C14 C15 -175.59(10) . . . . ? C12 C13 C14 O3 179.54(11) . . . . ? C12 C13 C14 C15 -0.27(18) . . . . ? O3 C14 C15 C16 -179.61(11) . . . . ? C13 C14 C15 C16 0.21(18) . . . . ? C14 C15 C16 C11 0.20(18) . . . . ? C12 C11 C16 C15 -0.53(17) . . . . ? C1 C11 C16 C15 -177.70(11) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.99 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.370 _refine_diff_density_min -0.294 _refine_diff_density_rms 0.077 #===END # [(CH3O-p-C6H4)SnMe2], Compound 3 data_jpd264_0m _audit_creation_method SHELXL-97 _chemical_name_systematic ; 4,5-Bis(4-methoxyphenyl)-2,2-dimethyl- [1,3,2]dithiastannole ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H20 O2 S2 Sn' _chemical_formula_sum 'C18 H20 O2 S2 Sn' _chemical_formula_weight 451.15 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Sn' 'Sn' -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2/n _symmetry_space_group_name_Hall '-P 2yac' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z-1/2' _cell_length_a 13.4064(19) _cell_length_b 10.7853(15) _cell_length_c 25.900(4) _cell_angle_alpha 90.00 _cell_angle_beta 99.379(2) _cell_angle_gamma 90.00 _cell_volume 3694.8(9) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9639 _cell_measurement_theta_min 2.47 _cell_measurement_theta_max 28.79 _exptl_crystal_description Parallelepiped _exptl_crystal_colour colourless _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.622 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1808 _exptl_absorpt_coefficient_mu 1.615 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7143 _exptl_absorpt_correction_T_max 0.8552 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008a)' _exptl_special_details ; The diffraction data were obtained from 3 sets of 400 frames, each of width 0.5 deg. in \w, collected at \f = 0.00, 90.00 and 180.00 deg. and 2 sets of 800 frames, each of width 0.45 deg in \f, collected at \w = -30.00 and 210.00 deg. The scan time was 10 sec/frame. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-I CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 64466 _diffrn_reflns_av_R_equivalents 0.0311 _diffrn_reflns_av_sigmaI/netI 0.0181 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 2.44 _diffrn_reflns_theta_max 28.83 _reflns_number_total 9570 _reflns_number_gt 8889 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker APEX2 (Bruker-AXS, 2008)' _computing_cell_refinement 'Bruker SAINT (Bruker-AXS 2008a)' _computing_data_reduction 'Bruker SAINT (Bruker-AXS 2008a)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL(Bruker-AXS 2008b)' _computing_publication_material 'Bruker SHELXTL(Bruker-AXS 2008b)' _publ_section_references ; Bruker-AXS (2008). APEX2, Version 2008.6-1, Madison, WI. Bruker-AXS (2008a). SAINT, Version 7.60A, Madison, WI Bruker-AXS (2008b). SHELXTL, Version 2008/4, Madison, WI Sheldrick, G. M. (2008). SHELXS-97 and SHELXL-97. University of G\"ottingen, Germany. Sheldrick, G, M. (2008a). SADABS, Version 2008/2. University of G\"ottingen, Germany. ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. H-atoms were placed in calculated positions (C---H = 0.95 - 0.98 \%A) and included as riding contributions with isotropic displacement parameters 1.2 - 1.5 times those of the attached carbon atoms. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0215P)^2^+2.2001P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00126(6) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 9570 _refine_ls_number_parameters 424 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0215 _refine_ls_R_factor_gt 0.0194 _refine_ls_wR_factor_ref 0.0499 _refine_ls_wR_factor_gt 0.0485 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.069 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sn1 Sn 0.922121(7) 0.487706(8) 1.147928(4) 0.01441(3) Uani 1 1 d . . . Sn2 Sn 0.866494(7) -0.000530(8) 0.116807(4) 0.01409(3) Uani 1 1 d . . . S1 S 0.86049(3) 0.35016(3) 1.075909(12) 0.01366(6) Uani 1 1 d . . . S2 S 0.86456(3) 0.66296(3) 1.092529(13) 0.01725(7) Uani 1 1 d . . . S3 S 0.92502(3) 0.17144(3) 0.174423(13) 0.01622(7) Uani 1 1 d . . . S4 S 0.91020(3) -0.14018(3) 0.189896(13) 0.01634(7) Uani 1 1 d . . . O1 O 0.72843(8) 0.25371(10) 0.82259(4) 0.0203(2) Uani 1 1 d . . . O2 O 0.74538(8) 0.93867(10) 0.86986(4) 0.0243(2) Uani 1 1 d . . . O3 O 0.98628(8) 0.43046(10) 0.40522(4) 0.0225(2) Uani 1 1 d . . . O4 O 0.97201(8) -0.24028(10) 0.44397(4) 0.0201(2) Uani 1 1 d . . . C1 C 0.83201(10) 0.46104(12) 1.02479(5) 0.0127(2) Uani 1 1 d . . . C2 C 0.83397(10) 0.58506(12) 1.03170(5) 0.0130(2) Uani 1 1 d . . . C3 C 0.93486(10) 0.09398(12) 0.23545(5) 0.0134(2) Uani 1 1 d . . . C4 C 0.92984(10) -0.03006(12) 0.24170(5) 0.0134(2) Uani 1 1 d . . . C5 C 0.80128(10) 0.40278(11) 0.97254(5) 0.0125(2) Uani 1 1 d . . . C6 C 0.86368(11) 0.31680(13) 0.95273(5) 0.0168(3) Uani 1 1 d . . . H6 H 0.9251 0.2915 0.9737 0.020 Uiso 1 1 calc R . . C7 C 0.83688(11) 0.26813(13) 0.90288(6) 0.0191(3) Uani 1 1 d . . . H7 H 0.8803 0.2108 0.8898 0.023 Uiso 1 1 calc R . . C8 C 0.74634(11) 0.30316(12) 0.87197(5) 0.0154(3) Uani 1 1 d . . . C9 C 0.68162(10) 0.38472(12) 0.89163(5) 0.0149(2) Uani 1 1 d . . . H9 H 0.6188 0.4068 0.8711 0.018 Uiso 1 1 calc R . . C10 C 0.70965(10) 0.43383(12) 0.94159(5) 0.0144(2) Uani 1 1 d . . . H10 H 0.6653 0.4898 0.9549 0.017 Uiso 1 1 calc R . . C11 C 0.64714(12) 0.30682(14) 0.78693(6) 0.0231(3) Uani 1 1 d . . . H11A H 0.5833 0.2921 0.7997 0.035 Uiso 1 1 calc R . . H11B H 0.6443 0.2685 0.7524 0.035 Uiso 1 1 calc R . . H11C H 0.6581 0.3963 0.7842 0.035 Uiso 1 1 calc R . . C12 C 0.81142(10) 0.67534(11) 0.98796(5) 0.0129(2) Uani 1 1 d . . . C13 C 0.87474(10) 0.68726(12) 0.95098(5) 0.0143(2) Uani 1 1 d . . . H13 H 0.9324 0.6352 0.9532 0.017 Uiso 1 1 calc R . . C14 C 0.85581(10) 0.77397(12) 0.91062(5) 0.0155(3) Uani 1 1 d . . . H14 H 0.9003 0.7811 0.8857 0.019 Uiso 1 1 calc R . . C15 C 0.77128(11) 0.84987(12) 0.90720(5) 0.0169(3) Uani 1 1 d . . . C16 C 0.70659(11) 0.83839(13) 0.94399(6) 0.0212(3) Uani 1 1 d . . . H16 H 0.6484 0.8897 0.9415 0.025 Uiso 1 1 calc R . . C17 C 0.72670(11) 0.75285(13) 0.98407(6) 0.0185(3) Uani 1 1 d . . . H17 H 0.6827 0.7466 1.0092 0.022 Uiso 1 1 calc R . . C18 C 0.80344(12) 0.94705(15) 0.82876(6) 0.0249(3) Uani 1 1 d . . . H18A H 0.8737 0.9669 0.8434 0.037 Uiso 1 1 calc R . . H18B H 0.7756 1.0124 0.8043 0.037 Uiso 1 1 calc R . . H18C H 0.8010 0.8676 0.8102 0.037 Uiso 1 1 calc R . . C19 C 0.84292(14) 0.49019(14) 1.21249(6) 0.0245(3) Uani 1 1 d . . . H19A H 0.8671 0.4223 1.2365 0.037 Uiso 1 1 calc R . . H19B H 0.7704 0.4798 1.1999 0.037 Uiso 1 1 calc R . . H19C H 0.8547 0.5695 1.2309 0.037 Uiso 1 1 calc R . . C20 C 1.08246(12) 0.48233(14) 1.16987(7) 0.0232(3) Uani 1 1 d . . . H20A H 1.1060 0.5605 1.1869 0.035 Uiso 1 1 calc R . . H20B H 1.1139 0.4706 1.1386 0.035 Uiso 1 1 calc R . . H20C H 1.1012 0.4134 1.1942 0.035 Uiso 1 1 calc R . . C21 C 0.94646(10) 0.18289(12) 0.28003(5) 0.0134(2) Uani 1 1 d . . . C22 C 0.86671(10) 0.20618(12) 0.30678(5) 0.0147(2) Uani 1 1 d . . . H22 H 0.8041 0.1649 0.2963 0.018 Uiso 1 1 calc R . . C23 C 0.87638(10) 0.28875(12) 0.34867(5) 0.0152(2) Uani 1 1 d . . . H23 H 0.8208 0.3037 0.3664 0.018 Uiso 1 1 calc R . . C24 C 0.96797(11) 0.34906(12) 0.36433(5) 0.0167(3) Uani 1 1 d . . . C25 C 1.04873(11) 0.32722(13) 0.33765(6) 0.0195(3) Uani 1 1 d . . . H25 H 1.1115 0.3681 0.3483 0.023 Uiso 1 1 calc R . . C26 C 1.03742(11) 0.24617(13) 0.29580(5) 0.0172(3) Uani 1 1 d . . . H26 H 1.0923 0.2332 0.2774 0.021 Uiso 1 1 calc R . . C27 C 0.90196(12) 0.46732(14) 0.42894(6) 0.0209(3) Uani 1 1 d . . . H27A H 0.8489 0.5012 0.4021 0.031 Uiso 1 1 calc R . . H27B H 0.9235 0.5307 0.4555 0.031 Uiso 1 1 calc R . . H27C H 0.8756 0.3952 0.4454 0.031 Uiso 1 1 calc R . . C28 C 0.94405(10) -0.08884(11) 0.29426(5) 0.0127(2) Uani 1 1 d . . . C29 C 1.02785(10) -0.05956(12) 0.33150(5) 0.0143(2) Uani 1 1 d . . . H29 H 1.0770 -0.0035 0.3225 0.017 Uiso 1 1 calc R . . C30 C 1.04138(10) -0.11031(12) 0.38148(5) 0.0147(2) Uani 1 1 d . . . H30 H 1.0994 -0.0897 0.4062 0.018 Uiso 1 1 calc R . . C31 C 0.96928(10) -0.19159(12) 0.39492(5) 0.0150(2) Uani 1 1 d . . . C32 C 0.88709(11) -0.22633(13) 0.35769(5) 0.0174(3) Uani 1 1 d . . . H32 H 0.8393 -0.2845 0.3664 0.021 Uiso 1 1 calc R . . C33 C 0.87527(11) -0.17576(12) 0.30783(5) 0.0159(3) Uani 1 1 d . . . H33 H 0.8195 -0.2006 0.2824 0.019 Uiso 1 1 calc R . . C34 C 1.04488(12) -0.18969(14) 0.48485(5) 0.0224(3) Uani 1 1 d . . . H34A H 1.1129 -0.2139 0.4795 0.034 Uiso 1 1 calc R . . H34B H 1.0323 -0.2214 0.5187 0.034 Uiso 1 1 calc R . . H34C H 1.0395 -0.0991 0.4845 0.034 Uiso 1 1 calc R . . C35 C 0.95366(13) -0.01919(14) 0.05585(6) 0.0216(3) Uani 1 1 d . . . H35A H 0.9279 -0.0889 0.0333 0.032 Uiso 1 1 calc R . . H35B H 1.0245 -0.0345 0.0710 0.032 Uiso 1 1 calc R . . H35C H 0.9489 0.0572 0.0351 0.032 Uiso 1 1 calc R . . C36 C 0.71074(12) 0.02193(14) 0.08549(6) 0.0226(3) Uani 1 1 d . . . H36A H 0.7013 0.0993 0.0654 0.034 Uiso 1 1 calc R . . H36B H 0.6712 0.0250 0.1141 0.034 Uiso 1 1 calc R . . H36C H 0.6880 -0.0481 0.0625 0.034 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sn1 0.01693(6) 0.01674(5) 0.00965(5) -0.00001(3) 0.00247(4) -0.00015(3) Sn2 0.01598(6) 0.01682(5) 0.00945(5) 0.00066(3) 0.00205(4) -0.00006(3) S1 0.01722(16) 0.01233(14) 0.01116(14) 0.00148(11) 0.00152(12) 0.00069(11) S2 0.02598(18) 0.01348(14) 0.01180(15) -0.00159(11) 0.00159(13) 0.00125(12) S3 0.02363(18) 0.01367(14) 0.01123(15) 0.00183(11) 0.00241(12) -0.00098(12) S4 0.02448(18) 0.01282(14) 0.01090(15) -0.00057(11) 0.00048(12) -0.00012(12) O1 0.0246(5) 0.0230(5) 0.0119(5) -0.0036(4) -0.0014(4) 0.0010(4) O2 0.0237(6) 0.0253(5) 0.0253(6) 0.0140(4) 0.0084(4) 0.0097(4) O3 0.0190(5) 0.0253(5) 0.0242(5) -0.0131(4) 0.0062(4) -0.0060(4) O4 0.0243(5) 0.0238(5) 0.0114(4) 0.0050(4) 0.0001(4) -0.0026(4) C1 0.0117(6) 0.0148(6) 0.0116(6) 0.0013(5) 0.0018(5) 0.0006(5) C2 0.0141(6) 0.0147(6) 0.0103(6) -0.0005(4) 0.0022(5) 0.0011(5) C3 0.0148(6) 0.0150(6) 0.0104(6) 0.0008(4) 0.0020(5) -0.0001(5) C4 0.0135(6) 0.0151(6) 0.0111(6) 0.0001(5) 0.0010(5) -0.0006(5) C5 0.0151(6) 0.0119(5) 0.0105(6) 0.0005(4) 0.0019(5) -0.0010(4) C6 0.0163(7) 0.0180(6) 0.0154(6) -0.0015(5) 0.0003(5) 0.0037(5) C7 0.0205(7) 0.0190(6) 0.0175(7) -0.0037(5) 0.0021(5) 0.0051(5) C8 0.0191(7) 0.0145(6) 0.0124(6) -0.0001(5) 0.0018(5) -0.0026(5) C9 0.0144(6) 0.0149(6) 0.0144(6) 0.0022(5) -0.0004(5) -0.0014(5) C10 0.0147(6) 0.0135(6) 0.0154(6) 0.0006(5) 0.0036(5) 0.0010(5) C11 0.0294(8) 0.0244(7) 0.0133(7) 0.0009(5) -0.0030(6) -0.0022(6) C12 0.0151(6) 0.0111(5) 0.0122(6) -0.0002(4) 0.0013(5) 0.0001(4) C13 0.0132(6) 0.0148(6) 0.0147(6) 0.0007(5) 0.0018(5) 0.0022(5) C14 0.0150(6) 0.0164(6) 0.0153(6) 0.0019(5) 0.0034(5) 0.0004(5) C15 0.0178(7) 0.0153(6) 0.0173(7) 0.0047(5) 0.0016(5) 0.0015(5) C16 0.0188(7) 0.0207(7) 0.0254(7) 0.0063(6) 0.0076(6) 0.0089(5) C17 0.0193(7) 0.0184(6) 0.0195(7) 0.0026(5) 0.0086(5) 0.0038(5) C18 0.0271(8) 0.0279(8) 0.0206(7) 0.0108(6) 0.0064(6) 0.0050(6) C19 0.0342(9) 0.0245(7) 0.0174(7) -0.0013(5) 0.0115(7) -0.0013(6) C20 0.0197(8) 0.0257(7) 0.0227(8) -0.0007(6) -0.0014(6) -0.0030(6) C21 0.0173(6) 0.0121(5) 0.0107(6) 0.0017(4) 0.0016(5) -0.0003(5) C22 0.0142(6) 0.0160(6) 0.0136(6) 0.0002(5) 0.0009(5) -0.0019(5) C23 0.0146(6) 0.0165(6) 0.0151(6) -0.0007(5) 0.0041(5) -0.0005(5) C24 0.0193(7) 0.0141(6) 0.0164(6) -0.0025(5) 0.0028(5) -0.0014(5) C25 0.0159(7) 0.0197(7) 0.0230(7) -0.0048(5) 0.0039(5) -0.0052(5) C26 0.0165(7) 0.0175(6) 0.0188(7) -0.0021(5) 0.0059(5) -0.0017(5) C27 0.0237(8) 0.0185(6) 0.0217(7) -0.0056(5) 0.0066(6) -0.0010(5) C28 0.0153(6) 0.0115(5) 0.0113(6) 0.0004(4) 0.0018(5) 0.0013(4) C29 0.0152(6) 0.0132(6) 0.0144(6) 0.0004(5) 0.0019(5) -0.0017(5) C30 0.0153(6) 0.0141(6) 0.0137(6) -0.0007(5) -0.0009(5) 0.0000(5) C31 0.0177(7) 0.0147(6) 0.0122(6) 0.0018(5) 0.0016(5) 0.0022(5) C32 0.0165(7) 0.0186(6) 0.0169(7) 0.0035(5) 0.0020(5) -0.0043(5) C33 0.0144(6) 0.0176(6) 0.0144(6) 0.0011(5) -0.0013(5) -0.0022(5) C34 0.0281(8) 0.0257(7) 0.0117(6) 0.0004(5) -0.0021(6) 0.0032(6) C35 0.0273(8) 0.0230(7) 0.0162(7) -0.0008(5) 0.0093(6) 0.0001(6) C36 0.0206(8) 0.0235(7) 0.0218(8) 0.0005(6) -0.0017(6) -0.0004(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sn1 C19 2.1220(16) . ? Sn1 C20 2.1328(17) . ? Sn1 S1 2.4208(4) . ? Sn1 S2 2.4220(4) . ? Sn2 C35 2.1213(15) . ? Sn2 C36 2.1271(16) . ? Sn2 S4 2.4153(4) . ? Sn2 S3 2.4292(4) . ? S1 C1 1.7787(14) . ? S2 C2 1.7736(13) . ? S3 C3 1.7735(13) . ? S4 C4 1.7790(14) . ? O1 C8 1.3704(16) . ? O1 C11 1.4285(18) . ? O2 C15 1.3651(16) . ? O2 C18 1.4203(18) . ? O3 C24 1.3666(16) . ? O3 C27 1.4281(18) . ? O4 C31 1.3697(16) . ? O4 C34 1.4269(17) . ? C1 C2 1.3491(18) . ? C1 C5 1.4881(18) . ? C2 C12 1.4871(17) . ? C3 C4 1.3506(18) . ? C3 C21 1.4895(18) . ? C4 C28 1.4853(18) . ? C5 C10 1.3938(19) . ? C5 C6 1.4011(18) . ? C6 C7 1.3858(19) . ? C6 H6 0.9500 . ? C7 C8 1.393(2) . ? C7 H7 0.9500 . ? C8 C9 1.3891(19) . ? C9 C10 1.3921(18) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.3853(18) . ? C12 C17 1.4006(18) . ? C13 C14 1.3947(18) . ? C13 H13 0.9500 . ? C14 C15 1.3890(19) . ? C14 H14 0.9500 . ? C15 C16 1.395(2) . ? C16 C17 1.3820(19) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.3882(19) . ? C21 C26 1.3990(19) . ? C22 C23 1.3932(18) . ? C22 H22 0.9500 . ? C23 C24 1.3903(19) . ? C23 H23 0.9500 . ? C24 C25 1.396(2) . ? C25 C26 1.3815(19) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.3925(18) . ? C28 C33 1.3994(18) . ? C29 C30 1.3897(18) . ? C29 H29 0.9500 . ? C30 C31 1.3905(19) . ? C30 H30 0.9500 . ? C31 C32 1.3922(19) . ? C32 C33 1.3869(19) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C19 Sn1 C20 113.73(7) . . ? C19 Sn1 S1 117.59(5) . . ? C20 Sn1 S1 113.03(4) . . ? C19 Sn1 S2 107.76(5) . . ? C20 Sn1 S2 112.89(4) . . ? S1 Sn1 S2 89.197(15) . . ? C35 Sn2 C36 110.65(7) . . ? C35 Sn2 S4 115.56(4) . . ? C36 Sn2 S4 117.88(4) . . ? C35 Sn2 S3 111.57(4) . . ? C36 Sn2 S3 110.24(4) . . ? S4 Sn2 S3 88.960(15) . . ? C1 S1 Sn1 99.58(5) . . ? C2 S2 Sn1 99.31(5) . . ? C3 S3 Sn2 99.06(5) . . ? C4 S4 Sn2 99.32(5) . . ? C8 O1 C11 116.52(11) . . ? C15 O2 C18 117.92(11) . . ? C24 O3 C27 117.22(11) . . ? C31 O4 C34 116.96(11) . . ? C2 C1 C5 122.39(12) . . ? C2 C1 S1 124.80(10) . . ? C5 C1 S1 112.77(9) . . ? C1 C2 C12 123.43(12) . . ? C1 C2 S2 125.74(10) . . ? C12 C2 S2 110.82(9) . . ? C4 C3 C21 123.07(12) . . ? C4 C3 S3 125.14(10) . . ? C21 C3 S3 111.77(9) . . ? C3 C4 C28 122.09(12) . . ? C3 C4 S4 125.09(10) . . ? C28 C4 S4 112.79(9) . . ? C10 C5 C6 118.12(12) . . ? C10 C5 C1 120.60(12) . . ? C6 C5 C1 121.28(12) . . ? C7 C6 C5 120.81(13) . . ? C7 C6 H6 119.6 . . ? C5 C6 H6 119.6 . . ? C6 C7 C8 120.13(13) . . ? C6 C7 H7 119.9 . . ? C8 C7 H7 119.9 . . ? O1 C8 C9 124.31(12) . . ? O1 C8 C7 115.75(12) . . ? C9 C8 C7 119.93(13) . . ? C8 C9 C10 119.45(13) . . ? C8 C9 H9 120.3 . . ? C10 C9 H9 120.3 . . ? C9 C10 C5 121.48(12) . . ? C9 C10 H10 119.3 . . ? C5 C10 H10 119.3 . . ? O1 C11 H11A 109.5 . . ? O1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? O1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 C12 C17 118.42(12) . . ? C13 C12 C2 121.06(12) . . ? C17 C12 C2 120.49(12) . . ? C12 C13 C14 121.55(12) . . ? C12 C13 H13 119.2 . . ? C14 C13 H13 119.2 . . ? C15 C14 C13 119.33(13) . . ? C15 C14 H14 120.3 . . ? C13 C14 H14 120.3 . . ? O2 C15 C14 124.71(13) . . ? O2 C15 C16 115.57(12) . . ? C14 C15 C16 119.72(13) . . ? C17 C16 C15 120.37(13) . . ? C17 C16 H16 119.8 . . ? C15 C16 H16 119.8 . . ? C16 C17 C12 120.60(13) . . ? C16 C17 H17 119.7 . . ? C12 C17 H17 119.7 . . ? O2 C18 H18A 109.5 . . ? O2 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? O2 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Sn1 C19 H19A 109.5 . . ? Sn1 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Sn1 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? Sn1 C20 H20A 109.5 . . ? Sn1 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? Sn1 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 C26 118.14(12) . . ? C22 C21 C3 120.78(12) . . ? C26 C21 C3 121.08(12) . . ? C21 C22 C23 121.52(13) . . ? C21 C22 H22 119.2 . . ? C23 C22 H22 119.2 . . ? C24 C23 C22 119.47(13) . . ? C24 C23 H23 120.3 . . ? C22 C23 H23 120.3 . . ? O3 C24 C23 124.41(13) . . ? O3 C24 C25 115.85(12) . . ? C23 C24 C25 119.73(13) . . ? C26 C25 C24 120.01(13) . . ? C26 C25 H25 120.0 . . ? C24 C25 H25 120.0 . . ? C25 C26 C21 121.11(13) . . ? C25 C26 H26 119.4 . . ? C21 C26 H26 119.4 . . ? O3 C27 H27A 109.5 . . ? O3 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? O3 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C29 C28 C33 117.91(12) . . ? C29 C28 C4 120.44(12) . . ? C33 C28 C4 121.64(12) . . ? C30 C29 C28 121.60(12) . . ? C30 C29 H29 119.2 . . ? C28 C29 H29 119.2 . . ? C29 C30 C31 119.40(12) . . ? C29 C30 H30 120.3 . . ? C31 C30 H30 120.3 . . ? O4 C31 C30 124.01(12) . . ? O4 C31 C32 115.96(12) . . ? C30 C31 C32 120.02(12) . . ? C33 C32 C31 119.77(12) . . ? C33 C32 H32 120.1 . . ? C31 C32 H32 120.1 . . ? C32 C33 C28 121.15(13) . . ? C32 C33 H33 119.4 . . ? C28 C33 H33 119.4 . . ? O4 C34 H34A 109.5 . . ? O4 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? O4 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? Sn2 C35 H35A 109.5 . . ? Sn2 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? Sn2 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? Sn2 C36 H36A 109.5 . . ? Sn2 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? Sn2 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 28.83 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.443 _refine_diff_density_min -0.490 _refine_diff_density_rms 0.120 #===END # [Pt(S2C2Me2)2], Compound 4 data_jpd141 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H12 Pt S4' _chemical_formula_weight 431.51 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pt' 'Pt' -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.9778(14) _cell_length_b 7.1911(14) _cell_length_c 7.5203(15) _cell_angle_alpha 62.622(3) _cell_angle_beta 62.445(2) _cell_angle_gamma 88.558(3) _cell_volume 288.52(10) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2639 _cell_measurement_theta_min 3.2895 _cell_measurement_theta_max 28.3095 _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.483 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 202 _exptl_absorpt_coefficient_mu 12.833 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3405 _exptl_absorpt_correction_T_max 0.5898 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-AXS SMART APEX' _diffrn_measurement_method '/f and /w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 2607 _diffrn_reflns_av_R_equivalents 0.0196 _diffrn_reflns_av_sigmaI/netI 0.0274 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 3.28 _diffrn_reflns_theta_max 28.27 _reflns_number_total 1320 _reflns_number_gt 1320 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART (Bruker-AXS, 2000)' _computing_cell_refinement 'Bruker SMART (Bruker-AXS, 2000)' _computing_data_reduction 'Bruker SAINT+ (Bruker-AXS, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker-AXS, 2000a)' _computing_publication_material 'Bruker SHELXTL (Bruker-AXS, 2000a)' _publ_section_references ; Bruker-AXS (2000). SMART, Version 5.625, Madison, WI. Bruker-AXS (2000a). SHELXTL, Version 6.10, Madison, WI. Bruker-AXS (2004). SAINT+, Version 7.03, Madison, WI Sheldrick, G. M. (1997). SHELXS-97 and SHELXL-97. University of G\"ottingen, Germany. Sheldrick, G, M. (2002). SADABS, Version 2.05. University of G\"ottingen, Germany. ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0222P)^2^+0.1143P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1320 _refine_ls_number_parameters 63 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0160 _refine_ls_R_factor_gt 0.0160 _refine_ls_wR_factor_ref 0.0390 _refine_ls_wR_factor_gt 0.0390 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.5000 0.5000 0.5000 0.01411(6) Uani 1 2 d S . . S1 S 0.18971(12) 0.62775(12) 0.56866(13) 0.01699(15) Uani 1 1 d . . . S2 S 0.55793(12) 0.63267(12) 0.69471(13) 0.01659(15) Uani 1 1 d . . . C1 C 0.1795(5) 0.7462(5) 0.7231(5) 0.0163(6) Uani 1 1 d . . . C2 C 0.3424(5) 0.7485(5) 0.7796(5) 0.0172(6) Uani 1 1 d . . . C3 C -0.0131(5) 0.8472(5) 0.7951(6) 0.0202(6) Uani 1 1 d . . . H3A H -0.0980 0.7779 0.9650 0.030 Uiso 1 1 calc R . . H3B H -0.1099 0.8280 0.7403 0.030 Uiso 1 1 calc R . . H3C H 0.0433 1.0015 0.7269 0.030 Uiso 1 1 calc R . . C4 C 0.3372(6) 0.8522(5) 0.9145(6) 0.0198(6) Uani 1 1 d . . . H4A H 0.3298 1.0026 0.8355 0.030 Uiso 1 1 calc R . . H4B H 0.4722 0.8473 0.9251 0.030 Uiso 1 1 calc R . . H4C H 0.2061 0.7744 1.0713 0.030 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.01292(9) 0.01515(9) 0.01385(9) -0.00798(7) -0.00597(6) 0.00529(6) S1 0.0144(3) 0.0201(3) 0.0187(4) -0.0116(3) -0.0085(3) 0.0072(3) S2 0.0155(3) 0.0187(3) 0.0181(4) -0.0108(3) -0.0090(3) 0.0071(3) C1 0.0165(14) 0.0132(12) 0.0135(13) -0.0064(11) -0.0040(11) 0.0036(11) C2 0.0202(15) 0.0123(12) 0.0159(14) -0.0059(11) -0.0081(12) 0.0049(11) C3 0.0172(15) 0.0207(14) 0.0203(15) -0.0108(13) -0.0076(12) 0.0075(12) C4 0.0217(15) 0.0196(14) 0.0194(15) -0.0118(13) -0.0095(12) 0.0071(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 S2 2.2516(8) 2_666 ? Pt1 S2 2.2516(8) . ? Pt1 S1 2.2584(8) . ? Pt1 S1 2.2584(8) 2_666 ? S1 C1 1.706(3) . ? S2 C2 1.703(3) . ? C1 C2 1.388(5) . ? C1 C3 1.505(4) . ? C2 C4 1.499(4) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S2 Pt1 S2 180.0 2_666 . ? S2 Pt1 S1 92.14(3) 2_666 . ? S2 Pt1 S1 87.86(3) . . ? S2 Pt1 S1 87.86(3) 2_666 2_666 ? S2 Pt1 S1 92.14(3) . 2_666 ? S1 Pt1 S1 180.0 . 2_666 ? C1 S1 Pt1 105.07(11) . . ? C2 S2 Pt1 105.66(12) . . ? C2 C1 C3 121.7(3) . . ? C2 C1 S1 121.1(2) . . ? C3 C1 S1 117.2(2) . . ? C1 C2 C4 122.0(3) . . ? C1 C2 S2 120.3(2) . . ? C4 C2 S2 117.7(2) . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.924 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.114 _refine_diff_density_min -0.745 _refine_diff_density_rms 0.136 #===END # [Pt(S2C2(C6H4-p-OMe)2)2].DCE, Compound 5.DCE data_jpd265_0m _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis(1,2-bis(4-methoxyphenyl)ethen-1,2-dithiolato) platinum(II) 1,2-dichloroethane solvate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H28 O4 Pt S4, C2 H4 Cl2' _chemical_formula_sum 'C34 H32 Cl2 O4 Pt S4' _chemical_formula_weight 898.83 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pt' 'Pt' -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.140(6) _cell_length_b 12.279(8) _cell_length_c 17.818(12) _cell_angle_alpha 109.932(9) _cell_angle_beta 95.950(10) _cell_angle_gamma 109.328(8) _cell_volume 1720(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3022 _cell_measurement_theta_min 2.43 _cell_measurement_theta_max 26.66 _exptl_crystal_description Plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.735 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 888 _exptl_absorpt_coefficient_mu 4.513 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3864 _exptl_absorpt_correction_T_max 0.9151 _exptl_absorpt_process_details 'TWINABS (Sheldrick, 2008b)' _exptl_special_details ; The diffraction data were collected in three sets of 606 frames (0.3 deg. width in \w) at \f = 0, 120 and 240 deg. A scan time of 70 sec/frame was used. The crystal was determined to have two components (CELL_NOW, Sheldrick, 2008a) and consequently the raw data were integrated using the multi-component version of SAINT under control of the two-component instruction file produced by CELL_NOW. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-I CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 10629 _diffrn_reflns_av_R_equivalents 0.0456 _diffrn_reflns_av_sigmaI/netI 0.0925 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.25 _diffrn_reflns_theta_max 26.76 _reflns_number_total 6782 _reflns_number_gt 5503 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker APEX2 (Bruker-AXS, 2008)' _computing_cell_refinement 'Bruker SAINT (Bruker-AXS 2008a)' _computing_data_reduction 'Bruker SAINT (Bruker-AXS 2008a)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL(Bruker-AXS 2008b)' _computing_publication_material 'Bruker SHELXTL(Bruker-AXS 2008b)' _publ_section_references ; Bruker-AXS (2008). APEX2, Version 2008.6-1, Madison, WI. Bruker-AXS (2008a). SAINT, Version 7.60A, Madison, WI Bruker-AXS (2008b). SHELXTL, Version 2008/4, Madison, WI Sheldrick, G. M. (2008). SHELXS-97 and SHELXL-97. University of G\"ottingen, Germany. Sheldrick, G, M. (2008a). CELL_NOW, Version 2008/2 University of G\"ottingen, Germany. Sheldrick, G, M. (2008b). TWINABS, Version 2008/2. University of G\"ottingen, Germany. ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. H-atoms were placed in calculated positions (C---H = 0.95 - 0.98 \%A) and included as riding contributions with isotropic displacement parameters 1.2 - 1.5 times those of the attached carbon atoms. Refinement of the final structure against the one-component reflection set produced by TWINABS proved to be superior than refinement against the full two-component reflections set, presumably because one component was dominant (ca. 75%). ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0827P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Patterson _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6782 _refine_ls_number_parameters 410 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0710 _refine_ls_R_factor_gt 0.0562 _refine_ls_wR_factor_ref 0.1438 _refine_ls_wR_factor_gt 0.1384 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.70361(3) 0.92570(3) 0.55010(2) 0.01401(12) Uani 1 1 d . . . S1 S 0.7167(2) 0.74045(18) 0.53493(13) 0.0170(4) Uani 1 1 d . . . S2 S 0.7653(2) 0.89733(17) 0.42775(13) 0.0171(4) Uani 1 1 d . . . S3 S 0.6333(2) 0.95053(18) 0.67000(14) 0.0183(4) Uani 1 1 d . . . S4 S 0.7122(2) 1.11844(17) 0.57086(13) 0.0167(4) Uani 1 1 d . . . O1 O 0.9353(7) 0.2710(5) 0.3711(4) 0.0186(13) Uani 1 1 d U . . O2 O 0.8968(7) 0.5886(6) 0.0774(4) 0.0260(14) Uani 1 1 d . . . O3 O 0.4375(8) 1.2272(7) 1.0063(4) 0.0341(17) Uani 1 1 d . . . O4 O 0.7454(8) 1.6814(5) 0.7937(4) 0.0264(15) Uani 1 1 d . . . C1 C 0.7676(9) 0.6881(7) 0.4444(5) 0.0158(17) Uani 1 1 d . . . C2 C 0.7844(8) 0.7558(7) 0.3942(5) 0.0146(17) Uani 1 1 d . . . C3 C 0.6302(9) 1.0978(7) 0.7081(6) 0.0195(19) Uani 1 1 d . . . C4 C 0.6721(9) 1.1742(7) 0.6649(5) 0.0159(17) Uani 1 1 d . . . C5 C 0.8066(9) 0.5752(7) 0.4255(5) 0.0156(17) Uani 1 1 d . . . C6 C 0.7113(9) 0.4708(7) 0.4385(5) 0.0162(17) Uani 1 1 d . . . H6 H 0.6196 0.4719 0.4589 0.019 Uiso 1 1 calc R . . C7 C 0.7489(10) 0.3650(7) 0.4219(5) 0.0185(18) Uani 1 1 d . . . H7 H 0.6852 0.2949 0.4317 0.022 Uiso 1 1 calc R . . C8 C 0.8817(9) 0.3652(7) 0.3909(5) 0.0155(17) Uani 1 1 d . . . C9 C 0.9777(9) 0.4694(7) 0.3789(6) 0.0187(18) Uani 1 1 d . . . H9 H 1.0700 0.4688 0.3590 0.022 Uiso 1 1 calc R . . C10 C 0.9401(9) 0.5722(7) 0.3957(5) 0.0177(18) Uani 1 1 d . . . H10 H 1.0059 0.6426 0.3868 0.021 Uiso 1 1 calc R . . C11 C 0.8444(11) 0.1600(7) 0.3831(6) 0.025(2) Uani 1 1 d . . . H11A H 0.8308 0.1843 0.4395 0.038 Uiso 1 1 calc R . . H11B H 0.9013 0.1034 0.3738 0.038 Uiso 1 1 calc R . . H11C H 0.7392 0.1168 0.3441 0.038 Uiso 1 1 calc R . . C12 C 0.8082(9) 0.7107(7) 0.3104(6) 0.0170(18) Uani 1 1 d . . . C13 C 0.7241(9) 0.5869(7) 0.2541(5) 0.0170(18) Uani 1 1 d . . . H13 H 0.6473 0.5312 0.2703 0.020 Uiso 1 1 calc R . . C14 C 0.7468(9) 0.5410(8) 0.1757(5) 0.0195(18) Uani 1 1 d . . . H14 H 0.6866 0.4560 0.1388 0.023 Uiso 1 1 calc R . . C15 C 0.8597(9) 0.6221(8) 0.1526(5) 0.0189(18) Uani 1 1 d . . . C16 C 0.9435(9) 0.7478(7) 0.2062(6) 0.0192(18) Uani 1 1 d . . . H16 H 1.0184 0.8036 0.1893 0.023 Uiso 1 1 calc R . . C17 C 0.9179(9) 0.7913(7) 0.2838(5) 0.0168(17) Uani 1 1 d . . . H17 H 0.9755 0.8771 0.3200 0.020 Uiso 1 1 calc R . . C18 C 0.8100(13) 0.4601(9) 0.0201(7) 0.036(2) Uani 1 1 d . . . H18A H 0.8149 0.4036 0.0471 0.054 Uiso 1 1 calc R . . H18B H 0.8578 0.4430 -0.0272 0.054 Uiso 1 1 calc R . . H18C H 0.6982 0.4462 0.0012 0.054 Uiso 1 1 calc R . . C19 C 0.5783(9) 1.1321(7) 0.7852(5) 0.0137(16) Uani 1 1 d . . . C20 C 0.6291(10) 1.1030(7) 0.8499(6) 0.0199(18) Uani 1 1 d . . . H20 H 0.6997 1.0603 0.8439 0.024 Uiso 1 1 calc R . . C21 C 0.5796(10) 1.1344(8) 0.9227(6) 0.024(2) Uani 1 1 d . . . H21 H 0.6156 1.1133 0.9657 0.029 Uiso 1 1 calc R . . C22 C 0.4769(10) 1.1969(8) 0.9316(6) 0.0229(19) Uani 1 1 d . . . C23 C 0.4225(10) 1.2242(8) 0.8675(6) 0.0205(19) Uani 1 1 d . . . H23 H 0.3504 1.2655 0.8729 0.025 Uiso 1 1 calc R . . C24 C 0.4727(9) 1.1917(7) 0.7960(5) 0.0194(18) Uani 1 1 d . . . H24 H 0.4336 1.2107 0.7526 0.023 Uiso 1 1 calc R . . C25 C 0.3455(12) 1.3048(11) 1.0223(7) 0.038(3) Uani 1 1 d . . . H25A H 0.4013 1.3826 1.0153 0.057 Uiso 1 1 calc R . . H25B H 0.3329 1.3254 1.0788 0.057 Uiso 1 1 calc R . . H25C H 0.2400 1.2589 0.9837 0.057 Uiso 1 1 calc R . . C26 C 0.6896(9) 1.3075(7) 0.6970(5) 0.0150(17) Uani 1 1 d . . . C27 C 0.7748(10) 1.3894(8) 0.7774(6) 0.0203(18) Uani 1 1 d . . . H27 H 0.8217 1.3591 0.8117 0.024 Uiso 1 1 calc R . . C28 C 0.7926(9) 1.5129(7) 0.8081(5) 0.0179(18) Uani 1 1 d . . . H28 H 0.8496 1.5667 0.8634 0.021 Uiso 1 1 calc R . . C29 C 0.7262(9) 1.5602(7) 0.7576(5) 0.0160(17) Uani 1 1 d . . . C30 C 0.6444(9) 1.4795(7) 0.6770(6) 0.0171(17) Uani 1 1 d . . . H30 H 0.5995 1.5099 0.6421 0.021 Uiso 1 1 calc R . . C31 C 0.6271(9) 1.3543(7) 0.6468(5) 0.0170(17) Uani 1 1 d . . . H31 H 0.5719 1.3004 0.5912 0.020 Uiso 1 1 calc R . . C32 C 0.6687(13) 1.7286(8) 0.7465(6) 0.033(2) Uani 1 1 d . . . H32A H 0.7167 1.7297 0.6999 0.050 Uiso 1 1 calc R . . H32B H 0.6819 1.8143 0.7811 0.050 Uiso 1 1 calc R . . H32C H 0.5546 1.6743 0.7259 0.050 Uiso 1 1 calc R . . C33 C 0.1657(17) 0.8729(12) 0.8296(8) 0.058(4) Uani 1 1 d . . . H33A H 0.2349 0.9440 0.8184 0.069 Uiso 1 1 calc R . . H33B H 0.0725 0.8197 0.7818 0.069 Uiso 1 1 calc R . . C34 C 0.1125(16) 0.9202(12) 0.9038(9) 0.055(3) Uani 1 1 d . . . H34A H 0.2063 0.9724 0.9514 0.066 Uiso 1 1 calc R . . H34B H 0.0438 0.8486 0.9147 0.066 Uiso 1 1 calc R . . Cl1 Cl 0.2740(5) 0.7829(3) 0.8451(2) 0.0736(11) Uani 1 1 d . . . Cl2 Cl 0.0018(5) 1.0133(3) 0.8918(3) 0.0834(13) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.01668(16) 0.00793(15) 0.0143(2) 0.00335(11) 0.00365(12) 0.00223(11) S1 0.0224(10) 0.0139(9) 0.0146(12) 0.0065(8) 0.0069(9) 0.0055(8) S2 0.0229(9) 0.0115(8) 0.0159(12) 0.0055(8) 0.0067(9) 0.0051(7) S3 0.0243(10) 0.0132(9) 0.0187(12) 0.0077(8) 0.0081(9) 0.0067(8) S4 0.0193(9) 0.0125(9) 0.0163(12) 0.0055(8) 0.0048(9) 0.0038(7) O1 0.027(3) 0.004(2) 0.027(3) 0.007(2) 0.009(2) 0.006(2) O2 0.029(3) 0.028(3) 0.011(3) 0.002(3) 0.006(3) 0.004(3) O3 0.041(4) 0.054(4) 0.022(4) 0.018(3) 0.016(3) 0.030(4) O4 0.044(4) 0.012(3) 0.027(4) 0.009(3) 0.009(3) 0.013(3) C1 0.012(3) 0.018(4) 0.016(5) 0.007(3) 0.002(3) 0.003(3) C2 0.009(3) 0.012(3) 0.016(5) 0.001(3) 0.004(3) 0.002(3) C3 0.018(4) 0.014(4) 0.026(5) 0.009(3) 0.006(4) 0.004(3) C4 0.013(3) 0.013(4) 0.021(5) 0.008(3) 0.005(3) 0.003(3) C5 0.019(4) 0.011(3) 0.010(4) 0.000(3) 0.001(3) 0.002(3) C6 0.012(3) 0.013(4) 0.020(5) 0.009(3) 0.006(3) -0.002(3) C7 0.023(4) 0.017(4) 0.019(5) 0.012(3) 0.009(4) 0.006(3) C8 0.023(4) 0.008(3) 0.013(5) 0.002(3) 0.001(3) 0.006(3) C9 0.019(4) 0.017(4) 0.023(5) 0.010(3) 0.011(4) 0.007(3) C10 0.015(4) 0.011(3) 0.022(5) 0.009(3) 0.001(3) -0.002(3) C11 0.036(5) 0.011(4) 0.039(6) 0.017(4) 0.024(5) 0.009(3) C12 0.016(4) 0.014(4) 0.022(5) 0.006(3) 0.008(3) 0.008(3) C13 0.018(4) 0.008(3) 0.021(5) 0.005(3) 0.002(3) 0.001(3) C14 0.021(4) 0.019(4) 0.016(5) 0.008(3) 0.004(4) 0.004(3) C15 0.021(4) 0.020(4) 0.015(5) 0.005(3) 0.005(4) 0.009(3) C16 0.020(4) 0.012(4) 0.023(5) 0.008(3) 0.010(4) 0.000(3) C17 0.020(4) 0.016(4) 0.013(5) 0.008(3) 0.002(3) 0.003(3) C18 0.046(6) 0.029(5) 0.026(6) 0.005(4) 0.008(5) 0.010(4) C19 0.017(4) 0.011(3) 0.007(4) 0.000(3) 0.002(3) 0.001(3) C20 0.029(4) 0.014(4) 0.022(5) 0.013(3) 0.009(4) 0.008(3) C21 0.031(5) 0.027(4) 0.019(5) 0.012(4) 0.009(4) 0.012(4) C22 0.026(4) 0.022(4) 0.018(5) 0.007(4) 0.010(4) 0.006(4) C23 0.021(4) 0.022(4) 0.023(5) 0.011(4) 0.008(4) 0.013(3) C24 0.020(4) 0.016(4) 0.016(5) 0.008(3) -0.001(4) 0.001(3) C25 0.038(5) 0.056(7) 0.028(6) 0.013(5) 0.017(5) 0.030(5) C26 0.017(4) 0.013(4) 0.012(4) 0.003(3) 0.009(3) 0.004(3) C27 0.028(4) 0.018(4) 0.020(5) 0.009(3) 0.011(4) 0.012(3) C28 0.020(4) 0.013(4) 0.013(5) 0.001(3) 0.000(3) 0.004(3) C29 0.016(4) 0.012(3) 0.024(5) 0.011(3) 0.008(3) 0.004(3) C30 0.017(4) 0.018(4) 0.021(5) 0.013(3) 0.008(4) 0.007(3) C31 0.016(4) 0.011(3) 0.017(5) 0.004(3) 0.008(3) -0.004(3) C32 0.061(7) 0.021(4) 0.023(6) 0.010(4) 0.000(5) 0.023(5) C33 0.088(10) 0.052(7) 0.035(8) 0.023(6) 0.002(7) 0.028(7) C34 0.067(8) 0.045(7) 0.050(9) 0.028(6) -0.002(7) 0.015(6) Cl1 0.109(3) 0.059(2) 0.056(2) 0.0186(18) 0.018(2) 0.042(2) Cl2 0.076(2) 0.0488(19) 0.111(4) 0.028(2) -0.005(2) 0.0195(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 S4 2.240(2) . ? Pt1 S1 2.243(2) . ? Pt1 S3 2.245(3) . ? Pt1 S2 2.249(3) . ? S1 C1 1.696(9) . ? S2 C2 1.710(7) . ? S3 C3 1.712(8) . ? S4 C4 1.709(9) . ? O1 C8 1.355(8) . ? O1 C11 1.443(9) . ? O2 C15 1.375(11) . ? O2 C18 1.437(11) . ? O3 C22 1.375(11) . ? O3 C25 1.445(10) . ? O4 C29 1.346(9) . ? O4 C32 1.418(11) . ? C1 C2 1.402(12) . ? C1 C5 1.482(10) . ? C2 C12 1.472(12) . ? C3 C4 1.391(12) . ? C3 C19 1.472(12) . ? C4 C26 1.484(10) . ? C5 C10 1.387(11) . ? C5 C6 1.400(11) . ? C6 C7 1.395(11) . ? C7 C8 1.384(11) . ? C8 C9 1.390(11) . ? C9 C10 1.361(10) . ? C12 C13 1.391(10) . ? C12 C17 1.403(12) . ? C13 C14 1.383(12) . ? C14 C15 1.384(12) . ? C15 C16 1.393(11) . ? C16 C17 1.378(12) . ? C19 C24 1.383(11) . ? C19 C20 1.396(12) . ? C20 C21 1.390(13) . ? C21 C22 1.386(11) . ? C22 C23 1.384(13) . ? C23 C24 1.374(13) . ? C26 C31 1.385(12) . ? C26 C27 1.392(12) . ? C27 C28 1.370(11) . ? C28 C29 1.412(12) . ? C29 C30 1.385(12) . ? C30 C31 1.391(10) . ? C33 C34 1.456(18) . ? C33 Cl1 1.774(12) . ? C34 Cl2 1.807(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S4 Pt1 S1 175.21(7) . . ? S4 Pt1 S3 87.70(7) . . ? S1 Pt1 S3 92.31(8) . . ? S4 Pt1 S2 92.51(8) . . ? S1 Pt1 S2 87.65(7) . . ? S3 Pt1 S2 178.08(8) . . ? C1 S1 Pt1 106.1(3) . . ? C2 S2 Pt1 106.0(3) . . ? C3 S3 Pt1 106.2(3) . . ? C4 S4 Pt1 105.8(3) . . ? C8 O1 C11 116.6(6) . . ? C15 O2 C18 116.4(7) . . ? C22 O3 C25 117.4(7) . . ? C29 O4 C32 117.1(7) . . ? C2 C1 C5 122.4(7) . . ? C2 C1 S1 120.7(6) . . ? C5 C1 S1 116.7(6) . . ? C1 C2 C12 124.7(7) . . ? C1 C2 S2 119.4(6) . . ? C12 C2 S2 115.7(6) . . ? C4 C3 C19 125.0(7) . . ? C4 C3 S3 119.4(7) . . ? C19 C3 S3 115.6(6) . . ? C3 C4 C26 123.4(8) . . ? C3 C4 S4 120.7(6) . . ? C26 C4 S4 115.9(6) . . ? C10 C5 C6 118.9(7) . . ? C10 C5 C1 120.3(7) . . ? C6 C5 C1 120.8(7) . . ? C7 C6 C5 121.1(7) . . ? C8 C7 C6 118.1(8) . . ? O1 C8 C7 126.1(7) . . ? O1 C8 C9 112.9(7) . . ? C7 C8 C9 121.0(7) . . ? C10 C9 C8 120.3(7) . . ? C9 C10 C5 120.7(8) . . ? C13 C12 C17 117.0(8) . . ? C13 C12 C2 121.8(8) . . ? C17 C12 C2 121.2(7) . . ? C14 C13 C12 123.2(8) . . ? C13 C14 C15 118.3(8) . . ? O2 C15 C14 124.5(7) . . ? O2 C15 C16 115.1(8) . . ? C14 C15 C16 120.4(8) . . ? C17 C16 C15 120.1(8) . . ? C16 C17 C12 121.1(7) . . ? C24 C19 C20 116.9(8) . . ? C24 C19 C3 121.3(8) . . ? C20 C19 C3 121.8(7) . . ? C21 C20 C19 122.1(7) . . ? C22 C21 C20 119.0(9) . . ? O3 C22 C23 125.2(8) . . ? O3 C22 C21 115.1(8) . . ? C23 C22 C21 119.7(8) . . ? C24 C23 C22 120.1(7) . . ? C23 C24 C19 122.2(8) . . ? C31 C26 C27 118.6(7) . . ? C31 C26 C4 120.8(7) . . ? C27 C26 C4 120.6(8) . . ? C28 C27 C26 121.4(8) . . ? C27 C28 C29 120.1(8) . . ? O4 C29 C30 125.5(8) . . ? O4 C29 C28 115.9(8) . . ? C30 C29 C28 118.5(7) . . ? C29 C30 C31 120.7(8) . . ? C26 C31 C30 120.6(8) . . ? C34 C33 Cl1 108.1(9) . . ? C33 C34 Cl2 110.2(9) . . ? _diffrn_measured_fraction_theta_max 0.923 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.953 _refine_diff_density_max 3.426 _refine_diff_density_min -4.400 _refine_diff_density_rms 0.268 #===END # [Pt(S2C2(C6H4-p-OMe)2)2(dppe)], Compound 6 data_jpd294 _audit_creation_method SHELXL-97 _chemical_name_systematic ; (1,2-bis(diphenylphosphino)ethane)bis(1,2-bis(4-methoxyphenyl) ethene-1,2-dithiolato)platinum(IV) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C58 H52 O4 P2 Pt S4' _chemical_formula_sum 'C58 H52 O4 P2 Pt S4' _chemical_formula_weight 1198.27 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pt' 'Pt' -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pccn _symmetry_space_group_name_Hall '-P 2ab 2ac' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-x, y+1/2, -z+1/2' 'x+1/2, -y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'x, -y-1/2, z-1/2' '-x-1/2, y, z-1/2' _cell_length_a 17.8597(12) _cell_length_b 18.7052(12) _cell_length_c 16.6577(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5564.8(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9689 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 28.31 _exptl_crystal_description Plate _exptl_crystal_colour blue _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.430 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2416 _exptl_absorpt_coefficient_mu 2.773 _exptl_absorpt_correction_type 'integration numerical gaussian' _exptl_absorpt_correction_T_min 0.7969 _exptl_absorpt_correction_T_max 0.9364 _exptl_absorpt_process_details 'APEX2 SCALE module (Bruker-AXS 2009)' _exptl_special_details ; The diffraction data were obtained from 3 sets of 400 frames, each of width 0.5 deg. in \w, collected at \f = 0.00, 90.00 and 180.00 deg. and 2 sets of 800 frames, each of width 0.45 deg in \f, collected at \w = -30.00 and 210.00 deg. The scan time was 15 sec/frame. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-I CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 93487 _diffrn_reflns_av_R_equivalents 0.0506 _diffrn_reflns_av_sigmaI/netI 0.0217 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 28.32 _reflns_number_total 6935 _reflns_number_gt 5831 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker APEX2 (Bruker-AXS, 2009)' _computing_cell_refinement 'Bruker SAINT (Bruker-AXS 2008)' _computing_data_reduction 'Bruker SAINT (Bruker-AXS 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL(Bruker-AXS 2008a)' _computing_publication_material 'Bruker SHELXTL(Bruker-AXS 2008a)' _publ_section_references ; Bruker-AXS (2009). APEX2, Version 2009.3-0, Madison, WI. Bruker-AXS (2008). SAINT, Version 7.60A, Madison, WI Bruker-AXS (2008a). SHELXTL, Version 2008/4, Madison, WI Sheldrick, G. M. (2008). SHELXS-97 and SHELXL-97. University of G\"ottingen, Germany. Spek, A. L. (2009). PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, THe Netherlands. ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. H-atoms were placed in calculated positions (C---H = 0.95 - 0.98 \%A) and included as riding contributions with isotropic displacement parameters 1.2 - 1.5 times those of the attached carbon atoms. In the final stages of refinement a region of residual density corresponding to ca. four carbon atoms and well-separated from the main molecule was observed. This could not be modeled by any reasonable ordered or disordered molecule of the solvents used for crystallization and so was removed with the SQUEEZE option of the PLATON package (Spek, 2009). ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0252P)^2^+3.5645P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6935 _refine_ls_number_parameters 314 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0322 _refine_ls_R_factor_gt 0.0236 _refine_ls_wR_factor_ref 0.0566 _refine_ls_wR_factor_gt 0.0538 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.091 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.2500 0.7500 0.215624(6) 0.01130(4) Uani 1 2 d S . . S1 S 0.14996(3) 0.66765(3) 0.20526(3) 0.01523(11) Uani 1 1 d . . . S2 S 0.18852(3) 0.82130(3) 0.11832(3) 0.01502(11) Uani 1 1 d . . . P1 P 0.19034(3) 0.81383(3) 0.31792(3) 0.01361(11) Uani 1 1 d . . . O1 O -0.12689(10) 0.51405(10) 0.02179(11) 0.0297(4) Uani 1 1 d . . . O2 O -0.11154(11) 0.92873(11) -0.07860(11) 0.0387(5) Uani 1 1 d . . . C1 C 0.09094(12) 0.70914(12) 0.13446(12) 0.0153(4) Uani 1 1 d . . . C2 C 0.10300(12) 0.77490(12) 0.10267(13) 0.0151(4) Uani 1 1 d . . . C3 C 0.03139(12) 0.65980(12) 0.10623(13) 0.0166(4) Uani 1 1 d . . . C4 C -0.01657(13) 0.62251(13) 0.15752(14) 0.0206(5) Uani 1 1 d . . . H4 H -0.0133 0.6301 0.2138 0.025 Uiso 1 1 calc R . . C5 C -0.06871(14) 0.57462(13) 0.12776(15) 0.0244(5) Uani 1 1 d . . . H5 H -0.1011 0.5500 0.1636 0.029 Uiso 1 1 calc R . . C6 C -0.07389(14) 0.56242(14) 0.04551(15) 0.0225(5) Uani 1 1 d . . . C7 C -0.02647(13) 0.59800(13) -0.00625(15) 0.0220(5) Uani 1 1 d . . . H7 H -0.0296 0.5898 -0.0624 0.026 Uiso 1 1 calc R . . C8 C 0.02547(13) 0.64554(13) 0.02396(14) 0.0204(5) Uani 1 1 d . . . H8 H 0.0582 0.6693 -0.0122 0.024 Uiso 1 1 calc R . . C9 C 0.04799(13) 0.81452(12) 0.05351(13) 0.0174(4) Uani 1 1 d . . . C10 C -0.02935(13) 0.80689(14) 0.06547(14) 0.0232(5) Uani 1 1 d . . . H10 H -0.0469 0.7748 0.1055 0.028 Uiso 1 1 calc R . . C11 C -0.08054(14) 0.84504(15) 0.02033(15) 0.0275(6) Uani 1 1 d . . . H11 H -0.1327 0.8385 0.0290 0.033 Uiso 1 1 calc R . . C12 C -0.05592(15) 0.89313(15) -0.03786(14) 0.0254(6) Uani 1 1 d . . . C13 C 0.02025(14) 0.90344(13) -0.04977(14) 0.0214(5) Uani 1 1 d . . . H13 H 0.0376 0.9369 -0.0884 0.026 Uiso 1 1 calc R . . C14 C 0.07069(13) 0.86395(12) -0.00419(13) 0.0182(5) Uani 1 1 d . . . H14 H 0.1228 0.8709 -0.0127 0.022 Uiso 1 1 calc R . . C15 C -0.13696(15) 0.50436(15) -0.06273(16) 0.0308(6) Uani 1 1 d . . . H15A H -0.1529 0.5496 -0.0870 0.046 Uiso 1 1 calc R . . H15B H -0.1753 0.4678 -0.0721 0.046 Uiso 1 1 calc R . . H15C H -0.0896 0.4891 -0.0869 0.046 Uiso 1 1 calc R . . C16 C -0.08783(18) 0.98166(17) -0.13444(16) 0.0416(8) Uani 1 1 d . . . H16A H -0.0564 1.0169 -0.1070 0.062 Uiso 1 1 calc R . . H16B H -0.1318 1.0056 -0.1573 0.062 Uiso 1 1 calc R . . H16C H -0.0590 0.9589 -0.1775 0.062 Uiso 1 1 calc R . . C17 C 0.20889(11) 0.76192(11) 0.40891(13) 0.0158(5) Uani 1 1 d . . . H17A H 0.1986 0.7915 0.4570 0.019 Uiso 1 1 calc R . . H17B H 0.1757 0.7195 0.4106 0.019 Uiso 1 1 calc R . . C18 C 0.23038(12) 0.90176(12) 0.33420(14) 0.0169(4) Uani 1 1 d . . . C19 C 0.24020(13) 0.94800(13) 0.26883(15) 0.0202(5) Uani 1 1 d . . . H19 H 0.2237 0.9337 0.2170 0.024 Uiso 1 1 calc R . . C20 C 0.27363(15) 1.01411(14) 0.27871(16) 0.0264(5) Uani 1 1 d . . . H20 H 0.2786 1.0456 0.2343 0.032 Uiso 1 1 calc R . . C21 C 0.29994(15) 1.03421(14) 0.35383(17) 0.0309(6) Uani 1 1 d . . . H21 H 0.3244 1.0789 0.3604 0.037 Uiso 1 1 calc R . . C22 C 0.29062(14) 0.98935(14) 0.41908(16) 0.0272(6) Uani 1 1 d . . . H22 H 0.3083 1.0035 0.4705 0.033 Uiso 1 1 calc R . . C23 C 0.25534(13) 0.92357(13) 0.40962(14) 0.0209(5) Uani 1 1 d . . . H23 H 0.2482 0.8933 0.4548 0.025 Uiso 1 1 calc R . . C24 C 0.08982(12) 0.82376(12) 0.30917(12) 0.0161(4) Uani 1 1 d . . . C25 C 0.04216(13) 0.76726(13) 0.32861(14) 0.0198(5) Uani 1 1 d . . . H25 H 0.0622 0.7241 0.3498 0.024 Uiso 1 1 calc R . . C26 C -0.03455(14) 0.77396(14) 0.31704(15) 0.0241(5) Uani 1 1 d . . . H26 H -0.0670 0.7358 0.3313 0.029 Uiso 1 1 calc R . . C27 C -0.06395(13) 0.83626(15) 0.28474(14) 0.0266(6) Uani 1 1 d . . . H27 H -0.1163 0.8401 0.2755 0.032 Uiso 1 1 calc R . . C28 C -0.01744(14) 0.89251(14) 0.26601(15) 0.0265(6) Uani 1 1 d . . . H28 H -0.0379 0.9354 0.2448 0.032 Uiso 1 1 calc R . . C29 C 0.05959(13) 0.88687(13) 0.27806(14) 0.0218(5) Uani 1 1 d . . . H29 H 0.0915 0.9259 0.2651 0.026 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.01265(6) 0.01134(6) 0.00991(6) 0.000 0.000 0.00056(4) S1 0.0161(2) 0.0145(3) 0.0151(2) 0.0022(2) -0.0016(2) -0.0009(2) S2 0.0169(2) 0.0144(3) 0.0138(2) 0.0023(2) -0.0016(2) -0.0014(2) P1 0.0144(2) 0.0142(3) 0.0122(2) 0.0000(2) 0.0000(2) 0.0022(2) O1 0.0289(10) 0.0329(11) 0.0271(10) -0.0033(8) -0.0021(8) -0.0143(8) O2 0.0338(11) 0.0526(13) 0.0297(10) 0.0160(9) -0.0018(8) 0.0234(10) C1 0.0131(10) 0.0195(11) 0.0132(10) -0.0013(9) -0.0001(8) 0.0019(8) C2 0.0160(10) 0.0163(10) 0.0131(10) 0.0008(8) 0.0011(8) 0.0002(8) C3 0.0159(10) 0.0170(11) 0.0168(11) 0.0032(9) -0.0016(9) 0.0008(8) C4 0.0234(11) 0.0235(12) 0.0148(11) 0.0022(9) 0.0016(9) -0.0024(9) C5 0.0264(12) 0.0248(13) 0.0220(12) 0.0032(10) 0.0030(10) -0.0088(10) C6 0.0194(11) 0.0220(12) 0.0262(13) -0.0010(10) -0.0021(10) -0.0042(10) C7 0.0235(12) 0.0252(13) 0.0175(11) 0.0003(10) -0.0010(10) -0.0037(10) C8 0.0199(11) 0.0238(13) 0.0173(11) 0.0005(9) 0.0008(9) -0.0052(10) C9 0.0204(11) 0.0175(11) 0.0142(10) -0.0015(9) -0.0019(9) 0.0030(9) C10 0.0206(11) 0.0290(13) 0.0200(12) 0.0062(10) 0.0023(9) 0.0033(10) C11 0.0184(12) 0.0400(16) 0.0241(12) 0.0039(11) 0.0024(10) 0.0083(11) C12 0.0279(13) 0.0313(15) 0.0169(11) 0.0013(10) -0.0035(10) 0.0148(11) C13 0.0298(13) 0.0188(12) 0.0156(11) 0.0020(9) -0.0010(10) 0.0064(10) C14 0.0202(11) 0.0186(11) 0.0159(11) -0.0001(9) -0.0010(9) 0.0021(9) C15 0.0325(14) 0.0310(15) 0.0290(14) -0.0049(11) -0.0090(12) -0.0089(12) C16 0.0532(19) 0.0467(18) 0.0250(14) 0.0126(13) -0.0007(13) 0.0268(15) C17 0.0144(10) 0.0194(12) 0.0137(10) 0.0016(8) 0.0023(8) 0.0033(8) C18 0.0159(10) 0.0151(10) 0.0196(11) -0.0034(9) -0.0009(8) 0.0034(8) C19 0.0240(12) 0.0164(11) 0.0204(11) -0.0024(9) 0.0000(9) 0.0013(9) C20 0.0308(13) 0.0190(12) 0.0293(14) -0.0018(10) 0.0052(11) -0.0001(10) C21 0.0321(14) 0.0208(13) 0.0397(15) -0.0088(12) 0.0046(12) -0.0032(11) C22 0.0247(13) 0.0291(14) 0.0277(13) -0.0118(11) -0.0038(10) 0.0008(10) C23 0.0210(11) 0.0202(11) 0.0215(11) -0.0035(9) -0.0026(10) 0.0052(10) C24 0.0161(10) 0.0211(11) 0.0112(9) -0.0021(9) 0.0020(8) 0.0041(9) C25 0.0202(11) 0.0229(12) 0.0163(11) -0.0003(9) 0.0020(9) 0.0008(9) C26 0.0195(11) 0.0289(13) 0.0238(12) -0.0033(11) 0.0028(10) -0.0030(10) C27 0.0150(11) 0.0407(15) 0.0242(13) -0.0056(11) -0.0014(9) 0.0044(10) C28 0.0216(12) 0.0303(14) 0.0275(13) 0.0042(11) -0.0019(10) 0.0110(10) C29 0.0212(11) 0.0216(12) 0.0225(12) 0.0043(10) -0.0002(9) 0.0031(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 P1 2.3376(6) 2_565 ? Pt1 P1 2.3376(6) . ? Pt1 S1 2.3654(6) 2_565 ? Pt1 S1 2.3654(5) . ? Pt1 S2 2.3688(5) 2_565 ? Pt1 S2 2.3688(5) . ? S1 C1 1.762(2) . ? S2 C2 1.776(2) . ? P1 C24 1.811(2) . ? P1 C18 1.814(2) . ? P1 C17 1.830(2) . ? O1 C6 1.368(3) . ? O1 C15 1.431(3) . ? O2 C12 1.375(3) . ? O2 C16 1.423(3) . ? C1 C2 1.356(3) . ? C1 C3 1.484(3) . ? C2 C9 1.478(3) . ? C3 C4 1.397(3) . ? C3 C8 1.400(3) . ? C4 C5 1.384(3) . ? C4 H4 0.9500 . ? C5 C6 1.392(3) . ? C5 H5 0.9500 . ? C6 C7 1.380(3) . ? C7 C8 1.380(3) . ? C7 H7 0.9500 . ? C8 H8 0.9500 . ? C9 C14 1.394(3) . ? C9 C10 1.403(3) . ? C10 C11 1.382(3) . ? C10 H10 0.9500 . ? C11 C12 1.394(4) . ? C11 H11 0.9500 . ? C12 C13 1.388(4) . ? C13 C14 1.391(3) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C17 1.535(4) 2_565 ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C23 1.394(3) . ? C18 C19 1.402(3) . ? C19 C20 1.383(3) . ? C19 H19 0.9500 . ? C20 C21 1.389(4) . ? C20 H20 0.9500 . ? C21 C22 1.383(4) . ? C21 H21 0.9500 . ? C22 C23 1.391(3) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 C25 1.395(3) . ? C24 C29 1.398(3) . ? C25 C26 1.389(3) . ? C25 H25 0.9500 . ? C26 C27 1.387(4) . ? C26 H26 0.9500 . ? C27 C28 1.376(4) . ? C27 H27 0.9500 . ? C28 C29 1.394(3) . ? C28 H28 0.9500 . ? C29 H29 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Pt1 P1 86.41(3) 2_565 . ? P1 Pt1 S1 92.38(2) 2_565 2_565 ? P1 Pt1 S1 93.721(19) . 2_565 ? P1 Pt1 S1 93.721(19) 2_565 . ? P1 Pt1 S1 92.38(2) . . ? S1 Pt1 S1 171.63(3) 2_565 . ? P1 Pt1 S2 89.996(19) 2_565 2_565 ? P1 Pt1 S2 176.035(19) . 2_565 ? S1 Pt1 S2 88.085(19) 2_565 2_565 ? S1 Pt1 S2 86.189(19) . 2_565 ? P1 Pt1 S2 176.035(19) 2_565 . ? P1 Pt1 S2 89.995(19) . . ? S1 Pt1 S2 86.191(19) 2_565 . ? S1 Pt1 S2 88.085(19) . . ? S2 Pt1 S2 93.65(3) 2_565 . ? C1 S1 Pt1 102.35(8) . . ? C2 S2 Pt1 102.94(7) . . ? C24 P1 C18 108.06(10) . . ? C24 P1 C17 107.49(10) . . ? C18 P1 C17 106.61(10) . . ? C24 P1 Pt1 116.47(7) . . ? C18 P1 Pt1 113.10(7) . . ? C17 P1 Pt1 104.49(7) . . ? C6 O1 C15 117.08(19) . . ? C12 O2 C16 116.4(2) . . ? C2 C1 C3 123.63(19) . . ? C2 C1 S1 124.46(17) . . ? C3 C1 S1 111.51(16) . . ? C1 C2 C9 124.4(2) . . ? C1 C2 S2 121.49(16) . . ? C9 C2 S2 114.08(16) . . ? C4 C3 C8 117.2(2) . . ? C4 C3 C1 123.8(2) . . ? C8 C3 C1 118.9(2) . . ? C5 C4 C3 121.1(2) . . ? C5 C4 H4 119.4 . . ? C3 C4 H4 119.4 . . ? C4 C5 C6 120.2(2) . . ? C4 C5 H5 119.9 . . ? C6 C5 H5 119.9 . . ? O1 C6 C7 124.3(2) . . ? O1 C6 C5 116.0(2) . . ? C7 C6 C5 119.7(2) . . ? C6 C7 C8 119.7(2) . . ? C6 C7 H7 120.1 . . ? C8 C7 H7 120.1 . . ? C7 C8 C3 122.0(2) . . ? C7 C8 H8 119.0 . . ? C3 C8 H8 119.0 . . ? C14 C9 C10 116.9(2) . . ? C14 C9 C2 121.4(2) . . ? C10 C9 C2 121.7(2) . . ? C11 C10 C9 121.4(2) . . ? C11 C10 H10 119.3 . . ? C9 C10 H10 119.3 . . ? C10 C11 C12 120.2(2) . . ? C10 C11 H11 119.9 . . ? C12 C11 H11 119.9 . . ? O2 C12 C13 124.8(2) . . ? O2 C12 C11 115.3(2) . . ? C13 C12 C11 119.9(2) . . ? C12 C13 C14 118.9(2) . . ? C12 C13 H13 120.6 . . ? C14 C13 H13 120.6 . . ? C13 C14 C9 122.7(2) . . ? C13 C14 H14 118.6 . . ? C9 C14 H14 118.6 . . ? O1 C15 H15A 109.5 . . ? O1 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? O1 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O2 C16 H16A 109.5 . . ? O2 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? O2 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C17 C17 P1 109.11(11) 2_565 . ? C17 C17 H17A 109.9 2_565 . ? P1 C17 H17A 109.9 . . ? C17 C17 H17B 109.9 2_565 . ? P1 C17 H17B 109.9 . . ? H17A C17 H17B 108.3 . . ? C23 C18 C19 118.7(2) . . ? C23 C18 P1 121.74(18) . . ? C19 C18 P1 119.52(17) . . ? C20 C19 C18 120.9(2) . . ? C20 C19 H19 119.6 . . ? C18 C19 H19 119.6 . . ? C19 C20 C21 119.7(2) . . ? C19 C20 H20 120.2 . . ? C21 C20 H20 120.2 . . ? C22 C21 C20 120.2(2) . . ? C22 C21 H21 119.9 . . ? C20 C21 H21 119.9 . . ? C21 C22 C23 120.1(2) . . ? C21 C22 H22 119.9 . . ? C23 C22 H22 119.9 . . ? C22 C23 C18 120.4(2) . . ? C22 C23 H23 119.8 . . ? C18 C23 H23 119.8 . . ? C25 C24 C29 119.3(2) . . ? C25 C24 P1 120.57(17) . . ? C29 C24 P1 119.96(18) . . ? C26 C25 C24 120.1(2) . . ? C26 C25 H25 120.0 . . ? C24 C25 H25 120.0 . . ? C27 C26 C25 120.2(2) . . ? C27 C26 H26 119.9 . . ? C25 C26 H26 119.9 . . ? C28 C27 C26 120.1(2) . . ? C28 C27 H27 119.9 . . ? C26 C27 H27 119.9 . . ? C27 C28 C29 120.3(2) . . ? C27 C28 H28 119.8 . . ? C29 C28 H28 119.8 . . ? C28 C29 C24 119.9(2) . . ? C28 C29 H29 120.0 . . ? C24 C29 H29 120.0 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.32 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.163 _refine_diff_density_min -0.641 _refine_diff_density_rms 0.085 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.250 0.250 -0.033 407 67 ' ' 2 0.750 0.750 -0.019 407 67 ' ' #===END # [Pt(S2C2(C6H4-p-OMe)2)(dppe)].DCE, Compound 7.DCE data_jpd295_0m _audit_creation_method SHELXL-97 _chemical_name_systematic ; (1,2-Bis(diphenylphosphino)ethane)(1,2-bis(4-methoxyphenyl) ethene-1,2-dithiolato)platinum(II) 1,2-dichloroethane solvate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H38 O2 P2 Pt S2, C2 H4 Cl2' _chemical_formula_sum 'C44 H42 Cl2 O2 P2 Pt S2' _chemical_formula_weight 994.83 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pt' 'Pt' -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 23.093(4) _cell_length_b 13.429(2) _cell_length_c 27.953(5) _cell_angle_alpha 90.00 _cell_angle_beta 110.592(2) _cell_angle_gamma 90.00 _cell_volume 8115(2) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9068 _cell_measurement_theta_min 2.49 _cell_measurement_theta_max 28.83 _exptl_crystal_description Slat _exptl_crystal_colour yellow _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.629 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3968 _exptl_absorpt_coefficient_mu 3.809 _exptl_absorpt_correction_type 'integration numerical gaussian' _exptl_absorpt_correction_T_min 0.3616 _exptl_absorpt_correction_T_max 0.8295 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008a)' _exptl_special_details ; The diffraction data were obtained from 3 sets of 400 frames, each of width 0.5 deg. in \w, collected at \f = 0.00, 90.00 and 180.00 deg. and 2 sets of 800 frames, each of width 0.45 deg in \f, collected at \w = -30.00 and 210.00 deg. The scan time was 15 sec/frame. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-I CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 138117 _diffrn_reflns_av_R_equivalents 0.0489 _diffrn_reflns_av_sigmaI/netI 0.0312 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 28.00 _reflns_number_total 19435 _reflns_number_gt 15288 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker APEX2 (Bruker-AXS, 2009)' _computing_cell_refinement 'Bruker SAINT (Bruker-AXS 2008)' _computing_data_reduction 'Bruker SAINT (Bruker-AXS 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL(Bruker-AXS 2008a)' _computing_publication_material 'Bruker SHELXTL(Bruker-AXS 2008a)' _publ_section_references ; Bruker-AXS (2009). APEX2, Version 2009.3-0, Madison, WI. Bruker-AXS (2008). SAINT, Version 7.60A, Madison, WI Bruker-AXS (2008a). SHELXTL, Version 2008/4, Madison, WI Sheldrick, G. M. (2008). SHELXS-97 and SHELXL-97. Acta Cryst. A64, 112-122. Sheldrick, G, M. (2008a). SADABS, Version 2008/2. University of G\"ottingen, Germany. ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. H-atoms were placed in calculated positions (C---H = 0.95 - 0.98 \%A) and included as riding contributions with isotropic displacement parameters 1.2 - 1.5 times those of the attached carbon atoms. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0198P)^2^+11.1160P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 19435 _refine_ls_number_parameters 959 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0432 _refine_ls_R_factor_gt 0.0262 _refine_ls_wR_factor_ref 0.0593 _refine_ls_wR_factor_gt 0.0520 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.760482(5) 0.883144(8) 0.177115(4) 0.01144(3) Uani 1 1 d . . . Pt2 Pt 0.727881(5) 0.121988(8) 0.816706(4) 0.01180(3) Uani 1 1 d . . . S1 S 0.83861(3) 0.79163(5) 0.23273(3) 0.01391(14) Uani 1 1 d . . . S2 S 0.76659(3) 0.78169(5) 0.11251(3) 0.01389(14) Uani 1 1 d . . . S3 S 0.72306(3) 0.21932(5) 0.88259(3) 0.01511(15) Uani 1 1 d . . . S4 S 0.65421(3) 0.22284(5) 0.76199(3) 0.01436(14) Uani 1 1 d . . . P1 P 0.75190(3) 0.97087(5) 0.24310(3) 0.01262(15) Uani 1 1 d . . . P2 P 0.69182(3) 0.99290(6) 0.12607(3) 0.01355(15) Uani 1 1 d . . . P3 P 0.79357(3) 0.01093(6) 0.86900(3) 0.01437(15) Uani 1 1 d . . . P4 P 0.73887(3) 0.03395(5) 0.75173(3) 0.01290(15) Uani 1 1 d . . . O1 O 1.05836(10) 0.48408(16) 0.32690(9) 0.0229(5) Uani 1 1 d . . . O2 O 0.91591(11) 0.49593(18) 0.00442(9) 0.0293(6) Uani 1 1 d . . . O3 O 0.58812(10) 0.51051(17) 0.99831(9) 0.0237(5) Uani 1 1 d . . . O4 O 0.46331(10) 0.59607(16) 0.68828(9) 0.0265(5) Uani 1 1 d . . . C1 C 0.86183(13) 0.7093(2) 0.19365(11) 0.0141(6) Uani 1 1 d . . . C2 C 0.83135(12) 0.7050(2) 0.14282(11) 0.0138(6) Uani 1 1 d . . . C3 C 0.66412(13) 0.3055(2) 0.85336(11) 0.0143(6) Uani 1 1 d . . . C4 C 0.63538(13) 0.3086(2) 0.80227(11) 0.0133(6) Uani 1 1 d . . . C5 C 0.91554(13) 0.6474(2) 0.22356(11) 0.0149(6) Uani 1 1 d . . . C6 C 0.91675(13) 0.5448(2) 0.21779(12) 0.0165(6) Uani 1 1 d . . . H6 H 0.8849 0.5133 0.1906 0.020 Uiso 1 1 calc R . . C7 C 0.96403(13) 0.4873(2) 0.25125(12) 0.0186(6) Uani 1 1 d . . . H7 H 0.9642 0.4171 0.2470 0.022 Uiso 1 1 calc R . . C8 C 1.01080(13) 0.5330(2) 0.29070(12) 0.0177(6) Uani 1 1 d . . . C9 C 1.01173(13) 0.6353(2) 0.29584(12) 0.0192(6) Uani 1 1 d . . . H9 H 1.0446 0.6668 0.3221 0.023 Uiso 1 1 calc R . . C10 C 0.96462(13) 0.6917(2) 0.26259(12) 0.0178(6) Uani 1 1 d . . . H10 H 0.9656 0.7620 0.2663 0.021 Uiso 1 1 calc R . . C11 C 1.05531(15) 0.3788(2) 0.32731(14) 0.0271(7) Uani 1 1 d . . . H11A H 1.0163 0.3581 0.3309 0.041 Uiso 1 1 calc R . . H11B H 1.0901 0.3528 0.3561 0.041 Uiso 1 1 calc R . . H11C H 1.0574 0.3525 0.2953 0.041 Uiso 1 1 calc R . . C12 C 0.85242(13) 0.6467(2) 0.10674(11) 0.0157(6) Uani 1 1 d . . . C13 C 0.90972(14) 0.6668(2) 0.10242(12) 0.0198(7) Uani 1 1 d . . . H13 H 0.9358 0.7162 0.1236 0.024 Uiso 1 1 calc R . . C14 C 0.92897(15) 0.6155(2) 0.06763(13) 0.0248(7) Uani 1 1 d . . . H14 H 0.9679 0.6304 0.0649 0.030 Uiso 1 1 calc R . . C15 C 0.89196(14) 0.5431(2) 0.03703(12) 0.0208(7) Uani 1 1 d . . . C16 C 0.83531(15) 0.5210(2) 0.04079(13) 0.0235(7) Uani 1 1 d . . . H16 H 0.8098 0.4706 0.0200 0.028 Uiso 1 1 calc R . . C17 C 0.81607(14) 0.5738(2) 0.07544(12) 0.0210(7) Uani 1 1 d . . . H17 H 0.7768 0.5593 0.0776 0.025 Uiso 1 1 calc R . . C18 C 0.87921(17) 0.4216(3) -0.02847(14) 0.0340(9) Uani 1 1 d . . . H18A H 0.8692 0.3695 -0.0080 0.051 Uiso 1 1 calc R . . H18B H 0.9022 0.3923 -0.0485 0.051 Uiso 1 1 calc R . . H18C H 0.8409 0.4515 -0.0516 0.051 Uiso 1 1 calc R . . C19 C 0.73244(13) 0.8979(2) 0.29003(11) 0.0147(6) Uani 1 1 d . . . C20 C 0.76618(14) 0.9008(2) 0.34196(12) 0.0213(7) Uani 1 1 d . . . H20 H 0.8023 0.9408 0.3544 0.026 Uiso 1 1 calc R . . C21 C 0.74719(16) 0.8453(3) 0.37591(14) 0.0283(8) Uani 1 1 d . . . H21 H 0.7702 0.8480 0.4115 0.034 Uiso 1 1 calc R . . C22 C 0.69498(16) 0.7863(2) 0.35786(14) 0.0265(8) Uani 1 1 d . . . H22 H 0.6819 0.7490 0.3811 0.032 Uiso 1 1 calc R . . C23 C 0.66186(15) 0.7815(2) 0.30604(14) 0.0258(7) Uani 1 1 d . . . H23 H 0.6262 0.7404 0.2937 0.031 Uiso 1 1 calc R . . C24 C 0.68035(14) 0.8364(2) 0.27194(13) 0.0211(7) Uani 1 1 d . . . H24 H 0.6577 0.8323 0.2363 0.025 Uiso 1 1 calc R . . C25 C 0.81669(13) 1.0491(2) 0.27946(11) 0.0143(6) Uani 1 1 d . . . C26 C 0.87429(13) 1.0389(2) 0.27422(12) 0.0167(6) Uani 1 1 d . . . H26 H 0.8799 0.9905 0.2514 0.020 Uiso 1 1 calc R . . C27 C 0.92342(14) 1.0990(2) 0.30214(12) 0.0200(7) Uani 1 1 d . . . H27 H 0.9625 1.0919 0.2984 0.024 Uiso 1 1 calc R . . C28 C 0.91543(14) 1.1695(2) 0.33543(12) 0.0195(6) Uani 1 1 d . . . H28 H 0.9491 1.2105 0.3546 0.023 Uiso 1 1 calc R . . C29 C 0.85838(14) 1.1805(2) 0.34089(12) 0.0185(6) Uani 1 1 d . . . H29 H 0.8531 1.2291 0.3638 0.022 Uiso 1 1 calc R . . C30 C 0.80905(14) 1.1210(2) 0.31312(11) 0.0171(6) Uani 1 1 d . . . H30 H 0.7700 1.1289 0.3169 0.021 Uiso 1 1 calc R . . C31 C 0.61233(13) 0.9513(2) 0.09383(12) 0.0175(6) Uani 1 1 d . . . C32 C 0.60223(15) 0.8738(2) 0.05919(13) 0.0259(7) Uani 1 1 d . . . H32 H 0.6362 0.8456 0.0523 0.031 Uiso 1 1 calc R . . C33 C 0.54332(16) 0.8369(3) 0.03452(15) 0.0343(9) Uani 1 1 d . . . H33 H 0.5367 0.7841 0.0106 0.041 Uiso 1 1 calc R . . C34 C 0.49412(16) 0.8775(3) 0.04499(15) 0.0401(10) Uani 1 1 d . . . H34 H 0.4537 0.8516 0.0287 0.048 Uiso 1 1 calc R . . C35 C 0.50335(16) 0.9550(3) 0.07881(15) 0.0409(10) Uani 1 1 d . . . H35 H 0.4691 0.9832 0.0854 0.049 Uiso 1 1 calc R . . C36 C 0.56271(15) 0.9927(3) 0.10366(14) 0.0300(8) Uani 1 1 d . . . H36 H 0.5690 1.0463 0.1271 0.036 Uiso 1 1 calc R . . C37 C 0.71244(14) 1.0542(2) 0.07663(11) 0.0164(6) Uani 1 1 d . . . C38 C 0.76991(14) 1.0382(2) 0.07262(12) 0.0197(6) Uani 1 1 d . . . H38 H 0.7962 0.9874 0.0924 0.024 Uiso 1 1 calc R . . C39 C 0.78924(15) 1.0960(2) 0.04000(12) 0.0234(7) Uani 1 1 d . . . H39 H 0.8289 1.0855 0.0378 0.028 Uiso 1 1 calc R . . C40 C 0.75105(17) 1.1683(3) 0.01083(13) 0.0268(8) Uani 1 1 d . . . H40 H 0.7648 1.2087 -0.0110 0.032 Uiso 1 1 calc R . . C41 C 0.69265(17) 1.1830(3) 0.01294(13) 0.0290(8) Uani 1 1 d . . . H41 H 0.6660 1.2321 -0.0080 0.035 Uiso 1 1 calc R . . C42 C 0.67328(15) 1.1259(2) 0.04569(12) 0.0217(7) Uani 1 1 d . . . H42 H 0.6332 1.1355 0.0471 0.026 Uiso 1 1 calc R . . C43 C 0.68693(13) 1.0565(2) 0.21764(11) 0.0145(6) Uani 1 1 d . . . H43A H 0.6475 1.0212 0.2124 0.017 Uiso 1 1 calc R . . H43B H 0.6907 1.1118 0.2420 0.017 Uiso 1 1 calc R . . C44 C 0.68766(14) 1.0972(2) 0.16683(12) 0.0173(6) Uani 1 1 d . . . H44A H 0.7238 1.1414 0.1729 0.021 Uiso 1 1 calc R . . H44B H 0.6497 1.1365 0.1498 0.021 Uiso 1 1 calc R . . C45 C 0.64551(13) 0.3641(2) 0.89110(11) 0.0148(6) Uani 1 1 d . . . C46 C 0.68608(14) 0.4264(2) 0.92658(12) 0.0193(6) Uani 1 1 d . . . H46 H 0.7267 0.4347 0.9261 0.023 Uiso 1 1 calc R . . C47 C 0.66920(14) 0.4774(2) 0.96291(12) 0.0212(7) Uani 1 1 d . . . H47 H 0.6978 0.5207 0.9865 0.025 Uiso 1 1 calc R . . C48 C 0.61041(14) 0.4644(2) 0.96446(12) 0.0192(6) Uani 1 1 d . . . C49 C 0.56939(14) 0.4013(2) 0.92981(13) 0.0210(7) Uani 1 1 d . . . H49 H 0.5292 0.3912 0.9311 0.025 Uiso 1 1 calc R . . C50 C 0.58673(13) 0.3526(2) 0.89323(12) 0.0193(6) Uani 1 1 d . . . H50 H 0.5578 0.3106 0.8691 0.023 Uiso 1 1 calc R . . C51 C 0.62883(16) 0.5761(3) 1.03486(13) 0.0298(8) Uani 1 1 d . . . H51A H 0.6649 0.5388 1.0567 0.045 Uiso 1 1 calc R . . H51B H 0.6072 0.6055 1.0559 0.045 Uiso 1 1 calc R . . H51C H 0.6424 0.6291 1.0171 0.045 Uiso 1 1 calc R . . C52 C 0.58734(13) 0.3817(2) 0.77431(11) 0.0157(6) Uani 1 1 d . . . C53 C 0.53738(14) 0.3535(2) 0.73134(12) 0.0195(6) Uani 1 1 d . . . H53 H 0.5324 0.2852 0.7219 0.023 Uiso 1 1 calc R . . C54 C 0.49452(14) 0.4222(2) 0.70183(13) 0.0220(7) Uani 1 1 d . . . H54 H 0.4609 0.4010 0.6727 0.026 Uiso 1 1 calc R . . C55 C 0.50137(13) 0.5218(2) 0.71530(13) 0.0198(7) Uani 1 1 d . . . C56 C 0.55018(14) 0.5515(2) 0.75858(13) 0.0201(7) Uani 1 1 d . . . H56 H 0.5544 0.6197 0.7683 0.024 Uiso 1 1 calc R . . C57 C 0.59245(13) 0.4831(2) 0.78758(12) 0.0173(6) Uani 1 1 d . . . H57 H 0.6255 0.5047 0.8170 0.021 Uiso 1 1 calc R . . C58 C 0.40815(14) 0.5644(3) 0.64948(13) 0.0255(7) Uani 1 1 d . . . H58A H 0.4185 0.5266 0.6236 0.038 Uiso 1 1 calc R . . H58B H 0.3833 0.6226 0.6335 0.038 Uiso 1 1 calc R . . H58C H 0.3845 0.5220 0.6645 0.038 Uiso 1 1 calc R . . C59 C 0.76712(14) -0.0497(2) 0.91566(11) 0.0168(6) Uani 1 1 d . . . C60 C 0.70588(14) -0.0382(2) 0.91242(12) 0.0201(7) Uani 1 1 d . . . H60 H 0.6790 0.0047 0.8874 0.024 Uiso 1 1 calc R . . C61 C 0.68425(15) -0.0895(2) 0.94585(13) 0.0227(7) Uani 1 1 d . . . H61 H 0.6426 -0.0814 0.9438 0.027 Uiso 1 1 calc R . . C62 C 0.72310(15) -0.1521(2) 0.98197(12) 0.0242(7) Uani 1 1 d . . . H62 H 0.7080 -0.1873 1.0047 0.029 Uiso 1 1 calc R . . C63 C 0.78428(16) -0.1642(2) 0.98546(13) 0.0256(7) Uani 1 1 d . . . H63 H 0.8109 -0.2076 1.0104 0.031 Uiso 1 1 calc R . . C64 C 0.80633(15) -0.1128(2) 0.95250(12) 0.0221(7) Uani 1 1 d . . . H64 H 0.8482 -0.1206 0.9550 0.027 Uiso 1 1 calc R . . C65 C 0.87135(14) 0.0541(2) 0.90659(12) 0.0184(6) Uani 1 1 d . . . C66 C 0.87836(15) 0.1190(2) 0.94672(13) 0.0244(7) Uani 1 1 d . . . H66 H 0.8430 0.1389 0.9541 0.029 Uiso 1 1 calc R . . C67 C 0.93590(16) 0.1554(3) 0.97621(14) 0.0296(8) Uani 1 1 d . . . H67 H 0.9400 0.1992 1.0039 0.036 Uiso 1 1 calc R . . C68 C 0.98716(17) 0.1278(4) 0.96522(16) 0.0465(11) Uani 1 1 d . . . H68 H 1.0268 0.1530 0.9849 0.056 Uiso 1 1 calc R . . C69 C 0.98046(18) 0.0635(5) 0.92552(18) 0.0655(16) Uani 1 1 d . . . H69 H 1.0159 0.0439 0.9181 0.079 Uiso 1 1 calc R . . C70 C 0.92292(16) 0.0266(4) 0.89595(15) 0.0428(11) Uani 1 1 d . . . H70 H 0.9191 -0.0176 0.8684 0.051 Uiso 1 1 calc R . . C71 C 0.67693(13) -0.0499(2) 0.71623(11) 0.0155(6) Uani 1 1 d . . . C72 C 0.61974(13) -0.0455(2) 0.72244(12) 0.0180(6) Uani 1 1 d . . . H72 H 0.6127 0.0023 0.7449 0.022 Uiso 1 1 calc R . . C73 C 0.57277(14) -0.1111(2) 0.69569(12) 0.0202(6) Uani 1 1 d . . . H73 H 0.5337 -0.1079 0.6999 0.024 Uiso 1 1 calc R . . C74 C 0.58290(14) -0.1811(2) 0.66303(12) 0.0213(7) Uani 1 1 d . . . H74 H 0.5508 -0.2257 0.6448 0.026 Uiso 1 1 calc R . . C75 C 0.63995(14) -0.1858(2) 0.65708(12) 0.0191(6) Uani 1 1 d . . . H75 H 0.6468 -0.2339 0.6347 0.023 Uiso 1 1 calc R . . C76 C 0.68699(13) -0.1213(2) 0.68343(11) 0.0162(6) Uani 1 1 d . . . H76 H 0.7260 -0.1253 0.6793 0.019 Uiso 1 1 calc R . . C77 C 0.75780(13) 0.1059(2) 0.70417(11) 0.0140(6) Uani 1 1 d . . . C78 C 0.80660(14) 0.1735(2) 0.72240(12) 0.0188(6) Uani 1 1 d . . . H78 H 0.8260 0.1836 0.7581 0.023 Uiso 1 1 calc R . . C79 C 0.82684(15) 0.2259(2) 0.68859(13) 0.0236(7) Uani 1 1 d . . . H79 H 0.8602 0.2714 0.7012 0.028 Uiso 1 1 calc R . . C80 C 0.79866(16) 0.2120(2) 0.63667(13) 0.0246(7) Uani 1 1 d . . . H80 H 0.8132 0.2471 0.6136 0.030 Uiso 1 1 calc R . . C81 C 0.74931(16) 0.1472(2) 0.61824(13) 0.0257(7) Uani 1 1 d . . . H81 H 0.7292 0.1391 0.5824 0.031 Uiso 1 1 calc R . . C82 C 0.72900(15) 0.0938(2) 0.65198(12) 0.0219(7) Uani 1 1 d . . . H82 H 0.6953 0.0490 0.6391 0.026 Uiso 1 1 calc R . . C83 C 0.80410(14) -0.0903(2) 0.82911(12) 0.0179(6) Uani 1 1 d . . . H83B H 0.8432 -0.1259 0.8473 0.021 Uiso 1 1 calc R . . H83A H 0.7696 -0.1384 0.8219 0.021 Uiso 1 1 calc R . . C84 C 0.80585(13) -0.0471(2) 0.77928(11) 0.0165(6) Uani 1 1 d . . . H84A H 0.8049 -0.1015 0.7551 0.020 Uiso 1 1 calc R . . H84B H 0.8444 -0.0085 0.7859 0.020 Uiso 1 1 calc R . . Cl1 Cl 0.92194(5) 0.70879(9) 0.92021(5) 0.0540(3) Uani 1 1 d . . . Cl2 Cl 1.05211(5) 0.70598(8) 0.89258(4) 0.0493(3) Uani 1 1 d . . . C85 C 0.95730(17) 0.6009(3) 0.90521(15) 0.0338(9) Uani 1 1 d . . . H85A H 0.9884 0.5745 0.9369 0.041 Uiso 1 1 calc R . . H85B H 0.9254 0.5490 0.8911 0.041 Uiso 1 1 calc R . . C86 C 0.98793(18) 0.6227(3) 0.86753(16) 0.0396(9) Uani 1 1 d . . . H86A H 0.9573 0.6526 0.8365 0.048 Uiso 1 1 calc R . . H86B H 1.0026 0.5596 0.8574 0.048 Uiso 1 1 calc R . . Cl3 Cl 0.41763(4) 0.69418(7) 0.92517(4) 0.0397(2) Uani 1 1 d . . . Cl4 Cl 0.55714(5) 0.71205(8) 0.91216(4) 0.0486(3) Uani 1 1 d . . . C87 C 0.45824(16) 0.5964(3) 0.90802(14) 0.0282(8) Uani 1 1 d . . . H87A H 0.4867 0.5645 0.9394 0.034 Uiso 1 1 calc R . . H87B H 0.4283 0.5454 0.8884 0.034 Uiso 1 1 calc R . . C88 C 0.49470(19) 0.6329(3) 0.87653(15) 0.0385(9) Uani 1 1 d . . . H88A H 0.4669 0.6700 0.8467 0.046 Uiso 1 1 calc R . . H88B H 0.5114 0.5751 0.8636 0.046 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.01158(5) 0.01180(5) 0.01163(6) 0.00017(4) 0.00493(4) 0.00089(4) Pt2 0.01298(5) 0.01152(6) 0.01183(6) 0.00007(4) 0.00553(4) 0.00087(4) S1 0.0152(3) 0.0140(3) 0.0125(4) 0.0000(3) 0.0048(3) 0.0032(3) S2 0.0135(3) 0.0150(3) 0.0130(4) -0.0015(3) 0.0044(3) 0.0021(3) S3 0.0163(3) 0.0159(4) 0.0126(4) -0.0007(3) 0.0044(3) 0.0038(3) S4 0.0160(3) 0.0144(3) 0.0130(4) -0.0004(3) 0.0056(3) 0.0022(3) P1 0.0131(3) 0.0137(4) 0.0120(4) 0.0003(3) 0.0056(3) 0.0011(3) P2 0.0140(3) 0.0143(4) 0.0127(4) 0.0007(3) 0.0051(3) 0.0025(3) P3 0.0161(4) 0.0147(4) 0.0131(4) 0.0015(3) 0.0061(3) 0.0021(3) P4 0.0143(3) 0.0130(4) 0.0126(4) -0.0008(3) 0.0061(3) 0.0003(3) O1 0.0177(11) 0.0192(11) 0.0278(13) 0.0068(10) 0.0028(10) 0.0049(9) O2 0.0293(13) 0.0361(14) 0.0263(13) -0.0113(11) 0.0144(11) 0.0065(10) O3 0.0242(12) 0.0288(13) 0.0206(12) -0.0077(10) 0.0108(10) 0.0036(9) O4 0.0192(11) 0.0213(12) 0.0316(14) 0.0005(10) -0.0001(10) 0.0062(9) C1 0.0135(13) 0.0140(14) 0.0171(15) -0.0022(12) 0.0082(12) -0.0007(11) C2 0.0114(13) 0.0132(14) 0.0175(15) -0.0002(12) 0.0060(12) 0.0000(10) C3 0.0129(13) 0.0128(14) 0.0179(15) -0.0023(12) 0.0062(12) -0.0003(11) C4 0.0123(13) 0.0132(14) 0.0156(15) -0.0020(12) 0.0065(12) -0.0008(10) C5 0.0138(13) 0.0175(15) 0.0157(15) -0.0006(12) 0.0080(12) 0.0023(11) C6 0.0149(14) 0.0189(15) 0.0169(15) -0.0028(12) 0.0071(12) -0.0009(11) C7 0.0180(15) 0.0140(15) 0.0277(18) 0.0025(13) 0.0127(14) 0.0021(11) C8 0.0137(14) 0.0235(16) 0.0177(16) 0.0064(13) 0.0077(12) 0.0052(12) C9 0.0153(14) 0.0236(16) 0.0175(16) 0.0007(13) 0.0043(12) 0.0001(12) C10 0.0187(15) 0.0161(15) 0.0186(16) -0.0002(12) 0.0067(13) 0.0015(11) C11 0.0258(17) 0.0204(17) 0.035(2) 0.0065(15) 0.0109(15) 0.0063(14) C12 0.0162(14) 0.0178(15) 0.0135(15) -0.0006(12) 0.0057(12) 0.0033(11) C13 0.0175(15) 0.0222(16) 0.0221(17) -0.0056(13) 0.0101(13) -0.0028(12) C14 0.0193(15) 0.0309(19) 0.0269(18) -0.0043(15) 0.0115(14) -0.0003(14) C15 0.0226(16) 0.0225(16) 0.0179(16) -0.0018(13) 0.0077(13) 0.0085(13) C16 0.0210(16) 0.0258(17) 0.0208(17) -0.0088(14) 0.0038(14) 0.0009(13) C17 0.0152(14) 0.0247(17) 0.0230(17) -0.0056(14) 0.0066(13) -0.0029(12) C18 0.038(2) 0.039(2) 0.027(2) -0.0113(17) 0.0127(17) 0.0118(17) C19 0.0186(14) 0.0116(14) 0.0161(15) -0.0001(12) 0.0089(12) 0.0024(11) C20 0.0201(15) 0.0244(17) 0.0183(16) 0.0061(13) 0.0054(13) 0.0016(12) C21 0.0352(19) 0.0293(19) 0.0214(18) 0.0072(15) 0.0111(16) 0.0035(15) C22 0.039(2) 0.0197(17) 0.0307(19) 0.0086(15) 0.0250(17) 0.0033(14) C23 0.0272(17) 0.0205(17) 0.033(2) 0.0001(15) 0.0154(16) -0.0051(13) C24 0.0233(16) 0.0207(16) 0.0210(17) 0.0001(13) 0.0097(14) -0.0026(12) C25 0.0167(14) 0.0143(14) 0.0117(14) 0.0027(12) 0.0049(12) 0.0009(11) C26 0.0193(15) 0.0160(15) 0.0164(15) 0.0009(12) 0.0082(13) 0.0013(11) C27 0.0173(14) 0.0229(16) 0.0206(16) 0.0007(13) 0.0077(13) 0.0005(12) C28 0.0185(15) 0.0188(16) 0.0189(16) 0.0004(13) 0.0038(13) -0.0031(12) C29 0.0206(15) 0.0163(15) 0.0171(16) -0.0011(12) 0.0046(13) 0.0019(12) C30 0.0188(14) 0.0162(15) 0.0151(15) -0.0008(12) 0.0045(12) 0.0031(12) C31 0.0144(14) 0.0230(16) 0.0137(15) 0.0053(13) 0.0033(12) 0.0019(12) C32 0.0211(16) 0.0266(18) 0.0258(18) -0.0013(15) 0.0029(14) 0.0006(13) C33 0.0260(18) 0.034(2) 0.034(2) -0.0040(17) -0.0005(16) -0.0063(15) C34 0.0167(16) 0.064(3) 0.030(2) 0.012(2) -0.0035(15) -0.0098(18) C35 0.0180(17) 0.072(3) 0.031(2) 0.001(2) 0.0065(16) 0.0027(18) C36 0.0187(16) 0.047(2) 0.0219(18) -0.0021(16) 0.0037(14) 0.0048(15) C37 0.0200(15) 0.0151(15) 0.0126(15) -0.0006(12) 0.0038(12) -0.0001(11) C38 0.0217(15) 0.0181(15) 0.0189(16) 0.0018(13) 0.0064(13) 0.0018(12) C39 0.0251(16) 0.0280(18) 0.0206(17) 0.0007(14) 0.0122(14) -0.0005(13) C40 0.040(2) 0.0266(18) 0.0156(17) 0.0010(14) 0.0114(15) -0.0055(15) C41 0.038(2) 0.0269(18) 0.0188(18) 0.0075(15) 0.0059(16) 0.0045(15) C42 0.0228(15) 0.0221(16) 0.0189(16) 0.0032(14) 0.0058(13) 0.0042(13) C43 0.0150(14) 0.0146(14) 0.0144(15) -0.0007(12) 0.0056(12) 0.0017(11) C44 0.0188(14) 0.0155(15) 0.0176(16) 0.0010(12) 0.0063(13) 0.0036(11) C45 0.0154(13) 0.0136(14) 0.0156(15) -0.0017(12) 0.0055(12) 0.0017(11) C46 0.0166(14) 0.0216(16) 0.0196(16) -0.0053(13) 0.0062(13) -0.0029(12) C47 0.0200(15) 0.0253(17) 0.0159(16) -0.0098(14) 0.0034(13) -0.0030(13) C48 0.0219(15) 0.0195(16) 0.0168(16) -0.0003(13) 0.0075(13) 0.0039(12) C49 0.0162(14) 0.0220(16) 0.0271(18) -0.0041(14) 0.0104(13) 0.0015(12) C50 0.0149(14) 0.0201(16) 0.0223(17) -0.0071(13) 0.0056(13) -0.0036(11) C51 0.0343(19) 0.036(2) 0.0184(17) -0.0103(15) 0.0080(15) 0.0053(16) C52 0.0140(13) 0.0176(15) 0.0173(15) 0.0015(12) 0.0077(12) 0.0018(11) C53 0.0192(15) 0.0180(15) 0.0203(16) -0.0035(13) 0.0056(13) 0.0015(12) C54 0.0169(15) 0.0236(17) 0.0201(17) -0.0015(14) -0.0001(13) 0.0027(12) C55 0.0139(14) 0.0201(16) 0.0271(18) 0.0035(13) 0.0093(13) 0.0052(12) C56 0.0180(15) 0.0146(15) 0.0276(18) -0.0023(13) 0.0081(13) 0.0016(11) C57 0.0135(14) 0.0190(15) 0.0191(16) -0.0007(13) 0.0053(12) -0.0002(11) C58 0.0183(15) 0.0304(19) 0.0248(18) 0.0022(15) 0.0037(14) 0.0071(13) C59 0.0218(15) 0.0171(15) 0.0110(15) -0.0023(12) 0.0050(12) -0.0027(12) C60 0.0240(16) 0.0175(15) 0.0201(17) 0.0003(13) 0.0092(14) 0.0027(12) C61 0.0248(16) 0.0230(17) 0.0251(18) -0.0057(14) 0.0149(15) -0.0046(13) C62 0.0322(18) 0.0256(17) 0.0184(17) -0.0016(14) 0.0134(15) -0.0082(14) C63 0.0354(19) 0.0229(17) 0.0144(16) 0.0029(14) 0.0036(15) -0.0013(14) C64 0.0236(16) 0.0238(17) 0.0167(16) 0.0033(14) 0.0043(13) 0.0009(13) C65 0.0172(14) 0.0242(16) 0.0140(15) 0.0054(13) 0.0057(12) 0.0028(12) C66 0.0210(15) 0.0236(17) 0.0252(18) 0.0021(15) 0.0037(14) 0.0044(13) C67 0.0278(18) 0.0259(18) 0.0271(19) -0.0005(15) -0.0004(15) -0.0017(14) C68 0.0214(18) 0.075(3) 0.037(2) -0.007(2) 0.0025(17) -0.013(2) C69 0.0162(19) 0.134(5) 0.048(3) -0.031(3) 0.0123(19) -0.008(2) C70 0.0210(18) 0.081(3) 0.028(2) -0.019(2) 0.0101(16) -0.0035(19) C71 0.0176(14) 0.0145(14) 0.0138(15) 0.0020(12) 0.0048(12) 0.0001(11) C72 0.0187(15) 0.0188(15) 0.0181(16) -0.0006(13) 0.0084(13) 0.0001(12) C73 0.0164(14) 0.0238(17) 0.0210(16) -0.0007(14) 0.0072(13) -0.0002(12) C74 0.0191(15) 0.0201(16) 0.0212(17) -0.0013(13) 0.0028(13) -0.0027(12) C75 0.0207(15) 0.0160(15) 0.0192(16) -0.0020(13) 0.0054(13) 0.0024(12) C76 0.0183(14) 0.0160(15) 0.0163(15) 0.0002(12) 0.0087(12) 0.0013(12) C77 0.0174(14) 0.0117(14) 0.0162(15) 0.0018(12) 0.0100(12) 0.0010(11) C78 0.0206(15) 0.0168(15) 0.0194(16) 0.0002(13) 0.0074(13) 0.0017(12) C79 0.0223(16) 0.0179(16) 0.035(2) 0.0031(14) 0.0155(15) -0.0012(12) C80 0.0341(18) 0.0202(17) 0.0273(19) 0.0097(14) 0.0205(16) 0.0032(14) C81 0.0386(19) 0.0246(17) 0.0153(16) 0.0049(14) 0.0112(15) 0.0040(14) C82 0.0251(16) 0.0205(16) 0.0205(17) 0.0013(13) 0.0088(14) 0.0000(12) C83 0.0224(15) 0.0161(15) 0.0164(16) 0.0011(12) 0.0085(13) 0.0037(12) C84 0.0170(14) 0.0157(15) 0.0178(16) 0.0009(12) 0.0074(12) 0.0021(11) Cl1 0.0397(6) 0.0557(7) 0.0607(8) -0.0127(6) 0.0104(5) 0.0132(5) Cl2 0.0385(5) 0.0529(7) 0.0526(7) 0.0136(5) 0.0111(5) -0.0105(5) C85 0.0281(18) 0.036(2) 0.034(2) 0.0022(17) 0.0066(16) 0.0018(15) C86 0.040(2) 0.040(2) 0.037(2) 0.0009(19) 0.0110(18) -0.0068(18) Cl3 0.0341(5) 0.0363(5) 0.0452(6) -0.0053(4) 0.0097(4) 0.0115(4) Cl4 0.0444(6) 0.0503(6) 0.0504(7) 0.0175(5) 0.0158(5) -0.0061(5) C87 0.0284(18) 0.0258(18) 0.030(2) -0.0016(15) 0.0102(16) 0.0057(14) C88 0.047(2) 0.040(2) 0.029(2) 0.0051(18) 0.0143(18) 0.0053(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 P1 2.2553(8) . ? Pt1 P2 2.2651(8) . ? Pt1 S1 2.2824(7) . ? Pt1 S2 2.3057(8) . ? Pt2 P4 2.2550(8) . ? Pt2 P3 2.2589(8) . ? Pt2 S4 2.2885(8) . ? Pt2 S3 2.2926(8) . ? S1 C1 1.765(3) . ? S2 C2 1.767(3) . ? S3 C3 1.755(3) . ? S4 C4 1.769(3) . ? P1 C19 1.816(3) . ? P1 C25 1.818(3) . ? P1 C43 1.824(3) . ? P2 C37 1.810(3) . ? P2 C31 1.825(3) . ? P2 C44 1.829(3) . ? P3 C59 1.816(3) . ? P3 C65 1.827(3) . ? P3 C83 1.828(3) . ? P4 C77 1.817(3) . ? P4 C71 1.817(3) . ? P4 C84 1.825(3) . ? O1 C8 1.371(3) . ? O1 C11 1.416(4) . ? O2 C15 1.376(4) . ? O2 C18 1.419(4) . ? O3 C48 1.373(4) . ? O3 C51 1.424(4) . ? O4 C55 1.368(4) . ? O4 C58 1.417(4) . ? C1 C2 1.347(4) . ? C1 C5 1.483(4) . ? C2 C12 1.487(4) . ? C3 C4 1.347(4) . ? C3 C45 1.495(4) . ? C4 C52 1.481(4) . ? C5 C6 1.388(4) . ? C5 C10 1.400(4) . ? C6 C7 1.395(4) . ? C6 H6 0.9500 . ? C7 C8 1.386(4) . ? C7 H7 0.9500 . ? C8 C9 1.381(4) . ? C9 C10 1.382(4) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C17 1.383(4) . ? C12 C13 1.397(4) . ? C13 C14 1.386(4) . ? C13 H13 0.9500 . ? C14 C15 1.376(4) . ? C14 H14 0.9500 . ? C15 C16 1.381(4) . ? C16 C17 1.393(4) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.386(4) . ? C19 C24 1.399(4) . ? C20 C21 1.394(4) . ? C20 H20 0.9500 . ? C21 C22 1.381(5) . ? C21 H21 0.9500 . ? C22 C23 1.381(5) . ? C22 H22 0.9500 . ? C23 C24 1.386(4) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C26 1.395(4) . ? C25 C30 1.402(4) . ? C26 C27 1.388(4) . ? C26 H26 0.9500 . ? C27 C28 1.384(4) . ? C27 H27 0.9500 . ? C28 C29 1.387(4) . ? C28 H28 0.9500 . ? C29 C30 1.385(4) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C32 1.385(4) . ? C31 C36 1.385(4) . ? C32 C33 1.383(4) . ? C32 H32 0.9500 . ? C33 C34 1.381(5) . ? C33 H33 0.9500 . ? C34 C35 1.371(6) . ? C34 H34 0.9500 . ? C35 C36 1.396(5) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 C38 1.387(4) . ? C37 C42 1.394(4) . ? C38 C39 1.385(4) . ? C38 H38 0.9500 . ? C39 C40 1.372(5) . ? C39 H39 0.9500 . ? C40 C41 1.384(5) . ? C40 H40 0.9500 . ? C41 C42 1.384(5) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C43 C44 1.528(4) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C46 1.381(4) . ? C45 C50 1.388(4) . ? C46 C47 1.389(4) . ? C46 H46 0.9500 . ? C47 C48 1.384(4) . ? C47 H47 0.9500 . ? C48 C49 1.382(4) . ? C49 C50 1.386(4) . ? C49 H49 0.9500 . ? C50 H50 0.9500 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 C53 1.394(4) . ? C52 C57 1.405(4) . ? C53 C54 1.392(4) . ? C53 H53 0.9500 . ? C54 C55 1.383(4) . ? C54 H54 0.9500 . ? C55 C56 1.391(4) . ? C56 C57 1.378(4) . ? C56 H56 0.9500 . ? C57 H57 0.9500 . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C59 C60 1.393(4) . ? C59 C64 1.394(4) . ? C60 C61 1.388(4) . ? C60 H60 0.9500 . ? C61 C62 1.376(5) . ? C61 H61 0.9500 . ? C62 C63 1.391(5) . ? C62 H62 0.9500 . ? C63 C64 1.383(4) . ? C63 H63 0.9500 . ? C64 H64 0.9500 . ? C65 C70 1.376(5) . ? C65 C66 1.384(4) . ? C66 C67 1.383(4) . ? C66 H66 0.9500 . ? C67 C68 1.375(5) . ? C67 H67 0.9500 . ? C68 C69 1.371(6) . ? C68 H68 0.9500 . ? C69 C70 1.387(5) . ? C69 H69 0.9500 . ? C70 H70 0.9500 . ? C71 C72 1.393(4) . ? C71 C76 1.401(4) . ? C72 C73 1.394(4) . ? C72 H72 0.9500 . ? C73 C74 1.386(4) . ? C73 H73 0.9500 . ? C74 C75 1.386(4) . ? C74 H74 0.9500 . ? C75 C76 1.382(4) . ? C75 H75 0.9500 . ? C76 H76 0.9500 . ? C77 C82 1.384(4) . ? C77 C78 1.396(4) . ? C78 C79 1.385(4) . ? C78 H78 0.9500 . ? C79 C80 1.378(5) . ? C79 H79 0.9500 . ? C80 C81 1.382(5) . ? C80 H80 0.9500 . ? C81 C82 1.391(4) . ? C81 H81 0.9500 . ? C82 H82 0.9500 . ? C83 C84 1.523(4) . ? C83 H83B 0.9900 . ? C83 H83A 0.9900 . ? C84 H84A 0.9900 . ? C84 H84B 0.9900 . ? Cl1 C85 1.783(4) . ? Cl2 C86 1.791(4) . ? C85 C86 1.490(5) . ? C85 H85A 0.9900 . ? C85 H85B 0.9900 . ? C86 H86A 0.9900 . ? C86 H86B 0.9900 . ? Cl3 C87 1.775(3) . ? Cl4 C88 1.786(4) . ? C87 C88 1.499(5) . ? C87 H87A 0.9900 . ? C87 H87B 0.9900 . ? C88 H88A 0.9900 . ? C88 H88B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Pt1 P2 86.09(3) . . ? P1 Pt1 S1 90.00(3) . . ? P2 Pt1 S1 171.86(3) . . ? P1 Pt1 S2 175.12(3) . . ? P2 Pt1 S2 96.50(3) . . ? S1 Pt1 S2 87.92(3) . . ? P4 Pt2 P3 86.26(3) . . ? P4 Pt2 S4 92.28(3) . . ? P3 Pt2 S4 174.50(3) . . ? P4 Pt2 S3 175.46(3) . . ? P3 Pt2 S3 93.90(3) . . ? S4 Pt2 S3 87.98(3) . . ? C1 S1 Pt1 104.79(10) . . ? C2 S2 Pt1 104.09(10) . . ? C3 S3 Pt2 104.54(10) . . ? C4 S4 Pt2 104.56(10) . . ? C19 P1 C25 105.80(13) . . ? C19 P1 C43 104.08(13) . . ? C25 P1 C43 104.83(13) . . ? C19 P1 Pt1 115.09(10) . . ? C25 P1 Pt1 117.87(10) . . ? C43 P1 Pt1 107.87(10) . . ? C37 P2 C31 104.54(14) . . ? C37 P2 C44 102.29(14) . . ? C31 P2 C44 106.12(14) . . ? C37 P2 Pt1 117.58(10) . . ? C31 P2 Pt1 118.15(10) . . ? C44 P2 Pt1 106.52(10) . . ? C59 P3 C65 103.89(14) . . ? C59 P3 C83 104.79(14) . . ? C65 P3 C83 105.79(14) . . ? C59 P3 Pt2 116.20(10) . . ? C65 P3 Pt2 117.60(10) . . ? C83 P3 Pt2 107.43(10) . . ? C77 P4 C71 106.01(14) . . ? C77 P4 C84 103.84(13) . . ? C71 P4 C84 104.38(14) . . ? C77 P4 Pt2 115.78(10) . . ? C71 P4 Pt2 118.36(10) . . ? C84 P4 Pt2 106.94(10) . . ? C8 O1 C11 117.1(3) . . ? C15 O2 C18 117.8(3) . . ? C48 O3 C51 117.4(3) . . ? C55 O4 C58 115.7(3) . . ? C2 C1 C5 126.5(3) . . ? C2 C1 S1 121.3(2) . . ? C5 C1 S1 112.2(2) . . ? C1 C2 C12 124.3(3) . . ? C1 C2 S2 121.4(2) . . ? C12 C2 S2 113.9(2) . . ? C4 C3 C45 125.1(3) . . ? C4 C3 S3 121.7(2) . . ? C45 C3 S3 112.8(2) . . ? C3 C4 C52 125.3(3) . . ? C3 C4 S4 121.0(2) . . ? C52 C4 S4 113.7(2) . . ? C6 C5 C10 117.9(3) . . ? C6 C5 C1 122.5(3) . . ? C10 C5 C1 119.2(3) . . ? C5 C6 C7 121.0(3) . . ? C5 C6 H6 119.5 . . ? C7 C6 H6 119.5 . . ? C8 C7 C6 119.7(3) . . ? C8 C7 H7 120.2 . . ? C6 C7 H7 120.2 . . ? O1 C8 C9 114.9(3) . . ? O1 C8 C7 124.9(3) . . ? C9 C8 C7 120.2(3) . . ? C8 C9 C10 119.7(3) . . ? C8 C9 H9 120.2 . . ? C10 C9 H9 120.2 . . ? C9 C10 C5 121.4(3) . . ? C9 C10 H10 119.3 . . ? C5 C10 H10 119.3 . . ? O1 C11 H11A 109.5 . . ? O1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? O1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C17 C12 C13 117.7(3) . . ? C17 C12 C2 122.1(3) . . ? C13 C12 C2 120.2(3) . . ? C14 C13 C12 120.8(3) . . ? C14 C13 H13 119.6 . . ? C12 C13 H13 119.6 . . ? C15 C14 C13 120.3(3) . . ? C15 C14 H14 119.8 . . ? C13 C14 H14 119.8 . . ? O2 C15 C14 115.5(3) . . ? O2 C15 C16 124.3(3) . . ? C14 C15 C16 120.1(3) . . ? C15 C16 C17 119.1(3) . . ? C15 C16 H16 120.5 . . ? C17 C16 H16 120.5 . . ? C12 C17 C16 121.9(3) . . ? C12 C17 H17 119.0 . . ? C16 C17 H17 119.0 . . ? O2 C18 H18A 109.5 . . ? O2 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? O2 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 C24 119.4(3) . . ? C20 C19 P1 123.4(2) . . ? C24 C19 P1 117.2(2) . . ? C19 C20 C21 120.2(3) . . ? C19 C20 H20 119.9 . . ? C21 C20 H20 119.9 . . ? C22 C21 C20 120.1(3) . . ? C22 C21 H21 119.9 . . ? C20 C21 H21 119.9 . . ? C21 C22 C23 120.0(3) . . ? C21 C22 H22 120.0 . . ? C23 C22 H22 120.0 . . ? C22 C23 C24 120.4(3) . . ? C22 C23 H23 119.8 . . ? C24 C23 H23 119.8 . . ? C23 C24 C19 119.9(3) . . ? C23 C24 H24 120.0 . . ? C19 C24 H24 120.0 . . ? C26 C25 C30 119.2(3) . . ? C26 C25 P1 120.8(2) . . ? C30 C25 P1 120.0(2) . . ? C27 C26 C25 120.3(3) . . ? C27 C26 H26 119.9 . . ? C25 C26 H26 119.9 . . ? C28 C27 C26 120.0(3) . . ? C28 C27 H27 120.0 . . ? C26 C27 H27 120.0 . . ? C27 C28 C29 120.2(3) . . ? C27 C28 H28 119.9 . . ? C29 C28 H28 119.9 . . ? C30 C29 C28 120.2(3) . . ? C30 C29 H29 119.9 . . ? C28 C29 H29 119.9 . . ? C29 C30 C25 120.1(3) . . ? C29 C30 H30 120.0 . . ? C25 C30 H30 120.0 . . ? C32 C31 C36 119.5(3) . . ? C32 C31 P2 117.9(2) . . ? C36 C31 P2 122.6(3) . . ? C33 C32 C31 120.8(3) . . ? C33 C32 H32 119.6 . . ? C31 C32 H32 119.6 . . ? C34 C33 C32 119.4(4) . . ? C34 C33 H33 120.3 . . ? C32 C33 H33 120.3 . . ? C35 C34 C33 120.4(3) . . ? C35 C34 H34 119.8 . . ? C33 C34 H34 119.8 . . ? C34 C35 C36 120.4(4) . . ? C34 C35 H35 119.8 . . ? C36 C35 H35 119.8 . . ? C31 C36 C35 119.5(3) . . ? C31 C36 H36 120.3 . . ? C35 C36 H36 120.3 . . ? C38 C37 C42 119.2(3) . . ? C38 C37 P2 120.5(2) . . ? C42 C37 P2 120.0(2) . . ? C39 C38 C37 120.4(3) . . ? C39 C38 H38 119.8 . . ? C37 C38 H38 119.8 . . ? C40 C39 C38 120.0(3) . . ? C40 C39 H39 120.0 . . ? C38 C39 H39 120.0 . . ? C39 C40 C41 120.5(3) . . ? C39 C40 H40 119.7 . . ? C41 C40 H40 119.7 . . ? C42 C41 C40 119.7(3) . . ? C42 C41 H41 120.1 . . ? C40 C41 H41 120.1 . . ? C41 C42 C37 120.2(3) . . ? C41 C42 H42 119.9 . . ? C37 C42 H42 119.9 . . ? C44 C43 P1 108.17(19) . . ? C44 C43 H43A 110.1 . . ? P1 C43 H43A 110.1 . . ? C44 C43 H43B 110.1 . . ? P1 C43 H43B 110.1 . . ? H43A C43 H43B 108.4 . . ? C43 C44 P2 109.0(2) . . ? C43 C44 H44A 109.9 . . ? P2 C44 H44A 109.9 . . ? C43 C44 H44B 109.9 . . ? P2 C44 H44B 109.9 . . ? H44A C44 H44B 108.3 . . ? C46 C45 C50 117.6(3) . . ? C46 C45 C3 122.3(3) . . ? C50 C45 C3 120.0(3) . . ? C45 C46 C47 122.0(3) . . ? C45 C46 H46 119.0 . . ? C47 C46 H46 119.0 . . ? C48 C47 C46 119.4(3) . . ? C48 C47 H47 120.3 . . ? C46 C47 H47 120.3 . . ? O3 C48 C49 115.4(3) . . ? O3 C48 C47 125.1(3) . . ? C49 C48 C47 119.5(3) . . ? C48 C49 C50 120.1(3) . . ? C48 C49 H49 119.9 . . ? C50 C49 H49 119.9 . . ? C49 C50 C45 121.3(3) . . ? C49 C50 H50 119.3 . . ? C45 C50 H50 119.3 . . ? O3 C51 H51A 109.5 . . ? O3 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? O3 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C53 C52 C57 117.2(3) . . ? C53 C52 C4 121.0(3) . . ? C57 C52 C4 121.6(3) . . ? C54 C53 C52 122.1(3) . . ? C54 C53 H53 118.9 . . ? C52 C53 H53 118.9 . . ? C55 C54 C53 119.4(3) . . ? C55 C54 H54 120.3 . . ? C53 C54 H54 120.3 . . ? O4 C55 C54 124.4(3) . . ? O4 C55 C56 116.0(3) . . ? C54 C55 C56 119.6(3) . . ? C57 C56 C55 120.6(3) . . ? C57 C56 H56 119.7 . . ? C55 C56 H56 119.7 . . ? C56 C57 C52 121.0(3) . . ? C56 C57 H57 119.5 . . ? C52 C57 H57 119.5 . . ? O4 C58 H58A 109.5 . . ? O4 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? O4 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C60 C59 C64 119.7(3) . . ? C60 C59 P3 119.6(2) . . ? C64 C59 P3 120.5(2) . . ? C61 C60 C59 119.9(3) . . ? C61 C60 H60 120.0 . . ? C59 C60 H60 120.0 . . ? C62 C61 C60 120.1(3) . . ? C62 C61 H61 120.0 . . ? C60 C61 H61 120.0 . . ? C61 C62 C63 120.4(3) . . ? C61 C62 H62 119.8 . . ? C63 C62 H62 119.8 . . ? C64 C63 C62 119.9(3) . . ? C64 C63 H63 120.1 . . ? C62 C63 H63 120.1 . . ? C63 C64 C59 120.0(3) . . ? C63 C64 H64 120.0 . . ? C59 C64 H64 120.0 . . ? C70 C65 C66 118.7(3) . . ? C70 C65 P3 122.8(3) . . ? C66 C65 P3 118.5(2) . . ? C67 C66 C65 121.3(3) . . ? C67 C66 H66 119.3 . . ? C65 C66 H66 119.3 . . ? C68 C67 C66 119.6(4) . . ? C68 C67 H67 120.2 . . ? C66 C67 H67 120.2 . . ? C69 C68 C67 119.3(4) . . ? C69 C68 H68 120.3 . . ? C67 C68 H68 120.3 . . ? C68 C69 C70 121.3(4) . . ? C68 C69 H69 119.4 . . ? C70 C69 H69 119.4 . . ? C65 C70 C69 119.7(4) . . ? C65 C70 H70 120.1 . . ? C69 C70 H70 120.1 . . ? C72 C71 C76 119.6(3) . . ? C72 C71 P4 120.3(2) . . ? C76 C71 P4 120.1(2) . . ? C71 C72 C73 119.9(3) . . ? C71 C72 H72 120.0 . . ? C73 C72 H72 120.0 . . ? C74 C73 C72 120.2(3) . . ? C74 C73 H73 119.9 . . ? C72 C73 H73 119.9 . . ? C73 C74 C75 119.9(3) . . ? C73 C74 H74 120.1 . . ? C75 C74 H74 120.1 . . ? C76 C75 C74 120.6(3) . . ? C76 C75 H75 119.7 . . ? C74 C75 H75 119.7 . . ? C75 C76 C71 119.8(3) . . ? C75 C76 H76 120.1 . . ? C71 C76 H76 120.1 . . ? C82 C77 C78 119.2(3) . . ? C82 C77 P4 124.0(2) . . ? C78 C77 P4 116.7(2) . . ? C79 C78 C77 120.3(3) . . ? C79 C78 H78 119.9 . . ? C77 C78 H78 119.9 . . ? C80 C79 C78 120.2(3) . . ? C80 C79 H79 119.9 . . ? C78 C79 H79 119.9 . . ? C79 C80 C81 120.0(3) . . ? C79 C80 H80 120.0 . . ? C81 C80 H80 120.0 . . ? C80 C81 C82 120.2(3) . . ? C80 C81 H81 119.9 . . ? C82 C81 H81 119.9 . . ? C77 C82 C81 120.2(3) . . ? C77 C82 H82 119.9 . . ? C81 C82 H82 119.9 . . ? C84 C83 P3 109.0(2) . . ? C84 C83 H83B 109.9 . . ? P3 C83 H83B 109.9 . . ? C84 C83 H83A 109.9 . . ? P3 C83 H83A 109.9 . . ? H83B C83 H83A 108.3 . . ? C83 C84 P4 108.8(2) . . ? C83 C84 H84A 109.9 . . ? P4 C84 H84A 109.9 . . ? C83 C84 H84B 109.9 . . ? P4 C84 H84B 109.9 . . ? H84A C84 H84B 108.3 . . ? C86 C85 Cl1 112.1(3) . . ? C86 C85 H85A 109.2 . . ? Cl1 C85 H85A 109.2 . . ? C86 C85 H85B 109.2 . . ? Cl1 C85 H85B 109.2 . . ? H85A C85 H85B 107.9 . . ? C85 C86 Cl2 112.3(3) . . ? C85 C86 H86A 109.1 . . ? Cl2 C86 H86A 109.1 . . ? C85 C86 H86B 109.1 . . ? Cl2 C86 H86B 109.1 . . ? H86A C86 H86B 107.9 . . ? C88 C87 Cl3 112.1(3) . . ? C88 C87 H87A 109.2 . . ? Cl3 C87 H87A 109.2 . . ? C88 C87 H87B 109.2 . . ? Cl3 C87 H87B 109.2 . . ? H87A C87 H87B 107.9 . . ? C87 C88 Cl4 112.2(3) . . ? C87 C88 H88A 109.2 . . ? Cl4 C88 H88A 109.2 . . ? C87 C88 H88B 109.2 . . ? Cl4 C88 H88B 109.2 . . ? H88A C88 H88B 107.9 . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.203 _refine_diff_density_min -1.685 _refine_diff_density_rms 0.111 #===END # [Pt(S2C2(C6H4-p-OMe)2)2(PMe3)2], Compound 8 data_jpd269_0m _audit_creation_method SHELXL-97 _chemical_name_systematic ; trans-Bis(trimethylphosphine)bis(1,2-bis(4-methoxyphenyl) ethene-1,2-dithiolato)platinum(IV) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H46 O4 P2 Pt S4' _chemical_formula_sum 'C38 H46 O4 P2 Pt S4' _chemical_formula_weight 952.02 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pt' 'Pt' -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.4203(9) _cell_length_b 13.7295(14) _cell_length_c 33.591(4) _cell_angle_alpha 90.00 _cell_angle_beta 93.757(1) _cell_angle_gamma 90.00 _cell_volume 3875.0(7) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9880 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 28.73 _exptl_crystal_description column _exptl_crystal_colour orange _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.632 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1912 _exptl_absorpt_coefficient_mu 3.958 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5422 _exptl_absorpt_correction_T_max 0.7347 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008a)' _exptl_special_details ; The diffraction data were obtained from 3 sets of 400 frames, each of width 0.5 deg. in \w, collected at \f = 0.00, 90.00 and 180.00 deg. and 2 sets of 800 frames, each of width 0.45 deg in \f, collected at \w = -30.00 and 210.00 deg. The scan time was 10 sec/frame. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-I CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 68500 _diffrn_reflns_av_R_equivalents 0.0388 _diffrn_reflns_av_sigmaI/netI 0.0240 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -45 _diffrn_reflns_limit_l_max 45 _diffrn_reflns_theta_min 2.35 _diffrn_reflns_theta_max 28.75 _reflns_number_total 10000 _reflns_number_gt 9294 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker APEX2 (Bruker-AXS, 2009)' _computing_cell_refinement 'Bruker SAINT (Bruker-AXS 2008)' _computing_data_reduction 'Bruker SAINT (Bruker-AXS 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL(Bruker-AXS 2008a)' _computing_publication_material 'Bruker SHELXTL(Bruker-AXS 2008a)' _publ_section_references ; Bruker-AXS (2009). APEX2, Version 2009.1-0, Madison, WI. Bruker-AXS (2008). SAINT, Version 7.60A, Madison, WI Bruker-AXS (2008a). SHELXTL, Version 2008/4, Madison, WI Sheldrick, G. M. (2008). SHELXS-97 and SHELXL-97. University of G\"ottingen, Germany. Sheldrick, G, M. (2008a). SADABS, Version 2008/2. University of G\"ottingen, Germany. ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. H-atoms were placed in calculated positions (C---H = 0.95 - 0.98 \%A) and included as riding contributions with isotropic displacement parameters 1.2 - 1.5 times those of the attached carbon atoms. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0148P)^2^+3.4173P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Patterson _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10000 _refine_ls_number_parameters 452 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0221 _refine_ls_R_factor_gt 0.0193 _refine_ls_wR_factor_ref 0.0437 _refine_ls_wR_factor_gt 0.0426 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.011 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.514216(8) 0.869230(5) 0.752389(2) 0.01051(2) Uani 1 1 d . . . S1 S 0.33085(6) 0.77928(3) 0.710823(14) 0.01327(9) Uani 1 1 d . . . S2 S 0.50340(6) 0.99360(3) 0.703492(14) 0.01471(9) Uani 1 1 d . . . S3 S 0.52215(6) 0.74508(3) 0.801205(14) 0.01489(9) Uani 1 1 d . . . S4 S 0.70003(6) 0.95822(3) 0.794161(14) 0.01324(9) Uani 1 1 d . . . P1 P 0.72885(6) 0.80329(4) 0.719483(15) 0.01476(10) Uani 1 1 d . . . P2 P 0.29840(6) 0.93364(4) 0.785259(16) 0.01715(10) Uani 1 1 d . . . O1 O -0.11254(18) 0.68416(11) 0.54863(4) 0.0223(3) Uani 1 1 d . . . O2 O 0.31079(19) 1.19107(11) 0.53124(4) 0.0215(3) Uani 1 1 d . . . O3 O 0.67258(19) 0.56199(11) 0.97814(4) 0.0222(3) Uani 1 1 d . . . O4 O 1.13786(17) 1.02530(11) 0.96339(4) 0.0192(3) Uani 1 1 d . . . C1 C 0.3040(2) 0.85524(14) 0.66832(5) 0.0129(4) Uani 1 1 d . . . C2 C 0.3734(2) 0.94269(14) 0.66567(5) 0.0133(4) Uani 1 1 d . . . C3 C 0.6509(2) 0.79569(14) 0.83937(6) 0.0136(4) Uani 1 1 d . . . C4 C 0.7258(2) 0.88166(14) 0.83651(5) 0.0132(4) Uani 1 1 d . . . C5 C 0.1969(2) 0.81036(14) 0.63635(5) 0.0133(4) Uani 1 1 d . . . C6 C 0.2249(2) 0.71613(14) 0.62317(6) 0.0165(4) Uani 1 1 d . . . H6 H 0.3146 0.6816 0.6345 0.020 Uiso 1 1 calc R . . C7 C 0.1256(2) 0.67083(15) 0.59386(6) 0.0174(4) Uani 1 1 d . . . H7 H 0.1484 0.6069 0.5851 0.021 Uiso 1 1 calc R . . C8 C -0.0071(2) 0.72058(15) 0.57771(6) 0.0160(4) Uani 1 1 d . . . C9 C -0.0382(2) 0.81458(15) 0.59081(6) 0.0170(4) Uani 1 1 d . . . H9 H -0.1294 0.8484 0.5800 0.020 Uiso 1 1 calc R . . C10 C 0.0627(2) 0.85893(14) 0.61950(6) 0.0148(4) Uani 1 1 d . . . H10 H 0.0406 0.9233 0.6279 0.018 Uiso 1 1 calc R . . C11 C -0.0778(3) 0.59113(17) 0.53223(7) 0.0258(5) Uani 1 1 d . . . H11A H 0.0282 0.5926 0.5218 0.039 Uiso 1 1 calc R . . H11B H -0.1573 0.5756 0.5105 0.039 Uiso 1 1 calc R . . H11C H -0.0804 0.5413 0.5531 0.039 Uiso 1 1 calc R . . C12 C 0.4169(2) 0.97792(15) 0.59419(6) 0.0174(4) Uani 1 1 d . . . H12 H 0.4676 0.9163 0.5927 0.021 Uiso 1 1 calc R . . C13 C 0.4052(3) 1.03743(15) 0.56069(6) 0.0191(4) Uani 1 1 d . . . H13 H 0.4484 1.0169 0.5366 0.023 Uiso 1 1 calc R . . C14 C 0.3301(2) 1.12702(14) 0.56254(6) 0.0171(4) Uani 1 1 d . . . C15 C 0.2676(3) 1.15644(15) 0.59797(6) 0.0187(4) Uani 1 1 d . . . H15 H 0.2152 1.2175 0.5993 0.022 Uiso 1 1 calc R . . C16 C 0.2815(2) 1.09726(15) 0.63127(6) 0.0175(4) Uani 1 1 d . . . H16 H 0.2399 1.1185 0.6554 0.021 Uiso 1 1 calc R . . C17 C 0.3561(2) 1.00648(14) 0.62978(6) 0.0133(4) Uani 1 1 d . . . C18 C 0.3813(3) 1.16423(17) 0.49537(6) 0.0235(5) Uani 1 1 d . . . H18A H 0.4967 1.1578 0.5006 0.035 Uiso 1 1 calc R . . H18B H 0.3588 1.2145 0.4751 0.035 Uiso 1 1 calc R . . H18C H 0.3368 1.1019 0.4857 0.035 Uiso 1 1 calc R . . C19 C 0.8365(2) 0.92241(14) 0.86880(5) 0.0128(4) Uani 1 1 d . . . C20 C 0.8215(2) 1.01771(14) 0.88190(6) 0.0159(4) Uani 1 1 d . . . H20 H 0.7419 1.0582 0.8692 0.019 Uiso 1 1 calc R . . C21 C 0.9202(2) 1.05571(14) 0.91318(6) 0.0173(4) Uani 1 1 d . . . H21 H 0.9073 1.1210 0.9217 0.021 Uiso 1 1 calc R . . C22 C 1.0367(2) 0.99736(15) 0.93159(6) 0.0155(4) Uani 1 1 d . . . C23 C 1.0572(2) 0.90217(15) 0.91839(6) 0.0162(4) Uani 1 1 d . . . H23 H 1.1391 0.8626 0.9306 0.019 Uiso 1 1 calc R . . C24 C 0.9585(2) 0.86543(14) 0.88750(6) 0.0151(4) Uani 1 1 d . . . H24 H 0.9733 0.8005 0.8787 0.018 Uiso 1 1 calc R . . C25 C 1.1040(3) 1.11622(16) 0.98179(6) 0.0230(5) Uani 1 1 d . . . H25A H 1.1193 1.1694 0.9630 0.035 Uiso 1 1 calc R . . H25B H 1.1759 1.1252 1.0056 0.035 Uiso 1 1 calc R . . H25C H 0.9936 1.1163 0.9894 0.035 Uiso 1 1 calc R . . C26 C 0.6574(2) 0.73558(14) 0.87623(6) 0.0136(4) Uani 1 1 d . . . C27 C 0.6147(2) 0.77508(14) 0.91212(6) 0.0162(4) Uani 1 1 d . . . H27 H 0.5827 0.8414 0.9130 0.019 Uiso 1 1 calc R . . C28 C 0.6177(2) 0.71952(15) 0.94692(6) 0.0176(4) Uani 1 1 d . . . H28 H 0.5883 0.7477 0.9712 0.021 Uiso 1 1 calc R . . C29 C 0.6638(2) 0.62308(14) 0.94568(6) 0.0168(4) Uani 1 1 d . . . C30 C 0.7054(3) 0.58189(15) 0.90995(6) 0.0183(4) Uani 1 1 d . . . H30 H 0.7362 0.5154 0.9092 0.022 Uiso 1 1 calc R . . C31 C 0.7021(2) 0.63736(14) 0.87562(6) 0.0161(4) Uani 1 1 d . . . H31 H 0.7305 0.6086 0.8514 0.019 Uiso 1 1 calc R . . C32 C 0.6122(3) 0.59937(17) 1.01391(6) 0.0243(5) Uani 1 1 d . . . H32A H 0.6806 0.6526 1.0243 0.037 Uiso 1 1 calc R . . H32B H 0.6108 0.5473 1.0338 0.037 Uiso 1 1 calc R . . H32C H 0.5038 0.6238 1.0081 0.037 Uiso 1 1 calc R . . C33 C 0.8315(3) 0.70650(15) 0.74693(7) 0.0224(4) Uani 1 1 d . . . H33A H 0.7606 0.6502 0.7484 0.034 Uiso 1 1 calc R . . H33B H 0.8632 0.7290 0.7740 0.034 Uiso 1 1 calc R . . H33C H 0.9264 0.6878 0.7334 0.034 Uiso 1 1 calc R . . C34 C 0.6792(3) 0.75043(18) 0.67082(7) 0.0257(5) Uani 1 1 d . . . H34A H 0.7772 0.7326 0.6584 0.039 Uiso 1 1 calc R . . H34B H 0.6196 0.7979 0.6540 0.039 Uiso 1 1 calc R . . H34C H 0.6139 0.6921 0.6738 0.039 Uiso 1 1 calc R . . C35 C 0.8789(3) 0.89239(16) 0.70950(6) 0.0211(4) Uani 1 1 d . . . H35A H 0.9734 0.8592 0.7007 0.032 Uiso 1 1 calc R . . H35B H 0.9075 0.9294 0.7339 0.032 Uiso 1 1 calc R . . H35C H 0.8371 0.9369 0.6886 0.032 Uiso 1 1 calc R . . C36 C 0.3480(3) 0.9853(2) 0.83408(7) 0.0336(6) Uani 1 1 d . . . H36A H 0.2499 1.0016 0.8468 0.050 Uiso 1 1 calc R . . H36B H 0.4116 1.0443 0.8313 0.050 Uiso 1 1 calc R . . H36C H 0.4092 0.9378 0.8506 0.050 Uiso 1 1 calc R . . C37 C 0.1488(3) 0.84398(16) 0.79521(7) 0.0220(4) Uani 1 1 d . . . H37A H 0.0530 0.8770 0.8034 0.033 Uiso 1 1 calc R . . H37B H 0.1899 0.8005 0.8166 0.033 Uiso 1 1 calc R . . H37C H 0.1223 0.8059 0.7710 0.033 Uiso 1 1 calc R . . C38 C 0.1939(3) 1.02972(16) 0.75776(8) 0.0261(5) Uani 1 1 d . . . H38A H 0.1593 1.0062 0.7311 0.039 Uiso 1 1 calc R . . H38B H 0.2650 1.0857 0.7555 0.039 Uiso 1 1 calc R . . H38C H 0.1008 1.0495 0.7718 0.039 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.01146(4) 0.01064(4) 0.00917(4) -0.00042(2) -0.00129(2) -0.00007(3) S1 0.0156(2) 0.0126(2) 0.0112(2) 0.00076(16) -0.00227(17) -0.00269(17) S2 0.0177(2) 0.0120(2) 0.0137(2) 0.00092(16) -0.00435(17) -0.00249(18) S3 0.0187(2) 0.0130(2) 0.0125(2) 0.00107(16) -0.00263(18) -0.00350(18) S4 0.0155(2) 0.0129(2) 0.0109(2) 0.00133(16) -0.00269(17) -0.00276(17) P1 0.0138(2) 0.0163(2) 0.0142(2) -0.00216(18) 0.00046(18) 0.00122(19) P2 0.0146(3) 0.0196(3) 0.0171(2) -0.00566(19) 0.00026(19) 0.0008(2) O1 0.0222(8) 0.0236(8) 0.0198(8) -0.0081(6) -0.0080(6) -0.0010(6) O2 0.0297(9) 0.0178(7) 0.0164(7) 0.0059(6) -0.0022(6) 0.0019(6) O3 0.0307(9) 0.0211(8) 0.0152(7) 0.0066(6) 0.0042(6) 0.0034(6) O4 0.0204(8) 0.0206(7) 0.0155(7) -0.0034(6) -0.0063(6) -0.0017(6) C1 0.0137(9) 0.0150(9) 0.0098(8) -0.0001(7) -0.0011(7) 0.0012(7) C2 0.0149(9) 0.0146(9) 0.0100(8) -0.0004(7) -0.0021(7) 0.0013(7) C3 0.0141(9) 0.0147(9) 0.0117(9) -0.0004(7) -0.0016(7) 0.0002(7) C4 0.0144(9) 0.0152(9) 0.0098(8) 0.0010(7) -0.0009(7) 0.0009(7) C5 0.0156(9) 0.0144(9) 0.0096(8) 0.0000(7) 0.0000(7) -0.0024(7) C6 0.0159(10) 0.0153(9) 0.0177(10) 0.0001(7) -0.0030(7) 0.0000(7) C7 0.0218(11) 0.0147(9) 0.0154(9) -0.0023(7) -0.0019(8) -0.0004(8) C8 0.0160(10) 0.0197(10) 0.0120(9) -0.0009(7) -0.0008(7) -0.0043(8) C9 0.0157(10) 0.0200(10) 0.0150(9) -0.0011(7) -0.0013(7) 0.0012(8) C10 0.0164(10) 0.0137(9) 0.0140(9) -0.0007(7) -0.0002(7) -0.0005(7) C11 0.0256(12) 0.0254(12) 0.0255(11) -0.0118(9) -0.0035(9) -0.0031(9) C12 0.0217(10) 0.0149(9) 0.0154(10) 0.0020(7) -0.0007(8) 0.0031(8) C13 0.0249(11) 0.0194(10) 0.0132(9) -0.0001(7) 0.0009(8) 0.0014(8) C14 0.0182(10) 0.0159(10) 0.0166(9) 0.0038(7) -0.0038(8) -0.0016(8) C15 0.0213(11) 0.0138(9) 0.0206(10) 0.0018(7) -0.0017(8) 0.0038(8) C16 0.0196(10) 0.0171(10) 0.0156(9) -0.0005(7) 0.0004(8) 0.0009(8) C17 0.0134(9) 0.0126(9) 0.0135(9) 0.0019(7) -0.0030(7) -0.0013(7) C18 0.0272(12) 0.0253(11) 0.0177(10) 0.0061(8) 0.0003(8) -0.0013(9) C19 0.0134(9) 0.0141(9) 0.0109(8) 0.0007(7) 0.0006(7) -0.0015(7) C20 0.0160(10) 0.0160(9) 0.0152(9) 0.0019(7) -0.0027(7) 0.0004(7) C21 0.0205(10) 0.0135(9) 0.0175(10) -0.0011(7) -0.0017(8) -0.0001(8) C22 0.0158(10) 0.0193(10) 0.0113(9) -0.0004(7) -0.0007(7) -0.0032(8) C23 0.0152(10) 0.0170(10) 0.0161(9) 0.0011(7) -0.0019(7) 0.0026(8) C24 0.0167(10) 0.0146(9) 0.0139(9) -0.0001(7) 0.0004(7) 0.0008(7) C25 0.0264(12) 0.0229(11) 0.0193(10) -0.0061(8) -0.0020(8) -0.0038(9) C26 0.0139(9) 0.0143(9) 0.0124(9) 0.0013(7) -0.0015(7) -0.0022(7) C27 0.0203(10) 0.0124(9) 0.0159(9) 0.0008(7) 0.0007(7) 0.0005(7) C28 0.0211(10) 0.0196(10) 0.0122(9) -0.0005(7) 0.0019(8) -0.0012(8) C29 0.0171(10) 0.0188(10) 0.0142(9) 0.0055(7) -0.0009(7) -0.0020(8) C30 0.0214(11) 0.0134(9) 0.0200(10) 0.0015(7) -0.0001(8) 0.0018(8) C31 0.0189(10) 0.0155(10) 0.0137(9) -0.0006(7) 0.0008(7) 0.0006(8) C32 0.0296(12) 0.0288(12) 0.0148(10) 0.0051(8) 0.0033(8) 0.0004(9) C33 0.0188(11) 0.0187(10) 0.0298(12) 0.0009(8) 0.0022(9) 0.0044(8) C34 0.0226(11) 0.0332(13) 0.0215(11) -0.0118(9) 0.0022(9) 0.0023(9) C35 0.0172(10) 0.0260(11) 0.0204(10) -0.0004(8) 0.0044(8) -0.0019(8) C36 0.0224(12) 0.0523(16) 0.0259(12) -0.0213(11) 0.0009(9) 0.0049(11) C37 0.0178(10) 0.0272(11) 0.0216(11) 0.0013(8) 0.0049(8) 0.0002(9) C38 0.0184(11) 0.0187(11) 0.0411(14) -0.0022(9) 0.0014(9) 0.0038(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 P2 2.3594(6) . ? Pt1 P1 2.3599(5) . ? Pt1 S1 2.3614(5) . ? Pt1 S3 2.3631(5) . ? Pt1 S2 2.3669(5) . ? Pt1 S4 2.3711(5) . ? S1 C1 1.7706(19) . ? S2 C2 1.7658(19) . ? S3 C3 1.7662(19) . ? S4 C4 1.7707(19) . ? P1 C33 1.805(2) . ? P1 C35 1.806(2) . ? P1 C34 1.812(2) . ? P2 C38 1.806(2) . ? P2 C37 1.808(2) . ? P2 C36 1.810(2) . ? O1 C8 1.371(2) . ? O1 C11 1.429(3) . ? O2 C14 1.372(2) . ? O2 C18 1.426(3) . ? O3 C29 1.374(2) . ? O3 C32 1.430(3) . ? O4 C22 1.376(2) . ? O4 C25 1.430(2) . ? C1 C2 1.341(3) . ? C1 C5 1.490(3) . ? C2 C17 1.490(3) . ? C3 C4 1.344(3) . ? C3 C26 1.486(3) . ? C4 C19 1.492(3) . ? C5 C6 1.393(3) . ? C5 C10 1.399(3) . ? C6 C7 1.395(3) . ? C6 H6 0.9500 . ? C7 C8 1.389(3) . ? C7 H7 0.9500 . ? C8 C9 1.394(3) . ? C9 C10 1.383(3) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C17 1.388(3) . ? C12 C13 1.389(3) . ? C12 H12 0.9500 . ? C13 C14 1.386(3) . ? C13 H13 0.9500 . ? C14 C15 1.392(3) . ? C15 C16 1.381(3) . ? C15 H15 0.9500 . ? C16 C17 1.398(3) . ? C16 H16 0.9500 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.389(3) . ? C19 C24 1.406(3) . ? C20 C21 1.397(3) . ? C20 H20 0.9500 . ? C21 C22 1.381(3) . ? C21 H21 0.9500 . ? C22 C23 1.394(3) . ? C23 C24 1.382(3) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 C27 1.391(3) . ? C26 C31 1.400(3) . ? C27 C28 1.395(3) . ? C27 H27 0.9500 . ? C28 C29 1.381(3) . ? C28 H28 0.9500 . ? C29 C30 1.392(3) . ? C30 C31 1.381(3) . ? C30 H30 0.9500 . ? C31 H31 0.9500 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P2 Pt1 P1 179.437(18) . . ? P2 Pt1 S1 88.792(19) . . ? P1 Pt1 S1 90.776(19) . . ? P2 Pt1 S3 86.17(2) . . ? P1 Pt1 S3 93.475(19) . . ? S1 Pt1 S3 91.189(17) . . ? P2 Pt1 S2 93.355(19) . . ? P1 Pt1 S2 86.995(19) . . ? S1 Pt1 S2 88.456(17) . . ? S3 Pt1 S2 179.415(18) . . ? P2 Pt1 S4 91.635(19) . . ? P1 Pt1 S4 88.794(19) . . ? S1 Pt1 S4 179.440(17) . . ? S3 Pt1 S4 88.479(18) . . ? S2 Pt1 S4 91.880(17) . . ? C1 S1 Pt1 102.29(7) . . ? C2 S2 Pt1 101.98(7) . . ? C3 S3 Pt1 102.00(7) . . ? C4 S4 Pt1 102.17(7) . . ? C33 P1 C35 106.03(11) . . ? C33 P1 C34 103.91(11) . . ? C35 P1 C34 103.11(11) . . ? C33 P1 Pt1 113.51(8) . . ? C35 P1 Pt1 113.18(7) . . ? C34 P1 Pt1 115.95(8) . . ? C38 P2 C37 105.66(11) . . ? C38 P2 C36 104.67(12) . . ? C37 P2 C36 102.78(12) . . ? C38 P2 Pt1 113.50(8) . . ? C37 P2 Pt1 113.50(8) . . ? C36 P2 Pt1 115.58(8) . . ? C8 O1 C11 117.48(16) . . ? C14 O2 C18 116.54(16) . . ? C29 O3 C32 116.37(16) . . ? C22 O4 C25 116.62(16) . . ? C2 C1 C5 124.65(17) . . ? C2 C1 S1 123.19(14) . . ? C5 C1 S1 112.15(14) . . ? C1 C2 C17 124.06(17) . . ? C1 C2 S2 124.00(15) . . ? C17 C2 S2 111.89(14) . . ? C4 C3 C26 123.71(17) . . ? C4 C3 S3 124.20(15) . . ? C26 C3 S3 111.94(14) . . ? C3 C4 C19 123.44(17) . . ? C3 C4 S4 123.03(14) . . ? C19 C4 S4 113.52(14) . . ? C6 C5 C10 117.61(17) . . ? C6 C5 C1 120.42(17) . . ? C10 C5 C1 121.94(17) . . ? C5 C6 C7 122.15(18) . . ? C5 C6 H6 118.9 . . ? C7 C6 H6 118.9 . . ? C8 C7 C6 119.07(19) . . ? C8 C7 H7 120.5 . . ? C6 C7 H7 120.5 . . ? O1 C8 C7 124.46(18) . . ? O1 C8 C9 115.86(18) . . ? C7 C8 C9 119.67(18) . . ? C10 C9 C8 120.52(19) . . ? C10 C9 H9 119.7 . . ? C8 C9 H9 119.7 . . ? C9 C10 C5 120.98(18) . . ? C9 C10 H10 119.5 . . ? C5 C10 H10 119.5 . . ? O1 C11 H11A 109.5 . . ? O1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? O1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C17 C12 C13 121.42(19) . . ? C17 C12 H12 119.3 . . ? C13 C12 H12 119.3 . . ? C14 C13 C12 119.60(19) . . ? C14 C13 H13 120.2 . . ? C12 C13 H13 120.2 . . ? O2 C14 C13 124.44(19) . . ? O2 C14 C15 115.91(18) . . ? C13 C14 C15 119.65(18) . . ? C16 C15 C14 120.35(19) . . ? C16 C15 H15 119.8 . . ? C14 C15 H15 119.8 . . ? C15 C16 C17 120.65(19) . . ? C15 C16 H16 119.7 . . ? C17 C16 H16 119.7 . . ? C12 C17 C16 118.33(18) . . ? C12 C17 C2 120.60(17) . . ? C16 C17 C2 121.05(18) . . ? O2 C18 H18A 109.5 . . ? O2 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? O2 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 C24 117.49(17) . . ? C20 C19 C4 121.20(17) . . ? C24 C19 C4 121.30(17) . . ? C19 C20 C21 121.87(18) . . ? C19 C20 H20 119.1 . . ? C21 C20 H20 119.1 . . ? C22 C21 C20 119.36(18) . . ? C22 C21 H21 120.3 . . ? C20 C21 H21 120.3 . . ? O4 C22 C21 124.83(18) . . ? O4 C22 C23 115.15(17) . . ? C21 C22 C23 120.01(18) . . ? C24 C23 C22 120.01(18) . . ? C24 C23 H23 120.0 . . ? C22 C23 H23 120.0 . . ? C23 C24 C19 121.22(18) . . ? C23 C24 H24 119.4 . . ? C19 C24 H24 119.4 . . ? O4 C25 H25A 109.5 . . ? O4 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? O4 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C27 C26 C31 118.25(18) . . ? C27 C26 C3 120.54(17) . . ? C31 C26 C3 121.19(18) . . ? C26 C27 C28 121.45(18) . . ? C26 C27 H27 119.3 . . ? C28 C27 H27 119.3 . . ? C29 C28 C27 119.26(19) . . ? C29 C28 H28 120.4 . . ? C27 C28 H28 120.4 . . ? O3 C29 C28 124.20(19) . . ? O3 C29 C30 115.64(18) . . ? C28 C29 C30 120.16(18) . . ? C31 C30 C29 120.24(19) . . ? C31 C30 H30 119.9 . . ? C29 C30 H30 119.9 . . ? C30 C31 C26 120.63(19) . . ? C30 C31 H31 119.7 . . ? C26 C31 H31 119.7 . . ? O3 C32 H32A 109.5 . . ? O3 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? O3 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? P1 C33 H33A 109.5 . . ? P1 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? P1 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? P1 C34 H34A 109.5 . . ? P1 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? P1 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? P1 C35 H35A 109.5 . . ? P1 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? P1 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? P2 C36 H36A 109.5 . . ? P2 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? P2 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? P2 C37 H37A 109.5 . . ? P2 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? P2 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? P2 C38 H38A 109.5 . . ? P2 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? P2 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 28.75 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.934 _refine_diff_density_min -0.851 _refine_diff_density_rms 0.084 #===END # [Pt(S2C2Me2)2(PMe3)2], Compound 9 data_jpd281a _audit_creation_method SHELXL-97 _chemical_name_systematic ; trans-Bis(trimethylphosphine)bis(but-2-ene-2,3-dithiolato) platinum(IV) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H30 P2 Pt S4' _chemical_formula_sum 'C14 H30 P2 Pt S4' _chemical_formula_weight 583.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pt' 'Pt' -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Cmca _symmetry_space_group_name_Hall '-C 2bc 2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z+1/2' '-x, y+1/2, -z+1/2' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1, z+1/2' '-x+1/2, y+1, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x, y-1/2, -z-1/2' 'x, -y-1/2, z-1/2' '-x, y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, y, -z-1/2' 'x+1/2, -y, z-1/2' '-x+1/2, y+1/2, z' _cell_length_a 15.543(3) _cell_length_b 12.222(2) _cell_length_c 11.3826(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2162.2(6) _cell_formula_units_Z 4 _cell_measurement_temperature 195(2) _cell_measurement_reflns_used 9916 _cell_measurement_theta_min 2.62 _cell_measurement_theta_max 28.73 _exptl_crystal_description Plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.793 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1144 _exptl_absorpt_coefficient_mu 7.017 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4718 _exptl_absorpt_correction_T_max 0.7031 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008a)' _exptl_special_details ; The diffraction data were obtained from 3 sets of 400 frames, each of width 0.5 deg. in \w, collected at \f = 0.00, 90.00 and 180.00 deg. and 2 sets of 800 frames, each of width 0.45 deg in \f, collected at \w = -30.00 and 210.00 deg. The scan time was 20 sec/frame. ; _diffrn_ambient_temperature 195(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-I CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 18292 _diffrn_reflns_av_R_equivalents 0.0404 _diffrn_reflns_av_sigmaI/netI 0.0163 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.62 _diffrn_reflns_theta_max 28.75 _reflns_number_total 1457 _reflns_number_gt 1301 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker APEX2 (Bruker-AXS, 2009)' _computing_cell_refinement 'Bruker SAINT (Bruker-AXS 2008)' _computing_data_reduction 'Bruker SAINT (Bruker-AXS 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL(Bruker-AXS 2008a)' _computing_publication_material 'Bruker SHELXTL(Bruker-AXS 2008a)' _publ_section_references ; Bruker-AXS (2009). APEX2, Version 2009.1-0, Madison, WI. Bruker-AXS (2008). SAINT, Version 7.60A, Madison, WI Bruker-AXS (2008a). SHELXTL, Version 2008/4, Madison, WI Sheldrick, G. M. (2008). SHELXS-97 and SHELXL-97. University of G\"ottingen, Germany. Sheldrick, G, M. (2008a). SADABS, Version 2008/2. University of G\"ottingen, Germany. ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. H-atoms were placed in calculated positions (C---H = 0.98 \%A) and included as riding contributions with isotropic displacement parameters 1.5 times those of the attached carbon atoms. Despite evidence from the displacement ellipsoids of P1 and C3 that the trimethyl phosphine ligand might be disordered, attempts to refine a disordered model in this and the lower symmetry space group C2/c were unsuccessful ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0173P)^2^+6.7524P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00114(10) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1457 _refine_ls_number_parameters 57 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0203 _refine_ls_R_factor_gt 0.0178 _refine_ls_wR_factor_ref 0.0459 _refine_ls_wR_factor_gt 0.0442 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.266 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 1.0000 0.0000 0.0000 0.02488(9) Uani 1 4 d S . . S1 S 0.89094(5) -0.11014(6) 0.08304(7) 0.03548(18) Uani 1 1 d . . . P1 P 1.0000 0.12277(9) 0.16032(11) 0.0460(3) Uani 1 2 d S . . C1 C 0.7958(2) -0.0454(3) 0.0334(3) 0.0388(7) Uani 1 1 d . . . C2 C 0.7161(3) -0.1047(3) 0.0737(4) 0.0525(10) Uani 1 1 d . . . H2A H 0.6652 -0.0691 0.0403 0.079 Uiso 1 1 calc R . . H2B H 0.7128 -0.1025 0.1596 0.079 Uiso 1 1 calc R . . H2C H 0.7185 -0.1809 0.0473 0.079 Uiso 1 1 calc R . . C3 C 0.9066(5) 0.1115(4) 0.2535(6) 0.117(2) Uani 1 1 d U . . H3A H 0.9120 0.1625 0.3195 0.175 Uiso 1 1 calc R . . H3B H 0.9022 0.0365 0.2835 0.175 Uiso 1 1 calc R . . H3C H 0.8549 0.1292 0.2081 0.175 Uiso 1 1 calc R . . C4 C 1.0000 0.2656(3) 0.1235(5) 0.0373(10) Uani 1 2 d S . . H4A H 0.9590 0.2788 0.0596 0.056 Uiso 0.50 1 calc PR . . H4B H 1.0578 0.2875 0.0982 0.056 Uiso 0.50 1 calc PR . . H4C H 0.9832 0.3086 0.1925 0.056 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.03517(14) 0.01660(12) 0.02287(13) 0.00137(7) 0.000 0.000 S1 0.0435(4) 0.0252(3) 0.0377(4) 0.0052(3) 0.0062(3) -0.0036(3) P1 0.0906(11) 0.0205(5) 0.0268(6) -0.0023(4) 0.000 0.000 C1 0.0388(17) 0.0379(17) 0.0397(17) -0.0065(15) 0.0034(14) -0.0030(14) C2 0.0435(19) 0.054(2) 0.060(2) -0.0130(19) 0.0132(18) -0.0099(17) C3 0.187(5) 0.068(3) 0.095(4) -0.038(3) 0.092(4) -0.052(3) C4 0.042(2) 0.0236(19) 0.046(3) -0.0047(18) 0.000 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 S1 2.3619(8) . ? Pt1 S1 2.3620(8) 9_755 ? Pt1 S1 2.3620(8) 12_755 ? Pt1 S1 2.3620(8) 4 ? Pt1 P1 2.3625(12) 9_755 ? Pt1 P1 2.3625(12) . ? S1 C1 1.769(4) . ? P1 C4 1.796(4) . ? P1 C3 1.802(6) 12_755 ? P1 C3 1.802(6) . ? C1 C1 1.345(7) 4 ? C1 C2 1.506(5) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S1 Pt1 S1 180.0 . 9_755 ? S1 Pt1 S1 91.73(4) . 12_755 ? S1 Pt1 S1 88.28(4) 9_755 12_755 ? S1 Pt1 S1 88.27(4) . 4 ? S1 Pt1 S1 91.72(4) 9_755 4 ? S1 Pt1 S1 180.00(5) 12_755 4 ? S1 Pt1 P1 86.97(3) . 9_755 ? S1 Pt1 P1 93.03(3) 9_755 9_755 ? S1 Pt1 P1 86.97(3) 12_755 9_755 ? S1 Pt1 P1 93.03(3) 4 9_755 ? S1 Pt1 P1 93.03(3) . . ? S1 Pt1 P1 86.97(3) 9_755 . ? S1 Pt1 P1 93.03(3) 12_755 . ? S1 Pt1 P1 86.97(3) 4 . ? P1 Pt1 P1 180.0 9_755 . ? C1 S1 Pt1 102.53(12) . . ? C4 P1 C3 102.2(2) . 12_755 ? C4 P1 C3 102.2(2) . . ? C3 P1 C3 107.2(6) 12_755 . ? C4 P1 Pt1 115.92(17) . . ? C3 P1 Pt1 113.93(19) 12_755 . ? C3 P1 Pt1 113.93(19) . . ? C1 C1 C2 124.6(2) 4 . ? C1 C1 S1 123.32(12) 4 . ? C2 C1 S1 112.0(3) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? P1 C3 H3A 109.5 . . ? P1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? P1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? P1 C4 H4A 109.5 . . ? P1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? P1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.75 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.857 _refine_diff_density_min -0.712 _refine_diff_density_rms 0.092 #===END # [Pd(S2C2(C6H4-p-OMe)2)2], Compound 10 data_jpd219_0m _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis(1,2-bis(4-methoxyphenyl)ethen-1,2-dithiolato) palladium(II) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H28 O4 Pd S4' _chemical_formula_sum 'C32 H28 O4 Pd S4' _chemical_formula_weight 711.18 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.792(3) _cell_length_b 12.201(3) _cell_length_c 14.106(4) _cell_angle_alpha 104.443(4) _cell_angle_beta 104.466(4) _cell_angle_gamma 105.890(4) _cell_volume 1475.3(7) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3485 _cell_measurement_theta_min 2.94 _cell_measurement_theta_max 24.76 _exptl_crystal_description Parallelepiped _exptl_crystal_colour orange _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.601 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 724 _exptl_absorpt_coefficient_mu 0.949 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7284 _exptl_absorpt_correction_T_max 0.9767 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008a)' _exptl_special_details ; The diffraction data were collected in three sets of 606 frames (0.3 deg. width in \w) at \f = 0, 120 and 240 deg. A scan time of 90 sec/frame was used. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-I CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 10542 _diffrn_reflns_av_R_equivalents 0.0570 _diffrn_reflns_av_sigmaI/netI 0.0915 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 24.80 _reflns_number_total 5061 _reflns_number_gt 3415 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker APEX2 (Bruker-AXS, 2008)' _computing_cell_refinement 'Bruker SAINT (Bruker-AXS 2008a)' _computing_data_reduction 'Bruker SAINT (Bruker-AXS 2008a)' _computing_structure_solution 'SHELXM (Sheldrick, 2004)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL(Bruker-AXS 2000)' _computing_publication_material 'Bruker SHELXTL(Bruker-AXS 2000)' _publ_section_references ; Bruker-AXS (2008). APEX2, Version 2008.2-0, Madison, WI. Bruker-AXS (2008a). SAINT, Version 7.53A, Madison, WI Bruker-AXS (2000). SHELXTL, Version 6.14, Madison, WI Sheldrick, G, M. (2004). XM, Version 2004/1. University of G\"ottingen, Germany. Sheldrick, G. M. (2008). SHELXL-97. University of G\"ottingen, Germany. Sheldrick, G, M. (2008a). SADABS, Version 2008/2. University of G\"ottingen, Germany. ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. H-atoms were placed in calculated positions (C---H = 0.95 - 0.98 \%A) and included as riding contributions with isotropic displacement parameters 1.2 - 1.5 times those of the attached carbon atoms. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0731P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5061 _refine_ls_number_parameters 374 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0898 _refine_ls_R_factor_gt 0.0523 _refine_ls_wR_factor_ref 0.1396 _refine_ls_wR_factor_gt 0.1218 _refine_ls_goodness_of_fit_ref 0.977 _refine_ls_restrained_S_all 0.977 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.21602(6) 0.41828(4) 0.05543(4) 0.01721(17) Uani 1 1 d . . . S1 S 0.07490(18) 0.41021(14) -0.10094(12) 0.0188(4) Uani 1 1 d . . . S2 S 0.03437(18) 0.24543(14) 0.03557(12) 0.0195(4) Uani 1 1 d . . . S3 S 0.37003(18) 0.42152(14) 0.20689(12) 0.0182(4) Uani 1 1 d . . . S4 S 0.39023(18) 0.59444(14) 0.07511(12) 0.0195(4) Uani 1 1 d . . . O1 O -0.4442(5) 0.1334(4) -0.5688(3) 0.0226(10) Uani 1 1 d . . . O2 O -0.6419(5) -0.1618(4) -0.1458(3) 0.0237(10) Uani 1 1 d . . . O3 O 1.0050(5) 0.6358(4) 0.6069(3) 0.0235(10) Uani 1 1 d . . . O4 O 1.0027(5) 1.0857(4) 0.3232(3) 0.0233(10) Uani 1 1 d . . . C1 C -0.0741(7) 0.2772(5) -0.1478(5) 0.0174(14) Uani 1 1 d . . . C2 C -0.0986(7) 0.2052(5) -0.0846(5) 0.0167(14) Uani 1 1 d . . . C3 C 0.5261(7) 0.5498(5) 0.2462(5) 0.0175(14) Uani 1 1 d . . . C4 C 0.5320(7) 0.6303(5) 0.1895(5) 0.0172(14) Uani 1 1 d . . . C5 C -0.1708(7) 0.2414(5) -0.2586(5) 0.0160(14) Uani 1 1 d . . . C6 C -0.2292(7) 0.3232(5) -0.2930(5) 0.0173(14) Uani 1 1 d . . . H6 H -0.2046 0.4022 -0.2458 0.021 Uiso 1 1 calc R . . C7 C -0.3233(7) 0.2896(5) -0.3961(5) 0.0180(14) Uani 1 1 d . . . H7 H -0.3647 0.3445 -0.4184 0.022 Uiso 1 1 calc R . . C8 C -0.3559(7) 0.1747(6) -0.4660(4) 0.0159(13) Uani 1 1 d . . . C9 C -0.2959(7) 0.0952(6) -0.4316(5) 0.0174(14) Uani 1 1 d . . . H9 H -0.3183 0.0171 -0.4795 0.021 Uiso 1 1 calc R . . C10 C -0.2047(7) 0.1259(6) -0.3300(5) 0.0184(14) Uani 1 1 d . . . H10 H -0.1652 0.0697 -0.3084 0.022 Uiso 1 1 calc R . . C11 C -0.5302(7) 0.2021(6) -0.6035(5) 0.0260(16) Uani 1 1 d . . . H11A H -0.5940 0.2135 -0.5611 0.039 Uiso 1 1 calc R . . H11B H -0.5940 0.1587 -0.6767 0.039 Uiso 1 1 calc R . . H11C H -0.4616 0.2814 -0.5966 0.039 Uiso 1 1 calc R . . C12 C -0.2370(7) 0.1000(5) -0.1106(5) 0.0156(14) Uani 1 1 d . . . C13 C -0.2345(7) 0.0071(5) -0.0691(5) 0.0184(14) Uani 1 1 d . . . H13 H -0.1399 0.0064 -0.0314 0.022 Uiso 1 1 calc R . . C14 C -0.3650(7) -0.0833(6) -0.0813(5) 0.0202(15) Uani 1 1 d . . . H14 H -0.3597 -0.1466 -0.0544 0.024 Uiso 1 1 calc R . . C15 C -0.5039(7) -0.0811(6) -0.1331(5) 0.0220(15) Uani 1 1 d . . . C16 C -0.5110(7) 0.0065(5) -0.1790(5) 0.0219(15) Uani 1 1 d . . . H16 H -0.6062 0.0047 -0.2183 0.026 Uiso 1 1 calc R . . C17 C -0.3801(7) 0.0963(5) -0.1677(5) 0.0195(14) Uani 1 1 d . . . H17 H -0.3864 0.1563 -0.1987 0.023 Uiso 1 1 calc R . . C18 C -0.6407(8) -0.2520(6) -0.0971(5) 0.0293(17) Uani 1 1 d . . . H18A H -0.5909 -0.3040 -0.1273 0.044 Uiso 1 1 calc R . . H18B H -0.7448 -0.3014 -0.1086 0.044 Uiso 1 1 calc R . . H18C H -0.5856 -0.2120 -0.0221 0.044 Uiso 1 1 calc R . . C19 C 0.6525(7) 0.5708(5) 0.3395(5) 0.0174(14) Uani 1 1 d . . . C20 C 0.8013(7) 0.6054(5) 0.3399(5) 0.0200(15) Uani 1 1 d . . . H20 H 0.8197 0.6122 0.2783 0.024 Uiso 1 1 calc R . . C21 C 0.9222(7) 0.6299(6) 0.4277(5) 0.0203(15) Uani 1 1 d . . . H21 H 1.0226 0.6557 0.4270 0.024 Uiso 1 1 calc R . . C22 C 0.8948(7) 0.6162(6) 0.5166(5) 0.0205(15) Uani 1 1 d . . . C23 C 0.7484(7) 0.5790(5) 0.5169(5) 0.0207(15) Uani 1 1 d . . . H23 H 0.7300 0.5702 0.5781 0.025 Uiso 1 1 calc R . . C24 C 0.6294(7) 0.5548(5) 0.4292(5) 0.0184(14) Uani 1 1 d . . . H24 H 0.5292 0.5264 0.4298 0.022 Uiso 1 1 calc R . . C25 C 1.1585(7) 0.6883(6) 0.6132(5) 0.0285(16) Uani 1 1 d . . . H25A H 1.1771 0.6369 0.5561 0.043 Uiso 1 1 calc R . . H25B H 1.2267 0.6946 0.6800 0.043 Uiso 1 1 calc R . . H25C H 1.1765 0.7693 0.6079 0.043 Uiso 1 1 calc R . . C26 C 0.6556(7) 0.7498(5) 0.2236(5) 0.0162(14) Uani 1 1 d . . . C27 C 0.7140(7) 0.7875(6) 0.1530(5) 0.0174(14) Uani 1 1 d . . . H27 H 0.6739 0.7358 0.0822 0.021 Uiso 1 1 calc R . . C28 C 0.8302(7) 0.8990(6) 0.1817(5) 0.0178(14) Uani 1 1 d . . . H28 H 0.8683 0.9225 0.1313 0.021 Uiso 1 1 calc R . . C29 C 0.8889(7) 0.9751(6) 0.2853(5) 0.0191(14) Uani 1 1 d . . . C30 C 0.8289(7) 0.9394(6) 0.3580(5) 0.0201(14) Uani 1 1 d . . . H30 H 0.8677 0.9915 0.4286 0.024 Uiso 1 1 calc R . . C31 C 0.7137(7) 0.8289(6) 0.3274(5) 0.0195(14) Uani 1 1 d . . . H31 H 0.6732 0.8060 0.3771 0.023 Uiso 1 1 calc R . . C32 C 1.0423(8) 1.1338(6) 0.2466(5) 0.0279(16) Uani 1 1 d . . . H32A H 1.0891 1.0844 0.2095 0.042 Uiso 1 1 calc R . . H32B H 1.1137 1.2175 0.2811 0.042 Uiso 1 1 calc R . . H32C H 0.9511 1.1322 0.1969 0.042 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0178(3) 0.0156(3) 0.0147(3) 0.0033(2) 0.0042(2) 0.0037(2) S1 0.0200(9) 0.0148(8) 0.0174(9) 0.0043(7) 0.0045(7) 0.0027(7) S2 0.0210(9) 0.0191(9) 0.0161(9) 0.0075(7) 0.0045(7) 0.0038(7) S3 0.0184(9) 0.0163(9) 0.0167(9) 0.0049(7) 0.0042(7) 0.0036(7) S4 0.0221(9) 0.0162(9) 0.0174(9) 0.0055(7) 0.0050(7) 0.0046(7) O1 0.025(3) 0.018(2) 0.020(3) 0.0055(19) 0.004(2) 0.007(2) O2 0.024(3) 0.016(2) 0.023(3) 0.006(2) 0.004(2) -0.001(2) O3 0.015(2) 0.030(3) 0.021(2) 0.007(2) 0.004(2) 0.006(2) O4 0.022(2) 0.019(2) 0.024(3) 0.006(2) 0.006(2) 0.001(2) C1 0.017(3) 0.014(3) 0.019(3) 0.001(3) 0.005(3) 0.008(3) C2 0.023(4) 0.013(3) 0.023(4) 0.008(3) 0.015(3) 0.012(3) C3 0.022(4) 0.013(3) 0.017(3) 0.001(3) 0.009(3) 0.006(3) C4 0.019(4) 0.012(3) 0.018(3) -0.001(3) 0.008(3) 0.005(3) C5 0.012(3) 0.015(3) 0.021(3) 0.006(3) 0.008(3) 0.004(3) C6 0.023(4) 0.012(3) 0.020(4) 0.007(3) 0.010(3) 0.008(3) C7 0.020(3) 0.010(3) 0.022(4) 0.005(3) 0.006(3) 0.004(3) C8 0.014(3) 0.022(4) 0.012(3) 0.007(3) 0.006(3) 0.003(3) C9 0.018(3) 0.016(3) 0.018(3) 0.005(3) 0.008(3) 0.005(3) C10 0.022(4) 0.020(3) 0.017(3) 0.009(3) 0.008(3) 0.010(3) C11 0.023(4) 0.035(4) 0.023(4) 0.013(3) 0.007(3) 0.012(3) C12 0.019(3) 0.011(3) 0.012(3) -0.001(3) 0.007(3) 0.003(3) C13 0.023(4) 0.015(3) 0.016(3) 0.004(3) 0.003(3) 0.009(3) C14 0.025(4) 0.019(4) 0.017(4) 0.007(3) 0.008(3) 0.008(3) C15 0.024(4) 0.016(3) 0.019(4) -0.002(3) 0.010(3) 0.002(3) C16 0.021(4) 0.017(4) 0.023(4) 0.005(3) 0.004(3) 0.005(3) C17 0.029(4) 0.014(3) 0.018(3) 0.006(3) 0.009(3) 0.009(3) C18 0.027(4) 0.029(4) 0.028(4) 0.010(3) 0.012(3) 0.002(3) C19 0.017(3) 0.010(3) 0.017(3) 0.000(3) 0.001(3) 0.002(3) C20 0.022(4) 0.015(3) 0.023(4) 0.005(3) 0.013(3) 0.004(3) C21 0.017(4) 0.024(4) 0.023(4) 0.007(3) 0.011(3) 0.010(3) C22 0.023(4) 0.015(3) 0.020(4) 0.004(3) 0.003(3) 0.006(3) C23 0.023(4) 0.019(4) 0.022(4) 0.007(3) 0.008(3) 0.010(3) C24 0.019(3) 0.013(3) 0.020(4) 0.005(3) 0.006(3) 0.004(3) C25 0.022(4) 0.030(4) 0.030(4) 0.006(3) 0.004(3) 0.012(3) C26 0.018(3) 0.015(3) 0.020(3) 0.007(3) 0.008(3) 0.009(3) C27 0.014(3) 0.020(3) 0.016(3) 0.002(3) 0.002(3) 0.009(3) C28 0.023(4) 0.020(3) 0.018(3) 0.008(3) 0.010(3) 0.012(3) C29 0.019(4) 0.018(3) 0.025(4) 0.010(3) 0.009(3) 0.010(3) C30 0.019(4) 0.017(3) 0.022(4) 0.006(3) 0.006(3) 0.005(3) C31 0.024(4) 0.023(4) 0.019(4) 0.013(3) 0.010(3) 0.013(3) C32 0.031(4) 0.022(4) 0.028(4) 0.006(3) 0.015(3) 0.003(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 S4 2.2505(18) . ? Pd1 S1 2.2535(18) . ? Pd1 S2 2.2566(18) . ? Pd1 S3 2.2706(18) . ? S1 C1 1.699(6) . ? S2 C2 1.715(6) . ? S3 C3 1.711(6) . ? S4 C4 1.708(6) . ? O1 C8 1.370(7) . ? O1 C11 1.427(7) . ? O2 C15 1.375(7) . ? O2 C18 1.436(8) . ? O3 C22 1.365(7) . ? O3 C25 1.433(7) . ? O4 C29 1.367(7) . ? O4 C32 1.436(8) . ? C1 C2 1.417(9) . ? C1 C5 1.491(8) . ? C2 C12 1.478(8) . ? C3 C4 1.411(9) . ? C3 C19 1.474(8) . ? C4 C26 1.489(8) . ? C5 C6 1.405(8) . ? C5 C10 1.406(8) . ? C6 C7 1.400(9) . ? C6 H6 0.9500 . ? C7 C8 1.395(8) . ? C7 H7 0.9500 . ? C8 C9 1.388(8) . ? C9 C10 1.379(8) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.401(9) . ? C12 C17 1.414(9) . ? C13 C14 1.380(8) . ? C13 H13 0.9500 . ? C14 C15 1.384(9) . ? C14 H14 0.9500 . ? C15 C16 1.388(9) . ? C16 C17 1.383(8) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C24 1.391(9) . ? C19 C20 1.399(8) . ? C20 C21 1.383(9) . ? C20 H20 0.9500 . ? C21 C22 1.387(9) . ? C21 H21 0.9500 . ? C22 C23 1.381(9) . ? C23 C24 1.373(9) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 C27 1.378(8) . ? C26 C31 1.405(8) . ? C27 C28 1.399(8) . ? C27 H27 0.9500 . ? C28 C29 1.393(9) . ? C28 H28 0.9500 . ? C29 C30 1.404(8) . ? C30 C31 1.383(8) . ? C30 H30 0.9500 . ? C31 H31 0.9500 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S4 Pd1 S1 91.10(6) . . ? S4 Pd1 S2 177.66(7) . . ? S1 Pd1 S2 87.82(6) . . ? S4 Pd1 S3 87.96(6) . . ? S1 Pd1 S3 175.59(7) . . ? S2 Pd1 S3 93.27(6) . . ? C1 S1 Pd1 105.8(2) . . ? C2 S2 Pd1 106.0(2) . . ? C3 S3 Pd1 105.3(2) . . ? C4 S4 Pd1 105.9(2) . . ? C8 O1 C11 118.4(5) . . ? C15 O2 C18 116.9(5) . . ? C22 O3 C25 117.1(5) . . ? C29 O4 C32 115.9(5) . . ? C2 C1 C5 123.5(6) . . ? C2 C1 S1 120.7(5) . . ? C5 C1 S1 115.7(5) . . ? C1 C2 C12 125.0(6) . . ? C1 C2 S2 119.2(5) . . ? C12 C2 S2 115.6(4) . . ? C4 C3 C19 122.2(6) . . ? C4 C3 S3 120.3(5) . . ? C19 C3 S3 117.4(4) . . ? C3 C4 C26 124.0(6) . . ? C3 C4 S4 120.3(5) . . ? C26 C4 S4 115.7(5) . . ? C6 C5 C10 119.1(6) . . ? C6 C5 C1 120.1(5) . . ? C10 C5 C1 120.8(5) . . ? C7 C6 C5 120.7(6) . . ? C7 C6 H6 119.7 . . ? C5 C6 H6 119.7 . . ? C8 C7 C6 119.5(6) . . ? C8 C7 H7 120.3 . . ? C6 C7 H7 120.3 . . ? O1 C8 C9 116.4(5) . . ? O1 C8 C7 124.3(6) . . ? C9 C8 C7 119.4(6) . . ? C10 C9 C8 122.0(6) . . ? C10 C9 H9 119.0 . . ? C8 C9 H9 119.0 . . ? C9 C10 C5 119.3(6) . . ? C9 C10 H10 120.4 . . ? C5 C10 H10 120.4 . . ? O1 C11 H11A 109.5 . . ? O1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? O1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 C12 C17 117.0(6) . . ? C13 C12 C2 121.4(6) . . ? C17 C12 C2 121.1(5) . . ? C14 C13 C12 122.1(6) . . ? C14 C13 H13 118.9 . . ? C12 C13 H13 118.9 . . ? C13 C14 C15 119.5(6) . . ? C13 C14 H14 120.2 . . ? C15 C14 H14 120.2 . . ? O2 C15 C14 125.3(6) . . ? O2 C15 C16 114.7(6) . . ? C14 C15 C16 120.0(6) . . ? C17 C16 C15 120.3(6) . . ? C17 C16 H16 119.8 . . ? C15 C16 H16 119.8 . . ? C16 C17 C12 120.8(6) . . ? C16 C17 H17 119.6 . . ? C12 C17 H17 119.6 . . ? O2 C18 H18A 109.5 . . ? O2 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? O2 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C24 C19 C20 117.3(6) . . ? C24 C19 C3 121.9(6) . . ? C20 C19 C3 120.8(6) . . ? C21 C20 C19 121.8(6) . . ? C21 C20 H20 119.1 . . ? C19 C20 H20 119.1 . . ? C20 C21 C22 119.0(6) . . ? C20 C21 H21 120.5 . . ? C22 C21 H21 120.5 . . ? O3 C22 C23 115.9(6) . . ? O3 C22 C21 124.1(6) . . ? C23 C22 C21 120.0(6) . . ? C24 C23 C22 120.4(6) . . ? C24 C23 H23 119.8 . . ? C22 C23 H23 119.8 . . ? C23 C24 C19 121.3(6) . . ? C23 C24 H24 119.3 . . ? C19 C24 H24 119.3 . . ? O3 C25 H25A 109.5 . . ? O3 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? O3 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C27 C26 C31 118.0(6) . . ? C27 C26 C4 120.5(6) . . ? C31 C26 C4 121.5(5) . . ? C26 C27 C28 122.4(6) . . ? C26 C27 H27 118.8 . . ? C28 C27 H27 118.8 . . ? C29 C28 C27 118.9(6) . . ? C29 C28 H28 120.5 . . ? C27 C28 H28 120.5 . . ? O4 C29 C28 124.5(6) . . ? O4 C29 C30 115.9(6) . . ? C28 C29 C30 119.5(6) . . ? C31 C30 C29 120.3(6) . . ? C31 C30 H30 119.9 . . ? C29 C30 H30 119.9 . . ? C30 C31 C26 120.9(6) . . ? C30 C31 H31 119.6 . . ? C26 C31 H31 119.6 . . ? O4 C32 H32A 109.5 . . ? O4 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? O4 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 24.80 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.476 _refine_diff_density_min -1.232 _refine_diff_density_rms 0.145 #===END # [Pd(S2C2(C6H4-p-OMe)2)(PMe3)2], Compound 11 data_jpd297_0m _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis(trimethyphosphine)(1,2-bis(4-methoxyphenyl)ethene- 1,2-dithiolato)palladium(II) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H32 O2 P2 Pd S2' _chemical_formula_sum 'C22 H32 O2 P2 Pd S2' _chemical_formula_weight 560.94 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.9483(6) _cell_length_b 20.1445(14) _cell_length_c 14.4855(10) _cell_angle_alpha 90.00 _cell_angle_beta 106.924(1) _cell_angle_gamma 90.00 _cell_volume 2498.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9978 _cell_measurement_theta_min 2.59 _cell_measurement_theta_max 28.71 _exptl_crystal_description Slab _exptl_crystal_colour orange _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.491 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1152 _exptl_absorpt_coefficient_mu 1.054 _exptl_absorpt_correction_type 'integration numerical gaussian' _exptl_absorpt_correction_T_min 0.7601 _exptl_absorpt_correction_T_max 0.8929 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008a)' _exptl_special_details ; The diffraction data were obtained from 3 sets of 400 frames, each of width 0.5 deg. in \w, collected at \f = 0.00, 90.00 and 180.00 deg. and 2 sets of 800 frames, each of width 0.45 deg in \f, collected at \w = -30.00 and 210.00 deg. The scan time was 15 sec/frame. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-I CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 42874 _diffrn_reflns_av_R_equivalents 0.0340 _diffrn_reflns_av_sigmaI/netI 0.0201 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.38 _diffrn_reflns_theta_max 28.71 _reflns_number_total 6432 _reflns_number_gt 5878 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 (Bruker-AXS, 2009)' _computing_cell_refinement 'Bruker SAINT (Bruker-AXS 2008)' _computing_data_reduction 'Bruker SAINT (Bruker-AXS 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL(Bruker-AXS 2008a)' _computing_publication_material 'Bruker SHELXTL(Bruker-AXS 2008a)' _publ_section_references ; Bruker-AXS (2009). APEX2, Version 2009.3-0, Madison, WI. Bruker-AXS (2008). SAINT, Version 7.60A, Madison, WI Bruker-AXS (2008a). SHELXTL, Version 2008/4, Madison, WI Sheldrick, G. M. (2008). SHELXS-97 and SHELXL-97. Acta Cryst. A64, 112-122. Sheldrick, G, M. (2008a). SADABS, Version 2008/2. University of G\"ottingen, Germany. Sheldrick, G, M. (2008b). CELL_NOW, Version 2008/2 University of G\"ottingen, Germany. ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. H-atoms were placed in calculated positions (C---H = 0.95 - 0.98 \%A) and included as riding contributions with isotropic displacement parameters 1.2 - 1.5 times those of the attached carbon atoms. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0237P)^2^+1.6584P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6432 _refine_ls_number_parameters 270 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0250 _refine_ls_R_factor_gt 0.0215 _refine_ls_wR_factor_ref 0.0559 _refine_ls_wR_factor_gt 0.0536 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.084808(13) 0.368677(6) 0.560568(8) 0.01565(4) Uani 1 1 d . . . S1 S 0.32322(4) 0.42062(2) 0.60062(3) 0.01845(8) Uani 1 1 d . . . S2 S 0.14057(4) 0.339148(19) 0.71962(3) 0.01733(8) Uani 1 1 d . . . P1 P 0.04612(5) 0.40629(2) 0.40481(3) 0.01912(8) Uani 1 1 d . . . P2 P -0.14382(5) 0.30899(2) 0.52992(3) 0.02342(9) Uani 1 1 d . . . O1 O 0.99551(13) 0.52569(6) 0.88689(9) 0.0248(2) Uani 1 1 d . . . O2 O 0.51637(13) 0.33042(6) 1.18315(8) 0.0208(2) Uani 1 1 d . . . C10 C 0.38263(17) 0.36109(7) 0.88353(11) 0.0152(3) Uani 1 1 d . . . C1 C 0.40317(17) 0.40776(7) 0.72506(11) 0.0162(3) Uani 1 1 d . . . C2 C 0.32638(17) 0.37354(7) 0.77759(11) 0.0155(3) Uani 1 1 d . . . C3 C 0.56129(16) 0.43763(7) 0.76409(10) 0.0152(3) Uani 1 1 d . . . C4 C 0.69463(17) 0.39831(8) 0.79005(11) 0.0185(3) Uani 1 1 d . . . H4 H 0.6847 0.3517 0.7797 0.022 Uiso 1 1 calc R . . C5 C 0.84287(18) 0.42544(8) 0.83097(11) 0.0195(3) Uani 1 1 d . . . H5 H 0.9328 0.3978 0.8477 0.023 Uiso 1 1 calc R . . C6 C 0.85675(17) 0.49350(8) 0.84683(11) 0.0191(3) Uani 1 1 d . . . C7 C 0.72473(18) 0.53374(8) 0.82008(12) 0.0199(3) Uani 1 1 d . . . H7 H 0.7346 0.5802 0.8311 0.024 Uiso 1 1 calc R . . C8 C 0.57921(17) 0.50637(8) 0.77746(11) 0.0180(3) Uani 1 1 d . . . H8 H 0.4904 0.5345 0.7570 0.022 Uiso 1 1 calc R . . C9 C 1.13277(18) 0.48505(9) 0.91491(13) 0.0266(4) Uani 1 1 d . . . H9A H 1.1183 0.4498 0.9581 0.040 Uiso 1 1 calc R . . H9B H 1.2229 0.5124 0.9484 0.040 Uiso 1 1 calc R . . H9C H 1.1510 0.4652 0.8574 0.040 Uiso 1 1 calc R . . C11 C 0.47961(17) 0.40526(8) 0.94951(11) 0.0173(3) Uani 1 1 d . . . H11 H 0.5167 0.4441 0.9262 0.021 Uiso 1 1 calc R . . C12 C 0.52218(17) 0.39320(8) 1.04792(11) 0.0183(3) Uani 1 1 d . . . H12 H 0.5886 0.4237 1.0909 0.022 Uiso 1 1 calc R . . C13 C 0.46866(17) 0.33688(8) 1.08461(11) 0.0167(3) Uani 1 1 d . . . C14 C 0.37345(19) 0.29218(8) 1.02136(12) 0.0211(3) Uani 1 1 d . . . H14 H 0.3365 0.2534 1.0450 0.025 Uiso 1 1 calc R . . C15 C 0.33266(18) 0.30485(8) 0.92247(11) 0.0205(3) Uani 1 1 d . . . H15 H 0.2679 0.2738 0.8797 0.025 Uiso 1 1 calc R . . C16 C 0.4485(2) 0.27720(9) 1.22192(13) 0.0289(4) Uani 1 1 d . . . H16A H 0.3344 0.2814 1.2004 0.043 Uiso 1 1 calc R . . H16B H 0.4854 0.2788 1.2926 0.043 Uiso 1 1 calc R . . H16C H 0.4788 0.2348 1.1995 0.043 Uiso 1 1 calc R . . C17 C 0.1393(2) 0.48511(8) 0.39738(12) 0.0249(3) Uani 1 1 d . . . H17A H 0.2522 0.4810 0.4274 0.037 Uiso 1 1 calc R . . H17B H 0.0973 0.5192 0.4313 0.037 Uiso 1 1 calc R . . H17C H 0.1189 0.4978 0.3295 0.037 Uiso 1 1 calc R . . C18 C 0.1272(2) 0.35160(9) 0.33199(13) 0.0284(4) Uani 1 1 d . . . H18A H 0.1091 0.3707 0.2674 0.043 Uiso 1 1 calc R . . H18B H 0.0765 0.3081 0.3268 0.043 Uiso 1 1 calc R . . H18C H 0.2397 0.3465 0.3625 0.043 Uiso 1 1 calc R . . C19 C -0.1504(2) 0.42212(10) 0.32654(13) 0.0307(4) Uani 1 1 d . . . H19A H -0.2011 0.4556 0.3563 0.046 Uiso 1 1 calc R . . H19B H -0.2111 0.3809 0.3172 0.046 Uiso 1 1 calc R . . H19C H -0.1446 0.4384 0.2639 0.046 Uiso 1 1 calc R . . C20 C -0.1754(2) 0.25025(10) 0.43085(15) 0.0366(4) Uani 1 1 d . . . H20A H -0.2696 0.2241 0.4265 0.055 Uiso 1 1 calc R . . H20B H -0.0852 0.2205 0.4423 0.055 Uiso 1 1 calc R . . H20C H -0.1885 0.2744 0.3703 0.055 Uiso 1 1 calc R . . C21 C -0.3254(2) 0.35548(11) 0.50453(16) 0.0352(4) Uani 1 1 d . . . H21A H -0.3348 0.3847 0.4490 0.053 Uiso 1 1 calc R . . H21B H -0.3256 0.3823 0.5610 0.053 Uiso 1 1 calc R . . H21C H -0.4137 0.3245 0.4900 0.053 Uiso 1 1 calc R . . C22 C -0.1609(2) 0.25473(11) 0.62660(15) 0.0393(5) Uani 1 1 d . . . H22A H -0.2640 0.2336 0.6080 0.059 Uiso 1 1 calc R . . H22B H -0.1482 0.2808 0.6855 0.059 Uiso 1 1 calc R . . H22C H -0.0797 0.2205 0.6384 0.059 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.01507(6) 0.01598(6) 0.01393(6) -0.00189(4) 0.00111(4) 0.00008(4) S1 0.01682(16) 0.02297(18) 0.01448(17) 0.00123(14) 0.00284(13) -0.00184(14) S2 0.01464(16) 0.02064(18) 0.01538(17) -0.00125(13) 0.00229(13) -0.00372(13) P1 0.02318(19) 0.01726(18) 0.01462(18) -0.00143(14) 0.00191(14) 0.00393(15) P2 0.02032(19) 0.0239(2) 0.0222(2) -0.00327(16) 0.00002(16) -0.00546(16) O1 0.0144(5) 0.0239(6) 0.0355(7) -0.0039(5) 0.0065(5) -0.0042(4) O2 0.0232(5) 0.0230(6) 0.0151(5) 0.0041(4) 0.0040(4) -0.0024(4) C10 0.0142(6) 0.0155(7) 0.0154(7) -0.0002(5) 0.0034(5) 0.0002(5) C1 0.0150(6) 0.0162(7) 0.0157(7) -0.0020(5) 0.0021(5) 0.0006(5) C2 0.0139(6) 0.0158(7) 0.0152(7) -0.0022(5) 0.0018(5) -0.0003(5) C3 0.0148(6) 0.0176(7) 0.0136(6) 0.0004(5) 0.0045(5) -0.0008(5) C4 0.0185(7) 0.0166(7) 0.0196(7) 0.0000(6) 0.0045(6) 0.0000(6) C5 0.0161(7) 0.0211(7) 0.0209(7) 0.0011(6) 0.0048(6) 0.0024(6) C6 0.0155(7) 0.0229(8) 0.0197(7) -0.0009(6) 0.0063(6) -0.0034(6) C7 0.0191(7) 0.0158(7) 0.0263(8) -0.0014(6) 0.0091(6) -0.0021(6) C8 0.0160(7) 0.0178(7) 0.0211(7) 0.0019(6) 0.0068(6) 0.0013(5) C9 0.0151(7) 0.0324(9) 0.0306(9) 0.0003(7) 0.0041(6) -0.0021(6) C11 0.0175(7) 0.0166(7) 0.0173(7) -0.0001(5) 0.0044(5) -0.0029(5) C12 0.0180(7) 0.0189(7) 0.0169(7) -0.0021(6) 0.0031(5) -0.0047(6) C13 0.0165(6) 0.0180(7) 0.0153(7) 0.0026(5) 0.0042(5) 0.0021(5) C14 0.0252(8) 0.0158(7) 0.0218(8) 0.0026(6) 0.0060(6) -0.0038(6) C15 0.0229(7) 0.0180(7) 0.0185(7) -0.0020(6) 0.0028(6) -0.0064(6) C16 0.0333(9) 0.0299(9) 0.0216(8) 0.0089(7) 0.0053(7) -0.0051(7) C17 0.0364(9) 0.0192(8) 0.0175(7) 0.0009(6) 0.0055(7) 0.0013(7) C18 0.0418(10) 0.0207(8) 0.0254(9) -0.0019(7) 0.0141(8) 0.0054(7) C19 0.0296(9) 0.0322(9) 0.0233(8) 0.0035(7) -0.0032(7) 0.0070(7) C20 0.0379(10) 0.0273(9) 0.0380(11) -0.0116(8) 0.0003(8) -0.0070(8) C21 0.0189(8) 0.0400(11) 0.0447(12) -0.0045(9) 0.0063(8) -0.0010(7) C22 0.0325(10) 0.0452(12) 0.0338(10) 0.0069(9) -0.0007(8) -0.0209(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 S2 2.2895(4) . ? Pd1 S1 2.2940(4) . ? Pd1 P2 2.3020(4) . ? Pd1 P1 2.3087(4) . ? S1 C1 1.7543(15) . ? S2 C2 1.7711(15) . ? P1 C17 1.8112(18) . ? P1 C18 1.8160(18) . ? P1 C19 1.8214(17) . ? P2 C20 1.8176(19) . ? P2 C22 1.818(2) . ? P2 C21 1.8179(19) . ? O1 C6 1.3710(18) . ? O1 C9 1.433(2) . ? O2 C13 1.3719(18) . ? O2 C16 1.426(2) . ? C10 C15 1.396(2) . ? C10 C11 1.406(2) . ? C10 C2 1.490(2) . ? C1 C2 1.353(2) . ? C1 C3 1.489(2) . ? C3 C4 1.390(2) . ? C3 C8 1.401(2) . ? C4 C5 1.397(2) . ? C4 H4 0.9500 . ? C5 C6 1.390(2) . ? C5 H5 0.9500 . ? C6 C7 1.392(2) . ? C7 C8 1.383(2) . ? C7 H7 0.9500 . ? C8 H8 0.9500 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C11 C12 1.386(2) . ? C11 H11 0.9500 . ? C12 C13 1.395(2) . ? C12 H12 0.9500 . ? C13 C14 1.386(2) . ? C14 C15 1.395(2) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S2 Pd1 S1 87.124(13) . . ? S2 Pd1 P2 88.824(15) . . ? S1 Pd1 P2 174.796(15) . . ? S2 Pd1 P1 174.565(15) . . ? S1 Pd1 P1 87.781(15) . . ? P2 Pd1 P1 96.368(16) . . ? C1 S1 Pd1 105.28(5) . . ? C2 S2 Pd1 105.96(5) . . ? C17 P1 C18 103.21(9) . . ? C17 P1 C19 100.80(9) . . ? C18 P1 C19 102.77(9) . . ? C17 P1 Pd1 113.90(5) . . ? C18 P1 Pd1 113.38(6) . . ? C19 P1 Pd1 120.58(7) . . ? C20 P2 C22 100.85(10) . . ? C20 P2 C21 104.56(10) . . ? C22 P2 C21 101.24(11) . . ? C20 P2 Pd1 114.68(7) . . ? C22 P2 Pd1 115.77(6) . . ? C21 P2 Pd1 117.50(7) . . ? C6 O1 C9 116.46(13) . . ? C13 O2 C16 116.22(13) . . ? C15 C10 C11 116.49(14) . . ? C15 C10 C2 120.05(13) . . ? C11 C10 C2 123.38(13) . . ? C2 C1 C3 125.05(13) . . ? C2 C1 S1 122.08(11) . . ? C3 C1 S1 112.87(11) . . ? C1 C2 C10 126.17(13) . . ? C1 C2 S2 119.54(11) . . ? C10 C2 S2 114.29(11) . . ? C4 C3 C8 118.12(13) . . ? C4 C3 C1 121.23(13) . . ? C8 C3 C1 120.64(13) . . ? C3 C4 C5 121.75(14) . . ? C3 C4 H4 119.1 . . ? C5 C4 H4 119.1 . . ? C6 C5 C4 118.96(14) . . ? C6 C5 H5 120.5 . . ? C4 C5 H5 120.5 . . ? O1 C6 C5 124.26(14) . . ? O1 C6 C7 115.67(14) . . ? C5 C6 C7 120.06(14) . . ? C8 C7 C6 120.31(14) . . ? C8 C7 H7 119.8 . . ? C6 C7 H7 119.8 . . ? C7 C8 C3 120.72(14) . . ? C7 C8 H8 119.6 . . ? C3 C8 H8 119.6 . . ? O1 C9 H9A 109.5 . . ? O1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? O1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C12 C11 C10 121.26(14) . . ? C12 C11 H11 119.4 . . ? C10 C11 H11 119.4 . . ? C11 C12 C13 120.81(14) . . ? C11 C12 H12 119.6 . . ? C13 C12 H12 119.6 . . ? O2 C13 C14 124.85(14) . . ? O2 C13 C12 115.85(13) . . ? C14 C13 C12 119.31(14) . . ? C13 C14 C15 119.12(14) . . ? C13 C14 H14 120.4 . . ? C15 C14 H14 120.4 . . ? C14 C15 C10 123.00(14) . . ? C14 C15 H15 118.5 . . ? C10 C15 H15 118.5 . . ? O2 C16 H16A 109.5 . . ? O2 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? O2 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? P1 C17 H17A 109.5 . . ? P1 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? P1 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? P1 C18 H18A 109.5 . . ? P1 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? P1 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? P1 C19 H19A 109.5 . . ? P1 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? P1 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? P2 C20 H20A 109.5 . . ? P2 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? P2 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? P2 C21 H21A 109.5 . . ? P2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? P2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? P2 C22 H22A 109.5 . . ? P2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? P2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 28.71 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.466 _refine_diff_density_min -0.453 _refine_diff_density_rms 0.070 #===END # [Pd(S2C2Me2)(PPh3)2], Compound 12 data_jpd167_0m _audit_creation_method SHELXL-97 _chemical_name_systematic ; (2,3-cis-but-2-enedithiolato-\k^2^S,S')bis(triphenyl phosphine)palladium(II) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H36 P2 Pd S2' _chemical_formula_weight 749.15 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M Pn _symmetry_space_group_name_Hall 'P -2yac' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y, z+1/2' _cell_length_a 9.0024(4) _cell_length_b 10.9590(4) _cell_length_c 17.4224(7) _cell_angle_alpha 90.00 _cell_angle_beta 99.862(1) _cell_angle_gamma 90.00 _cell_volume 1693.5(1) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9283 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 29.45 _exptl_crystal_description Block _exptl_crystal_colour blue _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.469 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 768 _exptl_absorpt_coefficient_mu 0.794 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8382 _exptl_absorpt_correction_T_max 0.9051 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2007)' _exptl_special_details ; The diffraction data were obtained from 3 sets of 400 frames, each of width 0.5 deg. in omega, collected at phi = 0.00, 90.00 and 180.00 deg. and 2 sets of 800 frames, each of width 0.45 deg in phi, collected at omega = -30.00 and 210.00 deg. The scan time was 15 sec/frame. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-AXS Smart APEX CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29561 _diffrn_reflns_av_R_equivalents 0.0264 _diffrn_reflns_av_sigmaI/netI 0.0267 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 28.84 _reflns_number_total 8645 _reflns_number_gt 8567 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker APEX2 (Bruker-AXS, 2007)' _computing_cell_refinement 'Bruker APEX2 (Bruker-AXS, 2007)' _computing_data_reduction 'Bruker SAINT+ (Bruker-AXS, 2006)' _computing_structure_solution 'XM (Sheldrick, 2004)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker APEX2 (Bruker-AXS, 2007)' _computing_publication_material 'Bruker APEX2 (Bruker-AXS, 2007)' _publ_section_references ; Bruker-AXS (2007). APEX2, Version 2.1-4, Madison, WI. Bruker-AXS (2006). SAINT+, Version 7.34A, Madison, WI Sheldrick, G. M. (1997). SHELXL-97. University of G\"ottingen, Germany. Sheldrick, G, M. (2004). XM, Version 2004/1. University of G\"ottingen, Germany. Sheldrick, G, M. (2007). SADABS, Version 2007/4. University of G\"ottingen, Germany. ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. H-atoms were placed in calculated positions (C---H = 0.95 - 0.98 \%A) and included as riding contributions with isotropic displacement parameters 1.2 - 1.5 times those of the attached carbon atoms. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0222P)^2^+0.1039P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.003(9) _refine_ls_number_reflns 8645 _refine_ls_number_parameters 408 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0171 _refine_ls_R_factor_gt 0.0169 _refine_ls_wR_factor_ref 0.0447 _refine_ls_wR_factor_gt 0.0446 _refine_ls_goodness_of_fit_ref 1.131 _refine_ls_restrained_S_all 1.131 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.353659(9) 0.205496(8) 0.685160(7) 0.00912(3) Uani 1 1 d . . . S1 S 0.37361(4) 0.11641(3) 0.56916(2) 0.01285(7) Uani 1 1 d . . . S2 S 0.49645(4) 0.36386(3) 0.64985(2) 0.01296(7) Uani 1 1 d . . . P1 P 0.25504(4) 0.02615(3) 0.72324(2) 0.00978(7) Uani 1 1 d . . . P2 P 0.28795(4) 0.32998(4) 0.78230(2) 0.01093(7) Uani 1 1 d . . . C1 C 0.45858(18) 0.22827(16) 0.51808(9) 0.0139(3) Uani 1 1 d . . . C2 C 0.51403(18) 0.33120(15) 0.55270(9) 0.0139(3) Uani 1 1 d . . . C3 C 0.4524(2) 0.19571(16) 0.43344(10) 0.0198(3) Uani 1 1 d . . . H3A H 0.3526 0.2161 0.4041 0.030 Uiso 1 1 calc R . . H3B H 0.4707 0.1081 0.4288 0.030 Uiso 1 1 calc R . . H3C H 0.5297 0.2418 0.4124 0.030 Uiso 1 1 calc R . . C4 C 0.5980(2) 0.42772(16) 0.51467(10) 0.0206(3) Uani 1 1 d . . . H4A H 0.6356 0.3920 0.4701 0.031 Uiso 1 1 calc R . . H4B H 0.6831 0.4581 0.5526 0.031 Uiso 1 1 calc R . . H4C H 0.5296 0.4954 0.4968 0.031 Uiso 1 1 calc R . . C5 C 0.29714(17) -0.11461(13) 0.67444(8) 0.0116(3) Uani 1 1 d . . . C6 C 0.4062(2) -0.19782(14) 0.70812(10) 0.0159(3) Uani 1 1 d . . . H6 H 0.4641 -0.1815 0.7580 0.019 Uiso 1 1 calc R . . C7 C 0.4305(2) -0.30495(15) 0.66885(10) 0.0189(3) Uani 1 1 d . . . H7 H 0.5043 -0.3618 0.6922 0.023 Uiso 1 1 calc R . . C8 C 0.3471(2) -0.32884(15) 0.59562(10) 0.0183(3) Uani 1 1 d . . . H8 H 0.3639 -0.4018 0.5690 0.022 Uiso 1 1 calc R . . C9 C 0.23937(19) -0.24580(15) 0.56155(9) 0.0172(3) Uani 1 1 d . . . H9 H 0.1832 -0.2616 0.5112 0.021 Uiso 1 1 calc R . . C10 C 0.21335(18) -0.13974(14) 0.60070(9) 0.0146(3) Uani 1 1 d . . . H10 H 0.1383 -0.0839 0.5774 0.018 Uiso 1 1 calc R . . C11 C 0.05051(17) 0.01715(14) 0.71138(8) 0.0118(3) Uani 1 1 d . . . C12 C -0.03656(19) 0.11737(15) 0.68147(9) 0.0147(3) Uani 1 1 d . . . H12 H 0.0118 0.1903 0.6695 0.018 Uiso 1 1 calc R . . C13 C -0.19310(19) 0.11175(15) 0.66900(9) 0.0174(3) Uani 1 1 d . . . H13 H -0.2513 0.1805 0.6489 0.021 Uiso 1 1 calc R . . C14 C -0.26409(18) 0.00466(17) 0.68616(9) 0.0190(3) Uani 1 1 d . . . H14 H -0.3711 0.0007 0.6780 0.023 Uiso 1 1 calc R . . C15 C -0.17964(18) -0.09632(15) 0.71516(9) 0.0171(3) Uani 1 1 d . . . H15 H -0.2287 -0.1689 0.7271 0.020 Uiso 1 1 calc R . . C16 C -0.02260(17) -0.09100(14) 0.72669(9) 0.0143(3) Uani 1 1 d . . . H16 H 0.0352 -0.1609 0.7450 0.017 Uiso 1 1 calc R . . C17 C 0.33690(17) -0.00701(13) 0.82382(8) 0.0116(3) Uani 1 1 d . . . C18 C 0.49168(18) 0.01571(14) 0.84646(9) 0.0149(3) Uani 1 1 d . . . H18 H 0.5464 0.0560 0.8118 0.018 Uiso 1 1 calc R . . C19 C 0.56484(18) -0.02091(15) 0.91979(9) 0.0167(3) Uani 1 1 d . . . H19 H 0.6701 -0.0077 0.9347 0.020 Uiso 1 1 calc R . . C20 C 0.48385(19) -0.07678(15) 0.97132(9) 0.0172(3) Uani 1 1 d . . . H20 H 0.5343 -0.1027 1.0210 0.021 Uiso 1 1 calc R . . C21 C 0.33068(19) -0.09463(15) 0.95042(9) 0.0179(3) Uani 1 1 d . . . H21 H 0.2751 -0.1299 0.9865 0.021 Uiso 1 1 calc R . . C22 C 0.25724(18) -0.06086(15) 0.87636(9) 0.0157(3) Uani 1 1 d . . . H22 H 0.1520 -0.0748 0.8618 0.019 Uiso 1 1 calc R . . C23 C 0.13632(17) 0.43256(14) 0.73881(8) 0.0132(3) Uani 1 1 d . . . C24 C 0.10795(18) 0.44945(15) 0.65809(9) 0.0157(3) Uani 1 1 d . . . H24 H 0.1693 0.4094 0.6266 0.019 Uiso 1 1 calc R . . C25 C -0.00982(19) 0.52471(16) 0.62335(10) 0.0196(3) Uani 1 1 d . . . H25 H -0.0274 0.5365 0.5685 0.024 Uiso 1 1 calc R . . C26 C -0.1011(2) 0.58223(16) 0.66870(10) 0.0208(3) Uani 1 1 d . . . H26 H -0.1824 0.6322 0.6450 0.025 Uiso 1 1 calc R . . C27 C -0.0732(2) 0.56648(16) 0.74914(10) 0.0208(3) Uani 1 1 d . . . H27 H -0.1348 0.6067 0.7804 0.025 Uiso 1 1 calc R . . C28 C 0.04371(19) 0.49269(15) 0.78386(9) 0.0178(3) Uani 1 1 d . . . H28 H 0.0616 0.4825 0.8388 0.021 Uiso 1 1 calc R . . C29 C 0.44139(18) 0.42639(14) 0.83085(8) 0.0143(3) Uani 1 1 d . . . C30 C 0.4156(2) 0.54105(16) 0.86086(11) 0.0218(3) Uani 1 1 d . . . H30 H 0.3177 0.5762 0.8503 0.026 Uiso 1 1 calc R . . C31 C 0.5335(2) 0.60387(17) 0.90629(12) 0.0280(4) Uani 1 1 d . . . H31 H 0.5156 0.6819 0.9266 0.034 Uiso 1 1 calc R . . C32 C 0.6769(2) 0.55334(16) 0.92216(10) 0.0238(4) Uani 1 1 d . . . H32 H 0.7563 0.5958 0.9543 0.029 Uiso 1 1 calc R . . C33 C 0.70387(19) 0.44110(16) 0.89110(10) 0.0208(3) Uani 1 1 d . . . H33 H 0.8023 0.4069 0.9012 0.025 Uiso 1 1 calc R . . C34 C 0.58711(18) 0.37786(15) 0.84492(9) 0.0166(3) Uani 1 1 d . . . H34 H 0.6067 0.3014 0.8229 0.020 Uiso 1 1 calc R . . C35 C 0.21543(19) 0.26668(15) 0.86640(9) 0.0137(3) Uani 1 1 d . . . C36 C 0.31210(19) 0.24819(15) 0.93722(9) 0.0159(3) Uani 1 1 d . . . H36 H 0.4150 0.2716 0.9424 0.019 Uiso 1 1 calc R . . C37 C 0.2589(2) 0.19559(15) 1.00059(10) 0.0199(3) Uani 1 1 d . . . H37 H 0.3258 0.1830 1.0484 0.024 Uiso 1 1 calc R . . C38 C 0.1086(2) 0.16177(16) 0.99365(10) 0.0214(3) Uani 1 1 d . . . H38 H 0.0723 0.1263 1.0366 0.026 Uiso 1 1 calc R . . C39 C 0.0114(2) 0.18004(16) 0.92341(10) 0.0200(3) Uani 1 1 d . . . H39 H -0.0915 0.1569 0.9185 0.024 Uiso 1 1 calc R . . C40 C 0.06407(19) 0.23221(15) 0.86007(9) 0.0154(3) Uani 1 1 d . . . H40 H -0.0032 0.2444 0.8124 0.019 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.01008(5) 0.00898(5) 0.00841(4) -0.00015(4) 0.00186(3) 0.00023(4) S1 0.01416(17) 0.01422(17) 0.01044(15) -0.00203(13) 0.00287(13) -0.00053(13) S2 0.01482(17) 0.01160(16) 0.01303(15) -0.00008(13) 0.00400(13) -0.00146(13) P1 0.00987(16) 0.00972(16) 0.00956(15) 0.00018(13) 0.00115(13) 0.00051(13) P2 0.01280(18) 0.01057(17) 0.00945(16) -0.00069(13) 0.00196(13) 0.00022(14) C1 0.0121(7) 0.0205(8) 0.0093(7) 0.0016(6) 0.0023(6) 0.0040(6) C2 0.0133(7) 0.0172(7) 0.0118(6) 0.0032(6) 0.0041(5) 0.0044(6) C3 0.0224(9) 0.0248(9) 0.0135(8) -0.0011(6) 0.0068(7) 0.0044(7) C4 0.0216(8) 0.0223(8) 0.0191(7) 0.0036(6) 0.0069(6) -0.0032(7) C5 0.0126(6) 0.0094(6) 0.0133(6) 0.0002(5) 0.0038(5) -0.0019(5) C6 0.0160(7) 0.0155(8) 0.0157(7) -0.0006(5) 0.0014(6) 0.0021(6) C7 0.0198(9) 0.0152(8) 0.0215(8) 0.0011(6) 0.0028(7) 0.0048(6) C8 0.0221(8) 0.0131(7) 0.0210(8) -0.0044(6) 0.0075(6) -0.0004(6) C9 0.0200(8) 0.0161(8) 0.0152(7) -0.0033(6) 0.0020(6) -0.0025(6) C10 0.0157(7) 0.0137(7) 0.0139(7) 0.0007(5) 0.0012(6) 0.0012(6) C11 0.0101(7) 0.0147(7) 0.0107(6) -0.0019(5) 0.0019(5) 0.0018(5) C12 0.0170(8) 0.0152(7) 0.0117(6) 0.0001(5) 0.0019(6) 0.0023(6) C13 0.0148(7) 0.0210(8) 0.0161(7) 0.0005(6) 0.0015(6) 0.0076(6) C14 0.0114(7) 0.0302(9) 0.0151(7) -0.0030(6) 0.0016(6) 0.0027(7) C15 0.0136(7) 0.0195(8) 0.0182(7) -0.0020(6) 0.0032(6) -0.0027(6) C16 0.0127(7) 0.0142(7) 0.0152(7) 0.0005(5) 0.0001(6) 0.0005(5) C17 0.0133(7) 0.0105(6) 0.0105(6) -0.0012(5) 0.0004(5) 0.0017(5) C18 0.0138(7) 0.0157(7) 0.0149(7) -0.0013(5) 0.0015(6) -0.0006(6) C19 0.0139(7) 0.0178(8) 0.0172(7) -0.0015(6) -0.0004(6) 0.0005(6) C20 0.0216(8) 0.0155(7) 0.0126(6) 0.0007(6) -0.0018(6) 0.0018(6) C21 0.0202(8) 0.0208(8) 0.0125(7) 0.0033(6) 0.0026(6) -0.0029(6) C22 0.0140(7) 0.0177(7) 0.0150(7) 0.0002(6) 0.0015(6) -0.0015(6) C23 0.0146(7) 0.0108(7) 0.0140(7) -0.0001(5) 0.0017(6) 0.0000(5) C24 0.0152(7) 0.0172(7) 0.0151(7) 0.0018(6) 0.0037(6) 0.0006(6) C25 0.0199(8) 0.0215(8) 0.0165(7) 0.0042(6) 0.0002(6) 0.0011(6) C26 0.0174(7) 0.0185(8) 0.0255(8) 0.0040(6) 0.0002(6) 0.0044(6) C27 0.0216(8) 0.0185(8) 0.0234(8) -0.0016(6) 0.0069(7) 0.0053(7) C28 0.0216(8) 0.0161(7) 0.0161(7) -0.0006(6) 0.0046(6) 0.0021(6) C29 0.0165(7) 0.0147(7) 0.0114(6) -0.0002(5) 0.0016(6) -0.0033(6) C30 0.0212(8) 0.0169(8) 0.0260(8) -0.0047(6) 0.0006(7) 0.0014(7) C31 0.0326(10) 0.0179(8) 0.0318(9) -0.0101(7) 0.0005(8) -0.0049(7) C32 0.0254(9) 0.0232(9) 0.0212(8) -0.0022(7) -0.0011(7) -0.0110(7) C33 0.0173(8) 0.0237(9) 0.0206(8) 0.0023(6) 0.0006(6) -0.0037(7) C34 0.0175(8) 0.0165(7) 0.0155(7) -0.0004(6) 0.0021(6) -0.0016(6) C35 0.0184(8) 0.0109(7) 0.0131(7) -0.0026(6) 0.0062(6) 0.0010(6) C36 0.0185(8) 0.0153(8) 0.0142(7) -0.0009(6) 0.0039(6) 0.0004(6) C37 0.0285(9) 0.0198(8) 0.0119(7) 0.0012(6) 0.0045(7) 0.0020(6) C38 0.0298(9) 0.0199(8) 0.0175(7) 0.0031(6) 0.0129(7) 0.0024(7) C39 0.0216(8) 0.0192(8) 0.0220(8) -0.0003(6) 0.0116(7) 0.0014(7) C40 0.0166(8) 0.0150(7) 0.0150(7) -0.0014(6) 0.0034(6) 0.0010(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 S1 2.2791(4) . ? Pd1 P1 2.3007(4) . ? Pd1 S2 2.3052(4) . ? Pd1 P2 2.3277(4) . ? S1 C1 1.7644(17) . ? S2 C2 1.7634(16) . ? P1 C17 1.8175(15) . ? P1 C11 1.8200(16) . ? P1 C5 1.8320(15) . ? P2 C29 1.8275(16) . ? P2 C23 1.8295(16) . ? P2 C35 1.8391(16) . ? C1 C2 1.335(2) . ? C1 C3 1.509(2) . ? C2 C4 1.517(2) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C6 1.394(2) . ? C5 C10 1.401(2) . ? C6 C7 1.395(2) . ? C6 H6 0.9500 . ? C7 C8 1.390(2) . ? C7 H7 0.9500 . ? C8 C9 1.387(2) . ? C8 H8 0.9500 . ? C9 C10 1.388(2) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C12 1.397(2) . ? C11 C16 1.403(2) . ? C12 C13 1.390(2) . ? C12 H12 0.9500 . ? C13 C14 1.393(3) . ? C13 H13 0.9500 . ? C14 C15 1.388(2) . ? C14 H14 0.9500 . ? C15 C16 1.395(2) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 C22 1.388(2) . ? C17 C18 1.404(2) . ? C18 C19 1.392(2) . ? C18 H18 0.9500 . ? C19 C20 1.392(2) . ? C19 H19 0.9500 . ? C20 C21 1.378(2) . ? C20 H20 0.9500 . ? C21 C22 1.395(2) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 C24 1.398(2) . ? C23 C28 1.403(2) . ? C24 C25 1.397(2) . ? C24 H24 0.9500 . ? C25 C26 1.386(2) . ? C25 H25 0.9500 . ? C26 C27 1.392(2) . ? C26 H26 0.9500 . ? C27 C28 1.382(2) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 C30 1.396(2) . ? C29 C34 1.398(2) . ? C30 C31 1.392(3) . ? C30 H30 0.9500 . ? C31 C32 1.389(3) . ? C31 H31 0.9500 . ? C32 C33 1.382(3) . ? C32 H32 0.9500 . ? C33 C34 1.394(2) . ? C33 H33 0.9500 . ? C34 H34 0.9500 . ? C35 C36 1.398(2) . ? C35 C40 1.400(2) . ? C36 C37 1.400(2) . ? C36 H36 0.9500 . ? C37 C38 1.388(3) . ? C37 H37 0.9500 . ? C38 C39 1.392(3) . ? C38 H38 0.9500 . ? C39 C40 1.396(2) . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S1 Pd1 P1 89.007(13) . . ? S1 Pd1 S2 87.341(14) . . ? P1 Pd1 S2 168.669(14) . . ? S1 Pd1 P2 164.633(14) . . ? P1 Pd1 P2 97.605(14) . . ? S2 Pd1 P2 88.601(14) . . ? C1 S1 Pd1 104.86(6) . . ? C2 S2 Pd1 104.43(6) . . ? C17 P1 C11 109.50(7) . . ? C17 P1 C5 101.37(7) . . ? C11 P1 C5 100.80(7) . . ? C17 P1 Pd1 109.64(5) . . ? C11 P1 Pd1 116.52(5) . . ? C5 P1 Pd1 117.70(5) . . ? C29 P2 C23 106.72(7) . . ? C29 P2 C35 101.11(7) . . ? C23 P2 C35 102.73(7) . . ? C29 P2 Pd1 114.16(5) . . ? C23 P2 Pd1 108.87(5) . . ? C35 P2 Pd1 121.82(5) . . ? C2 C1 C3 126.14(15) . . ? C2 C1 S1 121.33(12) . . ? C3 C1 S1 112.46(12) . . ? C1 C2 C4 124.58(14) . . ? C1 C2 S2 121.13(12) . . ? C4 C2 S2 114.28(12) . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C6 C5 C10 119.15(14) . . ? C6 C5 P1 122.84(12) . . ? C10 C5 P1 117.99(12) . . ? C5 C6 C7 120.18(16) . . ? C5 C6 H6 119.9 . . ? C7 C6 H6 119.9 . . ? C8 C7 C6 120.22(16) . . ? C8 C7 H7 119.9 . . ? C6 C7 H7 119.9 . . ? C9 C8 C7 119.83(15) . . ? C9 C8 H8 120.1 . . ? C7 C8 H8 120.1 . . ? C8 C9 C10 120.24(15) . . ? C8 C9 H9 119.9 . . ? C10 C9 H9 119.9 . . ? C9 C10 C5 120.37(14) . . ? C9 C10 H10 119.8 . . ? C5 C10 H10 119.8 . . ? C12 C11 C16 118.90(14) . . ? C12 C11 P1 119.45(12) . . ? C16 C11 P1 121.50(11) . . ? C13 C12 C11 120.83(15) . . ? C13 C12 H12 119.6 . . ? C11 C12 H12 119.6 . . ? C12 C13 C14 119.59(15) . . ? C12 C13 H13 120.2 . . ? C14 C13 H13 120.2 . . ? C15 C14 C13 120.47(15) . . ? C15 C14 H14 119.8 . . ? C13 C14 H14 119.8 . . ? C14 C15 C16 119.85(15) . . ? C14 C15 H15 120.1 . . ? C16 C15 H15 120.1 . . ? C15 C16 C11 120.32(14) . . ? C15 C16 H16 119.8 . . ? C11 C16 H16 119.8 . . ? C22 C17 C18 119.36(13) . . ? C22 C17 P1 123.44(12) . . ? C18 C17 P1 117.03(11) . . ? C19 C18 C17 119.83(14) . . ? C19 C18 H18 120.1 . . ? C17 C18 H18 120.1 . . ? C20 C19 C18 120.07(15) . . ? C20 C19 H19 120.0 . . ? C18 C19 H19 120.0 . . ? C21 C20 C19 120.18(14) . . ? C21 C20 H20 119.9 . . ? C19 C20 H20 119.9 . . ? C20 C21 C22 120.06(15) . . ? C20 C21 H21 120.0 . . ? C22 C21 H21 120.0 . . ? C17 C22 C21 120.42(15) . . ? C17 C22 H22 119.8 . . ? C21 C22 H22 119.8 . . ? C24 C23 C28 118.48(14) . . ? C24 C23 P2 119.53(12) . . ? C28 C23 P2 121.96(11) . . ? C25 C24 C23 120.56(15) . . ? C25 C24 H24 119.7 . . ? C23 C24 H24 119.7 . . ? C26 C25 C24 120.13(15) . . ? C26 C25 H25 119.9 . . ? C24 C25 H25 119.9 . . ? C25 C26 C27 119.68(16) . . ? C25 C26 H26 120.2 . . ? C27 C26 H26 120.2 . . ? C28 C27 C26 120.43(15) . . ? C28 C27 H27 119.8 . . ? C26 C27 H27 119.8 . . ? C27 C28 C23 120.71(15) . . ? C27 C28 H28 119.6 . . ? C23 C28 H28 119.6 . . ? C30 C29 C34 119.23(15) . . ? C30 C29 P2 122.20(13) . . ? C34 C29 P2 118.26(12) . . ? C31 C30 C29 119.90(17) . . ? C31 C30 H30 120.1 . . ? C29 C30 H30 120.1 . . ? C32 C31 C30 120.55(17) . . ? C32 C31 H31 119.7 . . ? C30 C31 H31 119.7 . . ? C33 C32 C31 119.77(16) . . ? C33 C32 H32 120.1 . . ? C31 C32 H32 120.1 . . ? C32 C33 C34 120.20(17) . . ? C32 C33 H33 119.9 . . ? C34 C33 H33 119.9 . . ? C33 C34 C29 120.29(15) . . ? C33 C34 H34 119.9 . . ? C29 C34 H34 119.9 . . ? C36 C35 C40 118.75(14) . . ? C36 C35 P2 120.38(13) . . ? C40 C35 P2 120.84(12) . . ? C35 C36 C37 120.69(16) . . ? C35 C36 H36 119.7 . . ? C37 C36 H36 119.7 . . ? C38 C37 C36 120.07(16) . . ? C38 C37 H37 120.0 . . ? C36 C37 H37 120.0 . . ? C37 C38 C39 119.67(16) . . ? C37 C38 H38 120.2 . . ? C39 C38 H38 120.2 . . ? C38 C39 C40 120.43(17) . . ? C38 C39 H39 119.8 . . ? C40 C39 H39 119.8 . . ? C39 C40 C35 120.39(15) . . ? C39 C40 H40 119.8 . . ? C35 C40 H40 119.8 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 28.84 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.259 _refine_diff_density_min -0.425 _refine_diff_density_rms 0.087 #===END # [Pd2(mu-S2C2Me2)2(PPh3)2], Compound 13 data_jpd165_0m _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C44 H42 P2 Pd2 S4' _chemical_formula_sum 'C44 H42 P2 Pd2 S4' _chemical_formula_weight 973.76 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.8658(3) _cell_length_b 10.4704(3) _cell_length_c 21.2026(7) _cell_angle_alpha 85.8090(10) _cell_angle_beta 83.2370(10) _cell_angle_gamma 68.4700(10) _cell_volume 2022.15(11) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9149 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 29.52 _exptl_crystal_description Block _exptl_crystal_colour red _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.599 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 984 _exptl_absorpt_coefficient_mu 1.207 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8091 _exptl_absorpt_correction_T_max 0.8848 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2007)' _exptl_special_details ; The diffraction data were obtained from 3 sets of 400 frames, each of width 0.5 deg. in \w, collected at \f = 0.00, 90.00 and 180.00 deg. and 2 sets of 800 frames, each of width 0.45 deg in \f, collected at \w = -30.00 and 210.00 deg. The scan time was 15 sec/frame. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-AXS Smart APEX CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36097 _diffrn_reflns_av_R_equivalents 0.0291 _diffrn_reflns_av_sigmaI/netI 0.0257 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 28.50 _reflns_number_total 10091 _reflns_number_gt 9312 _reflns_threshold_expression >2\s(I) _computing_cell_refinement 'Bruker APEX2 (Bruker-AXS, 2007)' _computing_data_reduction 'Bruker SAINT+ (Bruker-AXS, 2006)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker APEX2 (Bruker-AXS, 2007)' _computing_publication_material 'Bruker APEX2 (Bruker-AXS, 2007)' _publ_section_references ; Bruker-AXS (2007). APEX2, Version 2.1-4, Madison, WI. Bruker-AXS (2006). SAINT+, Version 7.34A, Madison, WI Sheldrick, G. M. (1997). SHELXS-97 and SHELXL-97. University of G\"ottingen, Germany. Sheldrick, G, M. (2007). SADABS, Version 2007/4. University of G\"ottingen, Germany. ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. H-atoms were placed in calculated positions (C---H = 0.95 - 0.98 \%A) and included as riding contributions with isotropic displacement parameters 1.2 - 1.5 times those of the attached carbon atoms. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0190P)^2^+1.3450P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10091 _refine_ls_number_parameters 472 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0234 _refine_ls_R_factor_gt 0.0208 _refine_ls_wR_factor_ref 0.0524 _refine_ls_wR_factor_gt 0.0509 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.261898(12) 0.219934(12) 0.268438(5) 0.01112(3) Uani 1 1 d . . . Pd2 Pd 0.428682(13) 0.298099(12) 0.156544(5) 0.01135(3) Uani 1 1 d . . . S1 S 0.39138(4) 0.02897(4) 0.325513(19) 0.01451(8) Uani 1 1 d . . . S2 S 0.37169(4) 0.09664(4) 0.177852(18) 0.01376(8) Uani 1 1 d . . . S3 S 0.43173(4) 0.51501(4) 0.14983(2) 0.01684(8) Uani 1 1 d . . . S4 S 0.17939(4) 0.39169(4) 0.186321(18) 0.01419(8) Uani 1 1 d . . . P1 P 0.14803(4) 0.33830(4) 0.358030(19) 0.01254(8) Uani 1 1 d . . . P2 P 0.67637(4) 0.21346(4) 0.130726(19) 0.01199(8) Uani 1 1 d . . . C1 C 0.50682(18) -0.08439(16) 0.26775(8) 0.0159(3) Uani 1 1 d . . . C2 C 0.50403(18) -0.05794(16) 0.20487(8) 0.0157(3) Uani 1 1 d . . . C3 C 0.25155(19) 0.61763(17) 0.17622(8) 0.0174(3) Uani 1 1 d . . . C4 C 0.14513(18) 0.56806(16) 0.19579(8) 0.0164(3) Uani 1 1 d . . . C5 C 0.6135(2) -0.21392(17) 0.29590(9) 0.0223(4) Uani 1 1 d . . . H5A H 0.6431 -0.2875 0.2654 0.034 Uiso 1 1 calc R . . H5B H 0.5665 -0.2414 0.3351 0.034 Uiso 1 1 calc R . . H5C H 0.7000 -0.1968 0.3055 0.034 Uiso 1 1 calc R . . C6 C 0.5963(2) -0.15643(17) 0.15435(9) 0.0209(3) Uani 1 1 d . . . H6A H 0.7002 -0.1795 0.1593 0.031 Uiso 1 1 calc R . . H6B H 0.5752 -0.1133 0.1122 0.031 Uiso 1 1 calc R . . H6C H 0.5734 -0.2403 0.1587 0.031 Uiso 1 1 calc R . . C7 C 0.2286(2) 0.76811(18) 0.17427(10) 0.0258(4) Uani 1 1 d . . . H7A H 0.1292 0.8202 0.1928 0.039 Uiso 1 1 calc R . . H7B H 0.2416 0.7996 0.1301 0.039 Uiso 1 1 calc R . . H7C H 0.2999 0.7824 0.1987 0.039 Uiso 1 1 calc R . . C8 C -0.00789(19) 0.65378(18) 0.22184(9) 0.0225(4) Uani 1 1 d . . . H8A H -0.0089 0.6686 0.2670 0.034 Uiso 1 1 calc R . . H8B H -0.0744 0.6058 0.2168 0.034 Uiso 1 1 calc R . . H8C H -0.0399 0.7426 0.1986 0.034 Uiso 1 1 calc R . . C9 C -0.04796(18) 0.37054(16) 0.37070(8) 0.0150(3) Uani 1 1 d . . . C10 C -0.12754(18) 0.39175(16) 0.31809(8) 0.0164(3) Uani 1 1 d . . . H10 H -0.0791 0.3886 0.2764 0.020 Uiso 1 1 calc R . . C11 C -0.27674(19) 0.41745(17) 0.32625(9) 0.0205(3) Uani 1 1 d . . . H11 H -0.3305 0.4339 0.2903 0.025 Uiso 1 1 calc R . . C12 C -0.3475(2) 0.41916(19) 0.38688(10) 0.0244(4) Uani 1 1 d . . . H12 H -0.4493 0.4352 0.3924 0.029 Uiso 1 1 calc R . . C13 C -0.2696(2) 0.3975(2) 0.43940(9) 0.0253(4) Uani 1 1 d . . . H13 H -0.3181 0.3985 0.4809 0.030 Uiso 1 1 calc R . . C14 C -0.12046(19) 0.37430(19) 0.43164(8) 0.0207(3) Uani 1 1 d . . . H14 H -0.0679 0.3610 0.4678 0.025 Uiso 1 1 calc R . . C15 C 0.16618(18) 0.50456(16) 0.35982(7) 0.0144(3) Uani 1 1 d . . . C16 C 0.28706(18) 0.52286(17) 0.32535(8) 0.0169(3) Uani 1 1 d . . . H16 H 0.3532 0.4518 0.2993 0.020 Uiso 1 1 calc R . . C17 C 0.3117(2) 0.64479(18) 0.32880(9) 0.0214(4) Uani 1 1 d . . . H17 H 0.3950 0.6564 0.3055 0.026 Uiso 1 1 calc R . . C18 C 0.2147(2) 0.74932(18) 0.36627(9) 0.0233(4) Uani 1 1 d . . . H18 H 0.2318 0.8323 0.3689 0.028 Uiso 1 1 calc R . . C19 C 0.0924(2) 0.73241(18) 0.39996(9) 0.0237(4) Uani 1 1 d . . . H19 H 0.0256 0.8044 0.4253 0.028 Uiso 1 1 calc R . . C20 C 0.0672(2) 0.61126(17) 0.39691(8) 0.0187(3) Uani 1 1 d . . . H20 H -0.0168 0.6006 0.4199 0.022 Uiso 1 1 calc R . . C21 C 0.21772(18) 0.25336(17) 0.43201(7) 0.0154(3) Uani 1 1 d . . . C22 C 0.3020(2) 0.30119(19) 0.46570(8) 0.0221(4) Uani 1 1 d . . . H22 H 0.3169 0.3839 0.4520 0.026 Uiso 1 1 calc R . . C23 C 0.3642(2) 0.2289(2) 0.51895(9) 0.0287(4) Uani 1 1 d . . . H23 H 0.4207 0.2628 0.5417 0.034 Uiso 1 1 calc R . . C24 C 0.3446(2) 0.1075(2) 0.53927(9) 0.0277(4) Uani 1 1 d . . . H24 H 0.3889 0.0574 0.5753 0.033 Uiso 1 1 calc R . . C25 C 0.2599(2) 0.05949(19) 0.50666(9) 0.0245(4) Uani 1 1 d . . . H25 H 0.2450 -0.0230 0.5208 0.029 Uiso 1 1 calc R . . C26 C 0.19687(19) 0.13156(18) 0.45332(8) 0.0194(3) Uani 1 1 d . . . H26 H 0.1392 0.0979 0.4312 0.023 Uiso 1 1 calc R . . C27 C 0.74418(17) 0.34144(16) 0.09050(7) 0.0135(3) Uani 1 1 d . . . C28 C 0.7080(2) 0.38386(18) 0.02859(8) 0.0191(3) Uani 1 1 d . . . H28 H 0.6561 0.3411 0.0080 0.023 Uiso 1 1 calc R . . C29 C 0.7471(2) 0.48754(19) -0.00305(9) 0.0235(4) Uani 1 1 d . . . H29 H 0.7228 0.5150 -0.0452 0.028 Uiso 1 1 calc R . . C30 C 0.8217(2) 0.55113(19) 0.02693(9) 0.0258(4) Uani 1 1 d . . . H30 H 0.8488 0.6222 0.0053 0.031 Uiso 1 1 calc R . . C31 C 0.8568(2) 0.51106(19) 0.08832(10) 0.0261(4) Uani 1 1 d . . . H31 H 0.9083 0.5546 0.1087 0.031 Uiso 1 1 calc R . . C32 C 0.8172(2) 0.40734(17) 0.12047(8) 0.0200(3) Uani 1 1 d . . . H32 H 0.8401 0.3815 0.1629 0.024 Uiso 1 1 calc R . . C33 C 0.73840(19) 0.07669(17) 0.07355(8) 0.0168(3) Uani 1 1 d . . . C34 C 0.8735(2) -0.03060(18) 0.07329(10) 0.0240(4) Uani 1 1 d . . . H34 H 0.9353 -0.0388 0.1057 0.029 Uiso 1 1 calc R . . C35 C 0.9180(2) -0.12593(19) 0.02537(11) 0.0329(5) Uani 1 1 d . . . H35 H 1.0096 -0.1998 0.0256 0.039 Uiso 1 1 calc R . . C36 C 0.8296(3) -0.1135(2) -0.02248(10) 0.0340(5) Uani 1 1 d . . . H36 H 0.8616 -0.1771 -0.0557 0.041 Uiso 1 1 calc R . . C37 C 0.6950(3) -0.0087(2) -0.02178(9) 0.0328(5) Uani 1 1 d . . . H37 H 0.6339 -0.0010 -0.0544 0.039 Uiso 1 1 calc R . . C38 C 0.6478(2) 0.08582(19) 0.02631(9) 0.0246(4) Uani 1 1 d . . . H38 H 0.5539 0.1566 0.0270 0.030 Uiso 1 1 calc R . . C39 C 0.77690(18) 0.14863(16) 0.19998(8) 0.0145(3) Uani 1 1 d . . . C40 C 0.69708(19) 0.13084(17) 0.25656(8) 0.0174(3) Uani 1 1 d . . . H40 H 0.5945 0.1527 0.2575 0.021 Uiso 1 1 calc R . . C41 C 0.7661(2) 0.08155(19) 0.31137(9) 0.0233(4) Uani 1 1 d . . . H41 H 0.7108 0.0696 0.3496 0.028 Uiso 1 1 calc R . . C42 C 0.9154(2) 0.04965(18) 0.31047(9) 0.0247(4) Uani 1 1 d . . . H42 H 0.9625 0.0160 0.3481 0.030 Uiso 1 1 calc R . . C43 C 0.99638(19) 0.06690(17) 0.25449(9) 0.0209(4) Uani 1 1 d . . . H43 H 1.0989 0.0450 0.2539 0.025 Uiso 1 1 calc R . . C44 C 0.92815(18) 0.11598(16) 0.19938(8) 0.0178(3) Uani 1 1 d . . . H44 H 0.9840 0.1275 0.1612 0.021 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.00924(6) 0.01298(6) 0.01029(6) -0.00145(4) -0.00023(4) -0.00304(4) Pd2 0.00944(6) 0.01308(6) 0.01028(6) -0.00101(4) -0.00027(4) -0.00268(4) S1 0.01376(18) 0.01404(17) 0.01402(18) 0.00027(14) 0.00009(14) -0.00360(14) S2 0.01277(18) 0.01565(17) 0.01310(18) -0.00356(14) 0.00000(14) -0.00524(14) S3 0.01390(19) 0.01373(17) 0.0205(2) -0.00071(15) 0.00151(15) -0.00311(15) S4 0.01030(18) 0.01743(18) 0.01247(17) 0.00012(14) -0.00166(14) -0.00220(14) P1 0.01091(19) 0.01470(18) 0.01077(18) -0.00113(14) -0.00046(14) -0.00324(15) P2 0.01075(19) 0.01294(17) 0.01144(18) -0.00139(14) 0.00025(14) -0.00350(15) C1 0.0133(8) 0.0137(7) 0.0208(8) -0.0014(6) 0.0008(6) -0.0056(6) C2 0.0128(8) 0.0129(7) 0.0212(8) -0.0030(6) 0.0012(6) -0.0048(6) C3 0.0158(8) 0.0152(7) 0.0167(8) -0.0012(6) -0.0009(6) -0.0003(6) C4 0.0150(8) 0.0151(7) 0.0141(7) 0.0004(6) -0.0019(6) 0.0003(6) C5 0.0198(9) 0.0153(8) 0.0277(9) 0.0010(7) -0.0003(7) -0.0023(7) C6 0.0207(9) 0.0171(8) 0.0221(9) -0.0050(7) 0.0038(7) -0.0045(7) C7 0.0235(9) 0.0164(8) 0.0318(10) 0.0002(7) 0.0012(8) -0.0019(7) C8 0.0145(8) 0.0233(8) 0.0219(9) -0.0006(7) -0.0002(7) 0.0016(7) C9 0.0114(7) 0.0154(7) 0.0168(8) -0.0019(6) 0.0004(6) -0.0038(6) C10 0.0158(8) 0.0151(7) 0.0172(8) 0.0000(6) -0.0019(6) -0.0044(6) C11 0.0163(8) 0.0191(8) 0.0257(9) 0.0001(7) -0.0057(7) -0.0051(7) C12 0.0110(8) 0.0263(9) 0.0348(10) -0.0009(8) -0.0008(7) -0.0059(7) C13 0.0173(9) 0.0326(10) 0.0233(9) -0.0020(8) 0.0048(7) -0.0078(8) C14 0.0168(8) 0.0272(9) 0.0168(8) -0.0022(7) -0.0004(6) -0.0065(7) C15 0.0151(8) 0.0157(7) 0.0125(7) 0.0010(6) -0.0043(6) -0.0050(6) C16 0.0134(8) 0.0197(8) 0.0168(8) -0.0013(6) -0.0028(6) -0.0047(6) C17 0.0171(8) 0.0247(9) 0.0242(9) 0.0021(7) -0.0025(7) -0.0102(7) C18 0.0298(10) 0.0178(8) 0.0242(9) 0.0013(7) -0.0059(8) -0.0103(7) C19 0.0310(10) 0.0167(8) 0.0196(9) -0.0030(7) 0.0009(7) -0.0047(7) C20 0.0196(8) 0.0192(8) 0.0151(8) -0.0012(6) 0.0020(6) -0.0053(7) C21 0.0129(8) 0.0195(8) 0.0100(7) -0.0008(6) 0.0010(6) -0.0020(6) C22 0.0224(9) 0.0279(9) 0.0175(8) 0.0024(7) -0.0055(7) -0.0106(7) C23 0.0267(10) 0.0409(11) 0.0207(9) 0.0041(8) -0.0097(8) -0.0135(9) C24 0.0223(9) 0.0367(10) 0.0185(9) 0.0089(8) -0.0045(7) -0.0053(8) C25 0.0231(9) 0.0245(9) 0.0198(9) 0.0059(7) 0.0022(7) -0.0042(7) C26 0.0171(8) 0.0227(8) 0.0163(8) -0.0007(6) 0.0008(6) -0.0054(7) C27 0.0104(7) 0.0135(7) 0.0146(7) -0.0009(6) 0.0020(6) -0.0027(6) C28 0.0203(9) 0.0209(8) 0.0169(8) 0.0009(6) -0.0037(7) -0.0082(7) C29 0.0275(10) 0.0241(9) 0.0173(8) 0.0053(7) -0.0036(7) -0.0081(7) C30 0.0279(10) 0.0206(8) 0.0297(10) 0.0076(7) -0.0012(8) -0.0117(8) C31 0.0298(10) 0.0231(9) 0.0313(10) 0.0029(8) -0.0082(8) -0.0157(8) C32 0.0239(9) 0.0193(8) 0.0185(8) 0.0016(6) -0.0054(7) -0.0093(7) C33 0.0196(8) 0.0162(7) 0.0156(8) -0.0045(6) 0.0061(6) -0.0092(6) C34 0.0187(9) 0.0188(8) 0.0333(10) -0.0063(7) 0.0061(8) -0.0071(7) C35 0.0311(11) 0.0177(8) 0.0454(12) -0.0107(8) 0.0198(9) -0.0091(8) C36 0.0568(15) 0.0250(9) 0.0239(10) -0.0122(8) 0.0202(9) -0.0241(10) C37 0.0572(15) 0.0296(10) 0.0179(9) -0.0049(8) 0.0011(9) -0.0239(10) C38 0.0350(11) 0.0214(8) 0.0189(9) -0.0040(7) -0.0010(8) -0.0117(8) C39 0.0138(8) 0.0130(7) 0.0163(7) -0.0002(6) -0.0027(6) -0.0039(6) C40 0.0158(8) 0.0191(8) 0.0187(8) 0.0025(6) -0.0037(6) -0.0081(6) C41 0.0282(10) 0.0278(9) 0.0188(8) 0.0083(7) -0.0066(7) -0.0164(8) C42 0.0302(10) 0.0192(8) 0.0284(10) 0.0086(7) -0.0160(8) -0.0110(7) C43 0.0141(8) 0.0142(7) 0.0341(10) -0.0006(7) -0.0096(7) -0.0026(6) C44 0.0141(8) 0.0150(7) 0.0240(9) -0.0006(6) -0.0013(6) -0.0050(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 P1 2.2860(4) . ? Pd1 S1 2.2869(4) . ? Pd1 S2 2.3183(4) . ? Pd1 S4 2.3937(4) . ? Pd1 Pd2 2.96498(17) . ? Pd2 S3 2.2762(4) . ? Pd2 P2 2.2853(4) . ? Pd2 S4 2.3159(4) . ? Pd2 S2 2.3750(4) . ? S1 C1 1.7600(17) . ? S2 C2 1.7726(17) . ? S3 C3 1.7548(17) . ? S4 C4 1.7734(17) . ? P1 C15 1.8177(16) . ? P1 C21 1.8236(16) . ? P1 C9 1.8267(17) . ? P2 C39 1.8176(16) . ? P2 C27 1.8241(16) . ? P2 C33 1.8250(17) . ? C1 C2 1.343(2) . ? C1 C5 1.512(2) . ? C2 C6 1.511(2) . ? C3 C4 1.345(2) . ? C3 C7 1.505(2) . ? C4 C8 1.507(2) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C14 1.397(2) . ? C9 C10 1.397(2) . ? C10 C11 1.388(2) . ? C10 H10 0.9500 . ? C11 C12 1.387(3) . ? C11 H11 0.9500 . ? C12 C13 1.385(3) . ? C12 H12 0.9500 . ? C13 C14 1.392(3) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 C16 1.391(2) . ? C15 C20 1.402(2) . ? C16 C17 1.393(2) . ? C16 H16 0.9500 . ? C17 C18 1.387(3) . ? C17 H17 0.9500 . ? C18 C19 1.390(3) . ? C18 H18 0.9500 . ? C19 C20 1.387(2) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C22 1.397(2) . ? C21 C26 1.400(2) . ? C22 C23 1.386(2) . ? C22 H22 0.9500 . ? C23 C24 1.385(3) . ? C23 H23 0.9500 . ? C24 C25 1.387(3) . ? C24 H24 0.9500 . ? C25 C26 1.390(2) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C32 1.392(2) . ? C27 C28 1.398(2) . ? C28 C29 1.385(2) . ? C28 H28 0.9500 . ? C29 C30 1.386(3) . ? C29 H29 0.9500 . ? C30 C31 1.382(3) . ? C30 H30 0.9500 . ? C31 C32 1.392(2) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C33 C34 1.393(2) . ? C33 C38 1.395(3) . ? C34 C35 1.394(3) . ? C34 H34 0.9500 . ? C35 C36 1.383(3) . ? C35 H35 0.9500 . ? C36 C37 1.377(3) . ? C36 H36 0.9500 . ? C37 C38 1.391(3) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? C39 C40 1.395(2) . ? C39 C44 1.402(2) . ? C40 C41 1.386(2) . ? C40 H40 0.9500 . ? C41 C42 1.384(3) . ? C41 H41 0.9500 . ? C42 C43 1.389(3) . ? C42 H42 0.9500 . ? C43 C44 1.388(2) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Pd1 S1 92.755(15) . . ? P1 Pd1 S2 178.145(15) . . ? S1 Pd1 S2 87.054(15) . . ? P1 Pd1 S4 101.977(15) . . ? S1 Pd1 S4 164.174(15) . . ? S2 Pd1 S4 78.407(14) . . ? P1 Pd1 Pd2 129.916(11) . . ? S1 Pd1 Pd2 115.625(11) . . ? S2 Pd1 Pd2 51.677(10) . . ? S4 Pd1 Pd2 49.824(10) . . ? S3 Pd2 P2 89.547(15) . . ? S3 Pd2 S4 88.253(15) . . ? P2 Pd2 S4 176.960(15) . . ? S3 Pd2 S2 166.456(15) . . ? P2 Pd2 S2 103.199(14) . . ? S4 Pd2 S2 78.835(14) . . ? S3 Pd2 Pd1 118.192(12) . . ? P2 Pd2 Pd1 127.503(11) . . ? S4 Pd2 Pd1 52.161(10) . . ? S2 Pd2 Pd1 49.977(10) . . ? C1 S1 Pd1 104.47(6) . . ? C2 S2 Pd1 105.41(6) . . ? C2 S2 Pd2 120.74(6) . . ? Pd1 S2 Pd2 78.346(12) . . ? C3 S3 Pd2 103.77(6) . . ? C4 S4 Pd2 104.03(6) . . ? C4 S4 Pd1 123.02(6) . . ? Pd2 S4 Pd1 78.015(12) . . ? C15 P1 C21 103.10(7) . . ? C15 P1 C9 106.25(7) . . ? C21 P1 C9 104.01(7) . . ? C15 P1 Pd1 113.73(5) . . ? C21 P1 Pd1 114.81(5) . . ? C9 P1 Pd1 113.80(5) . . ? C39 P2 C27 107.11(7) . . ? C39 P2 C33 107.62(8) . . ? C27 P2 C33 102.36(7) . . ? C39 P2 Pd2 112.37(6) . . ? C27 P2 Pd2 112.74(5) . . ? C33 P2 Pd2 113.94(6) . . ? C2 C1 C5 122.89(15) . . ? C2 C1 S1 123.84(13) . . ? C5 C1 S1 113.24(12) . . ? C1 C2 C6 124.86(15) . . ? C1 C2 S2 118.51(13) . . ? C6 C2 S2 116.37(12) . . ? C4 C3 C7 123.49(15) . . ? C4 C3 S3 124.02(13) . . ? C7 C3 S3 112.49(13) . . ? C3 C4 C8 124.71(15) . . ? C3 C4 S4 119.10(13) . . ? C8 C4 S4 116.06(13) . . ? C1 C5 H5A 109.5 . . ? C1 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C1 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C2 C6 H6A 109.5 . . ? C2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C3 C7 H7A 109.5 . . ? C3 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C3 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C4 C8 H8A 109.5 . . ? C4 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C4 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C14 C9 C10 119.07(15) . . ? C14 C9 P1 121.74(13) . . ? C10 C9 P1 119.19(12) . . ? C11 C10 C9 120.47(16) . . ? C11 C10 H10 119.8 . . ? C9 C10 H10 119.8 . . ? C12 C11 C10 120.08(16) . . ? C12 C11 H11 120.0 . . ? C10 C11 H11 120.0 . . ? C13 C12 C11 119.97(17) . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? C12 C13 C14 120.30(17) . . ? C12 C13 H13 119.9 . . ? C14 C13 H13 119.9 . . ? C13 C14 C9 120.09(16) . . ? C13 C14 H14 120.0 . . ? C9 C14 H14 120.0 . . ? C16 C15 C20 119.44(15) . . ? C16 C15 P1 118.11(12) . . ? C20 C15 P1 122.37(13) . . ? C15 C16 C17 120.36(16) . . ? C15 C16 H16 119.8 . . ? C17 C16 H16 119.8 . . ? C18 C17 C16 120.01(16) . . ? C18 C17 H17 120.0 . . ? C16 C17 H17 120.0 . . ? C17 C18 C19 119.84(16) . . ? C17 C18 H18 120.1 . . ? C19 C18 H18 120.1 . . ? C20 C19 C18 120.53(17) . . ? C20 C19 H19 119.7 . . ? C18 C19 H19 119.7 . . ? C19 C20 C15 119.80(16) . . ? C19 C20 H20 120.1 . . ? C15 C20 H20 120.1 . . ? C22 C21 C26 118.64(15) . . ? C22 C21 P1 121.33(13) . . ? C26 C21 P1 119.84(13) . . ? C23 C22 C21 120.51(17) . . ? C23 C22 H22 119.7 . . ? C21 C22 H22 119.7 . . ? C24 C23 C22 120.51(18) . . ? C24 C23 H23 119.7 . . ? C22 C23 H23 119.7 . . ? C23 C24 C25 119.61(17) . . ? C23 C24 H24 120.2 . . ? C25 C24 H24 120.2 . . ? C24 C25 C26 120.25(17) . . ? C24 C25 H25 119.9 . . ? C26 C25 H25 119.9 . . ? C25 C26 C21 120.47(17) . . ? C25 C26 H26 119.8 . . ? C21 C26 H26 119.8 . . ? C32 C27 C28 118.91(15) . . ? C32 C27 P2 123.08(13) . . ? C28 C27 P2 117.71(12) . . ? C29 C28 C27 120.71(16) . . ? C29 C28 H28 119.6 . . ? C27 C28 H28 119.6 . . ? C28 C29 C30 119.88(17) . . ? C28 C29 H29 120.1 . . ? C30 C29 H29 120.1 . . ? C31 C30 C29 119.96(16) . . ? C31 C30 H30 120.0 . . ? C29 C30 H30 120.0 . . ? C30 C31 C32 120.42(17) . . ? C30 C31 H31 119.8 . . ? C32 C31 H31 119.8 . . ? C27 C32 C31 120.10(16) . . ? C27 C32 H32 120.0 . . ? C31 C32 H32 120.0 . . ? C34 C33 C38 119.38(16) . . ? C34 C33 P2 123.09(14) . . ? C38 C33 P2 117.45(13) . . ? C33 C34 C35 119.86(19) . . ? C33 C34 H34 120.1 . . ? C35 C34 H34 120.1 . . ? C36 C35 C34 120.4(2) . . ? C36 C35 H35 119.8 . . ? C34 C35 H35 119.8 . . ? C37 C36 C35 119.84(18) . . ? C37 C36 H36 120.1 . . ? C35 C36 H36 120.1 . . ? C36 C37 C38 120.5(2) . . ? C36 C37 H37 119.7 . . ? C38 C37 H37 119.7 . . ? C37 C38 C33 119.99(19) . . ? C37 C38 H38 120.0 . . ? C33 C38 H38 120.0 . . ? C40 C39 C44 118.97(15) . . ? C40 C39 P2 117.22(12) . . ? C44 C39 P2 123.81(13) . . ? C41 C40 C39 120.59(16) . . ? C41 C40 H40 119.7 . . ? C39 C40 H40 119.7 . . ? C42 C41 C40 120.14(17) . . ? C42 C41 H41 119.9 . . ? C40 C41 H41 119.9 . . ? C41 C42 C43 119.94(16) . . ? C41 C42 H42 120.0 . . ? C43 C42 H42 120.0 . . ? C44 C43 C42 120.28(16) . . ? C44 C43 H43 119.9 . . ? C42 C43 H43 119.9 . . ? C43 C44 C39 120.08(16) . . ? C43 C44 H44 120.0 . . ? C39 C44 H44 120.0 . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 28.50 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.457 _refine_diff_density_min -0.491 _refine_diff_density_rms 0.075 #===END