# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'P G Edwards' _publ_contact_author_email EDWARDSPG@CARDIFF.AC.UK _publ_section_title ; Synthesis of (1R,4S,6R)-5,5,6-trimethyl-2-phosphabicyclo[2.2.2]octane and derivatives ; loop_ _publ_author_name 'P G Edwards' 'James C. Knight' 'Paul Newman' # Attachment 'compound9.cif' data_compound9 _database_code_depnum_ccdc_archive 'CCDC 756173' #TrackingRef 'compound9.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common pge0506 _chemical_melting_point ? _chemical_formula_moiety 'C12 H24 P, I' _chemical_formula_sum 'C12 H24 I P' _chemical_formula_weight 326.18 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' 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 7.1710(2) _cell_length_b 10.4460(3) _cell_length_c 18.5870(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1392.32(7) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6068 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.485 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.556 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 656 _exptl_absorpt_coefficient_mu 2.382 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4136 _exptl_absorpt_correction_T_max 0.5551 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7691 _diffrn_reflns_av_R_equivalents 0.0848 _diffrn_reflns_av_sigmaI/netI 0.0598 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 27.50 _reflns_number_total 3068 _reflns_number_gt 2955 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'Sir-92 (A. Altomare et al., 1992)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0392P)^2^+1.1036P] 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 -0.09(3) _refine_ls_number_reflns 3068 _refine_ls_number_parameters 132 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0348 _refine_ls_R_factor_gt 0.0317 _refine_ls_wR_factor_ref 0.0836 _refine_ls_wR_factor_gt 0.0823 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _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 C9 C 0.7758(7) 1.0552(4) 0.2703(2) 0.0223(9) Uani 1 1 d . . . H1A H 0.6658 1.0535 0.3016 0.033 Uiso 1 1 calc R . . H1B H 0.7718 1.1318 0.2399 0.033 Uiso 1 1 calc R . . H1C H 0.8889 1.0571 0.2999 0.033 Uiso 1 1 calc R . . C2 C 0.7749(8) 0.7779(4) 0.2722(2) 0.0235(9) Uani 1 1 d . . . H2A H 0.8836 0.7800 0.3041 0.035 Uiso 1 1 calc R . . H2B H 0.7787 0.7000 0.2428 0.035 Uiso 1 1 calc R . . H2C H 0.6606 0.7783 0.3011 0.035 Uiso 1 1 calc R . . C3 C 0.9743(6) 0.9149(5) 0.15296(18) 0.0216(8) Uani 1 1 d . . . H3A H 1.0369 0.9993 0.1535 0.026 Uiso 1 1 calc R . . H3B H 1.0660 0.8490 0.1676 0.026 Uiso 1 1 calc R . . C4 C 0.8995(6) 0.8851(4) 0.0762(2) 0.0186(8) Uani 1 1 d . . . H4 H 1.0088 0.8715 0.0437 0.022 Uiso 1 1 calc R . . C8 C 0.7863(7) 0.7604(4) 0.0787(2) 0.0227(9) Uani 1 1 d . . . H5A H 0.8542 0.6960 0.1078 0.027 Uiso 1 1 calc R . . H5B H 0.7721 0.7261 0.0294 0.027 Uiso 1 1 calc R . . C7 C 0.5907(7) 0.7839(4) 0.1121(2) 0.0208(9) Uani 1 1 d . . . H6A H 0.4954 0.7836 0.0735 0.025 Uiso 1 1 calc R . . H6B H 0.5608 0.7140 0.1461 0.025 Uiso 1 1 calc R . . C1 C 0.5851(5) 0.9123(4) 0.15170(18) 0.0161(7) Uani 1 1 d . . . H7 H 0.4639 0.9223 0.1777 0.019 Uiso 1 1 calc R . . C5 C 0.7801(7) 0.9965(4) 0.0450(2) 0.0210(8) Uani 1 1 d . . . C6 C 0.6154(6) 1.0263(4) 0.0988(2) 0.0181(8) Uani 1 1 d . . . H9 H 0.6544 1.1017 0.1284 0.022 Uiso 1 1 calc R . . C10 C 0.4299(7) 1.0611(5) 0.0629(2) 0.0287(10) Uani 1 1 d . . . H10A H 0.3774 0.9850 0.0396 0.043 Uiso 1 1 calc R . . H10B H 0.4510 1.1279 0.0268 0.043 Uiso 1 1 calc R . . H10C H 0.3426 1.0927 0.0994 0.043 Uiso 1 1 calc R . . C11 C 0.7136(7) 0.9570(4) -0.0305(2) 0.0274(10) Uani 1 1 d . . . H11A H 0.8219 0.9385 -0.0609 0.041 Uiso 1 1 calc R . . H11B H 0.6411 1.0269 -0.0518 0.041 Uiso 1 1 calc R . . H11C H 0.6354 0.8803 -0.0268 0.041 Uiso 1 1 calc R . . C12 C 0.8956(8) 1.1187(4) 0.0351(3) 0.0311(11) Uani 1 1 d . . . H12A H 0.9986 1.1018 0.0017 0.047 Uiso 1 1 calc R . . H12B H 0.9459 1.1458 0.0817 0.047 Uiso 1 1 calc R . . H12C H 0.8161 1.1866 0.0155 0.047 Uiso 1 1 calc R . . P1 P 0.77785(13) 0.91534(9) 0.21484(4) 0.01518(19) Uani 1 1 d . . . I1 I 0.72753(4) 1.41530(2) 0.169366(13) 0.02099(9) 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 C9 0.026(2) 0.0217(19) 0.0191(17) -0.0049(14) 0.0012(17) 0.001(2) C2 0.028(3) 0.0240(19) 0.0184(17) 0.0053(14) -0.0009(18) -0.001(2) C3 0.0175(19) 0.030(2) 0.0173(18) 0.001(2) 0.0034(13) -0.002(2) C4 0.020(2) 0.020(2) 0.0157(17) 0.0021(14) 0.0037(14) 0.0022(17) C8 0.030(2) 0.0146(17) 0.0234(18) -0.0021(15) 0.0019(17) 0.006(2) C7 0.023(2) 0.020(2) 0.0192(19) -0.0015(15) -0.0035(16) -0.0049(18) C1 0.0196(19) 0.0140(16) 0.0148(16) 0.0021(17) -0.0003(12) 0.002(2) C5 0.027(2) 0.0199(17) 0.0159(17) 0.0017(14) 0.0034(17) 0.0026(19) C6 0.020(2) 0.0151(17) 0.0190(18) -0.0001(15) 0.0007(16) 0.0042(17) C10 0.028(2) 0.031(3) 0.027(2) 0.0066(18) -0.0038(18) 0.012(2) C11 0.034(3) 0.033(2) 0.0146(17) 0.0011(15) -0.0013(17) 0.009(2) C12 0.039(3) 0.024(2) 0.030(2) 0.0070(18) 0.016(2) -0.002(2) P1 0.0168(5) 0.0166(4) 0.0122(4) 0.0010(3) 0.0007(3) -0.0005(6) I1 0.02092(14) 0.02021(14) 0.02185(13) 0.00050(10) 0.00082(9) 0.00052(11) _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 C9 P1 1.789(4) . ? C9 H1A 0.9800 . ? C9 H1B 0.9800 . ? C9 H1C 0.9800 . ? C2 P1 1.789(4) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.556(5) . ? C3 P1 1.819(4) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C8 1.536(6) . ? C4 C5 1.556(6) . ? C4 H4 1.0000 . ? C8 C7 1.553(6) . ? C8 H5A 0.9900 . ? C8 H5B 0.9900 . ? C7 C1 1.530(6) . ? C7 H6A 0.9900 . ? C7 H6B 0.9900 . ? C1 C6 1.559(5) . ? C1 P1 1.814(4) . ? C1 H7 1.0000 . ? C5 C12 1.533(6) . ? C5 C11 1.538(5) . ? C5 C6 1.579(6) . ? C6 C10 1.532(6) . ? C6 H9 1.0000 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 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 P1 C9 H1A 109.5 . . ? P1 C9 H1B 109.5 . . ? H1A C9 H1B 109.5 . . ? P1 C9 H1C 109.5 . . ? H1A C9 H1C 109.5 . . ? H1B C9 H1C 109.5 . . ? P1 C2 H2A 109.5 . . ? P1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? P1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 P1 108.3(3) . . ? C4 C3 H3A 110.0 . . ? P1 C3 H3A 110.0 . . ? C4 C3 H3B 110.0 . . ? P1 C3 H3B 110.0 . . ? H3A C3 H3B 108.4 . . ? C8 C4 C3 108.8(3) . . ? C8 C4 C5 110.8(4) . . ? C3 C4 C5 112.5(3) . . ? C8 C4 H4 108.2 . . ? C3 C4 H4 108.2 . . ? C5 C4 H4 108.2 . . ? C4 C8 C7 110.8(3) . . ? C4 C8 H5A 109.5 . . ? C7 C8 H5A 109.5 . . ? C4 C8 H5B 109.5 . . ? C7 C8 H5B 109.5 . . ? H5A C8 H5B 108.1 . . ? C1 C7 C8 110.8(3) . . ? C1 C7 H6A 109.5 . . ? C8 C7 H6A 109.5 . . ? C1 C7 H6B 109.5 . . ? C8 C7 H6B 109.5 . . ? H6A C7 H6B 108.1 . . ? C7 C1 C6 111.2(3) . . ? C7 C1 P1 107.9(3) . . ? C6 C1 P1 106.7(3) . . ? C7 C1 H7 110.3 . . ? C6 C1 H7 110.3 . . ? P1 C1 H7 110.3 . . ? C12 C5 C11 106.3(3) . . ? C12 C5 C4 111.7(4) . . ? C11 C5 C4 108.1(3) . . ? C12 C5 C6 108.4(3) . . ? C11 C5 C6 113.5(4) . . ? C4 C5 C6 108.8(3) . . ? C10 C6 C1 109.5(4) . . ? C10 C6 C5 114.9(3) . . ? C1 C6 C5 110.7(3) . . ? C10 C6 H9 107.1 . . ? C1 C6 H9 107.1 . . ? C5 C6 H9 107.1 . . ? C6 C10 H10A 109.5 . . ? C6 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C6 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C5 C11 H11A 109.5 . . ? C5 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C5 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C5 C12 H12A 109.5 . . ? C5 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C5 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C2 P1 C9 108.19(18) . . ? C2 P1 C1 111.3(2) . . ? C9 P1 C1 112.4(2) . . ? C2 P1 C3 112.6(2) . . ? C9 P1 C3 111.9(2) . . ? C1 P1 C3 100.43(17) . . ? 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 P1 C3 C4 C8 -54.0(4) . . . . ? P1 C3 C4 C5 69.1(4) . . . . ? C3 C4 C8 C7 76.9(4) . . . . ? C5 C4 C8 C7 -47.3(4) . . . . ? C4 C8 C7 C1 -15.9(5) . . . . ? C8 C7 C1 C6 63.8(4) . . . . ? C8 C7 C1 P1 -53.0(4) . . . . ? C8 C4 C5 C12 -174.5(3) . . . . ? C3 C4 C5 C12 63.5(4) . . . . ? C8 C4 C5 C11 -57.8(4) . . . . ? C3 C4 C5 C11 -179.9(4) . . . . ? C8 C4 C5 C6 65.8(4) . . . . ? C3 C4 C5 C6 -56.2(5) . . . . ? C7 C1 C6 C10 83.5(4) . . . . ? P1 C1 C6 C10 -159.1(3) . . . . ? C7 C1 C6 C5 -44.2(4) . . . . ? P1 C1 C6 C5 73.2(4) . . . . ? C12 C5 C6 C10 95.7(5) . . . . ? C11 C5 C6 C10 -22.2(5) . . . . ? C4 C5 C6 C10 -142.6(4) . . . . ? C12 C5 C6 C1 -139.6(4) . . . . ? C11 C5 C6 C1 102.5(4) . . . . ? C4 C5 C6 C1 -17.9(5) . . . . ? C7 C1 P1 C2 -53.5(3) . . . . ? C6 C1 P1 C2 -173.1(3) . . . . ? C7 C1 P1 C9 -175.0(3) . . . . ? C6 C1 P1 C9 65.4(3) . . . . ? C7 C1 P1 C3 65.9(3) . . . . ? C6 C1 P1 C3 -53.7(3) . . . . ? C4 C3 P1 C2 107.4(3) . . . . ? C4 C3 P1 C9 -130.5(3) . . . . ? C4 C3 P1 C1 -11.0(3) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.506 _refine_diff_density_min -0.916 _refine_diff_density_rms 0.121 _chemical_absolute_configuration rm # Attachment 'compound14.cif' data_compound14 _database_code_depnum_ccdc_archive 'CCDC 756174' #TrackingRef 'compound14.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common pge0708 _chemical_melting_point ? _chemical_formula_moiety 'C28 H44 Cl2 P2 Pd, C2 H3 N' _chemical_formula_sum 'C30 H47 Cl2 N P2 Pd' _chemical_formula_weight 660.93 _chemical_absolute_configuration rm 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' Pd Pd -0.9988 1.0072 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' 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 7.8766(2) _cell_length_b 18.4788(4) _cell_length_c 21.4062(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3115.67(14) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 20483 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.485 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.409 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1376 _exptl_absorpt_coefficient_mu 0.890 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7286 _exptl_absorpt_correction_T_max 0.8781 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20635 _diffrn_reflns_av_R_equivalents 0.0914 _diffrn_reflns_av_sigmaI/netI 0.0980 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.91 _diffrn_reflns_theta_max 27.48 _reflns_number_total 7042 _reflns_number_gt 5599 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0294P)^2^+1.1198P] 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 -0.02(3) _refine_ls_number_reflns 7042 _refine_ls_number_parameters 332 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0747 _refine_ls_R_factor_gt 0.0500 _refine_ls_wR_factor_ref 0.0968 _refine_ls_wR_factor_gt 0.0873 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _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 C1 C 0.3933(5) 0.6462(3) 0.8274(2) 0.0199(11) Uani 1 1 d . . . H1 H 0.4885 0.6352 0.7980 0.024 Uiso 1 1 calc R . . C2 C 0.4661(6) 0.6610(3) 0.8936(2) 0.0260(11) Uani 1 1 d . . . H2 H 0.5081 0.7121 0.8934 0.031 Uiso 1 1 calc R . . C3 C 0.6197(7) 0.6134(3) 0.9062(3) 0.0436(16) Uani 1 1 d . . . H3A H 0.7077 0.6234 0.8750 0.065 Uiso 1 1 calc R . . H3B H 0.5864 0.5624 0.9036 0.065 Uiso 1 1 calc R . . H3C H 0.6642 0.6237 0.9480 0.065 Uiso 1 1 calc R . . C4 C 0.3215(6) 0.6577(3) 0.9431(2) 0.0284(13) Uani 1 1 d . . . C5 C 0.3184(8) 0.5857(3) 0.9806(3) 0.0480(17) Uani 1 1 d . . . H5A H 0.3153 0.5447 0.9515 0.072 Uiso 1 1 calc R . . H5B H 0.2174 0.5845 1.0073 0.072 Uiso 1 1 calc R . . H5C H 0.4205 0.5824 1.0066 0.072 Uiso 1 1 calc R . . C6 C 0.3489(8) 0.7182(3) 0.9916(3) 0.0432(16) Uani 1 1 d . . . H6A H 0.2588 0.7160 1.0231 0.065 Uiso 1 1 calc R . . H6B H 0.3459 0.7653 0.9706 0.065 Uiso 1 1 calc R . . H6C H 0.4594 0.7116 1.0118 0.065 Uiso 1 1 calc R . . C7 C 0.1487(5) 0.6659(3) 0.9103(2) 0.0225(11) Uani 1 1 d . . . H7 H 0.0583 0.6688 0.9430 0.027 Uiso 1 1 calc R . . C8 C 0.1108(6) 0.6009(3) 0.8681(2) 0.0255(12) Uani 1 1 d . . . H8A H 0.0139 0.6122 0.8403 0.031 Uiso 1 1 calc R . . H8B H 0.0796 0.5585 0.8940 0.031 Uiso 1 1 calc R . . C9 C 0.2688(6) 0.5828(3) 0.8283(3) 0.0254(12) Uani 1 1 d . . . H9A H 0.3258 0.5395 0.8458 0.031 Uiso 1 1 calc R . . H9B H 0.2332 0.5714 0.7851 0.031 Uiso 1 1 calc R . . C10 C 0.1407(5) 0.7351(3) 0.8705(2) 0.0170(10) Uani 1 1 d . . . H10A H 0.1699 0.7774 0.8968 0.020 Uiso 1 1 calc R . . H10B H 0.0234 0.7419 0.8549 0.020 Uiso 1 1 calc R . . C11 C 0.1945(6) 0.9335(2) 0.8711(2) 0.0190(11) Uani 1 1 d . . . H11 H 0.1895 0.8912 0.9002 0.023 Uiso 1 1 calc R . . C12 C 0.3409(6) 0.9847(2) 0.8906(2) 0.0206(11) Uani 1 1 d . . . H12 H 0.4475 0.9631 0.8734 0.025 Uiso 1 1 calc R . . C13 C 0.3620(7) 0.9860(3) 0.9618(2) 0.0323(13) Uani 1 1 d . . . H13A H 0.3912 0.9374 0.9767 0.048 Uiso 1 1 calc R . . H13B H 0.2554 1.0016 0.9812 0.048 Uiso 1 1 calc R . . H13C H 0.4527 1.0198 0.9731 0.048 Uiso 1 1 calc R . . C14 C 0.2403(7) 1.1182(3) 0.9038(2) 0.0316(13) Uani 1 1 d . . . H14A H 0.2143 1.1620 0.8800 0.047 Uiso 1 1 calc R . . H14B H 0.3198 1.1300 0.9376 0.047 Uiso 1 1 calc R . . H14C H 0.1354 1.0985 0.9217 0.047 Uiso 1 1 calc R . . C15 C 0.4960(6) 1.0898(3) 0.8425(2) 0.0311(13) Uani 1 1 d . . . H15A H 0.4844 1.1390 0.8258 0.047 Uiso 1 1 calc R . . H15B H 0.5476 1.0585 0.8108 0.047 Uiso 1 1 calc R . . H15C H 0.5682 1.0909 0.8797 0.047 Uiso 1 1 calc R . . C16 C 0.3222(6) 1.0608(3) 0.8597(2) 0.0224(11) Uani 1 1 d . . . C17 C 0.2072(6) 1.0520(2) 0.8014(2) 0.0205(11) Uani 1 1 d . . . H17 H 0.2059 1.0991 0.7784 0.025 Uiso 1 1 calc R . . C18 C 0.0232(6) 1.0344(3) 0.8218(2) 0.0249(11) Uani 1 1 d . . . H18A H -0.0299 1.0782 0.8398 0.030 Uiso 1 1 calc R . . H18B H -0.0440 1.0197 0.7848 0.030 Uiso 1 1 calc R . . C19 C 0.0216(6) 0.9729(2) 0.8706(2) 0.0230(11) Uani 1 1 d . . . H19A H -0.0016 0.9932 0.9125 0.028 Uiso 1 1 calc R . . H19B H -0.0697 0.9381 0.8604 0.028 Uiso 1 1 calc R . . C20 C 0.2711(5) 0.9925(2) 0.7563(2) 0.0203(11) Uani 1 1 d . . . H20A H 0.3920 1.0011 0.7462 0.024 Uiso 1 1 calc R . . H20B H 0.2053 0.9945 0.7169 0.024 Uiso 1 1 calc R . . C21 C 0.0555(5) 0.8648(2) 0.7557(2) 0.0192(10) Uani 1 1 d . . . H21A H 0.0100 0.8253 0.7821 0.023 Uiso 1 1 calc R . . H21B H -0.0322 0.9030 0.7526 0.023 Uiso 1 1 calc R . . C22 C 0.0948(5) 0.8359(3) 0.6916(2) 0.0210(11) Uani 1 1 d . . . C23 C 0.0769(7) 0.8797(3) 0.6396(2) 0.0347(14) Uani 1 1 d . . . H23 H 0.0376 0.9279 0.6453 0.042 Uiso 1 1 calc R . . C24 C 0.1133(9) 0.8567(3) 0.5805(3) 0.0501(18) Uani 1 1 d . . . H24 H 0.1017 0.8888 0.5461 0.060 Uiso 1 1 calc R . . C25 C 0.1672(8) 0.7863(3) 0.5709(3) 0.0445(16) Uani 1 1 d . . . H25 H 0.1922 0.7698 0.5299 0.053 Uiso 1 1 calc R . . C26 C 0.1843(7) 0.7403(3) 0.6211(2) 0.0292(12) Uani 1 1 d . . . H26 H 0.2209 0.6919 0.6144 0.035 Uiso 1 1 calc R . . C27 C 0.1488(6) 0.7635(3) 0.6817(2) 0.0221(11) Uani 1 1 d . . . C28 C 0.1580(5) 0.7094(2) 0.7348(2) 0.0179(11) Uani 1 1 d . . . H28A H 0.1999 0.6632 0.7172 0.021 Uiso 1 1 calc R . . H28B H 0.0406 0.7008 0.7495 0.021 Uiso 1 1 calc R . . C29 C 0.6272(10) 0.8355(5) 0.6104(3) 0.077(2) Uani 1 1 d . . . H29A H 0.5991 0.8732 0.6409 0.115 Uiso 1 1 calc R . . H29B H 0.7310 0.8105 0.6235 0.115 Uiso 1 1 calc R . . H29C H 0.5336 0.8007 0.6079 0.115 Uiso 1 1 calc R . . C30 C 0.6534(11) 0.8681(4) 0.5500(4) 0.064(2) Uani 1 1 d . . . P1 P 0.28832(14) 0.73059(7) 0.80347(5) 0.0161(3) Uani 1 1 d . . . P2 P 0.24735(13) 0.90233(6) 0.79205(6) 0.0161(3) Uani 1 1 d . . . Cl1 Cl 0.70061(13) 0.74439(7) 0.77331(7) 0.0317(3) Uani 1 1 d . . . Cl2 Cl 0.65031(14) 0.92156(7) 0.76524(8) 0.0385(4) Uani 1 1 d . . . Pd1 Pd 0.46757(4) 0.82456(2) 0.785747(17) 0.01724(10) Uani 1 1 d . . . N1 N 0.6827(11) 0.8954(4) 0.5038(3) 0.094(2) 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 C1 0.015(2) 0.020(3) 0.024(3) 0.001(2) -0.001(2) 0.0034(19) C2 0.022(2) 0.025(3) 0.031(3) 0.002(2) -0.010(2) 0.000(2) C3 0.034(3) 0.054(4) 0.043(4) 0.011(3) -0.011(3) 0.008(3) C4 0.036(3) 0.029(3) 0.021(3) 0.008(2) -0.007(2) 0.001(2) C5 0.052(4) 0.053(4) 0.039(4) 0.021(3) -0.011(3) 0.002(3) C6 0.045(4) 0.059(5) 0.025(3) 0.000(3) -0.007(3) -0.001(3) C7 0.022(2) 0.024(3) 0.021(3) 0.007(2) 0.0041(19) -0.001(2) C8 0.028(3) 0.018(3) 0.030(3) 0.000(2) 0.004(2) -0.003(2) C9 0.031(3) 0.011(3) 0.034(3) 0.002(2) -0.003(2) -0.002(2) C10 0.017(2) 0.018(3) 0.015(3) -0.005(2) 0.0049(19) -0.004(2) C11 0.021(2) 0.014(3) 0.021(3) 0.003(2) 0.002(2) 0.000(2) C12 0.024(3) 0.015(3) 0.022(3) -0.003(2) -0.001(2) -0.001(2) C13 0.042(3) 0.026(3) 0.029(3) -0.001(3) -0.002(3) -0.002(3) C14 0.047(3) 0.025(3) 0.024(3) -0.003(2) 0.003(3) -0.001(2) C15 0.034(3) 0.018(3) 0.041(3) -0.002(2) -0.001(2) -0.010(2) C16 0.027(3) 0.017(3) 0.023(3) 0.002(2) -0.003(2) 0.000(2) C17 0.029(2) 0.010(2) 0.023(3) 0.007(2) 0.000(2) 0.004(2) C18 0.021(2) 0.020(3) 0.034(3) 0.001(2) -0.002(2) 0.004(2) C19 0.022(2) 0.021(3) 0.026(3) 0.001(2) 0.003(2) 0.002(2) C20 0.015(2) 0.022(3) 0.024(3) 0.005(2) 0.003(2) 0.000(2) C21 0.020(2) 0.016(3) 0.022(3) -0.004(2) -0.002(2) -0.001(2) C22 0.019(2) 0.021(3) 0.022(3) 0.000(2) -0.0047(19) 0.003(2) C23 0.060(4) 0.024(3) 0.021(3) 0.005(2) -0.011(3) 0.008(3) C24 0.099(5) 0.029(4) 0.022(3) 0.012(3) -0.014(3) 0.011(3) C25 0.077(4) 0.038(4) 0.019(3) 0.000(3) -0.005(3) 0.005(3) C26 0.042(3) 0.024(3) 0.022(3) 0.000(2) 0.001(2) 0.005(3) C27 0.020(2) 0.024(3) 0.023(3) 0.003(2) -0.005(2) 0.001(2) C28 0.019(2) 0.019(3) 0.016(3) -0.003(2) -0.0042(19) -0.0021(19) C29 0.089(6) 0.086(6) 0.056(5) 0.005(5) -0.005(4) -0.020(5) C30 0.092(6) 0.034(5) 0.064(6) -0.005(4) -0.012(5) -0.006(4) P1 0.0144(5) 0.0158(7) 0.0180(7) -0.0015(5) -0.0002(5) 0.0000(5) P2 0.0136(5) 0.0147(6) 0.0198(7) -0.0013(6) 0.0008(5) 0.0011(4) Cl1 0.0150(5) 0.0200(7) 0.0601(10) -0.0019(7) 0.0054(6) 0.0027(5) Cl2 0.0152(5) 0.0201(7) 0.0803(12) 0.0022(7) 0.0109(6) -0.0020(5) Pd1 0.01128(14) 0.01589(18) 0.02454(19) -0.00086(18) 0.00062(15) -0.00015(14) N1 0.145(7) 0.057(5) 0.079(5) 0.009(4) -0.021(5) -0.019(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 C1 C9 1.528(6) . ? C1 C2 1.553(6) . ? C1 P1 1.838(5) . ? C1 H1 1.0000 . ? C2 C3 1.520(7) . ? C2 C4 1.556(7) . ? C2 H2 1.0000 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C7 1.539(6) . ? C4 C6 1.540(7) . ? C4 C5 1.554(7) . ? 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 C8 1.534(7) . ? C7 C10 1.537(6) . ? C7 H7 1.0000 . ? C8 C9 1.544(7) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 P1 1.849(4) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C19 1.544(6) . ? C11 C12 1.548(6) . ? C11 P2 1.835(5) . ? C11 H11 1.0000 . ? C12 C13 1.534(7) . ? C12 C16 1.561(6) . ? C12 H12 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C16 1.560(7) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.516(6) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.550(6) . ? C17 C18 1.547(6) . ? C17 C20 1.549(6) . ? C17 H17 1.0000 . ? C18 C19 1.544(6) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 P2 1.843(5) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.504(6) . ? C21 P2 1.836(4) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.384(6) . ? C22 C27 1.420(7) . ? C23 C24 1.367(7) . ? C23 H23 0.9500 . ? C24 C25 1.384(8) . ? C24 H24 0.9500 . ? C25 C26 1.377(7) . ? C25 H25 0.9500 . ? C26 C27 1.394(7) . ? C26 H26 0.9500 . ? C27 C28 1.515(6) . ? C28 P1 1.836(4) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.442(10) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 N1 1.134(9) . ? P1 Pd1 2.2699(12) . ? P2 Pd1 2.2567(11) . ? Cl1 Pd1 2.3738(11) . ? Cl2 Pd1 2.3405(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 C9 C1 C2 111.1(4) . . ? C9 C1 P1 111.4(3) . . ? C2 C1 P1 105.7(3) . . ? C9 C1 H1 109.5 . . ? C2 C1 H1 109.5 . . ? P1 C1 H1 109.5 . . ? C3 C2 C1 110.7(4) . . ? C3 C2 C4 116.1(4) . . ? C1 C2 C4 110.1(4) . . ? C3 C2 H2 106.5 . . ? C1 C2 H2 106.5 . . ? C4 C2 H2 106.5 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C7 C4 C6 111.0(4) . . ? C7 C4 C5 107.8(4) . . ? C6 C4 C5 106.0(4) . . ? C7 C4 C2 109.5(4) . . ? C6 C4 C2 109.1(4) . . ? C5 C4 C2 113.4(4) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C8 C7 C10 108.5(4) . . ? C8 C7 C4 111.3(4) . . ? C10 C7 C4 111.8(4) . . ? C8 C7 H7 108.4 . . ? C10 C7 H7 108.4 . . ? C4 C7 H7 108.4 . . ? C7 C8 C9 109.8(4) . . ? C7 C8 H8A 109.7 . . ? C9 C8 H8A 109.7 . . ? C7 C8 H8B 109.7 . . ? C9 C8 H8B 109.7 . . ? H8A C8 H8B 108.2 . . ? C1 C9 C8 111.0(4) . . ? C1 C9 H9A 109.4 . . ? C8 C9 H9A 109.4 . . ? C1 C9 H9B 109.4 . . ? C8 C9 H9B 109.4 . . ? H9A C9 H9B 108.0 . . ? C7 C10 P1 111.5(3) . . ? C7 C10 H10A 109.3 . . ? P1 C10 H10A 109.3 . . ? C7 C10 H10B 109.3 . . ? P1 C10 H10B 109.3 . . ? H10A C10 H10B 108.0 . . ? C19 C11 C12 111.8(4) . . ? C19 C11 P2 110.0(3) . . ? C12 C11 P2 105.7(3) . . ? C19 C11 H11 109.8 . . ? C12 C11 H11 109.8 . . ? P2 C11 H11 109.8 . . ? C13 C12 C11 111.0(4) . . ? C13 C12 C16 114.6(4) . . ? C11 C12 C16 111.4(4) . . ? C13 C12 H12 106.4 . . ? C11 C12 H12 106.4 . . ? C16 C12 H12 106.4 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C16 C14 H14A 109.5 . . ? C16 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C16 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 H15A 109.5 . . ? C16 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C16 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C15 C16 C17 111.7(4) . . ? C15 C16 C14 106.2(4) . . ? C17 C16 C14 108.4(4) . . ? C15 C16 C12 109.7(4) . . ? C17 C16 C12 107.6(4) . . ? C14 C16 C12 113.3(4) . . ? C18 C17 C16 110.1(4) . . ? C18 C17 C20 109.3(4) . . ? C16 C17 C20 112.7(4) . . ? C18 C17 H17 108.2 . . ? C16 C17 H17 108.2 . . ? C20 C17 H17 108.2 . . ? C19 C18 C17 110.6(4) . . ? C19 C18 H18A 109.5 . . ? C17 C18 H18A 109.5 . . ? C19 C18 H18B 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 108.1 . . ? C11 C19 C18 110.2(4) . . ? C11 C19 H19A 109.6 . . ? C18 C19 H19A 109.6 . . ? C11 C19 H19B 109.6 . . ? C18 C19 H19B 109.6 . . ? H19A C19 H19B 108.1 . . ? C17 C20 P2 110.5(3) . . ? C17 C20 H20A 109.6 . . ? P2 C20 H20A 109.6 . . ? C17 C20 H20B 109.6 . . ? P2 C20 H20B 109.6 . . ? H20A C20 H20B 108.1 . . ? C22 C21 P2 110.6(3) . . ? C22 C21 H21A 109.5 . . ? P2 C21 H21A 109.5 . . ? C22 C21 H21B 109.5 . . ? P2 C21 H21B 109.5 . . ? H21A C21 H21B 108.1 . . ? C23 C22 C27 117.4(5) . . ? C23 C22 C21 120.3(4) . . ? C27 C22 C21 122.2(4) . . ? C24 C23 C22 122.8(5) . . ? C24 C23 H23 118.6 . . ? C22 C23 H23 118.6 . . ? C23 C24 C25 119.6(5) . . ? C23 C24 H24 120.2 . . ? C25 C24 H24 120.2 . . ? C26 C25 C24 119.6(6) . . ? C26 C25 H25 120.2 . . ? C24 C25 H25 120.2 . . ? C25 C26 C27 121.1(5) . . ? C25 C26 H26 119.5 . . ? C27 C26 H26 119.5 . . ? C26 C27 C22 119.3(5) . . ? C26 C27 C28 119.0(4) . . ? C22 C27 C28 121.5(4) . . ? C27 C28 P1 119.1(3) . . ? C27 C28 H28A 107.5 . . ? P1 C28 H28A 107.5 . . ? C27 C28 H28B 107.5 . . ? P1 C28 H28B 107.5 . . ? H28A C28 H28B 107.0 . . ? C30 C29 H29A 109.5 . . ? C30 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C30 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N1 C30 C29 176.0(9) . . ? C28 P1 C1 107.1(2) . . ? C28 P1 C10 106.2(2) . . ? C1 P1 C10 96.0(2) . . ? C28 P1 Pd1 112.14(15) . . ? C1 P1 Pd1 114.57(15) . . ? C10 P1 Pd1 119.10(16) . . ? C11 P2 C21 108.8(2) . . ? C11 P2 C20 97.0(2) . . ? C21 P2 C20 104.4(2) . . ? C11 P2 Pd1 115.43(15) . . ? C21 P2 Pd1 111.50(15) . . ? C20 P2 Pd1 118.22(14) . . ? P2 Pd1 P1 89.95(4) . . ? P2 Pd1 Cl2 89.78(4) . . ? P1 Pd1 Cl2 178.76(6) . . ? P2 Pd1 Cl1 176.90(5) . . ? P1 Pd1 Cl1 91.28(4) . . ? Cl2 Pd1 Cl1 88.93(4) . . ? 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 C9 C1 C2 C3 85.9(5) . . . . ? P1 C1 C2 C3 -153.1(4) . . . . ? C9 C1 C2 C4 -43.7(5) . . . . ? P1 C1 C2 C4 77.3(4) . . . . ? C3 C2 C4 C7 -145.2(5) . . . . ? C1 C2 C4 C7 -18.6(6) . . . . ? C3 C2 C4 C6 93.1(5) . . . . ? C1 C2 C4 C6 -140.2(4) . . . . ? C3 C2 C4 C5 -24.8(6) . . . . ? C1 C2 C4 C5 101.9(5) . . . . ? C6 C4 C7 C8 -172.9(4) . . . . ? C5 C4 C7 C8 -57.2(5) . . . . ? C2 C4 C7 C8 66.6(5) . . . . ? C6 C4 C7 C10 65.7(5) . . . . ? C5 C4 C7 C10 -178.6(4) . . . . ? C2 C4 C7 C10 -54.8(5) . . . . ? C10 C7 C8 C9 77.1(5) . . . . ? C4 C7 C8 C9 -46.3(5) . . . . ? C2 C1 C9 C8 64.7(5) . . . . ? P1 C1 C9 C8 -52.9(5) . . . . ? C7 C8 C9 C1 -17.2(6) . . . . ? C8 C7 C10 P1 -56.5(4) . . . . ? C4 C7 C10 P1 66.6(4) . . . . ? C19 C11 C12 C13 87.5(5) . . . . ? P2 C11 C12 C13 -152.9(3) . . . . ? C19 C11 C12 C16 -41.6(5) . . . . ? P2 C11 C12 C16 78.0(4) . . . . ? C13 C12 C16 C15 89.9(5) . . . . ? C11 C12 C16 C15 -143.0(4) . . . . ? C13 C12 C16 C17 -148.5(4) . . . . ? C11 C12 C16 C17 -21.4(5) . . . . ? C13 C12 C16 C14 -28.6(6) . . . . ? C11 C12 C16 C14 98.5(5) . . . . ? C15 C16 C17 C18 -170.7(4) . . . . ? C14 C16 C17 C18 -54.0(5) . . . . ? C12 C16 C17 C18 68.8(5) . . . . ? C15 C16 C17 C20 66.9(5) . . . . ? C14 C16 C17 C20 -176.4(4) . . . . ? C12 C16 C17 C20 -53.5(5) . . . . ? C16 C17 C18 C19 -48.4(5) . . . . ? C20 C17 C18 C19 75.9(5) . . . . ? C12 C11 C19 C18 62.6(5) . . . . ? P2 C11 C19 C18 -54.5(5) . . . . ? C17 C18 C19 C11 -15.6(5) . . . . ? C18 C17 C20 P2 -54.2(4) . . . . ? C16 C17 C20 P2 68.6(4) . . . . ? P2 C21 C22 C23 -91.9(5) . . . . ? P2 C21 C22 C27 89.0(5) . . . . ? C27 C22 C23 C24 -1.9(8) . . . . ? C21 C22 C23 C24 178.9(5) . . . . ? C22 C23 C24 C25 1.4(10) . . . . ? C23 C24 C25 C26 -0.3(10) . . . . ? C24 C25 C26 C27 -0.2(9) . . . . ? C25 C26 C27 C22 -0.2(8) . . . . ? C25 C26 C27 C28 175.8(5) . . . . ? C23 C22 C27 C26 1.2(7) . . . . ? C21 C22 C27 C26 -179.6(4) . . . . ? C23 C22 C27 C28 -174.7(4) . . . . ? C21 C22 C27 C28 4.5(7) . . . . ? C26 C27 C28 P1 127.3(4) . . . . ? C22 C27 C28 P1 -56.7(5) . . . . ? C27 C28 P1 C1 -140.8(4) . . . . ? C27 C28 P1 C10 117.4(4) . . . . ? C27 C28 P1 Pd1 -14.3(4) . . . . ? C9 C1 P1 C28 -45.9(4) . . . . ? C2 C1 P1 C28 -166.7(3) . . . . ? C9 C1 P1 C10 63.2(4) . . . . ? C2 C1 P1 C10 -57.7(3) . . . . ? C9 C1 P1 Pd1 -170.9(3) . . . . ? C2 C1 P1 Pd1 68.2(3) . . . . ? C7 C10 P1 C28 102.1(3) . . . . ? C7 C10 P1 C1 -7.7(4) . . . . ? C7 C10 P1 Pd1 -130.2(3) . . . . ? C19 C11 P2 C21 -42.0(4) . . . . ? C12 C11 P2 C21 -162.9(3) . . . . ? C19 C11 P2 C20 65.9(3) . . . . ? C12 C11 P2 C20 -55.0(3) . . . . ? C19 C11 P2 Pd1 -168.3(3) . . . . ? C12 C11 P2 Pd1 70.9(3) . . . . ? C22 C21 P2 C11 -177.8(3) . . . . ? C22 C21 P2 C20 79.4(4) . . . . ? C22 C21 P2 Pd1 -49.3(4) . . . . ? C17 C20 P2 C11 -10.2(3) . . . . ? C17 C20 P2 C21 101.3(3) . . . . ? C17 C20 P2 Pd1 -134.1(3) . . . . ? C11 P2 Pd1 P1 86.53(17) . . . . ? C21 P2 Pd1 P1 -38.32(17) . . . . ? C20 P2 Pd1 P1 -159.33(18) . . . . ? C11 P2 Pd1 Cl2 -94.68(17) . . . . ? C21 P2 Pd1 Cl2 140.47(17) . . . . ? C20 P2 Pd1 Cl2 19.47(18) . . . . ? C28 P1 Pd1 P2 74.61(16) . . . . ? C1 P1 Pd1 P2 -163.03(18) . . . . ? C10 P1 Pd1 P2 -50.28(18) . . . . ? C28 P1 Pd1 Cl1 -102.55(17) . . . . ? C1 P1 Pd1 Cl1 19.82(18) . . . . ? C10 P1 Pd1 Cl1 132.56(18) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.559 _refine_diff_density_min -0.934 _refine_diff_density_rms 0.118 # Attachment 'compound15.cif' data_compound15 _database_code_depnum_ccdc_archive 'CCDC 756175' #TrackingRef 'compound15.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common pge0812 _chemical_melting_point ? _chemical_formula_moiety 'C28 H44 Cl2 P2 Pt, C2 H3 N' _chemical_formula_sum 'C30 H47 Cl2 N P2 Pt' _chemical_formula_weight 749.62 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' Pt Pt -1.7033 8.3905 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P212121 _symmetry_space_group_name_Hall 'P 2ac 2ab' 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 7.92200(10) _cell_length_b 21.3381(3) _cell_length_c 18.4545(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3119.56(8) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 20844 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.485 _chemical_absolute_configuration rm _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.596 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1504 _exptl_absorpt_coefficient_mu 4.792 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.245 _exptl_absorpt_correction_T_max 0.350 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24594 _diffrn_reflns_av_R_equivalents 0.1288 _diffrn_reflns_av_sigmaI/netI 0.0916 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 27.50 _reflns_number_total 7129 _reflns_number_gt 6277 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0778P)^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 -0.021(9) _refine_ls_number_reflns 7129 _refine_ls_number_parameters 332 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0664 _refine_ls_R_factor_gt 0.0560 _refine_ls_wR_factor_ref 0.1342 _refine_ls_wR_factor_gt 0.1273 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _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 C1 C 0.5711(17) 0.2313(5) 0.6637(6) 0.048(3) Uani 1 1 d . . . H1A H 0.6781 0.2538 0.6694 0.072 Uiso 1 1 calc R . . H1B H 0.5558 0.2023 0.7044 0.072 Uiso 1 1 calc R . . H1C H 0.4777 0.2614 0.6628 0.072 Uiso 1 1 calc R . . C2 C 0.6012(16) 0.2421(5) 0.5328(6) 0.045(3) Uani 1 1 d . . . H2A H 0.5068 0.2717 0.5319 0.068 Uiso 1 1 calc R . . H2B H 0.6081 0.2204 0.4861 0.068 Uiso 1 1 calc R . . H2C H 0.7067 0.2649 0.5416 0.068 Uiso 1 1 calc R . . C3 C 0.5735(13) 0.1945(4) 0.5929(5) 0.030(2) Uani 1 1 d . . . C4 C 0.7176(13) 0.1433(4) 0.5899(5) 0.0269(19) Uani 1 1 d . . . H4 H 0.7592 0.1431 0.5387 0.032 Uiso 1 1 calc R . . C5 C 0.8713(14) 0.1559(5) 0.6368(7) 0.047(3) Uani 1 1 d . . . H5A H 0.8379 0.1560 0.6880 0.070 Uiso 1 1 calc R . . H5B H 0.9196 0.1967 0.6241 0.070 Uiso 1 1 calc R . . H5C H 0.9556 0.1230 0.6287 0.070 Uiso 1 1 calc R . . C6 C 0.6469(12) 0.0771(4) 0.6041(4) 0.0191(17) Uani 1 1 d . . . H6 H 0.7411 0.0473 0.6151 0.023 Uiso 1 1 calc R . . C7 C 0.5183(13) 0.0780(5) 0.6677(5) 0.029(2) Uani 1 1 d . . . H7A H 0.4811 0.0347 0.6783 0.035 Uiso 1 1 calc R . . H7B H 0.5737 0.0948 0.7116 0.035 Uiso 1 1 calc R . . C8 C 0.3627(13) 0.1188(5) 0.6489(4) 0.030(2) Uani 1 1 d . . . H8A H 0.2653 0.0914 0.6375 0.036 Uiso 1 1 calc R . . H8B H 0.3323 0.1451 0.6911 0.036 Uiso 1 1 calc R . . C9 C 0.4021(11) 0.1606(4) 0.5839(5) 0.0245(19) Uani 1 1 d . . . H9 H 0.3122 0.1934 0.5810 0.029 Uiso 1 1 calc R . . C10 C 0.3931(12) 0.1216(4) 0.5149(4) 0.0213(18) Uani 1 1 d . . . H10A H 0.4225 0.1482 0.4727 0.026 Uiso 1 1 calc R . . H10B H 0.2763 0.1061 0.5080 0.026 Uiso 1 1 calc R . . C11 C 0.4070(12) -0.0145(4) 0.5413(5) 0.0232(19) Uani 1 1 d . . . H11A H 0.4484 -0.0325 0.5874 0.028 Uiso 1 1 calc R . . H11B H 0.2909 0.0009 0.5502 0.028 Uiso 1 1 calc R . . C12 C 0.3964(12) -0.0676(4) 0.4860(5) 0.0226(18) Uani 1 1 d . . . C13 C 0.4285(14) -0.1271(4) 0.5104(5) 0.031(2) Uani 1 1 d . . . H13 H 0.4656 -0.1335 0.5588 0.038 Uiso 1 1 calc R . . C14 C 0.407(2) -0.1786(5) 0.4639(6) 0.052(4) Uani 1 1 d . . . H14 H 0.4280 -0.2199 0.4807 0.062 Uiso 1 1 calc R . . C15 C 0.354(2) -0.1687(5) 0.3940(7) 0.066(5) Uani 1 1 d . . . H15 H 0.3395 -0.2033 0.3622 0.079 Uiso 1 1 calc R . . C16 C 0.3233(16) -0.1091(5) 0.3700(5) 0.044(3) Uani 1 1 d . . . H16 H 0.2876 -0.1029 0.3214 0.053 Uiso 1 1 calc R . . C17 C 0.3429(12) -0.0576(4) 0.4152(5) 0.028(2) Uani 1 1 d . . . C18 C 0.3074(11) 0.0072(4) 0.3849(5) 0.0222(18) Uani 1 1 d . . . H18A H 0.2616 0.0342 0.4238 0.027 Uiso 1 1 calc R . . H18B H 0.2212 0.0041 0.3463 0.027 Uiso 1 1 calc R . . C19 C 0.5220(11) 0.0060(4) 0.2584(5) 0.0227(18) Uani 1 1 d . . . H19A H 0.6419 -0.0049 0.2502 0.027 Uiso 1 1 calc R . . H19B H 0.4550 -0.0331 0.2568 0.027 Uiso 1 1 calc R . . C20 C 0.4610(12) 0.0511(4) 0.1975(4) 0.023(2) Uani 1 1 d . . . H20 H 0.4607 0.0273 0.1508 0.028 Uiso 1 1 calc R . . C21 C 0.5765(12) 0.1105(4) 0.1876(5) 0.0255(19) Uani 1 1 d . . . C22 C 0.7497(12) 0.0923(5) 0.1598(5) 0.031(2) Uani 1 1 d . . . H22A H 0.7380 0.0701 0.1136 0.046 Uiso 1 1 calc R . . H22B H 0.8052 0.0649 0.1951 0.046 Uiso 1 1 calc R . . H22C H 0.8178 0.1302 0.1526 0.046 Uiso 1 1 calc R . . C23 C 0.4949(16) 0.1537(5) 0.1309(5) 0.037(2) Uani 1 1 d . . . H23A H 0.5763 0.1858 0.1160 0.055 Uiso 1 1 calc R . . H23B H 0.3953 0.1740 0.1519 0.055 Uiso 1 1 calc R . . H23C H 0.4611 0.1290 0.0886 0.055 Uiso 1 1 calc R . . C24 C 0.5924(12) 0.1411(4) 0.2641(4) 0.0239(19) Uani 1 1 d . . . H24 H 0.6980 0.1241 0.2863 0.029 Uiso 1 1 calc R . . C25 C 0.6106(14) 0.2122(4) 0.2631(5) 0.029(2) Uani 1 1 d . . . H25A H 0.5080 0.2310 0.2429 0.044 Uiso 1 1 calc R . . H25B H 0.7078 0.2238 0.2331 0.044 Uiso 1 1 calc R . . H25C H 0.6278 0.2275 0.3126 0.044 Uiso 1 1 calc R . . C26 C 0.2782(13) 0.0710(4) 0.2142(5) 0.029(2) Uani 1 1 d . . . H26A H 0.2258 0.0886 0.1700 0.034 Uiso 1 1 calc R . . H26B H 0.2118 0.0339 0.2291 0.034 Uiso 1 1 calc R . . C27 C 0.2744(12) 0.1202(4) 0.2750(5) 0.0243(18) Uani 1 1 d . . . H27A H 0.1825 0.1101 0.3094 0.029 Uiso 1 1 calc R . . H27B H 0.2507 0.1620 0.2539 0.029 Uiso 1 1 calc R . . C28 C 0.4436(11) 0.1224(4) 0.3159(4) 0.0173(17) Uani 1 1 d . . . H28 H 0.4367 0.1521 0.3577 0.021 Uiso 1 1 calc R . . C29 C 0.133(2) 0.3636(8) 0.0841(8) 0.083(5) Uani 1 1 d . . . H29A H 0.2500 0.3659 0.0676 0.125 Uiso 1 1 calc R . . H29B H 0.1104 0.3977 0.1183 0.125 Uiso 1 1 calc R . . H29C H 0.0568 0.3674 0.0424 0.125 Uiso 1 1 calc R . . C30 C 0.103(2) 0.3020(6) 0.1208(7) 0.062(4) Uani 1 1 d . . . P1 P 0.5402(3) 0.05405(9) 0.51959(11) 0.0154(4) Uani 1 1 d . . . P2 P 0.4990(3) 0.04276(12) 0.34804(10) 0.0162(4) Uani 1 1 d . . . Cl1 Cl 0.9498(3) 0.02527(13) 0.50468(11) 0.0322(6) Uani 1 1 d . . . Cl2 Cl 0.9027(3) 0.01722(15) 0.33016(12) 0.0382(7) Uani 1 1 d . . . Pt1 Pt 0.71517(4) 0.037090(15) 0.425878(16) 0.01732(10) Uani 1 1 d . . . N1 N 0.073(2) 0.2534(7) 0.1445(7) 0.091(5) 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 C1 0.052(8) 0.040(6) 0.053(7) -0.018(6) -0.006(6) -0.016(6) C2 0.053(8) 0.028(5) 0.055(7) 0.006(5) 0.000(6) -0.013(5) C3 0.033(6) 0.020(4) 0.036(5) -0.005(4) -0.006(4) -0.010(4) C4 0.021(4) 0.034(5) 0.025(4) 0.000(4) 0.000(4) -0.004(4) C5 0.024(6) 0.051(7) 0.066(8) -0.008(6) -0.020(6) -0.006(5) C6 0.023(4) 0.020(4) 0.015(4) 0.003(3) -0.006(3) -0.002(4) C7 0.028(5) 0.037(5) 0.022(4) -0.003(4) 0.003(4) -0.009(4) C8 0.035(5) 0.040(5) 0.015(4) -0.010(4) 0.014(4) 0.005(5) C9 0.022(5) 0.022(4) 0.030(5) -0.007(4) 0.004(4) 0.003(3) C10 0.028(5) 0.023(4) 0.013(4) -0.002(3) 0.002(3) 0.006(4) C11 0.023(5) 0.025(4) 0.021(4) 0.000(4) 0.000(3) -0.002(4) C12 0.021(5) 0.026(4) 0.021(4) 0.000(4) 0.000(3) -0.002(4) C13 0.051(7) 0.019(4) 0.024(5) 0.001(4) 0.000(4) 0.005(4) C14 0.106(12) 0.016(5) 0.033(6) 0.000(5) -0.006(7) -0.004(6) C15 0.126(14) 0.025(5) 0.046(7) -0.012(5) -0.018(8) -0.003(7) C16 0.077(10) 0.030(5) 0.026(5) 0.001(4) -0.014(5) -0.032(6) C17 0.028(5) 0.023(4) 0.034(5) -0.004(4) 0.000(4) -0.005(4) C18 0.016(5) 0.029(4) 0.022(4) 0.004(4) 0.000(3) -0.003(4) C19 0.018(4) 0.018(4) 0.032(5) -0.005(4) -0.003(4) 0.002(3) C20 0.032(5) 0.028(5) 0.011(4) -0.006(3) -0.006(3) 0.010(4) C21 0.033(5) 0.024(4) 0.020(4) 0.002(4) 0.003(4) 0.002(4) C22 0.034(7) 0.041(5) 0.017(4) 0.000(4) 0.009(4) -0.001(4) C23 0.050(7) 0.036(6) 0.024(5) 0.000(4) -0.003(5) 0.009(5) C24 0.023(5) 0.029(5) 0.020(4) 0.003(4) 0.001(4) -0.003(4) C25 0.040(6) 0.026(5) 0.022(5) -0.001(4) 0.008(4) -0.006(4) C26 0.035(5) 0.032(5) 0.019(4) -0.011(4) -0.001(4) -0.002(5) C27 0.026(5) 0.024(4) 0.022(4) -0.003(4) -0.002(4) 0.009(4) C28 0.017(4) 0.017(4) 0.017(4) -0.006(3) 0.003(3) -0.001(3) C29 0.104(14) 0.079(10) 0.066(10) 0.013(9) 0.008(10) 0.009(10) C30 0.085(11) 0.052(8) 0.049(8) 0.012(7) -0.013(7) -0.002(8) P1 0.0140(10) 0.0169(11) 0.0154(9) -0.0012(8) 0.0019(8) -0.0014(8) P2 0.0133(10) 0.0206(11) 0.0147(9) -0.0012(9) -0.0006(7) -0.0001(9) Cl1 0.0157(10) 0.0607(17) 0.0203(10) 0.0024(11) -0.0026(8) 0.0078(11) Cl2 0.0149(11) 0.078(2) 0.0215(10) 0.0010(11) 0.0024(8) 0.0096(11) Pt1 0.01067(15) 0.02509(16) 0.01620(15) 0.00116(14) 0.00001(12) 0.00046(13) N1 0.136(15) 0.076(9) 0.061(8) 0.008(7) 0.017(9) 0.034(10) _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 C1 C3 1.524(13) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.520(14) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C9 1.547(13) . ? C3 C4 1.580(14) . ? C4 C5 1.518(13) . ? C4 C6 1.544(12) . ? C4 H4 1.0000 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.554(13) . ? C6 P1 1.841(8) . ? C6 H6 1.0000 . ? C7 C8 1.548(14) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.528(12) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.522(11) . ? C9 H9 1.0000 . ? C10 P1 1.856(9) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.528(12) . ? C11 P1 1.847(9) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.370(12) . ? C12 C17 1.390(13) . ? C13 C14 1.405(13) . ? C13 H13 0.9500 . ? C14 C15 1.370(16) . ? C14 H14 0.9500 . ? C15 C16 1.369(15) . ? C15 H15 0.9500 . ? C16 C17 1.388(13) . ? C16 H16 0.9500 . ? C17 C18 1.518(12) . ? C18 P2 1.828(9) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.555(12) . ? C19 P2 1.839(8) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C26 1.541(14) . ? C20 C21 1.574(13) . ? C20 H20 1.0000 . ? C21 C22 1.516(13) . ? C21 C23 1.538(13) . ? C21 C24 1.560(12) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.524(12) . ? C24 C28 1.570(11) . ? C24 H24 1.0000 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 C27 1.537(11) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.539(12) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 P2 1.852(8) . ? C28 H28 1.0000 . ? C29 C30 1.495(19) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 N1 1.150(18) . ? P1 Pt1 2.246(2) . ? P2 Pt1 2.239(2) . ? Cl1 Pt1 2.374(2) . ? Cl2 Pt1 2.346(2) . ? 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 C1 H1A 109.5 . . ? C3 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C3 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 H2A 109.5 . . ? C3 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C3 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C2 C3 C1 106.4(8) . . ? C2 C3 C9 111.1(9) . . ? C1 C3 C9 108.8(9) . . ? C2 C3 C4 109.3(9) . . ? C1 C3 C4 113.3(9) . . ? C9 C3 C4 107.9(7) . . ? C5 C4 C6 110.8(8) . . ? C5 C4 C3 115.9(8) . . ? C6 C4 C3 111.4(8) . . ? C5 C4 H4 106.0 . . ? C6 C4 H4 106.0 . . ? C3 C4 H4 106.0 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 C7 110.8(7) . . ? C4 C6 P1 105.4(5) . . ? C7 C6 P1 110.0(6) . . ? C4 C6 H6 110.2 . . ? C7 C6 H6 110.2 . . ? P1 C6 H6 110.2 . . ? C8 C7 C6 111.1(7) . . ? C8 C7 H7A 109.4 . . ? C6 C7 H7A 109.4 . . ? C8 C7 H7B 109.4 . . ? C6 C7 H7B 109.4 . . ? H7A C7 H7B 108.0 . . ? C9 C8 C7 109.9(7) . . ? C9 C8 H8A 109.7 . . ? C7 C8 H8A 109.7 . . ? C9 C8 H8B 109.7 . . ? C7 C8 H8B 109.7 . . ? H8A C8 H8B 108.2 . . ? C10 C9 C8 109.2(7) . . ? C10 C9 C3 112.7(8) . . ? C8 C9 C3 111.6(8) . . ? C10 C9 H9 107.7 . . ? C8 C9 H9 107.7 . . ? C3 C9 H9 107.7 . . ? C9 C10 P1 110.8(6) . . ? C9 C10 H10A 109.5 . . ? P1 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? P1 C10 H10B 109.5 . . ? H10A C10 H10B 108.1 . . ? C12 C11 P1 118.3(6) . . ? C12 C11 H11A 107.7 . . ? P1 C11 H11A 107.7 . . ? C12 C11 H11B 107.7 . . ? P1 C11 H11B 107.7 . . ? H11A C11 H11B 107.1 . . ? C13 C12 C17 120.6(8) . . ? C13 C12 C11 117.2(8) . . ? C17 C12 C11 122.0(8) . . ? C12 C13 C14 120.0(9) . . ? C12 C13 H13 120.0 . . ? C14 C13 H13 120.0 . . ? C15 C14 C13 119.5(10) . . ? C15 C14 H14 120.2 . . ? C13 C14 H14 120.2 . . ? C14 C15 C16 120.1(10) . . ? C14 C15 H15 120.0 . . ? C16 C15 H15 120.0 . . ? C15 C16 C17 121.4(10) . . ? C15 C16 H16 119.3 . . ? C17 C16 H16 119.3 . . ? C16 C17 C12 118.5(8) . . ? C16 C17 C18 118.6(8) . . ? C12 C17 C18 122.9(8) . . ? C17 C18 P2 111.2(6) . . ? C17 C18 H18A 109.4 . . ? P2 C18 H18A 109.4 . . ? C17 C18 H18B 109.4 . . ? P2 C18 H18B 109.4 . . ? H18A C18 H18B 108.0 . . ? C20 C19 P2 110.8(6) . . ? C20 C19 H19A 109.5 . . ? P2 C19 H19A 109.5 . . ? C20 C19 H19B 109.5 . . ? P2 C19 H19B 109.5 . . ? H19A C19 H19B 108.1 . . ? C26 C20 C19 108.5(7) . . ? C26 C20 C21 110.3(7) . . ? C19 C20 C21 113.6(7) . . ? C26 C20 H20 108.1 . . ? C19 C20 H20 108.1 . . ? C21 C20 H20 108.1 . . ? C22 C21 C23 107.6(8) . . ? C22 C21 C24 110.0(8) . . ? C23 C21 C24 113.5(8) . . ? C22 C21 C20 111.1(8) . . ? C23 C21 C20 108.5(8) . . ? C24 C21 C20 106.2(7) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 C24 C21 114.4(7) . . ? C25 C24 C28 109.4(7) . . ? C21 C24 C28 112.6(7) . . ? C25 C24 H24 106.6 . . ? C21 C24 H24 106.6 . . ? C28 C24 H24 106.6 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C27 C26 C20 110.7(8) . . ? C27 C26 H26A 109.5 . . ? C20 C26 H26A 109.5 . . ? C27 C26 H26B 109.5 . . ? C20 C26 H26B 109.5 . . ? H26A C26 H26B 108.1 . . ? C26 C27 C28 111.2(8) . . ? C26 C27 H27A 109.4 . . ? C28 C27 H27A 109.4 . . ? C26 C27 H27B 109.4 . . ? C28 C27 H27B 109.4 . . ? H27A C27 H27B 108.0 . . ? C27 C28 C24 111.2(7) . . ? C27 C28 P2 109.7(6) . . ? C24 C28 P2 104.5(6) . . ? C27 C28 H28 110.4 . . ? C24 C28 H28 110.4 . . ? P2 C28 H28 110.4 . . ? C30 C29 H29A 109.5 . . ? C30 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C30 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N1 C30 C29 174.9(17) . . ? C6 P1 C11 106.8(4) . . ? C6 P1 C10 96.9(4) . . ? C11 P1 C10 105.5(4) . . ? C6 P1 Pt1 114.3(3) . . ? C11 P1 Pt1 113.1(3) . . ? C10 P1 Pt1 118.5(3) . . ? C18 P2 C19 103.9(4) . . ? C18 P2 C28 107.6(4) . . ? C19 P2 C28 97.3(4) . . ? C18 P2 Pt1 111.9(3) . . ? C19 P2 Pt1 118.6(3) . . ? C28 P2 Pt1 115.9(3) . . ? P2 Pt1 P1 90.76(8) . . ? P2 Pt1 Cl2 90.63(8) . . ? P1 Pt1 Cl2 178.25(9) . . ? P2 Pt1 Cl1 176.42(9) . . ? P1 Pt1 Cl1 91.65(8) . . ? Cl2 Pt1 Cl1 86.92(8) . . ? 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 C2 C3 C4 C5 92.6(10) . . . . ? C1 C3 C4 C5 -26.0(12) . . . . ? C9 C3 C4 C5 -146.5(9) . . . . ? C2 C3 C4 C6 -139.5(8) . . . . ? C1 C3 C4 C6 102.0(9) . . . . ? C9 C3 C4 C6 -18.5(10) . . . . ? C5 C4 C6 C7 87.8(10) . . . . ? C3 C4 C6 C7 -42.8(9) . . . . ? C5 C4 C6 P1 -153.2(7) . . . . ? C3 C4 C6 P1 76.2(8) . . . . ? C4 C6 C7 C8 63.3(10) . . . . ? P1 C6 C7 C8 -52.9(9) . . . . ? C6 C7 C8 C9 -16.0(11) . . . . ? C7 C8 C9 C10 77.3(9) . . . . ? C7 C8 C9 C3 -48.0(10) . . . . ? C2 C3 C9 C10 64.0(10) . . . . ? C1 C3 C9 C10 -179.2(8) . . . . ? C4 C3 C9 C10 -55.9(10) . . . . ? C2 C3 C9 C8 -172.8(8) . . . . ? C1 C3 C9 C8 -55.9(10) . . . . ? C4 C3 C9 C8 67.4(9) . . . . ? C8 C9 C10 P1 -57.2(9) . . . . ? C3 C9 C10 P1 67.4(9) . . . . ? P1 C11 C12 C13 127.9(9) . . . . ? P1 C11 C12 C17 -57.3(11) . . . . ? C17 C12 C13 C14 -0.3(17) . . . . ? C11 C12 C13 C14 174.5(11) . . . . ? C12 C13 C14 C15 0(2) . . . . ? C13 C14 C15 C16 0(3) . . . . ? C14 C15 C16 C17 0(2) . . . . ? C15 C16 C17 C12 0.4(19) . . . . ? C15 C16 C17 C18 179.6(13) . . . . ? C13 C12 C17 C16 -0.1(15) . . . . ? C11 C12 C17 C16 -174.7(10) . . . . ? C13 C12 C17 C18 -179.3(9) . . . . ? C11 C12 C17 C18 6.2(14) . . . . ? C16 C17 C18 P2 -91.7(10) . . . . ? C12 C17 C18 P2 87.4(10) . . . . ? P2 C19 C20 C26 -55.4(8) . . . . ? P2 C19 C20 C21 67.8(8) . . . . ? C26 C20 C21 C22 -171.1(7) . . . . ? C19 C20 C21 C22 66.7(9) . . . . ? C26 C20 C21 C23 -53.0(9) . . . . ? C19 C20 C21 C23 -175.2(7) . . . . ? C26 C20 C21 C24 69.3(9) . . . . ? C19 C20 C21 C24 -52.8(9) . . . . ? C22 C21 C24 C25 91.6(10) . . . . ? C23 C21 C24 C25 -29.0(12) . . . . ? C20 C21 C24 C25 -148.2(8) . . . . ? C22 C21 C24 C28 -142.7(8) . . . . ? C23 C21 C24 C28 96.7(10) . . . . ? C20 C21 C24 C28 -22.4(10) . . . . ? C19 C20 C26 C27 76.3(9) . . . . ? C21 C20 C26 C27 -48.9(9) . . . . ? C20 C26 C27 C28 -15.7(10) . . . . ? C26 C27 C28 C24 61.4(9) . . . . ? C26 C27 C28 P2 -53.7(8) . . . . ? C25 C24 C28 C27 89.1(9) . . . . ? C21 C24 C28 C27 -39.4(10) . . . . ? C25 C24 C28 P2 -152.7(6) . . . . ? C21 C24 C28 P2 78.9(8) . . . . ? C4 C6 P1 C11 -165.3(6) . . . . ? C7 C6 P1 C11 -45.8(7) . . . . ? C4 C6 P1 C10 -56.8(7) . . . . ? C7 C6 P1 C10 62.7(7) . . . . ? C4 C6 P1 Pt1 68.8(6) . . . . ? C7 C6 P1 Pt1 -171.7(5) . . . . ? C12 C11 P1 C6 -140.7(7) . . . . ? C12 C11 P1 C10 116.9(7) . . . . ? C12 C11 P1 Pt1 -14.0(8) . . . . ? C9 C10 P1 C6 -7.9(7) . . . . ? C9 C10 P1 C11 101.7(7) . . . . ? C9 C10 P1 Pt1 -130.5(5) . . . . ? C17 C18 P2 C19 79.7(7) . . . . ? C17 C18 P2 C28 -177.9(6) . . . . ? C17 C18 P2 Pt1 -49.4(7) . . . . ? C20 C19 P2 C18 101.6(7) . . . . ? C20 C19 P2 C28 -8.7(7) . . . . ? C20 C19 P2 Pt1 -133.4(5) . . . . ? C27 C28 P2 C18 -43.2(6) . . . . ? C24 C28 P2 C18 -162.5(5) . . . . ? C27 C28 P2 C19 63.9(6) . . . . ? C24 C28 P2 C19 -55.4(6) . . . . ? C27 C28 P2 Pt1 -169.4(5) . . . . ? C24 C28 P2 Pt1 71.3(5) . . . . ? C18 P2 Pt1 P1 -37.4(3) . . . . ? C19 P2 Pt1 P1 -158.3(3) . . . . ? C18 P2 Pt1 Cl2 141.6(3) . . . . ? C19 P2 Pt1 Cl2 20.6(3) . . . . ? C28 P2 Pt1 Cl2 -94.5(3) . . . . ? C6 P1 Pt1 P2 -163.9(3) . . . . ? C11 P1 Pt1 P2 73.6(3) . . . . ? C10 P1 Pt1 P2 -50.5(3) . . . . ? C6 P1 Pt1 Cl1 18.8(3) . . . . ? C11 P1 Pt1 Cl1 -103.8(3) . . . . ? C10 P1 Pt1 Cl1 132.1(3) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.828 _refine_diff_density_min -3.370 _refine_diff_density_rms 0.274 # Attachment 'compound17.cif' data_compound17 _database_code_depnum_ccdc_archive 'CCDC 756176' #TrackingRef 'compound17.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C32 H44 Mo O4 P2), C7 H8' _chemical_formula_sum 'C71 H96 Mo2 O8 P4' _chemical_formula_weight 1393.24 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' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21' _symmetry_space_group_name_Hall 'P 2yb' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 17.118(3) _cell_length_b 8.9172(18) _cell_length_c 22.259(5) _cell_angle_alpha 90.00 _cell_angle_beta 97.60(3) _cell_angle_gamma 90.00 _cell_volume 3367.9(12) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 62125 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.374 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1460 _exptl_absorpt_coefficient_mu 0.521 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8807 _exptl_absorpt_correction_T_max 0.9120 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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-Nonius KappaCCD' _diffrn_measurement_method '\f and \w' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 44591 _diffrn_reflns_av_R_equivalents 0.1279 _diffrn_reflns_av_sigmaI/netI 0.1414 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 27.48 _reflns_number_total 15091 _reflns_number_gt 9763 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0627P)^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 -0.03(4) _refine_ls_number_reflns 15091 _refine_ls_number_parameters 806 _refine_ls_number_restraints 235 _refine_ls_R_factor_all 0.1204 _refine_ls_R_factor_gt 0.0669 _refine_ls_wR_factor_ref 0.1565 _refine_ls_wR_factor_gt 0.1356 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.029 _refine_ls_shift/su_mean 0.003 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 C1 C 0.3300(4) 0.6594(10) 0.5040(3) 0.0301(18) Uani 1 1 d . . . C2 C 0.1857(4) 0.7878(10) 0.5149(3) 0.031(2) Uani 1 1 d . . . C3 C 0.3127(4) 0.6865(9) 0.3786(3) 0.0258(19) Uani 1 1 d . . . C4 C 0.1916(4) 0.5566(10) 0.4304(3) 0.030(2) Uani 1 1 d . . . C5 C -0.0416(5) 0.6109(12) 0.3763(4) 0.057(3) Uani 1 1 d . . . H5A H -0.0752 0.6249 0.3375 0.086 Uiso 1 1 calc R . . H5B H -0.0747 0.5950 0.4084 0.086 Uiso 1 1 calc R . . H5C H -0.0076 0.5234 0.3736 0.086 Uiso 1 1 calc R . . C6 C 0.0100(4) 0.7520(9) 0.3909(3) 0.0352(16) Uani 1 1 d . . . H6 H 0.0495 0.7263 0.4266 0.042 Uiso 1 1 calc R . . C7 C -0.0348(4) 0.8935(13) 0.4790(3) 0.051(2) Uani 1 1 d . . . H7A H 0.0195 0.9102 0.4979 0.076 Uiso 1 1 calc R . . H7B H -0.0539 0.7976 0.4929 0.076 Uiso 1 1 calc R . . H7C H -0.0685 0.9749 0.4902 0.076 Uiso 1 1 calc R . . C8 C -0.0373(4) 0.8897(9) 0.4097(3) 0.0411(19) Uani 1 1 d . . . C9 C -0.1278(4) 0.8863(12) 0.3831(4) 0.060(3) Uani 1 1 d . . . H9A H -0.1518 0.9832 0.3903 0.090 Uiso 1 1 calc R . . H9B H -0.1543 0.8068 0.4031 0.090 Uiso 1 1 calc R . . H9C H -0.1331 0.8668 0.3394 0.090 Uiso 1 1 calc R . . C10 C 0.0003(4) 1.0297(9) 0.3871(3) 0.0372(17) Uani 1 1 d . . . H10 H -0.0256 1.1193 0.4029 0.045 Uiso 1 1 calc R . . C11 C -0.0130(4) 1.0357(11) 0.3173(3) 0.045(2) Uani 1 1 d . . . H11A H -0.0685 1.0628 0.3033 0.054 Uiso 1 1 calc R . . H11B H 0.0211 1.1141 0.3030 0.054 Uiso 1 1 calc R . . C12 C 0.0057(4) 0.8849(12) 0.2903(3) 0.048(2) Uani 1 1 d . . . H12A H 0.0344 0.9009 0.2550 0.058 Uiso 1 1 calc R . . H12B H -0.0440 0.8313 0.2761 0.058 Uiso 1 1 calc R . . C13 C 0.0884(4) 1.0398(10) 0.4081(3) 0.0403(19) Uani 1 1 d . . . H13A H 0.0979 1.0295 0.4528 0.048 Uiso 1 1 calc R . . H13B H 0.1077 1.1398 0.3975 0.048 Uiso 1 1 calc R . . C14 C 0.0567(4) 0.7890(9) 0.3386(3) 0.0328(18) Uani 1 1 d . . . H14 H 0.0732 0.6943 0.3198 0.039 Uiso 1 1 calc R . . C15 C 0.1798(4) 0.9905(11) 0.3070(3) 0.045(2) Uani 1 1 d . . . H15A H 0.1500 0.9494 0.2695 0.054 Uiso 1 1 calc R . . H15B H 0.1661 1.0981 0.3089 0.054 Uiso 1 1 calc R . . C16 C 0.2672(5) 0.9791(9) 0.3014(3) 0.035(2) Uani 1 1 d . . . C17 C 0.2895(5) 0.9025(10) 0.2516(3) 0.043(2) Uani 1 1 d . . . H17 H 0.2502 0.8537 0.2243 0.052 Uiso 1 1 calc R . . C18 C 0.3673(6) 0.8957(11) 0.2410(4) 0.051(2) Uani 1 1 d . . . H18 H 0.3817 0.8426 0.2071 0.062 Uiso 1 1 calc R . . C19 C 0.4220(5) 0.9667(10) 0.2801(3) 0.045(2) Uani 1 1 d . . . H19 H 0.4758 0.9608 0.2740 0.054 Uiso 1 1 calc R . . C20 C 0.4023(4) 1.0465(9) 0.3281(3) 0.038(2) Uani 1 1 d . . . H20 H 0.4422 1.0998 0.3531 0.045 Uiso 1 1 calc R . . C21 C 0.3245(4) 1.0518(10) 0.3415(3) 0.0279(18) Uani 1 1 d . . . C22 C 0.3053(4) 1.1307(9) 0.3970(3) 0.0303(17) Uani 1 1 d . . . H22A H 0.2506 1.1695 0.3896 0.036 Uiso 1 1 calc R . . H22B H 0.3412 1.2172 0.4060 0.036 Uiso 1 1 calc R . . C23 C 0.2891(4) 1.1168(9) 0.5277(3) 0.0282(18) Uani 1 1 d . . . H23 H 0.2305 1.1228 0.5259 0.034 Uiso 1 1 calc R . . C24 C 0.3251(3) 1.0317(8) 0.5862(3) 0.0270(14) Uani 1 1 d . . . H24 H 0.3178 0.9222 0.5776 0.032 Uiso 1 1 calc R . . C25 C 0.2799(4) 1.0672(10) 0.6392(3) 0.037(2) Uani 1 1 d . . . H25A H 0.2817 1.1754 0.6470 0.056 Uiso 1 1 calc R . . H25B H 0.3040 1.0138 0.6755 0.056 Uiso 1 1 calc R . . H25C H 0.2249 1.0353 0.6292 0.056 Uiso 1 1 calc R . . C26 C 0.4174(4) 1.0600(8) 0.6005(3) 0.0296(16) Uani 1 1 d . . . C27 C 0.4377(4) 1.1804(10) 0.6492(3) 0.034(2) Uani 1 1 d . . . H27A H 0.4251 1.1432 0.6882 0.052 Uiso 1 1 calc R . . H27B H 0.4069 1.2711 0.6379 0.052 Uiso 1 1 calc R . . H27C H 0.4940 1.2040 0.6526 0.052 Uiso 1 1 calc R . . C28 C 0.4564(4) 0.9149(9) 0.6242(3) 0.036(2) Uani 1 1 d . . . H28A H 0.5133 0.9305 0.6338 0.054 Uiso 1 1 calc R . . H28B H 0.4462 0.8366 0.5933 0.054 Uiso 1 1 calc R . . H28C H 0.4348 0.8838 0.6609 0.054 Uiso 1 1 calc R . . C29 C 0.4467(4) 1.1115(8) 0.5407(3) 0.0276(16) Uani 1 1 d . . . H29 H 0.5055 1.1179 0.5477 0.033 Uiso 1 1 calc R . . C30 C 0.4144(4) 1.2662(10) 0.5239(3) 0.0315(19) Uani 1 1 d . . . H30A H 0.4256 1.2922 0.4827 0.038 Uiso 1 1 calc R . . H30B H 0.4410 1.3409 0.5525 0.038 Uiso 1 1 calc R . . C31 C 0.3234(3) 1.2727(8) 0.5258(3) 0.0314(16) Uani 1 1 d . . . H31A H 0.3127 1.3294 0.5621 0.038 Uiso 1 1 calc R . . H31B H 0.2977 1.3261 0.4895 0.038 Uiso 1 1 calc R . . C32 C 0.4231(3) 0.9982(9) 0.4893(3) 0.0309(17) Uani 1 1 d . . . H32A H 0.4387 0.8961 0.5037 0.037 Uiso 1 1 calc R . . H32B H 0.4517 1.0219 0.4547 0.037 Uiso 1 1 calc R . . C33 C 0.0416(4) 0.4144(9) 0.8794(3) 0.036(2) Uani 1 1 d . . . H33A H -0.0081 0.3596 0.8784 0.054 Uiso 1 1 calc R . . H33B H 0.0544 0.4264 0.8380 0.054 Uiso 1 1 calc R . . H33C H 0.0365 0.5134 0.8976 0.054 Uiso 1 1 calc R . . C34 C 0.1084(4) 0.3257(8) 0.9178(3) 0.0288(15) Uani 1 1 d . . . H34 H 0.1566 0.3901 0.9211 0.035 Uiso 1 1 calc R . . C35 C 0.1294(4) 0.1756(8) 0.8873(3) 0.0298(16) Uani 1 1 d . . . C36 C 0.0621(4) 0.1072(11) 0.8431(3) 0.039(2) Uani 1 1 d . . . H36A H 0.0503 0.1730 0.8078 0.059 Uiso 1 1 calc R . . H36B H 0.0150 0.0968 0.8635 0.059 Uiso 1 1 calc R . . H36C H 0.0780 0.0083 0.8299 0.059 Uiso 1 1 calc R . . C37 C 0.1973(4) 0.2076(10) 0.8500(3) 0.037(2) Uani 1 1 d . . . H37A H 0.2437 0.2418 0.8770 0.056 Uiso 1 1 calc R . . H37B H 0.1810 0.2856 0.8199 0.056 Uiso 1 1 calc R . . H37C H 0.2103 0.1157 0.8293 0.056 Uiso 1 1 calc R . . C38 C 0.1574(4) 0.0631(8) 0.9391(3) 0.0297(16) Uani 1 1 d . . . H38 H 0.1794 -0.0284 0.9215 0.036 Uiso 1 1 calc R . . C39 C 0.0859(4) 0.0178(12) 0.9717(3) 0.037(2) Uani 1 1 d . . . H39A H 0.1049 -0.0323 1.0105 0.044 Uiso 1 1 calc R . . H39B H 0.0521 -0.0538 0.9461 0.044 Uiso 1 1 calc R . . C40 C 0.0369(4) 0.1597(9) 0.9839(3) 0.0355(18) Uani 1 1 d . . . H40A H -0.0090 0.1691 0.9520 0.043 Uiso 1 1 calc R . . H40B H 0.0170 0.1497 1.0235 0.043 Uiso 1 1 calc R . . C41 C 0.0890(4) 0.3003(8) 0.9841(3) 0.0295(16) Uani 1 1 d . . . H41 H 0.0601 0.3893 0.9974 0.035 Uiso 1 1 calc R . . C42 C 0.2209(4) 0.1337(10) 0.9863(3) 0.0336(19) Uani 1 1 d . . . H42A H 0.2627 0.1773 0.9649 0.040 Uiso 1 1 calc R . . H42B H 0.2453 0.0537 1.0133 0.040 Uiso 1 1 calc R . . C43 C 0.1619(4) 0.1688(9) 1.1001(3) 0.0362(19) Uani 1 1 d . . . H43A H 0.1085 0.1250 1.0911 0.043 Uiso 1 1 calc R . . H43B H 0.1999 0.0846 1.1063 0.043 Uiso 1 1 calc R . . C44 C 0.1663(4) 0.2572(10) 1.1590(3) 0.0312(17) Uani 1 1 d . . . C45 C 0.0948(4) 0.3005(9) 1.1788(3) 0.041(2) Uani 1 1 d . . . H45 H 0.0455 0.2764 1.1560 0.049 Uiso 1 1 calc R . . C46 C 0.0991(5) 0.3809(11) 1.2337(4) 0.049(2) Uani 1 1 d . . . H46 H 0.0517 0.4132 1.2475 0.059 Uiso 1 1 calc R . . C47 C 0.1685(5) 0.4134(11) 1.2671(3) 0.046(2) Uani 1 1 d . . . H47 H 0.1699 0.4676 1.3040 0.055 Uiso 1 1 calc R . . C48 C 0.2375(4) 0.3671(11) 1.2472(3) 0.039(2) Uani 1 1 d . . . H48 H 0.2862 0.3902 1.2711 0.047 Uiso 1 1 calc R . . C49 C 0.2384(4) 0.2889(10) 1.1944(3) 0.032(2) Uani 1 1 d . . . C50 C 0.3152(4) 0.2431(10) 1.1741(3) 0.0306(17) Uani 1 1 d . . . H50A H 0.3068 0.1499 1.1499 0.037 Uiso 1 1 calc R . . H50B H 0.3536 0.2206 1.2103 0.037 Uiso 1 1 calc R . . C51 C 0.4217(4) 0.4985(9) 1.1852(3) 0.0363(18) Uani 1 1 d . . . H51A H 0.4190 0.6057 1.1736 0.044 Uiso 1 1 calc R . . H51B H 0.4024 0.4890 1.2251 0.044 Uiso 1 1 calc R . . C52 C 0.5065(4) 0.4461(9) 1.1908(3) 0.0358(19) Uani 1 1 d . . . H52 H 0.5360 0.5004 1.2261 0.043 Uiso 1 1 calc R . . C53 C 0.5130(4) 0.2816(9) 1.2049(3) 0.0340(19) Uani 1 1 d . . . H53A H 0.4798 0.2562 1.2367 0.041 Uiso 1 1 calc R . . H53B H 0.5684 0.2560 1.2203 0.041 Uiso 1 1 calc R . . C54 C 0.4854(4) 0.1899(8) 1.1463(3) 0.0357(17) Uani 1 1 d . . . H54A H 0.5317 0.1459 1.1304 0.043 Uiso 1 1 calc R . . H54B H 0.4507 0.1068 1.1558 0.043 Uiso 1 1 calc R . . C55 C 0.4411(4) 0.2915(8) 1.0985(3) 0.0321(18) Uani 1 1 d . . . H55 H 0.4200 0.2297 1.0625 0.038 Uiso 1 1 calc R . . C56 C 0.4945(4) 0.4170(8) 1.0780(3) 0.0302(16) Uani 1 1 d . . . H56 H 0.4587 0.4986 1.0601 0.036 Uiso 1 1 calc R . . C57 C 0.5408(4) 0.3624(13) 1.0273(3) 0.051(3) Uani 1 1 d . . . H57A H 0.5725 0.2747 1.0415 0.077 Uiso 1 1 calc R . . H57B H 0.5755 0.4428 1.0167 0.077 Uiso 1 1 calc R . . H57C H 0.5038 0.3350 0.9916 0.077 Uiso 1 1 calc R . . C58 C 0.5468(4) 0.4861(10) 1.1342(3) 0.044(2) Uani 1 1 d . . . C59 C 0.5530(5) 0.6588(11) 1.1261(4) 0.053(3) Uani 1 1 d . . . H59A H 0.5014 0.7048 1.1280 0.079 Uiso 1 1 calc R . . H59B H 0.5701 0.6806 1.0867 0.079 Uiso 1 1 calc R . . H59C H 0.5914 0.6998 1.1585 0.079 Uiso 1 1 calc R . . C60 C 0.6309(4) 0.4213(13) 1.1422(4) 0.059(3) Uani 1 1 d . . . H60A H 0.6594 0.4597 1.1100 0.088 Uiso 1 1 calc R . . H60B H 0.6283 0.3116 1.1398 0.088 Uiso 1 1 calc R . . H60C H 0.6586 0.4513 1.1817 0.088 Uiso 1 1 calc R . . C61 C 0.3146(4) 0.7197(11) 1.0688(3) 0.032(2) Uani 1 1 d . . . C62 C 0.1839(4) 0.6287(10) 0.9896(3) 0.0307(18) Uani 1 1 d . . . C63 C 0.3249(4) 0.4812(10) 0.9833(3) 0.032(2) Uani 1 1 d . . . C64 C 0.1904(4) 0.5956(11) 1.1155(4) 0.036(2) Uani 1 1 d . . . O1 O 0.3791(3) 0.6094(7) 0.5385(2) 0.0390(13) Uani 1 1 d . . . O2 O 0.1512(3) 0.8001(8) 0.5565(2) 0.0466(17) Uani 1 1 d . . . O3 O 0.3507(3) 0.6326(8) 0.3467(2) 0.0434(15) Uani 1 1 d . . . O5 O 0.3443(3) 0.8339(7) 1.0799(2) 0.0416(16) Uani 1 1 d . . . O6 O 0.1432(3) 0.6929(7) 0.9540(2) 0.0447(15) Uani 1 1 d . . . O7 O 0.3571(3) 0.4614(7) 0.9433(2) 0.0440(16) Uani 1 1 d . . . O8 O 0.1534(3) 0.6547(8) 1.1474(2) 0.0448(16) Uani 1 1 d . . . O13 O 0.1630(3) 0.4394(7) 0.4212(2) 0.0393(15) Uani 1 1 d . . . P1 P 0.14450(11) 0.8936(3) 0.37338(8) 0.0278(5) Uani 1 1 d . . . P2 P 0.31527(9) 1.0016(3) 0.46345(8) 0.0235(5) Uani 1 1 d . . . P3 P 0.18322(11) 0.2797(3) 1.03247(8) 0.0276(5) Uani 1 1 d . . . P4 P 0.35756(11) 0.3880(3) 1.12816(8) 0.0273(5) Uani 1 1 d . . . Mo1 Mo 0.24634(3) 0.75105(17) 0.44516(2) 0.02388(17) Uani 1 1 d . . . Mo2 Mo 0.25927(3) 0.52452(17) 1.05206(2) 0.02545(18) Uani 1 1 d . . . C65A C 0.75388(3) 0.12483(17) 0.22048(2) 0.075(3) Uani 0.863(8) 1 d PRDU A 1 C66A C 0.76647(3) 0.20370(17) 0.27476(2) 0.079(3) Uani 0.863(8) 1 d PRDU A 1 H66A H 0.8042 0.2823 0.2798 0.095 Uiso 0.863(8) 1 calc PR A 1 C67A C 0.72382(3) 0.16755(17) 0.32173(2) 0.074(3) Uani 0.863(8) 1 d PRDU A 1 H67A H 0.7324 0.2215 0.3588 0.089 Uiso 0.863(8) 1 calc PR A 1 C68A C 0.66857(3) 0.05253(17) 0.31442(2) 0.046(2) Uani 0.863(8) 1 d PRDU A 1 H68A H 0.6394 0.0278 0.3465 0.055 Uiso 0.863(8) 1 calc PR A 1 C69A C 0.65598(3) -0.02634(17) 0.26013(2) 0.046(2) Uani 0.863(8) 1 d PRDU A 1 H69A H 0.6182 -0.1049 0.2551 0.056 Uiso 0.863(8) 1 calc PR A 1 C70A C 0.69863(3) 0.00981(17) 0.21317(2) 0.069(3) Uani 0.863(8) 1 d PRDU A 1 H70A H 0.6900 -0.0441 0.1761 0.082 Uiso 0.863(8) 1 calc PR A 1 C71A C 0.8044(5) 0.1714(9) 0.1799(5) 0.156(6) Uani 0.863(8) 1 d PDU A 1 H71A H 0.7938 0.1134 0.1424 0.234 Uiso 0.863(8) 1 calc PR A 1 H71B H 0.8592 0.1555 0.1980 0.234 Uiso 0.863(8) 1 calc PR A 1 H71C H 0.7959 0.2782 0.1709 0.234 Uiso 0.863(8) 1 calc PR A 1 C65B C 0.7071(5) 0.0582(9) 0.2609(5) 0.072(4) Uani 0.137(8) 1 d PRDU A 2 C66B C 0.7201(5) 0.0268(9) 0.2019(5) 0.080(5) Uani 0.137(8) 1 d PRDU A 2 H66B H 0.6902 -0.0493 0.1794 0.096 Uiso 0.137(8) 1 calc PR A 2 C67B C 0.7766(5) 0.1065(9) 0.1757(5) 0.093(6) Uani 0.137(8) 1 d PRDU A 2 H67B H 0.7854 0.0850 0.1354 0.111 Uiso 0.137(8) 1 calc PR A 2 C68B C 0.8202(5) 0.2177(9) 0.2086(5) 0.088(6) Uani 0.137(8) 1 d PRDU A 2 H68B H 0.8589 0.2723 0.1907 0.105 Uiso 0.137(8) 1 calc PR A 2 C69B C 0.8073(5) 0.2492(9) 0.2676(5) 0.080(6) Uani 0.137(8) 1 d PRDU A 2 H69B H 0.8371 0.3252 0.2901 0.096 Uiso 0.137(8) 1 calc PR A 2 C70B C 0.7508(5) 0.1695(9) 0.2938(5) 0.070(5) Uani 0.137(8) 1 d PRDU A 2 H70B H 0.7419 0.1910 0.3342 0.084 Uiso 0.137(8) 1 calc PR A 2 C71B C 0.653(2) -0.038(3) 0.2937(11) 0.078(10) Uani 0.137(8) 1 d PDU A 2 H71D H 0.6519 0.0005 0.3349 0.117 Uiso 0.137(8) 1 calc PR A 2 H71E H 0.6717 -0.1419 0.2958 0.117 Uiso 0.137(8) 1 calc PR A 2 H71F H 0.5992 -0.0350 0.2716 0.117 Uiso 0.137(8) 1 calc PR A 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 C1 0.040(4) 0.025(5) 0.025(4) 0.004(4) 0.001(3) -0.004(4) C2 0.019(3) 0.033(6) 0.038(4) -0.002(4) -0.006(3) 0.001(3) C3 0.021(4) 0.025(5) 0.029(4) -0.003(4) -0.004(3) -0.001(3) C4 0.040(4) 0.037(6) 0.014(4) 0.000(4) 0.005(3) -0.004(4) C5 0.048(5) 0.062(7) 0.059(6) 0.001(6) -0.004(5) -0.027(5) C6 0.035(4) 0.035(4) 0.035(4) 0.003(4) 0.002(3) -0.008(4) C7 0.042(5) 0.065(7) 0.047(5) -0.004(5) 0.013(4) 0.013(5) C8 0.038(4) 0.047(5) 0.037(4) 0.009(4) 0.001(3) 0.008(4) C9 0.031(4) 0.056(6) 0.094(7) 0.012(6) 0.013(4) 0.001(4) C10 0.035(4) 0.029(4) 0.048(4) 0.004(4) 0.005(3) 0.005(4) C11 0.028(4) 0.051(6) 0.054(5) 0.011(5) -0.002(4) 0.001(4) C12 0.041(4) 0.066(7) 0.035(5) 0.004(5) -0.005(4) -0.004(4) C13 0.042(4) 0.043(5) 0.035(4) 0.004(4) 0.000(3) 0.009(4) C14 0.028(4) 0.037(5) 0.034(4) -0.003(4) 0.007(3) -0.004(3) C15 0.031(4) 0.058(7) 0.045(5) 0.008(4) 0.004(3) -0.012(4) C16 0.059(5) 0.019(5) 0.028(4) 0.004(4) 0.016(4) 0.005(4) C17 0.069(6) 0.030(5) 0.031(4) 0.011(4) 0.010(4) -0.008(4) C18 0.087(7) 0.037(5) 0.035(5) 0.015(4) 0.027(5) 0.019(5) C19 0.055(5) 0.041(5) 0.041(5) 0.029(4) 0.018(4) 0.019(4) C20 0.037(4) 0.046(6) 0.031(4) 0.017(4) 0.008(3) 0.010(4) C21 0.033(4) 0.026(5) 0.026(4) 0.009(3) 0.007(3) 0.003(3) C22 0.031(4) 0.032(4) 0.028(4) 0.006(3) 0.005(3) 0.004(3) C23 0.025(3) 0.033(5) 0.029(4) -0.004(3) 0.013(3) 0.000(3) C24 0.022(3) 0.034(4) 0.026(3) 0.004(3) 0.004(3) 0.004(3) C25 0.037(4) 0.042(6) 0.036(4) -0.008(4) 0.014(3) 0.001(4) C26 0.027(3) 0.028(4) 0.031(4) 0.000(3) -0.008(3) 0.001(3) C27 0.032(4) 0.036(6) 0.033(4) -0.002(4) -0.003(3) -0.001(4) C28 0.038(4) 0.034(5) 0.035(4) -0.001(4) 0.002(3) 0.005(4) C29 0.014(3) 0.031(4) 0.037(4) -0.012(3) 0.003(3) -0.003(3) C30 0.037(4) 0.021(5) 0.038(4) 0.000(4) 0.010(3) -0.001(4) C31 0.025(3) 0.037(5) 0.031(4) -0.002(3) -0.002(3) 0.007(3) C32 0.024(3) 0.029(4) 0.043(4) 0.007(4) 0.017(3) 0.000(3) C33 0.044(4) 0.029(5) 0.034(4) 0.003(4) -0.004(3) 0.009(4) C34 0.029(4) 0.027(4) 0.029(4) 0.000(3) -0.001(3) 0.001(3) C35 0.027(4) 0.029(4) 0.035(4) 0.003(3) 0.008(3) -0.008(3) C36 0.044(5) 0.033(6) 0.044(5) -0.006(4) 0.014(4) -0.007(4) C37 0.042(4) 0.033(5) 0.040(4) -0.002(4) 0.017(3) 0.001(4) C38 0.031(4) 0.028(4) 0.032(4) -0.009(3) 0.009(3) -0.002(3) C39 0.035(4) 0.036(5) 0.040(4) -0.005(5) 0.009(3) -0.007(5) C40 0.040(4) 0.039(5) 0.031(4) -0.009(4) 0.014(3) 0.004(4) C41 0.028(3) 0.023(4) 0.040(4) -0.002(3) 0.012(3) 0.004(3) C42 0.042(4) 0.025(4) 0.034(4) 0.001(4) 0.007(3) -0.002(3) C43 0.045(4) 0.035(5) 0.030(4) 0.010(3) 0.008(3) -0.007(4) C44 0.041(4) 0.020(4) 0.033(4) 0.006(4) 0.012(3) 0.000(4) C45 0.036(4) 0.046(6) 0.043(5) 0.021(4) 0.015(3) 0.002(4) C46 0.056(5) 0.056(6) 0.042(5) 0.016(5) 0.030(4) 0.024(5) C47 0.056(5) 0.062(7) 0.023(4) 0.003(4) 0.018(4) 0.024(5) C48 0.048(5) 0.044(5) 0.027(4) 0.005(4) 0.009(3) 0.000(4) C49 0.029(4) 0.042(6) 0.028(4) 0.020(4) 0.008(3) 0.007(4) C50 0.037(4) 0.033(4) 0.023(3) 0.016(4) 0.005(3) 0.002(3) C51 0.051(4) 0.036(5) 0.021(3) -0.002(3) 0.000(3) 0.000(4) C52 0.043(4) 0.036(5) 0.026(4) -0.006(3) -0.002(3) 0.003(4) C53 0.036(4) 0.028(5) 0.036(4) 0.013(4) -0.004(3) -0.001(3) C54 0.026(4) 0.028(4) 0.052(5) 0.002(4) 0.001(3) 0.003(3) C55 0.032(4) 0.033(5) 0.031(4) -0.003(3) 0.005(3) 0.008(3) C56 0.025(3) 0.039(5) 0.025(4) 0.006(3) 0.000(3) -0.001(3) C57 0.039(5) 0.076(8) 0.041(5) 0.006(5) 0.017(4) -0.005(5) C58 0.037(4) 0.058(6) 0.034(4) 0.008(4) 0.000(3) -0.013(4) C59 0.054(5) 0.043(6) 0.056(6) 0.010(5) -0.009(5) -0.011(5) C60 0.031(4) 0.082(8) 0.059(5) 0.021(5) -0.009(4) -0.002(4) C61 0.030(4) 0.036(6) 0.031(4) 0.005(4) 0.006(3) 0.005(4) C62 0.036(4) 0.020(4) 0.037(4) -0.008(4) 0.007(4) 0.002(3) C63 0.037(4) 0.028(5) 0.031(4) -0.004(4) 0.000(3) -0.007(4) C64 0.032(4) 0.040(6) 0.037(5) 0.000(4) 0.006(4) -0.003(4) O1 0.043(3) 0.030(3) 0.042(3) 0.002(3) -0.002(3) 0.008(3) O2 0.037(3) 0.068(5) 0.037(3) -0.003(3) 0.015(3) -0.001(3) O3 0.042(3) 0.047(4) 0.045(3) -0.003(3) 0.017(3) 0.007(3) O5 0.045(3) 0.036(4) 0.044(3) -0.004(3) 0.007(3) -0.011(3) O6 0.053(3) 0.038(4) 0.040(3) 0.007(3) -0.005(3) 0.011(3) O7 0.053(3) 0.054(5) 0.027(3) -0.001(3) 0.015(3) -0.004(3) O8 0.048(3) 0.041(4) 0.049(3) -0.003(3) 0.020(3) 0.013(3) O13 0.052(4) 0.033(4) 0.033(3) -0.003(3) 0.010(3) -0.008(3) P1 0.0285(10) 0.0335(14) 0.0209(10) 0.0035(10) 0.0021(8) -0.0009(10) P2 0.0219(9) 0.0238(14) 0.0252(9) 0.0025(10) 0.0042(7) 0.0003(9) P3 0.0313(10) 0.0264(15) 0.0257(10) 0.0015(10) 0.0056(8) 0.0008(10) P4 0.0304(10) 0.0241(13) 0.0279(11) 0.0014(10) 0.0057(8) 0.0046(10) Mo1 0.0256(3) 0.0227(4) 0.0232(3) 0.0010(3) 0.0026(3) -0.0007(3) Mo2 0.0292(3) 0.0236(4) 0.0238(3) 0.0021(3) 0.0043(3) 0.0009(3) C65A 0.070(6) 0.072(6) 0.093(5) 0.052(5) 0.046(5) 0.046(4) C66A 0.059(6) 0.055(6) 0.120(6) 0.033(5) 0.001(5) 0.007(5) C67A 0.090(7) 0.056(6) 0.068(5) -0.009(5) -0.020(4) 0.010(4) C68A 0.068(5) 0.037(5) 0.031(4) 0.012(3) 0.005(4) 0.018(4) C69A 0.052(5) 0.032(5) 0.052(5) 0.008(4) -0.007(4) 0.003(4) C70A 0.085(6) 0.081(7) 0.041(4) -0.008(5) 0.011(4) 0.045(4) C71A 0.158(11) 0.152(13) 0.186(10) 0.098(10) 0.121(10) 0.074(9) C65B 0.076(8) 0.069(8) 0.073(7) 0.018(7) 0.012(7) 0.035(7) C66B 0.084(11) 0.084(11) 0.075(8) 0.019(9) 0.019(9) 0.047(9) C67B 0.096(12) 0.092(13) 0.097(11) 0.033(10) 0.037(10) 0.055(11) C68B 0.076(12) 0.078(13) 0.116(11) 0.046(12) 0.038(10) 0.056(10) C69B 0.063(12) 0.070(12) 0.106(11) 0.036(11) 0.014(11) 0.042(9) C70B 0.070(10) 0.062(9) 0.079(9) 0.025(8) 0.012(8) 0.037(8) C71B 0.08(2) 0.09(2) 0.067(18) 0.013(18) 0.005(16) 0.016(14) _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 C1 O1 1.151(8) . ? C1 Mo1 1.984(8) . ? C2 O2 1.168(8) . ? C2 Mo1 2.005(8) . ? C3 O3 1.131(8) . ? C3 Mo1 2.064(7) . ? C4 O13 1.161(9) . ? C4 Mo1 1.977(9) . ? C5 C6 1.547(11) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C14 1.532(9) . ? C6 C8 1.558(10) . ? C6 H6 1.0000 . ? C7 C8 1.537(10) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C10 1.520(10) . ? C8 C9 1.584(10) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C13 1.521(9) . ? C10 C11 1.542(10) . ? C10 H10 1.0000 . ? C11 C12 1.524(12) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C14 1.549(10) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 P1 1.848(8) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 P1 1.850(7) . ? C14 H14 1.0000 . ? C15 C16 1.522(9) . ? C15 P1 1.879(7) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C21 1.395(10) . ? C16 C17 1.396(10) . ? C17 C18 1.384(11) . ? C17 H17 0.9500 . ? C18 C19 1.350(11) . ? C18 H18 0.9500 . ? C19 C20 1.362(10) . ? C19 H19 0.9500 . ? C20 C21 1.403(9) . ? C20 H20 0.9500 . ? C21 C22 1.497(9) . ? C22 P2 1.864(7) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C31 1.512(10) . ? C23 C24 1.562(9) . ? C23 P2 1.863(7) . ? C23 H23 1.0000 . ? C24 C25 1.527(8) . ? C24 C26 1.590(8) . ? C24 H24 1.0000 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 C28 1.519(10) . ? C26 C27 1.532(9) . ? C26 C29 1.554(9) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C30 1.514(11) . ? C29 C32 1.539(9) . ? C29 H29 1.0000 . ? C30 C31 1.565(8) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 P2 1.859(6) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.550(9) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 C35 1.564(9) . ? C34 C41 1.572(9) . ? C34 H34 1.0000 . ? C35 C36 1.539(9) . ? C35 C37 1.543(9) . ? C35 C38 1.555(9) . ? 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 C42 1.542(9) . ? C38 C39 1.556(9) . ? C38 H38 1.0000 . ? C39 C40 1.561(11) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 C41 1.538(10) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 P3 1.827(7) . ? C41 H41 1.0000 . ? C42 P3 1.829(8) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.523(10) . ? C43 P3 1.877(7) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 C49 1.403(9) . ? C44 C45 1.408(9) . ? C45 C46 1.411(11) . ? C45 H45 0.9500 . ? C46 C47 1.348(11) . ? C46 H46 0.9500 . ? C47 C48 1.378(9) . ? C47 H47 0.9500 . ? C48 C49 1.369(10) . ? C48 H48 0.9500 . ? C49 C50 1.502(9) . ? C50 P4 1.855(7) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 C52 1.514(9) . ? C51 P4 1.850(7) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 C53 1.502(11) . ? C52 C58 1.555(9) . ? C52 H52 1.0000 . ? C53 C54 1.560(9) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 C55 1.521(9) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 C56 1.552(9) . ? C55 P4 1.862(7) . ? C55 H55 1.0000 . ? C56 C57 1.541(9) . ? C56 C58 1.565(9) . ? C56 H56 1.0000 . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C58 C60 1.540(10) . ? C58 C59 1.556(12) . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C61 O5 1.151(10) . ? C61 Mo2 1.993(10) . ? C62 O6 1.138(8) . ? C62 Mo2 1.996(8) . ? C63 O7 1.122(8) . ? C63 Mo2 2.051(8) . ? C64 O8 1.141(9) . ? C64 Mo2 2.055(8) . ? P1 Mo1 2.544(2) . ? P2 Mo1 2.534(2) . ? P3 Mo2 2.549(2) . ? P4 Mo2 2.535(2) . ? C65A C66A 1.3900 . ? C65A C70A 1.3900 . ? C65A C71A 1.394(5) . ? C66A C67A 1.3900 . ? C66A H66A 0.9500 . ? C67A C68A 1.3900 . ? C67A H67A 0.9500 . ? C68A C69A 1.3900 . ? C68A H68A 0.9500 . ? C69A C70A 1.3900 . ? C69A H69A 0.9500 . ? C70A H70A 0.9500 . ? C71A H71A 0.9800 . ? C71A H71B 0.9800 . ? C71A H71C 0.9800 . ? C65B C66B 1.3900 . ? C65B C70B 1.3900 . ? C65B C71B 1.524(10) . ? C66B C67B 1.3900 . ? C66B H66B 0.9500 . ? C67B C68B 1.3900 . ? C67B H67B 0.9500 . ? C68B C69B 1.3900 . ? C68B H68B 0.9500 . ? C69B C70B 1.3901 . ? C69B H69B 0.9500 . ? C70B H70B 0.9500 . ? C71B H71D 0.9800 . ? C71B H71E 0.9800 . ? C71B H71F 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 O1 C1 Mo1 178.4(7) . . ? O2 C2 Mo1 175.8(8) . . ? O3 C3 Mo1 170.2(7) . . ? O13 C4 Mo1 176.7(7) . . ? C6 C5 H5A 109.5 . . ? C6 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C6 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C14 C6 C5 110.9(6) . . ? C14 C6 C8 112.1(6) . . ? C5 C6 C8 113.3(6) . . ? C14 C6 H6 106.7 . . ? C5 C6 H6 106.7 . . ? C8 C6 H6 106.7 . . ? C8 C7 H7A 109.5 . . ? C8 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C8 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C10 C8 C7 110.9(7) . . ? C10 C8 C6 107.5(6) . . ? C7 C8 C6 109.9(7) . . ? C10 C8 C9 109.2(6) . . ? C7 C8 C9 105.7(6) . . ? C6 C8 C9 113.6(7) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 C13 113.1(6) . . ? C8 C10 C11 110.4(6) . . ? C13 C10 C11 108.4(6) . . ? C8 C10 H10 108.2 . . ? C13 C10 H10 108.2 . . ? C11 C10 H10 108.2 . . ? C12 C11 C10 110.9(7) . . ? C12 C11 H11A 109.5 . . ? C10 C11 H11A 109.5 . . ? C12 C11 H11B 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 108.1 . . ? C11 C12 C14 110.0(6) . . ? C11 C12 H12A 109.7 . . ? C14 C12 H12A 109.7 . . ? C11 C12 H12B 109.7 . . ? C14 C12 H12B 109.7 . . ? H12A C12 H12B 108.2 . . ? C10 C13 P1 112.2(5) . . ? C10 C13 H13A 109.2 . . ? P1 C13 H13A 109.2 . . ? C10 C13 H13B 109.2 . . ? P1 C13 H13B 109.2 . . ? H13A C13 H13B 107.9 . . ? C6 C14 C12 110.1(5) . . ? C6 C14 P1 105.5(4) . . ? C12 C14 P1 111.4(6) . . ? C6 C14 H14 109.9 . . ? C12 C14 H14 109.9 . . ? P1 C14 H14 109.9 . . ? C16 C15 P1 117.1(6) . . ? C16 C15 H15A 108.0 . . ? P1 C15 H15A 108.0 . . ? C16 C15 H15B 108.0 . . ? P1 C15 H15B 108.0 . . ? H15A C15 H15B 107.3 . . ? C21 C16 C17 119.5(7) . . ? C21 C16 C15 122.2(7) . . ? C17 C16 C15 118.2(7) . . ? C18 C17 C16 121.8(8) . . ? C18 C17 H17 119.1 . . ? C16 C17 H17 119.1 . . ? C19 C18 C17 118.1(8) . . ? C19 C18 H18 121.0 . . ? C17 C18 H18 121.0 . . ? C18 C19 C20 121.9(8) . . ? C18 C19 H19 119.1 . . ? C20 C19 H19 119.1 . . ? C19 C20 C21 121.6(8) . . ? C19 C20 H20 119.2 . . ? C21 C20 H20 119.2 . . ? C16 C21 C20 117.1(7) . . ? C16 C21 C22 122.3(6) . . ? C20 C21 C22 120.7(7) . . ? C21 C22 P2 111.0(5) . . ? C21 C22 H22A 109.4 . . ? P2 C22 H22A 109.4 . . ? C21 C22 H22B 109.4 . . ? P2 C22 H22B 109.4 . . ? H22A C22 H22B 108.0 . . ? C31 C23 C24 111.0(6) . . ? C31 C23 P2 110.6(4) . . ? C24 C23 P2 105.3(5) . . ? C31 C23 H23 109.9 . . ? C24 C23 H23 109.9 . . ? P2 C23 H23 109.9 . . ? C25 C24 C23 111.1(5) . . ? C25 C24 C26 113.8(5) . . ? C23 C24 C26 111.2(5) . . ? C25 C24 H24 106.8 . . ? C23 C24 H24 106.8 . . ? C26 C24 H24 106.8 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C28 C26 C27 107.7(5) . . ? C28 C26 C29 111.9(6) . . ? C27 C26 C29 109.3(6) . . ? C28 C26 C24 108.3(5) . . ? C27 C26 C24 112.3(6) . . ? C29 C26 C24 107.5(5) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C30 C29 C32 111.3(6) . . ? C30 C29 C26 109.4(5) . . ? C32 C29 C26 111.1(6) . . ? C30 C29 H29 108.3 . . ? C32 C29 H29 108.3 . . ? C26 C29 H29 108.3 . . ? C29 C30 C31 111.0(6) . . ? C29 C30 H30A 109.4 . . ? C31 C30 H30A 109.4 . . ? C29 C30 H30B 109.4 . . ? C31 C30 H30B 109.4 . . ? H30A C30 H30B 108.0 . . ? C23 C31 C30 111.0(6) . . ? C23 C31 H31A 109.4 . . ? C30 C31 H31A 109.4 . . ? C23 C31 H31B 109.4 . . ? C30 C31 H31B 109.4 . . ? H31A C31 H31B 108.0 . . ? C29 C32 P2 111.8(4) . . ? C29 C32 H32A 109.2 . . ? P2 C32 H32A 109.2 . . ? C29 C32 H32B 109.3 . . ? P2 C32 H32B 109.3 . . ? H32A C32 H32B 107.9 . . ? C34 C33 H33A 109.5 . . ? C34 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C34 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C33 C34 C35 113.2(5) . . ? C33 C34 C41 111.0(5) . . ? C35 C34 C41 111.9(5) . . ? C33 C34 H34 106.8 . . ? C35 C34 H34 106.8 . . ? C41 C34 H34 106.8 . . ? C36 C35 C37 106.4(5) . . ? C36 C35 C38 110.5(6) . . ? C37 C35 C38 109.8(5) . . ? C36 C35 C34 114.8(6) . . ? C37 C35 C34 107.9(5) . . ? C38 C35 C34 107.3(5) . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C35 C37 H37A 109.5 . . ? C35 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C35 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C42 C38 C35 111.2(6) . . ? C42 C38 C39 108.5(5) . . ? C35 C38 C39 109.2(6) . . ? C42 C38 H38 109.3 . . ? C35 C38 H38 109.3 . . ? C39 C38 H38 109.3 . . ? C38 C39 C40 110.2(7) . . ? C38 C39 H39A 109.6 . . ? C40 C39 H39A 109.6 . . ? C38 C39 H39B 109.6 . . ? C40 C39 H39B 109.6 . . ? H39A C39 H39B 108.1 . . ? C41 C40 C39 109.7(5) . . ? C41 C40 H40A 109.7 . . ? C39 C40 H40A 109.7 . . ? C41 C40 H40B 109.7 . . ? C39 C40 H40B 109.7 . . ? H40A C40 H40B 108.2 . . ? C40 C41 C34 108.0(6) . . ? C40 C41 P3 112.7(5) . . ? C34 C41 P3 106.7(4) . . ? C40 C41 H41 109.8 . . ? C34 C41 H41 109.8 . . ? P3 C41 H41 109.8 . . ? C38 C42 P3 113.8(5) . . ? C38 C42 H42A 108.8 . . ? P3 C42 H42A 108.8 . . ? C38 C42 H42B 108.8 . . ? P3 C42 H42B 108.8 . . ? H42A C42 H42B 107.7 . . ? C44 C43 P3 115.1(6) . . ? C44 C43 H43A 108.5 . . ? P3 C43 H43A 108.5 . . ? C44 C43 H43B 108.5 . . ? P3 C43 H43B 108.5 . . ? H43A C43 H43B 107.5 . . ? C49 C44 C45 120.3(7) . . ? C49 C44 C43 121.8(6) . . ? C45 C44 C43 117.7(7) . . ? C44 C45 C46 117.5(7) . . ? C44 C45 H45 121.2 . . ? C46 C45 H45 121.2 . . ? C47 C46 C45 122.0(7) . . ? C47 C46 H46 119.0 . . ? C45 C46 H46 119.0 . . ? C46 C47 C48 119.2(7) . . ? C46 C47 H47 120.4 . . ? C48 C47 H47 120.4 . . ? C49 C48 C47 122.5(7) . . ? C49 C48 H48 118.8 . . ? C47 C48 H48 118.8 . . ? C48 C49 C44 118.4(7) . . ? C48 C49 C50 120.5(7) . . ? C44 C49 C50 121.0(7) . . ? C49 C50 P4 113.5(6) . . ? C49 C50 H50A 108.9 . . ? P4 C50 H50A 108.9 . . ? C49 C50 H50B 108.9 . . ? P4 C50 H50B 108.9 . . ? H50A C50 H50B 107.7 . . ? C52 C51 P4 111.6(5) . . ? C52 C51 H51A 109.3 . . ? P4 C51 H51A 109.3 . . ? C52 C51 H51B 109.3 . . ? P4 C51 H51B 109.3 . . ? H51A C51 H51B 108.0 . . ? C53 C52 C51 111.2(7) . . ? C53 C52 C58 111.4(6) . . ? C51 C52 C58 112.7(6) . . ? C53 C52 H52 107.1 . . ? C51 C52 H52 107.1 . . ? C58 C52 H52 107.1 . . ? C52 C53 C54 109.3(6) . . ? C52 C53 H53A 109.8 . . ? C54 C53 H53A 109.8 . . ? C52 C53 H53B 109.8 . . ? C54 C53 H53B 109.8 . . ? H53A C53 H53B 108.3 . . ? C55 C54 C53 109.9(6) . . ? C55 C54 H54A 109.7 . . ? C53 C54 H54A 109.7 . . ? C55 C54 H54B 109.7 . . ? C53 C54 H54B 109.7 . . ? H54A C54 H54B 108.2 . . ? C54 C55 C56 112.1(5) . . ? C54 C55 P4 111.3(5) . . ? C56 C55 P4 106.3(5) . . ? C54 C55 H55 109.0 . . ? C56 C55 H55 109.0 . . ? P4 C55 H55 109.0 . . ? C57 C56 C55 111.6(7) . . ? C57 C56 C58 114.5(6) . . ? C55 C56 C58 110.2(5) . . ? C57 C56 H56 106.7 . . ? C55 C56 H56 106.7 . . ? C58 C56 H56 106.7 . . ? C56 C57 H57A 109.5 . . ? C56 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C56 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C60 C58 C52 109.2(6) . . ? C60 C58 C59 107.9(7) . . ? C52 C58 C59 111.4(7) . . ? C60 C58 C56 111.7(7) . . ? C52 C58 C56 106.8(5) . . ? C59 C58 C56 109.7(6) . . ? C58 C59 H59A 109.5 . . ? C58 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C58 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C58 C60 H60A 109.5 . . ? C58 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C58 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? O5 C61 Mo2 177.3(7) . . ? O6 C62 Mo2 177.1(7) . . ? O7 C63 Mo2 175.7(7) . . ? O8 C64 Mo2 170.3(8) . . ? C13 P1 C14 95.3(3) . . ? C13 P1 C15 104.1(4) . . ? C14 P1 C15 103.3(3) . . ? C13 P1 Mo1 116.1(2) . . ? C14 P1 Mo1 117.6(3) . . ? C15 P1 Mo1 117.3(2) . . ? C32 P2 C23 95.8(3) . . ? C32 P2 C22 103.8(3) . . ? C23 P2 C22 105.2(3) . . ? C32 P2 Mo1 117.2(3) . . ? C23 P2 Mo1 117.1(2) . . ? C22 P2 Mo1 115.2(3) . . ? C41 P3 C42 95.2(3) . . ? C41 P3 C43 106.0(3) . . ? C42 P3 C43 101.3(4) . . ? C41 P3 Mo2 114.0(2) . . ? C42 P3 Mo2 119.7(2) . . ? C43 P3 Mo2 117.6(2) . . ? C51 P4 C50 103.4(3) . . ? C51 P4 C55 94.3(3) . . ? C50 P4 C55 104.4(3) . . ? C51 P4 Mo2 119.0(3) . . ? C50 P4 Mo2 115.4(2) . . ? C55 P4 Mo2 117.3(2) . . ? C4 Mo1 C1 91.9(3) . . ? C4 Mo1 C2 89.4(3) . . ? C1 Mo1 C2 87.6(3) . . ? C4 Mo1 C3 86.0(3) . . ? C1 Mo1 C3 86.6(3) . . ? C2 Mo1 C3 172.5(3) . . ? C4 Mo1 P2 179.4(2) . . ? C1 Mo1 P2 88.7(2) . . ? C2 Mo1 P2 90.5(2) . . ? C3 Mo1 P2 94.2(2) . . ? C4 Mo1 P1 93.6(2) . . ? C1 Mo1 P1 174.4(2) . . ? C2 Mo1 P1 91.3(2) . . ? C3 Mo1 P1 94.91(19) . . ? P2 Mo1 P1 85.77(7) . . ? C61 Mo2 C62 88.3(3) . . ? C61 Mo2 C63 90.6(3) . . ? C62 Mo2 C63 86.3(3) . . ? C61 Mo2 C64 84.5(3) . . ? C62 Mo2 C64 87.6(3) . . ? C63 Mo2 C64 172.3(3) . . ? C61 Mo2 P4 92.1(2) . . ? C62 Mo2 P4 177.8(2) . . ? C63 Mo2 P4 91.6(2) . . ? C64 Mo2 P4 94.6(2) . . ? C61 Mo2 P3 177.5(2) . . ? C62 Mo2 P3 90.6(2) . . ? C63 Mo2 P3 91.7(2) . . ? C64 Mo2 P3 93.2(2) . . ? P4 Mo2 P3 88.97(7) . . ? C66A C65A C70A 120.0 . . ? C66A C65A C71A 112.0(4) . . ? C70A C65A C71A 128.0(4) . . ? C67A C66A C65A 120.0 . . ? C67A C66A H66A 120.0 . . ? C65A C66A H66A 120.0 . . ? C66A C67A C68A 120.0 . . ? C66A C67A H67A 120.0 . . ? C68A C67A H67A 120.0 . . ? C67A C68A C69A 120.0 . . ? C67A C68A H68A 120.0 . . ? C69A C68A H68A 120.0 . . ? C70A C69A C68A 120.0 . . ? C70A C69A H69A 120.0 . . ? C68A C69A H69A 120.0 . . ? C69A C70A C65A 120.0 . . ? C69A C70A H70A 120.0 . . ? C65A C70A H70A 120.0 . . ? C65A C71A H71A 109.5 . . ? C65A C71A H71B 109.5 . . ? H71A C71A H71B 109.5 . . ? C65A C71A H71C 109.5 . . ? H71A C71A H71C 109.5 . . ? H71B C71A H71C 109.5 . . ? C66B C65B C70B 120.0 . . ? C66B C65B C71B 121.6(7) . . ? C70B C65B C71B 118.1(7) . . ? C67B C66B C65B 120.0 . . ? C67B C66B H66B 120.0 . . ? C65B C66B H66B 120.0 . . ? C66B C67B C68B 120.0 . . ? C66B C67B H67B 120.0 . . ? C68B C67B H67B 120.0 . . ? C69B C68B C67B 120.0 . . ? C69B C68B H68B 120.0 . . ? C67B C68B H68B 120.0 . . ? C68B C69B C70B 120.0 . . ? C68B C69B H69B 120.0 . . ? C70B C69B H69B 120.0 . . ? C65B C70B C69B 120.0 . . ? C65B C70B H70B 120.0 . . ? C69B C70B H70B 120.0 . . ? C65B C71B H71D 109.5 . . ? C65B C71B H71E 109.5 . . ? H71D C71B H71E 109.5 . . ? C65B C71B H71F 109.5 . . ? H71D C71B H71F 109.5 . . ? H71E C71B H71F 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 C14 C6 C8 C10 -20.6(7) . . . . ? C5 C6 C8 C10 -147.0(6) . . . . ? C14 C6 C8 C7 -141.4(6) . . . . ? C5 C6 C8 C7 92.2(8) . . . . ? C14 C6 C8 C9 100.3(7) . . . . ? C5 C6 C8 C9 -26.1(9) . . . . ? C7 C8 C10 C13 66.4(8) . . . . ? C6 C8 C10 C13 -53.8(8) . . . . ? C9 C8 C10 C13 -177.5(7) . . . . ? C7 C8 C10 C11 -171.9(6) . . . . ? C6 C8 C10 C11 67.9(7) . . . . ? C9 C8 C10 C11 -55.8(8) . . . . ? C8 C10 C11 C12 -46.9(8) . . . . ? C13 C10 C11 C12 77.6(8) . . . . ? C10 C11 C12 C14 -18.1(9) . . . . ? C8 C10 C13 P1 67.7(7) . . . . ? C11 C10 C13 P1 -55.2(8) . . . . ? C5 C6 C14 C12 85.3(8) . . . . ? C8 C6 C14 C12 -42.5(8) . . . . ? C5 C6 C14 P1 -154.5(6) . . . . ? C8 C6 C14 P1 77.8(6) . . . . ? C11 C12 C14 C6 64.2(8) . . . . ? C11 C12 C14 P1 -52.4(7) . . . . ? P1 C15 C16 C21 -69.8(10) . . . . ? P1 C15 C16 C17 115.1(7) . . . . ? C21 C16 C17 C18 0.4(12) . . . . ? C15 C16 C17 C18 175.6(8) . . . . ? C16 C17 C18 C19 -0.5(12) . . . . ? C17 C18 C19 C20 -1.6(12) . . . . ? C18 C19 C20 C21 3.8(11) . . . . ? C17 C16 C21 C20 1.6(11) . . . . ? C15 C16 C21 C20 -173.4(7) . . . . ? C17 C16 C21 C22 -177.5(7) . . . . ? C15 C16 C21 C22 7.5(12) . . . . ? C19 C20 C21 C16 -3.7(11) . . . . ? C19 C20 C21 C22 175.4(7) . . . . ? C16 C21 C22 P2 90.9(8) . . . . ? C20 C21 C22 P2 -88.2(8) . . . . ? C31 C23 C24 C25 86.1(7) . . . . ? P2 C23 C24 C25 -154.2(5) . . . . ? C31 C23 C24 C26 -41.8(7) . . . . ? P2 C23 C24 C26 77.9(6) . . . . ? C25 C24 C26 C28 91.7(7) . . . . ? C23 C24 C26 C28 -141.9(6) . . . . ? C25 C24 C26 C27 -27.0(8) . . . . ? C23 C24 C26 C27 99.3(6) . . . . ? C25 C24 C26 C29 -147.2(6) . . . . ? C23 C24 C26 C29 -20.9(7) . . . . ? C28 C26 C29 C30 -172.4(6) . . . . ? C27 C26 C29 C30 -53.3(7) . . . . ? C24 C26 C29 C30 68.8(7) . . . . ? C28 C26 C29 C32 64.3(7) . . . . ? C27 C26 C29 C32 -176.5(5) . . . . ? C24 C26 C29 C32 -54.5(7) . . . . ? C32 C29 C30 C31 73.2(7) . . . . ? C26 C29 C30 C31 -49.9(7) . . . . ? C24 C23 C31 C30 62.1(7) . . . . ? P2 C23 C31 C30 -54.4(7) . . . . ? C29 C30 C31 C23 -14.7(8) . . . . ? C30 C29 C32 P2 -51.3(7) . . . . ? C26 C29 C32 P2 70.9(6) . . . . ? C33 C34 C35 C36 -25.9(8) . . . . ? C41 C34 C35 C36 100.5(6) . . . . ? C33 C34 C35 C37 92.6(7) . . . . ? C41 C34 C35 C37 -141.0(6) . . . . ? C33 C34 C35 C38 -149.1(5) . . . . ? C41 C34 C35 C38 -22.7(7) . . . . ? C36 C35 C38 C42 -176.1(5) . . . . ? C37 C35 C38 C42 66.8(7) . . . . ? C34 C35 C38 C42 -50.2(7) . . . . ? C36 C35 C38 C39 -56.5(7) . . . . ? C37 C35 C38 C39 -173.5(6) . . . . ? C34 C35 C38 C39 69.4(7) . . . . ? C42 C38 C39 C40 76.3(7) . . . . ? C35 C38 C39 C40 -45.0(7) . . . . ? C38 C39 C40 C41 -22.4(8) . . . . ? C39 C40 C41 C34 67.9(7) . . . . ? C39 C40 C41 P3 -49.7(7) . . . . ? C33 C34 C41 C40 84.8(7) . . . . ? C35 C34 C41 C40 -42.7(7) . . . . ? C33 C34 C41 P3 -153.8(5) . . . . ? C35 C34 C41 P3 78.7(6) . . . . ? C35 C38 C42 P3 70.5(6) . . . . ? C39 C38 C42 P3 -49.6(8) . . . . ? P3 C43 C44 C49 -80.4(9) . . . . ? P3 C43 C44 C45 102.8(7) . . . . ? C49 C44 C45 C46 2.5(12) . . . . ? C43 C44 C45 C46 179.3(7) . . . . ? C44 C45 C46 C47 -1.4(12) . . . . ? C45 C46 C47 C48 0.1(13) . . . . ? C46 C47 C48 C49 0.1(14) . . . . ? C47 C48 C49 C44 1.0(13) . . . . ? C47 C48 C49 C50 178.9(8) . . . . ? C45 C44 C49 C48 -2.3(12) . . . . ? C43 C44 C49 C48 -179.0(7) . . . . ? C45 C44 C49 C50 179.8(7) . . . . ? C43 C44 C49 C50 3.1(12) . . . . ? C48 C49 C50 P4 -87.6(8) . . . . ? C44 C49 C50 P4 90.3(9) . . . . ? P4 C51 C52 C53 -55.6(7) . . . . ? P4 C51 C52 C58 70.3(7) . . . . ? C51 C52 C53 C54 76.3(7) . . . . ? C58 C52 C53 C54 -50.3(8) . . . . ? C52 C53 C54 C55 -14.9(8) . . . . ? C53 C54 C55 C56 63.8(7) . . . . ? C53 C54 C55 P4 -55.2(7) . . . . ? C54 C55 C56 C57 85.1(7) . . . . ? P4 C55 C56 C57 -153.0(5) . . . . ? C54 C55 C56 C58 -43.3(8) . . . . ? P4 C55 C56 C58 78.6(6) . . . . ? C53 C52 C58 C60 -51.0(9) . . . . ? C51 C52 C58 C60 -176.9(7) . . . . ? C53 C52 C58 C59 -170.2(6) . . . . ? C51 C52 C58 C59 64.0(8) . . . . ? C53 C52 C58 C56 70.0(8) . . . . ? C51 C52 C58 C56 -55.8(8) . . . . ? C57 C56 C58 C60 -27.1(10) . . . . ? C55 C56 C58 C60 99.7(7) . . . . ? C57 C56 C58 C52 -146.5(7) . . . . ? C55 C56 C58 C52 -19.7(8) . . . . ? C57 C56 C58 C59 92.5(9) . . . . ? C55 C56 C58 C59 -140.6(6) . . . . ? C10 C13 P1 C14 -8.6(6) . . . . ? C10 C13 P1 C15 96.6(6) . . . . ? C10 C13 P1 Mo1 -132.9(5) . . . . ? C6 C14 P1 C13 -55.6(5) . . . . ? C12 C14 P1 C13 63.8(5) . . . . ? C6 C14 P1 C15 -161.4(5) . . . . ? C12 C14 P1 C15 -42.0(6) . . . . ? C6 C14 P1 Mo1 67.6(5) . . . . ? C12 C14 P1 Mo1 -173.0(4) . . . . ? C16 C15 P1 C13 128.9(6) . . . . ? C16 C15 P1 C14 -132.1(6) . . . . ? C16 C15 P1 Mo1 -1.0(8) . . . . ? C29 C32 P2 C23 -12.0(6) . . . . ? C29 C32 P2 C22 95.2(5) . . . . ? C29 C32 P2 Mo1 -136.5(4) . . . . ? C31 C23 P2 C32 65.6(5) . . . . ? C24 C23 P2 C32 -54.4(5) . . . . ? C31 C23 P2 C22 -40.5(5) . . . . ? C24 C23 P2 C22 -160.5(4) . . . . ? C31 C23 P2 Mo1 -169.8(4) . . . . ? C24 C23 P2 Mo1 70.2(4) . . . . ? C21 C22 P2 C32 80.2(6) . . . . ? C21 C22 P2 C23 -179.8(5) . . . . ? C21 C22 P2 Mo1 -49.3(5) . . . . ? C40 C41 P3 C42 66.3(5) . . . . ? C34 C41 P3 C42 -52.1(5) . . . . ? C40 C41 P3 C43 -37.1(6) . . . . ? C34 C41 P3 C43 -155.4(5) . . . . ? C40 C41 P3 Mo2 -167.9(4) . . . . ? C34 C41 P3 Mo2 73.7(5) . . . . ? C38 C42 P3 C41 -13.8(6) . . . . ? C38 C42 P3 C43 93.7(6) . . . . ? C38 C42 P3 Mo2 -135.2(4) . . . . ? C44 C43 P3 C41 -108.5(6) . . . . ? C44 C43 P3 C42 152.7(5) . . . . ? C44 C43 P3 Mo2 20.2(6) . . . . ? C52 C51 P4 C50 96.0(6) . . . . ? C52 C51 P4 C55 -9.8(6) . . . . ? C52 C51 P4 Mo2 -134.4(5) . . . . ? C49 C50 P4 C51 91.3(6) . . . . ? C49 C50 P4 C55 -170.6(5) . . . . ? C49 C50 P4 Mo2 -40.5(6) . . . . ? C54 C55 P4 C51 65.5(5) . . . . ? C56 C55 P4 C51 -56.9(5) . . . . ? C54 C55 P4 C50 -39.6(6) . . . . ? C56 C55 P4 C50 -162.0(4) . . . . ? C54 C55 P4 Mo2 -168.7(4) . . . . ? C56 C55 P4 Mo2 68.9(5) . . . . ? C32 P2 Mo1 C1 25.8(3) . . . . ? C23 P2 Mo1 C1 -87.2(3) . . . . ? C22 P2 Mo1 C1 148.4(3) . . . . ? C32 P2 Mo1 C2 113.4(3) . . . . ? C23 P2 Mo1 C2 0.4(3) . . . . ? C22 P2 Mo1 C2 -124.0(3) . . . . ? C32 P2 Mo1 C3 -60.7(3) . . . . ? C23 P2 Mo1 C3 -173.7(3) . . . . ? C22 P2 Mo1 C3 61.9(3) . . . . ? C32 P2 Mo1 P1 -155.4(2) . . . . ? C23 P2 Mo1 P1 91.7(3) . . . . ? C22 P2 Mo1 P1 -32.8(2) . . . . ? C13 P1 Mo1 C4 116.4(3) . . . . ? C14 P1 Mo1 C4 4.6(3) . . . . ? C15 P1 Mo1 C4 -119.6(4) . . . . ? C13 P1 Mo1 C2 27.0(4) . . . . ? C14 P1 Mo1 C2 -84.9(3) . . . . ? C15 P1 Mo1 C2 150.9(4) . . . . ? C13 P1 Mo1 C3 -157.3(4) . . . . ? C14 P1 Mo1 C3 90.9(3) . . . . ? C15 P1 Mo1 C3 -33.3(4) . . . . ? C13 P1 Mo1 P2 -63.5(3) . . . . ? C14 P1 Mo1 P2 -175.3(2) . . . . ? C15 P1 Mo1 P2 60.5(3) . . . . ? C51 P4 Mo2 C61 17.0(3) . . . . ? C50 P4 Mo2 C61 140.9(4) . . . . ? C55 P4 Mo2 C61 -95.5(3) . . . . ? C51 P4 Mo2 C63 107.7(3) . . . . ? C50 P4 Mo2 C63 -128.4(4) . . . . ? C55 P4 Mo2 C63 -4.8(3) . . . . ? C51 P4 Mo2 C64 -67.6(4) . . . . ? C50 P4 Mo2 C64 56.3(4) . . . . ? C55 P4 Mo2 C64 179.9(4) . . . . ? C51 P4 Mo2 P3 -160.7(3) . . . . ? C50 P4 Mo2 P3 -36.8(3) . . . . ? C55 P4 Mo2 P3 86.8(3) . . . . ? C41 P3 Mo2 C62 -9.7(3) . . . . ? C42 P3 Mo2 C62 101.8(3) . . . . ? C43 P3 Mo2 C62 -134.6(3) . . . . ? C41 P3 Mo2 C63 -96.0(3) . . . . ? C42 P3 Mo2 C63 15.5(3) . . . . ? C43 P3 Mo2 C63 139.1(3) . . . . ? C41 P3 Mo2 C64 77.9(3) . . . . ? C42 P3 Mo2 C64 -170.5(3) . . . . ? C43 P3 Mo2 C64 -47.0(4) . . . . ? C41 P3 Mo2 P4 172.4(2) . . . . ? C42 P3 Mo2 P4 -76.0(3) . . . . ? C43 P3 Mo2 P4 47.5(3) . . . . ? C70A C65A C66A C67A 0.0 . . . . ? C71A C65A C66A C67A -177.0(5) . . . . ? C65A C66A C67A C68A 0.0 . . . . ? C66A C67A C68A C69A 0.0 . . . . ? C67A C68A C69A C70A 0.0 . . . . ? C68A C69A C70A C65A 0.0 . . . . ? C66A C65A C70A C69A 0.0 . . . . ? C71A C65A C70A C69A 176.5(6) . . . . ? C70B C65B C66B C67B 0.0 . . . . ? C71B C65B C66B C67B -173(2) . . . . ? C65B C66B C67B C68B 0.0 . . . . ? C66B C67B C68B C69B 0.0 . . . . ? C67B C68B C69B C70B 0.0 . . . . ? C66B C65B C70B C69B 0.0 . . . . ? C71B C65B C70B C69B 173(2) . . . . ? C68B C69B C70B C65B 0.0 . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.755 _refine_diff_density_min -1.169 _refine_diff_density_rms 0.109 _chemical_absolute_configuration rm