data_leung94 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H27 As Cl5 P Pd' _chemical_formula_weight 741.03 _chemical_absolute_configuration ad 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'As' 'As' 0.0499 2.0058 '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 Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 8.6453(3) _cell_length_b 14.7344(6) _cell_length_c 22.8349(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2908.78(19) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5516 _cell_measurement_theta_min 2.52 _cell_measurement_theta_max 29.26 _exptl_crystal_description fragment _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.692 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1472 _exptl_absorpt_coefficient_mu 2.298 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5974 _exptl_absorpt_correction_T_max 0.7244 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 '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 38758 _diffrn_reflns_av_R_equivalents 0.0450 _diffrn_reflns_av_sigmaI/netI 0.0507 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 30.63 _reflns_number_total 8929 _reflns_number_gt 7780 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0369P)^2^+0.0000P] 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 -0.001(8) _refine_ls_number_reflns 8929 _refine_ls_number_parameters 318 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0410 _refine_ls_R_factor_gt 0.0296 _refine_ls_wR_factor_ref 0.0805 _refine_ls_wR_factor_gt 0.0613 _refine_ls_goodness_of_fit_ref 1.087 _refine_ls_restrained_S_all 1.087 _refine_ls_shift/su_max 0.002 _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 1.13950(3) 0.109935(15) 0.791616(10) 0.01851(6) Uani 1 1 d . . . As1 As 1.01768(4) 0.01973(2) 0.861295(13) 0.01854(7) Uani 1 1 d . . . P1 P 0.89538(10) 0.15356(5) 0.77016(4) 0.01949(17) Uani 1 1 d . . . Cl1 Cl 1.37823(10) 0.06194(6) 0.82927(4) 0.02870(17) Uani 1 1 d . . . Cl2 Cl 1.25707(12) 0.21282(6) 0.72660(4) 0.0373(2) Uani 1 1 d . . . Cl3 Cl 0.58416(14) 0.27363(7) 0.91435(5) 0.0494(3) Uani 1 1 d . . . Cl4 Cl 0.26441(18) 0.24304(10) 0.94425(6) 0.0688(4) Uani 1 1 d . . . Cl5 Cl 0.34875(14) 0.39412(8) 0.87152(6) 0.0573(3) Uani 1 1 d . . . C1 C 1.1149(4) -0.0232(2) 0.93173(13) 0.0221(6) Uani 1 1 d . . . C2 C 1.1979(5) -0.1032(3) 0.93103(16) 0.0330(8) Uani 1 1 d . . . H2 H 1.2089 -0.1362 0.8955 0.040 Uiso 1 1 calc R . . C3 C 1.2649(5) -0.1352(3) 0.98194(17) 0.0403(10) Uani 1 1 d . . . H3 H 1.3221 -0.1903 0.9814 0.048 Uiso 1 1 calc R . . C4 C 1.2488(5) -0.0875(3) 1.03370(16) 0.0344(9) Uani 1 1 d . . . H4 H 1.2936 -0.1099 1.0688 0.041 Uiso 1 1 calc R . . C5 C 1.1676(5) -0.0073(3) 1.03392(16) 0.0336(9) Uani 1 1 d . . . H5 H 1.1577 0.0261 1.0693 0.040 Uiso 1 1 calc R . . C6 C 1.1002(4) 0.0252(2) 0.98328(15) 0.0293(7) Uani 1 1 d . . . H6 H 1.0440 0.0806 0.9839 0.035 Uiso 1 1 calc R . . C7 C 0.8647(4) -0.0727(2) 0.83669(13) 0.0228(6) Uani 1 1 d . . . H7 H 0.9085 -0.1318 0.8230 0.027 Uiso 1 1 calc R . . C8 C 0.7643(4) -0.0773(2) 0.89088(13) 0.0245(7) Uani 1 1 d . . . C9 C 0.7008(6) -0.1662(3) 0.91066(17) 0.0406(10) Uani 1 1 d . . . H9A H 0.6456 -0.1580 0.9478 0.061 Uiso 1 1 calc R . . H9B H 0.7858 -0.2093 0.9162 0.061 Uiso 1 1 calc R . . H9C H 0.6293 -0.1896 0.8810 0.061 Uiso 1 1 calc R . . C10 C 0.6305(5) 0.0302(2) 0.96240(15) 0.0312(8) Uani 1 1 d . . . H10A H 0.5432 0.0658 0.9476 0.047 Uiso 1 1 calc R . . H10B H 0.6881 0.0661 0.9912 0.047 Uiso 1 1 calc R . . H10C H 0.5919 -0.0253 0.9810 0.047 Uiso 1 1 calc R . . C11 C 0.7352(4) 0.0056(2) 0.91257(14) 0.0221(7) Uani 1 1 d . . . C12 C 0.8201(4) 0.0793(2) 0.87864(13) 0.0191(6) Uani 1 1 d . . . H12 H 0.8279 0.1395 0.8987 0.023 Uiso 1 1 calc R . . C13 C 0.7755(4) -0.0172(2) 0.79030(15) 0.0246(6) Uani 1 1 d . . . H13A H 0.6709 -0.0429 0.7844 0.030 Uiso 1 1 calc R . . H13B H 0.8312 -0.0182 0.7524 0.030 Uiso 1 1 calc R . . C14 C 0.7642(4) 0.0822(2) 0.81408(13) 0.0206(6) Uani 1 1 d . . . H14 H 0.6555 0.1051 0.8116 0.025 Uiso 1 1 calc R . . C15 C 0.8201(4) 0.1430(2) 0.69581(13) 0.0226(7) Uani 1 1 d . . . C16 C 0.6629(4) 0.1282(2) 0.68683(15) 0.0305(8) Uani 1 1 d . . . H16 H 0.5958 0.1211 0.7195 0.037 Uiso 1 1 calc R . . C17 C 0.6032(5) 0.1237(2) 0.63010(16) 0.0358(9) Uani 1 1 d . . . H17 H 0.4955 0.1146 0.6242 0.043 Uiso 1 1 calc R . . C18 C 0.7014(5) 0.1323(3) 0.58252(16) 0.0364(9) Uani 1 1 d . . . H18 H 0.6618 0.1277 0.5438 0.044 Uiso 1 1 calc R . . C19 C 0.8559(6) 0.1477(3) 0.59159(16) 0.0390(9) Uani 1 1 d . . . H19 H 0.9227 0.1547 0.5589 0.047 Uiso 1 1 calc R . . C20 C 0.9162(5) 0.1531(2) 0.64771(15) 0.0303(8) Uani 1 1 d . . . H20 H 1.0236 0.1638 0.6532 0.036 Uiso 1 1 calc R . . C21 C 0.8597(4) 0.27143(19) 0.78987(14) 0.0233(6) Uani 1 1 d . . . C22 C 0.7319(6) 0.3177(3) 0.76855(18) 0.0417(10) Uani 1 1 d . . . H22 H 0.6608 0.2878 0.7433 0.050 Uiso 1 1 calc R . . C23 C 0.7077(6) 0.4078(3) 0.78404(18) 0.0489(12) Uani 1 1 d . . . H23 H 0.6196 0.4390 0.7694 0.059 Uiso 1 1 calc R . . C24 C 0.8079(6) 0.4519(3) 0.8197(2) 0.0431(11) Uani 1 1 d . . . H24 H 0.7909 0.5137 0.8296 0.052 Uiso 1 1 calc R . . C25 C 0.9325(5) 0.4073(3) 0.8413(2) 0.0494(12) Uani 1 1 d . . . H25 H 1.0021 0.4377 0.8668 0.059 Uiso 1 1 calc R . . C26 C 0.9592(5) 0.3164(3) 0.8262(2) 0.0391(9) Uani 1 1 d . . . H26 H 1.0473 0.2858 0.8413 0.047 Uiso 1 1 calc R . . C27 C 0.3910(5) 0.2808(3) 0.89026(19) 0.0406(10) Uani 1 1 d . . . H27 H 0.3783 0.2419 0.8547 0.049 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 0.01390(11) 0.02163(10) 0.02001(10) 0.00118(9) 0.00093(9) -0.00071(9) As1 0.01710(17) 0.02060(14) 0.01792(14) 0.00130(12) -0.00027(12) -0.00045(12) P1 0.0165(4) 0.0231(4) 0.0189(4) 0.0036(3) 0.0006(3) 0.0005(3) Cl1 0.0152(4) 0.0358(4) 0.0351(4) 0.0001(3) -0.0036(3) 0.0015(3) Cl2 0.0277(5) 0.0393(5) 0.0448(5) 0.0183(4) 0.0079(4) -0.0025(4) Cl3 0.0459(7) 0.0417(5) 0.0607(7) -0.0008(5) -0.0035(5) 0.0097(5) Cl4 0.0671(10) 0.0726(9) 0.0667(8) 0.0037(7) 0.0264(7) -0.0108(7) Cl5 0.0399(6) 0.0425(5) 0.0894(9) 0.0051(6) -0.0107(6) 0.0020(5) C1 0.0218(18) 0.0239(14) 0.0206(14) 0.0040(12) -0.0019(13) -0.0009(13) C2 0.042(2) 0.0309(17) 0.0257(17) -0.0006(15) -0.0035(15) 0.0099(16) C3 0.050(3) 0.0352(19) 0.036(2) 0.0087(16) -0.0035(19) 0.0172(18) C4 0.035(2) 0.041(2) 0.0276(18) 0.0097(15) -0.0052(16) 0.0060(17) C5 0.039(2) 0.0388(19) 0.0232(16) -0.0006(14) -0.0056(15) 0.0059(16) C6 0.030(2) 0.0314(17) 0.0262(17) -0.0031(15) -0.0019(15) 0.0052(15) C7 0.0261(18) 0.0196(13) 0.0228(15) -0.0015(11) 0.0005(14) -0.0024(14) C8 0.031(2) 0.0249(15) 0.0179(15) 0.0002(12) -0.0003(14) -0.0069(14) C9 0.057(3) 0.0318(19) 0.033(2) 0.0031(16) 0.0078(19) -0.0168(18) C10 0.030(2) 0.0380(18) 0.0262(16) 0.0029(14) 0.0099(16) -0.0015(17) C11 0.0174(17) 0.0285(16) 0.0204(14) 0.0047(12) 0.0005(12) -0.0018(12) C12 0.0184(17) 0.0210(13) 0.0180(14) 0.0027(11) 0.0020(12) 0.0005(11) C13 0.0246(18) 0.0291(15) 0.0202(14) 0.0022(14) -0.0004(14) -0.0077(13) C14 0.0166(16) 0.0262(15) 0.0189(14) 0.0023(12) 0.0017(12) -0.0011(12) C15 0.0202(18) 0.0272(15) 0.0204(15) 0.0028(12) -0.0010(12) 0.0033(12) C16 0.022(2) 0.045(2) 0.0243(16) 0.0047(14) -0.0021(14) 0.0001(15) C17 0.032(2) 0.043(2) 0.0327(19) 0.0038(16) -0.0087(16) -0.0009(16) C18 0.046(3) 0.041(2) 0.0222(17) 0.0020(15) -0.0112(16) 0.0048(17) C19 0.041(3) 0.051(2) 0.0247(17) 0.0022(16) 0.0054(18) 0.003(2) C20 0.028(2) 0.0364(18) 0.0267(18) 0.0044(15) 0.0049(14) 0.0026(15) C21 0.0242(17) 0.0233(13) 0.0223(14) 0.0043(12) 0.0052(15) 0.0021(13) C22 0.052(3) 0.038(2) 0.034(2) -0.0003(16) -0.0093(19) 0.0160(19) C23 0.069(3) 0.041(2) 0.036(2) 0.0100(19) 0.003(2) 0.029(2) C24 0.054(3) 0.0256(18) 0.050(2) 0.0024(17) 0.023(2) 0.0032(17) C25 0.036(3) 0.039(2) 0.072(3) -0.019(2) 0.010(2) -0.0029(18) C26 0.025(2) 0.0336(19) 0.059(3) -0.0097(18) 0.0001(19) 0.0009(16) C27 0.037(3) 0.037(2) 0.048(2) -0.0087(17) 0.0037(19) -0.0037(17) _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 2.2600(9) . ? Pd1 As1 2.3254(4) . ? Pd1 Cl1 2.3449(9) . ? Pd1 Cl2 2.3527(9) . ? As1 C1 1.922(3) . ? As1 C12 1.961(3) . ? As1 C7 1.980(3) . ? P1 C21 1.820(3) . ? P1 C15 1.825(3) . ? P1 C14 1.843(3) . ? Cl3 C27 1.761(5) . ? Cl4 C27 1.740(5) . ? Cl5 C27 1.761(4) . ? C1 C2 1.380(5) . ? C1 C6 1.382(5) . ? C2 C3 1.382(5) . ? C3 C4 1.383(5) . ? C4 C5 1.374(5) . ? C5 C6 1.380(5) . ? C7 C8 1.513(5) . ? C7 C13 1.545(5) . ? C8 C11 1.342(5) . ? C8 C9 1.490(5) . ? C10 C11 1.498(5) . ? C11 C12 1.522(4) . ? C12 C14 1.552(4) . ? C13 C14 1.565(4) . ? C15 C20 1.385(5) . ? C15 C16 1.392(5) . ? C16 C17 1.396(5) . ? C17 C18 1.385(6) . ? C18 C19 1.371(6) . ? C19 C20 1.386(5) . ? C21 C26 1.366(5) . ? C21 C22 1.387(5) . ? C22 C23 1.390(6) . ? C23 C24 1.356(7) . ? C24 C25 1.355(7) . ? C25 C26 1.401(5) . ? 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 As1 83.57(2) . . ? P1 Pd1 Cl1 170.82(3) . . ? As1 Pd1 Cl1 88.59(2) . . ? P1 Pd1 Cl2 94.78(3) . . ? As1 Pd1 Cl2 174.70(3) . . ? Cl1 Pd1 Cl2 92.60(3) . . ? C1 As1 C12 111.05(13) . . ? C1 As1 C7 107.67(14) . . ? C12 As1 C7 77.49(14) . . ? C1 As1 Pd1 124.23(10) . . ? C12 As1 Pd1 106.07(9) . . ? C7 As1 Pd1 120.10(9) . . ? C21 P1 C15 104.54(15) . . ? C21 P1 C14 107.76(15) . . ? C15 P1 C14 103.77(15) . . ? C21 P1 Pd1 112.09(12) . . ? C15 P1 Pd1 120.70(11) . . ? C14 P1 Pd1 107.12(11) . . ? C2 C1 C6 119.9(3) . . ? C2 C1 As1 119.9(2) . . ? C6 C1 As1 120.2(3) . . ? C1 C2 C3 120.0(3) . . ? C2 C3 C4 120.2(3) . . ? C5 C4 C3 119.5(3) . . ? C4 C5 C6 120.7(3) . . ? C5 C6 C1 119.7(3) . . ? C8 C7 C13 107.3(3) . . ? C8 C7 As1 100.5(2) . . ? C13 C7 As1 99.43(19) . . ? C11 C8 C9 128.3(3) . . ? C11 C8 C7 111.6(3) . . ? C9 C8 C7 119.9(3) . . ? C8 C11 C10 127.8(3) . . ? C8 C11 C12 111.8(3) . . ? C10 C11 C12 120.4(3) . . ? C11 C12 C14 110.7(3) . . ? C11 C12 As1 101.8(2) . . ? C14 C12 As1 95.28(19) . . ? C7 C13 C14 106.8(3) . . ? C12 C14 C13 106.5(3) . . ? C12 C14 P1 109.9(2) . . ? C13 C14 P1 107.8(2) . . ? C20 C15 C16 119.1(3) . . ? C20 C15 P1 121.0(3) . . ? C16 C15 P1 119.9(3) . . ? C15 C16 C17 120.3(3) . . ? C18 C17 C16 119.8(4) . . ? C19 C18 C17 119.6(3) . . ? C18 C19 C20 121.1(4) . . ? C15 C20 C19 120.1(4) . . ? C26 C21 C22 118.4(3) . . ? C26 C21 P1 120.4(3) . . ? C22 C21 P1 121.2(3) . . ? C21 C22 C23 120.0(4) . . ? C24 C23 C22 120.9(4) . . ? C25 C24 C23 119.6(4) . . ? C24 C25 C26 120.3(4) . . ? C21 C26 C25 120.6(4) . . ? Cl4 C27 Cl5 110.2(2) . . ? Cl4 C27 Cl3 110.8(2) . . ? Cl5 C27 Cl3 109.2(2) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 30.63 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.711 _refine_diff_density_min -0.657 _refine_diff_density_rms 0.269