#============================================================================== data_global #============================================================================== _audit_creation_date 02-April-2004 _audit_creation_method SHELXTL _audit_update_record ; ? ; # 1. Submission Details _publ_contact_author_name 'Ulli Englert' _publ_contact_author_address ; Institut fuer Anorganische Chemie RWTH Aachen Prof.-Pirlet-Str.1 52074 Aachen Germany ; _publ_contact_author_email 'ullrich.englert@ac.rwth-aachen.de' _publ_contact_author_fax '0049-241-8092288' _publ_contact_author_phone '0049-241-8094666' _publ_requested_journal 'Organometallics' _publ_requested_category ? _publ_requested_coeditor_name ? _publ_contact_letter ; ? ; # 2. Processing Summary (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? # 3. Title and Author List _publ_section_title ; see text ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address 'Englert, Ulli' #<--'Last name, first name' ; Institut fuer Anorganische Chemie RWTH Aachen Prof.-Pirlet-Str. 1 52074 Aachen Germany ; 'Hu, Chunhua' #<--'Last name, first name' ; Institut fuer Anorganische Chemie RWTH Aachen Prof.-Pirlet-Str. 1 52074 Aachen Germany ; 'Salzer, Albrecht' #<--'Last name, first name' ; Institut fuer Anorganische Chemie RWTH Aachen Prof.-Pirlet-Str. 1 52074 Aachen Germany ; 'Alberico, Elisabetta' #<--'Last name, first name' ; Institute for Biomolecular Chemistry National Research Council I 07040 Sassari Italy ; # 4. Text _publ_section_abstract ; see text ; _publ_section_comment ; see text ; _publ_section_exptl_prep ; see text ; _publ_section_exptl_refinement ; see text ; _publ_section_references ; see text ; _publ_section_figure_captions ; see text ; _publ_section_table_legends ; see text ; _publ_section_acknowledgements ; see text ; #========================================================================== data_4 _chemical_name_systematic ; compound code syn-(S,Sp)-4 ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H24 Cr N O3 P' _chemical_formula_weight 481.43 _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 'Cr' 'Cr' 0.3209 0.6236 '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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' _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+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 10.399(3) _cell_length_b 12.562(5) _cell_length_c 18.042(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2356.9(13) _cell_formula_units_Z 4 _cell_measurement_temperature 253(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7 _cell_measurement_theta_max 14 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.357 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1000 _exptl_absorpt_coefficient_mu 0.581 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.938 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'PSI scans' _exptl_special_details ; ? ; _diffrn_ambient_temperature 253(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type Enraf_Nonius_CAD4 _diffrn_measurement_method \q/2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 1.43 _diffrn_reflns_number 6798 _diffrn_reflns_av_R_equivalents 0.0740 _diffrn_reflns_av_sigmaI/netI 0.1532 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.24 _diffrn_reflns_theta_max 25.10 _reflns_number_total 4184 _reflns_number_gt 2502 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 (Enraf-Nonius, 1977)' _computing_cell_refinement 'CAD4 (Enraf-Nonius, 1977)' _computing_data_reduction 'PROCESS_MolEN (Fair, 1990)' _computing_structure_solution 'SHELXTL (Sheldrick, 1998)' _computing_structure_refinement 'SHELXTL (Sheldrick, 1998)' _computing_molecular_graphics 'Platon (Spek, 2003)' _computing_publication_material ? _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^)+(0.0326P)^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 0.04(4) _refine_ls_number_reflns 4184 _refine_ls_number_parameters 289 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1411 _refine_ls_R_factor_gt 0.0704 _refine_ls_wR_factor_ref 0.1156 _refine_ls_wR_factor_gt 0.1052 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.061 _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 Cr Cr 0.10802(9) 0.38342(7) 0.06131(5) 0.0420(3) Uani 1 1 d . . . P P 0.39531(18) 0.47447(11) 0.16555(8) 0.0377(4) Uani 1 1 d . . . C1 C 0.0999(7) 0.5233(5) 0.0883(3) 0.0505(16) Uani 1 1 d . . . O1 O 0.0849(5) 0.6112(3) 0.1057(2) 0.0719(14) Uani 1 1 d . . . C2 C 0.0111(7) 0.4154(5) -0.0202(4) 0.0551(19) Uani 1 1 d . . . O2 O -0.0502(5) 0.4330(4) -0.0718(2) 0.0867(18) Uani 1 1 d . . . C3 C -0.0422(7) 0.3660(6) 0.1101(4) 0.0502(18) Uani 1 1 d . . . O3 O -0.1385(4) 0.3605(4) 0.1415(3) 0.0829(18) Uani 1 1 d . . . C11 C 0.3103(5) 0.3757(5) 0.1085(3) 0.0302(13) Uani 1 1 d . . . C12 C 0.2356(6) 0.2956(5) 0.1410(3) 0.0425(16) Uani 1 1 d . . . C13 C 0.1647(6) 0.2211(5) 0.0975(5) 0.059(2) Uani 1 1 d . . . C14 C 0.1700(7) 0.2257(5) 0.0197(5) 0.068(2) Uani 1 1 d . . . H14 H 0.1226 0.1746 -0.0109 0.088 Uiso 1 1 calc R . . C15 C 0.2434(7) 0.3039(6) -0.0119(4) 0.058(2) Uani 1 1 d . . . H15 H 0.2473 0.3083 -0.0661 0.075 Uiso 1 1 calc R . . C16 C 0.3115(5) 0.3763(5) 0.0290(3) 0.0426(15) Uani 1 1 d . . . H16 H 0.3628 0.4303 0.0032 0.055 Uiso 1 1 calc R . . C17 C 0.2243(7) 0.2632(5) 0.2209(4) 0.058(2) Uani 1 1 d . . . H17 H 0.2969 0.2153 0.2301 0.076 Uiso 1 1 calc R . . C18 C 0.1037(8) 0.1925(6) 0.2229(5) 0.087(3) Uani 1 1 d . . . H18A H 0.1113 0.1379 0.2615 0.114 Uiso 1 1 calc R . . H18B H 0.0266 0.2351 0.2324 0.114 Uiso 1 1 calc R . . C19 C 0.0979(8) 0.1417(5) 0.1463(5) 0.093(3) Uani 1 1 d . . . H19A H 0.1426 0.0730 0.1458 0.121 Uiso 1 1 calc R . . H19B H 0.0086 0.1310 0.1305 0.121 Uiso 1 1 calc R . . C21 C 0.4923(5) 0.5433(4) 0.0950(3) 0.0336(14) Uani 1 1 d . . . C22 C 0.4336(5) 0.6254(5) 0.0555(3) 0.0498(16) Uani 1 1 d . . . H22 H 0.3433 0.6430 0.0652 0.065 Uiso 1 1 calc R . . C23 C 0.5015(7) 0.6822(5) 0.0028(4) 0.059(2) Uani 1 1 d . . . H23 H 0.4585 0.7387 -0.0253 0.077 Uiso 1 1 calc R . . C24 C 0.6280(7) 0.6603(5) -0.0104(4) 0.057(2) Uani 1 1 d . . . H24 H 0.6766 0.7007 -0.0476 0.074 Uiso 1 1 calc R . . C25 C 0.6844(7) 0.5822(5) 0.0286(4) 0.057(2) Uani 1 1 d . . . H25 H 0.7753 0.5666 0.0193 0.075 Uiso 1 1 calc R . . C26 C 0.6197(6) 0.5226(4) 0.0813(3) 0.0469(16) Uani 1 1 d . . . H26 H 0.6645 0.4662 0.1086 0.061 Uiso 1 1 calc R . . C31 C 0.5161(6) 0.3902(5) 0.2090(3) 0.0392(14) Uani 1 1 d . . . C32 C 0.5476(6) 0.2880(5) 0.1867(3) 0.0414(16) Uani 1 1 d . . . H32 H 0.5049 0.2575 0.1433 0.054 Uiso 1 1 calc R . . C33 C 0.6372(6) 0.2286(5) 0.2241(4) 0.054(2) Uani 1 1 d . . . H33 H 0.6567 0.1559 0.2081 0.070 Uiso 1 1 calc R . . C34 C 0.6990(7) 0.2715(6) 0.2837(4) 0.067(2) Uani 1 1 d . . . H34 H 0.7629 0.2293 0.3108 0.087 Uiso 1 1 calc R . . C35 C 0.6716(7) 0.3743(7) 0.3059(4) 0.074(2) Uani 1 1 d . . . H35 H 0.7183 0.4061 0.3475 0.097 Uiso 1 1 calc R . . C36 C 0.5792(7) 0.4314(6) 0.2697(3) 0.059(2) Uani 1 1 d . . . H36 H 0.5575 0.5030 0.2871 0.077 Uiso 1 1 calc R . . N N 0.2387(6) 0.3500(5) 0.2740(3) 0.0641(18) Uani 1 1 d . . . C4 C 0.2870(8) 0.3156(7) 0.3456(3) 0.108(3) Uani 1 1 d . . . H4A H 0.2938 0.3759 0.3781 0.141 Uiso 1 1 calc R . . H4B H 0.3702 0.2837 0.3395 0.141 Uiso 1 1 calc R . . H4C H 0.2289 0.2645 0.3666 0.141 Uiso 1 1 calc R . . C5 C 0.1296(7) 0.4219(6) 0.2814(3) 0.082(3) Uani 1 1 d . . . H5A H 0.1494 0.4760 0.3172 0.106 Uiso 1 1 calc R . . H5B H 0.0556 0.3825 0.2974 0.106 Uiso 1 1 calc R . . H5C H 0.1120 0.4545 0.2343 0.106 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 Cr 0.0342(6) 0.0361(5) 0.0558(6) -0.0017(5) -0.0029(6) 0.0012(6) P 0.0404(10) 0.0345(8) 0.0380(8) -0.0014(7) 0.0014(10) 0.0031(10) C1 0.036(4) 0.050(4) 0.065(4) 0.002(3) -0.002(4) 0.008(4) O1 0.068(4) 0.037(2) 0.110(4) -0.012(3) -0.009(3) 0.018(3) C2 0.065(5) 0.050(4) 0.051(4) -0.003(4) 0.003(4) 0.013(4) O2 0.092(4) 0.108(4) 0.060(3) -0.001(3) -0.018(3) 0.022(3) C3 0.033(4) 0.054(5) 0.064(5) 0.004(4) 0.001(4) 0.004(4) O3 0.048(3) 0.108(4) 0.093(4) 0.028(3) 0.019(3) -0.003(3) C11 0.026(3) 0.028(3) 0.037(4) 0.006(3) 0.009(3) 0.004(3) C12 0.036(4) 0.041(4) 0.051(4) 0.011(3) 0.000(3) 0.010(4) C13 0.034(4) 0.031(4) 0.112(6) 0.008(4) -0.012(5) 0.004(4) C14 0.057(6) 0.043(5) 0.103(7) -0.025(5) -0.015(5) 0.011(4) C15 0.037(5) 0.066(5) 0.070(5) -0.026(4) 0.003(4) -0.007(4) C16 0.037(4) 0.042(3) 0.049(4) -0.009(3) 0.003(3) 0.000(4) C17 0.039(5) 0.050(4) 0.087(6) 0.031(4) 0.011(4) 0.014(4) C18 0.048(5) 0.083(5) 0.132(7) 0.070(5) 0.010(6) -0.004(6) C19 0.068(6) 0.044(4) 0.168(8) 0.029(5) -0.020(7) 0.000(5) C21 0.028(4) 0.033(3) 0.040(3) -0.005(3) -0.003(3) -0.004(3) C22 0.036(4) 0.053(4) 0.061(4) 0.017(4) -0.003(4) -0.002(4) C23 0.054(5) 0.061(4) 0.062(4) 0.020(4) -0.003(4) -0.005(4) C24 0.062(6) 0.047(4) 0.063(5) 0.012(3) 0.016(4) -0.018(4) C25 0.045(5) 0.049(4) 0.079(5) -0.011(4) 0.013(4) -0.002(4) C26 0.051(5) 0.033(3) 0.057(4) 0.002(3) 0.011(4) 0.006(4) C31 0.044(4) 0.045(4) 0.029(3) 0.005(3) -0.002(3) -0.003(4) C32 0.040(4) 0.036(4) 0.048(4) 0.005(3) 0.004(3) 0.006(3) C33 0.044(5) 0.045(4) 0.073(5) 0.019(4) -0.005(4) 0.013(4) C34 0.054(5) 0.080(6) 0.067(5) 0.037(4) -0.013(4) 0.003(5) C35 0.076(6) 0.077(5) 0.070(5) 0.007(5) -0.028(4) 0.006(5) C36 0.066(6) 0.066(4) 0.046(4) 0.009(4) -0.006(4) 0.005(4) N 0.057(4) 0.092(5) 0.044(3) 0.029(3) 0.008(3) 0.018(4) C4 0.093(7) 0.171(8) 0.061(5) 0.053(5) 0.018(5) 0.037(7) C5 0.071(6) 0.112(7) 0.061(5) 0.010(4) 0.021(5) 0.015(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 Cr C3 1.806(7) . ? Cr C1 1.825(7) . ? Cr C2 1.828(7) . ? Cr C15 2.174(7) . ? Cr C16 2.197(6) . ? Cr C14 2.214(6) . ? Cr C13 2.221(6) . ? Cr C12 2.246(6) . ? Cr C11 2.271(5) . ? P C31 1.820(6) . ? P C11 1.839(6) . ? P C21 1.840(6) . ? C1 O1 1.158(6) . ? C2 O2 1.148(7) . ? C3 O3 1.153(7) . ? C11 C12 1.399(8) . ? C11 C16 1.434(6) . ? C12 C13 1.427(8) . ? C12 C17 1.502(8) . ? C13 C14 1.406(9) . ? C13 C19 1.501(9) . ? C14 C15 1.368(9) . ? C14 H14 0.9800 . ? C15 C16 1.369(8) . ? C15 H15 0.9800 . ? C16 H16 0.9800 . ? C17 N 1.460(8) . ? C17 C18 1.538(9) . ? C17 H17 0.9800 . ? C18 C19 1.523(9) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C21 C26 1.373(8) . ? C21 C22 1.394(7) . ? C22 C23 1.383(8) . ? C22 H22 0.9800 . ? C23 C24 1.365(9) . ? C23 H23 0.9800 . ? C24 C25 1.342(8) . ? C24 H24 0.9800 . ? C25 C26 1.385(8) . ? C25 H25 0.9800 . ? C26 H26 0.9800 . ? C31 C36 1.378(7) . ? C31 C32 1.384(8) . ? C32 C33 1.371(8) . ? C32 H32 0.9800 . ? C33 C34 1.363(8) . ? C33 H33 0.9800 . ? C34 C35 1.382(10) . ? C34 H34 0.9800 . ? C35 C36 1.365(9) . ? C35 H35 0.9800 . ? C36 H36 0.9800 . ? N C4 1.452(7) . ? N C5 1.455(8) . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? 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 C3 Cr C1 86.9(3) . . ? C3 Cr C2 86.7(3) . . ? C1 Cr C2 88.7(3) . . ? C3 Cr C15 143.2(3) . . ? C1 Cr C15 129.4(3) . . ? C2 Cr C15 88.2(3) . . ? C3 Cr C16 163.2(3) . . ? C1 Cr C16 98.9(3) . . ? C2 Cr C16 109.1(3) . . ? C15 Cr C16 36.5(2) . . ? C3 Cr C14 108.0(3) . . ? C1 Cr C14 164.8(3) . . ? C2 Cr C14 94.8(3) . . ? C15 Cr C14 36.3(2) . . ? C16 Cr C14 66.0(3) . . ? C3 Cr C13 88.6(3) . . ? C1 Cr C13 144.8(3) . . ? C2 Cr C13 125.8(3) . . ? C15 Cr C13 65.5(3) . . ? C16 Cr C13 77.6(2) . . ? C14 Cr C13 37.0(2) . . ? C3 Cr C12 98.0(3) . . ? C1 Cr C12 109.2(3) . . ? C2 Cr C12 161.6(3) . . ? C15 Cr C12 77.3(2) . . ? C16 Cr C12 65.2(2) . . ? C14 Cr C12 66.8(2) . . ? C13 Cr C12 37.2(2) . . ? C3 Cr C11 127.8(2) . . ? C1 Cr C11 89.1(3) . . ? C2 Cr C11 145.3(3) . . ? C15 Cr C11 66.9(2) . . ? C16 Cr C11 37.38(16) . . ? C14 Cr C11 79.6(2) . . ? C13 Cr C11 66.7(2) . . ? C12 Cr C11 36.1(2) . . ? C31 P C11 100.4(3) . . ? C31 P C21 101.1(3) . . ? C11 P C21 101.1(2) . . ? O1 C1 Cr 174.9(7) . . ? O2 C2 Cr 178.4(6) . . ? O3 C3 Cr 176.5(7) . . ? C12 C11 C16 115.4(6) . . ? C12 C11 P 121.1(4) . . ? C16 C11 P 123.5(5) . . ? C12 C11 Cr 71.0(3) . . ? C16 C11 Cr 68.5(3) . . ? P C11 Cr 128.8(3) . . ? C11 C12 C13 121.9(5) . . ? C11 C12 C17 129.8(6) . . ? C13 C12 C17 108.0(6) . . ? C11 C12 Cr 72.9(3) . . ? C13 C12 Cr 70.4(3) . . ? C17 C12 Cr 134.5(5) . . ? C14 C13 C12 120.1(7) . . ? C14 C13 C19 129.2(7) . . ? C12 C13 C19 110.6(7) . . ? C14 C13 Cr 71.2(4) . . ? C12 C13 Cr 72.3(3) . . ? C19 C13 Cr 131.3(5) . . ? C15 C14 C13 117.9(7) . . ? C15 C14 Cr 70.2(4) . . ? C13 C14 Cr 71.8(4) . . ? C15 C14 H14 121.1 . . ? C13 C14 H14 121.1 . . ? Cr C14 H14 129.1 . . ? C14 C15 C16 122.7(6) . . ? C14 C15 Cr 73.5(4) . . ? C16 C15 Cr 72.7(4) . . ? C14 C15 H15 118.6 . . ? C16 C15 H15 118.6 . . ? Cr C15 H15 127.4 . . ? C15 C16 C11 122.0(6) . . ? C15 C16 Cr 70.8(4) . . ? C11 C16 Cr 74.1(3) . . ? C15 C16 H16 119.0 . . ? C11 C16 H16 119.0 . . ? Cr C16 H16 128.5 . . ? N C17 C12 114.8(5) . . ? N C17 C18 120.0(6) . . ? C12 C17 C18 104.1(6) . . ? N C17 H17 105.6 . . ? C12 C17 H17 105.6 . . ? C18 C17 H17 105.6 . . ? C19 C18 C17 104.6(7) . . ? C19 C18 H18A 110.8 . . ? C17 C18 H18A 110.8 . . ? C19 C18 H18B 110.8 . . ? C17 C18 H18B 110.8 . . ? H18A C18 H18B 108.9 . . ? C13 C19 C18 103.6(6) . . ? C13 C19 H19A 111.0 . . ? C18 C19 H19A 111.0 . . ? C13 C19 H19B 111.0 . . ? C18 C19 H19B 111.0 . . ? H19A C19 H19B 109.0 . . ? C26 C21 C22 118.1(5) . . ? C26 C21 P 124.4(5) . . ? C22 C21 P 117.4(4) . . ? C23 C22 C21 120.6(6) . . ? C23 C22 H22 119.7 . . ? C21 C22 H22 119.7 . . ? C24 C23 C22 120.6(6) . . ? C24 C23 H23 119.7 . . ? C22 C23 H23 119.7 . . ? C25 C24 C23 118.5(6) . . ? C25 C24 H24 120.8 . . ? C23 C24 H24 120.8 . . ? C24 C25 C26 122.9(7) . . ? C24 C25 H25 118.6 . . ? C26 C25 H25 118.6 . . ? C21 C26 C25 119.3(6) . . ? C21 C26 H26 120.3 . . ? C25 C26 H26 120.3 . . ? C36 C31 C32 117.8(6) . . ? C36 C31 P 116.9(5) . . ? C32 C31 P 125.3(5) . . ? C33 C32 C31 121.6(6) . . ? C33 C32 H32 119.2 . . ? C31 C32 H32 119.2 . . ? C34 C33 C32 119.5(6) . . ? C34 C33 H33 120.2 . . ? C32 C33 H33 120.2 . . ? C33 C34 C35 120.0(7) . . ? C33 C34 H34 120.0 . . ? C35 C34 H34 120.0 . . ? C36 C35 C34 119.8(7) . . ? C36 C35 H35 120.1 . . ? C34 C35 H35 120.1 . . ? C35 C36 C31 121.2(7) . . ? C35 C36 H36 119.4 . . ? C31 C36 H36 119.4 . . ? C4 N C5 111.9(6) . . ? C4 N C17 113.4(6) . . ? C5 N C17 116.3(6) . . ? N C4 H4A 109.5 . . ? N C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N C5 H5A 109.5 . . ? N C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.10 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.469 _refine_diff_density_min -0.269 _refine_diff_density_rms 0.064 #===END data_6a _chemical_name_systematic ; compound code (S,Rp)-6a.benzene ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H34 Cr O3 P2' _chemical_formula_weight 700.63 _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' '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' 'Cr' 'Cr' 0.3209 0.6236 '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) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 10.7821(17) _cell_length_b 13.220(7) _cell_length_c 12.5118(18) _cell_angle_alpha 90.00 _cell_angle_beta 100.691(12) _cell_angle_gamma 90.00 _cell_volume 1752.4(10) _cell_formula_units_Z 2 _cell_measurement_temperature 228(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10 _cell_measurement_theta_max 13 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.64 _exptl_crystal_size_mid 0.48 _exptl_crystal_size_min 0.44 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.328 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 728 _exptl_absorpt_coefficient_mu 0.457 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7587 _exptl_absorpt_correction_T_max 0.8243 _exptl_absorpt_process_details 'PSI scans' _exptl_special_details ; ? ; _diffrn_ambient_temperature 228(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 Enraf_Nonius_CAD4 _diffrn_measurement_method \q/2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 2.24 _diffrn_reflns_number 7476 _diffrn_reflns_av_R_equivalents 0.0999 _diffrn_reflns_av_sigmaI/netI 0.1682 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 25.10 _reflns_number_total 6225 _reflns_number_gt 3754 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 (Enraf-Nonius, 1977)' _computing_cell_refinement 'CAD4 (Enraf-Nonius, 1977)' _computing_data_reduction 'PROCESS_MolEN (Fair, 1990)' _computing_structure_solution 'SHELXTL (Sheldrick, 1998)' _computing_structure_refinement 'SHELXTL (Sheldrick, 1998)' _computing_molecular_graphics 'Platon (Spek, 2003)' _computing_publication_material ? _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^)+(0.1400P)^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 0.00(6) _refine_ls_number_reflns 6225 _refine_ls_number_parameters 391 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1656 _refine_ls_R_factor_gt 0.1000 _refine_ls_wR_factor_ref 0.2592 _refine_ls_wR_factor_gt 0.2259 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.007 _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 Cr Cr 0.60320(13) 0.20386(12) 0.23650(11) 0.0304(4) Uani 1 1 d . . . P1 P 0.7932(2) 0.0170(2) 0.4179(2) 0.0341(7) Uani 1 1 d . . . P2 P 0.5405(2) -0.1450(2) 0.35144(19) 0.0321(6) Uani 1 1 d . . . O1 O 0.8217(8) 0.3477(7) 0.2665(7) 0.065(2) Uani 1 1 d . . . O2 O 0.4678(9) 0.3452(7) 0.0678(6) 0.063(2) Uani 1 1 d . . . O3 O 0.7096(8) 0.0875(7) 0.0693(7) 0.065(2) Uani 1 1 d . . . C1 C 0.7402(10) 0.2893(9) 0.2565(8) 0.041(3) Uani 1 1 d . . . C2 C 0.5209(10) 0.2906(8) 0.1321(8) 0.036(2) Uani 1 1 d . . . C3 C 0.6713(10) 0.1342(8) 0.1329(8) 0.036(2) Uani 1 1 d . . . C11 C 0.6508(8) 0.0939(7) 0.3730(7) 0.027(2) Uani 1 1 d . . . C12 C 0.5510(8) 0.0552(7) 0.2947(7) 0.028(2) Uani 1 1 d . . . C13 C 0.4382(9) 0.1105(8) 0.2601(7) 0.030(2) Uani 1 1 d . . . C14 C 0.4261(8) 0.2063(9) 0.3000(6) 0.033(2) Uani 1 1 d . . . H14 H 0.3516 0.2428 0.2749 0.043 Uiso 1 1 d R . . C15 C 0.5251(10) 0.2478(9) 0.3786(8) 0.040(3) Uani 1 1 d . . . H15 H 0.5163 0.3131 0.4061 0.052 Uiso 1 1 d R . . C16 C 0.6372(9) 0.1924(9) 0.4146(7) 0.035(2) Uani 1 1 d . . . H16 H 0.7028 0.2189 0.4672 0.046 Uiso 1 1 d R . . C17 C 0.5430(9) -0.0465(8) 0.2437(7) 0.031(2) Uani 1 1 d . . . H17 H 0.6193 -0.0570 0.2116 0.040 Uiso 1 1 d R . . C18 C 0.4255(10) -0.0372(8) 0.1486(8) 0.037(2) Uani 1 1 d . . . H18A H 0.4536 -0.0212 0.0804 0.047 Uiso 1 1 d R . . H18B H 0.3763 -0.0999 0.1387 0.047 Uiso 1 1 d R . . C19 C 0.3472(9) 0.0513(8) 0.1794(7) 0.032(2) Uani 1 1 d . . . H19A H 0.3111 0.0928 0.1164 0.042 Uiso 1 1 d R . . H19B H 0.2787 0.0255 0.2135 0.042 Uiso 1 1 d R . . C21 C 0.7924(10) 0.0075(9) 0.5641(8) 0.037(2) Uani 1 1 d . . . C22 C 0.9015(11) -0.0226(11) 0.6336(9) 0.054(3) Uani 1 1 d . . . H22 H 0.9757 -0.0324 0.6057 0.070 Uiso 1 1 d R . . C23 C 0.9052(11) -0.0400(12) 0.7424(9) 0.065(4) Uani 1 1 d . . . H23 H 0.9806 -0.0598 0.7881 0.085 Uiso 1 1 d R . . C24 C 0.7928(13) -0.0294(12) 0.7841(9) 0.067(4) Uani 1 1 d . . . H24 H 0.7936 -0.0426 0.8581 0.087 Uiso 1 1 d R . . C25 C 0.6833(11) -0.0020(11) 0.7159(8) 0.056(3) Uani 1 1 d . . . H25 H 0.6079 0.0048 0.7429 0.073 Uiso 1 1 d R . . C26 C 0.6829(10) 0.0183(9) 0.6079(9) 0.041(3) Uani 1 1 d . . . H26 H 0.6072 0.0370 0.5620 0.054 Uiso 1 1 d R . . C31 C 0.9230(9) 0.1058(8) 0.4119(8) 0.037(3) Uani 1 1 d . . . C32 C 0.9704(10) 0.1083(10) 0.3148(10) 0.054(3) Uani 1 1 d . . . H32 H 0.9359 0.0664 0.2560 0.070 Uiso 1 1 d R . . C33 C 1.0674(12) 0.1706(11) 0.3078(12) 0.068(4) Uani 1 1 d . . . H33 H 1.0934 0.1757 0.2403 0.089 Uiso 1 1 d R . . C34 C 1.1282(12) 0.2294(11) 0.3930(14) 0.077(5) Uani 1 1 d . . . H34 H 1.1978 0.2702 0.3864 0.100 Uiso 1 1 d R . . C35 C 1.0831(11) 0.2255(13) 0.4882(13) 0.076(5) Uani 1 1 d . . . H35 H 1.1233 0.2627 0.5489 0.098 Uiso 1 1 d R . . C36 C 0.9818(10) 0.1646(9) 0.4981(10) 0.055(3) Uani 1 1 d . . . H36 H 0.9506 0.1649 0.5635 0.071 Uiso 1 1 d R . . C41 C 0.5705(9) -0.2614(9) 0.2836(8) 0.041(3) Uani 1 1 d . . . C42 C 0.6238(11) -0.3421(9) 0.3461(9) 0.048(3) Uani 1 1 d . . . H42 H 0.6419 -0.3363 0.4223 0.062 Uiso 1 1 d R . . C43 C 0.6559(12) -0.4304(9) 0.3020(10) 0.057(3) Uani 1 1 d . . . H43 H 0.6885 -0.4843 0.3477 0.074 Uiso 1 1 d R . . C44 C 0.6375(11) -0.4419(9) 0.1911(9) 0.051(3) Uani 1 1 d . . . H44 H 0.6602 -0.5025 0.1604 0.066 Uiso 1 1 d R . . C45 C 0.5841(12) -0.3654(10) 0.1273(9) 0.053(3) Uani 1 1 d . . . H45 H 0.5686 -0.3734 0.0513 0.069 Uiso 1 1 d R . . C46 C 0.5525(12) -0.2746(9) 0.1706(8) 0.054(3) Uani 1 1 d . . . H46 H 0.5209 -0.2213 0.1236 0.070 Uiso 1 1 d R . . C51 C 0.3704(9) -0.1478(7) 0.3549(7) 0.029(2) Uani 1 1 d . . . C52 C 0.3292(11) -0.0744(9) 0.4200(8) 0.045(3) Uani 1 1 d . . . H52 H 0.3875 -0.0302 0.4613 0.059 Uiso 1 1 d R . . C53 C 0.2026(12) -0.0677(10) 0.4224(9) 0.048(3) Uani 1 1 d . . . H53 H 0.1734 -0.0181 0.4656 0.063 Uiso 1 1 d R . . C54 C 0.1159(11) -0.1307(11) 0.3613(10) 0.057(4) Uani 1 1 d . . . H54 H 0.0291 -0.1238 0.3613 0.074 Uiso 1 1 d R . . C55 C 0.1575(11) -0.2044(11) 0.3010(10) 0.054(3) Uani 1 1 d . . . H55 H 0.0986 -0.2506 0.2637 0.071 Uiso 1 1 d R . . C56 C 0.2860(9) -0.2126(8) 0.2972(7) 0.034(2) Uani 1 1 d . . . H56 H 0.3133 -0.2627 0.2536 0.045 Uiso 1 1 d R . . C61 C 0.0286(14) 0.7020(8) 0.0193(11) 0.122(6) Uiso 1 1 d G . . H61 H 0.0588 0.6377 0.0047 0.158 Uiso 1 1 calc R . . C62 C -0.0835(14) 0.7109(10) 0.0583(11) 0.161(9) Uiso 1 1 d G . . H62 H -0.1291 0.6526 0.0701 0.210 Uiso 1 1 calc R . . C63 C -0.1282(11) 0.8059(13) 0.0799(10) 0.128(7) Uiso 1 1 d G . . H63 H -0.2040 0.8120 0.1063 0.167 Uiso 1 1 calc R . . C64 C -0.0607(13) 0.8921(9) 0.0626(10) 0.106(6) Uiso 1 1 d G . . H64 H -0.0909 0.9564 0.0772 0.138 Uiso 1 1 calc R . . C65 C 0.0514(12) 0.8832(9) 0.0236(10) 0.107(6) Uiso 1 1 d G . . H65 H 0.0971 0.9414 0.0118 0.140 Uiso 1 1 calc R . . C66 C 0.0961(10) 0.7881(12) 0.0019(10) 0.118(7) Uiso 1 1 d G . . H66 H 0.1719 0.7821 -0.0244 0.153 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 Cr 0.0248(8) 0.0363(9) 0.0327(8) -0.0003(8) 0.0120(6) -0.0009(8) P1 0.0259(14) 0.0437(17) 0.0328(13) -0.0016(12) 0.0060(11) 0.0061(13) P2 0.0336(14) 0.0365(15) 0.0265(12) 0.0047(11) 0.0059(10) 0.0002(13) O1 0.039(5) 0.059(6) 0.096(7) 0.004(5) 0.012(4) -0.011(5) O2 0.075(6) 0.072(6) 0.045(4) 0.015(5) 0.016(4) 0.012(5) O3 0.065(6) 0.073(6) 0.067(5) -0.012(5) 0.042(5) 0.005(5) C1 0.032(6) 0.050(7) 0.043(6) -0.003(5) 0.008(5) -0.006(6) C2 0.040(6) 0.034(6) 0.036(5) -0.005(5) 0.015(5) -0.004(5) C3 0.031(6) 0.036(6) 0.045(6) 0.005(5) 0.013(5) -0.004(5) C11 0.019(5) 0.033(6) 0.029(5) 0.002(4) 0.009(4) 0.000(4) C12 0.022(5) 0.030(6) 0.033(5) 0.014(4) 0.008(4) 0.005(4) C13 0.027(5) 0.038(6) 0.029(5) 0.001(5) 0.010(4) -0.009(5) C14 0.030(5) 0.043(6) 0.029(4) 0.012(5) 0.016(4) 0.012(6) C15 0.038(6) 0.048(6) 0.038(6) -0.005(5) 0.021(5) -0.004(5) C16 0.034(5) 0.046(6) 0.025(4) -0.006(5) 0.002(4) -0.006(6) C17 0.023(5) 0.040(6) 0.030(5) -0.004(4) 0.005(4) 0.000(5) C18 0.045(6) 0.033(6) 0.030(5) 0.005(4) 0.001(5) -0.006(5) C19 0.022(5) 0.038(6) 0.036(5) 0.009(5) 0.005(4) 0.002(5) C21 0.039(6) 0.044(6) 0.032(5) 0.001(5) 0.015(4) 0.009(5) C22 0.029(6) 0.087(10) 0.040(6) 0.005(6) -0.006(5) 0.008(6) C23 0.038(7) 0.115(12) 0.038(6) 0.005(7) -0.005(5) 0.036(8) C24 0.076(10) 0.090(10) 0.034(6) 0.015(6) 0.010(6) 0.028(8) C25 0.044(7) 0.093(10) 0.035(6) 0.013(6) 0.016(5) -0.005(7) C26 0.028(6) 0.049(7) 0.047(6) 0.007(5) 0.008(5) 0.014(5) C31 0.015(5) 0.048(7) 0.050(6) -0.007(5) 0.008(4) -0.001(5) C32 0.027(6) 0.074(9) 0.065(7) 0.008(7) 0.021(5) 0.014(6) C33 0.039(7) 0.079(11) 0.097(10) 0.004(8) 0.037(7) 0.013(7) C34 0.030(7) 0.066(11) 0.147(14) -0.020(10) 0.049(8) -0.006(7) C35 0.031(6) 0.092(13) 0.110(11) -0.018(10) 0.030(7) -0.008(7) C36 0.027(6) 0.064(8) 0.079(8) -0.025(6) 0.025(6) -0.003(6) C41 0.022(5) 0.063(8) 0.041(6) 0.005(5) 0.015(4) -0.007(5) C42 0.050(7) 0.054(7) 0.039(6) 0.000(5) 0.005(5) 0.007(6) C43 0.070(9) 0.037(7) 0.062(8) 0.017(6) 0.012(6) 0.010(6) C44 0.053(8) 0.042(7) 0.057(7) -0.002(6) 0.009(6) 0.017(6) C45 0.062(8) 0.057(8) 0.042(6) -0.007(6) 0.011(6) 0.001(7) C46 0.081(9) 0.048(8) 0.031(5) -0.004(5) 0.007(5) 0.021(7) C51 0.038(5) 0.025(5) 0.024(4) 0.001(4) 0.008(4) -0.007(5) C52 0.050(7) 0.052(8) 0.036(5) 0.003(5) 0.016(5) -0.004(6) C53 0.050(7) 0.063(8) 0.035(6) 0.002(6) 0.017(5) 0.004(6) C54 0.036(7) 0.081(10) 0.058(7) 0.018(7) 0.016(6) 0.016(7) C55 0.030(6) 0.072(9) 0.058(7) 0.014(7) 0.000(5) -0.007(6) C56 0.036(6) 0.038(6) 0.032(5) 0.002(4) 0.013(4) 0.002(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 Cr C2 1.838(11) . ? Cr C1 1.840(11) . ? Cr C3 1.849(11) . ? Cr C15 2.182(10) . ? Cr C16 2.195(8) . ? Cr C14 2.200(8) . ? Cr C12 2.206(9) . ? Cr C13 2.229(9) . ? Cr C11 2.229(9) . ? P1 C21 1.836(10) . ? P1 C11 1.840(10) . ? P1 C31 1.839(10) . ? P2 C41 1.816(11) . ? P2 C51 1.843(10) . ? P2 C17 1.878(10) . ? O1 C1 1.158(13) . ? O2 C2 1.152(12) . ? O3 C3 1.143(12) . ? C11 C12 1.411(12) . ? C11 C16 1.420(14) . ? C12 C13 1.416(13) . ? C12 C17 1.483(14) . ? C13 C14 1.375(15) . ? C13 C19 1.492(13) . ? C14 C15 1.421(14) . ? C14 H14 0.9401 . ? C15 C16 1.414(14) . ? C15 H15 0.9400 . ? C16 H16 0.9399 . ? C17 C18 1.575(13) . ? C17 H17 0.9901 . ? C18 C19 1.533(14) . ? C18 H18A 0.9801 . ? C18 H18B 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9801 . ? C21 C22 1.385(14) . ? C21 C26 1.398(14) . ? C22 C23 1.374(16) . ? C22 H22 0.9400 . ? C23 C24 1.413(17) . ? C23 H23 0.9400 . ? C24 C25 1.371(16) . ? C24 H24 0.9400 . ? C25 C26 1.377(14) . ? C25 H25 0.9400 . ? C26 H26 0.9399 . ? C31 C36 1.384(15) . ? C31 C32 1.404(15) . ? C32 C33 1.347(17) . ? C32 H32 0.9400 . ? C33 C34 1.383(19) . ? C33 H33 0.9399 . ? C34 C35 1.368(19) . ? C34 H34 0.9400 . ? C35 C36 1.380(17) . ? C35 H35 0.9401 . ? C36 H36 0.9400 . ? C41 C42 1.382(15) . ? C41 C46 1.401(14) . ? C42 C43 1.364(16) . ? C42 H42 0.9400 . ? C43 C44 1.373(16) . ? C43 H43 0.9400 . ? C44 C45 1.349(16) . ? C44 H44 0.9401 . ? C45 C46 1.386(16) . ? C45 H45 0.9399 . ? C46 H46 0.9400 . ? C51 C56 1.355(13) . ? C51 C52 1.392(14) . ? C52 C53 1.374(16) . ? C52 H52 0.9400 . ? C53 C54 1.374(18) . ? C53 H53 0.9399 . ? C54 C55 1.359(18) . ? C54 H54 0.9401 . ? C55 C56 1.399(14) . ? C55 H55 0.9401 . ? C56 H56 0.9400 . ? C61 C62 1.3900 . ? C61 C66 1.3900 . ? C61 H61 0.9400 . ? C62 C63 1.3900 . ? C62 H62 0.9400 . ? C63 C64 1.3900 . ? C63 H63 0.9400 . ? C64 C65 1.3900 . ? C64 H64 0.9400 . ? C65 C66 1.3900 . ? C65 H65 0.9400 . ? C66 H66 0.9400 . ? 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 C2 Cr C1 89.1(5) . . ? C2 Cr C3 90.9(4) . . ? C1 Cr C3 89.3(5) . . ? C2 Cr C15 101.8(4) . . ? C1 Cr C15 98.5(4) . . ? C3 Cr C15 165.2(4) . . ? C2 Cr C16 137.1(4) . . ? C1 Cr C16 85.7(4) . . ? C3 Cr C16 131.6(4) . . ? C15 Cr C16 37.7(4) . . ? C2 Cr C14 84.9(4) . . ? C1 Cr C14 132.1(5) . . ? C3 Cr C14 138.1(4) . . ? C15 Cr C14 37.8(4) . . ? C16 Cr C14 68.1(3) . . ? C2 Cr C12 132.2(4) . . ? C1 Cr C12 138.6(4) . . ? C3 Cr C12 86.9(4) . . ? C15 Cr C12 78.9(4) . . ? C16 Cr C12 66.9(4) . . ? C14 Cr C12 66.5(4) . . ? C2 Cr C13 98.5(4) . . ? C1 Cr C13 164.2(4) . . ? C3 Cr C13 104.3(4) . . ? C15 Cr C13 66.5(4) . . ? C16 Cr C13 79.3(4) . . ? C14 Cr C13 36.2(4) . . ? C12 Cr C13 37.2(3) . . ? C2 Cr C11 164.5(4) . . ? C1 Cr C11 103.4(4) . . ? C3 Cr C11 98.5(4) . . ? C15 Cr C11 67.6(4) . . ? C16 Cr C11 37.4(4) . . ? C14 Cr C11 79.9(3) . . ? C12 Cr C11 37.1(3) . . ? C13 Cr C11 67.3(3) . . ? C21 P1 C11 100.6(4) . . ? C21 P1 C31 103.2(5) . . ? C11 P1 C31 103.5(5) . . ? C41 P2 C51 104.9(4) . . ? C41 P2 C17 103.0(4) . . ? C51 P2 C17 100.2(4) . . ? O1 C1 Cr 175.9(10) . . ? O2 C2 Cr 178.8(9) . . ? O3 C3 Cr 176.8(9) . . ? C12 C11 C16 118.0(8) . . ? C12 C11 P1 119.8(7) . . ? C16 C11 P1 122.2(7) . . ? C12 C11 Cr 70.5(5) . . ? C16 C11 Cr 70.0(5) . . ? P1 C11 Cr 130.9(4) . . ? C11 C12 C13 121.7(9) . . ? C11 C12 C17 127.1(8) . . ? C13 C12 C17 111.0(8) . . ? C11 C12 Cr 72.4(5) . . ? C13 C12 Cr 72.3(5) . . ? C17 C12 Cr 131.5(6) . . ? C14 C13 C12 119.9(8) . . ? C14 C13 C19 129.3(9) . . ? C12 C13 C19 110.8(9) . . ? C14 C13 Cr 70.8(5) . . ? C12 C13 Cr 70.5(5) . . ? C19 C13 Cr 129.9(6) . . ? C13 C14 C15 119.8(9) . . ? C13 C14 Cr 73.1(5) . . ? C15 C14 Cr 70.4(5) . . ? C13 C14 H14 118.9 . . ? C15 C14 H14 121.2 . . ? Cr C14 H14 129.2 . . ? C16 C15 C14 120.5(10) . . ? C16 C15 Cr 71.6(5) . . ? C14 C15 Cr 71.8(5) . . ? C16 C15 H15 119.9 . . ? C14 C15 H15 119.6 . . ? Cr C15 H15 128.6 . . ? C15 C16 C11 119.9(9) . . ? C15 C16 Cr 70.7(5) . . ? C11 C16 Cr 72.6(5) . . ? C15 C16 H16 121.1 . . ? C11 C16 H16 118.9 . . ? Cr C16 H16 130.4 . . ? C12 C17 C18 103.2(8) . . ? C12 C17 P2 109.1(6) . . ? C18 C17 P2 118.7(7) . . ? C12 C17 H17 108.4 . . ? C18 C17 H17 108.5 . . ? P2 C17 H17 108.5 . . ? C19 C18 C17 105.8(8) . . ? C19 C18 H18A 109.2 . . ? C17 C18 H18A 109.8 . . ? C19 C18 H18B 111.5 . . ? C17 C18 H18B 111.7 . . ? H18A C18 H18B 108.8 . . ? C13 C19 C18 104.3(8) . . ? C13 C19 H19A 111.4 . . ? C18 C19 H19A 112.3 . . ? C13 C19 H19B 110.0 . . ? C18 C19 H19B 109.7 . . ? H19A C19 H19B 109.0 . . ? C22 C21 C26 117.6(10) . . ? C22 C21 P1 119.0(8) . . ? C26 C21 P1 123.0(8) . . ? C23 C22 C21 122.4(11) . . ? C23 C22 H22 118.4 . . ? C21 C22 H22 119.3 . . ? C22 C23 C24 118.7(10) . . ? C22 C23 H23 120.8 . . ? C24 C23 H23 120.5 . . ? C25 C24 C23 119.7(10) . . ? C25 C24 H24 120.8 . . ? C23 C24 H24 119.5 . . ? C24 C25 C26 120.5(11) . . ? C24 C25 H25 120.2 . . ? C26 C25 H25 119.2 . . ? C25 C26 C21 121.1(10) . . ? C25 C26 H26 119.7 . . ? C21 C26 H26 119.2 . . ? C36 C31 C32 118.3(10) . . ? C36 C31 P1 124.7(8) . . ? C32 C31 P1 116.8(8) . . ? C33 C32 C31 118.8(13) . . ? C33 C32 H32 120.6 . . ? C31 C32 H32 120.6 . . ? C32 C33 C34 123.8(13) . . ? C32 C33 H33 117.8 . . ? C34 C33 H33 118.3 . . ? C35 C34 C33 117.1(12) . . ? C35 C34 H34 121.1 . . ? C33 C34 H34 121.8 . . ? C34 C35 C36 121.0(14) . . ? C34 C35 H35 119.9 . . ? C36 C35 H35 119.0 . . ? C35 C36 C31 120.8(11) . . ? C35 C36 H36 119.5 . . ? C31 C36 H36 119.6 . . ? C42 C41 C46 116.1(10) . . ? C42 C41 P2 118.7(8) . . ? C46 C41 P2 125.0(9) . . ? C43 C42 C41 122.8(10) . . ? C43 C42 H42 117.3 . . ? C41 C42 H42 119.8 . . ? C42 C43 C44 120.2(11) . . ? C42 C43 H43 119.9 . . ? C44 C43 H43 119.9 . . ? C45 C44 C43 118.8(11) . . ? C45 C44 H44 120.7 . . ? C43 C44 H44 120.5 . . ? C44 C45 C46 121.8(10) . . ? C44 C45 H45 119.4 . . ? C46 C45 H45 118.9 . . ? C45 C46 C41 120.3(11) . . ? C45 C46 H46 119.4 . . ? C41 C46 H46 120.3 . . ? C56 C51 C52 119.8(9) . . ? C56 C51 P2 125.0(8) . . ? C52 C51 P2 115.2(8) . . ? C53 C52 C51 119.0(11) . . ? C53 C52 H52 120.9 . . ? C51 C52 H52 120.2 . . ? C54 C53 C52 121.7(12) . . ? C54 C53 H53 118.5 . . ? C52 C53 H53 119.9 . . ? C55 C54 C53 118.9(11) . . ? C55 C54 H54 120.0 . . ? C53 C54 H54 121.1 . . ? C54 C55 C56 120.3(12) . . ? C54 C55 H55 118.6 . . ? C56 C55 H55 121.0 . . ? C51 C56 C55 120.3(10) . . ? C51 C56 H56 120.2 . . ? C55 C56 H56 119.5 . . ? C62 C61 C66 120.0 . . ? C62 C61 H61 120.0 . . ? C66 C61 H61 120.0 . . ? C63 C62 C61 120.0 . . ? C63 C62 H62 120.0 . . ? C61 C62 H62 120.0 . . ? C62 C63 C64 120.0 . . ? C62 C63 H63 120.0 . . ? C64 C63 H63 120.0 . . ? C65 C64 C63 120.0 . . ? C65 C64 H64 120.0 . . ? C63 C64 H64 120.0 . . ? C64 C65 C66 120.0 . . ? C64 C65 H65 120.0 . . ? C66 C65 H65 120.0 . . ? C65 C66 C61 120.0 . . ? C65 C66 H66 120.0 . . ? C61 C66 H66 120.0 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.10 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.013 _refine_diff_density_min -0.604 _refine_diff_density_rms 0.126