# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Peter Junk' _publ_contact_author_email daisy.pathmarajan@monash.edu loop_ _publ_author_name D.P.Daniels G.B.Deacon F.Jaroschik P.Junk # Attachment '- 8b.CIF' data_8b.CIF _database_code_depnum_ccdc_archive 'CCDC 795650' #TrackingRef '- 8b.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common DPBa _chemical_melting_point ? _chemical_formula_moiety 'C42 H48 Ba O4 P2' _chemical_formula_sum 'C42 H48 Ba O4 P2' _chemical_formula_weight 816.08 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' Ba Ba -0.3244 2.2819 '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 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 9.2423(12) _cell_length_b 17.0996(15) _cell_length_c 25.117(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3969.5(7) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 13592 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 27.50 _exptl_crystal_description Needles _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.366 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1672 _exptl_absorpt_coefficient_mu 1.120 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8727 _exptl_absorpt_correction_T_max 0.9725 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 X8 Apex II CCD' _diffrn_measurement_method 'Phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13592 _diffrn_reflns_av_R_equivalents 0.0930 _diffrn_reflns_av_sigmaI/netI 0.2305 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.35 _diffrn_reflns_theta_max 27.50 _reflns_number_total 8932 _reflns_number_gt 4908 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker)' _computing_cell_refinement 'Bruker SMART (Bruker)' _computing_data_reduction 'Bruker SMART (Bruker)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _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^)+(0.0109P)^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 ? _refine_ls_extinction_coef none _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.01(3) _refine_ls_number_reflns 8932 _refine_ls_number_parameters 422 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1594 _refine_ls_R_factor_gt 0.0770 _refine_ls_wR_factor_ref 0.1214 _refine_ls_wR_factor_gt 0.0961 _refine_ls_goodness_of_fit_ref 0.949 _refine_ls_restrained_S_all 0.949 _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 Ba1 Ba 0.26700(6) 0.88494(3) 0.78305(2) 0.01889(12) Uani 1 1 d . . . P1 P 0.2344(3) 1.11057(15) 0.86319(8) 0.0259(5) Uani 1 1 d . . . P2 P 0.2661(4) 0.64786(12) 0.84640(8) 0.0255(6) Uani 1 1 d . . . O1 O 0.4728(7) 0.7836(4) 0.7361(2) 0.0263(18) Uani 1 1 d . . . O2 O 0.1981(8) 0.8004(4) 0.6878(2) 0.0321(19) Uani 1 1 d . . . O3 O 0.3360(9) 0.9704(4) 0.6875(3) 0.042(2) Uani 1 1 d . . . O4 O 0.0652(9) 0.9868(4) 0.7347(3) 0.051(2) Uani 1 1 d . . . C1 C 0.3970(12) 0.9664(6) 0.8808(4) 0.0294(19) Uani 1 1 d . . . H1 H 0.3535 0.9498 0.9131 0.035 Uiso 1 1 calc R . . C2 C 0.5175(13) 0.9312(6) 0.8559(4) 0.037(3) Uani 1 1 d . . . H2 H 0.5696 0.8873 0.8688 0.045 Uiso 1 1 calc R . . C3 C 0.5470(14) 0.9723(6) 0.8088(5) 0.043(2) Uani 1 1 d . . . H3 H 0.6216 0.9607 0.7840 0.051 Uiso 1 1 calc R . . C4 C 0.4486(12) 1.0326(6) 0.8049(4) 0.033(2) Uani 1 1 d . . . H4 H 0.4452 1.0699 0.7769 0.039 Uiso 1 1 calc R . . C5 C 0.3525(11) 1.0301(5) 0.8495(3) 0.021(2) Uani 1 1 d . . . C6 C 0.1645(11) 0.7375(5) 0.8457(3) 0.022(2) Uani 1 1 d . . . C7 C 0.1628(13) 0.7995(6) 0.8825(4) 0.033(2) Uani 1 1 d . . . H7 H 0.2277 0.8058 0.9115 0.039 Uiso 1 1 calc R . . C8 C 0.0501(13) 0.8503(6) 0.8694(5) 0.043(2) Uani 1 1 d . . . H8 H 0.0256 0.8969 0.8879 0.051 Uiso 1 1 calc R . . C9 C -0.0200(12) 0.8212(6) 0.8248(5) 0.042(3) Uani 1 1 d . . . H9 H -0.1011 0.8439 0.8075 0.050 Uiso 1 1 calc R . . C10 C 0.0514(12) 0.7518(5) 0.8099(4) 0.0294(19) Uani 1 1 d . . . H10 H 0.0267 0.7198 0.7803 0.035 Uiso 1 1 calc R . . C11 C -0.0601(17) 1.0097(8) 0.7580(5) 0.092(6) Uani 1 1 d . . . H11A H -0.0552 1.0656 0.7663 0.137 Uiso 1 1 calc R . . H11B H -0.0749 0.9799 0.7909 0.137 Uiso 1 1 calc R . . H11C H -0.1410 1.0000 0.7336 0.137 Uiso 1 1 calc R . . C12 C 0.1270(14) 1.0443(7) 0.6989(5) 0.059(4) Uani 1 1 d . . . H12A H 0.1811 1.0838 0.7197 0.071 Uiso 1 1 calc R . . H12B H 0.0484 1.0715 0.6795 0.071 Uiso 1 1 calc R . . C13 C 0.2255(18) 1.0065(7) 0.6602(4) 0.070(5) Uani 1 1 d . . . H13A H 0.1717 0.9674 0.6389 0.084 Uiso 1 1 calc R . . H13B H 0.2657 1.0462 0.6356 0.084 Uiso 1 1 calc R . . C14 C 0.4445(17) 0.9470(7) 0.6514(5) 0.081(5) Uani 1 1 d . . . H14A H 0.4019 0.9137 0.6238 0.122 Uiso 1 1 calc R . . H14B H 0.5195 0.9177 0.6705 0.122 Uiso 1 1 calc R . . H14C H 0.4877 0.9933 0.6348 0.122 Uiso 1 1 calc R . . C15 C 0.0558(13) 0.7944(6) 0.6661(4) 0.045(3) Uani 1 1 d . . . H15A H 0.0620 0.7814 0.6282 0.068 Uiso 1 1 calc R . . H15B H 0.0053 0.8444 0.6704 0.068 Uiso 1 1 calc R . . H15C H 0.0023 0.7532 0.6848 0.068 Uiso 1 1 calc R . . C16 C 0.2746(14) 0.7273(5) 0.6881(4) 0.036(3) Uani 1 1 d . . . H16A H 0.2486 0.6966 0.6560 0.043 Uiso 1 1 calc R . . H16B H 0.2469 0.6966 0.7199 0.043 Uiso 1 1 calc R . . C17 C 0.4326(13) 0.7422(6) 0.6886(4) 0.028(3) Uani 1 1 d . . . H17A H 0.4854 0.6919 0.6871 0.034 Uiso 1 1 calc R . . H17B H 0.4599 0.7734 0.6570 0.034 Uiso 1 1 calc R . . C18 C 0.6264(11) 0.7886(6) 0.7403(4) 0.038(3) Uani 1 1 d . . . H18A H 0.6680 0.7359 0.7393 0.056 Uiso 1 1 calc R . . H18B H 0.6523 0.8140 0.7739 0.056 Uiso 1 1 calc R . . H18C H 0.6645 0.8193 0.7104 0.056 Uiso 1 1 calc R . . C19 C 0.3464(11) 1.1697(5) 0.9087(4) 0.022(2) Uani 1 1 d . . . C20 C 0.2993(11) 1.2435(5) 0.9243(4) 0.028(2) Uani 1 1 d . . . H20 H 0.2053 1.2604 0.9143 0.034 Uiso 1 1 calc R . . C21 C 0.3863(13) 1.2931(6) 0.9543(4) 0.035(3) Uani 1 1 d . . . H21 H 0.3511 1.3430 0.9648 0.042 Uiso 1 1 calc R . . C22 C 0.5230(15) 1.2700(6) 0.9687(5) 0.048(3) Uani 1 1 d . . . H22 H 0.5820 1.3039 0.9893 0.058 Uiso 1 1 calc R . . C23 C 0.5753(13) 1.1981(6) 0.9535(4) 0.029(3) Uani 1 1 d . . . H23 H 0.6705 1.1823 0.9629 0.035 Uiso 1 1 calc R . . C24 C 0.4862(12) 1.1490(5) 0.9241(4) 0.025(3) Uani 1 1 d . . . H24 H 0.5220 1.0990 0.9141 0.030 Uiso 1 1 calc R . . C25 C 0.0985(12) 1.0698(5) 0.9098(4) 0.029(3) Uani 1 1 d . . . C26 C -0.0425(14) 1.0644(6) 0.8942(6) 0.048(4) Uani 1 1 d . . . H26 H -0.0712 1.0856 0.8609 0.058 Uiso 1 1 calc R . . C27 C -0.1451(13) 1.0282(6) 0.9267(6) 0.074(5) Uani 1 1 d . . . H27 H -0.2426 1.0245 0.9150 0.088 Uiso 1 1 calc R . . C28 C -0.1079(16) 0.9984(7) 0.9746(5) 0.048(3) Uani 1 1 d . . . H28 H -0.1781 0.9721 0.9956 0.058 Uiso 1 1 calc R . . C29 C 0.0313(18) 1.0062(7) 0.9929(5) 0.063(5) Uani 1 1 d . . . H5 H 0.0565 0.9879 1.0274 0.075 Uiso 1 1 calc R . . C30 C 0.1361(14) 1.0415(6) 0.9602(4) 0.045(3) Uani 1 1 d . . . H30 H 0.2330 1.0462 0.9724 0.054 Uiso 1 1 calc R . . C31 C 0.4248(12) 0.6733(5) 0.8860(4) 0.022(3) Uani 1 1 d . . . C32 C 0.5537(12) 0.6888(6) 0.8608(4) 0.033(3) Uani 1 1 d . . . H32 H 0.5600 0.6828 0.8233 0.039 Uiso 1 1 calc R . . C33 C 0.6744(14) 0.7128(6) 0.8889(5) 0.055(4) Uani 1 1 d . . . H33 H 0.7606 0.7255 0.8702 0.066 Uiso 1 1 calc R . . C34 C 0.6720(13) 0.7184(6) 0.9422(5) 0.045(3) Uani 1 1 d . . . H34 H 0.7566 0.7329 0.9613 0.054 Uiso 1 1 calc R . . C35 C 0.5434(16) 0.7027(7) 0.9691(5) 0.052(4) Uani 1 1 d . . . H35 H 0.5394 0.7083 1.0067 0.062 Uiso 1 1 calc R . . C36 C 0.4228(12) 0.6794(6) 0.9418(4) 0.036(3) Uani 1 1 d . . . H36 H 0.3368 0.6671 0.9607 0.043 Uiso 1 1 calc R . . C37 C 0.1627(12) 0.5888(5) 0.8952(4) 0.026(3) Uani 1 1 d . . . C38 C 0.0589(13) 0.6189(7) 0.9285(4) 0.043(3) Uani 1 1 d . . . H38 H 0.0386 0.6734 0.9278 0.052 Uiso 1 1 calc R . . C39 C -0.0171(16) 0.5702(7) 0.9632(5) 0.053(4) Uani 1 1 d . . . H39 H -0.0871 0.5917 0.9867 0.063 Uiso 1 1 calc R . . C40 C 0.0092(14) 0.4908(8) 0.9634(5) 0.048(4) Uani 1 1 d . . . H40 H -0.0417 0.4583 0.9877 0.058 Uiso 1 1 calc R . . C41 C 0.1066(14) 0.4583(6) 0.9296(5) 0.042(3) Uani 1 1 d . . . H41 H 0.1226 0.4035 0.9296 0.050 Uiso 1 1 calc R . . C42 C 0.1841(12) 0.5074(6) 0.8944(4) 0.035(3) Uani 1 1 d . . . H42 H 0.2509 0.4852 0.8699 0.042 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ba1 0.0194(3) 0.0167(2) 0.0205(2) -0.0013(3) 0.0000(3) -0.0007(3) P1 0.0319(15) 0.0221(11) 0.0238(11) -0.0028(11) -0.0080(14) 0.0059(18) P2 0.0364(18) 0.0204(12) 0.0198(12) -0.0006(9) 0.0026(17) 0.0008(14) O1 0.028(4) 0.027(4) 0.024(4) -0.009(3) -0.002(3) 0.005(3) O2 0.033(5) 0.026(4) 0.037(4) -0.003(3) -0.010(4) -0.001(3) O3 0.057(6) 0.036(5) 0.033(5) 0.013(4) 0.001(5) -0.011(4) O4 0.045(6) 0.039(5) 0.070(7) 0.018(4) -0.002(5) 0.006(4) C1 0.038(5) 0.021(4) 0.029(4) -0.007(3) -0.010(4) 0.001(4) C2 0.039(8) 0.028(7) 0.045(8) -0.018(5) -0.015(6) -0.003(5) C3 0.034(5) 0.032(5) 0.063(6) -0.012(4) 0.022(5) -0.008(4) C4 0.040(5) 0.028(5) 0.031(5) 0.000(3) 0.001(4) -0.018(4) C5 0.029(6) 0.019(6) 0.015(5) -0.011(4) 0.000(5) -0.005(4) C6 0.031(6) 0.017(5) 0.016(5) -0.005(4) 0.006(5) -0.007(4) C7 0.040(5) 0.028(5) 0.031(5) 0.000(3) 0.001(4) -0.018(4) C8 0.034(5) 0.032(5) 0.063(6) -0.012(4) 0.022(5) -0.008(4) C9 0.024(7) 0.018(6) 0.084(10) 0.010(6) 0.004(7) -0.007(5) C10 0.038(5) 0.021(4) 0.029(4) -0.007(3) -0.010(4) 0.001(4) C11 0.093(14) 0.111(14) 0.071(11) 0.047(9) 0.031(10) 0.065(11) C12 0.056(9) 0.045(8) 0.077(11) 0.043(7) -0.010(8) 0.012(7) C13 0.084(13) 0.082(10) 0.043(7) 0.030(7) -0.019(10) -0.050(11) C14 0.096(14) 0.100(13) 0.048(9) 0.019(8) 0.039(10) 0.007(10) C15 0.047(9) 0.035(8) 0.054(8) 0.003(6) -0.032(7) -0.014(6) C16 0.046(7) 0.032(6) 0.029(5) -0.007(4) -0.007(7) 0.006(7) C17 0.041(8) 0.018(6) 0.025(6) -0.007(5) 0.003(6) 0.001(5) C18 0.021(6) 0.043(7) 0.049(7) 0.006(5) -0.004(6) 0.004(5) C19 0.021(6) 0.020(6) 0.025(6) 0.012(4) 0.004(5) -0.004(4) C20 0.020(6) 0.016(5) 0.048(6) -0.003(5) 0.003(6) -0.001(4) C21 0.044(8) 0.016(6) 0.045(7) -0.017(5) 0.008(6) -0.009(5) C22 0.058(7) 0.029(5) 0.058(7) -0.010(4) 0.020(6) -0.006(5) C23 0.041(8) 0.026(6) 0.020(6) 0.002(5) -0.014(5) -0.021(6) C24 0.044(7) 0.014(5) 0.018(5) -0.004(5) 0.005(6) -0.003(5) C25 0.026(7) 0.013(6) 0.048(8) -0.018(5) 0.003(6) -0.003(5) C26 0.034(8) 0.013(6) 0.097(11) -0.003(6) -0.017(8) 0.003(5) C27 0.016(7) 0.019(7) 0.187(17) -0.005(9) 0.006(10) 0.003(5) C28 0.058(7) 0.029(5) 0.058(7) -0.010(4) 0.020(6) -0.006(5) C29 0.100(14) 0.046(9) 0.042(8) -0.024(7) 0.029(9) -0.031(9) C30 0.045(9) 0.057(8) 0.032(7) -0.010(6) 0.017(7) -0.028(7) C31 0.036(7) 0.007(5) 0.024(6) -0.002(4) -0.006(5) -0.004(5) C32 0.027(7) 0.038(7) 0.034(7) 0.013(5) -0.004(6) 0.009(6) C33 0.051(10) 0.036(7) 0.078(10) 0.017(7) -0.019(8) -0.001(6) C34 0.030(7) 0.037(7) 0.067(9) -0.003(6) -0.027(7) 0.002(6) C35 0.073(11) 0.049(9) 0.033(8) -0.006(6) -0.030(8) -0.013(8) C36 0.026(7) 0.044(8) 0.037(7) -0.002(6) -0.006(6) 0.002(6) C37 0.038(7) 0.014(5) 0.025(6) -0.003(4) -0.019(5) -0.008(4) C38 0.073(9) 0.028(6) 0.029(6) 0.009(6) 0.010(6) -0.004(7) C39 0.064(11) 0.053(9) 0.042(8) 0.016(7) 0.009(8) -0.003(8) C40 0.035(8) 0.058(10) 0.051(9) 0.024(7) -0.022(7) -0.016(7) C41 0.051(8) 0.022(6) 0.052(8) 0.014(6) -0.025(7) -0.019(6) C42 0.028(7) 0.033(7) 0.044(7) -0.005(5) -0.010(6) 0.000(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 Ba1 O4 2.827(8) . ? Ba1 O1 2.831(6) . ? Ba1 O2 2.867(6) . ? Ba1 O3 2.881(7) . ? Ba1 C8 3.011(11) . ? Ba1 C7 3.049(10) . ? Ba1 C9 3.053(11) . ? Ba1 C2 3.055(10) . ? Ba1 C3 3.058(12) . ? Ba1 C1 3.067(10) . ? Ba1 C4 3.081(10) . ? Ba1 C5 3.094(8) . ? P1 C5 1.790(10) . ? P1 C19 1.844(10) . ? P1 C25 1.853(11) . ? P2 C6 1.798(9) . ? P2 C31 1.825(11) . ? P2 C37 1.853(10) . ? O1 C18 1.426(11) . ? O1 C17 1.434(10) . ? O2 C15 1.428(12) . ? O2 C16 1.437(10) . ? O3 C13 1.376(15) . ? O3 C14 1.410(14) . ? O4 C11 1.355(15) . ? O4 C12 1.449(12) . ? C1 C5 1.405(12) . ? C1 C2 1.411(15) . ? C2 C3 1.402(15) . ? C3 C4 1.378(15) . ? C4 C5 1.431(13) . ? C6 C10 1.400(13) . ? C6 C7 1.407(11) . ? C7 C8 1.395(14) . ? C8 C9 1.386(14) . ? C9 C10 1.409(13) . ? C12 C13 1.481(16) . ? C16 C17 1.483(17) . ? C19 C20 1.391(11) . ? C19 C24 1.394(13) . ? C20 C21 1.390(13) . ? C21 C22 1.372(16) . ? C22 C23 1.375(14) . ? C23 C24 1.388(12) . ? C25 C26 1.364(15) . ? C25 C30 1.398(14) . ? C26 C27 1.397(16) . ? C27 C28 1.350(17) . ? C28 C29 1.372(18) . ? C29 C30 1.407(15) . ? C31 C32 1.375(14) . ? C31 C36 1.403(13) . ? C32 C33 1.383(15) . ? C33 C34 1.341(14) . ? C34 C35 1.394(17) . ? C35 C36 1.369(15) . ? C37 C38 1.372(14) . ? C37 C42 1.407(12) . ? C38 C39 1.396(14) . ? C39 C40 1.379(15) . ? C40 C41 1.356(16) . ? C41 C42 1.414(14) . ? 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 O4 Ba1 O1 129.9(2) . . ? O4 Ba1 O2 78.8(2) . . ? O1 Ba1 O2 59.5(2) . . ? O4 Ba1 O3 58.4(2) . . ? O1 Ba1 O3 79.3(2) . . ? O2 Ba1 O3 67.04(19) . . ? O4 Ba1 C8 89.5(3) . . ? O1 Ba1 C8 128.8(2) . . ? O2 Ba1 C8 110.7(3) . . ? O3 Ba1 C8 147.8(3) . . ? O4 Ba1 C7 116.0(3) . . ? O1 Ba1 C7 105.1(2) . . ? O2 Ba1 C7 111.8(2) . . ? O3 Ba1 C7 174.3(3) . . ? C8 Ba1 C7 26.6(3) . . ? O4 Ba1 C9 78.1(3) . . ? O1 Ba1 C9 120.6(2) . . ? O2 Ba1 C9 85.1(3) . . ? O3 Ba1 C9 131.3(3) . . ? C8 Ba1 C9 26.4(3) . . ? C7 Ba1 C9 43.4(3) . . ? O4 Ba1 C2 126.7(3) . . ? O1 Ba1 C2 84.2(3) . . ? O2 Ba1 C2 143.0(3) . . ? O3 Ba1 C2 101.5(3) . . ? C8 Ba1 C2 97.1(3) . . ? C7 Ba1 C2 82.7(3) . . ? C9 Ba1 C2 123.0(3) . . ? O4 Ba1 C3 110.4(3) . . ? O1 Ba1 C3 79.5(3) . . ? O2 Ba1 C3 127.7(3) . . ? O3 Ba1 C3 75.0(3) . . ? C8 Ba1 C3 120.5(3) . . ? C7 Ba1 C3 109.2(3) . . ? C9 Ba1 C3 146.8(3) . . ? C2 Ba1 C3 26.5(3) . . ? O4 Ba1 C1 108.8(3) . . ? O1 Ba1 C1 110.4(3) . . ? O2 Ba1 C1 169.6(3) . . ? O3 Ba1 C1 110.4(2) . . ? C8 Ba1 C1 76.9(3) . . ? C7 Ba1 C1 71.7(3) . . ? C9 Ba1 C1 103.2(3) . . ? C2 Ba1 C1 26.6(3) . . ? C3 Ba1 C1 43.7(3) . . ? O4 Ba1 C4 86.0(3) . . ? O1 Ba1 C4 102.1(3) . . ? O2 Ba1 C4 133.0(2) . . ? O3 Ba1 C4 67.1(2) . . ? C8 Ba1 C4 113.3(3) . . ? C7 Ba1 C4 114.8(3) . . ? C9 Ba1 C4 134.8(3) . . ? C2 Ba1 C4 43.0(3) . . ? C3 Ba1 C4 25.9(3) . . ? C1 Ba1 C4 43.3(3) . . ? O4 Ba1 C5 84.6(2) . . ? O1 Ba1 C5 123.0(2) . . ? O2 Ba1 C5 155.7(2) . . ? O3 Ba1 C5 89.2(2) . . ? C8 Ba1 C5 86.5(3) . . ? C7 Ba1 C5 91.3(3) . . ? C9 Ba1 C5 108.8(3) . . ? C2 Ba1 C5 43.6(3) . . ? C3 Ba1 C5 43.7(3) . . ? C1 Ba1 C5 26.4(2) . . ? C4 Ba1 C5 26.8(2) . . ? C5 P1 C19 101.4(5) . . ? C5 P1 C25 104.2(5) . . ? C19 P1 C25 101.3(4) . . ? C6 P2 C31 102.8(4) . . ? C6 P2 C37 101.6(5) . . ? C31 P2 C37 100.6(4) . . ? C18 O1 C17 110.4(8) . . ? C18 O1 Ba1 127.0(6) . . ? C17 O1 Ba1 118.3(6) . . ? C15 O2 C16 113.1(8) . . ? C15 O2 Ba1 124.0(6) . . ? C16 O2 Ba1 109.0(5) . . ? C13 O3 C14 109.5(9) . . ? C13 O3 Ba1 118.6(7) . . ? C14 O3 Ba1 123.3(7) . . ? C11 O4 C12 114.1(9) . . ? C11 O4 Ba1 123.8(7) . . ? C12 O4 Ba1 115.1(7) . . ? C5 C1 C2 108.3(10) . . ? C5 C1 Ba1 77.9(5) . . ? C2 C1 Ba1 76.2(6) . . ? C3 C2 C1 108.3(10) . . ? C3 C2 Ba1 76.9(6) . . ? C1 C2 Ba1 77.2(6) . . ? C4 C3 C2 107.9(11) . . ? C4 C3 Ba1 78.0(7) . . ? C2 C3 Ba1 76.6(6) . . ? C3 C4 C5 109.3(9) . . ? C3 C4 Ba1 76.1(7) . . ? C5 C4 Ba1 77.1(5) . . ? C1 C5 C4 106.2(9) . . ? C1 C5 P1 131.9(8) . . ? C4 C5 P1 120.4(7) . . ? C1 C5 Ba1 75.7(5) . . ? C4 C5 Ba1 76.1(5) . . ? P1 C5 Ba1 124.4(4) . . ? C10 C6 C7 106.3(9) . . ? C10 C6 P2 123.1(7) . . ? C7 C6 P2 130.0(8) . . ? C10 C6 Ba1 76.2(5) . . ? C7 C6 Ba1 74.0(5) . . ? P2 C6 Ba1 122.4(4) . . ? C8 C7 C6 108.9(10) . . ? C8 C7 Ba1 75.2(6) . . ? C6 C7 Ba1 79.6(5) . . ? C9 C8 C7 108.4(10) . . ? C9 C8 Ba1 78.5(6) . . ? C7 C8 Ba1 78.2(6) . . ? C8 C9 C10 107.4(10) . . ? C8 C9 Ba1 75.1(6) . . ? C10 C9 Ba1 78.6(7) . . ? C6 C10 C9 109.1(9) . . ? C6 C10 Ba1 77.8(6) . . ? C9 C10 Ba1 74.9(6) . . ? O4 C12 C13 110.7(10) . . ? O3 C13 C12 108.9(9) . . ? O2 C16 C17 109.6(8) . . ? O1 C17 C16 110.4(9) . . ? C20 C19 C24 116.2(9) . . ? C20 C19 P1 119.8(7) . . ? C24 C19 P1 123.6(8) . . ? C21 C20 C19 121.7(10) . . ? C22 C21 C20 120.0(10) . . ? C21 C22 C23 120.5(11) . . ? C22 C23 C24 118.7(11) . . ? C23 C24 C19 122.9(10) . . ? C26 C25 C30 118.3(12) . . ? C26 C25 P1 119.4(10) . . ? C30 C25 P1 122.3(9) . . ? C25 C26 C27 120.7(13) . . ? C28 C27 C26 121.0(13) . . ? C27 C28 C29 120.1(14) . . ? C28 C29 C30 119.4(13) . . ? C25 C30 C29 120.4(12) . . ? C32 C31 C36 117.1(10) . . ? C32 C31 P2 119.4(8) . . ? C36 C31 P2 123.5(9) . . ? C31 C32 C33 121.4(11) . . ? C34 C33 C32 121.1(13) . . ? C33 C34 C35 119.0(12) . . ? C36 C35 C34 120.4(11) . . ? C35 C36 C31 120.8(12) . . ? C38 C37 C42 118.6(10) . . ? C38 C37 P2 124.0(8) . . ? C42 C37 P2 117.2(8) . . ? C37 C38 C39 120.6(12) . . ? C40 C39 C38 120.1(13) . . ? C41 C40 C39 121.1(12) . . ? C40 C41 C42 119.1(11) . . ? C37 C42 C41 120.4(11) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.756 _refine_diff_density_min -1.435 _refine_diff_density_rms 0.160 # Attachment '- 10b.CIF' data_10b.CIF _database_code_depnum_ccdc_archive 'CCDC 795651' #TrackingRef '- 10b.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common DP145C _chemical_melting_point ? _chemical_formula_moiety 'C54 H70 O4.50 P2 Pt Sr' _chemical_formula_sum 'C54 H70 O4.50 P2 Pt Sr' _chemical_formula_weight 1135.75 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' Sr Sr -1.5307 3.2498 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.084(3) _cell_length_b 13.542(3) _cell_length_c 15.058(3) _cell_angle_alpha 89.93(3) _cell_angle_beta 70.99(3) _cell_angle_gamma 82.52(3) _cell_volume 2498.7(9) _cell_formula_units_Z 2 _cell_measurement_temperature 123 _cell_measurement_reflns_used 25434 _cell_measurement_theta_min 1.43 _cell_measurement_theta_max 27.50 _exptl_crystal_description Needles _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.510 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1152 _exptl_absorpt_coefficient_mu 3.972 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.3539 _exptl_absorpt_correction_T_max 0.8261 _exptl_absorpt_process_details SORTAV _exptl_special_details ; ? ; _diffrn_ambient_temperature 123 _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 'Nonius KappaCCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25434 _diffrn_reflns_av_R_equivalents 0.1135 _diffrn_reflns_av_sigmaI/netI 0.1899 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.43 _diffrn_reflns_theta_max 27.50 _reflns_number_total 11393 _reflns_number_gt 6656 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Hooft, 1999)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _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^)+(0.0651P)^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 ? _refine_ls_extinction_coef none _refine_ls_number_reflns 11393 _refine_ls_number_parameters 557 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1552 _refine_ls_R_factor_gt 0.0710 _refine_ls_wR_factor_ref 0.1560 _refine_ls_wR_factor_gt 0.1266 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.008 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.74877(3) 0.11122(3) 0.20687(2) 0.01831(12) Uani 1 1 d . . . Sr1 Sr 0.64246(7) 0.49701(6) 0.21518(5) 0.0166(2) Uani 1 1 d . . . P1 P 0.69891(19) 0.19876(16) 0.09249(14) 0.0170(5) Uani 1 1 d . . . P2 P 0.82563(19) 0.23054(17) 0.26169(14) 0.0171(5) Uani 1 1 d . . . O1 O 0.8004(5) 0.6073(4) 0.1835(4) 0.0234(14) Uani 1 1 d . . . O2 O 0.5524(5) 0.6807(4) 0.2455(4) 0.0244(15) Uani 1 1 d . . . O3 O 0.4289(5) 0.5090(4) 0.2663(4) 0.0264(15) Uani 1 1 d . . . O4 O 1.3166(10) 0.2445(6) 0.4612(6) 0.084(3) Uani 1 1 d . . . O5 O 0.9983(11) 0.4863(9) 0.3958(8) 0.034(3) Uiso 0.50 1 d P A -1 C1 C 0.6031(7) 0.3951(6) 0.0625(5) 0.021(2) Uani 1 1 d . . . H1 H 0.5310 0.3801 0.0747 0.025 Uiso 1 1 calc R . . C2 C 0.6397(8) 0.4834(6) 0.0270(5) 0.024(2) Uani 1 1 d . . . H2 H 0.5969 0.5387 0.0117 0.029 Uiso 1 1 calc R . . C3 C 0.7503(8) 0.4771(6) 0.0177(5) 0.020(2) Uani 1 1 d . . . H3 H 0.7965 0.5264 -0.0058 0.024 Uiso 1 1 calc R . . C4 C 0.7797(8) 0.3845(6) 0.0494(5) 0.023(2) Uani 1 1 d . . . H4 H 0.8503 0.3606 0.0518 0.028 Uiso 1 1 calc R . . C5 C 0.6892(7) 0.3315(6) 0.0775(5) 0.0165(19) Uani 1 1 d . . . C6 C 0.7395(7) 0.3433(6) 0.3074(5) 0.0171(19) Uani 1 1 d . . . C7 C 0.7648(7) 0.4335(6) 0.3402(5) 0.0142(19) Uani 1 1 d . . . H7 H 0.8354 0.4531 0.3254 0.017 Uiso 1 1 calc R . . C8 C 0.6654(7) 0.4883(6) 0.3989(5) 0.020(2) Uani 1 1 d . . . H8 H 0.6577 0.5514 0.4297 0.024 Uiso 1 1 calc R . . C9 C 0.5795(8) 0.4318(7) 0.4032(5) 0.026(2) Uani 1 1 d . . . H9 H 0.5045 0.4501 0.4382 0.031 Uiso 1 1 calc R . . C10 C 0.6249(7) 0.3445(6) 0.3468(5) 0.017(2) Uani 1 1 d . . . H10 H 0.5853 0.2941 0.3366 0.021 Uiso 1 1 calc R . . C11 C 0.7681(8) 0.0154(7) 0.3102(5) 0.030(2) Uani 1 1 d . . . H11A H 0.6968 -0.0018 0.3482 0.046 Uiso 1 1 calc R . . H11B H 0.8002 0.0483 0.3506 0.046 Uiso 1 1 calc R . . H11C H 0.8164 -0.0454 0.2804 0.046 Uiso 1 1 calc R . . C12 C 0.6880(7) -0.0095(6) 0.1634(5) 0.020(2) Uani 1 1 d . . . H12A H 0.7375 -0.0710 0.1613 0.030 Uiso 1 1 calc R . . H12B H 0.6826 0.0018 0.1006 0.030 Uiso 1 1 calc R . . H12C H 0.6156 -0.0155 0.2078 0.030 Uiso 1 1 calc R . . C13 C 0.9140(7) 0.5664(7) 0.1354(6) 0.025(2) Uani 1 1 d . . . H13A H 0.9375 0.5859 0.0692 0.030 Uiso 1 1 calc R . . H13B H 0.9238 0.4927 0.1365 0.030 Uiso 1 1 calc R . . C14 C 0.9794(8) 0.6095(8) 0.1884(6) 0.037(3) Uani 1 1 d . . . H14A H 0.9875 0.5659 0.2392 0.045 Uiso 1 1 calc R . . H14B H 1.0528 0.6189 0.1457 0.045 Uiso 1 1 calc R . . C15 C 0.9118(9) 0.7084(8) 0.2281(8) 0.046(3) Uani 1 1 d . . . H15A H 0.9245 0.7296 0.2861 0.055 Uiso 1 1 calc R . . H15B H 0.9289 0.7608 0.1817 0.055 Uiso 1 1 calc R . . C16 C 0.7968(8) 0.6880(7) 0.2488(7) 0.037(3) Uani 1 1 d . . . H16A H 0.7666 0.6682 0.3145 0.044 Uiso 1 1 calc R . . H16B H 0.7502 0.7483 0.2397 0.044 Uiso 1 1 calc R . . C17 C 0.4877(8) 0.7185(7) 0.3392(6) 0.033(2) Uani 1 1 d . . . H17A H 0.5291 0.7041 0.3834 0.039 Uiso 1 1 calc R . . H17B H 0.4196 0.6878 0.3617 0.039 Uiso 1 1 calc R . . C18 C 0.4625(8) 0.8291(6) 0.3312(6) 0.029(2) Uani 1 1 d . . . H18A H 0.5222 0.8643 0.3366 0.034 Uiso 1 1 calc R . . H18B H 0.3934 0.8569 0.3800 0.034 Uiso 1 1 calc R . . C19 C 0.7822(7) 0.1555(6) -0.0285(5) 0.0158(19) Uani 1 1 d . . . C20 C 0.7741(7) 0.2119(6) -0.1051(5) 0.022(2) Uani 1 1 d . . . H20 H 0.7228 0.2707 -0.0946 0.027 Uiso 1 1 calc R . . C21 C 0.8402(7) 0.1823(6) -0.1951(6) 0.023(2) Uani 1 1 d . . . H21 H 0.8326 0.2200 -0.2463 0.028 Uiso 1 1 calc R . . C22 C 0.9168(8) 0.0991(6) -0.2119(6) 0.026(2) Uani 1 1 d . . . H22 H 0.9626 0.0801 -0.2743 0.031 Uiso 1 1 calc R . . C23 C 0.9274(8) 0.0427(6) -0.1378(6) 0.028(2) Uani 1 1 d . . . H23 H 0.9804 -0.0150 -0.1486 0.033 Uiso 1 1 calc R . . C24 C 0.8590(8) 0.0721(6) -0.0475(6) 0.024(2) Uani 1 1 d . . . H24 H 0.8656 0.0330 0.0032 0.029 Uiso 1 1 calc R . . C25 C 0.5615(7) 0.1755(6) 0.1000(5) 0.019(2) Uani 1 1 d . . . C26 C 0.4796(8) 0.1909(7) 0.1876(6) 0.030(2) Uani 1 1 d . . . H26 H 0.4966 0.2150 0.2397 0.036 Uiso 1 1 calc R . . C27 C 0.3756(8) 0.1721(7) 0.2002(7) 0.036(3) Uani 1 1 d . . . H27 H 0.3212 0.1845 0.2603 0.043 Uiso 1 1 calc R . . C28 C 0.3495(8) 0.1356(7) 0.1269(7) 0.033(2) Uani 1 1 d . . . H28 H 0.2777 0.1211 0.1364 0.040 Uiso 1 1 calc R . . C29 C 0.4268(8) 0.1201(7) 0.0403(7) 0.033(2) Uani 1 1 d . . . H29 H 0.4083 0.0963 -0.0111 0.040 Uiso 1 1 calc R . . C30 C 0.5332(9) 0.1391(7) 0.0265(6) 0.031(2) Uani 1 1 d . . . H30 H 0.5868 0.1269 -0.0339 0.037 Uiso 1 1 calc R . . C31 C 0.8712(7) 0.1971(6) 0.3623(5) 0.0187(14) Uani 1 1 d . . . C32 C 0.9708(9) 0.1394(7) 0.3506(6) 0.031(2) Uani 1 1 d . . . H32 H 1.0175 0.1180 0.2891 0.037 Uiso 1 1 calc R . . C33 C 1.0035(9) 0.1122(7) 0.4278(7) 0.039(3) Uani 1 1 d . . . H33 H 1.0727 0.0740 0.4183 0.047 Uiso 1 1 calc R . . C34 C 0.9357(10) 0.1407(7) 0.5177(7) 0.041(3) Uani 1 1 d . . . H34 H 0.9569 0.1202 0.5703 0.049 Uiso 1 1 calc R . . C35 C 0.8375(9) 0.1987(7) 0.5309(6) 0.036(3) Uani 1 1 d . . . H35 H 0.7918 0.2200 0.5928 0.043 Uiso 1 1 calc R . . C36 C 0.8037(8) 0.2268(7) 0.4547(5) 0.026(2) Uani 1 1 d . . . H36 H 0.7349 0.2661 0.4652 0.031 Uiso 1 1 calc R . . C37 C 0.9550(7) 0.2561(6) 0.1770(5) 0.0187(14) Uani 1 1 d U . . C38 C 0.9934(7) 0.2065(6) 0.0903(5) 0.021(2) Uani 1 1 d . . . H38 H 0.9490 0.1639 0.0747 0.025 Uiso 1 1 calc R . . C39 C 1.0949(8) 0.2162(6) 0.0244(6) 0.027(2) Uani 1 1 d . . . H39 H 1.1195 0.1808 -0.0348 0.032 Uiso 1 1 calc R . . C40 C 1.1581(8) 0.2787(7) 0.0476(6) 0.028(2) Uani 1 1 d . . . H40 H 1.2272 0.2868 0.0038 0.033 Uiso 1 1 calc R . . C41 C 1.1216(8) 0.3301(7) 0.1349(6) 0.029(2) Uani 1 1 d . . . H41 H 1.1652 0.3739 0.1502 0.034 Uiso 1 1 calc R . . C42 C 1.0211(7) 0.3169(6) 0.1993(6) 0.021(2) Uani 1 1 d . . . H42 H 0.9974 0.3501 0.2595 0.025 Uiso 1 1 calc R . . C43 C 0.4529(8) 0.8363(7) 0.2326(6) 0.033(2) Uani 1 1 d . . . H43A H 0.3811 0.8212 0.2319 0.039 Uiso 1 1 calc R . . H43B H 0.4651 0.9028 0.2071 0.039 Uiso 1 1 calc R . . C44 C 0.5441(8) 0.7565(6) 0.1802(6) 0.026(2) Uani 1 1 d . . . H44A H 0.5280 0.7279 0.1265 0.031 Uiso 1 1 calc R . . H44B H 0.6136 0.7847 0.1557 0.031 Uiso 1 1 calc R . . C45 C 0.3675(8) 0.5686(7) 0.2158(6) 0.030(2) Uani 1 1 d . . . H45A H 0.4043 0.5578 0.1472 0.037 Uiso 1 1 calc R . . H45B H 0.3619 0.6403 0.2324 0.037 Uiso 1 1 calc R . . C46 C 0.2548(8) 0.5367(8) 0.2438(7) 0.043(3) Uani 1 1 d . . . H46A H 0.2016 0.5820 0.2940 0.051 Uiso 1 1 calc R . . H46B H 0.2285 0.5351 0.1892 0.051 Uiso 1 1 calc R . . C47 C 0.2719(9) 0.4341(8) 0.2786(8) 0.054(3) Uani 1 1 d . . . H47A H 0.2993 0.3832 0.2261 0.065 Uiso 1 1 calc R . . H47B H 0.2038 0.4166 0.3244 0.065 Uiso 1 1 calc R . . C48 C 0.3582(8) 0.4445(8) 0.3256(6) 0.038(3) Uani 1 1 d . . . H48A H 0.3236 0.4746 0.3901 0.045 Uiso 1 1 calc R . . H48B H 0.3995 0.3787 0.3288 0.045 Uiso 1 1 calc R . . C49 C 1.2306(11) 0.1874(9) 0.4704(8) 0.062(4) Uani 1 1 d . . . H49A H 1.1888 0.2114 0.4285 0.074 Uiso 1 1 calc R . . H49B H 1.1803 0.1923 0.5360 0.074 Uiso 1 1 calc R . . C50 C 1.2838(10) 0.0811(8) 0.4428(7) 0.053(3) Uani 1 1 d . . . H50A H 1.2448 0.0343 0.4879 0.063 Uiso 1 1 calc R . . H50B H 1.2850 0.0621 0.3789 0.063 Uiso 1 1 calc R . . C51 C 1.3969(10) 0.0811(9) 0.4455(8) 0.058(3) Uani 1 1 d . . . H51A H 1.4150 0.0275 0.4849 0.070 Uiso 1 1 calc R . . H51B H 1.4509 0.0713 0.3815 0.070 Uiso 1 1 calc R . . C52 C 1.3955(14) 0.1800(11) 0.4869(10) 0.088(5) Uani 1 1 d . . . H52A H 1.3752 0.1780 0.5561 0.106 Uiso 1 1 calc R . . H52B H 1.4682 0.2024 0.4616 0.106 Uiso 1 1 calc R . . C53 C 0.987(2) 0.4165(19) 0.4638(16) 0.029(6) Uiso 0.50 1 d P A -1 H53A H 1.0257 0.3508 0.4347 0.035 Uiso 0.50 1 calc PR A -1 H53B H 0.9088 0.4101 0.4939 0.035 Uiso 0.50 1 calc PR A -1 C54 C 1.034(2) 0.4484(19) 0.5368(17) 0.042(7) Uiso 0.50 1 d P A -1 H54A H 1.1077 0.4124 0.5273 0.050 Uiso 0.50 1 calc PR A -1 H54B H 0.9857 0.4393 0.6015 0.050 Uiso 0.50 1 calc PR A -1 C55 C 1.037(3) 0.559(2) 0.515(2) 0.056(10) Uiso 0.50 1 d P A -1 H55A H 1.1130 0.5717 0.4870 0.067 Uiso 0.50 1 calc PR A -1 H55B H 1.0027 0.6006 0.5742 0.067 Uiso 0.50 1 calc PR A -1 C56 C 0.973(2) 0.5840(19) 0.4466(17) 0.043(7) Uiso 0.50 1 d P A -1 H56A H 0.8937 0.6021 0.4796 0.051 Uiso 0.50 1 calc PR A -1 H56B H 1.0012 0.6377 0.4048 0.051 Uiso 0.50 1 calc PR A -1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.0207(2) 0.0194(2) 0.01654(17) 0.00229(13) -0.00783(14) -0.00431(15) Sr1 0.0157(5) 0.0194(5) 0.0156(4) -0.0009(3) -0.0067(3) -0.0012(4) P1 0.0199(14) 0.0200(13) 0.0128(10) 0.0013(9) -0.0077(9) -0.0028(11) P2 0.0179(14) 0.0216(13) 0.0124(10) 0.0002(9) -0.0064(9) -0.0012(11) O1 0.017(4) 0.026(4) 0.031(3) -0.002(3) -0.013(3) -0.004(3) O2 0.015(4) 0.023(3) 0.035(3) 0.004(3) -0.009(3) 0.003(3) O3 0.013(4) 0.040(4) 0.029(3) 0.006(3) -0.011(3) -0.006(3) O4 0.148(11) 0.036(5) 0.079(6) 0.016(5) -0.048(7) -0.030(6) C1 0.019(5) 0.025(5) 0.017(4) -0.003(4) -0.008(4) 0.007(4) C2 0.045(7) 0.014(5) 0.020(4) 0.003(4) -0.021(4) -0.003(5) C3 0.033(6) 0.015(5) 0.012(4) 0.010(3) -0.004(4) -0.009(4) C4 0.025(6) 0.026(5) 0.016(4) 0.000(4) -0.005(4) 0.001(5) C5 0.019(5) 0.011(4) 0.017(4) -0.004(3) -0.005(4) 0.003(4) C6 0.019(5) 0.016(5) 0.020(4) 0.004(4) -0.013(4) 0.000(4) C7 0.015(5) 0.018(5) 0.007(4) 0.000(3) -0.002(3) -0.001(4) C8 0.025(6) 0.022(5) 0.014(4) -0.004(4) -0.012(4) 0.003(4) C9 0.022(6) 0.040(6) 0.015(4) -0.003(4) -0.006(4) -0.001(5) C10 0.020(5) 0.024(5) 0.007(4) 0.003(3) -0.003(3) -0.002(4) C11 0.042(7) 0.031(6) 0.019(5) 0.020(4) -0.009(4) -0.010(5) C12 0.021(5) 0.013(5) 0.022(4) 0.000(4) -0.004(4) 0.003(4) C13 0.016(6) 0.032(6) 0.027(5) -0.002(4) -0.008(4) -0.002(5) C14 0.022(6) 0.067(8) 0.024(5) 0.002(5) -0.005(4) -0.013(6) C15 0.037(7) 0.036(7) 0.064(7) -0.013(6) -0.017(6) -0.003(6) C16 0.029(7) 0.030(6) 0.047(6) -0.007(5) -0.007(5) -0.002(5) C17 0.037(7) 0.032(6) 0.027(5) -0.004(4) -0.010(5) -0.001(5) C18 0.019(6) 0.025(6) 0.036(5) -0.004(4) -0.007(4) 0.009(4) C19 0.018(5) 0.019(5) 0.010(4) 0.001(3) -0.003(3) -0.004(4) C20 0.023(6) 0.014(5) 0.026(5) -0.004(4) -0.007(4) 0.008(4) C21 0.024(6) 0.023(5) 0.023(5) 0.001(4) -0.009(4) -0.002(4) C22 0.031(6) 0.026(5) 0.019(4) 0.005(4) -0.009(4) 0.003(5) C23 0.036(7) 0.015(5) 0.032(5) 0.001(4) -0.012(5) 0.001(5) C24 0.035(6) 0.015(5) 0.025(5) 0.004(4) -0.013(4) 0.000(5) C25 0.025(6) 0.017(5) 0.019(4) 0.004(4) -0.011(4) -0.003(4) C26 0.031(7) 0.027(6) 0.038(5) -0.002(4) -0.018(5) -0.004(5) C27 0.017(6) 0.046(7) 0.037(6) 0.000(5) 0.002(5) -0.002(5) C28 0.022(6) 0.039(6) 0.050(6) 0.011(5) -0.022(5) -0.016(5) C29 0.031(7) 0.038(6) 0.040(6) -0.004(5) -0.024(5) -0.006(5) C30 0.043(7) 0.035(6) 0.021(5) 0.005(4) -0.016(5) -0.014(5) C31 0.024(4) 0.012(3) 0.024(3) 0.005(2) -0.015(3) 0.002(3) C32 0.044(7) 0.027(6) 0.027(5) 0.005(4) -0.019(5) -0.008(5) C33 0.042(7) 0.034(6) 0.052(7) 0.010(5) -0.032(6) -0.001(5) C34 0.063(9) 0.036(7) 0.032(6) 0.013(5) -0.028(6) -0.005(6) C35 0.061(8) 0.035(6) 0.015(5) 0.004(4) -0.016(5) -0.012(6) C36 0.027(6) 0.033(6) 0.019(4) 0.008(4) -0.006(4) -0.011(5) C37 0.024(4) 0.012(3) 0.024(3) 0.005(2) -0.015(3) 0.002(3) C38 0.023(6) 0.027(5) 0.017(4) 0.007(4) -0.012(4) -0.004(4) C39 0.032(6) 0.018(5) 0.025(5) 0.009(4) 0.000(4) -0.003(5) C40 0.019(6) 0.032(6) 0.024(5) 0.009(4) 0.003(4) -0.003(5) C41 0.030(6) 0.025(5) 0.036(5) 0.009(4) -0.016(5) -0.008(5) C42 0.016(5) 0.023(5) 0.024(4) 0.001(4) -0.008(4) -0.003(4) C43 0.023(6) 0.032(6) 0.044(6) 0.007(5) -0.013(5) 0.000(5) C44 0.025(6) 0.020(5) 0.037(5) 0.007(4) -0.014(4) -0.007(5) C45 0.032(6) 0.039(6) 0.028(5) 0.009(4) -0.021(5) -0.005(5) C46 0.027(7) 0.050(7) 0.059(7) 0.011(6) -0.022(5) -0.012(6) C47 0.038(8) 0.050(8) 0.085(9) 0.019(6) -0.028(7) -0.019(6) C48 0.025(6) 0.056(7) 0.040(6) 0.019(5) -0.014(5) -0.022(6) C49 0.072(10) 0.051(8) 0.065(8) -0.006(6) -0.027(7) -0.002(8) C50 0.071(10) 0.044(7) 0.043(6) 0.013(5) -0.020(6) -0.009(7) C51 0.049(9) 0.067(9) 0.061(8) -0.002(7) -0.028(7) 0.004(7) C52 0.129(15) 0.097(12) 0.084(10) 0.035(9) -0.078(10) -0.066(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 Pt1 C11 2.082(8) . ? Pt1 C12 2.101(8) . ? Pt1 P2 2.296(2) . ? Pt1 P1 2.307(2) . ? Sr1 O2 2.584(6) . ? Sr1 O1 2.624(6) . ? Sr1 O3 2.629(6) . ? Sr1 C10 2.840(8) . ? Sr1 C3 2.842(7) . ? Sr1 C2 2.852(8) . ? Sr1 C9 2.853(8) . ? Sr1 C4 2.856(8) . ? Sr1 C8 2.879(7) . ? Sr1 C6 2.886(8) . ? Sr1 C1 2.902(8) . ? Sr1 C7 2.907(8) . ? P1 C5 1.805(8) . ? P1 C25 1.832(9) . ? P1 C19 1.842(7) . ? P2 C6 1.768(8) . ? P2 C37 1.832(9) . ? P2 C31 1.836(8) . ? O1 C16 1.457(10) . ? O1 C13 1.459(10) . ? O2 C44 1.439(10) . ? O2 C17 1.441(9) . ? O3 C48 1.444(10) . ? O3 C45 1.450(10) . ? O4 C52 1.417(16) . ? O4 C49 1.416(14) . ? O5 C53 1.38(3) . ? O5 C56 1.47(3) . ? C1 C2 1.387(11) . ? C1 C5 1.405(11) . ? C2 C3 1.399(12) . ? C3 C4 1.393(11) . ? C4 C5 1.411(12) . ? C6 C10 1.419(11) . ? C6 C7 1.435(11) . ? C7 C8 1.424(11) . ? C8 C9 1.424(12) . ? C9 C10 1.401(11) . ? C13 C14 1.511(12) . ? C14 C15 1.512(13) . ? C15 C16 1.497(13) . ? C17 C18 1.504(12) . ? C18 C43 1.532(12) . ? C19 C24 1.373(11) . ? C19 C20 1.407(11) . ? C20 C21 1.375(11) . ? C21 C22 1.371(12) . ? C22 C23 1.386(11) . ? C23 C24 1.387(11) . ? C25 C30 1.385(12) . ? C25 C26 1.398(12) . ? C26 C27 1.369(13) . ? C27 C28 1.367(13) . ? C28 C29 1.362(12) . ? C29 C30 1.397(13) . ? C31 C32 1.388(12) . ? C31 C36 1.410(11) . ? C32 C33 1.396(12) . ? C33 C34 1.378(13) . ? C34 C35 1.371(14) . ? C35 C36 1.393(12) . ? C37 C38 1.377(11) . ? C37 C42 1.383(11) . ? C38 C39 1.398(11) . ? C39 C40 1.375(12) . ? C40 C41 1.396(12) . ? C41 C42 1.391(12) . ? C43 C44 1.507(12) . ? C45 C46 1.517(13) . ? C46 C47 1.500(14) . ? C47 C48 1.536(14) . ? C49 C50 1.511(15) . ? C50 C51 1.493(15) . ? C51 C52 1.473(16) . ? C53 C54 1.51(4) . ? C54 C55 1.53(3) . ? C55 C56 1.54(4) . ? 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 C11 Pt1 C12 83.1(3) . . ? C11 Pt1 P2 91.1(3) . . ? C12 Pt1 P2 173.7(2) . . ? C11 Pt1 P1 168.2(3) . . ? C12 Pt1 P1 86.3(2) . . ? P2 Pt1 P1 99.63(8) . . ? O2 Sr1 O1 72.92(18) . . ? O2 Sr1 O3 69.21(19) . . ? O1 Sr1 O3 142.13(19) . . ? O2 Sr1 C10 127.9(2) . . ? O1 Sr1 C10 120.0(2) . . ? O3 Sr1 C10 84.5(2) . . ? O2 Sr1 C3 104.6(2) . . ? O1 Sr1 C3 75.2(2) . . ? O3 Sr1 C3 114.4(2) . . ? C10 Sr1 C3 127.3(2) . . ? O2 Sr1 C2 94.8(2) . . ? O1 Sr1 C2 97.4(2) . . ? O3 Sr1 C2 86.0(2) . . ? C10 Sr1 C2 128.3(2) . . ? C3 Sr1 C2 28.4(3) . . ? O2 Sr1 C9 99.9(2) . . ? O1 Sr1 C9 111.4(2) . . ? O3 Sr1 C9 75.6(2) . . ? C10 Sr1 C9 28.5(2) . . ? C3 Sr1 C9 155.5(2) . . ? C2 Sr1 C9 150.4(3) . . ? O2 Sr1 C4 132.8(2) . . ? O1 Sr1 C4 85.4(2) . . ? O3 Sr1 C4 121.1(2) . . ? C10 Sr1 C4 99.2(2) . . ? C3 Sr1 C4 28.3(2) . . ? C2 Sr1 C4 46.2(3) . . ? C9 Sr1 C4 127.2(2) . . ? O2 Sr1 C8 92.1(2) . . ? O1 Sr1 C8 82.6(2) . . ? O3 Sr1 C8 98.5(2) . . ? C10 Sr1 C8 47.1(2) . . ? C3 Sr1 C8 146.5(3) . . ? C2 Sr1 C8 172.7(3) . . ? C9 Sr1 C8 28.8(2) . . ? C4 Sr1 C8 126.6(2) . . ? O2 Sr1 C6 139.3(2) . . ? O1 Sr1 C6 95.4(2) . . ? O3 Sr1 C6 113.1(2) . . ? C10 Sr1 C6 28.7(2) . . ? C3 Sr1 C6 109.9(2) . . ? C2 Sr1 C6 125.7(2) . . ? C9 Sr1 C6 47.2(2) . . ? C4 Sr1 C6 82.8(2) . . ? C8 Sr1 C6 47.2(2) . . ? O2 Sr1 C1 113.9(2) . . ? O1 Sr1 C1 121.4(2) . . ? O3 Sr1 C1 75.6(2) . . ? C10 Sr1 C1 101.0(2) . . ? C3 Sr1 C1 46.3(3) . . ? C2 Sr1 C1 27.9(2) . . ? C9 Sr1 C1 123.1(2) . . ? C4 Sr1 C1 45.8(3) . . ? C8 Sr1 C1 148.1(2) . . ? C6 Sr1 C1 105.6(2) . . ? O2 Sr1 C7 113.5(2) . . ? O1 Sr1 C7 73.0(2) . . ? O3 Sr1 C7 122.7(2) . . ? C10 Sr1 C7 47.1(2) . . ? C3 Sr1 C7 119.0(2) . . ? C2 Sr1 C7 144.7(2) . . ? C9 Sr1 C7 47.1(2) . . ? C4 Sr1 C7 98.6(2) . . ? C8 Sr1 C7 28.5(2) . . ? C6 Sr1 C7 28.7(2) . . ? C1 Sr1 C7 132.6(2) . . ? C5 P1 C25 101.3(4) . . ? C5 P1 C19 99.1(4) . . ? C25 P1 C19 103.3(4) . . ? C5 P1 Pt1 127.7(3) . . ? C25 P1 Pt1 108.5(3) . . ? C19 P1 Pt1 114.0(3) . . ? C6 P2 C37 110.3(4) . . ? C6 P2 C31 99.8(4) . . ? C37 P2 C31 99.6(4) . . ? C6 P2 Pt1 116.2(3) . . ? C37 P2 Pt1 113.0(3) . . ? C31 P2 Pt1 115.9(3) . . ? C16 O1 C13 108.9(7) . . ? C16 O1 Sr1 121.9(5) . . ? C13 O1 Sr1 121.7(5) . . ? C44 O2 C17 108.8(6) . . ? C44 O2 Sr1 130.1(5) . . ? C17 O2 Sr1 120.6(5) . . ? C48 O3 C45 108.1(7) . . ? C48 O3 Sr1 128.9(6) . . ? C45 O3 Sr1 121.1(5) . . ? C52 O4 C49 104.5(9) . . ? C53 O5 C56 105.6(17) . . ? C2 C1 C5 109.4(8) . . ? C2 C1 Sr1 74.1(5) . . ? C5 C1 Sr1 76.8(5) . . ? C1 C2 C3 108.4(8) . . ? C1 C2 Sr1 78.1(5) . . ? C3 C2 Sr1 75.4(5) . . ? C4 C3 C2 106.8(8) . . ? C4 C3 Sr1 76.4(4) . . ? C2 C3 Sr1 76.2(4) . . ? C3 C4 C5 110.0(8) . . ? C3 C4 Sr1 75.3(4) . . ? C5 C4 Sr1 78.4(4) . . ? C1 C5 C4 105.4(7) . . ? C1 C5 P1 127.9(7) . . ? C4 C5 P1 124.1(7) . . ? C1 C5 Sr1 75.3(4) . . ? C4 C5 Sr1 73.3(4) . . ? P1 C5 Sr1 130.5(4) . . ? C10 C6 C7 107.1(7) . . ? C10 C6 P2 120.4(6) . . ? C7 C6 P2 129.5(7) . . ? C10 C6 Sr1 73.9(5) . . ? C7 C6 Sr1 76.5(5) . . ? P2 C6 Sr1 130.6(4) . . ? C8 C7 C6 107.8(8) . . ? C8 C7 Sr1 74.7(5) . . ? C6 C7 Sr1 74.8(5) . . ? C7 C8 C9 107.8(7) . . ? C7 C8 Sr1 76.8(4) . . ? C9 C8 Sr1 74.6(4) . . ? C10 C9 C8 108.1(8) . . ? C10 C9 Sr1 75.2(4) . . ? C8 C9 Sr1 76.6(5) . . ? C9 C10 C6 109.2(8) . . ? C9 C10 Sr1 76.3(5) . . ? C6 C10 Sr1 77.5(4) . . ? O1 C13 C14 105.9(7) . . ? C15 C14 C13 103.2(8) . . ? C16 C15 C14 103.7(8) . . ? O1 C16 C15 106.6(7) . . ? O2 C17 C18 105.3(7) . . ? C17 C18 C43 102.5(7) . . ? C24 C19 C20 117.4(7) . . ? C24 C19 P1 122.2(6) . . ? C20 C19 P1 120.3(6) . . ? C21 C20 C19 120.3(8) . . ? C22 C21 C20 121.0(8) . . ? C21 C22 C23 120.0(8) . . ? C22 C23 C24 118.6(8) . . ? C19 C24 C23 122.7(8) . . ? C30 C25 C26 117.0(9) . . ? C30 C25 P1 125.2(7) . . ? C26 C25 P1 117.7(6) . . ? C27 C26 C25 121.6(9) . . ? C28 C27 C26 120.4(9) . . ? C29 C28 C27 119.9(9) . . ? C28 C29 C30 120.2(9) . . ? C25 C30 C29 120.9(9) . . ? C32 C31 C36 117.8(8) . . ? C32 C31 P2 121.6(6) . . ? C36 C31 P2 120.6(7) . . ? C31 C32 C33 121.1(9) . . ? C34 C33 C32 120.2(10) . . ? C35 C34 C33 119.6(9) . . ? C34 C35 C36 120.9(9) . . ? C35 C36 C31 120.3(9) . . ? C38 C37 C42 118.0(8) . . ? C38 C37 P2 119.2(7) . . ? C42 C37 P2 122.6(6) . . ? C37 C38 C39 122.8(9) . . ? C40 C39 C38 118.1(8) . . ? C39 C40 C41 120.6(8) . . ? C42 C41 C40 119.5(9) . . ? C37 C42 C41 121.0(8) . . ? C44 C43 C18 100.1(7) . . ? O2 C44 C43 107.2(7) . . ? O3 C45 C46 107.5(7) . . ? C47 C46 C45 103.3(9) . . ? C46 C47 C48 101.8(9) . . ? O3 C48 C47 104.8(8) . . ? O4 C49 C50 106.2(10) . . ? C51 C50 C49 104.0(10) . . ? C52 C51 C50 104.7(11) . . ? O4 C52 C51 105.5(10) . . ? O5 C53 C54 109.5(19) . . ? C53 C54 C55 100(2) . . ? C54 C55 C56 108(3) . . ? O5 C56 C55 98.1(19) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 2.527 _refine_diff_density_min -1.661 _refine_diff_density_rms 0.238 data_6b.CIF _database_code_depnum_ccdc_archive 'CCDC 825581' #TrackingRef '- 6b.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 6b _chemical_melting_point ? _chemical_formula_moiety 'C38 H38 Ca O2 P2' _chemical_formula_sum 'C38 H38 Ca O2 P2' _chemical_formula_weight 628.70 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' Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y, z-1/2' _cell_length_a 8.4669(2) _cell_length_b 14.9498(4) _cell_length_c 26.8694(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3401.09(17) _cell_formula_units_Z 4 _cell_measurement_temperature 123 _cell_measurement_reflns_used 29274 _cell_measurement_theta_min 2.72 _cell_measurement_theta_max 27.50 _exptl_crystal_description Prism _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.228 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1328 _exptl_absorpt_coefficient_mu 0.310 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9406 _exptl_absorpt_correction_T_max 0.9847 _exptl_absorpt_process_details ? _exptl_special_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET) (compiled Aug 2 2010,13:00:58) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 123 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Ruby, Gemini ultra' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29274 _diffrn_reflns_av_R_equivalents 0.0487 _diffrn_reflns_av_sigmaI/netI 0.0335 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 2.72 _diffrn_reflns_theta_max 27.50 _reflns_number_total 3905 _reflns_number_gt 2958 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlisPro, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlisPro, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlisPro, Oxford Diffraction Ltd' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999' _computing_publication_material 'CIFTAB (Sheldrick, 1997' _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^)+(0.0404P)^2^+1.5517P] 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 ? _refine_ls_extinction_coef none _refine_ls_number_reflns 3905 _refine_ls_number_parameters 196 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0629 _refine_ls_R_factor_gt 0.0408 _refine_ls_wR_factor_ref 0.0961 _refine_ls_wR_factor_gt 0.0871 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.020 _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 Ca1 Ca 0.5000 0.19661(3) 0.7500 0.01929(12) Uani 1 2 d S . . P1 P 0.50978(5) 0.38266(3) 0.852312(17) 0.02422(12) Uani 1 1 d . . . O1 O 0.39923(15) 0.06641(8) 0.71089(5) 0.0296(3) Uani 1 1 d . . . C1 C 0.30767(19) 0.32848(12) 0.77528(7) 0.0266(4) Uani 1 1 d . . . H1 H 0.3230 0.3825 0.7573 0.032 Uiso 1 1 calc R . . C2 C 0.2056(2) 0.25885(13) 0.76181(7) 0.0305(4) Uani 1 1 d . . . H2 H 0.1404 0.2572 0.7330 0.037 Uiso 1 1 calc R . . C3 C 0.2166(2) 0.19157(13) 0.79838(7) 0.0293(4) Uani 1 1 d . . . H3 H 0.1600 0.1367 0.7985 0.035 Uiso 1 1 calc R . . C4 C 0.3251(2) 0.21963(12) 0.83440(7) 0.0250(4) Uani 1 1 d . . . H4 H 0.3544 0.1872 0.8634 0.030 Uiso 1 1 calc R . . C5 C 0.38398(19) 0.30494(11) 0.82018(6) 0.0233(4) Uani 1 1 d . . . C17 C 0.4847(2) -0.01329(11) 0.72262(7) 0.0319(4) Uani 1 1 d . . . H17A H 0.5858 -0.0147 0.7041 0.038 Uiso 1 1 calc R . . H17B H 0.4222 -0.0666 0.7132 0.038 Uiso 1 1 calc R . . C18 C 0.3412(3) 0.06744(14) 0.66077(8) 0.0429(5) Uani 1 1 d . . . H18A H 0.4303 0.0643 0.6376 0.064 Uiso 1 1 calc R . . H18B H 0.2821 0.1228 0.6550 0.064 Uiso 1 1 calc R . . H18C H 0.2716 0.0159 0.6555 0.064 Uiso 1 1 calc R . . C19 C 0.6223(2) 0.31002(11) 0.89471(7) 0.0252(4) Uani 1 1 d . . . C20 C 0.5562(2) 0.26797(12) 0.93585(7) 0.0300(4) Uani 1 1 d . . . H20 H 0.4479 0.2775 0.9435 0.036 Uiso 1 1 calc R . . C21 C 0.6461(3) 0.21227(13) 0.96589(7) 0.0384(5) Uani 1 1 d . . . H21 H 0.5996 0.1844 0.9941 0.046 Uiso 1 1 calc R . . C22 C 0.8032(3) 0.19738(14) 0.95485(8) 0.0409(5) Uani 1 1 d . . . H22 H 0.8643 0.1587 0.9752 0.049 Uiso 1 1 calc R . . C23 C 0.8715(2) 0.23837(14) 0.91442(8) 0.0410(5) Uani 1 1 d . . . H23 H 0.9795 0.2279 0.9068 0.049 Uiso 1 1 calc R . . C24 C 0.7820(2) 0.29519(13) 0.88467(8) 0.0325(4) Uani 1 1 d . . . H24 H 0.8302 0.3243 0.8572 0.039 Uiso 1 1 calc R . . C25 C 0.3727(2) 0.43568(12) 0.89644(7) 0.0279(4) Uani 1 1 d . . . C26 C 0.4291(3) 0.50318(15) 0.92681(9) 0.0532(7) Uani 1 1 d . . . H26 H 0.5379 0.5186 0.9256 0.064 Uiso 1 1 calc R . . C27 C 0.3294(3) 0.54864(16) 0.95895(10) 0.0619(8) Uani 1 1 d . . . H27 H 0.3705 0.5940 0.9801 0.074 Uiso 1 1 calc R . . C28 C 0.1717(3) 0.52825(14) 0.96031(8) 0.0458(6) Uani 1 1 d . . . H28 H 0.1030 0.5602 0.9819 0.055 Uiso 1 1 calc R . . C29 C 0.1135(2) 0.46159(15) 0.93050(7) 0.0391(5) Uani 1 1 d . . . H29 H 0.0044 0.4469 0.9317 0.047 Uiso 1 1 calc R . . C30 C 0.2130(2) 0.41544(13) 0.89853(7) 0.0325(4) Uani 1 1 d . . . H30 H 0.1714 0.3695 0.8779 0.039 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ca1 0.0181(2) 0.0191(2) 0.0207(3) 0.000 0.00032(18) 0.000 P1 0.0269(2) 0.0224(2) 0.0234(2) -0.00242(17) 0.00481(18) -0.0016(2) O1 0.0336(7) 0.0231(6) 0.0320(7) -0.0032(5) -0.0061(5) -0.0002(6) C1 0.0213(8) 0.0310(9) 0.0274(10) 0.0014(8) 0.0050(7) 0.0088(7) C2 0.0179(8) 0.0453(11) 0.0284(11) -0.0016(8) -0.0004(7) 0.0053(8) C3 0.0203(8) 0.0374(10) 0.0302(10) -0.0036(8) 0.0056(7) -0.0056(8) C4 0.0263(8) 0.0275(9) 0.0210(9) 0.0007(7) 0.0040(7) -0.0010(7) C5 0.0220(8) 0.0256(8) 0.0223(9) -0.0019(7) 0.0031(7) 0.0030(7) C17 0.0411(11) 0.0209(8) 0.0338(11) -0.0021(7) 0.0037(9) -0.0001(8) C18 0.0551(13) 0.0347(11) 0.0389(13) -0.0036(9) -0.0181(10) -0.0120(10) C19 0.0269(9) 0.0246(9) 0.0242(10) -0.0067(7) -0.0018(7) -0.0025(7) C20 0.0333(9) 0.0329(10) 0.0238(10) -0.0046(8) -0.0009(7) -0.0005(8) C21 0.0516(13) 0.0389(11) 0.0248(11) -0.0031(9) -0.0062(9) -0.0021(10) C22 0.0475(12) 0.0380(11) 0.0373(12) -0.0098(9) -0.0205(10) 0.0073(10) C23 0.0286(10) 0.0450(12) 0.0494(14) -0.0106(10) -0.0096(9) 0.0025(9) C24 0.0275(9) 0.0346(10) 0.0353(11) -0.0062(8) 0.0001(8) -0.0042(8) C25 0.0340(9) 0.0234(9) 0.0263(10) 0.0002(7) 0.0060(8) 0.0026(8) C26 0.0483(13) 0.0446(13) 0.0666(17) -0.0284(12) 0.0260(12) -0.0147(11) C27 0.0707(17) 0.0448(13) 0.0704(19) -0.0338(13) 0.0304(14) -0.0155(12) C28 0.0567(14) 0.0366(11) 0.0441(14) -0.0010(10) 0.0241(11) 0.0118(11) C29 0.0359(11) 0.0506(12) 0.0308(12) 0.0032(9) 0.0077(9) 0.0117(10) C30 0.0322(10) 0.0401(11) 0.0253(10) -0.0003(8) 0.0014(8) 0.0049(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ca1 O1 2.3709(12) . ? Ca1 O1 2.3709(12) 4_656 ? Ca1 C1 2.6456(17) . ? Ca1 C1 2.6456(17) 4_656 ? Ca1 C5 2.6727(17) . ? Ca1 C5 2.6727(17) 4_656 ? Ca1 C2 2.6792(17) 4_656 ? Ca1 C2 2.6792(17) . ? Ca1 C4 2.7302(17) . ? Ca1 C4 2.7302(17) 4_656 ? Ca1 C3 2.7304(17) 4_656 ? Ca1 C3 2.7304(17) . ? P1 C5 1.7972(18) . ? P1 C25 1.8387(18) . ? P1 C19 1.8397(18) . ? O1 C17 1.429(2) . ? O1 C18 1.434(2) . ? C1 C2 1.400(3) . ? C1 C5 1.413(2) . ? C2 C3 1.409(3) . ? C3 C4 1.399(2) . ? C4 C5 1.422(2) . ? C17 C17 1.494(4) 4_656 ? C19 C20 1.390(3) . ? C19 C24 1.397(2) . ? C20 C21 1.387(3) . ? C21 C22 1.381(3) . ? C22 C23 1.375(3) . ? C23 C24 1.391(3) . ? C25 C26 1.383(3) . ? C25 C30 1.387(3) . ? C26 C27 1.385(3) . ? C27 C28 1.370(3) . ? C28 C29 1.370(3) . ? C29 C30 1.387(3) . ? 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 Ca1 O1 69.63(6) . 4_656 ? O1 Ca1 C1 120.27(5) . . ? O1 Ca1 C1 136.01(5) 4_656 . ? O1 Ca1 C1 136.01(5) . 4_656 ? O1 Ca1 C1 120.27(5) 4_656 4_656 ? C1 Ca1 C1 83.66(8) . 4_656 ? O1 Ca1 C5 132.68(5) . . ? O1 Ca1 C5 108.48(5) 4_656 . ? C1 Ca1 C5 30.81(5) . . ? C1 Ca1 C5 87.47(6) 4_656 . ? O1 Ca1 C5 108.48(5) . 4_656 ? O1 Ca1 C5 132.68(5) 4_656 4_656 ? C1 Ca1 C5 87.47(6) . 4_656 ? C1 Ca1 C5 30.81(5) 4_656 4_656 ? C5 Ca1 C5 105.41(7) . 4_656 ? O1 Ca1 C2 124.57(5) . 4_656 ? O1 Ca1 C2 90.16(5) 4_656 4_656 ? C1 Ca1 C2 110.14(6) . 4_656 ? C1 Ca1 C2 30.49(6) 4_656 4_656 ? C5 Ca1 C2 102.42(6) . 4_656 ? C5 Ca1 C2 50.51(5) 4_656 4_656 ? O1 Ca1 C2 90.16(5) . . ? O1 Ca1 C2 124.57(5) 4_656 . ? C1 Ca1 C2 30.49(6) . . ? C1 Ca1 C2 110.14(6) 4_656 . ? C5 Ca1 C2 50.51(5) . . ? C5 Ca1 C2 102.42(6) 4_656 . ? C2 Ca1 C2 139.36(9) 4_656 . ? O1 Ca1 C4 106.05(5) . . ? O1 Ca1 C4 86.01(5) 4_656 . ? C1 Ca1 C4 50.13(5) . . ? C1 Ca1 C4 116.95(6) 4_656 . ? C5 Ca1 C4 30.49(5) . . ? C5 Ca1 C4 135.16(5) 4_656 . ? C2 Ca1 C4 124.00(5) 4_656 . ? C2 Ca1 C4 49.71(5) . . ? O1 Ca1 C4 86.01(5) . 4_656 ? O1 Ca1 C4 106.05(5) 4_656 4_656 ? C1 Ca1 C4 116.95(6) . 4_656 ? C1 Ca1 C4 50.13(5) 4_656 4_656 ? C5 Ca1 C4 135.16(5) . 4_656 ? C5 Ca1 C4 30.49(5) 4_656 4_656 ? C2 Ca1 C4 49.71(5) 4_656 4_656 ? C2 Ca1 C4 124.00(5) . 4_656 ? C4 Ca1 C4 165.52(8) . 4_656 ? O1 Ca1 C3 94.74(5) . 4_656 ? O1 Ca1 C3 82.65(5) 4_656 4_656 ? C1 Ca1 C3 133.14(6) . 4_656 ? C1 Ca1 C3 50.01(6) 4_656 4_656 ? C5 Ca1 C3 132.51(6) . 4_656 ? C5 Ca1 C3 50.04(5) 4_656 4_656 ? C2 Ca1 C3 30.18(6) 4_656 4_656 ? C2 Ca1 C3 152.08(6) . 4_656 ? C4 Ca1 C3 151.12(5) . 4_656 ? C4 Ca1 C3 29.69(5) 4_656 4_656 ? O1 Ca1 C3 82.65(5) . . ? O1 Ca1 C3 94.74(5) 4_656 . ? C1 Ca1 C3 50.01(6) . . ? C1 Ca1 C3 133.14(6) 4_656 . ? C5 Ca1 C3 50.04(5) . . ? C5 Ca1 C3 132.51(6) 4_656 . ? C2 Ca1 C3 152.08(6) 4_656 . ? C2 Ca1 C3 30.18(6) . . ? C4 Ca1 C3 29.69(5) . . ? C4 Ca1 C3 151.12(5) 4_656 . ? C3 Ca1 C3 176.84(8) 4_656 . ? C5 P1 C25 102.38(8) . . ? C5 P1 C19 102.87(8) . . ? C25 P1 C19 100.49(8) . . ? C17 O1 C18 112.93(14) . . ? C17 O1 Ca1 113.86(10) . . ? C18 O1 Ca1 122.06(11) . . ? C2 C1 C5 108.52(16) . . ? C2 C1 Ca1 76.08(10) . . ? C5 C1 Ca1 75.65(10) . . ? C1 C2 C3 108.05(16) . . ? C1 C2 Ca1 73.43(10) . . ? C3 C2 Ca1 76.92(10) . . ? C4 C3 C2 108.15(16) . . ? C4 C3 Ca1 75.15(10) . . ? C2 C3 Ca1 72.90(10) . . ? C3 C4 C5 108.26(16) . . ? C3 C4 Ca1 75.16(10) . . ? C5 C4 Ca1 72.52(9) . . ? C1 C5 C4 107.01(16) . . ? C1 C5 P1 121.34(13) . . ? C4 C5 P1 131.20(14) . . ? C1 C5 Ca1 73.54(10) . . ? C4 C5 Ca1 76.99(10) . . ? P1 C5 Ca1 120.85(8) . . ? O1 C17 C17 107.76(13) . 4_656 ? C20 C19 C24 118.16(17) . . ? C20 C19 P1 123.44(14) . . ? C24 C19 P1 118.39(14) . . ? C21 C20 C19 120.89(18) . . ? C22 C21 C20 120.0(2) . . ? C23 C22 C21 120.20(19) . . ? C22 C23 C24 119.83(19) . . ? C23 C24 C19 120.88(19) . . ? C26 C25 C30 118.16(18) . . ? C26 C25 P1 118.52(15) . . ? C30 C25 P1 123.19(14) . . ? C25 C26 C27 121.0(2) . . ? C28 C27 C26 120.1(2) . . ? C27 C28 C29 119.8(2) . . ? C28 C29 C30 120.4(2) . . ? C25 C30 C29 120.58(19) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.301 _refine_diff_density_min -0.229 _refine_diff_density_rms 0.049 # Attachment '- 9b.CIF' data_9b.CIF _database_code_depnum_ccdc_archive 'CCDC 825582' #TrackingRef '- 9b.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common DP368 _chemical_melting_point ? _chemical_formula_moiety 'C50 H62 Ca O3.50 P2 Pt' _chemical_formula_sum 'C50 H62 Ca O3.50 P2 Pt' _chemical_formula_weight 1016.11 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' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.7626(4) _cell_length_b 14.1010(3) _cell_length_c 14.9014(4) _cell_angle_alpha 112.945(2) _cell_angle_beta 100.743(2) _cell_angle_gamma 106.299(2) _cell_volume 2233.61(10) _cell_formula_units_Z 2 _cell_measurement_temperature 123 _cell_measurement_reflns_used 33633 _cell_measurement_theta_min 1.91 _cell_measurement_theta_max 27.50 _exptl_crystal_description Prism _exptl_crystal_colour Colourless _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 1.511 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1036 _exptl_absorpt_coefficient_mu 3.370 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.82063 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details ? _exptl_special_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET) (compiled Aug 2 2010,13:00:58) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 123 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Ruby, Gemini ultra' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33633 _diffrn_reflns_av_R_equivalents 0.0391 _diffrn_reflns_av_sigmaI/netI 0.0386 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 27.50 _reflns_number_total 10261 _reflns_number_gt 9328 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlisPro, Oxford Diffraction Ltd.,' _computing_cell_refinement 'CrysAlisPro, Oxford Diffraction Ltd.,' _computing_data_reduction 'CrysAlisPro, Oxford Diffraction Ltd.,' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _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^)+(0.0324P)^2^+0.9037P] 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 ? _refine_ls_extinction_coef none _refine_ls_number_reflns 10261 _refine_ls_number_parameters 564 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0333 _refine_ls_R_factor_gt 0.0276 _refine_ls_wR_factor_ref 0.0678 _refine_ls_wR_factor_gt 0.0647 _refine_ls_goodness_of_fit_ref 1.111 _refine_ls_restrained_S_all 1.111 _refine_ls_shift/su_max 0.025 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.720331(9) 0.824378(8) 0.727878(8) 0.01713(4) Uani 1 1 d . . . Ca1 Ca 1.11594(5) 0.81350(5) 0.76495(4) 0.01837(12) Uani 1 1 d . C . P1 P 0.83548(6) 0.86535(6) 0.63614(6) 0.01667(14) Uani 1 1 d . . . P2 P 0.78939(6) 0.70639(6) 0.76611(6) 0.01691(14) Uani 1 1 d . C . O1 O 1.30117(19) 0.95907(18) 0.84484(18) 0.0303(5) Uani 1 1 d . . . O2 O 1.19019(19) 0.66873(17) 0.72834(17) 0.0251(5) Uani 1 1 d . . . O3 O 1.8487(4) 1.4469(4) 0.9186(4) 0.0948(13) Uani 1 1 d . . . O51 O 0.5356(11) 1.0880(10) 0.6128(10) 0.052(3) Uiso 0.25 1 d PD A -1 O61 O 0.525(4) 0.978(3) 0.455(4) 0.37(4) Uiso 0.25 1 d PD B -2 C1 C 1.0713(3) 0.9081(3) 0.6395(2) 0.0221(6) Uani 1 1 d . . . H1 H 1.0975 0.9873 0.6704 0.027 Uiso 1 1 calc R C . C2 C 1.1352(3) 0.8449(3) 0.5999(2) 0.0264(7) Uani 1 1 d . C . H2 H 1.2121 0.8739 0.6002 0.032 Uiso 1 1 calc R . . C3 C 1.0653(3) 0.7317(3) 0.5601(2) 0.0251(6) Uani 1 1 d . . . H3 H 1.0863 0.6705 0.5277 0.030 Uiso 1 1 calc R C . C4 C 0.9588(3) 0.7239(2) 0.5763(2) 0.0212(6) Uani 1 1 d . C . H4 H 0.8958 0.6568 0.5576 0.025 Uiso 1 1 calc R . . C5 C 0.9619(2) 0.8342(2) 0.6256(2) 0.0185(6) Uani 1 1 d . C . C6 C 0.9418(2) 0.7635(2) 0.8352(2) 0.0184(6) Uani 1 1 d . . . C7 C 1.0148(3) 0.7146(3) 0.8671(2) 0.0233(6) Uani 1 1 d . C . H7 H 0.9968 0.6366 0.8409 0.028 Uiso 1 1 calc R . . C8 C 1.1171(3) 0.7999(3) 0.9433(2) 0.0267(7) Uani 1 1 d . . . H8 H 1.1810 0.7901 0.9771 0.032 Uiso 1 1 calc R C . C9 C 1.1096(3) 0.9029(3) 0.9615(2) 0.0257(7) Uani 1 1 d . C . H9 H 1.1673 0.9747 1.0100 0.031 Uiso 1 1 calc R . . C10 C 1.0021(3) 0.8811(2) 0.8956(2) 0.0212(6) Uani 1 1 d . C . H10 H 0.9744 0.9359 0.8919 0.025 Uiso 1 1 calc R . . C11 C 0.6044(3) 0.8102(3) 0.8081(3) 0.0301(7) Uani 1 1 d . . . H11A H 0.5976 0.8821 0.8424 0.045 Uiso 1 1 calc R . . H11B H 0.6327 0.7888 0.8601 0.045 Uiso 1 1 calc R . . H11C H 0.5283 0.7529 0.7596 0.045 Uiso 1 1 calc R . . C12 C 0.6455(3) 0.9302(3) 0.7006(3) 0.0254(7) Uani 1 1 d . . . H12A H 0.5609 0.8933 0.6771 0.038 Uiso 1 1 calc R . . H12B H 0.6690 0.9462 0.6474 0.038 Uiso 1 1 calc R . . H12C H 0.6718 1.0003 0.7647 0.038 Uiso 1 1 calc R . . C13 C 1.3220(13) 1.0781(9) 0.8688(14) 0.098(6) Uani 0.589(16) 1 d P C 2 H13C H 1.2964 1.0828 0.8043 0.117 Uiso 0.589(16) 1 calc PR C 2 H13D H 1.2787 1.1073 0.9141 0.117 Uiso 0.589(16) 1 calc PR C 2 C13A C 1.3155(13) 1.0703(14) 0.8972(13) 0.0343(8) Uani 0.411(16) 1 d P C 1 H13A H 1.2900 1.0821 0.9581 0.041 Uiso 0.411(16) 1 calc PR C 1 H13B H 1.2663 1.0876 0.8512 0.041 Uiso 0.411(16) 1 calc PR C 1 C14 C 1.4389(13) 1.1383(10) 0.9180(14) 0.086(5) Uani 0.589(16) 1 d P C 2 H14C H 1.4620 1.1547 0.9913 0.103 Uiso 0.589(16) 1 calc PR C 2 H14D H 1.4641 1.2093 0.9141 0.103 Uiso 0.589(16) 1 calc PR C 2 C14A C 1.4443(17) 1.1508(17) 0.9334(17) 0.0407(9) Uani 0.411(16) 1 d P C 1 H14A H 1.4570 1.1862 0.8885 0.049 Uiso 0.411(16) 1 calc PR C 1 H14B H 1.4708 1.2095 1.0061 0.049 Uiso 0.411(16) 1 calc PR C 1 C15 C 1.4837(15) 1.0633(11) 0.8596(18) 0.140(10) Uani 0.589(16) 1 d P C 2 H15C H 1.5587 1.0740 0.9038 0.168 Uiso 0.589(16) 1 calc PR C 2 H15D H 1.4964 1.0772 0.8015 0.168 Uiso 0.589(16) 1 calc PR C 2 C15A C 1.5011(10) 1.0704(13) 0.9215(13) 0.050(4) Uani 0.411(16) 1 d P C 1 H15A H 1.5650 1.0974 0.9859 0.060 Uiso 0.411(16) 1 calc PR C 1 H15B H 1.5328 1.0596 0.8641 0.060 Uiso 0.411(16) 1 calc PR C 1 C16 C 1.4008(7) 0.9512(6) 0.8206(8) 0.041(2) Uani 0.589(16) 1 d P C 2 H16A H 1.3813 0.9090 0.7448 0.049 Uiso 0.589(16) 1 calc PR C 2 H16B H 1.4332 0.9117 0.8531 0.049 Uiso 0.589(16) 1 calc PR C 2 C16A C 1.4070(11) 0.9627(12) 0.898(3) 0.114(12) Uani 0.411(16) 1 d P C 1 H16C H 1.4225 0.8978 0.8550 0.137 Uiso 0.411(16) 1 calc PR C 1 H16D H 1.4040 0.9603 0.9632 0.137 Uiso 0.411(16) 1 calc PR C 1 C17 C 1.2850(3) 0.6649(3) 0.7966(3) 0.0343(8) Uani 1 1 d . C . H17A H 1.2855 0.6986 0.8688 0.041 Uiso 1 1 calc R . . H17B H 1.3603 0.7064 0.7943 0.041 Uiso 1 1 calc R . . C18 C 1.2638(4) 0.5417(3) 0.7571(3) 0.0407(9) Uani 1 1 d . . . H18A H 1.3059 0.5184 0.7084 0.049 Uiso 1 1 calc R C . H18B H 1.2879 0.5256 0.8149 0.049 Uiso 1 1 calc R . . C19 C 1.1337(4) 0.4838(3) 0.7026(3) 0.0398(9) Uani 1 1 d . C . H19A H 1.1113 0.4055 0.6499 0.048 Uiso 1 1 calc R . . H19B H 1.0918 0.4846 0.7523 0.048 Uiso 1 1 calc R . . C20 C 1.1114(3) 0.5553(3) 0.6534(3) 0.0323(8) Uani 1 1 d . C . H20A H 1.1276 0.5328 0.5874 0.039 Uiso 1 1 calc R . . H20B H 1.0300 0.5484 0.6398 0.039 Uiso 1 1 calc R . . C21 C 0.7539(3) 0.8067(2) 0.4987(2) 0.0209(6) Uani 1 1 d . . . C22 C 0.6331(3) 0.7562(3) 0.4624(3) 0.0280(7) Uani 1 1 d . . . H22 H 0.5928 0.7498 0.5087 0.034 Uiso 1 1 calc R . . C23 C 0.5716(3) 0.7154(3) 0.3591(3) 0.0401(9) Uani 1 1 d . . . H23 H 0.4895 0.6801 0.3349 0.048 Uiso 1 1 calc R . . C24 C 0.6288(4) 0.7258(3) 0.2912(3) 0.0423(10) Uani 1 1 d . . . H24 H 0.5860 0.7011 0.2213 0.051 Uiso 1 1 calc R . . C25 C 0.7483(4) 0.7721(3) 0.3252(3) 0.0370(9) Uani 1 1 d . . . H25 H 0.7879 0.7772 0.2782 0.044 Uiso 1 1 calc R . . C26 C 0.8108(3) 0.8111(3) 0.4279(2) 0.0278(7) Uani 1 1 d . . . H26 H 0.8930 0.8412 0.4504 0.033 Uiso 1 1 calc R . . C27 C 0.8925(2) 1.0179(2) 0.6824(2) 0.0180(6) Uani 1 1 d . . . C28 C 0.9237(3) 1.0867(2) 0.7875(2) 0.0232(6) Uani 1 1 d . . . H28 H 0.9169 1.0545 0.8326 0.028 Uiso 1 1 calc R . . C29 C 0.9648(3) 1.2025(3) 0.8279(2) 0.0272(7) Uani 1 1 d . . . H29 H 0.9868 1.2488 0.9002 0.033 Uiso 1 1 calc R . . C30 C 0.9738(3) 1.2502(3) 0.7628(3) 0.0268(7) Uani 1 1 d . . . H30 H 1.0018 1.3292 0.7902 0.032 Uiso 1 1 calc R . . C31 C 0.9417(3) 1.1823(3) 0.6577(2) 0.0273(7) Uani 1 1 d . . . H31 H 0.9466 1.2148 0.6127 0.033 Uiso 1 1 calc R . . C32 C 0.9024(3) 1.0675(3) 0.6176(2) 0.0248(6) Uani 1 1 d . . . H32 H 0.8819 1.0217 0.5454 0.030 Uiso 1 1 calc R . . C33 C 0.7470(3) 0.5695(2) 0.6542(2) 0.0205(6) Uani 1 1 d . . . C34 C 0.7829(3) 0.4864(3) 0.6595(3) 0.0273(7) Uani 1 1 d . C . H34 H 0.8351 0.5013 0.7224 0.033 Uiso 1 1 calc R . . C35 C 0.7432(3) 0.3824(3) 0.5738(3) 0.0333(8) Uani 1 1 d . . . H35 H 0.7689 0.3268 0.5782 0.040 Uiso 1 1 calc R C . C36 C 0.6661(3) 0.3591(3) 0.4819(3) 0.0341(8) Uani 1 1 d . C . H36 H 0.6392 0.2876 0.4233 0.041 Uiso 1 1 calc R . . C37 C 0.6286(3) 0.4391(3) 0.4753(3) 0.0345(8) Uani 1 1 d . . . H37 H 0.5750 0.4228 0.4125 0.041 Uiso 1 1 calc R C . C38 C 0.6693(3) 0.5445(3) 0.5612(2) 0.0269(7) Uani 1 1 d . C . H38 H 0.6436 0.5998 0.5561 0.032 Uiso 1 1 calc R . . C39 C 0.7285(3) 0.6614(2) 0.8523(2) 0.0207(6) Uani 1 1 d . . . C40 C 0.7888(3) 0.7143(3) 0.9567(2) 0.0268(7) Uani 1 1 d . C . H40 H 0.8645 0.7705 0.9831 0.032 Uiso 1 1 calc R . . C41 C 0.7405(3) 0.6869(3) 1.0245(3) 0.0344(8) Uani 1 1 d . . . H41 H 0.7839 0.7227 1.0961 0.041 Uiso 1 1 calc R C . C42 C 0.6287(3) 0.6070(3) 0.9864(3) 0.0355(8) Uani 1 1 d . C . H42 H 0.5947 0.5883 1.0319 0.043 Uiso 1 1 calc R . . C43 C 0.5674(3) 0.5550(3) 0.8826(3) 0.0354(8) Uani 1 1 d . . . H43 H 0.4906 0.5009 0.8565 0.042 Uiso 1 1 calc R C . C44 C 0.6170(3) 0.5810(3) 0.8156(3) 0.0284(7) Uani 1 1 d . C . H44 H 0.5742 0.5434 0.7437 0.034 Uiso 1 1 calc R . . C45 C 1.7078(3) 1.3352(3) 0.9599(3) 0.0323(8) Uani 1 1 d . . . H45A H 1.6409 1.3558 0.9684 0.039 Uiso 1 1 calc R . . H45B H 1.7140 1.2880 0.9937 0.039 Uiso 1 1 calc R . . C46 C 1.6914(4) 1.2756(4) 0.8538(4) 0.0556(12) Uani 1 1 d . . . H46A H 1.6077 1.2352 0.8132 0.067 Uiso 1 1 calc R . . H46B H 1.7278 1.2203 0.8424 0.067 Uiso 1 1 calc R . . C50 C 1.7459(4) 1.3579(4) 0.8218(3) 0.0486(10) Uani 1 1 d . . . H50A H 1.6917 1.3901 0.8016 0.058 Uiso 1 1 calc R . . H50B H 1.7722 1.3237 0.7631 0.058 Uiso 1 1 calc R . . C51 C 1.8086(4) 1.4310(3) 1.0051(3) 0.0448(10) Uani 1 1 d . . . H51A H 1.8696 1.4235 1.0506 0.054 Uiso 1 1 calc R . . H51B H 1.7940 1.4968 1.0477 0.054 Uiso 1 1 calc R . . C70 C 0.590(4) 1.099(2) 0.536(2) 0.107(16) Uiso 0.25 1 d PD A -1 H70A H 0.5698 1.1491 0.5115 0.128 Uiso 0.25 1 calc PR A -1 H70B H 0.6754 1.1243 0.5634 0.128 Uiso 0.25 1 calc PR A -1 C71 C 0.5352(12) 0.9805(10) 0.4547(10) 0.016(2) Uiso 0.25 1 d PD A -1 H71A H 0.5923 0.9457 0.4577 0.019 Uiso 0.25 1 calc PR A -1 H71B H 0.5163 0.9791 0.3866 0.019 Uiso 0.25 1 calc PR A -1 C72 C 0.428(2) 0.9112(18) 0.461(2) 0.048(7) Uiso 0.25 1 d PD A -1 H72A H 0.3606 0.8784 0.3981 0.058 Uiso 0.25 1 calc PR A -1 H72B H 0.4384 0.8516 0.4769 0.058 Uiso 0.25 1 calc PR A -1 C73 C 0.4221(14) 1.0011(13) 0.5487(14) 0.034(4) Uiso 0.25 1 d PD A -1 H73A H 0.3715 1.0333 0.5230 0.040 Uiso 0.25 1 calc PR A -1 H73B H 0.3874 0.9704 0.5906 0.040 Uiso 0.25 1 calc PR A -1 C80 C 0.4109(16) 0.8904(15) 0.4280(13) 0.029(4) Uiso 0.25 1 d PD B -2 H80A H 0.4119 0.8151 0.3925 0.035 Uiso 0.25 1 calc PR B -2 H80B H 0.3490 0.8965 0.3821 0.035 Uiso 0.25 1 calc PR B -2 C81 C 0.3914(11) 0.9107(9) 0.5292(9) 0.024(3) Uiso 0.25 1 d PD B -2 H81A H 0.3078 0.8796 0.5195 0.029 Uiso 0.25 1 calc PR B -2 H81B H 0.4324 0.8782 0.5645 0.029 Uiso 0.25 1 calc PR B -2 C82 C 0.4395(15) 1.0297(13) 0.5850(15) 0.040(4) Uiso 0.25 1 d PD B -2 H82A H 0.4670 1.0548 0.6602 0.048 Uiso 0.25 1 calc PR B -2 H82B H 0.3798 1.0589 0.5703 0.048 Uiso 0.25 1 calc PR B -2 C83 C 0.5365(13) 1.0721(13) 0.5527(13) 0.027(3) Uiso 0.25 1 d PD B -2 H83A H 0.6113 1.0972 0.6064 0.032 Uiso 0.25 1 calc PR B -2 H83B H 0.5333 1.1360 0.5414 0.032 Uiso 0.25 1 calc PR B -2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.01737(6) 0.01858(6) 0.01818(6) 0.00988(5) 0.00707(4) 0.00823(4) Ca1 0.0185(3) 0.0221(3) 0.0171(3) 0.0101(2) 0.0070(2) 0.0095(2) P1 0.0181(3) 0.0182(3) 0.0151(3) 0.0087(3) 0.0054(3) 0.0077(3) P2 0.0193(3) 0.0183(3) 0.0164(4) 0.0098(3) 0.0080(3) 0.0082(3) O1 0.0241(11) 0.0277(12) 0.0334(13) 0.0119(10) 0.0065(10) 0.0079(10) O2 0.0271(11) 0.0219(10) 0.0282(12) 0.0113(9) 0.0101(10) 0.0122(9) O3 0.092(3) 0.087(3) 0.103(3) 0.047(3) 0.033(3) 0.028(2) C1 0.0234(15) 0.0260(15) 0.0221(15) 0.0154(13) 0.0095(13) 0.0094(12) C2 0.0231(15) 0.0418(18) 0.0235(16) 0.0204(15) 0.0128(13) 0.0146(14) C3 0.0306(16) 0.0375(17) 0.0178(15) 0.0156(14) 0.0122(13) 0.0211(14) C4 0.0235(14) 0.0243(15) 0.0159(14) 0.0094(12) 0.0055(12) 0.0103(12) C5 0.0210(14) 0.0251(14) 0.0146(14) 0.0108(12) 0.0082(12) 0.0124(12) C6 0.0214(14) 0.0229(14) 0.0159(14) 0.0113(12) 0.0093(12) 0.0102(12) C7 0.0273(15) 0.0308(16) 0.0247(16) 0.0193(14) 0.0139(13) 0.0165(13) C8 0.0245(15) 0.0434(19) 0.0210(16) 0.0194(14) 0.0091(13) 0.0181(14) C9 0.0248(15) 0.0340(17) 0.0138(14) 0.0074(13) 0.0051(12) 0.0120(14) C10 0.0238(15) 0.0250(15) 0.0163(14) 0.0089(12) 0.0080(12) 0.0117(12) C11 0.0329(17) 0.0382(18) 0.0341(18) 0.0209(16) 0.0225(15) 0.0213(15) C12 0.0237(15) 0.0294(16) 0.0316(18) 0.0177(14) 0.0094(14) 0.0169(13) C13 0.082(8) 0.019(4) 0.128(13) 0.020(6) -0.047(8) 0.004(4) C13A 0.0254(16) 0.0373(18) 0.047(2) 0.0232(16) 0.0133(15) 0.0162(14) C14 0.060(5) 0.022(5) 0.151(13) 0.011(6) 0.078(8) -0.003(4) C14A 0.052(2) 0.044(2) 0.046(2) 0.0271(18) 0.0237(19) 0.0327(19) C15 0.118(13) 0.028(5) 0.25(2) 0.016(11) 0.152(16) 0.009(7) C15A 0.011(4) 0.030(6) 0.089(11) 0.012(7) 0.013(6) 0.005(4) C16 0.028(4) 0.034(4) 0.059(5) 0.014(4) 0.025(4) 0.014(3) C16A 0.027(6) 0.038(7) 0.23(3) 0.036(13) -0.005(12) 0.014(5) C17 0.0254(16) 0.0373(18) 0.047(2) 0.0232(16) 0.0133(15) 0.0162(14) C18 0.052(2) 0.044(2) 0.046(2) 0.0271(18) 0.0237(19) 0.0327(19) C19 0.062(3) 0.0249(17) 0.032(2) 0.0150(15) 0.0166(19) 0.0146(17) C20 0.043(2) 0.0232(16) 0.0265(17) 0.0097(14) 0.0104(16) 0.0104(15) C21 0.0254(15) 0.0183(14) 0.0176(14) 0.0079(12) 0.0038(12) 0.0094(12) C22 0.0274(16) 0.0253(16) 0.0259(17) 0.0096(13) 0.0022(14) 0.0107(13) C23 0.0365(19) 0.0327(19) 0.0310(19) 0.0054(16) -0.0092(16) 0.0129(16) C24 0.059(3) 0.037(2) 0.0184(17) 0.0079(15) -0.0042(17) 0.0206(19) C25 0.060(2) 0.0320(18) 0.0184(16) 0.0106(14) 0.0107(17) 0.0213(18) C26 0.0387(18) 0.0261(16) 0.0192(15) 0.0113(13) 0.0095(14) 0.0127(14) C27 0.0185(13) 0.0208(14) 0.0175(14) 0.0099(12) 0.0074(11) 0.0093(11) C28 0.0282(16) 0.0238(15) 0.0204(15) 0.0135(12) 0.0075(13) 0.0099(13) C29 0.0343(17) 0.0244(15) 0.0176(15) 0.0072(13) 0.0076(14) 0.0087(14) C30 0.0317(17) 0.0192(14) 0.0297(17) 0.0122(13) 0.0108(14) 0.0086(13) C31 0.0368(18) 0.0256(16) 0.0259(16) 0.0173(14) 0.0135(15) 0.0115(14) C32 0.0311(16) 0.0244(15) 0.0210(15) 0.0117(13) 0.0110(13) 0.0105(13) C33 0.0228(14) 0.0199(14) 0.0204(15) 0.0095(12) 0.0110(12) 0.0082(12) C34 0.0314(17) 0.0232(15) 0.0286(17) 0.0129(13) 0.0112(14) 0.0105(13) C35 0.042(2) 0.0223(16) 0.040(2) 0.0123(15) 0.0219(17) 0.0167(15) C36 0.0391(19) 0.0226(16) 0.0299(18) 0.0035(14) 0.0146(16) 0.0080(15) C37 0.0372(19) 0.0314(18) 0.0213(17) 0.0064(14) 0.0055(15) 0.0063(15) C38 0.0296(16) 0.0246(15) 0.0258(16) 0.0112(13) 0.0106(14) 0.0099(13) C39 0.0263(15) 0.0216(14) 0.0253(15) 0.0154(12) 0.0144(13) 0.0144(12) C40 0.0313(17) 0.0349(17) 0.0246(16) 0.0190(14) 0.0159(14) 0.0157(14) C41 0.043(2) 0.045(2) 0.0264(18) 0.0216(16) 0.0194(16) 0.0205(17) C42 0.046(2) 0.041(2) 0.039(2) 0.0280(17) 0.0313(18) 0.0211(17) C43 0.0387(19) 0.0312(18) 0.043(2) 0.0206(16) 0.0246(17) 0.0113(16) C44 0.0306(17) 0.0274(16) 0.0297(17) 0.0156(14) 0.0135(15) 0.0092(14) C45 0.0264(16) 0.043(2) 0.0246(17) 0.0199(15) 0.0098(14) 0.0023(15) C46 0.045(2) 0.058(3) 0.053(3) 0.029(2) 0.008(2) 0.005(2) C50 0.042(2) 0.065(3) 0.043(2) 0.033(2) 0.0074(19) 0.021(2) C51 0.057(3) 0.043(2) 0.036(2) 0.0224(18) 0.0096(19) 0.0197(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 C11 2.083(3) . ? Pt1 C12 2.105(3) . ? Pt1 P2 2.2900(7) . ? Pt1 P1 2.2913(7) . ? Ca1 O1 2.354(2) . ? Ca1 O2 2.403(2) . ? Ca1 C6 2.664(3) . ? Ca1 C3 2.677(3) . ? Ca1 C10 2.682(3) . ? Ca1 C4 2.689(3) . ? Ca1 C7 2.704(3) . ? Ca1 C2 2.705(3) . ? Ca1 C9 2.727(3) . ? Ca1 C8 2.735(3) . ? Ca1 C5 2.744(3) . ? Ca1 C1 2.752(3) . ? P1 C5 1.806(3) . ? P1 C21 1.834(3) . ? P1 C27 1.847(3) . ? P2 C6 1.794(3) . ? P2 C33 1.835(3) . ? P2 C39 1.841(3) . ? O1 C13A 1.390(17) . ? O1 C16 1.407(7) . ? O1 C16A 1.410(16) . ? O1 C13 1.503(10) . ? O2 C20 1.450(4) . ? O2 C17 1.457(4) . ? O3 C50 1.528(6) . ? O3 C51 1.543(6) . ? O51 C73 1.445(16) . ? O51 C70 1.478(19) . ? O61 C80 1.48(2) . ? O61 C83 1.48(2) . ? C1 C2 1.410(4) . ? C1 C5 1.409(4) . ? C2 C3 1.400(5) . ? C3 C4 1.406(4) . ? C4 C5 1.422(4) . ? C6 C10 1.420(4) . ? C6 C7 1.422(4) . ? C7 C8 1.394(4) . ? C8 C9 1.404(5) . ? C9 C10 1.403(4) . ? C13 C14 1.37(2) . ? C13A C14A 1.56(3) . ? C14 C15 1.418(19) . ? C14A C15A 1.48(2) . ? C15 C16 1.439(15) . ? C15A C16A 1.51(2) . ? C17 C18 1.523(5) . ? C18 C19 1.517(6) . ? C19 C20 1.516(5) . ? C21 C22 1.396(4) . ? C21 C26 1.398(4) . ? C22 C23 1.386(5) . ? C23 C24 1.382(6) . ? C24 C25 1.380(6) . ? C25 C26 1.386(5) . ? C27 C28 1.386(4) . ? C27 C32 1.399(4) . ? C28 C29 1.392(4) . ? C29 C30 1.383(4) . ? C30 C31 1.381(4) . ? C31 C32 1.382(4) . ? C33 C38 1.392(4) . ? C33 C34 1.396(4) . ? C34 C35 1.385(5) . ? C35 C36 1.385(5) . ? C36 C37 1.373(5) . ? C37 C38 1.398(4) . ? C39 C40 1.377(4) . ? C39 C44 1.389(4) . ? C40 C41 1.398(4) . ? C41 C42 1.387(5) . ? C42 C43 1.373(5) . ? C43 C44 1.386(5) . ? C45 C51 1.387(5) . ? C45 C46 1.411(5) . ? C46 C50 1.470(6) . ? C70 C71 1.478(19) . ? C71 C72 1.483(18) . ? C72 C73 1.455(17) . ? C80 C81 1.504(15) . ? C81 C82 1.424(15) . ? C82 C83 1.467(17) . ? 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 C11 Pt1 C12 82.56(13) . . ? C11 Pt1 P2 91.81(9) . . ? C12 Pt1 P2 174.37(9) . . ? C11 Pt1 P1 168.84(9) . . ? C12 Pt1 P1 86.33(9) . . ? P2 Pt1 P1 99.30(3) . . ? O1 Ca1 O2 93.82(8) . . ? O1 Ca1 C6 131.88(9) . . ? O2 Ca1 C6 108.69(8) . . ? O1 Ca1 C3 107.79(9) . . ? O2 Ca1 C3 79.75(9) . . ? C6 Ca1 C3 117.55(10) . . ? O1 Ca1 C10 103.66(9) . . ? O2 Ca1 C10 130.81(9) . . ? C6 Ca1 C10 30.80(9) . . ? C3 Ca1 C10 133.94(10) . . ? O1 Ca1 C4 131.19(9) . . ? O2 Ca1 C4 97.24(8) . . ? C6 Ca1 C4 88.47(9) . . ? C3 Ca1 C4 30.39(9) . . ? C10 Ca1 C4 104.21(9) . . ? O1 Ca1 C7 122.18(9) . . ? O2 Ca1 C7 81.68(8) . . ? C6 Ca1 C7 30.71(9) . . ? C3 Ca1 C7 127.45(10) . . ? C10 Ca1 C7 50.02(9) . . ? C4 Ca1 C7 106.44(10) . . ? O1 Ca1 C2 81.71(9) . . ? O2 Ca1 C2 96.26(9) . . ? C6 Ca1 C2 134.28(9) . . ? C3 Ca1 C2 30.16(10) . . ? C10 Ca1 C2 131.26(10) . . ? C4 Ca1 C2 49.94(9) . . ? C7 Ca1 C2 156.06(10) . . ? O1 Ca1 C9 82.01(9) . . ? O2 Ca1 C9 112.94(9) . . ? C6 Ca1 C9 50.26(9) . . ? C3 Ca1 C9 163.91(10) . . ? C10 Ca1 C9 30.06(9) . . ? C4 Ca1 C9 134.14(9) . . ? C7 Ca1 C9 49.36(10) . . ? C2 Ca1 C9 147.33(10) . . ? O1 Ca1 C8 92.57(9) . . ? O2 Ca1 C8 84.58(9) . . ? C6 Ca1 C8 50.10(9) . . ? C3 Ca1 C8 154.95(10) . . ? C10 Ca1 C8 49.57(9) . . ? C4 Ca1 C8 135.67(10) . . ? C7 Ca1 C8 29.68(9) . . ? C2 Ca1 C8 174.25(10) . . ? C9 Ca1 C8 29.78(10) . . ? O1 Ca1 C5 114.74(9) . . ? O2 Ca1 C5 126.83(8) . . ? C6 Ca1 C5 85.15(9) . . ? C3 Ca1 C5 49.91(9) . . ? C10 Ca1 C5 86.57(9) . . ? C4 Ca1 C5 30.33(9) . . ? C7 Ca1 C5 113.32(9) . . ? C2 Ca1 C5 49.65(9) . . ? C9 Ca1 C5 114.67(9) . . ? C8 Ca1 C5 133.70(9) . . ? O1 Ca1 C1 86.14(9) . . ? O2 Ca1 C1 125.68(8) . . ? C6 Ca1 C1 111.04(9) . . ? C3 Ca1 C1 49.45(9) . . ? C10 Ca1 C1 101.39(9) . . ? C4 Ca1 C1 49.49(9) . . ? C7 Ca1 C1 141.31(9) . . ? C2 Ca1 C1 29.93(9) . . ? C9 Ca1 C1 120.75(10) . . ? C8 Ca1 C1 149.74(10) . . ? C5 Ca1 C1 29.70(9) . . ? C5 P1 C21 99.83(13) . . ? C5 P1 C27 102.12(13) . . ? C21 P1 C27 103.65(13) . . ? C5 P1 Pt1 127.29(10) . . ? C21 P1 Pt1 112.65(10) . . ? C27 P1 Pt1 108.64(9) . . ? C6 P2 C33 110.25(13) . . ? C6 P2 C39 101.26(13) . . ? C33 P2 C39 99.75(13) . . ? C6 P2 Pt1 115.72(10) . . ? C33 P2 Pt1 113.69(10) . . ? C39 P2 Pt1 114.41(9) . . ? C13A O1 C16 110.8(7) . . ? C13A O1 C16A 101.0(10) . . ? C16 O1 C16A 45.4(13) . . ? C13A O1 C13 19.1(10) . . ? C16 O1 C13 100.4(9) . . ? C16A O1 C13 105.5(7) . . ? C13A O1 Ca1 121.2(6) . . ? C16 O1 Ca1 125.2(4) . . ? C16A O1 Ca1 129.7(7) . . ? C13 O1 Ca1 123.5(5) . . ? C20 O2 C17 108.9(2) . . ? C20 O2 Ca1 118.04(19) . . ? C17 O2 Ca1 127.92(19) . . ? C50 O3 C51 101.9(3) . . ? C73 O51 C70 102.8(19) . . ? C80 O61 C83 104(2) . . ? C2 C1 C5 108.5(3) . . ? C2 C1 Ca1 73.19(17) . . ? C5 C1 Ca1 74.84(16) . . ? C3 C2 C1 107.9(3) . . ? C3 C2 Ca1 73.81(17) . . ? C1 C2 Ca1 76.88(17) . . ? C2 C3 C4 108.4(3) . . ? C2 C3 Ca1 76.03(18) . . ? C4 C3 Ca1 75.26(17) . . ? C3 C4 C5 108.0(3) . . ? C3 C4 Ca1 74.35(17) . . ? C5 C4 Ca1 77.00(16) . . ? C1 C5 C4 107.2(3) . . ? C1 C5 P1 127.2(2) . . ? C4 C5 P1 123.9(2) . . ? C1 C5 Ca1 75.45(17) . . ? C4 C5 Ca1 72.67(16) . . ? P1 C5 Ca1 129.03(13) . . ? C10 C6 C7 106.5(3) . . ? C10 C6 P2 119.6(2) . . ? C7 C6 P2 131.4(2) . . ? C10 C6 Ca1 75.31(16) . . ? C7 C6 Ca1 76.20(16) . . ? P2 C6 Ca1 127.75(13) . . ? C8 C7 C6 108.6(3) . . ? C8 C7 Ca1 76.41(18) . . ? C6 C7 Ca1 73.08(16) . . ? C7 C8 C9 108.3(3) . . ? C7 C8 Ca1 73.90(17) . . ? C9 C8 Ca1 74.80(18) . . ? C10 C9 C8 108.1(3) . . ? C10 C9 Ca1 73.17(17) . . ? C8 C9 Ca1 75.42(17) . . ? C9 C10 C6 108.4(3) . . ? C9 C10 Ca1 76.77(17) . . ? C6 C10 Ca1 73.89(16) . . ? C14 C13 O1 106.5(10) . . ? O1 C13A C14A 111.3(12) . . ? C13 C14 C15 101.2(14) . . ? C15A C14A C13A 100.0(14) . . ? C14 C15 C16 107.9(10) . . ? C14A C15A C16A 105.3(12) . . ? O1 C16 C15 107.5(7) . . ? O1 C16A C15A 107.5(14) . . ? O2 C17 C18 106.1(3) . . ? C19 C18 C17 102.8(3) . . ? C20 C19 C18 101.7(3) . . ? O2 C20 C19 104.9(3) . . ? C22 C21 C26 118.5(3) . . ? C22 C21 P1 120.5(2) . . ? C26 C21 P1 121.0(2) . . ? C23 C22 C21 120.3(3) . . ? C24 C23 C22 120.5(4) . . ? C25 C24 C23 119.8(3) . . ? C24 C25 C26 120.1(4) . . ? C25 C26 C21 120.6(3) . . ? C28 C27 C32 118.4(3) . . ? C28 C27 P1 117.5(2) . . ? C32 C27 P1 124.1(2) . . ? C27 C28 C29 120.8(3) . . ? C30 C29 C28 120.1(3) . . ? C31 C30 C29 119.6(3) . . ? C30 C31 C32 120.4(3) . . ? C31 C32 C27 120.7(3) . . ? C38 C33 C34 118.3(3) . . ? C38 C33 P2 118.4(2) . . ? C34 C33 P2 123.2(2) . . ? C35 C34 C33 120.7(3) . . ? C36 C35 C34 120.3(3) . . ? C37 C36 C35 120.0(3) . . ? C36 C37 C38 119.9(3) . . ? C33 C38 C37 120.9(3) . . ? C40 C39 C44 118.5(3) . . ? C40 C39 P2 120.3(2) . . ? C44 C39 P2 121.0(2) . . ? C39 C40 C41 121.2(3) . . ? C42 C41 C40 119.4(3) . . ? C43 C42 C41 119.7(3) . . ? C42 C43 C44 120.5(3) . . ? C43 C44 C39 120.7(3) . . ? C51 C45 C46 108.7(3) . . ? C45 C46 C50 107.1(4) . . ? C46 C50 O3 103.3(4) . . ? C45 C51 O3 108.6(3) . . ? C71 C70 O51 99.0(15) . . ? C70 C71 C72 115.4(15) . . ? C73 C72 C71 96.4(16) . . ? O51 C73 C72 111.3(17) . . ? O61 C80 C81 105(2) . . ? C82 C81 C80 101.7(12) . . ? C81 C82 C83 108.5(13) . . ? C82 C83 O61 106.6(19) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.287 _refine_diff_density_min -0.855 _refine_diff_density_rms 0.113 # Attachment '- 11b.CIF' data_11b.CIF _database_code_depnum_ccdc_archive 'CCDC 828930' #TrackingRef '- 11b.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 1 _chemical_melting_point ? _chemical_formula_moiety 'C52 H66 Ba O4 P2 Pt' _chemical_formula_sum 'C52 H66 Ba O4 P2 Pt' _chemical_formula_weight 1149.42 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' Ba Ba -0.3244 2.2819 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.2232(3) _cell_length_b 22.8323(6) _cell_length_c 26.7122(7) _cell_angle_alpha 68.8400(10) _cell_angle_beta 81.1030(10) _cell_angle_gamma 75.6370(10) _cell_volume 7267.1(3) _cell_formula_units_Z 6 _cell_measurement_temperature 123 _cell_measurement_reflns_used 123721 _cell_measurement_theta_min 1.04 _cell_measurement_theta_max 27.50 _exptl_crystal_description Prism _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.576 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3444 _exptl_absorpt_coefficient_mu 3.801 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.4500 _exptl_absorpt_correction_T_max 0.5169 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 123 _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 X8 Apex II CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 123721 _diffrn_reflns_av_R_equivalents 0.0678 _diffrn_reflns_av_sigmaI/netI 0.0829 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.04 _diffrn_reflns_theta_max 27.50 _reflns_number_total 32973 _reflns_number_gt 21958 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker)' _computing_cell_refinement 'Bruker SMART (Bruker)' _computing_data_reduction 'Bruker SMART (Bruker)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _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 fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0302P)^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 ? _refine_ls_extinction_coef none _refine_ls_number_reflns 32973 _refine_ls_number_parameters 1627 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0848 _refine_ls_R_factor_gt 0.0415 _refine_ls_wR_factor_ref 0.0880 _refine_ls_wR_factor_gt 0.0737 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.017 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.589970(15) 0.106310(10) 0.337670(8) 0.020 Uani 1 1 d . . . Pt1A Pt 0.790830(15) 0.229300(9) -0.000620(8) 0.016 Uani 1 1 d . . . Pt1B Pt 0.892090(16) 0.446650(10) -0.332830(8) 0.020 Uani 1 1 d . . . Ba1 Ba 0.36054(2) 0.027700(15) 0.236850(13) 0.020 Uani 1 1 d . . . Ba2 Ba 1.04340(2) 0.303530(14) 0.090800(12) 0.018 Uani 1 1 d . . . Ba3 Ba 0.68769(2) 0.335770(16) -0.412490(13) 0.022 Uani 1 1 d . . . P1 P 0.64102(10) 0.01446(6) 0.31485(6) 0.019 Uani 1 1 d . . . P1A P 0.75298(10) 0.31948(6) 0.02421(5) 0.016 Uani 1 1 d . . . P1B P 0.71891(10) 0.44183(6) -0.31182(5) 0.019 Uani 1 1 d . . . P2 P 0.41329(10) 0.11122(6) 0.35164(5) 0.018 Uani 1 1 d . . . P2A P 0.96912(10) 0.21815(6) -0.01665(5) 0.017 Uani 1 1 d . . . P2B P 0.95944(10) 0.35139(6) -0.34960(5) 0.019 Uani 1 1 d . . . O1 O 0.4342(3) 0.06617(19) 0.13067(15) 0.035 Uani 1 1 d . . . O1A O 0.9476(3) 0.27703(18) 0.19499(15) 0.034 Uani 1 1 d . . . O1B O 0.5376(3) 0.27214(18) -0.34584(15) 0.030 Uani 1 1 d . . . O2 O 0.2635(3) -0.02493(17) 0.17991(15) 0.030 Uani 1 1 d . . . O2A O 1.1039(3) 0.37805(18) 0.13990(15) 0.032 Uani 1 1 d . . . O2B O 0.6023(3) 0.2880(2) -0.47418(16) 0.039 Uani 1 1 d . . . O3 O 0.1992(3) -0.02507(19) 0.30055(15) 0.035 Uani 1 1 d . . . O3A O 1.2358(3) 0.33210(18) 0.04598(16) 0.035 Uani 1 1 d . . . O3B O 0.7721(3) 0.38682(19) -0.51506(15) 0.042 Uani 1 1 d . . . O4 O -0.0248(3) -0.1230(2) 0.60293(18) 0.051 Uani 1 1 d . . . O4A O 0.3519(3) 0.1833(2) -0.04711(18) 0.053 Uani 1 1 d . . . O4B O 0.6622(3) 0.58635(19) -0.79436(16) 0.041 Uani 1 1 d . . . C1 C 0.5869(4) -0.0505(2) 0.2512(2) 0.023 Uani 1 1 d . . . H1 H 0.6342 -0.0368 0.2221 0.028 Uiso 1 1 calc R . . C1A C 0.9861(4) 0.1824(2) 0.0934(2) 0.019 Uani 1 1 d . . . H1A H 0.9147 0.1840 0.1013 0.023 Uiso 1 1 calc R . . C1B C 0.5486(4) 0.4237(3) -0.3572(2) 0.027 Uani 1 1 d . . . H1B H 0.5146 0.4020 -0.3252 0.032 Uiso 1 1 calc R . . C2 C 0.5268(4) -0.0953(2) 0.2575(2) 0.025 Uani 1 1 d . . . H2 H 0.5261 -0.1160 0.2334 0.030 Uiso 1 1 calc R . . C2A C 1.0608(4) 0.1590(2) 0.1316(2) 0.023 Uani 1 1 d . . . H2A H 1.0482 0.1422 0.1688 0.028 Uiso 1 1 calc R . . C2B C 0.5093(4) 0.4467(3) -0.4075(2) 0.028 Uani 1 1 d . . . H2B H 0.4459 0.4423 -0.4152 0.033 Uiso 1 1 calc R . . C3 C 0.4668(4) -0.1033(2) 0.3075(2) 0.024 Uani 1 1 d . . . H3 H 0.4207 -0.1311 0.3222 0.029 Uiso 1 1 calc R . . C3A C 1.1594(4) 0.1656(2) 0.1030(2) 0.024 Uani 1 1 d . . . H3A H 1.2231 0.1544 0.1183 0.029 Uiso 1 1 calc R . . C3B C 0.5834(4) 0.4779(3) -0.4448(2) 0.031 Uani 1 1 d . . . H3B H 0.5765 0.4989 -0.4814 0.037 Uiso 1 1 calc R . . C4 C 0.4888(4) -0.0623(2) 0.3310(2) 0.022 Uani 1 1 d . . . H4 H 0.4588 -0.0578 0.3636 0.026 Uiso 1 1 calc R . . C4A C 1.1443(4) 0.1921(2) 0.0477(2) 0.018 Uani 1 1 d . . . H4A H 1.1965 0.2007 0.0201 0.022 Uiso 1 1 calc R . . C4B C 0.6692(4) 0.4718(2) -0.4170(2) 0.026 Uani 1 1 d . . . H4B H 0.7298 0.4872 -0.4321 0.031 Uiso 1 1 calc R . . C5 C 0.5646(4) -0.0289(2) 0.2967(2) 0.020 Uani 1 1 d . . . C5A C 1.0357(4) 0.2034(2) 0.0411(2) 0.018 Uani 1 1 d . . . C5B C 0.6474(4) 0.4382(2) -0.3619(2) 0.020 Uani 1 1 d . . . C6 C 0.3511(4) 0.1242(2) 0.2930(2) 0.019 Uani 1 1 d . . . C6A C 0.8409(4) 0.3620(2) 0.0351(2) 0.018 Uani 1 1 d . . . C6B C 0.8937(4) 0.2977(2) -0.3611(2) 0.020 Uani 1 1 d . . . C7 C 0.2438(4) 0.1311(2) 0.2845(2) 0.022 Uani 1 1 d . . . H7 H 0.1917 0.1183 0.3112 0.027 Uiso 1 1 calc R . . C7A C 0.9184(4) 0.3873(2) -0.0038(2) 0.021 Uani 1 1 d . . . H7A H 0.9429 0.3764 -0.0345 0.025 Uiso 1 1 calc R . . C7B C 0.9197(4) 0.2716(2) -0.4033(2) 0.024 Uani 1 1 d . . . H7B H 0.9628 0.2860 -0.4342 0.029 Uiso 1 1 calc R . . C8 C 0.2305(4) 0.1600(3) 0.2300(2) 0.029 Uani 1 1 d . . . H8 H 0.1678 0.1697 0.2142 0.035 Uiso 1 1 calc R . . C8A C 0.9523(4) 0.4312(2) 0.0113(2) 0.021 Uani 1 1 d . . . H8A H 1.0034 0.4543 -0.0074 0.025 Uiso 1 1 calc R . . C8B C 0.8691(4) 0.2202(3) -0.3903(2) 0.027 Uani 1 1 d . . . H8B H 0.8735 0.1945 -0.4110 0.033 Uiso 1 1 calc R . . C9 C 0.3279(4) 0.1727(2) 0.2017(2) 0.027 Uani 1 1 d . . . H9 H 0.3409 0.1913 0.1648 0.032 Uiso 1 1 calc R . . C9A C 0.8963(4) 0.4346(2) 0.0595(2) 0.024 Uani 1 1 d . . . H9A H 0.9030 0.4605 0.0784 0.029 Uiso 1 1 calc R . . C9B C 0.8107(4) 0.2140(3) -0.3405(2) 0.030 Uani 1 1 d . . . H9B H 0.7691 0.1840 -0.3231 0.035 Uiso 1 1 calc R . . C10 C 0.3995(4) 0.1514(2) 0.2410(2) 0.023 Uani 1 1 d . . . H10 H 0.4694 0.1546 0.2342 0.028 Uiso 1 1 calc R . . C10A C 0.8280(4) 0.3919(2) 0.0742(2) 0.021 Uani 1 1 d . . . H10A H 0.7819 0.3845 0.1047 0.026 Uiso 1 1 calc R . . C10B C 0.8262(4) 0.2608(2) -0.3218(2) 0.024 Uani 1 1 d . . . H10B H 0.7975 0.2669 -0.2896 0.029 Uiso 1 1 calc R . . C11 C 0.5724(4) 0.1883(3) 0.3579(2) 0.033 Uani 1 1 d . . . H11G H 0.5490 0.1793 0.3952 0.050 Uiso 1 1 calc R . . H11H H 0.5218 0.2222 0.3362 0.050 Uiso 1 1 calc R . . H11I H 0.6383 0.2012 0.3514 0.050 Uiso 1 1 calc R . . C11A C 0.7972(4) 0.1499(2) -0.0228(2) 0.023 Uani 1 1 d . . . H11A H 0.7285 0.1408 -0.0177 0.035 Uiso 1 1 calc R . . H11B H 0.8439 0.1134 -0.0009 0.035 Uiso 1 1 calc R . . H11C H 0.8221 0.1588 -0.0600 0.035 Uiso 1 1 calc R . . C11B C 1.0462(4) 0.4602(3) -0.3463(2) 0.030 Uani 1 1 d . . . H11D H 1.0527 0.4954 -0.3791 0.045 Uiso 1 1 calc R . . H11E H 1.0930 0.4219 -0.3493 0.045 Uiso 1 1 calc R . . H11F H 1.0634 0.4696 -0.3168 0.045 Uiso 1 1 calc R . . C12 C 0.7479(4) 0.1112(3) 0.3253(2) 0.031 Uani 1 1 d . . . H12D H 0.7581 0.1469 0.2936 0.046 Uiso 1 1 calc R . . H12E H 0.7891 0.0722 0.3208 0.046 Uiso 1 1 calc R . . H12F H 0.7690 0.1166 0.3559 0.046 Uiso 1 1 calc R . . C12A C 0.6303(4) 0.2309(2) 0.0136(2) 0.023 Uani 1 1 d . . . H12A H 0.6080 0.2176 -0.0124 0.035 Uiso 1 1 calc R . . H12B H 0.5928 0.2737 0.0105 0.035 Uiso 1 1 calc R . . H12C H 0.6164 0.2022 0.0491 0.035 Uiso 1 1 calc R . . C12B C 0.8620(4) 0.5366(3) -0.3251(2) 0.038 Uani 1 1 d . . . H12G H 0.8565 0.5321 -0.2877 0.057 Uiso 1 1 calc R . . H12H H 0.7975 0.5615 -0.3407 0.057 Uiso 1 1 calc R . . H12I H 0.9181 0.5580 -0.3434 0.057 Uiso 1 1 calc R . . C13 C 0.5267(4) 0.0919(3) 0.1237(2) 0.034 Uani 1 1 d . . . H13E H 0.5549 0.0812 0.1580 0.041 Uiso 1 1 calc R . . H13F H 0.5112 0.1382 0.1067 0.041 Uiso 1 1 calc R . . C13A C 0.9340(5) 0.2191(3) 0.2392(2) 0.035 Uani 1 1 d . . . H13C H 1.0003 0.1887 0.2463 0.042 Uiso 1 1 calc R . . H13D H 0.8850 0.1990 0.2311 0.042 Uiso 1 1 calc R . . C13B C 0.5360(4) 0.2584(3) -0.2880(2) 0.030 Uani 1 1 d . . . H13A H 0.5813 0.2815 -0.2807 0.036 Uiso 1 1 calc R . . H13B H 0.5609 0.2128 -0.2699 0.036 Uiso 1 1 calc R . . C14 C 0.6026(5) 0.0606(3) 0.0881(2) 0.044 Uani 1 1 d . . . H14E H 0.6339 0.0166 0.1079 0.053 Uiso 1 1 calc R . . H14F H 0.6573 0.0844 0.0710 0.053 Uiso 1 1 calc R . . C14A C 0.8924(8) 0.2408(4) 0.2860(3) 0.085 Uani 1 1 d . . . H14C H 0.8211 0.2349 0.2967 0.102 Uiso 1 1 calc R . . H14D H 0.9348 0.2160 0.3163 0.102 Uiso 1 1 calc R . . C14B C 0.4233(4) 0.2795(3) -0.2673(2) 0.037 Uani 1 1 d . . . H14A H 0.4193 0.3090 -0.2481 0.045 Uiso 1 1 calc R . . H14B H 0.3952 0.2428 -0.2435 0.045 Uiso 1 1 calc R . . C15 C 0.5306(5) 0.0643(3) 0.0479(2) 0.048 Uani 1 1 d . . . H15C H 0.5583 0.0312 0.0317 0.057 Uiso 1 1 calc R . . H15D H 0.5208 0.1060 0.0197 0.057 Uiso 1 1 calc R . . C15A C 0.8954(7) 0.3077(4) 0.2698(3) 0.087 Uani 1 1 d . . . H15E H 0.9585 0.3131 0.2805 0.104 Uiso 1 1 calc R . . H15F H 0.8350 0.3307 0.2857 0.104 Uiso 1 1 calc R . . C15B C 0.3640(4) 0.3128(3) -0.3187(2) 0.037 Uani 1 1 d . . . H15A H 0.2936 0.3049 -0.3126 0.045 Uiso 1 1 calc R . . H15B H 0.3604 0.3588 -0.3319 0.045 Uiso 1 1 calc R . . C16 C 0.4270(5) 0.0534(3) 0.0818(2) 0.045 Uani 1 1 d . . . H16E H 0.3677 0.0824 0.0626 0.054 Uiso 1 1 calc R . . H16F H 0.4194 0.0096 0.0904 0.054 Uiso 1 1 calc R . . C16A C 0.8941(5) 0.3306(3) 0.2112(2) 0.049 Uani 1 1 d . . . H16C H 0.8227 0.3447 0.2005 0.059 Uiso 1 1 calc R . . H16D H 0.9296 0.3662 0.1949 0.059 Uiso 1 1 calc R . . C16B C 0.4310(4) 0.2812(3) -0.3574(2) 0.035 Uani 1 1 d . . . H16A H 0.4138 0.2402 -0.3517 0.042 Uiso 1 1 calc R . . H16B H 0.4201 0.3085 -0.3943 0.042 Uiso 1 1 calc R . . C17 C 0.1880(4) -0.0042(3) 0.1404(2) 0.035 Uani 1 1 d . . . H17E H 0.2114 0.0264 0.1073 0.042 Uiso 1 1 calc R . . H17F H 0.1210 0.0160 0.1536 0.042 Uiso 1 1 calc R . . C17A C 1.1775(5) 0.3378(3) 0.1798(2) 0.036 Uani 1 1 d . . . H17C H 1.2422 0.3202 0.1627 0.044 Uiso 1 1 calc R . . H17D H 1.1483 0.3026 0.2055 0.044 Uiso 1 1 calc R . . C17B C 0.5916(5) 0.2225(3) -0.4592(3) 0.046 Uani 1 1 d . . . H17A H 0.5832 0.2033 -0.4204 0.055 Uiso 1 1 calc R . . H17B H 0.6529 0.1973 -0.4725 0.055 Uiso 1 1 calc R . . C18 C 0.1787(5) -0.0635(3) 0.1306(2) 0.038 Uani 1 1 d . . . H18E H 0.2308 -0.0728 0.1032 0.046 Uiso 1 1 calc R . . H18F H 0.1095 -0.0594 0.1203 0.046 Uiso 1 1 calc R . . C18A C 1.1969(5) 0.3802(3) 0.2070(3) 0.051 Uani 1 1 d . . . H18C H 1.2676 0.3668 0.2186 0.061 Uiso 1 1 calc R . . H18D H 1.1476 0.3800 0.2380 0.061 Uiso 1 1 calc R . . C18B C 0.4965(5) 0.2250(3) -0.4842(3) 0.049 Uani 1 1 d . . . H18A H 0.4339 0.2298 -0.4605 0.058 Uiso 1 1 calc R . . H18B H 0.5030 0.1868 -0.4935 0.058 Uiso 1 1 calc R . . C19 C 0.1985(5) -0.1142(3) 0.1856(3) 0.048 Uani 1 1 d . . . H19C H 0.1365 -0.1131 0.2103 0.057 Uiso 1 1 calc R . . H19D H 0.2217 -0.1569 0.1832 0.057 Uiso 1 1 calc R . . C19A C 1.1812(5) 0.4459(3) 0.1639(3) 0.045 Uani 1 1 d . . . H19E H 1.2434 0.4515 0.1396 0.054 Uiso 1 1 calc R . . H19F H 1.1623 0.4798 0.1795 0.054 Uiso 1 1 calc R . . C19B C 0.4952(5) 0.2844(3) -0.5344(3) 0.054 Uani 1 1 d . . . H19A H 0.5345 0.2731 -0.5646 0.065 Uiso 1 1 calc R . . H19B H 0.4240 0.3051 -0.5439 0.065 Uiso 1 1 calc R . . C20 C 0.2827(4) -0.0941(3) 0.2023(2) 0.038 Uani 1 1 d . . . H20E H 0.2812 -0.1081 0.2412 0.045 Uiso 1 1 calc R . . H20F H 0.3507 -0.1127 0.1888 0.045 Uiso 1 1 calc R . . C20A C 1.0917(4) 0.4442(3) 0.1356(2) 0.035 Uani 1 1 d . . . H20A H 1.0249 0.4589 0.1528 0.042 Uiso 1 1 calc R . . H20B H 1.0951 0.4715 0.0982 0.042 Uiso 1 1 calc R . . C20B C 0.5434(6) 0.3264(3) -0.5206(3) 0.064 Uani 1 1 d . . . H20C H 0.5896 0.3462 -0.5505 0.077 Uiso 1 1 calc R . . H20D H 0.4902 0.3601 -0.5124 0.077 Uiso 1 1 calc R . . C21 C 0.0920(5) -0.0025(4) 0.2860(3) 0.054 Uani 1 1 d . . . H21C H 0.0824 -0.0166 0.2572 0.064 Uiso 1 1 calc R . . H21D H 0.0735 0.0440 0.2740 0.064 Uiso 1 1 calc R . . C21A C 1.2499(4) 0.3977(3) 0.0283(2) 0.031 Uani 1 1 d . . . H21E H 1.2886 0.4033 0.0537 0.037 Uiso 1 1 calc R . . H21F H 1.1827 0.4274 0.0253 0.037 Uiso 1 1 calc R . . C21B C 0.7631(5) 0.4512(3) -0.5518(2) 0.060 Uani 1 1 d . . . H21A H 0.8239 0.4680 -0.5523 0.072 Uiso 1 1 calc R . . H21B H 0.7008 0.4791 -0.5424 0.072 Uiso 1 1 calc R . . C22 C 0.0262(5) -0.0302(4) 0.3349(3) 0.061 Uani 1 1 d . . . H22C H 0.0138 -0.0708 0.3360 0.074 Uiso 1 1 calc R . . H22D H -0.0406 -0.0010 0.3363 0.074 Uiso 1 1 calc R . . C22A C 1.3099(5) 0.4092(3) -0.0254(3) 0.054 Uani 1 1 d . . . H22E H 1.3656 0.4310 -0.0276 0.065 Uiso 1 1 calc R . . H22F H 1.2641 0.4352 -0.0540 0.065 Uiso 1 1 calc R . . C22B C 0.7559(5) 0.4452(3) -0.6057(3) 0.051 Uani 1 1 d . . . H22A H 0.6843 0.4471 -0.6113 0.061 Uiso 1 1 calc R . . H22B H 0.7824 0.4790 -0.6349 0.061 Uiso 1 1 calc R . . C23 C 0.0885(4) -0.0395(3) 0.3798(2) 0.041 Uani 1 1 d . . . H23C H 0.0716 -0.0740 0.4117 0.049 Uiso 1 1 calc R . . H23D H 0.0765 -0.0005 0.3885 0.049 Uiso 1 1 calc R . . C23A C 1.3551(5) 0.3426(3) -0.0298(2) 0.037 Uani 1 1 d . . . H23E H 1.3217 0.3361 -0.0567 0.045 Uiso 1 1 calc R . . H23F H 1.4300 0.3366 -0.0389 0.045 Uiso 1 1 calc R . . C23B C 0.8214(6) 0.3824(3) -0.6018(3) 0.065 Uani 1 1 d . . . H23A H 0.8878 0.3870 -0.6225 0.078 Uiso 1 1 calc R . . H23B H 0.7869 0.3590 -0.6154 0.078 Uiso 1 1 calc R . . C24 C 0.1999(4) -0.0565(3) 0.3577(2) 0.030 Uani 1 1 d . . . H24C H 0.2466 -0.0413 0.3726 0.036 Uiso 1 1 calc R . . H24D H 0.2226 -0.1026 0.3665 0.036 Uiso 1 1 calc R . . C24A C 1.3306(4) 0.2974(3) 0.0260(2) 0.033 Uani 1 1 d . . . H24E H 1.3197 0.2577 0.0244 0.040 Uiso 1 1 calc R . . H24F H 1.3871 0.2875 0.0489 0.040 Uiso 1 1 calc R . . C24B C 0.8383(6) 0.3473(3) -0.5421(3) 0.060 Uani 1 1 d . . . H24A H 0.8200 0.3055 -0.5303 0.073 Uiso 1 1 calc R . . H24B H 0.9109 0.3413 -0.5354 0.073 Uiso 1 1 calc R . . C25 C 0.7358(4) 0.0280(3) 0.2557(2) 0.024 Uani 1 1 d . . . C25A C 0.6673(4) 0.3078(2) 0.08671(19) 0.018 Uani 1 1 d . . . C25B C 0.6949(4) 0.3768(2) -0.2496(2) 0.020 Uani 1 1 d . . . C26 C 0.8271(4) -0.0171(3) 0.2510(2) 0.024 Uani 1 1 d . . . H26 H 0.8452 -0.0547 0.2798 0.028 Uiso 1 1 calc R . . C26A C 0.7110(4) 0.2709(2) 0.1355(2) 0.026 Uani 1 1 d . . . H26A H 0.7828 0.2547 0.1363 0.031 Uiso 1 1 calc R . . C26B C 0.7807(4) 0.3326(2) -0.2226(2) 0.024 Uani 1 1 d . . . H26B H 0.8484 0.3366 -0.2370 0.029 Uiso 1 1 calc R . . C27 C 0.8913(4) -0.0055(3) 0.2030(2) 0.028 Uani 1 1 d . . . H27 H 0.9517 -0.0357 0.2001 0.033 Uiso 1 1 calc R . . C27A C 0.6472(4) 0.2583(2) 0.1830(2) 0.030 Uani 1 1 d . . . H27A H 0.6766 0.2329 0.2154 0.036 Uiso 1 1 calc R . . C27B C 0.7662(4) 0.2832(2) -0.1750(2) 0.023 Uani 1 1 d . . . H27B H 0.8239 0.2542 -0.1581 0.027 Uiso 1 1 calc R . . C28 C 0.8655(4) 0.0509(3) 0.1594(2) 0.029 Uani 1 1 d . . . H28 H 0.9077 0.0578 0.1274 0.035 Uiso 1 1 calc R . . C28A C 0.5400(4) 0.2832(3) 0.1828(2) 0.029 Uani 1 1 d . . . H28A H 0.4983 0.2754 0.2150 0.035 Uiso 1 1 calc R . . C28B C 0.6659(4) 0.2768(2) -0.1526(2) 0.025 Uani 1 1 d . . . H28B H 0.6560 0.2435 -0.1208 0.030 Uiso 1 1 calc R . . C29 C 0.7767(4) 0.0963(3) 0.1643(2) 0.030 Uani 1 1 d . . . H29 H 0.7594 0.1344 0.1358 0.036 Uiso 1 1 calc R . . C29A C 0.4957(4) 0.3197(3) 0.1345(2) 0.027 Uani 1 1 d . . . H29A H 0.4238 0.3355 0.1338 0.033 Uiso 1 1 calc R . . C29B C 0.5809(4) 0.3208(3) -0.1780(2) 0.028 Uani 1 1 d . . . H29B H 0.5134 0.3170 -0.1631 0.034 Uiso 1 1 calc R . . C30 C 0.7141(4) 0.0845(3) 0.2118(2) 0.025 Uani 1 1 d . . . H30 H 0.6550 0.1155 0.2147 0.030 Uiso 1 1 calc R . . C30A C 0.5598(4) 0.3323(2) 0.0871(2) 0.024 Uani 1 1 d . . . H30A H 0.5302 0.3577 0.0548 0.029 Uiso 1 1 calc R . . C30B C 0.5951(4) 0.3703(3) -0.2255(2) 0.026 Uani 1 1 d . . . H30B H 0.5370 0.3998 -0.2417 0.031 Uiso 1 1 calc R . . C31 C 0.7179(4) -0.0517(3) 0.3673(2) 0.024 Uani 1 1 d . . . C31A C 0.6724(3) 0.3869(2) -0.02479(19) 0.015 Uani 1 1 d . . . C31B C 0.6303(4) 0.5103(2) -0.2960(2) 0.024 Uani 1 1 d . . . C32 C 0.7590(4) -0.0383(3) 0.4054(2) 0.031 Uani 1 1 d . . . H32 H 0.7422 0.0033 0.4066 0.037 Uiso 1 1 calc R . . C32A C 0.6428(4) 0.4474(2) -0.0189(2) 0.022 Uani 1 1 d . . . H32A H 0.6648 0.4539 0.0098 0.027 Uiso 1 1 calc R . . C32B C 0.6393(4) 0.5211(3) -0.2490(2) 0.027 Uani 1 1 d . . . H32B H 0.6875 0.4924 -0.2249 0.032 Uiso 1 1 calc R . . C33 C 0.8249(4) -0.0858(3) 0.4420(2) 0.035 Uani 1 1 d . . . H33 H 0.8536 -0.0760 0.4669 0.042 Uiso 1 1 calc R . . C33A C 0.5810(4) 0.4977(3) -0.0556(2) 0.029 Uani 1 1 d . . . H33A H 0.5600 0.5374 -0.0507 0.035 Uiso 1 1 calc R . . C33B C 0.5773(4) 0.5741(3) -0.2376(2) 0.032 Uani 1 1 d . . . H33B H 0.5836 0.5812 -0.2061 0.038 Uiso 1 1 calc R . . C34 C 0.8477(5) -0.1478(3) 0.4413(2) 0.040 Uani 1 1 d . . . H34 H 0.8925 -0.1798 0.4655 0.048 Uiso 1 1 calc R . . C34A C 0.5502(4) 0.4894(3) -0.0994(2) 0.033 Uani 1 1 d . . . H34A H 0.5074 0.5230 -0.1235 0.040 Uiso 1 1 calc R . . C34B C 0.5053(5) 0.6165(3) -0.2741(2) 0.039 Uani 1 1 d . . . H34B H 0.4635 0.6524 -0.2671 0.047 Uiso 1 1 calc R . . C35 C 0.8039(4) -0.1625(3) 0.4046(2) 0.035 Uani 1 1 d . . . H35 H 0.8181 -0.2044 0.4044 0.042 Uiso 1 1 calc R . . C35A C 0.5839(4) 0.4303(3) -0.1068(2) 0.029 Uani 1 1 d . . . H35A H 0.5657 0.4250 -0.1369 0.035 Uiso 1 1 calc R . . C35B C 0.4958(5) 0.6057(3) -0.3202(2) 0.044 Uani 1 1 d . . . H35B H 0.4465 0.6339 -0.3438 0.052 Uiso 1 1 calc R . . C36 C 0.7387(4) -0.1141(3) 0.3682(2) 0.033 Uani 1 1 d . . . H36 H 0.7084 -0.1241 0.3439 0.040 Uiso 1 1 calc R . . C36A C 0.6445(4) 0.3790(2) -0.0701(2) 0.020 Uani 1 1 d . . . H36A H 0.6664 0.3396 -0.0755 0.024 Uiso 1 1 calc R . . C36B C 0.5586(4) 0.5535(3) -0.3319(2) 0.034 Uani 1 1 d . . . H36B H 0.5528 0.5474 -0.3638 0.041 Uiso 1 1 calc R . . C37 C 0.3755(4) 0.0438(2) 0.4076(2) 0.019 Uani 1 1 d . . . C37A C 1.0361(4) 0.1495(2) -0.0383(2) 0.018 Uani 1 1 d . . . C37B C 1.0480(4) 0.2935(2) -0.29821(19) 0.020 Uani 1 1 d . . . C38 C 0.4516(4) -0.0015(2) 0.4405(2) 0.024 Uani 1 1 d . . . H38 H 0.5214 0.0015 0.4319 0.029 Uiso 1 1 calc R . . C38A C 1.0457(4) 0.1528(3) -0.0918(2) 0.023 Uani 1 1 d . . . H38A H 1.0228 0.1919 -0.1183 0.028 Uiso 1 1 calc R . . C38B C 1.0874(4) 0.2308(3) -0.2977(2) 0.031 Uani 1 1 d . . . H38B H 1.0670 0.2175 -0.3230 0.037 Uiso 1 1 calc R . . C39 C 0.4257(4) -0.0508(3) 0.4855(2) 0.027 Uani 1 1 d . . . H39 H 0.4776 -0.0802 0.5069 0.032 Uiso 1 1 calc R . . C39A C 1.0882(4) 0.0994(3) -0.1064(2) 0.028 Uani 1 1 d . . . H39A H 1.0937 0.1024 -0.1423 0.033 Uiso 1 1 calc R . . C39B C 1.1555(4) 0.1886(3) -0.2610(2) 0.036 Uani 1 1 d . . . H39B H 1.1825 0.1473 -0.2620 0.043 Uiso 1 1 calc R . . C40 C 0.3224(4) -0.0559(3) 0.4985(2) 0.031 Uani 1 1 d . . . H40 H 0.3047 -0.0891 0.5285 0.037 Uiso 1 1 calc R . . C40A C 1.1228(4) 0.0410(3) -0.0672(2) 0.030 Uani 1 1 d . . . H40A H 1.1525 0.0049 -0.0770 0.037 Uiso 1 1 calc R . . C40B C 1.1843(4) 0.2072(3) -0.2224(2) 0.029 Uani 1 1 d . . . H40B H 1.2313 0.1786 -0.1976 0.035 Uiso 1 1 calc R . . C41 C 0.2459(4) -0.0123(3) 0.4671(2) 0.029 Uani 1 1 d . . . H41 H 0.1764 -0.0161 0.4760 0.034 Uiso 1 1 calc R . . C41A C 1.1132(4) 0.0363(3) -0.0136(2) 0.027 Uani 1 1 d . . . H41A H 1.1354 -0.0033 0.0125 0.032 Uiso 1 1 calc R . . C41B C 1.1429(4) 0.2686(3) -0.2205(2) 0.029 Uani 1 1 d . . . H41B H 1.1602 0.2809 -0.1938 0.035 Uiso 1 1 calc R . . C42 C 0.2715(4) 0.0378(2) 0.4219(2) 0.026 Uani 1 1 d . . . H42 H 0.2188 0.0674 0.4012 0.031 Uiso 1 1 calc R . . C42A C 1.0713(4) 0.0895(2) 0.0012(2) 0.023 Uani 1 1 d . . . H42A H 1.0661 0.0860 0.0372 0.028 Uiso 1 1 calc R . . C42B C 1.0757(4) 0.3115(3) -0.2586(2) 0.023 Uani 1 1 d . . . H42B H 1.0487 0.3528 -0.2578 0.027 Uiso 1 1 calc R . . C43 C 0.3371(4) 0.1786(2) 0.3733(2) 0.020 Uani 1 1 d . . . C43A C 1.0083(4) 0.2848(2) -0.0730(2) 0.020 Uani 1 1 d . . . C43B C 1.0452(4) 0.3683(2) -0.4121(2) 0.023 Uani 1 1 d . . . C44 C 0.3282(4) 0.1741(3) 0.4266(2) 0.023 Uani 1 1 d . . . H44 H 0.3555 0.1355 0.4525 0.028 Uiso 1 1 calc R . . C44A C 0.9334(4) 0.3240(2) -0.1091(2) 0.024 Uani 1 1 d . . . H44A H 0.8672 0.3148 -0.1044 0.028 Uiso 1 1 calc R . . C44B C 1.0012(4) 0.4111(3) -0.4589(2) 0.033 Uani 1 1 d . . . H44B H 0.9308 0.4308 -0.4576 0.040 Uiso 1 1 calc R . . C45 C 0.2782(4) 0.2272(3) 0.4421(2) 0.033 Uani 1 1 d . . . H45 H 0.2723 0.2238 0.4781 0.039 Uiso 1 1 calc R . . C45A C 0.9564(4) 0.3765(3) -0.1521(2) 0.029 Uani 1 1 d . . . H45A H 0.9062 0.4016 -0.1763 0.035 Uiso 1 1 calc R . . C45B C 1.0605(5) 0.4250(3) -0.5078(2) 0.039 Uani 1 1 d . . . H45B H 1.0294 0.4530 -0.5391 0.047 Uiso 1 1 calc R . . C46 C 0.2378(5) 0.2847(3) 0.4039(2) 0.034 Uani 1 1 d . . . H46 H 0.2039 0.3200 0.4140 0.040 Uiso 1 1 calc R . . C46A C 1.0528(4) 0.3914(3) -0.1588(2) 0.032 Uani 1 1 d . . . H46A H 1.0673 0.4274 -0.1870 0.038 Uiso 1 1 calc R . . C46B C 1.1646(4) 0.3975(3) -0.5098(2) 0.033 Uani 1 1 d . . . H46B H 1.2044 0.4068 -0.5425 0.040 Uiso 1 1 calc R . . C47 C 0.2485(5) 0.2892(3) 0.3499(2) 0.037 Uani 1 1 d . . . H47 H 0.2227 0.3280 0.3238 0.045 Uiso 1 1 calc R . . C47A C 1.1288(4) 0.3528(3) -0.1237(2) 0.032 Uani 1 1 d . . . H47A H 1.1945 0.3628 -0.1286 0.038 Uiso 1 1 calc R . . C47B C 1.2110(5) 0.3562(3) -0.4638(2) 0.042 Uani 1 1 d . . . H47B H 1.2822 0.3383 -0.4652 0.051 Uiso 1 1 calc R . . C48 C 0.2971(4) 0.2364(3) 0.3352(2) 0.029 Uani 1 1 d . . . H48 H 0.3030 0.2398 0.2991 0.034 Uiso 1 1 calc R . . C48A C 1.1078(4) 0.3001(3) -0.0819(2) 0.025 Uani 1 1 d . . . H48A H 1.1600 0.2740 -0.0592 0.030 Uiso 1 1 calc R . . C48B C 1.1506(4) 0.3411(3) -0.4145(2) 0.034 Uani 1 1 d . . . H48B H 1.1818 0.3128 -0.3834 0.041 Uiso 1 1 calc R . . C49 C 0.0512(5) -0.1003(3) 0.5618(3) 0.056 Uani 1 1 d . . . H49E H 0.0943 -0.0799 0.5738 0.068 Uiso 1 1 calc R . . H49F H 0.0179 -0.0694 0.5300 0.068 Uiso 1 1 calc R . . C49A C 0.4216(5) 0.2140(3) -0.0874(3) 0.051 Uani 1 1 d . . . H49A H 0.4696 0.2273 -0.0716 0.061 Uiso 1 1 calc R . . H49B H 0.3833 0.2519 -0.1132 0.061 Uiso 1 1 calc R . . C49B C 0.7105(5) 0.5471(3) -0.7463(3) 0.052 Uani 1 1 d . . . H49C H 0.6582 0.5410 -0.7161 0.062 Uiso 1 1 calc R . . H49D H 0.7608 0.5675 -0.7397 0.062 Uiso 1 1 calc R . . C50 C 0.1170(5) -0.1590(4) 0.5495(3) 0.069 Uani 1 1 d . . . H50E H 0.1785 -0.1770 0.5700 0.083 Uiso 1 1 calc R . . H50F H 0.1387 -0.1486 0.5114 0.083 Uiso 1 1 calc R . . C50A C 0.4803(5) 0.1679(3) -0.1143(3) 0.058 Uani 1 1 d . . . H50C H 0.4955 0.1897 -0.1524 0.069 Uiso 1 1 calc R . . H50D H 0.5454 0.1443 -0.0978 0.069 Uiso 1 1 calc R . . C50B C 0.7652(5) 0.4827(3) -0.7515(3) 0.054 Uani 1 1 d . . . H50A H 0.7375 0.4480 -0.7240 0.065 Uiso 1 1 calc R . . H50B H 0.8400 0.4750 -0.7489 0.065 Uiso 1 1 calc R . . C51 C 0.0417(5) -0.2050(4) 0.5668(3) 0.070 Uani 1 1 d . . . H51C H 0.0262 -0.2134 0.5360 0.084 Uiso 1 1 calc R . . H51D H 0.0723 -0.2455 0.5930 0.084 Uiso 1 1 calc R . . C51A C 0.4074(6) 0.1249(4) -0.1060(3) 0.077 Uani 1 1 d . . . H51E H 0.3790 0.1324 -0.1396 0.093 Uiso 1 1 calc R . . H51F H 0.4435 0.0803 -0.0923 0.093 Uiso 1 1 calc R . . C51B C 0.7408(5) 0.4895(3) -0.8071(3) 0.058 Uani 1 1 d . . . H51A H 0.7270 0.4499 -0.8077 0.070 Uiso 1 1 calc R . . H51B H 0.7978 0.5014 -0.8336 0.070 Uiso 1 1 calc R . . C52 C -0.0549(5) -0.1731(3) 0.5909(3) 0.053 Uani 1 1 d . . . H52C H -0.1093 -0.1549 0.5658 0.064 Uiso 1 1 calc R . . H52D H -0.0805 -0.2034 0.6235 0.064 Uiso 1 1 calc R . . C52A C 0.3240(6) 0.1393(4) -0.0671(4) 0.080 Uani 1 1 d . . . H52E H 0.2584 0.1584 -0.0842 0.096 Uiso 1 1 calc R . . H52F H 0.3156 0.1002 -0.0377 0.096 Uiso 1 1 calc R . . C52B C 0.6435(5) 0.5427(3) -0.8173(3) 0.044 Uani 1 1 d . . . H52A H 0.6349 0.5634 -0.8556 0.053 Uiso 1 1 calc R . . H52B H 0.5815 0.5261 -0.7999 0.053 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.020 0.020 0.020 -0.007 -0.002 -0.006 Pt1A 0.017 0.015 0.018 -0.007 -0.002 -0.004 Pt1B 0.024 0.019 0.020 -0.006 -0.002 -0.007 Ba1 0.022 0.020 0.020 -0.008 -0.001 -0.006 Ba2 0.020 0.016 0.018 -0.006 -0.003 -0.005 Ba3 0.025 0.024 0.021 -0.009 -0.004 -0.006 P1 0.018 0.019 0.020 -0.006 -0.002 -0.004 P1A 0.017 0.014 0.017 -0.006 -0.002 -0.004 P1B 0.023 0.018 0.018 -0.007 -0.003 -0.004 P2 0.019 0.018 0.018 -0.008 -0.002 -0.005 P2A 0.018 0.017 0.018 -0.007 -0.002 -0.004 P2B 0.023 0.018 0.017 -0.006 0.000 -0.005 O1 0.036 0.043 0.029 -0.012 0.005 -0.017 O1A 0.041 0.031 0.024 -0.009 0.004 -0.002 O1B 0.023 0.038 0.030 -0.012 0.000 -0.010 O2 0.036 0.025 0.032 -0.010 -0.005 -0.012 O2A 0.040 0.027 0.036 -0.014 -0.013 -0.009 O2B 0.049 0.045 0.032 -0.014 -0.015 -0.019 O3 0.026 0.046 0.031 -0.007 0.002 -0.014 O3A 0.027 0.030 0.048 -0.016 0.008 -0.010 O3B 0.048 0.041 0.027 -0.006 0.007 -0.006 O4 0.042 0.050 0.061 -0.020 0.001 -0.009 O4A 0.056 0.064 0.048 -0.027 0.013 -0.024 O4B 0.045 0.039 0.037 -0.014 -0.002 -0.007 C1 0.023 0.024 0.021 -0.007 0.002 -0.006 C1A 0.021 0.017 0.020 -0.006 0.000 -0.006 C1B 0.031 0.026 0.025 -0.011 -0.005 -0.002 C2 0.026 0.027 0.025 -0.013 0.006 -0.008 C2A 0.036 0.017 0.017 -0.004 -0.007 -0.006 C2B 0.029 0.028 0.031 -0.015 -0.009 -0.003 C3 0.030 0.017 0.025 -0.006 0.000 -0.009 C3A 0.024 0.019 0.029 -0.008 -0.008 0.000 C3B 0.035 0.032 0.026 -0.007 -0.013 -0.004 C4 0.025 0.023 0.015 -0.005 0.001 -0.006 C4A 0.019 0.018 0.020 -0.010 0.001 -0.002 C4B 0.032 0.023 0.021 -0.003 -0.005 -0.007 C5 0.021 0.018 0.023 -0.009 0.001 -0.005 C5A 0.026 0.015 0.017 -0.009 -0.003 -0.004 C5B 0.030 0.017 0.017 -0.009 -0.009 -0.002 C6 0.018 0.024 0.020 -0.012 -0.002 -0.005 C6A 0.020 0.015 0.020 -0.005 -0.008 -0.001 C6B 0.025 0.014 0.020 -0.007 -0.003 0.002 C7 0.022 0.024 0.021 -0.010 -0.002 0.000 C7A 0.026 0.017 0.021 -0.007 -0.005 -0.005 C7B 0.026 0.020 0.024 -0.008 -0.002 0.000 C8 0.034 0.024 0.030 -0.011 -0.009 0.001 C8A 0.024 0.017 0.022 -0.005 -0.006 -0.004 C8B 0.027 0.029 0.027 -0.011 -0.002 -0.006 C9 0.031 0.022 0.026 -0.009 -0.005 -0.001 C9A 0.031 0.020 0.027 -0.013 -0.009 -0.003 C9B 0.042 0.028 0.025 -0.013 -0.007 -0.010 C10 0.027 0.018 0.028 -0.010 0.000 -0.007 C10A 0.022 0.017 0.022 -0.006 -0.006 0.003 C10B 0.033 0.025 0.017 -0.007 0.001 -0.011 C11 0.040 0.027 0.040 -0.016 -0.003 -0.014 C11A 0.029 0.020 0.030 -0.015 -0.003 -0.009 C11B 0.031 0.028 0.034 -0.005 -0.001 -0.020 C12 0.027 0.038 0.029 -0.007 -0.006 -0.014 C12A 0.020 0.026 0.030 -0.013 -0.003 -0.011 C12B 0.039 0.025 0.053 -0.013 -0.004 -0.010 C13 0.033 0.035 0.035 -0.009 -0.001 -0.013 C13A 0.039 0.033 0.026 -0.002 0.003 -0.010 C13B 0.030 0.027 0.034 -0.009 -0.005 -0.009 C14 0.039 0.037 0.044 -0.006 0.006 -0.006 C14A 0.166 0.067 0.040 -0.030 0.009 -0.051 C14B 0.036 0.045 0.033 -0.012 -0.002 -0.014 C15 0.052 0.054 0.037 -0.020 0.011 -0.011 C15A 0.141 0.071 0.051 -0.029 0.009 -0.025 C15B 0.036 0.038 0.037 -0.015 -0.003 -0.004 C16 0.049 0.058 0.035 -0.023 0.002 -0.013 C16A 0.070 0.039 0.031 -0.016 0.017 -0.003 C16B 0.035 0.039 0.036 -0.016 -0.006 -0.011 C17 0.037 0.038 0.030 -0.008 -0.014 -0.005 C17A 0.042 0.029 0.037 -0.004 -0.017 -0.008 C17B 0.050 0.047 0.051 -0.025 -0.006 -0.012 C18 0.044 0.040 0.044 -0.024 -0.011 -0.010 C18A 0.069 0.053 0.041 -0.017 -0.031 -0.010 C18B 0.055 0.042 0.058 -0.018 -0.018 -0.016 C19 0.054 0.037 0.057 -0.011 -0.016 -0.018 C19A 0.054 0.037 0.050 -0.014 -0.011 -0.019 C19B 0.063 0.065 0.051 -0.024 -0.013 -0.031 C20 0.040 0.035 0.035 -0.005 -0.010 -0.008 C20A 0.038 0.025 0.040 -0.009 -0.008 -0.002 C20B 0.087 0.064 0.042 0.003 -0.032 -0.034 C21 0.034 0.082 0.039 -0.008 -0.009 -0.015 C21A 0.034 0.028 0.034 -0.014 0.003 -0.009 C21B 0.051 0.056 0.036 0.008 0.004 0.014 C22 0.043 0.087 0.047 -0.019 0.001 -0.011 C22A 0.067 0.047 0.041 -0.015 0.016 -0.011 C22B 0.036 0.065 0.040 0.004 -0.009 -0.021 C23 0.030 0.050 0.039 -0.015 0.001 -0.003 C23A 0.034 0.041 0.040 -0.021 -0.001 -0.002 C23B 0.103 0.057 0.032 -0.015 0.007 -0.020 C24 0.032 0.034 0.028 -0.012 -0.002 -0.011 C24A 0.021 0.030 0.051 -0.017 -0.001 -0.007 C24B 0.080 0.056 0.034 -0.019 -0.004 0.011 C25 0.019 0.030 0.023 -0.008 0.000 -0.010 C25A 0.024 0.017 0.014 -0.006 0.000 -0.005 C25B 0.026 0.016 0.020 -0.009 -0.005 -0.002 C26 0.022 0.026 0.025 -0.010 -0.003 -0.005 C26A 0.024 0.027 0.026 -0.008 -0.004 -0.004 C26B 0.027 0.025 0.025 -0.009 -0.007 -0.005 C27 0.025 0.029 0.031 -0.015 0.006 -0.008 C27A 0.043 0.018 0.025 -0.006 -0.004 0.001 C27B 0.031 0.021 0.018 -0.008 -0.004 -0.006 C28 0.028 0.033 0.029 -0.014 0.014 -0.018 C28A 0.041 0.024 0.024 -0.009 0.008 -0.014 C28B 0.036 0.018 0.022 -0.004 -0.002 -0.011 C29 0.031 0.031 0.027 -0.006 0.003 -0.012 C29A 0.024 0.032 0.026 -0.010 0.004 -0.010 C29B 0.032 0.030 0.025 -0.008 0.001 -0.012 C30 0.023 0.025 0.026 -0.006 -0.001 -0.008 C30A 0.024 0.022 0.025 -0.009 0.000 -0.002 C30B 0.029 0.026 0.025 -0.013 -0.002 -0.004 C31 0.022 0.024 0.023 -0.006 0.002 -0.003 C31A 0.014 0.021 0.011 -0.004 -0.001 -0.005 C31B 0.027 0.019 0.024 -0.007 0.002 -0.003 C32 0.028 0.032 0.029 -0.008 -0.003 -0.003 C32A 0.024 0.022 0.023 -0.008 -0.002 -0.007 C32B 0.031 0.030 0.022 -0.011 0.000 -0.008 C33 0.034 0.046 0.025 -0.011 -0.009 -0.004 C33A 0.033 0.024 0.025 -0.007 0.004 -0.001 C33B 0.040 0.034 0.026 -0.014 -0.004 -0.009 C34 0.041 0.042 0.025 -0.005 0.007 -0.003 C34A 0.027 0.032 0.030 0.004 -0.004 -0.007 C34B 0.048 0.032 0.037 -0.019 -0.002 0.004 C35 0.040 0.029 0.031 -0.012 -0.001 0.003 C35A 0.025 0.032 0.024 -0.004 -0.010 0.001 C35B 0.053 0.034 0.037 -0.012 -0.012 0.010 C36 0.042 0.033 0.026 -0.009 -0.003 -0.011 C36A 0.020 0.024 0.018 -0.008 -0.004 -0.004 C36B 0.039 0.038 0.025 -0.016 -0.010 0.004 C37 0.019 0.018 0.023 -0.007 -0.002 -0.010 C37A 0.019 0.016 0.020 -0.008 0.000 -0.004 C37B 0.025 0.023 0.012 -0.007 0.005 -0.004 C38 0.029 0.023 0.021 -0.010 -0.005 0.000 C38A 0.028 0.028 0.015 -0.011 -0.005 -0.004 C38B 0.041 0.028 0.023 -0.008 -0.009 -0.004 C39 0.029 0.023 0.029 -0.007 -0.008 -0.006 C39A 0.028 0.031 0.029 -0.018 0.003 -0.004 C39B 0.035 0.027 0.036 -0.006 -0.002 0.005 C40 0.039 0.037 0.021 -0.012 0.000 -0.013 C40A 0.041 0.021 0.034 -0.018 0.004 -0.007 C40B 0.027 0.030 0.020 0.002 -0.006 0.000 C41 0.025 0.032 0.028 -0.006 0.003 -0.013 C41A 0.031 0.020 0.029 -0.009 -0.006 0.000 C41B 0.030 0.038 0.018 -0.009 -0.007 -0.005 C42 0.026 0.023 0.026 -0.007 -0.003 -0.002 C42A 0.026 0.025 0.020 -0.010 -0.006 -0.001 C42B 0.023 0.025 0.018 -0.007 -0.003 0.000 C43 0.020 0.022 0.020 -0.009 -0.002 -0.004 C43A 0.020 0.017 0.025 -0.008 -0.004 -0.003 C43B 0.022 0.021 0.026 -0.007 -0.003 -0.005 C44 0.025 0.024 0.023 -0.009 -0.007 -0.004 C44A 0.027 0.025 0.021 -0.007 -0.003 -0.009 C44B 0.034 0.034 0.027 -0.009 -0.003 -0.001 C45 0.036 0.035 0.026 -0.013 -0.003 -0.003 C45A 0.033 0.028 0.029 -0.009 -0.002 -0.011 C45B 0.047 0.041 0.025 -0.007 -0.002 -0.009 C46 0.055 0.020 0.034 -0.016 0.001 -0.013 C46A 0.044 0.029 0.023 -0.005 0.003 -0.017 C46B 0.043 0.030 0.027 -0.008 0.011 -0.019 C47 0.054 0.023 0.031 -0.012 -0.010 0.006 C47A 0.030 0.035 0.035 -0.011 -0.001 -0.019 C47B 0.035 0.054 0.036 -0.016 0.009 -0.011 C48 0.043 0.029 0.017 -0.013 -0.001 -0.007 C48A 0.023 0.027 0.024 -0.005 -0.004 -0.009 C48B 0.034 0.044 0.023 -0.011 0.002 -0.007 C49 0.041 0.057 0.060 -0.010 -0.007 -0.004 C49A 0.059 0.049 0.054 -0.023 0.010 -0.030 C49B 0.048 0.061 0.040 -0.012 -0.021 0.002 C50 0.046 0.080 0.051 0.000 0.010 -0.001 C50A 0.058 0.052 0.065 -0.032 0.023 -0.012 C50B 0.055 0.048 0.050 -0.005 -0.019 -0.002 C51 0.060 0.075 0.076 -0.037 -0.014 0.006 C51A 0.094 0.073 0.075 -0.042 0.019 -0.024 C51B 0.066 0.047 0.054 -0.021 -0.008 0.010 C52 0.049 0.045 0.076 -0.031 -0.008 -0.009 C52A 0.067 0.086 0.110 -0.055 0.013 -0.037 C52B 0.039 0.057 0.035 -0.017 -0.007 -0.002 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 C11 2.079(5) . ? Pt1 C12 2.087(5) . ? Pt1 P2 2.2892(13) . ? Pt1 P1 2.3062(14) . ? Pt1A C11A 2.081(5) . ? Pt1A C12A 2.091(5) . ? Pt1A P2A 2.2967(13) . ? Pt1A P1A 2.3026(13) . ? Pt1B C12B 2.073(5) . ? Pt1B C11B 2.093(5) . ? Pt1B P1B 2.2922(14) . ? Pt1B P2B 2.3116(14) . ? Ba1 O1 2.745(4) . ? Ba1 O3 2.752(4) . ? Ba1 O2 2.845(4) . ? Ba1 C3 3.024(5) . ? Ba1 C9 3.033(5) . ? Ba1 C2 3.035(5) . ? Ba1 C10 3.037(5) . ? Ba1 C8 3.039(5) . ? Ba1 C4 3.047(5) . ? Ba1 C6 3.052(5) . ? Ba1 C7 3.056(5) . ? Ba1 C1 3.083(5) . ? Ba2 O3A 2.765(4) . ? Ba2 O1A 2.791(4) . ? Ba2 O2A 2.805(4) . ? Ba2 C7A 3.001(5) . ? Ba2 C8A 3.006(5) . ? Ba2 C1A 3.018(5) . ? Ba2 C6A 3.033(5) . ? Ba2 C2A 3.039(5) . ? Ba2 C9A 3.041(5) . ? Ba2 C10A 3.045(5) . ? Ba2 C5A 3.058(5) . ? Ba2 C3A 3.064(5) . ? Ba3 O3B 2.740(4) . ? Ba3 O2B 2.768(4) . ? Ba3 O1B 2.773(3) . ? Ba3 C9B 2.990(5) . ? Ba3 C10B 2.995(5) . ? Ba3 C5B 3.004(5) . ? Ba3 C1B 3.011(5) . ? Ba3 C4B 3.015(5) . ? Ba3 C2B 3.029(5) . ? Ba3 C6B 3.031(5) . ? Ba3 C8B 3.040(5) . ? Ba3 C3B 3.050(5) . ? P1 C5 1.798(5) . ? P1 C25 1.841(5) . ? P1 C31 1.851(5) . ? P1A C6A 1.802(5) . ? P1A C31A 1.839(5) . ? P1A C25A 1.840(5) . ? P1B C5B 1.788(5) . ? P1B C25B 1.832(5) . ? P1B C31B 1.846(5) . ? P2 C6 1.777(5) . ? P2 C37 1.828(5) . ? P2 C43 1.847(5) . ? P2A C5A 1.779(5) . ? P2A C43A 1.829(5) . ? P2A C37A 1.838(5) . ? P2B C6B 1.798(5) . ? P2B C43B 1.842(5) . ? P2B C37B 1.850(5) . ? O1 C13 1.443(6) . ? O1 C16 1.457(7) . ? O1A C16A 1.428(6) . ? O1A C13A 1.449(6) . ? O1B C16B 1.437(6) . ? O1B C13B 1.460(6) . ? O2 C17 1.438(6) . ? O2 C20 1.443(6) . ? O2A C20A 1.443(6) . ? O2A C17A 1.448(6) . ? O2B C17B 1.440(7) . ? O2B C20B 1.444(7) . ? O3 C24 1.435(6) . ? O3 C21 1.445(6) . ? O3A C24A 1.445(6) . ? O3A C21A 1.450(6) . ? O3B C24B 1.410(7) . ? O3B C21B 1.430(7) . ? O4 C49 1.411(7) . ? O4 C52 1.448(7) . ? O4A C49A 1.402(7) . ? O4A C52A 1.437(8) . ? O4B C49B 1.414(7) . ? O4B C52B 1.429(7) . ? C1 C2 1.394(7) . ? C1 C5 1.432(7) . ? C1A C2A 1.399(7) . ? C1A C5A 1.415(7) . ? C1B C2B 1.385(7) . ? C1B C5B 1.402(7) . ? C2 C3 1.419(7) . ? C2A C3A 1.419(7) . ? C2B C3B 1.411(7) . ? C3 C4 1.405(7) . ? C3A C4A 1.406(7) . ? C3B C4B 1.402(7) . ? C4 C5 1.421(7) . ? C4A C5A 1.421(7) . ? C4B C5B 1.416(7) . ? C6 C10 1.423(7) . ? C6 C7 1.433(7) . ? C6A C10A 1.409(7) . ? C6A C7A 1.412(7) . ? C6B C7B 1.417(7) . ? C6B C10B 1.433(7) . ? C7 C8 1.385(7) . ? C7A C8A 1.392(7) . ? C7B C8B 1.403(7) . ? C8 C9 1.427(7) . ? C8A C9A 1.400(7) . ? C8B C9B 1.409(7) . ? C9 C10 1.396(7) . ? C9A C10A 1.404(7) . ? C9B C10B 1.398(7) . ? C13 C14 1.501(7) . ? C13A C14A 1.486(8) . ? C13B C14B 1.530(7) . ? C14 C15 1.510(8) . ? C14A C15A 1.439(9) . ? C14B C15B 1.537(8) . ? C15 C16 1.544(8) . ? C15A C16A 1.463(9) . ? C15B C16B 1.521(7) . ? C17 C18 1.504(8) . ? C17A C18A 1.491(8) . ? C17B C18B 1.493(8) . ? C18 C19 1.519(8) . ? C18A C19A 1.513(8) . ? C18B C19B 1.524(8) . ? C19 C20 1.484(8) . ? C19A C20A 1.515(8) . ? C19B C20B 1.448(9) . ? C21 C22 1.479(8) . ? C21A C22A 1.494(7) . ? C21B C22B 1.512(9) . ? C22 C23 1.482(8) . ? C22A C23A 1.530(8) . ? C22B C23B 1.456(9) . ? C23 C24 1.510(7) . ? C23A C24A 1.515(7) . ? C23B C24B 1.528(8) . ? C25 C30 1.395(7) . ? C25 C26 1.401(7) . ? C25A C30A 1.392(6) . ? C25A C26A 1.393(7) . ? C25B C30B 1.393(7) . ? C25B C26B 1.409(7) . ? C26 C27 1.401(7) . ? C26A C27A 1.390(7) . ? C26B C27B 1.386(7) . ? C27 C28 1.396(7) . ? C27A C28A 1.390(7) . ? C27B C28B 1.388(7) . ? C28 C29 1.385(7) . ? C28A C29A 1.385(7) . ? C28B C29B 1.385(7) . ? C29 C30 1.381(7) . ? C29A C30A 1.390(7) . ? C29B C30B 1.386(7) . ? C31 C36 1.375(7) . ? C31 C32 1.379(7) . ? C31A C36A 1.399(7) . ? C31A C32A 1.400(7) . ? C31B C36B 1.389(7) . ? C31B C32B 1.391(7) . ? C32 C33 1.386(7) . ? C32A C33A 1.384(7) . ? C32B C33B 1.388(7) . ? C33 C34 1.378(8) . ? C33A C34A 1.385(8) . ? C33B C34B 1.393(7) . ? C34 C35 1.386(8) . ? C34A C35A 1.388(8) . ? C34B C35B 1.368(8) . ? C35 C36 1.387(7) . ? C35A C36A 1.388(7) . ? C35B C36B 1.381(7) . ? C37 C42 1.397(7) . ? C37 C38 1.398(7) . ? C37A C38A 1.393(7) . ? C37A C42A 1.415(7) . ? C37B C42B 1.389(7) . ? C37B C38B 1.391(7) . ? C38 C39 1.384(7) . ? C38A C39A 1.374(7) . ? C38B C39B 1.365(7) . ? C39 C40 1.380(7) . ? C39A C40A 1.385(7) . ? C39B C40B 1.381(8) . ? C40 C41 1.369(7) . ? C40A C41A 1.385(7) . ? C40B C41B 1.390(7) . ? C41 C42 1.396(7) . ? C41A C42A 1.373(7) . ? C41B C42B 1.383(7) . ? C43 C44 1.380(7) . ? C43 C48 1.381(7) . ? C43A C44A 1.395(7) . ? C43A C48A 1.407(7) . ? C43B C48B 1.379(7) . ? C43B C44B 1.385(7) . ? C44 C45 1.399(7) . ? C44A C45A 1.388(7) . ? C44B C45B 1.388(7) . ? C45 C46 1.379(7) . ? C45A C46A 1.369(7) . ? C45B C46B 1.366(8) . ? C46 C47 1.395(8) . ? C46A C47A 1.386(7) . ? C46B C47B 1.374(8) . ? C47 C48 1.379(7) . ? C47A C48A 1.369(7) . ? C47B C48B 1.404(7) . ? C49 C50 1.520(9) . ? C49A C50A 1.484(8) . ? C49B C50B 1.513(9) . ? C50 C51 1.528(10) . ? C50A C51A 1.479(9) . ? C50B C51B 1.515(9) . ? C51 C52 1.484(8) . ? C51A C52A 1.454(9) . ? C51B C52B 1.517(8) . ? 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 C11 Pt1 C12 83.5(2) . . ? C11 Pt1 P2 90.86(16) . . ? C12 Pt1 P2 174.21(16) . . ? C11 Pt1 P1 169.77(16) . . ? C12 Pt1 P1 86.38(16) . . ? P2 Pt1 P1 99.30(5) . . ? C11A Pt1A C12A 84.4(2) . . ? C11A Pt1A P2A 90.46(14) . . ? C12A Pt1A P2A 174.68(15) . . ? C11A Pt1A P1A 170.12(14) . . ? C12A Pt1A P1A 85.89(15) . . ? P2A Pt1A P1A 99.32(5) . . ? C12B Pt1B C11B 82.0(2) . . ? C12B Pt1B P1B 90.67(16) . . ? C11B Pt1B P1B 172.02(16) . . ? C12B Pt1B P2B 167.87(16) . . ? C11B Pt1B P2B 86.29(16) . . ? P1B Pt1B P2B 101.18(5) . . ? O1 Ba1 O3 139.61(12) . . ? O1 Ba1 O2 71.17(11) . . ? O3 Ba1 O2 69.79(11) . . ? O1 Ba1 C3 116.47(13) . . ? O3 Ba1 C3 75.59(13) . . ? O2 Ba1 C3 92.84(13) . . ? O1 Ba1 C9 74.56(13) . . ? O3 Ba1 C9 115.93(13) . . ? O2 Ba1 C9 117.94(13) . . ? C3 Ba1 C9 149.09(15) . . ? O1 Ba1 C2 89.47(13) . . ? O3 Ba1 C2 97.62(12) . . ? O2 Ba1 C2 85.84(13) . . ? C3 Ba1 C2 27.08(13) . . ? C9 Ba1 C2 143.50(14) . . ? O1 Ba1 C10 87.28(13) . . ? O3 Ba1 C10 119.99(13) . . ? O2 Ba1 C10 144.35(12) . . ? C3 Ba1 C10 122.51(14) . . ? C9 Ba1 C10 26.58(13) . . ? C2 Ba1 C10 123.01(14) . . ? O1 Ba1 C8 93.91(13) . . ? O3 Ba1 C8 88.82(13) . . ? O2 Ba1 C8 108.43(13) . . ? C3 Ba1 C8 147.56(14) . . ? C9 Ba1 C8 27.18(13) . . ? C2 Ba1 C8 165.67(16) . . ? C10 Ba1 C8 43.46(15) . . ? O1 Ba1 C4 125.68(12) . . ? O3 Ba1 C4 83.30(12) . . ? O2 Ba1 C4 119.33(12) . . ? C3 Ba1 C4 26.75(13) . . ? C9 Ba1 C4 122.72(14) . . ? C2 Ba1 C4 44.24(14) . . ? C10 Ba1 C4 96.28(14) . . ? C8 Ba1 C4 124.73(15) . . ? O1 Ba1 C6 114.21(13) . . ? O3 Ba1 C6 95.41(13) . . ? O2 Ba1 C6 150.60(11) . . ? C3 Ba1 C6 108.34(14) . . ? C9 Ba1 C6 44.83(14) . . ? C2 Ba1 C6 122.10(14) . . ? C10 Ba1 C6 27.02(13) . . ? C8 Ba1 C6 44.14(14) . . ? C4 Ba1 C6 82.22(14) . . ? O1 Ba1 C7 118.12(13) . . ? O3 Ba1 C7 76.96(13) . . ? O2 Ba1 C7 123.72(12) . . ? C3 Ba1 C7 121.30(14) . . ? C9 Ba1 C7 44.34(14) . . ? C2 Ba1 C7 143.70(14) . . ? C10 Ba1 C7 43.73(14) . . ? C8 Ba1 C7 26.27(13) . . ? C4 Ba1 C7 99.60(14) . . ? C6 Ba1 C7 27.14(13) . . ? O1 Ba1 C1 82.03(12) . . ? O3 Ba1 C1 119.18(12) . . ? O2 Ba1 C1 107.05(12) . . ? C3 Ba1 C1 43.59(13) . . ? C9 Ba1 C1 117.44(14) . . ? C2 Ba1 C1 26.33(13) . . ? C10 Ba1 C1 97.28(14) . . ? C8 Ba1 C1 140.73(15) . . ? C4 Ba1 C1 43.69(13) . . ? C6 Ba1 C1 102.35(13) . . ? C7 Ba1 C1 128.82(14) . . ? O3A Ba2 O1A 133.27(12) . . ? O3A Ba2 O2A 69.47(11) . . ? O1A Ba2 O2A 71.68(11) . . ? O3A Ba2 C7A 97.63(12) . . ? O1A Ba2 C7A 120.00(12) . . ? O2A Ba2 C7A 110.82(12) . . ? O3A Ba2 C8A 85.49(13) . . ? O1A Ba2 C8A 115.34(12) . . ? O2A Ba2 C8A 84.20(12) . . ? C7A Ba2 C8A 26.80(13) . . ? O3A Ba2 C1A 121.03(12) . . ? O1A Ba2 C1A 85.38(12) . . ? O2A Ba2 C1A 152.35(12) . . ? C7A Ba2 C1A 93.77(13) . . ? C8A Ba2 C1A 120.41(14) . . ? O3A Ba2 C6A 124.64(12) . . ? O1A Ba2 C6A 95.21(12) . . ? O2A Ba2 C6A 115.77(12) . . ? C7A Ba2 C6A 27.06(12) . . ? C8A Ba2 C6A 44.43(13) . . ? C1A Ba2 C6A 80.69(13) . . ? O3A Ba2 C2A 109.82(12) . . ? O1A Ba2 C2A 75.84(13) . . ? O2A Ba2 C2A 128.19(12) . . ? C7A Ba2 C2A 120.24(14) . . ? C8A Ba2 C2A 147.01(14) . . ? C1A Ba2 C2A 26.70(13) . . ? C6A Ba2 C2A 106.28(14) . . ? O3A Ba2 C9A 102.92(13) . . ? O1A Ba2 C9A 88.68(12) . . ? O2A Ba2 C9A 72.13(13) . . ? C7A Ba2 C9A 43.95(14) . . ? C8A Ba2 C9A 26.76(13) . . ? C1A Ba2 C9A 123.78(14) . . ? C6A Ba2 C9A 44.28(14) . . ? C2A Ba2 C9A 145.93(14) . . ? O3A Ba2 C10A 128.21(13) . . ? O1A Ba2 C10A 76.87(12) . . ? O2A Ba2 C10A 91.23(12) . . ? C7A Ba2 C10A 43.84(14) . . ? C8A Ba2 C10A 43.90(14) . . ? C1A Ba2 C10A 98.53(14) . . ? C6A Ba2 C10A 26.80(13) . . ? C2A Ba2 C10A 119.26(14) . . ? C9A Ba2 C10A 26.68(13) . . ? O3A Ba2 C5A 99.86(12) . . ? O1A Ba2 C5A 112.30(12) . . ? O2A Ba2 C5A 165.22(12) . . ? C7A Ba2 C5A 80.06(13) . . ? C8A Ba2 C5A 105.65(13) . . ? C1A Ba2 C5A 26.93(12) . . ? C6A Ba2 C5A 78.54(13) . . ? C2A Ba2 C5A 44.36(13) . . ? C9A Ba2 C5A 121.35(14) . . ? C10A Ba2 C5A 103.51(14) . . ? O3A Ba2 C3A 83.21(12) . . ? O1A Ba2 C3A 96.78(12) . . ? O2A Ba2 C3A 122.49(13) . . ? C7A Ba2 C3A 122.58(14) . . ? C8A Ba2 C3A 144.27(14) . . ? C1A Ba2 C3A 43.76(13) . . ? C6A Ba2 C3A 121.39(14) . . ? C2A Ba2 C3A 26.89(13) . . ? C9A Ba2 C3A 165.35(15) . . ? C10A Ba2 C3A 142.28(14) . . ? C5A Ba2 C3A 44.02(14) . . ? O3B Ba3 O2B 75.22(12) . . ? O3B Ba3 O1B 147.80(12) . . ? O2B Ba3 O1B 73.39(11) . . ? O3B Ba3 C9B 117.59(13) . . ? O2B Ba3 C9B 100.38(14) . . ? O1B Ba3 C9B 75.47(13) . . ? O3B Ba3 C10B 120.60(13) . . ? O2B Ba3 C10B 127.37(13) . . ? O1B Ba3 C10B 84.90(12) . . ? C9B Ba3 C10B 27.02(14) . . ? O3B Ba3 C5B 106.71(13) . . ? O2B Ba3 C5B 143.82(13) . . ? O1B Ba3 C5B 94.54(13) . . ? C9B Ba3 C5B 109.55(14) . . ? C10B Ba3 C5B 83.76(14) . . ? O3B Ba3 C1B 119.52(14) . . ? O2B Ba3 C1B 120.07(13) . . ? O1B Ba3 C1B 71.91(13) . . ? C9B Ba3 C1B 115.81(14) . . ? C10B Ba3 C1B 96.14(14) . . ? C5B Ba3 C1B 26.96(13) . . ? O3B Ba3 C4B 80.04(13) . . ? O2B Ba3 C4B 130.63(13) . . ? O1B Ba3 C4B 115.93(13) . . ? C9B Ba3 C4B 128.98(15) . . ? C10B Ba3 C4B 102.01(14) . . ? C5B Ba3 C4B 27.22(13) . . ? C1B Ba3 C4B 44.09(15) . . ? O3B Ba3 C2B 100.10(13) . . ? O2B Ba3 C2B 99.41(14) . . ? O1B Ba3 C2B 78.25(13) . . ? C9B Ba3 C2B 140.75(15) . . ? C10B Ba3 C2B 122.63(15) . . ? C5B Ba3 C2B 44.41(14) . . ? C1B Ba3 C2B 26.51(13) . . ? C4B Ba3 C2B 44.31(15) . . ? O3B Ba3 C6B 94.62(13) . . ? O2B Ba3 C6B 134.15(13) . . ? O1B Ba3 C6B 112.41(12) . . ? C9B Ba3 C6B 44.76(14) . . ? C10B Ba3 C6B 27.50(13) . . ? C5B Ba3 C6B 82.03(13) . . ? C1B Ba3 C6B 104.02(14) . . ? C4B Ba3 C6B 89.39(14) . . ? C2B Ba3 C6B 126.44(14) . . ? O3B Ba3 C8B 90.80(13) . . ? O2B Ba3 C8B 90.69(14) . . ? O1B Ba3 C8B 96.58(12) . . ? C9B Ba3 C8B 27.02(13) . . ? C10B Ba3 C8B 44.23(15) . . ? C5B Ba3 C8B 125.00(14) . . ? C1B Ba3 C8B 140.22(15) . . ? C4B Ba3 C8B 132.00(15) . . ? C2B Ba3 C8B 166.70(15) . . ? C6B Ba3 C8B 44.15(14) . . ? O3B Ba3 C3B 76.38(14) . . ? O2B Ba3 C3B 105.00(14) . . ? O1B Ba3 C3B 105.00(13) . . ? C9B Ba3 C3B 153.65(15) . . ? C10B Ba3 C3B 127.01(15) . . ? C5B Ba3 C3B 44.22(14) . . ? C1B Ba3 C3B 43.61(15) . . ? C4B Ba3 C3B 26.72(14) . . ? C2B Ba3 C3B 26.84(14) . . ? C6B Ba3 C3B 115.97(14) . . ? C8B Ba3 C3B 156.14(15) . . ? C5 P1 C25 99.1(2) . . ? C5 P1 C31 100.7(2) . . ? C25 P1 C31 102.9(2) . . ? C5 P1 Pt1 130.25(17) . . ? C25 P1 Pt1 109.36(18) . . ? C31 P1 Pt1 111.13(19) . . ? C6A P1A C31A 99.0(2) . . ? C6A P1A C25A 101.0(2) . . ? C31A P1A C25A 102.7(2) . . ? C6A P1A Pt1A 129.33(16) . . ? C31A P1A Pt1A 110.54(17) . . ? C25A P1A Pt1A 110.93(16) . . ? C5B P1B C25B 106.9(2) . . ? C5B P1B C31B 99.0(2) . . ? C25B P1B C31B 99.3(2) . . ? C5B P1B Pt1B 118.00(18) . . ? C25B P1B Pt1B 113.76(17) . . ? C31B P1B Pt1B 117.28(18) . . ? C6 P2 C37 110.7(2) . . ? C6 P2 C43 101.3(2) . . ? C37 P2 C43 99.9(2) . . ? C6 P2 Pt1 114.23(16) . . ? C37 P2 Pt1 114.18(16) . . ? C43 P2 Pt1 114.97(17) . . ? C5A P2A C43A 110.5(2) . . ? C5A P2A C37A 101.8(2) . . ? C43A P2A C37A 101.0(2) . . ? C5A P2A Pt1A 114.02(17) . . ? C43A P2A Pt1A 113.21(16) . . ? C37A P2A Pt1A 115.05(17) . . ? C6B P2B C43B 98.8(2) . . ? C6B P2B C37B 100.2(2) . . ? C43B P2B C37B 103.7(2) . . ? C6B P2B Pt1B 130.22(16) . . ? C43B P2B Pt1B 108.23(17) . . ? C37B P2B Pt1B 112.33(18) . . ? C13 O1 C16 107.9(4) . . ? C13 O1 Ba1 111.0(3) . . ? C16 O1 Ba1 138.4(3) . . ? C16A O1A C13A 107.7(4) . . ? C16A O1A Ba2 117.3(3) . . ? C13A O1A Ba2 135.0(3) . . ? C16B O1B C13B 106.3(4) . . ? C16B O1B Ba3 126.2(3) . . ? C13B O1B Ba3 118.3(3) . . ? C17 O2 C20 108.0(4) . . ? C17 O2 Ba1 139.4(3) . . ? C20 O2 Ba1 111.7(3) . . ? C20A O2A C17A 109.3(4) . . ? C20A O2A Ba2 140.5(3) . . ? C17A O2A Ba2 110.0(3) . . ? C17B O2B C20B 108.6(5) . . ? C17B O2B Ba3 125.0(3) . . ? C20B O2B Ba3 125.3(4) . . ? C24 O3 C21 109.0(4) . . ? C24 O3 Ba1 124.1(3) . . ? C21 O3 Ba1 122.4(3) . . ? C24A O3A C21A 104.7(4) . . ? C24A O3A Ba2 134.2(3) . . ? C21A O3A Ba2 120.2(3) . . ? C24B O3B C21B 106.1(5) . . ? C24B O3B Ba3 121.2(4) . . ? C21B O3B Ba3 132.7(3) . . ? C49 O4 C52 106.0(5) . . ? C49A O4A C52A 105.1(5) . . ? C49B O4B C52B 105.1(5) . . ? C2 C1 C5 109.3(5) . . ? C2 C1 Ba1 74.9(3) . . ? C5 C1 Ba1 77.3(3) . . ? C2A C1A C5A 109.8(4) . . ? C2A C1A Ba2 77.5(3) . . ? C5A C1A Ba2 78.1(3) . . ? C2B C1B C5B 109.8(5) . . ? C2B C1B Ba3 77.5(3) . . ? C5B C1B Ba3 76.2(3) . . ? C1 C2 C3 107.5(5) . . ? C1 C2 Ba1 78.7(3) . . ? C3 C2 Ba1 76.0(3) . . ? C1A C2A C3A 107.1(5) . . ? C1A C2A Ba2 75.8(3) . . ? C3A C2A Ba2 77.5(3) . . ? C1B C2B C3B 107.3(5) . . ? C1B C2B Ba3 76.0(3) . . ? C3B C2B Ba3 77.4(3) . . ? C4 C3 C2 108.4(5) . . ? C4 C3 Ba1 77.5(3) . . ? C2 C3 Ba1 76.9(3) . . ? C4A C3A C2A 108.3(5) . . ? C4A C3A Ba2 77.8(3) . . ? C2A C3A Ba2 75.6(3) . . ? C4B C3B C2B 108.3(5) . . ? C4B C3B Ba3 75.2(3) . . ? C2B C3B Ba3 75.8(3) . . ? C3 C4 C5 108.6(5) . . ? C3 C4 Ba1 75.7(3) . . ? C5 C4 Ba1 78.7(3) . . ? C3A C4A C5A 108.5(4) . . ? C3A C4A Ba2 75.8(3) . . ? C5A C4A Ba2 75.5(3) . . ? C3B C4B C5B 107.9(5) . . ? C3B C4B Ba3 78.0(3) . . ? C5B C4B Ba3 76.0(3) . . ? C4 C5 C1 106.2(5) . . ? C4 C5 P1 125.9(4) . . ? C1 C5 P1 126.1(4) . . ? C4 C5 Ba1 74.6(3) . . ? C1 C5 Ba1 75.9(3) . . ? P1 C5 Ba1 127.1(2) . . ? C1A C5A C4A 106.4(4) . . ? C1A C5A P2A 120.8(4) . . ? C4A C5A P2A 130.7(4) . . ? C1A C5A Ba2 74.9(3) . . ? C4A C5A Ba2 77.8(3) . . ? P2A C5A Ba2 125.7(2) . . ? C1B C5B C4B 106.7(5) . . ? C1B C5B P1B 129.9(4) . . ? C4B C5B P1B 120.2(4) . . ? C1B C5B Ba3 76.8(3) . . ? C4B C5B Ba3 76.8(3) . . ? P1B C5B Ba3 127.8(2) . . ? C10 C6 C7 105.2(4) . . ? C10 C6 P2 120.3(4) . . ? C7 C6 P2 131.6(4) . . ? C10 C6 Ba1 75.9(3) . . ? C7 C6 Ba1 76.6(3) . . ? P2 C6 Ba1 127.4(2) . . ? C10A C6A C7A 106.3(5) . . ? C10A C6A P1A 127.4(4) . . ? C7A C6A P1A 124.0(4) . . ? C10A C6A Ba2 77.1(3) . . ? C7A C6A Ba2 75.2(3) . . ? P1A C6A Ba2 126.8(2) . . ? C7B C6B C10B 107.1(5) . . ? C7B C6B P2B 126.1(4) . . ? C10B C6B P2B 124.9(4) . . ? C7B C6B Ba3 77.7(3) . . ? C10B C6B Ba3 74.9(3) . . ? P2B C6B Ba3 125.8(2) . . ? C8 C7 C6 108.6(5) . . ? C8 C7 Ba1 76.2(3) . . ? C6 C7 Ba1 76.3(3) . . ? C8A C7A C6A 109.0(5) . . ? C8A C7A Ba2 76.8(3) . . ? C6A C7A Ba2 77.7(3) . . ? C8B C7B C6B 108.0(5) . . ? C8B C7B Ba3 75.9(3) . . ? C6B C7B Ba3 75.4(3) . . ? C7 C8 C9 109.6(5) . . ? C7 C8 Ba1 77.5(3) . . ? C9 C8 Ba1 76.2(3) . . ? C7A C8A C9A 108.2(5) . . ? C7A C8A Ba2 76.4(3) . . ? C9A C8A Ba2 78.0(3) . . ? C7B C8B C9B 108.7(5) . . ? C7B C8B Ba3 77.5(3) . . ? C9B C8B Ba3 74.5(3) . . ? C10 C9 C8 105.7(5) . . ? C10 C9 Ba1 76.9(3) . . ? C8 C9 Ba1 76.7(3) . . ? C8A C9A C10A 107.5(5) . . ? C8A C9A Ba2 75.2(3) . . ? C10A C9A Ba2 76.8(3) . . ? C10B C9B C8B 108.0(5) . . ? C10B C9B Ba3 76.7(3) . . ? C8B C9B Ba3 78.5(3) . . ? C9 C10 C6 110.8(5) . . ? C9 C10 Ba1 76.5(3) . . ? C6 C10 Ba1 77.1(3) . . ? C9A C10A C6A 108.9(5) . . ? C9A C10A Ba2 76.5(3) . . ? C6A C10A Ba2 76.1(3) . . ? C9B C10B C6B 108.1(5) . . ? C9B C10B Ba3 76.3(3) . . ? C6B C10B Ba3 77.6(3) . . ? O1 C13 C14 104.8(5) . . ? O1A C13A C14A 105.1(5) . . ? O1B C13B C14B 108.1(4) . . ? C13 C14 C15 100.6(5) . . ? C15A C14A C13A 107.6(6) . . ? C13B C14B C15B 103.9(4) . . ? C14 C15 C16 103.8(5) . . ? C14A C15A C16A 104.2(7) . . ? C16B C15B C14B 102.1(5) . . ? O1 C16 C15 105.2(5) . . ? O1A C16A C15A 105.6(5) . . ? O1B C16B C15B 105.8(5) . . ? O2 C17 C18 106.4(4) . . ? O2A C17A C18A 106.0(5) . . ? O2B C17B C18B 106.1(5) . . ? C17 C18 C19 101.4(5) . . ? C17A C18A C19A 103.5(5) . . ? C17B C18B C19B 102.2(5) . . ? C20 C19 C18 101.6(5) . . ? C18A C19A C20A 101.7(5) . . ? C20B C19B C18B 105.5(6) . . ? O2 C20 C19 106.7(5) . . ? O2A C20A C19A 105.7(4) . . ? O2B C20B C19B 107.8(6) . . ? O3 C21 C22 106.5(5) . . ? O3A C21A C22A 106.2(5) . . ? O3B C21B C22B 103.9(6) . . ? C21 C22 C23 104.1(5) . . ? C21A C22A C23A 105.5(5) . . ? C23B C22B C21B 103.5(5) . . ? C22 C23 C24 103.1(5) . . ? C24A C23A C22A 103.4(5) . . ? C22B C23B C24B 106.2(6) . . ? O3 C24 C23 105.7(4) . . ? O3A C24A C23A 104.6(4) . . ? O3B C24B C23B 105.5(5) . . ? C30 C25 C26 117.5(5) . . ? C30 C25 P1 119.0(4) . . ? C26 C25 P1 123.4(4) . . ? C30A C25A C26A 118.6(4) . . ? C30A C25A P1A 122.6(4) . . ? C26A C25A P1A 118.7(4) . . ? C30B C25B C26B 117.4(5) . . ? C30B C25B P1B 123.2(4) . . ? C26B C25B P1B 119.3(4) . . ? C27 C26 C25 120.1(5) . . ? C27A C26A C25A 119.9(5) . . ? C27B C26B C25B 121.2(5) . . ? C28 C27 C26 120.8(5) . . ? C26A C27A C28A 120.9(5) . . ? C26B C27B C28B 120.3(5) . . ? C29 C28 C27 119.4(5) . . ? C29A C28A C27A 119.6(5) . . ? C29B C28B C27B 119.1(5) . . ? C30 C29 C28 119.4(5) . . ? C28A C29A C30A 119.3(5) . . ? C28B C29B C30B 120.8(5) . . ? C29 C30 C25 122.8(5) . . ? C29A C30A C25A 121.6(5) . . ? C29B C30B C25B 121.2(5) . . ? C36 C31 C32 118.7(5) . . ? C36 C31 P1 121.5(5) . . ? C32 C31 P1 119.8(4) . . ? C36A C31A C32A 119.1(4) . . ? C36A C31A P1A 120.2(4) . . ? C32A C31A P1A 120.6(4) . . ? C36B C31B C32B 119.1(5) . . ? C36B C31B P1B 120.9(4) . . ? C32B C31B P1B 119.9(4) . . ? C31 C32 C33 121.0(6) . . ? C33A C32A C31A 120.3(5) . . ? C33B C32B C31B 120.9(5) . . ? C34 C33 C32 119.7(6) . . ? C32A C33A C34A 120.6(5) . . ? C32B C33B C34B 118.8(6) . . ? C33 C34 C35 120.0(6) . . ? C33A C34A C35A 119.2(5) . . ? C35B C34B C33B 120.4(6) . . ? C34 C35 C36 119.3(6) . . ? C36A C35A C34A 121.1(5) . . ? C34B C35B C36B 120.8(6) . . ? C31 C36 C35 121.3(6) . . ? C35A C36A C31A 119.6(5) . . ? C35B C36B C31B 119.9(6) . . ? C42 C37 C38 117.5(5) . . ? C42 C37 P2 122.7(4) . . ? C38 C37 P2 119.7(4) . . ? C38A C37A C42A 118.2(5) . . ? C38A C37A P2A 122.5(4) . . ? C42A C37A P2A 119.0(4) . . ? C42B C37B C38B 118.4(5) . . ? C42B C37B P2B 120.5(4) . . ? C38B C37B P2B 121.1(4) . . ? C39 C38 C37 121.7(5) . . ? C39A C38A C37A 121.4(5) . . ? C39B C38B C37B 121.3(6) . . ? C40 C39 C38 119.6(5) . . ? C38A C39A C40A 119.7(5) . . ? C38B C39B C40B 120.0(6) . . ? C41 C40 C39 120.2(5) . . ? C39A C40A C41A 120.2(5) . . ? C39B C40B C41B 119.9(5) . . ? C40 C41 C42 120.4(5) . . ? C42A C41A C40A 120.5(5) . . ? C42B C41B C40B 119.6(5) . . ? C41 C42 C37 120.6(5) . . ? C41A C42A C37A 120.1(5) . . ? C41B C42B C37B 120.7(5) . . ? C44 C43 C48 119.2(5) . . ? C44 C43 P2 120.7(4) . . ? C48 C43 P2 119.8(4) . . ? C44A C43A C48A 117.7(5) . . ? C44A C43A P2A 117.5(4) . . ? C48A C43A P2A 124.8(4) . . ? C48B C43B C44B 118.7(5) . . ? C48B C43B P2B 123.4(4) . . ? C44B C43B P2B 117.9(4) . . ? C43 C44 C45 120.4(5) . . ? C45A C44A C43A 120.8(5) . . ? C43B C44B C45B 121.1(5) . . ? C46 C45 C44 120.1(5) . . ? C46A C45A C44A 120.2(5) . . ? C46B C45B C44B 119.7(6) . . ? C45 C46 C47 119.2(5) . . ? C45A C46A C47A 119.9(5) . . ? C45B C46B C47B 120.4(5) . . ? C48 C47 C46 120.3(5) . . ? C48A C47A C46A 120.4(5) . . ? C46B C47B C48B 119.9(6) . . ? C47 C48 C43 120.8(5) . . ? C47A C48A C43A 120.8(5) . . ? C43B C48B C47B 120.1(5) . . ? O4 C49 C50 106.0(5) . . ? O4A C49A C50A 107.9(5) . . ? O4B C49B C50B 109.1(5) . . ? C49 C50 C51 102.6(5) . . ? C51A C50A C49A 102.9(6) . . ? C49B C50B C51B 103.0(5) . . ? C52 C51 C50 106.4(6) . . ? C52A C51A C50A 107.0(6) . . ? C50B C51B C52B 102.6(5) . . ? O4 C52 C51 105.4(6) . . ? O4A C52A C51A 107.8(6) . . ? O4B C52B C51B 103.9(5) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 2.035 _refine_diff_density_min -1.165 _refine_diff_density_rms 0.162