Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2003 data_global _publ_contact_author_email ADW24@CUS.CAM.AC.UK _publ_contact_author_name 'Dr Anthony Woods' _journal_name_full 'J.Chem.Soc.,Dalton Trans.' _journal_coden_Cambridge 0186 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name A.Woods B.Ahrens J.M.Cole J.P.Hickey J.N.Martin M.J.Mays ; P.Raithby ; S.J.Teat data_for_complex_5 _database_code_CSD 197610 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C35 H28 Cl2 Co Fe Mo O10 P' _chemical_formula_weight 921.16 _chemical_melting_point ? _chemical_compound_source ? 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.3658(4) _cell_length_b 10.7100(4) _cell_length_c 18.1348(6) _cell_angle_alpha 81.443(2) _cell_angle_beta 80.052(2) _cell_angle_gamma 66.061(2) _cell_volume 1805.49(11) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour red _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.694 _exptl_crystal_density_method ? _exptl_crystal_F_000 924 _exptl_absorpt_coefficient_mu 1.441 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 1.032 _exptl_absorpt_correction_T_max 0.977 _exptl_absorpt_process_details 'from symmetry-related measurements, SORATAV (Blessing 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Nonius KappaCCD' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 20615 _diffrn_reflns_av_R_equivalents 0.0704 _diffrn_reflns_av_sigmaI/netI 0.0910 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.14 _diffrn_reflns_theta_max 27.52 _reflns_number_total 8217 _reflns_number_observed 5832 _reflns_observed_criterion >2sigma(I) _computing_data_collection ; "Collect" data collection software, Nonius' B.V., 1998. ; _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1995)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 17 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0289P)^2^+0.2972P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8200 _refine_ls_number_parameters 462 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0779 _refine_ls_R_factor_obs 0.0411 _refine_ls_wR_factor_all 0.1034 _refine_ls_wR_factor_obs 0.0760 _refine_ls_goodness_of_fit_all 1.025 _refine_ls_goodness_of_fit_obs 1.073 _refine_ls_restrained_S_all 1.217 _refine_ls_restrained_S_obs 1.073 _refine_ls_shift/esd_max -0.005 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Mo1 Mo 0.13124(3) 0.51542(3) 0.121352(14) 0.01982(8) Uani 1 d . . Co1 Co 0.37383(5) 0.36895(4) 0.18231(2) 0.01934(11) Uani 1 d . . Fe1 Fe 0.73823(5) 0.15169(4) 0.26941(2) 0.02126(12) Uani 1 d . . P1 P 0.50468(9) 0.18918(8) 0.25857(4) 0.0192(2) Uani 1 d . . O1 O -0.0909(3) 0.3908(3) 0.11161(14) 0.0427(7) Uani 1 d . . C1 C -0.0110(4) 0.4385(3) 0.1150(2) 0.0294(8) Uani 1 d . . O2 O 0.3045(3) 0.3686(2) -0.02295(13) 0.0419(6) Uani 1 d . . C2 C 0.2414(4) 0.4199(3) 0.0306(2) 0.0269(8) Uani 1 d . . O3 O 0.3787(3) 0.5976(2) 0.24913(14) 0.0427(7) Uani 1 d . . C3 C 0.3834(3) 0.5051(3) 0.2225(2) 0.0265(8) Uani 1 d . . O4 O 0.5760(3) 0.3427(3) 0.04522(14) 0.0516(8) Uani 1 d . . C4 C 0.4995(4) 0.3483(3) 0.0994(2) 0.0278(8) Uani 1 d . . O5 O 0.6880(3) 0.4414(2) 0.2496(2) 0.0463(7) Uani 1 d . . C5 C 0.7033(4) 0.3289(3) 0.2557(2) 0.0296(8) Uani 1 d . . O6 O 0.8227(3) 0.0960(2) 0.11198(13) 0.0403(6) Uani 1 d . . C6 C 0.7853(4) 0.1215(3) 0.1734(2) 0.0279(8) Uani 1 d . . O7 O 0.2315(3) 0.1499(2) 0.09680(12) 0.0308(6) Uani 1 d . . C7 C 0.2178(4) 0.0257(3) 0.0854(2) 0.0417(10) Uani 1 d . . H7A H 0.2475(25) 0.0073(14) 0.0324(4) 0.063 Uiso 1 calc R . H7B H 0.1184(6) 0.0363(9) 0.0990(13) 0.063 Uiso 1 calc R . H7C H 0.2782(19) -0.0511(5) 0.1169(10) 0.063 Uiso 1 calc R . O8 O 0.1798(3) 0.1049(2) 0.22115(12) 0.0349(6) Uani 1 d . . C8 C 0.2080(3) 0.1785(3) 0.1694(2) 0.0238(7) Uani 1 d . . O9 O -0.0148(2) 0.4009(2) 0.31382(12) 0.0301(5) Uani 1 d . . C9 C -0.1152(4) 0.4560(4) 0.3783(2) 0.0423(10) Uani 1 d . . H9A H -0.1861(15) 0.4149(18) 0.3876(8) 0.063 Uiso 1 calc R . H9B H -0.1630(18) 0.5557(5) 0.3685(5) 0.063 Uiso 1 calc R . H9C H -0.0648(5) 0.4350(20) 0.4224(3) 0.063 Uiso 1 calc R . O10 O 0.1052(3) 0.5210(2) 0.33790(12) 0.0320(6) Uani 1 d . . C10 C 0.0922(4) 0.4461(3) 0.2986(2) 0.0251(7) Uani 1 d . . C11 C 0.1826(3) 0.3994(3) 0.2285(2) 0.0209(7) Uani 1 d . . C12 C 0.2209(3) 0.3079(3) 0.1764(2) 0.0194(7) Uani 1 d . . C13 C 0.1065(4) 0.7242(3) 0.0498(2) 0.0327(8) Uani 1 d . . H13 H 0.1475(4) 0.7276(3) -0.0011(2) 0.039 Uiso 1 calc R . C14 C -0.0296(4) 0.7237(3) 0.0751(2) 0.0338(9) Uani 1 d . . H14 H -0.0960(4) 0.7257(3) 0.0443(2) 0.041 Uiso 1 calc R . C15 C -0.0502(4) 0.7197(3) 0.1545(2) 0.0300(8) Uani 1 d . . H15 H -0.1334(4) 0.7202(3) 0.1864(2) 0.036 Uiso 1 calc R . C16 C 0.0746(4) 0.7147(3) 0.1778(2) 0.0293(8) Uani 1 d . . H16 H 0.0911(4) 0.7095(3) 0.2283(2) 0.035 Uiso 1 calc R . C17 C 0.1713(4) 0.7187(3) 0.1130(2) 0.0308(8) Uani 1 d . . H17 H 0.2635(4) 0.7179(3) 0.1122(2) 0.037 Uiso 1 calc R . C18 C 0.3992(4) 0.2048(3) 0.3516(2) 0.0237(7) Uani 1 d . . C19 C 0.2970(4) 0.1478(3) 0.3723(2) 0.0289(8) Uani 1 d . . H19 H 0.2855(4) 0.0935(3) 0.3390(2) 0.035 Uiso 1 calc R . C20 C 0.2128(4) 0.1698(3) 0.4406(2) 0.0376(9) Uani 1 d . . H20 H 0.1462(4) 0.1276(3) 0.4546(2) 0.045 Uiso 1 calc R . C21 C 0.2233(4) 0.2522(4) 0.4893(2) 0.0385(9) Uani 1 d . . H21 H 0.1635(4) 0.2682(4) 0.5358(2) 0.046 Uiso 1 calc R . C22 C 0.3226(4) 0.3108(4) 0.4690(2) 0.0376(9) Uani 1 d . . H22 H 0.3314(4) 0.3672(4) 0.5020(2) 0.045 Uiso 1 calc R . C23 C 0.4089(4) 0.2879(3) 0.4011(2) 0.0314(8) Uani 1 d . . H23 H 0.4761(4) 0.3294(3) 0.3879(2) 0.038 Uiso 1 calc R . C24 C 0.5261(3) 0.0220(3) 0.2314(2) 0.0215(7) Uani 1 d . . C25 C 0.5378(4) -0.0929(3) 0.2823(2) 0.0260(8) Uani 1 d . . H25 H 0.5282(4) -0.0849(3) 0.3347(2) 0.031 Uiso 1 calc R . C26 C 0.5633(4) -0.2179(3) 0.2574(2) 0.0305(8) Uani 1 d . . H26 H 0.5690(4) -0.2943(3) 0.2928(2) 0.037 Uiso 1 calc R . C27 C 0.5805(4) -0.2325(3) 0.1811(2) 0.0297(8) Uani 1 d . . H27 H 0.5992(4) -0.3186(3) 0.1641(2) 0.036 Uiso 1 calc R . C28 C 0.5702(4) -0.1204(3) 0.1302(2) 0.0274(8) Uani 1 d . . H28 H 0.5819(4) -0.1292(3) 0.0779(2) 0.033 Uiso 1 calc R . C29 C 0.5429(3) 0.0053(3) 0.1554(2) 0.0242(7) Uani 1 d . . H29 H 0.5354(3) 0.0817(3) 0.1197(2) 0.029 Uiso 1 calc R . C30 C 0.8313(4) -0.0527(3) 0.3143(2) 0.0267(8) Uani 1 d . . H30 H 0.8272(4) -0.1288(3) 0.2952(2) 0.032 Uiso 1 calc R . C31 C 0.9379(4) 0.0015(3) 0.2917(2) 0.0276(8) Uani 1 d . . H31 H 1.0179(4) -0.0326(3) 0.2548(2) 0.033 Uiso 1 calc R . C32 C 0.9053(4) 0.1134(3) 0.3326(2) 0.0298(8) Uani 1 d . . H32 H 0.9591(4) 0.1683(3) 0.3286(2) 0.036 Uiso 1 calc R . C33 C 0.7768(4) 0.1306(3) 0.3815(2) 0.0307(8) Uani 1 d . . H33 H 0.7294(4) 0.1994(3) 0.4156(2) 0.037 Uiso 1 calc R . C34 C 0.7329(4) 0.0266(3) 0.3701(2) 0.0284(8) Uani 1 d . . H34 H 0.6511(4) 0.0127(3) 0.3957(2) 0.034 Uiso 1 calc R . C0 C 0.2455(5) -0.2779(5) 0.3956(2) 0.0579(12) Uani 1 d . . H0A H 0.2691(5) -0.2293(5) 0.3477(2) 0.070 Uiso 1 calc R . H0B H 0.2130(5) -0.3468(5) 0.3836(2) 0.070 Uiso 1 calc R . Cl3 Cl 0.39957(13) -0.36220(12) 0.44166(7) 0.0633(3) Uani 1 d . . Cl2 Cl 0.10968(13) -0.16145(12) 0.45053(6) 0.0647(3) Uani 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.0184(2) 0.01822(14) 0.0220(2) -0.00348(11) -0.00106(12) -0.00632(12) Co1 0.0178(3) 0.0176(2) 0.0230(2) -0.0022(2) -0.0012(2) -0.0077(2) Fe1 0.0204(3) 0.0196(2) 0.0237(2) -0.0003(2) -0.0031(2) -0.0081(2) P1 0.0205(5) 0.0178(4) 0.0197(4) -0.0028(3) -0.0006(3) -0.0082(4) O1 0.038(2) 0.051(2) 0.051(2) 0.0010(13) -0.0131(13) -0.0286(14) C1 0.029(2) 0.029(2) 0.029(2) -0.0006(14) -0.006(2) -0.010(2) O2 0.046(2) 0.0429(15) 0.0299(14) -0.0145(12) 0.0035(13) -0.0103(13) C2 0.029(2) 0.026(2) 0.024(2) -0.0012(14) -0.004(2) -0.009(2) O3 0.036(2) 0.0359(14) 0.065(2) -0.0228(13) -0.0021(13) -0.0181(13) C3 0.018(2) 0.023(2) 0.037(2) -0.0013(15) -0.002(2) -0.0081(15) O4 0.033(2) 0.067(2) 0.039(2) 0.0085(13) 0.0086(13) -0.0124(15) C4 0.021(2) 0.023(2) 0.033(2) 0.0055(14) -0.005(2) -0.0037(15) O5 0.039(2) 0.0230(13) 0.081(2) 0.0022(12) -0.0181(14) -0.0142(12) C5 0.018(2) 0.033(2) 0.040(2) -0.001(2) -0.007(2) -0.011(2) O6 0.037(2) 0.051(2) 0.0259(14) -0.0059(12) 0.0039(12) -0.0124(13) C6 0.021(2) 0.025(2) 0.036(2) 0.005(2) -0.005(2) -0.009(2) O7 0.044(2) 0.0242(12) 0.0306(13) -0.0082(10) -0.0050(11) -0.0176(12) C7 0.048(3) 0.029(2) 0.058(3) -0.013(2) -0.011(2) -0.020(2) O8 0.044(2) 0.0304(13) 0.0384(14) 0.0013(11) -0.0013(12) -0.0254(13) C8 0.015(2) 0.022(2) 0.034(2) -0.0043(14) -0.0067(15) -0.0062(14) O9 0.0243(14) 0.0360(13) 0.0335(13) -0.0118(10) 0.0079(11) -0.0169(11) C9 0.031(2) 0.055(2) 0.041(2) -0.021(2) 0.018(2) -0.020(2) O10 0.035(2) 0.0380(13) 0.0292(13) -0.0143(11) 0.0029(11) -0.0198(12) C10 0.024(2) 0.025(2) 0.027(2) -0.0024(14) -0.0015(15) -0.010(2) C11 0.021(2) 0.022(2) 0.023(2) -0.0006(13) -0.0035(14) -0.0116(15) C12 0.016(2) 0.0196(15) 0.024(2) -0.0004(13) -0.0024(13) -0.0094(14) C13 0.035(2) 0.022(2) 0.036(2) 0.0014(15) -0.001(2) -0.009(2) C14 0.029(2) 0.024(2) 0.043(2) 0.000(2) -0.012(2) -0.003(2) C15 0.023(2) 0.020(2) 0.040(2) -0.0070(14) 0.002(2) -0.002(2) C16 0.034(2) 0.018(2) 0.032(2) -0.0110(14) -0.003(2) -0.004(2) C17 0.030(2) 0.016(2) 0.048(2) -0.0040(15) -0.003(2) -0.011(2) C18 0.025(2) 0.022(2) 0.022(2) -0.0002(13) -0.0004(14) -0.0080(15) C19 0.030(2) 0.032(2) 0.026(2) -0.0033(14) 0.003(2) -0.016(2) C20 0.037(2) 0.041(2) 0.038(2) 0.002(2) 0.005(2) -0.023(2) C21 0.040(3) 0.047(2) 0.024(2) -0.003(2) 0.008(2) -0.017(2) C22 0.038(2) 0.045(2) 0.030(2) -0.013(2) -0.003(2) -0.014(2) C23 0.028(2) 0.038(2) 0.031(2) -0.008(2) 0.001(2) -0.015(2) C24 0.019(2) 0.019(2) 0.026(2) -0.0040(13) -0.0006(14) -0.0072(14) C25 0.030(2) 0.026(2) 0.024(2) 0.0014(14) -0.0050(15) -0.015(2) C26 0.030(2) 0.019(2) 0.042(2) 0.0011(15) -0.002(2) -0.012(2) C27 0.028(2) 0.019(2) 0.041(2) -0.0104(15) 0.003(2) -0.008(2) C28 0.027(2) 0.027(2) 0.027(2) -0.0113(14) 0.0024(15) -0.008(2) C29 0.022(2) 0.022(2) 0.028(2) -0.0001(13) -0.0024(15) -0.0083(15) C30 0.029(2) 0.017(2) 0.030(2) 0.0031(13) -0.007(2) -0.0051(15) C31 0.021(2) 0.024(2) 0.031(2) 0.0012(14) -0.006(2) -0.0027(15) C32 0.027(2) 0.031(2) 0.035(2) -0.0006(15) -0.009(2) -0.013(2) C33 0.032(2) 0.031(2) 0.026(2) -0.0056(15) -0.009(2) -0.007(2) C34 0.027(2) 0.031(2) 0.023(2) 0.0076(14) -0.007(2) -0.009(2) C0 0.045(3) 0.088(3) 0.043(2) -0.023(2) -0.012(2) -0.020(3) Cl3 0.0444(7) 0.0707(7) 0.0680(7) -0.0145(6) -0.0140(6) -0.0098(6) Cl2 0.0454(8) 0.0826(8) 0.0493(6) -0.0108(6) -0.0085(5) -0.0053(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 C1 1.984(4) . ? Mo1 C2 1.990(3) . ? Mo1 C11 2.169(3) . ? Mo1 C12 2.187(3) . ? Mo1 C15 2.312(3) . ? Mo1 C16 2.317(3) . ? Mo1 C14 2.317(3) . ? Mo1 C13 2.353(3) . ? Mo1 C17 2.356(3) . ? Mo1 Co1 2.6924(5) . ? Co1 C3 1.768(3) . ? Co1 C4 1.787(3) . ? Co1 C11 1.929(3) . ? Co1 C12 1.968(3) . ? Co1 P1 2.2794(9) . ? Fe1 C6 1.767(4) . ? Fe1 C5 1.769(3) . ? Fe1 C30 2.101(3) . ? Fe1 C33 2.101(3) . ? Fe1 C31 2.104(3) . ? Fe1 C34 2.105(3) . ? Fe1 C32 2.109(3) . ? Fe1 P1 2.3266(9) . ? P1 C18 1.836(3) . ? P1 C24 1.845(3) . ? O1 C1 1.150(4) . ? O2 C2 1.150(4) . ? O3 C3 1.146(4) . ? O4 C4 1.144(4) . ? O5 C5 1.140(4) . ? O6 C6 1.149(4) . ? O7 C8 1.355(4) . ? O7 C7 1.442(3) . ? O8 C8 1.207(3) . ? C8 C12 1.471(4) . ? O9 C10 1.353(4) . ? O9 C9 1.443(4) . ? O10 C10 1.208(3) . ? C10 C11 1.463(4) . ? C11 C12 1.358(4) . ? C13 C17 1.407(5) . ? C13 C14 1.408(5) . ? C14 C15 1.416(5) . ? C15 C16 1.407(5) . ? C16 C17 1.414(4) . ? C18 C19 1.397(4) . ? C18 C23 1.397(4) . ? C19 C20 1.378(4) . ? C20 C21 1.382(5) . ? C21 C22 1.383(5) . ? C22 C23 1.381(5) . ? C24 C29 1.388(4) . ? C24 C25 1.400(4) . ? C25 C26 1.386(4) . ? C26 C27 1.388(5) . ? C27 C28 1.380(4) . ? C28 C29 1.389(4) . ? C30 C34 1.408(4) . ? C30 C31 1.421(4) . ? C31 C32 1.397(4) . ? C32 C33 1.426(5) . ? C33 C34 1.415(4) . ? C0 Cl2 1.729(4) . ? C0 Cl3 1.770(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 C1 Mo1 C2 87.17(13) . . ? C1 Mo1 C11 91.90(12) . . ? C2 Mo1 C11 115.74(12) . . ? C1 Mo1 C12 76.57(12) . . ? C2 Mo1 C12 82.02(12) . . ? C11 Mo1 C12 36.33(11) . . ? C1 Mo1 C15 90.06(13) . . ? C2 Mo1 C15 140.59(12) . . ? C11 Mo1 C15 103.64(12) . . ? C12 Mo1 C15 135.24(11) . . ? C1 Mo1 C16 122.96(13) . . ? C2 Mo1 C16 141.59(12) . . ? C11 Mo1 C16 88.78(11) . . ? C12 Mo1 C16 124.80(11) . . ? C15 Mo1 C16 35.39(12) . . ? C1 Mo1 C14 86.86(13) . . ? C2 Mo1 C14 104.96(12) . . ? C11 Mo1 C14 139.17(12) . . ? C12 Mo1 C14 161.78(12) . . ? C15 Mo1 C14 35.63(12) . . ? C16 Mo1 C14 58.95(12) . . ? C1 Mo1 C13 116.87(13) . . ? C2 Mo1 C13 88.00(12) . . ? C11 Mo1 C13 144.25(12) . . ? C12 Mo1 C13 162.95(12) . . ? C15 Mo1 C13 58.64(12) . . ? C16 Mo1 C13 58.42(12) . . ? C14 Mo1 C13 35.10(12) . . ? C1 Mo1 C17 144.76(13) . . ? C2 Mo1 C17 106.42(12) . . ? C11 Mo1 C17 109.85(11) . . ? C12 Mo1 C17 136.51(12) . . ? C15 Mo1 C17 58.64(12) . . ? C16 Mo1 C17 35.22(11) . . ? C14 Mo1 C17 58.45(12) . . ? C13 Mo1 C17 34.78(11) . . ? C1 Mo1 Co1 122.68(9) . . ? C2 Mo1 Co1 83.51(10) . . ? C11 Mo1 Co1 45.18(8) . . ? C12 Mo1 Co1 46.14(8) . . ? C15 Mo1 Co1 129.33(9) . . ? C16 Mo1 Co1 96.42(9) . . ? C14 Mo1 Co1 150.00(9) . . ? C13 Mo1 Co1 119.13(9) . . ? C17 Mo1 Co1 91.58(9) . . ? C3 Co1 C4 103.51(14) . . ? C3 Co1 C11 94.83(14) . . ? C4 Co1 C11 149.21(14) . . ? C3 Co1 C12 134.75(14) . . ? C4 Co1 C12 113.90(14) . . ? C11 Co1 C12 40.78(12) . . ? C3 Co1 P1 99.33(11) . . ? C4 Co1 P1 99.63(10) . . ? C11 Co1 P1 101.55(9) . . ? C12 Co1 P1 98.58(9) . . ? C3 Co1 Mo1 97.22(11) . . ? C4 Co1 Mo1 99.77(10) . . ? C11 Co1 Mo1 52.91(9) . . ? C12 Co1 Mo1 53.27(8) . . ? P1 Co1 Mo1 150.71(3) . . ? C6 Fe1 C5 95.97(15) . . ? C6 Fe1 C30 97.62(13) . . ? C5 Fe1 C30 157.15(14) . . ? C6 Fe1 C33 154.74(15) . . ? C5 Fe1 C33 94.64(14) . . ? C30 Fe1 C33 65.97(13) . . ? C6 Fe1 C31 89.28(14) . . ? C5 Fe1 C31 122.76(14) . . ? C30 Fe1 C31 39.50(12) . . ? C33 Fe1 C31 65.75(13) . . ? C6 Fe1 C34 134.42(13) . . ? C5 Fe1 C34 129.53(14) . . ? C30 Fe1 C34 39.13(12) . . ? C33 Fe1 C34 39.32(12) . . ? C31 Fe1 C34 65.74(13) . . ? C6 Fe1 C32 117.13(14) . . ? C5 Fe1 C32 91.61(14) . . ? C30 Fe1 C32 65.83(12) . . ? C33 Fe1 C32 39.60(13) . . ? C31 Fe1 C32 38.72(12) . . ? C34 Fe1 C32 65.94(13) . . ? C6 Fe1 P1 89.38(11) . . ? C5 Fe1 P1 92.64(11) . . ? C30 Fe1 P1 105.77(10) . . ? C33 Fe1 P1 112.97(10) . . ? C31 Fe1 P1 144.52(9) . . ? C34 Fe1 P1 90.82(10) . . ? C32 Fe1 P1 152.54(10) . . ? C18 P1 C24 104.85(13) . . ? C18 P1 Co1 106.10(10) . . ? C24 P1 Co1 112.64(10) . . ? C18 P1 Fe1 110.11(11) . . ? C24 P1 Fe1 101.53(10) . . ? Co1 P1 Fe1 120.63(3) . . ? O1 C1 Mo1 178.3(3) . . ? O2 C2 Mo1 177.9(3) . . ? O3 C3 Co1 174.9(3) . . ? O4 C4 Co1 176.2(3) . . ? O5 C5 Fe1 175.4(3) . . ? O6 C6 Fe1 176.2(3) . . ? C8 O7 C7 115.0(2) . . ? O8 C8 O7 122.9(3) . . ? O8 C8 C12 125.3(3) . . ? O7 C8 C12 111.7(2) . . ? C10 O9 C9 114.0(2) . . ? O10 C10 O9 122.5(3) . . ? O10 C10 C11 125.3(3) . . ? O9 C10 C11 112.2(3) . . ? C12 C11 C10 145.0(3) . . ? C12 C11 Co1 71.1(2) . . ? C10 C11 Co1 138.5(2) . . ? C12 C11 Mo1 72.5(2) . . ? C10 C11 Mo1 121.2(2) . . ? Co1 C11 Mo1 81.90(10) . . ? C11 C12 C8 137.9(3) . . ? C11 C12 Co1 68.1(2) . . ? C8 C12 Co1 137.4(2) . . ? C11 C12 Mo1 71.1(2) . . ? C8 C12 Mo1 133.7(2) . . ? Co1 C12 Mo1 80.59(9) . . ? C17 C13 C14 108.3(3) . . ? C17 C13 Mo1 72.7(2) . . ? C14 C13 Mo1 71.1(2) . . ? C13 C14 C15 108.0(3) . . ? C13 C14 Mo1 73.8(2) . . ? C15 C14 Mo1 72.0(2) . . ? C16 C15 C14 107.7(3) . . ? C16 C15 Mo1 72.5(2) . . ? C14 C15 Mo1 72.4(2) . . ? C15 C16 C17 108.3(3) . . ? C15 C16 Mo1 72.1(2) . . ? C17 C16 Mo1 73.9(2) . . ? C13 C17 C16 107.8(3) . . ? C13 C17 Mo1 72.5(2) . . ? C16 C17 Mo1 70.9(2) . . ? C19 C18 C23 117.8(3) . . ? C19 C18 P1 122.2(2) . . ? C23 C18 P1 119.7(2) . . ? C20 C19 C18 120.6(3) . . ? C19 C20 C21 121.2(3) . . ? C22 C21 C20 118.9(3) . . ? C23 C22 C21 120.5(3) . . ? C22 C23 C18 121.1(3) . . ? C29 C24 C25 117.6(3) . . ? C29 C24 P1 118.2(2) . . ? C25 C24 P1 124.0(2) . . ? C26 C25 C24 120.9(3) . . ? C25 C26 C27 120.5(3) . . ? C28 C27 C26 119.3(3) . . ? C27 C28 C29 120.1(3) . . ? C24 C29 C28 121.6(3) . . ? C34 C30 C31 107.7(3) . . ? C34 C30 Fe1 70.6(2) . . ? C31 C30 Fe1 70.4(2) . . ? C32 C31 C30 108.6(3) . . ? C32 C31 Fe1 70.8(2) . . ? C30 C31 Fe1 70.1(2) . . ? C31 C32 C33 107.9(3) . . ? C31 C32 Fe1 70.4(2) . . ? C33 C32 Fe1 69.9(2) . . ? C34 C33 C32 107.6(3) . . ? C34 C33 Fe1 70.5(2) . . ? C32 C33 Fe1 70.5(2) . . ? C30 C34 C33 108.2(3) . . ? C30 C34 Fe1 70.3(2) . . ? C33 C34 Fe1 70.2(2) . . ? Cl2 C0 Cl3 111.6(2) . . ? _refine_diff_density_max 0.640 _refine_diff_density_min -0.850 _refine_diff_density_rms 0.102 #===END data_for_complex_6 _database_code_CSD 197611 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C30 H21 Co Mn Mo O11 P' _chemical_formula_weight 798.25 _chemical_melting_point ? _chemical_compound_source ? 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.2152(5) _cell_length_b 10.9665(3) _cell_length_c 19.4998(4) _cell_angle_alpha 90.00 _cell_angle_beta 108.314(2) _cell_angle_gamma 90.00 _cell_volume 3088.88(15) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour 'very dark' _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.717 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1592 _exptl_absorpt_coefficient_mu 1.445 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 1.059 _exptl_absorpt_correction_T_max 0.975 _exptl_absorpt_process_details 'from symmetry-related measurements, SORTAV (Blessing 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Nonius KappaCCD' _diffrn_measurement_method CCD _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 25149 _diffrn_reflns_av_R_equivalents 0.0606 _diffrn_reflns_av_sigmaI/netI 0.0562 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.41 _diffrn_reflns_theta_max 27.48 _reflns_number_total 7053 _reflns_number_observed 5826 _reflns_observed_criterion >2sigma(I) _computing_data_collection ; "Collect" data collection software, Nonius' B.V., 1998. ; _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1995)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 15 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+5.6190P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7038 _refine_ls_number_parameters 426 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0649 _refine_ls_R_factor_obs 0.0436 _refine_ls_wR_factor_all 0.3235 _refine_ls_wR_factor_obs 0.0877 _refine_ls_goodness_of_fit_all 1.155 _refine_ls_goodness_of_fit_obs 1.217 _refine_ls_restrained_S_all 4.057 _refine_ls_restrained_S_obs 1.217 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Mo1 Mo -0.30277(12) -0.38643(5) 0.30523(8) 0.0199(2) Uani 0.806(6) d P 1 Co1 Co -0.18009(3) -0.46185(4) 0.24472(2) 0.02069(12) Uani 0.806(6) d P 1 Mn1 Mn -0.35176(4) -0.42557(5) 0.15160(3) 0.02560(14) Uani 0.806(6) d P 1 Mo1' Mo -0.3417(5) -0.3805(2) 0.2812(3) 0.0225(10) Uani 0.194(6) d P 2 Co1' Co -0.35176(4) -0.42557(5) 0.15160(3) 0.02560(14) Uani 0.194(6) d P 2 Mn1' Mn -0.18009(3) -0.46185(4) 0.24472(2) 0.02069(12) Uani 0.194(6) d P 2 P1 P -0.21891(6) -0.45951(7) 0.12634(4) 0.0219(2) Uani 1 d . . C1 C -0.3833(2) -0.5849(3) 0.1279(2) 0.0298(8) Uani 1 d . . O1 O -0.4034(2) -0.6846(2) 0.11509(15) 0.0452(7) Uani 1 d . . C2 C -0.3948(3) -0.3458(4) 0.0674(2) 0.0390(9) Uani 1 d . . O2 O -0.4207(3) -0.2917(3) 0.0151(2) 0.0707(11) Uani 1 d . . C3 C -0.4706(3) -0.4165(4) 0.1599(3) 0.0298(11) Uani 0.806(6) d P 1 O3 O -0.5450(2) -0.4130(3) 0.1607(2) 0.0488(7) Uani 0.806(6) d P 1 C3' C -0.4621(16) -0.3935(21) 0.1996(14) 0.039(5) Uiso 0.194(6) d P 2 O3' O -0.5450(2) -0.4130(3) 0.1607(2) 0.0488(7) Uani 0.194(6) d P 2 C4 C -0.1720(3) -0.6264(3) 0.2558(2) 0.0321(8) Uani 1 d . . O4 O -0.1670(3) -0.7282(3) 0.2644(2) 0.0620(10) Uani 1 d . . C5 C -0.0598(3) -0.4311(3) 0.2625(2) 0.0313(8) Uani 1 d . . O5 O 0.0171(2) -0.4184(3) 0.2717(2) 0.0543(8) Uani 1 d . . C6 C -0.1775(3) -0.4386(4) 0.3638(2) 0.0248(10) Uani 0.806(6) d P 1 O6 O -0.1100(2) -0.4651(3) 0.41064(13) 0.0399(7) Uani 0.806(6) d P 1 C6' C -0.1407(15) -0.4748(19) 0.3498(11) 0.031(5) Uiso 0.194(6) d P 2 O6' O -0.1100(2) -0.4651(3) 0.41064(13) 0.0399(7) Uani 0.194(6) d P 2 C7 C -0.3390(3) -0.5611(3) 0.2843(2) 0.0287(8) Uani 1 d . . O7 O -0.3580(2) -0.6622(2) 0.28405(14) 0.0404(7) Uani 1 d . . C8 C -0.1385(4) 0.0002(4) 0.3465(3) 0.064(2) Uani 1 d . . H8A H -0.1788(4) 0.0639(14) 0.3552(17) 0.096 Uiso 1 calc R . H8B H -0.1027(19) 0.0332(21) 0.3167(9) 0.096 Uiso 1 calc R . H8C H -0.0960(17) -0.0280(8) 0.3927(9) 0.096 Uiso 1 calc R . O8 O -0.1945(2) -0.1013(3) 0.3091(2) 0.0607(10) Uani 1 d . . C9 C -0.1514(3) -0.1940(3) 0.2911(2) 0.0365(9) Uani 1 d . . O9 O -0.0700(3) -0.1942(3) 0.3028(3) 0.140(3) Uani 1 d . . C10 C -0.2152(2) -0.2907(3) 0.2510(2) 0.0222(7) Uani 1 d . . C11 C -0.3055(2) -0.2718(3) 0.2060(2) 0.0241(7) Uani 1 d . . C12 C -0.3515(3) -0.1513(3) 0.1859(2) 0.0330(8) Uani 1 d . . O12 O -0.4270(2) -0.1225(2) 0.1878(2) 0.0447(7) Uani 1 d . . C13 C -0.3381(4) 0.0412(4) 0.1352(4) 0.095(2) Uani 1 d . . H13A H -0.2945(16) 0.0874(17) 0.1175(26) 0.142 Uiso 1 calc R . H13B H -0.3483(32) 0.0844(17) 0.1760(7) 0.142 Uiso 1 calc R . H13C H -0.3971(18) 0.0329(5) 0.0963(18) 0.142 Uiso 1 calc R . O13 O -0.3004(2) -0.0788(3) 0.1584(2) 0.0645(10) Uani 1 d . . C14 C -0.3353(3) -0.3951(4) 0.4100(2) 0.0415(10) Uani 1 d . . H14 H -0.3081(3) -0.4592(4) 0.4425(2) 0.050 Uiso 1 calc R 1 C15 C -0.4226(3) -0.3981(4) 0.3564(2) 0.0405(10) Uani 1 d . . H15 H -0.4653(3) -0.4640(4) 0.3466(2) 0.049 Uiso 1 calc R 1 C16 C -0.4350(3) -0.2854(4) 0.3201(2) 0.0418(10) Uani 1 d . . H16 H -0.4874(3) -0.2620(4) 0.2810(2) 0.050 Uiso 1 calc R 1 C17 C -0.3565(3) -0.2137(3) 0.3517(2) 0.0364(9) Uani 1 d . . H17 H -0.3468(3) -0.1330(3) 0.3378(2) 0.044 Uiso 1 calc R 1 C18 C -0.2955(3) -0.2802(4) 0.4066(2) 0.0426(10) Uani 1 d . . H18 H -0.2369(3) -0.2531(4) 0.4369(2) 0.051 Uiso 1 calc R 1 C19 C -0.2123(2) -0.5978(3) 0.0759(2) 0.0246(7) Uani 1 d . . C20 C -0.1402(3) -0.6798(3) 0.1014(2) 0.0288(8) Uani 1 d . . H20 H -0.0956(3) -0.6677(3) 0.1475(2) 0.035 Uiso 1 calc R . C21 C -0.1329(3) -0.7800(3) 0.0596(2) 0.0358(9) Uani 1 d . . H21 H -0.0833(3) -0.8361(3) 0.0770(2) 0.043 Uiso 1 calc R . C22 C -0.1985(3) -0.7976(4) -0.0076(2) 0.0441(10) Uani 1 d . . H22 H -0.1934(3) -0.8656(4) -0.0362(2) 0.053 Uiso 1 calc R . C23 C -0.2710(3) -0.7171(4) -0.0330(2) 0.0474(11) Uani 1 d . . H23 H -0.3161(3) -0.7303(4) -0.0787(2) 0.057 Uiso 1 calc R . C24 C -0.2781(3) -0.6162(4) 0.0085(2) 0.0379(9) Uani 1 d . . H24 H -0.3276(3) -0.5601(4) -0.0091(2) 0.045 Uiso 1 calc R . C25 C -0.1549(2) -0.3530(3) 0.0879(2) 0.0263(7) Uani 1 d . . C26 C -0.1541(3) -0.2289(3) 0.1034(2) 0.0447(11) Uani 1 d . . H26 H -0.1938(3) -0.1979(3) 0.1285(2) 0.054 Uiso 1 calc R . C27 C -0.0956(4) -0.1504(4) 0.0825(2) 0.0504(12) Uani 1 d . . H27 H -0.0947(4) -0.0662(4) 0.0942(2) 0.061 Uiso 1 calc R . C28 C -0.0392(3) -0.1933(4) 0.0452(2) 0.0415(10) Uani 1 d . . H28 H 0.0016(3) -0.1393(4) 0.0321(2) 0.050 Uiso 1 calc R . C29 C -0.0420(3) -0.3141(4) 0.0268(2) 0.0472(11) Uani 1 d . . H29 H -0.0039(3) -0.3436(4) 0.0000(2) 0.057 Uiso 1 calc R . C30 C -0.1006(3) -0.3936(4) 0.0473(2) 0.0387(9) Uani 1 d . . H30 H -0.1034(3) -0.4768(4) 0.0333(2) 0.046 Uiso 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 Mo1 0.0200(5) 0.0194(2) 0.0209(4) -0.0011(2) 0.0074(4) -0.0006(2) Co1 0.0208(2) 0.0184(2) 0.0214(2) 0.0000(2) 0.0044(2) 0.0020(2) Mn1 0.0236(3) 0.0231(3) 0.0253(3) -0.0021(2) 0.0008(2) 0.0019(2) Mo1' 0.024(2) 0.0214(8) 0.024(2) 0.0015(8) 0.010(2) 0.0018(9) Co1' 0.0236(3) 0.0231(3) 0.0253(3) -0.0021(2) 0.0008(2) 0.0019(2) Mn1' 0.0208(2) 0.0184(2) 0.0214(2) 0.0000(2) 0.0044(2) 0.0020(2) P1 0.0261(5) 0.0197(4) 0.0201(4) -0.0004(3) 0.0073(3) 0.0008(4) C1 0.025(2) 0.036(2) 0.028(2) -0.0029(15) 0.0069(14) -0.002(2) O1 0.052(2) 0.0308(15) 0.052(2) -0.0087(13) 0.0158(14) -0.0138(14) C2 0.041(2) 0.042(2) 0.032(2) 0.002(2) 0.008(2) 0.004(2) O2 0.081(3) 0.082(3) 0.042(2) 0.031(2) 0.010(2) 0.013(2) C3 0.026(3) 0.029(2) 0.030(3) -0.003(2) 0.003(2) 0.001(2) O3 0.024(2) 0.064(2) 0.056(2) -0.0012(15) 0.0104(13) 0.0022(15) O3' 0.024(2) 0.064(2) 0.056(2) -0.0012(15) 0.0104(13) 0.0022(15) C4 0.035(2) 0.031(2) 0.034(2) 0.005(2) 0.016(2) 0.007(2) O4 0.082(3) 0.027(2) 0.092(2) 0.019(2) 0.049(2) 0.014(2) C5 0.032(2) 0.035(2) 0.029(2) -0.0067(15) 0.013(2) 0.001(2) O5 0.025(2) 0.076(2) 0.066(2) -0.021(2) 0.0202(14) -0.009(2) C6 0.030(3) 0.020(2) 0.027(2) 0.000(2) 0.013(2) -0.001(2) O6 0.038(2) 0.056(2) 0.0227(13) 0.0049(12) 0.0043(12) 0.0074(14) O6' 0.038(2) 0.056(2) 0.0227(13) 0.0049(12) 0.0043(12) 0.0074(14) C7 0.029(2) 0.030(2) 0.028(2) -0.0011(14) 0.0113(15) -0.004(2) O7 0.052(2) 0.0257(14) 0.048(2) 0.0005(12) 0.0217(14) -0.0089(13) C8 0.109(5) 0.036(2) 0.056(3) -0.023(2) 0.038(3) -0.037(3) O8 0.071(2) 0.041(2) 0.090(2) -0.038(2) 0.054(2) -0.030(2) C9 0.036(2) 0.021(2) 0.041(2) 0.000(2) -0.004(2) -0.003(2) O9 0.036(2) 0.047(2) 0.278(7) -0.062(3) -0.035(3) 0.003(2) C10 0.026(2) 0.018(2) 0.023(2) -0.0006(12) 0.0076(13) -0.0037(13) C11 0.026(2) 0.020(2) 0.028(2) -0.0008(13) 0.0099(14) 0.0003(14) C12 0.031(2) 0.025(2) 0.043(2) 0.001(2) 0.011(2) 0.003(2) O12 0.033(2) 0.0353(15) 0.068(2) 0.0112(14) 0.0188(14) 0.0132(13) C13 0.075(4) 0.039(3) 0.189(7) 0.056(4) 0.070(5) 0.025(3) O13 0.051(2) 0.028(2) 0.129(3) 0.034(2) 0.049(2) 0.0179(14) C14 0.053(3) 0.041(2) 0.036(2) 0.004(2) 0.022(2) 0.008(2) C15 0.039(2) 0.036(2) 0.058(3) -0.010(2) 0.033(2) -0.010(2) C16 0.028(2) 0.045(2) 0.049(2) -0.007(2) 0.007(2) 0.007(2) C17 0.046(2) 0.026(2) 0.047(2) -0.004(2) 0.029(2) 0.005(2) C18 0.037(2) 0.047(2) 0.041(2) -0.016(2) 0.008(2) 0.001(2) C19 0.026(2) 0.026(2) 0.024(2) -0.0026(13) 0.0102(14) -0.0014(14) C20 0.030(2) 0.027(2) 0.030(2) 0.0006(14) 0.0104(15) 0.001(2) C21 0.043(2) 0.025(2) 0.045(2) -0.002(2) 0.020(2) 0.004(2) C22 0.052(3) 0.034(2) 0.053(3) -0.021(2) 0.026(2) -0.006(2) C23 0.041(3) 0.056(3) 0.040(2) -0.026(2) 0.004(2) -0.001(2) C24 0.036(2) 0.042(2) 0.032(2) -0.011(2) 0.005(2) 0.008(2) C25 0.031(2) 0.026(2) 0.021(2) 0.0033(13) 0.0067(14) 0.0013(15) C26 0.077(3) 0.029(2) 0.042(2) -0.003(2) 0.039(2) -0.006(2) C27 0.080(4) 0.032(2) 0.046(2) -0.005(2) 0.029(2) -0.016(2) C28 0.042(2) 0.045(2) 0.039(2) 0.009(2) 0.015(2) -0.011(2) C29 0.051(3) 0.043(2) 0.060(3) 0.009(2) 0.036(2) 0.003(2) C30 0.044(2) 0.032(2) 0.048(2) 0.000(2) 0.025(2) 0.003(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 C6 1.974(5) . ? Mo1 C7 2.000(4) . ? Mo1 C10 2.210(3) . ? Mo1 C14 2.250(4) . ? Mo1 C18 2.267(4) . ? Mo1 C11 2.296(3) . ? Mo1 C15 2.342(4) . ? Mo1 C17 2.355(3) . ? Mo1 C16 2.393(4) . ? Mo1 Co1 2.6351(9) . ? Mo1 Mn1 2.8827(14) . ? Co1 C5 1.785(4) . ? Co1 C4 1.817(4) . ? Co1 C10 1.965(3) . ? Co1 P1 2.1958(9) . ? Co1 C6 2.325(4) . ? Co1 Mn1 2.7013(7) . ? Mn1 C2 1.792(4) . ? Mn1 C1 1.833(4) . ? Mn1 C3 1.868(5) . ? Mn1 C11 1.999(3) . ? Mn1 P1 2.2567(10) . ? Mo1' C7 1.982(4) . ? Mo1' C3' 2.02(3) . ? Mo1' C16 2.086(5) . ? Mo1' C11 2.093(4) . ? Mo1' C15 2.199(4) . ? Mo1' C17 2.342(4) . ? Mo1' C10 2.396(5) . ? Mo1' C14 2.487(6) . ? Mo1' Co1' 2.533(5) . ? Mo1' C18 2.569(7) . ? Mo1' Mn1' 2.907(5) . ? Co1' C2 1.792(4) . ? Co1' C1 1.833(4) . ? Co1' C11 1.999(3) . ? Co1' C3' 2.19(2) . ? Co1' P1 2.2567(10) . ? Co1' Mn1' 2.7013(7) . ? Mn1' C5 1.785(4) . ? Mn1' C4 1.817(4) . ? Mn1' C6' 1.95(2) . ? Mn1' C10 1.965(3) . ? Mn1' P1 2.1958(9) . ? P1 C25 1.826(3) . ? P1 C19 1.827(3) . ? C1 O1 1.142(4) . ? C2 O2 1.139(5) . ? C3 O3 1.137(5) . ? C3' O3' 1.27(2) . ? C4 O4 1.128(4) . ? C5 O5 1.135(4) . ? C6 O6 1.177(5) . ? C6' O6' 1.14(2) . ? C7 O7 1.145(4) . ? C8 O8 1.451(5) . ? O8 C9 1.315(5) . ? C9 O9 1.186(5) . ? C9 C10 1.484(5) . ? C10 C11 1.394(5) . ? C11 C12 1.489(5) . ? C12 O12 1.204(4) . ? C12 O13 1.337(5) . ? C13 O13 1.450(5) . ? C14 C18 1.408(6) . ? C14 C15 1.410(6) . ? C15 C16 1.407(6) . ? C16 C17 1.401(6) . ? C17 C18 1.384(6) . ? C19 C20 1.385(5) . ? C19 C24 1.394(5) . ? C20 C21 1.394(5) . ? C21 C22 1.389(6) . ? C22 C23 1.377(6) . ? C23 C24 1.395(5) . ? C25 C30 1.384(5) . ? C25 C26 1.393(5) . ? C26 C27 1.388(6) . ? C27 C28 1.371(6) . ? C28 C29 1.369(6) . ? C29 C30 1.393(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6 Mo1 C7 89.7(2) . . ? C6 Mo1 C10 78.3(2) . . ? C7 Mo1 C10 121.73(13) . . ? C6 Mo1 C14 84.8(2) . . ? C7 Mo1 C14 91.13(14) . . ? C10 Mo1 C14 142.4(2) . . ? C6 Mo1 C18 82.5(2) . . ? C7 Mo1 C18 127.23(15) . . ? C10 Mo1 C18 107.59(14) . . ? C14 Mo1 C18 36.33(15) . . ? C6 Mo1 C11 113.9(2) . . ? C7 Mo1 C11 114.93(13) . . ? C10 Mo1 C11 35.98(12) . . ? C14 Mo1 C11 146.83(14) . . ? C18 Mo1 C11 115.87(14) . . ? C6 Mo1 C15 118.5(2) . . ? C7 Mo1 C15 80.41(14) . . ? C10 Mo1 C15 153.87(14) . . ? C14 Mo1 C15 35.69(15) . . ? C18 Mo1 C15 59.16(15) . . ? C11 Mo1 C15 125.3(2) . . ? C6 Mo1 C17 113.5(2) . . ? C7 Mo1 C17 137.97(15) . . ? C10 Mo1 C17 97.87(12) . . ? C14 Mo1 C17 58.84(14) . . ? C18 Mo1 C17 34.78(14) . . ? C11 Mo1 C17 88.12(13) . . ? C15 Mo1 C17 57.91(14) . . ? C6 Mo1 C16 139.4(2) . . ? C7 Mo1 C16 106.3(2) . . ? C10 Mo1 C16 119.66(14) . . ? C14 Mo1 C16 58.43(15) . . ? C18 Mo1 C16 57.91(15) . . ? C11 Mo1 C16 93.17(14) . . ? C15 Mo1 C16 34.55(14) . . ? C17 Mo1 C16 34.30(14) . . ? C6 Mo1 Co1 58.50(14) . . ? C7 Mo1 Co1 78.24(10) . . ? C10 Mo1 Co1 46.84(8) . . ? C14 Mo1 Co1 141.43(13) . . ? C18 Mo1 Co1 134.78(13) . . ? C11 Mo1 Co1 67.84(8) . . ? C15 Mo1 Co1 158.42(10) . . ? C17 Mo1 Co1 143.64(10) . . ? C16 Mo1 Co1 160.13(12) . . ? C6 Mo1 Mn1 116.48(14) . . ? C7 Mo1 Mn1 71.37(10) . . ? C10 Mo1 Mn1 64.59(8) . . ? C14 Mo1 Mn1 151.45(13) . . ? C18 Mo1 Mn1 155.30(12) . . ? C11 Mo1 Mn1 43.60(8) . . ? C15 Mo1 Mn1 116.94(13) . . ? C17 Mo1 Mn1 120.81(12) . . ? C16 Mo1 Mn1 104.03(12) . . ? Co1 Mo1 Mn1 58.42(2) . . ? C5 Co1 C4 97.9(2) . . ? C5 Co1 C10 95.1(2) . . ? C4 Co1 C10 161.91(14) . . ? C5 Co1 P1 97.04(11) . . ? C4 Co1 P1 97.02(11) . . ? C10 Co1 P1 93.74(9) . . ? C5 Co1 C6 95.2(2) . . ? C4 Co1 C6 90.6(2) . . ? C10 Co1 C6 75.70(14) . . ? P1 Co1 C6 164.50(12) . . ? C5 Co1 Mo1 132.93(11) . . ? C4 Co1 Mo1 106.83(11) . . ? C10 Co1 Mo1 55.13(9) . . ? P1 Co1 Mo1 118.21(5) . . ? C6 Co1 Mo1 46.38(14) . . ? C5 Co1 Mn1 144.95(12) . . ? C4 Co1 Mn1 103.96(12) . . ? C10 Co1 Mn1 71.15(10) . . ? P1 Co1 Mn1 53.68(3) . . ? C6 Co1 Mn1 111.38(12) . . ? Mo1 Co1 Mn1 65.38(4) . . ? C2 Mn1 C1 104.1(2) . . ? C2 Mn1 C3 88.2(2) . . ? C1 Mn1 C3 83.6(2) . . ? C2 Mn1 C11 92.3(2) . . ? C1 Mn1 C11 163.54(14) . . ? C3 Mn1 C11 95.6(2) . . ? C2 Mn1 P1 88.58(13) . . ? C1 Mn1 P1 88.20(11) . . ? C3 Mn1 P1 170.2(2) . . ? C11 Mn1 P1 93.74(10) . . ? C2 Mn1 Co1 133.26(14) . . ? C1 Mn1 Co1 98.64(11) . . ? C3 Mn1 Co1 135.03(15) . . ? C11 Mn1 Co1 70.29(10) . . ? P1 Mn1 Co1 51.63(2) . . ? C2 Mn1 Mo1 141.23(13) . . ? C1 Mn1 Mo1 111.48(11) . . ? C3 Mn1 Mo1 81.0(2) . . ? C11 Mn1 Mo1 52.38(9) . . ? P1 Mn1 Mo1 107.13(4) . . ? Co1 Mn1 Mo1 56.20(3) . . ? C7 Mo1' C3' 87.6(7) . . ? C7 Mo1' C16 119.9(2) . . ? C3' Mo1' C16 76.7(7) . . ? C7 Mo1' C11 125.6(2) . . ? C3' Mo1' C11 82.0(7) . . ? C16 Mo1' C11 109.2(2) . . ? C7 Mo1' C15 84.5(2) . . ? C3' Mo1' C15 87.7(7) . . ? C16 Mo1' C15 38.2(2) . . ? C11 Mo1' C15 147.4(3) . . ? C7 Mo1' C17 140.2(2) . . ? C3' Mo1' C17 106.7(7) . . ? C16 Mo1' C17 36.30(15) . . ? C11 Mo1' C17 93.50(15) . . ? C15 Mo1' C17 60.00(15) . . ? C7 Mo1' C10 114.0(2) . . ? C3' Mo1' C10 115.8(7) . . ? C16 Mo1' C10 125.1(2) . . ? C11 Mo1' C10 35.38(13) . . ? C15 Mo1' C10 149.5(3) . . ? C17 Mo1' C10 93.2(2) . . ? C7 Mo1' C14 84.9(2) . . ? C3' Mo1' C14 122.0(7) . . ? C16 Mo1' C14 58.7(2) . . ? C11 Mo1' C14 143.9(3) . . ? C15 Mo1' C14 34.3(2) . . ? C17 Mo1' C14 55.8(2) . . ? C10 Mo1' C14 119.7(3) . . ? C7 Mo1' Co1' 80.16(15) . . ? C3' Mo1' Co1' 56.2(7) . . ? C16 Mo1' Co1' 128.7(4) . . ? C11 Mo1' Co1' 50.11(12) . . ? C15 Mo1' Co1' 141.0(4) . . ? C17 Mo1' Co1' 138.7(2) . . ? C10 Mo1' Co1' 68.61(9) . . ? C14 Mo1' Co1' 165.01(14) . . ? C7 Mo1' C18 113.7(3) . . ? C3' Mo1' C18 133.6(7) . . ? C16 Mo1' C18 56.9(2) . . ? C11 Mo1' C18 111.7(2) . . ? C15 Mo1' C18 56.4(2) . . ? C17 Mo1' C18 32.31(15) . . ? C10 Mo1' C18 93.3(3) . . ? C14 Mo1' C18 32.29(15) . . ? Co1' Mo1' C18 161.1(2) . . ? C7 Mo1' Mn1' 71.9(2) . . ? C3' Mo1' Mn1' 114.4(7) . . ? C16 Mo1' Mn1' 165.2(3) . . ? C11 Mo1' Mn1' 64.80(13) . . ? C15 Mo1' Mn1' 146.1(3) . . ? C17 Mo1' Mn1' 128.9(3) . . ? C10 Mo1' Mn1' 42.14(11) . . ? C14 Mo1' Mn1' 117.4(3) . . ? Co1' Mo1' Mn1' 59.07(5) . . ? C18 Mo1' Mn1' 111.4(3) . . ? C2 Co1' C1 104.1(2) . . ? C2 Co1' C11 92.3(2) . . ? C1 Co1' C11 163.54(14) . . ? C2 Co1' C3' 101.8(6) . . ? C1 Co1' C3' 94.9(6) . . ? C11 Co1' C3' 80.0(6) . . ? C2 Co1' P1 88.58(13) . . ? C1 Co1' P1 88.20(11) . . ? C11 Co1' P1 93.74(10) . . ? C3' Co1' P1 168.0(6) . . ? C2 Co1' Mo1' 135.1(2) . . ? C1 Co1' Mo1' 111.53(12) . . ? C11 Co1' Mo1' 53.46(11) . . ? C3' Co1' Mo1' 50.0(7) . . ? P1 Co1' Mo1' 118.2(2) . . ? C2 Co1' Mn1' 133.26(14) . . ? C1 Co1' Mn1' 98.64(11) . . ? C11 Co1' Mn1' 70.29(10) . . ? C3' Co1' Mn1' 116.4(6) . . ? P1 Co1' Mn1' 51.63(2) . . ? Mo1' Co1' Mn1' 67.4(2) . . ? C5 Mn1' C4 97.9(2) . . ? C5 Mn1' C6' 81.5(7) . . ? C4 Mn1' C6' 79.4(6) . . ? C5 Mn1' C10 95.1(2) . . ? C4 Mn1' C10 161.91(14) . . ? C6' Mn1' C10 90.2(6) . . ? C5 Mn1' P1 97.04(11) . . ? C4 Mn1' P1 97.02(11) . . ? C6' Mn1' P1 175.9(7) . . ? C10 Mn1' P1 93.74(9) . . ? C5 Mn1' Co1' 144.95(12) . . ? C4 Mn1' Co1' 103.96(12) . . ? C6' Mn1' Co1' 129.0(7) . . ? C10 Mn1' Co1' 71.15(10) . . ? P1 Mn1' Co1' 53.68(3) . . ? C5 Mn1' Mo1' 142.1(2) . . ? C4 Mn1' Mo1' 107.85(12) . . ? C6' Mn1' Mo1' 76.7(7) . . ? C10 Mn1' Mo1' 54.89(10) . . ? P1 Mn1' Mo1' 106.57(15) . . ? Co1' Mn1' Mo1' 53.54(15) . . ? C25 P1 C19 100.58(15) . . ? C25 P1 Co1 115.93(11) . . ? C19 P1 Co1 120.92(11) . . ? C25 P1 Mn1' 115.93(11) . . ? C19 P1 Mn1' 120.92(11) . . ? C25 P1 Co1' 127.87(12) . . ? C19 P1 Co1' 117.30(11) . . ? Mn1' P1 Co1' 74.69(3) . . ? C25 P1 Mn1 127.87(12) . . ? C19 P1 Mn1 117.30(11) . . ? Co1 P1 Mn1 74.69(3) . . ? O1 C1 Mn1 177.9(3) . . ? O1 C1 Co1' 177.9(3) . . ? O2 C2 Mn1 177.7(4) . . ? O2 C2 Co1' 177.7(4) . . ? O3 C3 Mn1 175.9(4) . . ? O3' C3' Mo1' 165.5(17) . . ? O3' C3' Co1' 117.9(16) . . ? Mo1' C3' Co1' 73.8(7) . . ? O4 C4 Co1 178.2(3) . . ? O4 C4 Mn1' 178.2(3) . . ? O5 C5 Co1 175.6(3) . . ? O5 C5 Mn1' 175.6(3) . . ? O6 C6 Mo1 165.9(4) . . ? O6 C6 Co1 118.9(3) . . ? Mo1 C6 Co1 75.12(14) . . ? O6' C6' Mn1' 168.7(15) . . ? O7 C7 Mo1' 164.6(4) . . ? O7 C7 Mo1 168.8(3) . . ? C9 O8 C8 117.6(4) . . ? O9 C9 O8 121.8(4) . . ? O9 C9 C10 124.8(4) . . ? O8 C9 C10 113.3(3) . . ? C11 C10 C9 125.3(3) . . ? C11 C10 Co1 109.7(2) . . ? C9 C10 Co1 124.7(3) . . ? C11 C10 Mn1' 109.7(2) . . ? C9 C10 Mn1' 124.7(3) . . ? C11 C10 Mo1 75.4(2) . . ? C9 C10 Mo1 118.6(2) . . ? Co1 C10 Mo1 78.03(11) . . ? C11 C10 Mo1' 60.4(3) . . ? C9 C10 Mo1' 127.3(3) . . ? Mn1' C10 Mo1' 82.97(13) . . ? C10 C11 C12 125.9(3) . . ? C10 C11 Mn1 108.7(2) . . ? C12 C11 Mn1 123.4(2) . . ? C10 C11 Co1' 108.7(2) . . ? C12 C11 Co1' 123.4(2) . . ? C10 C11 Mo1' 84.2(3) . . ? C12 C11 Mo1' 119.0(3) . . ? Co1' C11 Mo1' 76.4(2) . . ? C10 C11 Mo1 68.6(2) . . ? C12 C11 Mo1 126.2(2) . . ? Mn1 C11 Mo1 84.02(12) . . ? O12 C12 O13 122.5(3) . . ? O12 C12 C11 126.8(3) . . ? O13 C12 C11 110.5(3) . . ? C12 O13 C13 116.2(3) . . ? C18 C14 C15 107.7(4) . . ? C18 C14 Mo1 72.5(2) . . ? C15 C14 Mo1 75.7(2) . . ? C18 C14 Mo1' 77.1(2) . . ? C15 C14 Mo1' 61.6(3) . . ? C16 C15 C14 107.4(4) . . ? C16 C15 Mo1' 66.5(2) . . ? C14 C15 Mo1' 84.1(3) . . ? C16 C15 Mo1 74.7(2) . . ? C14 C15 Mo1 68.6(2) . . ? C17 C16 C15 108.2(4) . . ? C17 C16 Mo1' 81.8(3) . . ? C15 C16 Mo1' 75.2(2) . . ? C17 C16 Mo1 71.4(2) . . ? C15 C16 Mo1 70.7(2) . . ? C18 C17 C16 108.4(4) . . ? C18 C17 Mo1' 82.9(3) . . ? C16 C17 Mo1' 61.9(3) . . ? C18 C17 Mo1 69.1(2) . . ? C16 C17 Mo1 74.3(2) . . ? C17 C18 C14 108.3(4) . . ? C17 C18 Mo1 76.1(2) . . ? C14 C18 Mo1 71.2(2) . . ? C17 C18 Mo1' 64.7(2) . . ? C14 C18 Mo1' 70.6(2) . . ? C20 C19 C24 119.8(3) . . ? C20 C19 P1 121.1(3) . . ? C24 C19 P1 118.9(3) . . ? C19 C20 C21 120.1(3) . . ? C22 C21 C20 119.7(4) . . ? C23 C22 C21 120.5(3) . . ? C22 C23 C24 119.9(4) . . ? C19 C24 C23 119.9(4) . . ? C30 C25 C26 118.2(3) . . ? C30 C25 P1 121.3(3) . . ? C26 C25 P1 120.3(3) . . ? C27 C26 C25 120.3(4) . . ? C28 C27 C26 120.6(4) . . ? C29 C28 C27 119.9(4) . . ? C28 C29 C30 120.0(4) . . ? C25 C30 C29 120.9(4) . . ? _refine_diff_density_max 0.842 _refine_diff_density_min -0.695 _refine_diff_density_rms 0.083 #===END data_for_complex_9 _database_code_CSD 197612 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H22 Fe O12 Os3 P' _chemical_formula_weight 1255.92 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Os Os -1.2165 7.6030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.9577(19) _cell_length_b 10.834(2) _cell_length_c 34.169(7) _cell_angle_alpha 90.00 _cell_angle_beta 94.537(10) _cell_angle_gamma 90.00 _cell_volume 3305.7(12) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 14240 _cell_measurement_theta_min 2.96 _cell_measurement_theta_max 29.25 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.523 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2316 _exptl_absorpt_coefficient_mu 12.036 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5320 _exptl_absorpt_correction_T_max 0.7948 _exptl_absorpt_process_details 'from symmetry-related measurements, SORTAV (Blessing 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.69230 _diffrn_radiation_type Synchrotron _diffrn_radiation_source 'Synchrotron Radiation Source, Daresbury Laboratories, UK' _diffrn_radiation_monochromator Si(111) _diffrn_measurement_device_type 'Bruker SMART CCD' _diffrn_measurement_method 'Thin slice, \w-scans' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 22341 _diffrn_reflns_av_R_equivalents 0.0430 _diffrn_reflns_av_sigmaI/netI 0.0579 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -47 _diffrn_reflns_limit_l_max 48 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 29.29 _reflns_number_total 8711 _reflns_number_gt 6792 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'LSCELL (CLEGG, 1997)' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (Sheldrick, 1996)' _computing_publication_material 'SHELXL-97 (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. The osmium triangle was refined on two positions. Both positions are very similar, but refinement with full occupancy on one positions resulted in high rest electron density. The solvent molecule (hexane) is disorderd, the bond lengths and angles within were not restrained. ; _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^)+(0.0191P)^2^+38.3767P] 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 'methyl rigid, others riding' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8711 _refine_ls_number_parameters 469 _refine_ls_number_restraints 257 _refine_ls_R_factor_all 0.0786 _refine_ls_R_factor_gt 0.0559 _refine_ls_wR_factor_ref 0.0973 _refine_ls_wR_factor_gt 0.0935 _refine_ls_goodness_of_fit_ref 1.178 _refine_ls_restrained_S_all 1.163 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Os1 Os 0.32622(10) 0.20199(12) 0.41359(3) 0.0221(2) Uani 0.90 1 d P A 1 Os2 Os 0.60861(9) 0.07875(10) 0.41079(3) 0.0204(2) Uani 0.90 1 d P A 1 Os3 Os 0.54623(11) 0.30065(11) 0.36535(3) 0.0182(2) Uani 0.90 1 d P A 1 Fe1 Fe 0.65384(15) 0.48191(12) 0.31961(4) 0.0231(3) Uani 1 1 d . A 1 P1 P 0.4193(3) 0.4633(2) 0.33340(6) 0.0225(5) Uani 1 1 d . A 1 C1 C 0.2480(11) 0.1103(10) 0.3676(3) 0.031(2) Uani 1 1 d U A 1 C2 C 0.1686(13) 0.3181(10) 0.4054(3) 0.039(3) Uani 1 1 d U A 1 C3 C 0.2379(12) 0.0904(10) 0.4490(3) 0.034(2) Uani 1 1 d U A 1 C4 C 0.4133(12) 0.2992(10) 0.4576(3) 0.031(2) Uani 1 1 d U A 1 C5 C 0.8013(12) 0.0396(9) 0.3958(3) 0.032(2) Uani 1 1 d U A 1 C6 C 0.6941(12) 0.1775(9) 0.4541(3) 0.032(2) Uani 1 1 d U A 1 C7 C 0.5654(14) -0.0471(10) 0.4472(3) 0.038(2) Uani 1 1 d U A 1 C8 C 0.5201(12) -0.0188(9) 0.3668(3) 0.031(2) Uani 1 1 d U A 1 C9 C 0.6301(11) 0.3946(8) 0.4098(3) 0.0244(19) Uani 1 1 d U A 1 C10 C 0.4766(11) 0.1987(8) 0.3215(3) 0.0249(18) Uani 1 1 d U A 1 C11 C 0.7418(10) 0.3117(8) 0.3430(3) 0.0237(17) Uani 1 1 d U A 1 C12 C 0.6323(12) 0.4033(9) 0.2746(3) 0.030(2) Uani 1 1 d U A 1 C21 C 0.7614(12) 0.6234(9) 0.2924(3) 0.046(3) Uani 1 1 d DU A 1 H21 H 0.7639 0.6301 0.2647 0.055 Uiso 1 1 calc R A 1 C22 C 0.6530(13) 0.6744(9) 0.3146(3) 0.047(3) Uani 1 1 d DU A 1 H22 H 0.5688 0.7219 0.3050 0.056 Uiso 1 1 calc R A 1 C23 C 0.6923(12) 0.6422(9) 0.3540(3) 0.037(2) Uani 1 1 d DU A 1 H23 H 0.6380 0.6637 0.3757 0.044 Uiso 1 1 calc R A 1 C24 C 0.8224(12) 0.5744(9) 0.3557(3) 0.037(2) Uani 1 1 d DU A 1 H24 H 0.8738 0.5425 0.3789 0.044 Uiso 1 1 calc R A 1 C25 C 0.8662(12) 0.5604(9) 0.3177(3) 0.041(2) Uani 1 1 d DU A 1 H25 H 0.9513 0.5164 0.3103 0.049 Uiso 1 1 calc R A 1 C31 C 0.3293(10) 0.5842(8) 0.3602(2) 0.0262(18) Uani 1 1 d DU A 1 C32 C 0.3598(13) 0.5980(9) 0.4006(3) 0.044(3) Uani 1 1 d DU A 1 H32 H 0.4284 0.5431 0.4142 0.053 Uiso 1 1 calc R A 1 C33 C 0.2931(14) 0.6895(10) 0.4215(3) 0.051(3) Uani 1 1 d DU A 1 H33 H 0.3186 0.6986 0.4489 0.061 Uiso 1 1 calc R A 1 C34 C 0.1893(14) 0.7675(10) 0.4025(3) 0.048(3) Uani 1 1 d DU A 1 H34 H 0.1390 0.8276 0.4168 0.057 Uiso 1 1 calc R A 1 C35 C 0.1596(14) 0.7568(9) 0.3621(3) 0.045(3) Uani 1 1 d DU A 1 H35 H 0.0907 0.8120 0.3487 0.055 Uiso 1 1 calc R A 1 C36 C 0.2290(12) 0.6666(9) 0.3411(3) 0.034(2) Uani 1 1 d DU A 1 H36 H 0.2080 0.6611 0.3135 0.041 Uiso 1 1 calc R A 1 C41 C 0.2826(10) 0.4362(8) 0.2918(2) 0.0283(19) Uani 1 1 d DU A 1 C42 C 0.1656(10) 0.3536(9) 0.2946(3) 0.0291(19) Uani 1 1 d DU A 1 H42 H 0.1596 0.3059 0.3178 0.035 Uiso 1 1 calc R A 1 C43 C 0.0575(12) 0.3409(10) 0.2635(3) 0.041(2) Uani 1 1 d DU A 1 H43 H -0.0219 0.2835 0.2654 0.050 Uiso 1 1 calc R A 1 C44 C 0.0641(12) 0.4111(10) 0.2298(3) 0.044(3) Uani 1 1 d DU A 1 H44 H -0.0121 0.4041 0.2090 0.053 Uiso 1 1 calc R A 1 C45 C 0.1829(14) 0.4916(11) 0.2268(3) 0.047(3) Uani 1 1 d DU A 1 H45 H 0.1902 0.5373 0.2032 0.056 Uiso 1 1 calc R A 1 C46 C 0.2910(12) 0.5061(10) 0.2577(3) 0.038(2) Uani 1 1 d DU A 1 H46 H 0.3706 0.5631 0.2557 0.046 Uiso 1 1 calc R A 1 O1 O 0.1913(8) 0.0594(7) 0.3410(2) 0.0356(17) Uani 1 1 d U A 1 O2 O 0.0744(11) 0.3881(9) 0.4009(3) 0.065(3) Uani 1 1 d U A 1 O3 O 0.1845(11) 0.0239(8) 0.4698(2) 0.056(2) Uani 1 1 d U A 1 O4 O 0.4520(9) 0.3617(7) 0.4834(2) 0.0411(19) Uani 1 1 d U A 1 O5 O 0.9193(10) 0.0132(9) 0.3888(3) 0.057(2) Uani 1 1 d U A 1 O6 O 0.7526(10) 0.2291(7) 0.4803(2) 0.049(2) Uani 1 1 d U A 1 O7 O 0.5385(12) -0.1212(8) 0.4694(2) 0.061(3) Uani 1 1 d U A 1 O8 O 0.4773(10) -0.0845(7) 0.3423(2) 0.045(2) Uani 1 1 d U A 1 O9 O 0.6876(10) 0.4532(7) 0.4349(2) 0.043(2) Uani 1 1 d U A 1 O10 O 0.4418(8) 0.1414(7) 0.2940(2) 0.0345(16) Uani 1 1 d U A 1 O11 O 0.8588(8) 0.2689(6) 0.3389(2) 0.0356(17) Uani 1 1 d U A 1 O12 O 0.6235(9) 0.3515(7) 0.2450(2) 0.0412(18) Uani 1 1 d U A 1 Os1' Os 0.5329(14) 0.3074(13) 0.3666(3) 0.051(4) Uani 0.10 1 d P B 2 Os2' Os 0.3136(15) 0.1972(14) 0.4144(3) 0.057(5) Uani 0.10 1 d P B 2 Os3' Os 0.5975(15) 0.0829(13) 0.4094(3) 0.065(5) Uani 0.10 1 d P B 2 C99 C 1.042(4) 0.385(3) 0.5197(12) 0.190(13) Uani 1 1 d U . . H99A H 1.0735 0.3822 0.4926 0.227 Uiso 1 1 calc R . . H99B H 1.1220 0.4349 0.5338 0.227 Uiso 1 1 calc R . . C98 C 0.953(3) 0.490(4) 0.5113(7) 0.143(10) Uani 1 1 d U . . H98A H 0.8517 0.4729 0.4990 0.171 Uiso 1 1 calc R . . H98B H 0.9512 0.5500 0.5332 0.171 Uiso 1 1 calc R . . C97 C 1.116(3) 0.275(2) 0.5297(9) 0.170(14) Uani 1 1 d U . . H97A H 1.1402 0.2725 0.5581 0.256 Uiso 1 1 calc R . . H97B H 1.2079 0.2701 0.5162 0.256 Uiso 1 1 calc R . . H97C H 1.0503 0.2054 0.5218 0.256 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 Os1 0.0223(3) 0.0225(5) 0.0215(5) 0.0014(3) 0.0020(3) 0.0002(3) Os2 0.0213(3) 0.0181(4) 0.0215(4) 0.0046(3) 0.0001(2) 0.0014(2) Os3 0.0206(3) 0.0161(4) 0.0175(4) 0.0025(3) -0.0002(2) -0.0016(3) Fe1 0.0257(7) 0.0198(6) 0.0236(6) 0.0029(5) 0.0002(5) -0.0008(5) P1 0.0249(12) 0.0225(11) 0.0194(10) 0.0029(9) -0.0022(9) 0.0004(9) C1 0.023(5) 0.038(6) 0.032(5) 0.001(4) 0.001(4) 0.001(4) C2 0.036(6) 0.037(6) 0.042(6) -0.009(5) -0.014(5) -0.001(4) C3 0.041(6) 0.043(6) 0.019(4) -0.004(4) 0.000(4) -0.014(5) C4 0.040(6) 0.031(5) 0.022(4) 0.005(4) -0.001(4) -0.005(4) C5 0.029(5) 0.026(5) 0.043(6) 0.005(4) 0.006(4) 0.001(4) C6 0.045(6) 0.021(5) 0.030(5) 0.005(4) -0.007(4) 0.011(4) C7 0.052(7) 0.031(5) 0.031(5) 0.005(4) -0.002(5) -0.007(5) C8 0.037(6) 0.027(5) 0.027(5) 0.001(4) -0.004(4) 0.017(4) C9 0.031(5) 0.017(4) 0.024(4) 0.009(3) -0.004(4) -0.008(3) C10 0.031(5) 0.019(4) 0.025(4) 0.001(3) 0.000(3) 0.003(4) C11 0.025(4) 0.021(4) 0.025(4) -0.001(4) 0.000(3) -0.005(4) C12 0.035(5) 0.026(5) 0.028(4) 0.008(4) 0.005(4) -0.003(4) C21 0.061(7) 0.037(6) 0.040(5) 0.010(4) 0.008(5) -0.025(5) C22 0.050(6) 0.020(5) 0.066(7) 0.009(5) -0.016(5) -0.003(4) C23 0.034(5) 0.031(5) 0.047(5) -0.011(4) 0.015(4) -0.004(4) C24 0.036(5) 0.028(5) 0.046(5) 0.014(4) -0.004(4) -0.007(4) C25 0.033(5) 0.024(5) 0.069(7) -0.010(5) 0.016(5) -0.008(4) C31 0.031(5) 0.021(4) 0.025(4) 0.004(3) -0.003(3) -0.002(4) C32 0.064(8) 0.036(6) 0.032(5) -0.008(4) 0.000(5) 0.020(5) C33 0.074(9) 0.032(6) 0.047(6) -0.012(5) 0.001(5) 0.020(6) C34 0.058(8) 0.029(6) 0.056(6) -0.011(5) -0.002(6) 0.011(5) C35 0.060(8) 0.021(5) 0.053(6) 0.000(4) -0.010(5) 0.007(5) C36 0.037(6) 0.030(5) 0.034(5) 0.000(4) -0.009(4) 0.001(4) C41 0.036(5) 0.029(5) 0.020(4) 0.003(3) -0.002(4) 0.009(4) C42 0.031(5) 0.034(5) 0.022(4) -0.003(4) 0.000(3) 0.004(4) C43 0.048(6) 0.038(6) 0.035(5) -0.008(4) -0.015(5) 0.005(5) C44 0.047(6) 0.054(7) 0.029(5) -0.009(4) -0.017(4) 0.014(5) C45 0.060(7) 0.055(7) 0.022(5) 0.008(5) -0.013(5) 0.007(5) C46 0.045(6) 0.045(6) 0.023(5) 0.009(4) -0.003(4) -0.001(5) O1 0.035(4) 0.041(4) 0.030(4) -0.009(3) 0.002(3) -0.010(3) O2 0.061(6) 0.058(6) 0.071(6) -0.016(5) -0.018(5) 0.029(5) O3 0.073(7) 0.056(5) 0.040(4) 0.001(4) 0.017(4) -0.022(5) O4 0.055(5) 0.042(4) 0.026(4) -0.006(3) 0.005(3) -0.013(4) O5 0.035(5) 0.064(6) 0.073(6) 0.011(5) 0.017(4) 0.013(4) O6 0.066(6) 0.036(4) 0.041(4) -0.008(3) -0.022(4) 0.001(4) O7 0.087(7) 0.049(5) 0.045(5) 0.027(4) -0.012(5) -0.026(5) O8 0.059(5) 0.034(4) 0.042(4) -0.010(3) -0.005(4) 0.009(4) O9 0.068(6) 0.033(4) 0.026(4) 0.000(3) -0.011(4) -0.012(4) O10 0.040(4) 0.035(4) 0.029(4) -0.009(3) 0.004(3) -0.002(3) O11 0.033(4) 0.026(4) 0.049(4) 0.008(3) 0.004(3) 0.003(3) O12 0.051(5) 0.043(4) 0.031(4) 0.000(3) 0.008(3) -0.007(4) Os1' 0.098(8) 0.030(5) 0.017(4) -0.011(3) -0.036(4) 0.028(4) Os2' 0.105(9) 0.039(6) 0.019(5) -0.002(4) -0.040(4) -0.007(6) Os3' 0.131(10) 0.032(6) 0.025(5) -0.001(4) -0.043(4) 0.010(5) C99 0.11(2) 0.23(3) 0.22(3) -0.05(3) -0.03(2) -0.089(18) C98 0.093(19) 0.25(3) 0.086(17) -0.03(2) -0.011(13) -0.079(17) C97 0.088(16) 0.17(2) 0.27(3) -0.17(2) 0.115(18) -0.050(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Os1 C2 1.895(11) . ? Os1 C3 1.924(10) . ? Os1 C1 1.942(10) . ? Os1 C4 1.948(10) . ? Os1 Os2 2.8686(14) . ? Os1 Os3 2.8736(13) . ? Os2 C5 1.887(11) . ? Os2 C7 1.907(10) . ? Os2 C6 1.935(10) . ? Os2 C8 1.955(10) . ? Os2 Os3 2.8924(16) . ? Os3 C10 1.924(9) . ? Os3 C9 1.931(9) . ? Os3 C11 1.970(9) . ? Os3 P1 2.322(3) . ? Os3 Fe1 2.7325(16) . ? Fe1 C12 1.756(10) . ? Fe1 C21 2.070(10) . ? Fe1 C25 2.089(10) . ? Fe1 C22 2.092(10) . ? Fe1 C23 2.109(10) . ? Fe1 C24 2.123(10) . ? Fe1 C11 2.135(9) . ? Fe1 P1 2.199(3) . ? P1 C31 1.823(10) . ? P1 C41 1.824(9) . ? C1 O1 1.146(11) . ? C2 O2 1.136(13) . ? C3 O3 1.143(12) . ? C4 O4 1.144(11) . ? C5 O5 1.139(13) . ? C6 O6 1.145(12) . ? C7 O7 1.141(12) . ? C8 O8 1.140(12) . ? C9 O9 1.155(11) . ? C10 O10 1.149(11) . ? C11 O11 1.165(11) . ? C12 O12 1.155(12) . ? C21 C22 1.393(14) . ? C21 C25 1.402(13) . ? C22 C23 1.408(13) . ? C23 C24 1.374(15) . ? C24 C25 1.393(13) . ? C31 C36 1.392(11) . ? C31 C32 1.394(11) . ? C32 C33 1.384(13) . ? C33 C34 1.380(13) . ? C34 C35 1.388(13) . ? C35 C36 1.389(13) . ? C41 C42 1.387(11) . ? C41 C46 1.398(11) . ? C42 C43 1.386(11) . ? C43 C44 1.386(12) . ? C44 C45 1.386(13) . ? C45 C46 1.384(12) . ? Os1' Os3' 2.874(18) . ? Os1' Os2' 2.910(19) . ? Os2' Os3' 2.85(2) . ? C99 C97 1.39(4) . ? C99 C98 1.40(5) . ? C98 C98 1.20(4) 3_766 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Os1 C3 99.9(5) . . ? C2 Os1 C1 90.2(4) . . ? C3 Os1 C1 92.7(4) . . ? C2 Os1 C4 90.2(4) . . ? C3 Os1 C4 90.8(4) . . ? C1 Os1 C4 176.4(4) . . ? C2 Os1 Os2 162.3(4) . . ? C3 Os1 Os2 97.8(4) . . ? C1 Os1 Os2 89.9(3) . . ? C4 Os1 Os2 88.7(3) . . ? C2 Os1 Os3 101.8(4) . . ? C3 Os1 Os3 158.3(4) . . ? C1 Os1 Os3 86.9(3) . . ? C4 Os1 Os3 89.5(3) . . ? Os2 Os1 Os3 60.49(4) . . ? C5 Os2 C7 104.7(5) . . ? C5 Os2 C6 91.0(5) . . ? C7 Os2 C6 89.1(4) . . ? C5 Os2 C8 89.6(4) . . ? C7 Os2 C8 91.4(4) . . ? C6 Os2 C8 179.1(4) . . ? C5 Os2 Os1 160.3(3) . . ? C7 Os2 Os1 94.9(4) . . ? C6 Os2 Os1 90.8(3) . . ? C8 Os2 Os1 88.4(3) . . ? C5 Os2 Os3 100.6(3) . . ? C7 Os2 Os3 154.8(4) . . ? C6 Os2 Os3 90.0(3) . . ? C8 Os2 Os3 89.3(3) . . ? Os1 Os2 Os3 59.84(4) . . ? C10 Os3 C9 175.4(4) . . ? C10 Os3 C11 88.7(4) . . ? C9 Os3 C11 88.3(4) . . ? C10 Os3 P1 87.3(3) . . ? C9 Os3 P1 96.6(3) . . ? C11 Os3 P1 100.9(3) . . ? C10 Os3 Fe1 94.3(3) . . ? C9 Os3 Fe1 86.5(3) . . ? C11 Os3 Fe1 50.9(3) . . ? P1 Os3 Fe1 50.78(7) . . ? C10 Os3 Os1 92.2(3) . . ? C9 Os3 Os1 89.2(3) . . ? C11 Os3 Os1 156.4(3) . . ? P1 Os3 Os1 102.67(8) . . ? Fe1 Os3 Os1 152.18(6) . . ? C10 Os3 Os2 88.7(3) . . ? C9 Os3 Os2 88.2(2) . . ? C11 Os3 Os2 96.8(3) . . ? P1 Os3 Os2 161.74(7) . . ? Fe1 Os3 Os2 147.41(5) . . ? Os1 Os3 Os2 59.67(3) . . ? C12 Fe1 C21 89.3(4) . . ? C12 Fe1 C25 102.0(4) . . ? C21 Fe1 C25 39.4(4) . . ? C12 Fe1 C22 114.4(4) . . ? C21 Fe1 C22 39.1(4) . . ? C25 Fe1 C22 65.7(5) . . ? C12 Fe1 C23 152.8(4) . . ? C21 Fe1 C23 65.1(4) . . ? C25 Fe1 C23 64.7(4) . . ? C22 Fe1 C23 39.1(4) . . ? C12 Fe1 C24 139.6(5) . . ? C21 Fe1 C24 64.9(4) . . ? C25 Fe1 C24 38.6(4) . . ? C22 Fe1 C24 64.8(4) . . ? C23 Fe1 C24 37.9(4) . . ? C12 Fe1 C11 85.4(4) . . ? C21 Fe1 C11 129.5(4) . . ? C25 Fe1 C11 93.1(4) . . ? C22 Fe1 C11 152.9(4) . . ? C23 Fe1 C11 117.6(4) . . ? C24 Fe1 C11 88.1(4) . . ? C12 Fe1 P1 95.9(3) . . ? C21 Fe1 P1 130.6(3) . . ? C25 Fe1 P1 158.7(3) . . ? C22 Fe1 P1 96.4(4) . . ? C23 Fe1 P1 94.2(3) . . ? C24 Fe1 P1 124.5(3) . . ? C11 Fe1 P1 99.9(3) . . ? C12 Fe1 Os3 97.6(3) . . ? C21 Fe1 Os3 170.7(3) . . ? C25 Fe1 Os3 132.3(3) . . ? C22 Fe1 Os3 139.8(4) . . ? C23 Fe1 Os3 108.8(3) . . ? C24 Fe1 Os3 105.9(3) . . ? C11 Fe1 Os3 45.7(3) . . ? P1 Fe1 Os3 54.91(7) . . ? C31 P1 C41 102.1(4) . . ? C31 P1 Fe1 120.7(3) . . ? C41 P1 Fe1 116.2(3) . . ? C31 P1 Os3 121.9(3) . . ? C41 P1 Os3 121.2(3) . . ? Fe1 P1 Os3 74.32(8) . . ? O1 C1 Os1 174.8(9) . . ? O2 C2 Os1 179.2(10) . . ? O3 C3 Os1 179.4(10) . . ? O4 C4 Os1 173.7(10) . . ? O5 C5 Os2 176.2(10) . . ? O6 C6 Os2 174.9(9) . . ? O7 C7 Os2 179.0(12) . . ? O8 C8 Os2 173.5(8) . . ? O9 C9 Os3 175.5(9) . . ? O10 C10 Os3 175.6(9) . . ? O11 C11 Os3 149.2(8) . . ? O11 C11 Fe1 127.4(7) . . ? Os3 C11 Fe1 83.4(4) . . ? O12 C12 Fe1 177.6(10) . . ? C22 C21 C25 108.6(10) . . ? C22 C21 Fe1 71.3(6) . . ? C25 C21 Fe1 71.1(6) . . ? C21 C22 C23 106.8(9) . . ? C21 C22 Fe1 69.6(6) . . ? C23 C22 Fe1 71.1(5) . . ? C24 C23 C22 108.6(9) . . ? C24 C23 Fe1 71.6(6) . . ? C22 C23 Fe1 69.8(6) . . ? C23 C24 C25 108.6(8) . . ? C23 C24 Fe1 70.5(6) . . ? C25 C24 Fe1 69.4(6) . . ? C24 C25 C21 107.3(9) . . ? C24 C25 Fe1 72.0(6) . . ? C21 C25 Fe1 69.5(6) . . ? C36 C31 C32 117.7(9) . . ? C36 C31 P1 121.3(7) . . ? C32 C31 P1 121.0(7) . . ? C33 C32 C31 121.9(10) . . ? C34 C33 C32 119.9(10) . . ? C33 C34 C35 119.1(11) . . ? C34 C35 C36 120.9(10) . . ? C35 C36 C31 120.5(9) . . ? C42 C41 C46 119.9(9) . . ? C42 C41 P1 120.9(6) . . ? C46 C41 P1 119.1(7) . . ? C43 C42 C41 119.8(9) . . ? C44 C43 C42 120.6(10) . . ? C43 C44 C45 119.5(10) . . ? C46 C45 C44 120.5(10) . . ? C45 C46 C41 119.7(10) . . ? Os3' Os1' Os2' 58.9(5) . . ? Os3' Os2' Os1' 59.9(5) . . ? Os2' Os3' Os1' 61.2(5) . . ? C97 C99 C98 173(4) . . ? C98 C98 C99 82(4) 3_766 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2 Os1 Os2 C5 -9.2(14) . . . . ? C3 Os1 Os2 C5 173.6(10) . . . . ? C1 Os1 Os2 C5 80.9(10) . . . . ? C4 Os1 Os2 C5 -95.8(10) . . . . ? Os3 Os1 Os2 C5 -5.6(10) . . . . ? C2 Os1 Os2 C7 175.1(11) . . . . ? C3 Os1 Os2 C7 -2.1(4) . . . . ? C1 Os1 Os2 C7 -94.8(4) . . . . ? C4 Os1 Os2 C7 88.5(4) . . . . ? Os3 Os1 Os2 C7 178.6(3) . . . . ? C2 Os1 Os2 C6 85.9(11) . . . . ? C3 Os1 Os2 C6 -91.2(4) . . . . ? C1 Os1 Os2 C6 176.0(4) . . . . ? C4 Os1 Os2 C6 -0.6(4) . . . . ? Os3 Os1 Os2 C6 89.5(3) . . . . ? C2 Os1 Os2 C8 -93.6(11) . . . . ? C3 Os1 Os2 C8 89.2(4) . . . . ? C1 Os1 Os2 C8 -3.5(4) . . . . ? C4 Os1 Os2 C8 179.8(4) . . . . ? Os3 Os1 Os2 C8 -90.1(3) . . . . ? C2 Os1 Os2 Os3 -3.6(10) . . . . ? C3 Os1 Os2 Os3 179.3(3) . . . . ? C1 Os1 Os2 Os3 86.6(3) . . . . ? C4 Os1 Os2 Os3 -90.1(3) . . . . ? C2 Os1 Os3 C10 -93.9(4) . . . . ? C3 Os1 Os3 C10 85.3(8) . . . . ? C1 Os1 Os3 C10 -4.3(4) . . . . ? C4 Os1 Os3 C10 176.0(4) . . . . ? Os2 Os1 Os3 C10 87.2(3) . . . . ? C2 Os1 Os3 C9 90.5(4) . . . . ? C3 Os1 Os3 C9 -90.4(8) . . . . ? C1 Os1 Os3 C9 -180.0(4) . . . . ? C4 Os1 Os3 C9 0.4(4) . . . . ? Os2 Os1 Os3 C9 -88.4(3) . . . . ? C2 Os1 Os3 C11 174.5(7) . . . . ? C3 Os1 Os3 C11 -6.3(10) . . . . ? C1 Os1 Os3 C11 -95.9(7) . . . . ? C4 Os1 Os3 C11 84.4(7) . . . . ? Os2 Os1 Os3 C11 -4.4(6) . . . . ? C2 Os1 Os3 P1 -6.1(3) . . . . ? C3 Os1 Os3 P1 173.0(8) . . . . ? C1 Os1 Os3 P1 83.4(3) . . . . ? C4 Os1 Os3 P1 -96.2(3) . . . . ? Os2 Os1 Os3 P1 174.97(8) . . . . ? C2 Os1 Os3 Fe1 9.6(3) . . . . ? C3 Os1 Os3 Fe1 -171.3(8) . . . . ? C1 Os1 Os3 Fe1 99.1(3) . . . . ? C4 Os1 Os3 Fe1 -80.5(3) . . . . ? Os2 Os1 Os3 Fe1 -169.32(12) . . . . ? C2 Os1 Os3 Os2 178.9(3) . . . . ? C3 Os1 Os3 Os2 -2.0(8) . . . . ? C1 Os1 Os3 Os2 -91.6(3) . . . . ? C4 Os1 Os3 Os2 88.8(3) . . . . ? C5 Os2 Os3 C10 84.8(4) . . . . ? C7 Os2 Os3 C10 -96.4(8) . . . . ? C6 Os2 Os3 C10 175.8(4) . . . . ? C8 Os2 Os3 C10 -4.7(4) . . . . ? Os1 Os2 Os3 C10 -93.3(3) . . . . ? C5 Os2 Os3 C9 -91.8(4) . . . . ? C7 Os2 Os3 C9 87.0(8) . . . . ? C6 Os2 Os3 C9 -0.8(5) . . . . ? C8 Os2 Os3 C9 178.7(4) . . . . ? Os1 Os2 Os3 C9 90.1(3) . . . . ? C5 Os2 Os3 C11 -3.7(4) . . . . ? C7 Os2 Os3 C11 175.1(8) . . . . ? C6 Os2 Os3 C11 87.3(4) . . . . ? C8 Os2 Os3 C11 -93.2(4) . . . . ? Os1 Os2 Os3 C11 178.2(3) . . . . ? C5 Os2 Os3 P1 162.2(4) . . . . ? C7 Os2 Os3 P1 -19.0(8) . . . . ? C6 Os2 Os3 P1 -106.8(4) . . . . ? C8 Os2 Os3 P1 72.8(4) . . . . ? Os1 Os2 Os3 P1 -15.8(2) . . . . ? C5 Os2 Os3 Fe1 -11.2(3) . . . . ? C7 Os2 Os3 Fe1 167.6(7) . . . . ? C6 Os2 Os3 Fe1 79.8(4) . . . . ? C8 Os2 Os3 Fe1 -100.6(3) . . . . ? Os1 Os2 Os3 Fe1 170.76(11) . . . . ? C5 Os2 Os3 Os1 178.1(3) . . . . ? C7 Os2 Os3 Os1 -3.2(7) . . . . ? C6 Os2 Os3 Os1 -90.9(3) . . . . ? C8 Os2 Os3 Os1 88.6(3) . . . . ? C10 Os3 Fe1 C12 -8.9(4) . . . . ? C9 Os3 Fe1 C12 166.6(5) . . . . ? C11 Os3 Fe1 C12 75.9(5) . . . . ? P1 Os3 Fe1 C12 -91.9(4) . . . . ? Os1 Os3 Fe1 C12 -111.8(4) . . . . ? Os2 Os3 Fe1 C12 85.5(4) . . . . ? C10 Os3 Fe1 C21 -148(2) . . . . ? C9 Os3 Fe1 C21 28(2) . . . . ? C11 Os3 Fe1 C21 -63(2) . . . . ? P1 Os3 Fe1 C21 129(2) . . . . ? Os1 Os3 Fe1 C21 110(2) . . . . ? Os2 Os3 Fe1 C21 -53(2) . . . . ? C10 Os3 Fe1 C25 -122.8(5) . . . . ? C9 Os3 Fe1 C25 52.7(5) . . . . ? C11 Os3 Fe1 C25 -38.0(5) . . . . ? P1 Os3 Fe1 C25 154.2(4) . . . . ? Os1 Os3 Fe1 C25 134.3(4) . . . . ? Os2 Os3 Fe1 C25 -28.4(4) . . . . ? C10 Os3 Fe1 C22 134.7(5) . . . . ? C9 Os3 Fe1 C22 -49.9(6) . . . . ? C11 Os3 Fe1 C22 -140.6(6) . . . . ? P1 Os3 Fe1 C22 51.7(5) . . . . ? Os1 Os3 Fe1 C22 31.7(5) . . . . ? Os2 Os3 Fe1 C22 -131.0(5) . . . . ? C10 Os3 Fe1 C23 164.7(4) . . . . ? C9 Os3 Fe1 C23 -19.9(4) . . . . ? C11 Os3 Fe1 C23 -110.6(4) . . . . ? P1 Os3 Fe1 C23 81.7(3) . . . . ? Os1 Os3 Fe1 C23 61.7(3) . . . . ? Os2 Os3 Fe1 C23 -101.0(3) . . . . ? C10 Os3 Fe1 C24 -155.7(4) . . . . ? C9 Os3 Fe1 C24 19.8(4) . . . . ? C11 Os3 Fe1 C24 -70.9(5) . . . . ? P1 Os3 Fe1 C24 121.3(3) . . . . ? Os1 Os3 Fe1 C24 101.4(3) . . . . ? Os2 Os3 Fe1 C24 -61.3(3) . . . . ? C10 Os3 Fe1 C11 -84.8(4) . . . . ? C9 Os3 Fe1 C11 90.7(4) . . . . ? P1 Os3 Fe1 C11 -167.7(3) . . . . ? Os1 Os3 Fe1 C11 172.3(3) . . . . ? Os2 Os3 Fe1 C11 9.6(3) . . . . ? C10 Os3 Fe1 P1 83.0(3) . . . . ? C9 Os3 Fe1 P1 -101.5(3) . . . . ? C11 Os3 Fe1 P1 167.7(3) . . . . ? Os1 Os3 Fe1 P1 -19.93(14) . . . . ? Os2 Os3 Fe1 P1 177.33(13) . . . . ? C12 Fe1 P1 C31 -146.6(4) . . . . ? C21 Fe1 P1 C31 -52.4(5) . . . . ? C25 Fe1 P1 C31 0.5(10) . . . . ? C22 Fe1 P1 C31 -31.2(4) . . . . ? C23 Fe1 P1 C31 8.0(4) . . . . ? C24 Fe1 P1 C31 32.5(5) . . . . ? C11 Fe1 P1 C31 127.0(4) . . . . ? Os3 Fe1 P1 C31 118.1(3) . . . . ? C12 Fe1 P1 C41 -22.3(5) . . . . ? C21 Fe1 P1 C41 71.9(5) . . . . ? C25 Fe1 P1 C41 124.8(10) . . . . ? C22 Fe1 P1 C41 93.1(4) . . . . ? C23 Fe1 P1 C41 132.4(4) . . . . ? C24 Fe1 P1 C41 156.9(4) . . . . ? C11 Fe1 P1 C41 -108.6(4) . . . . ? Os3 Fe1 P1 C41 -117.5(3) . . . . ? C12 Fe1 P1 Os3 95.2(3) . . . . ? C21 Fe1 P1 Os3 -170.6(4) . . . . ? C25 Fe1 P1 Os3 -117.7(9) . . . . ? C22 Fe1 P1 Os3 -149.4(3) . . . . ? C23 Fe1 P1 Os3 -110.1(3) . . . . ? C24 Fe1 P1 Os3 -85.6(3) . . . . ? C11 Fe1 P1 Os3 8.9(2) . . . . ? C10 Os3 P1 C31 145.6(5) . . . . ? C9 Os3 P1 C31 -36.8(5) . . . . ? C11 Os3 P1 C31 -126.3(4) . . . . ? Fe1 Os3 P1 C31 -116.7(4) . . . . ? Os1 Os3 P1 C31 53.9(4) . . . . ? Os2 Os3 P1 C31 67.9(5) . . . . ? C10 Os3 P1 C41 13.7(4) . . . . ? C9 Os3 P1 C41 -168.6(4) . . . . ? C11 Os3 P1 C41 101.8(4) . . . . ? Fe1 Os3 P1 C41 111.5(4) . . . . ? Os1 Os3 P1 C41 -77.9(3) . . . . ? Os2 Os3 P1 C41 -63.9(4) . . . . ? C10 Os3 P1 Fe1 -97.8(3) . . . . ? C9 Os3 P1 Fe1 79.9(3) . . . . ? C11 Os3 P1 Fe1 -9.7(3) . . . . ? Os1 Os3 P1 Fe1 170.61(7) . . . . ? Os2 Os3 P1 Fe1 -175.4(2) . . . . ? C2 Os1 C1 O1 -28(10) . . . . ? C3 Os1 C1 O1 71(10) . . . . ? C4 Os1 C1 O1 -125(10) . . . . ? Os2 Os1 C1 O1 169(10) . . . . ? Os3 Os1 C1 O1 -130(10) . . . . ? C3 Os1 C2 O2 68(100) . . . . ? C1 Os1 C2 O2 161(100) . . . . ? C4 Os1 C2 O2 -23(100) . . . . ? Os2 Os1 C2 O2 -109(100) . . . . ? Os3 Os1 C2 O2 -112(100) . . . . ? C2 Os1 C3 O3 63(100) . . . . ? C1 Os1 C3 O3 -28(100) . . . . ? C4 Os1 C3 O3 153(100) . . . . ? Os2 Os1 C3 O3 -118(100) . . . . ? Os3 Os1 C3 O3 -116(100) . . . . ? C2 Os1 C4 O4 16(8) . . . . ? C3 Os1 C4 O4 -83(8) . . . . ? C1 Os1 C4 O4 113(9) . . . . ? Os2 Os1 C4 O4 179(100) . . . . ? Os3 Os1 C4 O4 118(8) . . . . ? C7 Os2 C5 O5 -31(15) . . . . ? C6 Os2 C5 O5 59(15) . . . . ? C8 Os2 C5 O5 -122(15) . . . . ? Os1 Os2 C5 O5 154(15) . . . . ? Os3 Os2 C5 O5 149(15) . . . . ? C5 Os2 C6 O6 -41(11) . . . . ? C7 Os2 C6 O6 63(11) . . . . ? C8 Os2 C6 O6 -172(100) . . . . ? Os1 Os2 C6 O6 158(11) . . . . ? Os3 Os2 C6 O6 -142(11) . . . . ? C5 Os2 C7 O7 144(67) . . . . ? C6 Os2 C7 O7 53(67) . . . . ? C8 Os2 C7 O7 -126(67) . . . . ? Os1 Os2 C7 O7 -38(67) . . . . ? Os3 Os2 C7 O7 -35(67) . . . . ? C5 Os2 C8 O8 51(9) . . . . ? C7 Os2 C8 O8 -54(9) . . . . ? C6 Os2 C8 O8 -179(100) . . . . ? Os1 Os2 C8 O8 -149(9) . . . . ? Os3 Os2 C8 O8 151(9) . . . . ? C10 Os3 C9 O9 67(12) . . . . ? C11 Os3 C9 O9 19(10) . . . . ? P1 Os3 C9 O9 -82(10) . . . . ? Fe1 Os3 C9 O9 -32(10) . . . . ? Os1 Os3 C9 O9 175(10) . . . . ? Os2 Os3 C9 O9 115(10) . . . . ? C9 Os3 C10 O10 -74(12) . . . . ? C11 Os3 C10 O10 -25(11) . . . . ? P1 Os3 C10 O10 76(11) . . . . ? Fe1 Os3 C10 O10 26(11) . . . . ? Os1 Os3 C10 O10 179(100) . . . . ? Os2 Os3 C10 O10 -122(11) . . . . ? C10 Os3 C11 O11 -83.1(15) . . . . ? C9 Os3 C11 O11 93.5(15) . . . . ? P1 Os3 C11 O11 -170.1(14) . . . . ? Fe1 Os3 C11 O11 -180(100) . . . . ? Os1 Os3 C11 O11 9(2) . . . . ? Os2 Os3 C11 O11 5.5(15) . . . . ? C10 Os3 C11 Fe1 96.6(3) . . . . ? C9 Os3 C11 Fe1 -86.8(3) . . . . ? P1 Os3 C11 Fe1 9.6(3) . . . . ? Os1 Os3 C11 Fe1 -171.0(4) . . . . ? Os2 Os3 C11 Fe1 -174.81(18) . . . . ? C12 Fe1 C11 O11 74.5(9) . . . . ? C21 Fe1 C11 O11 -10.9(11) . . . . ? C25 Fe1 C11 O11 -27.3(9) . . . . ? C22 Fe1 C11 O11 -64.2(14) . . . . ? C23 Fe1 C11 O11 -90.3(9) . . . . ? C24 Fe1 C11 O11 -65.6(9) . . . . ? P1 Fe1 C11 O11 169.7(8) . . . . ? Os3 Fe1 C11 O11 179.8(11) . . . . ? C12 Fe1 C11 Os3 -105.4(4) . . . . ? C21 Fe1 C11 Os3 169.3(4) . . . . ? C25 Fe1 C11 Os3 152.9(4) . . . . ? C22 Fe1 C11 Os3 115.9(9) . . . . ? C23 Fe1 C11 Os3 89.9(4) . . . . ? C24 Fe1 C11 Os3 114.6(4) . . . . ? P1 Fe1 C11 Os3 -10.2(3) . . . . ? C21 Fe1 C12 O12 60(21) . . . . ? C25 Fe1 C12 O12 22(21) . . . . ? C22 Fe1 C12 O12 91(21) . . . . ? C23 Fe1 C12 O12 79(21) . . . . ? C24 Fe1 C12 O12 12(21) . . . . ? C11 Fe1 C12 O12 -70(21) . . . . ? P1 Fe1 C12 O12 -169(21) . . . . ? Os3 Fe1 C12 O12 -114(21) . . . . ? C12 Fe1 C21 C22 131.9(7) . . . . ? C25 Fe1 C21 C22 -118.2(10) . . . . ? C23 Fe1 C21 C22 -38.3(6) . . . . ? C24 Fe1 C21 C22 -80.3(7) . . . . ? C11 Fe1 C21 C22 -144.6(6) . . . . ? P1 Fe1 C21 C22 34.7(8) . . . . ? Os3 Fe1 C21 C22 -89(2) . . . . ? C12 Fe1 C21 C25 -109.9(7) . . . . ? C22 Fe1 C21 C25 118.2(10) . . . . ? C23 Fe1 C21 C25 79.8(7) . . . . ? C24 Fe1 C21 C25 37.9(6) . . . . ? C11 Fe1 C21 C25 -26.4(8) . . . . ? P1 Fe1 C21 C25 152.9(5) . . . . ? Os3 Fe1 C21 C25 29(2) . . . . ? C25 C21 C22 C23 0.0(10) . . . . ? Fe1 C21 C22 C23 61.7(6) . . . . ? C25 C21 C22 Fe1 -61.6(7) . . . . ? C12 Fe1 C22 C21 -54.7(8) . . . . ? C25 Fe1 C22 C21 37.9(6) . . . . ? C23 Fe1 C22 C21 117.0(9) . . . . ? C24 Fe1 C22 C21 80.5(7) . . . . ? C11 Fe1 C22 C21 79.0(12) . . . . ? P1 Fe1 C22 C21 -154.2(6) . . . . ? Os3 Fe1 C22 C21 165.6(5) . . . . ? C12 Fe1 C22 C23 -171.8(6) . . . . ? C21 Fe1 C22 C23 -117.0(9) . . . . ? C25 Fe1 C22 C23 -79.2(7) . . . . ? C24 Fe1 C22 C23 -36.5(6) . . . . ? C11 Fe1 C22 C23 -38.0(13) . . . . ? P1 Fe1 C22 C23 88.8(6) . . . . ? Os3 Fe1 C22 C23 48.5(8) . . . . ? C21 C22 C23 C24 0.7(10) . . . . ? Fe1 C22 C23 C24 61.4(7) . . . . ? C21 C22 C23 Fe1 -60.7(6) . . . . ? C12 Fe1 C23 C24 -102.2(11) . . . . ? C21 Fe1 C23 C24 -80.5(6) . . . . ? C25 Fe1 C23 C24 -36.8(6) . . . . ? C22 Fe1 C23 C24 -118.8(8) . . . . ? C11 Fe1 C23 C24 42.8(7) . . . . ? P1 Fe1 C23 C24 146.2(5) . . . . ? Os3 Fe1 C23 C24 91.9(5) . . . . ? C12 Fe1 C23 C22 16.5(13) . . . . ? C21 Fe1 C23 C22 38.3(6) . . . . ? C25 Fe1 C23 C22 81.9(7) . . . . ? C24 Fe1 C23 C22 118.8(8) . . . . ? C11 Fe1 C23 C22 161.5(7) . . . . ? P1 Fe1 C23 C22 -95.0(6) . . . . ? Os3 Fe1 C23 C22 -149.3(6) . . . . ? C22 C23 C24 C25 -1.1(11) . . . . ? Fe1 C23 C24 C25 59.1(7) . . . . ? C22 C23 C24 Fe1 -60.2(7) . . . . ? C12 Fe1 C24 C23 136.4(7) . . . . ? C21 Fe1 C24 C23 81.1(6) . . . . ? C25 Fe1 C24 C23 119.7(8) . . . . ? C22 Fe1 C24 C23 37.7(6) . . . . ? C11 Fe1 C24 C23 -143.0(6) . . . . ? P1 Fe1 C24 C23 -42.3(6) . . . . ? Os3 Fe1 C24 C23 -100.4(5) . . . . ? C12 Fe1 C24 C25 16.7(9) . . . . ? C21 Fe1 C24 C25 -38.6(6) . . . . ? C22 Fe1 C24 C25 -82.0(7) . . . . ? C23 Fe1 C24 C25 -119.7(8) . . . . ? C11 Fe1 C24 C25 97.3(6) . . . . ? P1 Fe1 C24 C25 -162.0(5) . . . . ? Os3 Fe1 C24 C25 139.9(6) . . . . ? C23 C24 C25 C21 1.1(12) . . . . ? Fe1 C24 C25 C21 60.9(7) . . . . ? C23 C24 C25 Fe1 -59.8(7) . . . . ? C22 C21 C25 C24 -0.7(11) . . . . ? Fe1 C21 C25 C24 -62.5(7) . . . . ? C22 C21 C25 Fe1 61.8(7) . . . . ? C12 Fe1 C25 C24 -169.0(6) . . . . ? C21 Fe1 C25 C24 117.0(9) . . . . ? C22 Fe1 C25 C24 79.4(6) . . . . ? C23 Fe1 C25 C24 36.2(6) . . . . ? C11 Fe1 C25 C24 -83.1(6) . . . . ? P1 Fe1 C25 C24 44.5(13) . . . . ? Os3 Fe1 C25 C24 -56.9(7) . . . . ? C12 Fe1 C25 C21 74.0(7) . . . . ? C22 Fe1 C25 C21 -37.6(6) . . . . ? C23 Fe1 C25 C21 -80.9(7) . . . . ? C24 Fe1 C25 C21 -117.0(9) . . . . ? C11 Fe1 C25 C21 159.9(7) . . . . ? P1 Fe1 C25 C21 -72.5(12) . . . . ? Os3 Fe1 C25 C21 -173.9(5) . . . . ? C41 P1 C31 C36 -27.6(9) . . . . ? Fe1 P1 C31 C36 103.2(8) . . . . ? Os3 P1 C31 C36 -166.9(7) . . . . ? C41 P1 C31 C32 153.0(7) . . . . ? Fe1 P1 C31 C32 -76.2(8) . . . . ? Os3 P1 C31 C32 13.8(9) . . . . ? C36 C31 C32 C33 0.4(12) . . . . ? P1 C31 C32 C33 179.8(8) . . . . ? C31 C32 C33 C34 2.2(14) . . . . ? C32 C33 C34 C35 -3.4(18) . . . . ? C33 C34 C35 C36 2.1(19) . . . . ? C34 C35 C36 C31 0.5(18) . . . . ? C32 C31 C36 C35 -1.7(15) . . . . ? P1 C31 C36 C35 178.9(9) . . . . ? C31 P1 C41 C42 -86.9(7) . . . . ? Fe1 P1 C41 C42 139.7(6) . . . . ? Os3 P1 C41 C42 52.8(8) . . . . ? C31 P1 C41 C46 88.9(8) . . . . ? Fe1 P1 C41 C46 -44.5(9) . . . . ? Os3 P1 C41 C46 -131.4(7) . . . . ? C46 C41 C42 C43 -0.1(12) . . . . ? P1 C41 C42 C43 175.7(7) . . . . ? C41 C42 C43 C44 -0.8(12) . . . . ? C42 C43 C44 C45 2.2(16) . . . . ? C43 C44 C45 C46 -2.7(18) . . . . ? C44 C45 C46 C41 1.8(18) . . . . ? C42 C41 C46 C45 -0.4(15) . . . . ? P1 C41 C46 C45 -176.2(9) . . . . ? C97 C99 C98 C98 -159(33) . . . 3_766 ? _diffrn_measured_fraction_theta_max 0.892 _diffrn_reflns_theta_full 29.00 _diffrn_measured_fraction_theta_full 0.913 _refine_diff_density_max 1.689 _refine_diff_density_min -3.395 _refine_diff_density_rms 0.246 #===END data_for_complex_10 _database_code_CSD 197613 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H25 Au O10 Os3 P2' _chemical_formula_weight 1495.11 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' Au Au -2.0133 8.8022 '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' Os Os -1.2165 7.6030 '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' _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 10.0320(2) _cell_length_b 13.9040(2) _cell_length_c 16.4300(4) _cell_angle_alpha 94.6710(10) _cell_angle_beta 103.7790(10) _cell_angle_gamma 111.1270(10) _cell_volume 2040.47(7) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Orange _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.433 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1364 _exptl_absorpt_coefficient_mu 13.028 _exptl_absorpt_correction_type SORTAV _exptl_absorpt_correction_T_min 0.1213 _exptl_absorpt_correction_T_max 0.4624 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Nonius Kappa CCD Diffractometer' _diffrn_measurement_method 'Combined 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 26465 _diffrn_reflns_av_R_equivalents 0.0666 _diffrn_reflns_av_sigmaI/netI 0.0468 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.40 _diffrn_reflns_theta_max 26.37 _reflns_number_total 8336 _reflns_number_gt 7673 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Nonius control software' _computing_cell_refinement DENZO _computing_data_reduction DENZO _computing_structure_solution 'SHELXS-93 (Sheldrick, 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1991)' _computing_publication_material 'SHELXL-97 (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^)+(0.0525P)^2^+1.4713P] 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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00106(11) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 8336 _refine_ls_number_parameters 506 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0368 _refine_ls_R_factor_gt 0.0333 _refine_ls_wR_factor_ref 0.0880 _refine_ls_wR_factor_gt 0.0857 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _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 Os1 Os 0.25475(2) 0.263620(15) 0.226222(13) 0.01990(8) Uani 1 1 d . . . Os2 Os 0.46405(2) 0.160680(15) 0.218152(13) 0.02043(8) Uani 1 1 d . . . Os3 Os 0.41296(2) 0.294339(18) 0.098130(14) 0.02704(8) Uani 1 1 d . . . Au1 Au 0.17578(2) 0.049517(15) 0.226240(13) 0.02279(8) Uani 1 1 d . . . P2 P 0.02695(15) -0.11237(10) 0.24653(9) 0.0218(3) Uani 1 1 d . . . P1 P 0.48597(15) 0.29381(10) 0.32578(9) 0.0205(3) Uani 1 1 d . . . C11 C 0.1541(7) 0.2505(5) 0.3116(4) 0.0323(13) Uani 1 1 d . . . O11 O 0.0902(6) 0.2494(4) 0.3612(3) 0.0510(13) Uani 1 1 d . . . C12 C 0.2805(7) 0.4040(5) 0.2200(4) 0.0321(13) Uani 1 1 d . . . O12 O 0.2941(6) 0.4893(4) 0.2171(4) 0.0509(13) Uani 1 1 d . . . C13 C 0.0676(7) 0.1982(5) 0.1362(4) 0.0291(13) Uani 1 1 d . . . O13 O -0.0454(5) 0.1624(4) 0.0865(3) 0.0443(12) Uani 1 1 d . . . C21 C 0.6651(7) 0.2102(5) 0.2126(4) 0.0349(14) Uani 1 1 d . . . O21 O 0.7835(5) 0.2368(5) 0.2096(3) 0.0548(14) Uani 1 1 d . . . C22 C 0.4859(6) 0.0671(4) 0.2940(4) 0.0280(12) Uani 1 1 d . . . O22 O 0.5057(5) 0.0097(3) 0.3368(3) 0.0383(10) Uani 1 1 d . . . C23 C 0.3862(6) 0.0512(5) 0.1172(4) 0.0302(13) Uani 1 1 d . . . O23 O 0.3481(5) -0.0142(4) 0.0600(3) 0.0400(11) Uani 1 1 d . . . C31 C 0.3416(8) 0.3822(6) 0.0310(5) 0.0446(17) Uani 1 1 d . . . O31 O 0.3042(7) 0.4348(5) -0.0094(4) 0.078(2) Uani 1 1 d . . . C32 C 0.5493(8) 0.2726(7) 0.0424(5) 0.0501(19) Uani 1 1 d . . . O32 O 0.6350(7) 0.2608(7) 0.0131(4) 0.094(3) Uani 1 1 d . . . C33 C 0.5769(7) 0.4221(5) 0.1685(4) 0.0380(15) Uani 1 1 d . . . O33 O 0.6705(6) 0.5004(4) 0.1976(3) 0.0592(15) Uani 1 1 d . . . C34 C 0.2437(7) 0.1694(5) 0.0304(4) 0.0325(13) Uani 1 1 d . . . O34 O 0.1443(5) 0.0979(4) -0.0124(3) 0.0407(11) Uani 1 1 d . . . C201 C -0.1710(6) -0.1408(4) 0.2150(3) 0.0260(12) Uani 1 1 d . . . C202 C -0.2769(7) -0.2409(5) 0.2104(4) 0.0368(15) Uani 1 1 d . . . H202 H -0.2464 -0.2970 0.2213 0.044 Uiso 1 1 calc R . . C203 C -0.4282(7) -0.2580(6) 0.1898(5) 0.0473(18) Uani 1 1 d . . . H203 H -0.5008 -0.3259 0.1865 0.057 Uiso 1 1 calc R . . C204 C -0.4709(7) -0.1789(7) 0.1746(4) 0.0479(19) Uani 1 1 d . . . H204 H -0.5740 -0.1916 0.1604 0.057 Uiso 1 1 calc R . . C205 C -0.3679(8) -0.0788(7) 0.1792(5) 0.053(2) Uani 1 1 d . . . H205 H -0.3997 -0.0233 0.1684 0.064 Uiso 1 1 calc R . . C206 C -0.2188(7) -0.0611(5) 0.1997(4) 0.0379(15) Uani 1 1 d . . . H206 H -0.1475 0.0075 0.2034 0.045 Uiso 1 1 calc R . . C211 C 0.0469(6) -0.2235(4) 0.1930(4) 0.0246(11) Uani 1 1 d . . . C212 C 0.0271(7) -0.3157(5) 0.2256(4) 0.0342(14) Uani 1 1 d . . . H212 H 0.0037 -0.3213 0.2782 0.041 Uiso 1 1 calc R . . C213 C 0.0413(8) -0.3984(5) 0.1823(5) 0.0452(17) Uani 1 1 d . . . H213 H 0.0270 -0.4609 0.2049 0.054 Uiso 1 1 calc R . . C214 C 0.0757(8) -0.3916(6) 0.1066(5) 0.0439(17) Uani 1 1 d . . . H214 H 0.0877 -0.4487 0.0779 0.053 Uiso 1 1 calc R . . C215 C 0.0932(7) -0.3022(6) 0.0719(4) 0.0400(15) Uani 1 1 d . . . H215 H 0.1143 -0.2989 0.0186 0.048 Uiso 1 1 calc R . . C216 C 0.0800(6) -0.2171(5) 0.1144(4) 0.0298(13) Uani 1 1 d . . . H216 H 0.0931 -0.1553 0.0908 0.036 Uiso 1 1 calc R . . C221 C 0.0714(6) -0.1224(4) 0.3586(3) 0.0222(11) Uani 1 1 d . . . C222 C -0.0196(6) -0.1160(4) 0.4095(4) 0.0263(12) Uani 1 1 d . . . H222 H -0.1105 -0.1088 0.3847 0.032 Uiso 1 1 calc R . . C223 C 0.0202(7) -0.1201(5) 0.4951(4) 0.0329(13) Uani 1 1 d . . . H223 H -0.0423 -0.1148 0.5290 0.039 Uiso 1 1 calc R . . C224 C 0.1533(6) -0.1320(4) 0.5319(4) 0.0294(12) Uani 1 1 d . . . H224 H 0.1805 -0.1359 0.5906 0.035 Uiso 1 1 calc R . . C225 C 0.2440(7) -0.1379(5) 0.4829(4) 0.0314(13) Uani 1 1 d . . . H225 H 0.3344 -0.1457 0.5079 0.038 Uiso 1 1 calc R . . C226 C 0.2048(6) -0.1327(4) 0.3969(4) 0.0293(12) Uani 1 1 d . . . H226 H 0.2692 -0.1362 0.3637 0.035 Uiso 1 1 calc R . . C101 C 0.6448(6) 0.4192(4) 0.3571(4) 0.0256(12) Uani 1 1 d . . . C102 C 0.7879(7) 0.4214(5) 0.3680(4) 0.0344(14) Uani 1 1 d . . . H102 H 0.8017 0.3586 0.3543 0.041 Uiso 1 1 calc R . . C103 C 0.9112(7) 0.5167(5) 0.3995(4) 0.0409(16) Uani 1 1 d . . . H103 H 1.0089 0.5185 0.4068 0.049 Uiso 1 1 calc R . . C104 C 0.8923(8) 0.6078(5) 0.4198(5) 0.0450(17) Uani 1 1 d . . . H104 H 0.9768 0.6722 0.4408 0.054 Uiso 1 1 calc R . . C105 C 0.7509(8) 0.6059(5) 0.4099(4) 0.0455(17) Uani 1 1 d . . . H105 H 0.7375 0.6686 0.4245 0.055 Uiso 1 1 calc R . . C106 C 0.6285(7) 0.5114(4) 0.3782(4) 0.0348(14) Uani 1 1 d . . . H106 H 0.5311 0.5103 0.3710 0.042 Uiso 1 1 calc R . . C111 C 0.4792(6) 0.2629(4) 0.4322(3) 0.0210(11) Uani 1 1 d . . . C112 C 0.3753(6) 0.1680(4) 0.4403(3) 0.0252(11) Uani 1 1 d . . . H112 H 0.3064 0.1199 0.3905 0.030 Uiso 1 1 calc R . . C113 C 0.3708(7) 0.1426(5) 0.5202(4) 0.0310(13) Uani 1 1 d . . . H113 H 0.2993 0.0776 0.5245 0.037 Uiso 1 1 calc R . . C114 C 0.4707(7) 0.2123(5) 0.5933(4) 0.0336(14) Uani 1 1 d . . . H114 H 0.4676 0.1952 0.6478 0.040 Uiso 1 1 calc R . . C115 C 0.5738(7) 0.3056(5) 0.5869(4) 0.0369(14) Uani 1 1 d . . . H115 H 0.6427 0.3531 0.6370 0.044 Uiso 1 1 calc R . . C116 C 0.5776(7) 0.3310(4) 0.5074(4) 0.0296(13) Uani 1 1 d . . . H116 H 0.6491 0.3964 0.5040 0.036 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 Os1 0.01738(12) 0.02051(12) 0.02386(13) 0.00698(9) 0.00909(9) 0.00715(9) Os2 0.01566(12) 0.02167(12) 0.02349(13) 0.00244(9) 0.00690(9) 0.00637(9) Os3 0.02223(13) 0.03509(14) 0.02557(14) 0.01140(10) 0.01189(10) 0.00884(10) Au1 0.01880(12) 0.02066(12) 0.02616(13) 0.00587(9) 0.00683(9) 0.00407(9) P2 0.0169(7) 0.0202(6) 0.0289(7) 0.0070(5) 0.0092(6) 0.0059(5) P1 0.0186(7) 0.0174(6) 0.0239(7) 0.0041(5) 0.0077(5) 0.0041(5) C11 0.028(3) 0.033(3) 0.038(3) 0.011(3) 0.010(3) 0.013(3) O11 0.049(3) 0.081(4) 0.044(3) 0.023(3) 0.038(2) 0.032(3) C12 0.025(3) 0.029(3) 0.040(3) 0.010(3) 0.007(3) 0.009(2) O12 0.058(3) 0.031(2) 0.072(4) 0.022(2) 0.020(3) 0.024(2) C13 0.029(3) 0.036(3) 0.032(3) 0.014(3) 0.017(3) 0.016(3) O13 0.024(2) 0.062(3) 0.035(3) 0.005(2) 0.001(2) 0.010(2) C21 0.024(3) 0.041(3) 0.035(3) -0.002(3) 0.010(3) 0.009(3) O21 0.024(3) 0.076(4) 0.060(3) 0.000(3) 0.019(2) 0.014(2) C22 0.021(3) 0.027(3) 0.030(3) -0.003(2) 0.005(2) 0.006(2) O22 0.039(3) 0.038(2) 0.039(3) 0.015(2) 0.005(2) 0.019(2) C23 0.021(3) 0.035(3) 0.034(3) 0.002(3) 0.008(2) 0.011(2) O23 0.037(3) 0.044(3) 0.033(2) -0.007(2) 0.006(2) 0.015(2) C31 0.031(4) 0.052(4) 0.046(4) 0.022(3) 0.009(3) 0.009(3) O31 0.067(4) 0.079(4) 0.083(4) 0.054(4) 0.003(3) 0.027(3) C32 0.036(4) 0.081(6) 0.036(4) 0.008(4) 0.018(3) 0.022(4) O32 0.046(4) 0.175(8) 0.055(4) -0.013(4) 0.027(3) 0.037(4) C33 0.039(4) 0.037(3) 0.035(3) 0.016(3) 0.015(3) 0.008(3) O33 0.063(4) 0.042(3) 0.046(3) 0.011(2) 0.012(3) -0.008(3) C34 0.028(3) 0.043(3) 0.030(3) 0.009(3) 0.010(3) 0.016(3) O34 0.032(2) 0.045(3) 0.037(3) -0.001(2) 0.006(2) 0.010(2) C201 0.025(3) 0.031(3) 0.022(3) 0.004(2) 0.006(2) 0.010(2) C202 0.027(3) 0.030(3) 0.049(4) 0.010(3) 0.012(3) 0.004(3) C203 0.024(3) 0.057(4) 0.050(4) 0.006(3) 0.010(3) 0.005(3) C204 0.018(3) 0.081(5) 0.040(4) 0.000(4) 0.006(3) 0.017(3) C205 0.038(4) 0.064(5) 0.068(5) 0.008(4) 0.013(4) 0.033(4) C206 0.032(3) 0.036(3) 0.050(4) 0.005(3) 0.009(3) 0.020(3) C211 0.019(3) 0.024(3) 0.031(3) 0.004(2) 0.005(2) 0.010(2) C212 0.045(4) 0.026(3) 0.037(3) 0.009(3) 0.016(3) 0.016(3) C213 0.057(5) 0.035(3) 0.049(4) 0.006(3) 0.016(4) 0.025(3) C214 0.043(4) 0.047(4) 0.047(4) -0.004(3) 0.011(3) 0.027(3) C215 0.026(3) 0.058(4) 0.037(4) 0.001(3) 0.011(3) 0.018(3) C216 0.021(3) 0.034(3) 0.038(3) 0.009(3) 0.012(3) 0.012(2) C221 0.022(3) 0.020(2) 0.025(3) 0.005(2) 0.006(2) 0.009(2) C222 0.024(3) 0.024(3) 0.033(3) 0.007(2) 0.015(2) 0.009(2) C223 0.031(3) 0.032(3) 0.035(3) 0.003(3) 0.015(3) 0.010(3) C224 0.028(3) 0.025(3) 0.027(3) 0.002(2) 0.003(2) 0.005(2) C225 0.030(3) 0.032(3) 0.032(3) 0.005(2) 0.005(3) 0.014(3) C226 0.022(3) 0.028(3) 0.039(3) 0.007(2) 0.014(3) 0.009(2) C101 0.024(3) 0.020(3) 0.027(3) 0.007(2) 0.005(2) 0.002(2) C102 0.028(3) 0.025(3) 0.040(4) 0.004(3) 0.003(3) 0.003(2) C103 0.022(3) 0.036(3) 0.047(4) 0.007(3) 0.007(3) -0.007(3) C104 0.039(4) 0.027(3) 0.049(4) 0.007(3) 0.008(3) -0.007(3) C105 0.056(5) 0.024(3) 0.044(4) 0.001(3) 0.004(3) 0.009(3) C106 0.033(3) 0.022(3) 0.044(4) 0.005(3) 0.012(3) 0.004(2) C111 0.020(3) 0.021(2) 0.025(3) 0.006(2) 0.007(2) 0.011(2) C112 0.029(3) 0.026(3) 0.021(3) 0.004(2) 0.009(2) 0.009(2) C113 0.035(3) 0.032(3) 0.030(3) 0.008(2) 0.015(3) 0.014(3) C114 0.044(4) 0.041(3) 0.024(3) 0.008(3) 0.016(3) 0.024(3) C115 0.040(4) 0.039(3) 0.023(3) 0.001(3) 0.005(3) 0.010(3) C116 0.029(3) 0.025(3) 0.028(3) 0.000(2) 0.006(2) 0.006(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Os1 C12 1.889(6) . ? Os1 C11 1.898(6) . ? Os1 C13 1.941(6) . ? Os1 P1 2.3688(14) . ? Os1 Au1 2.7910(3) . ? Os1 Os3 2.8947(3) . ? Os1 Os2 2.9568(3) . ? Os2 C22 1.907(6) . ? Os2 C21 1.909(6) . ? Os2 C23 1.948(6) . ? Os2 P1 2.3643(13) . ? Os2 Au1 2.7864(3) . ? Os2 Os3 2.8995(3) . ? Os3 C32 1.910(7) . ? Os3 C31 1.923(7) . ? Os3 C34 1.949(6) . ? Os3 C33 1.962(7) . ? Au1 P2 2.3116(13) . ? P2 C201 1.811(6) . ? P2 C211 1.813(5) . ? P2 C221 1.817(6) . ? P1 C101 1.818(5) . ? P1 C111 1.845(5) . ? C11 O11 1.149(7) . ? C12 O12 1.150(7) . ? C13 O13 1.134(7) . ? C21 O21 1.125(7) . ? C22 O22 1.144(7) . ? C23 O23 1.138(7) . ? C31 O31 1.128(8) . ? C32 O32 1.134(9) . ? C33 O33 1.122(8) . ? C34 O34 1.147(7) . ? C201 C206 1.375(8) . ? C201 C202 1.396(8) . ? C202 C203 1.400(9) . ? C203 C204 1.336(11) . ? C204 C205 1.386(11) . ? C205 C206 1.375(9) . ? C211 C212 1.396(8) . ? C211 C216 1.410(8) . ? C212 C213 1.371(9) . ? C213 C214 1.369(10) . ? C214 C215 1.382(10) . ? C215 C216 1.388(9) . ? C221 C222 1.397(7) . ? C221 C226 1.400(7) . ? C222 C223 1.380(8) . ? C223 C224 1.403(8) . ? C224 C225 1.369(9) . ? C225 C226 1.389(8) . ? C101 C106 1.378(8) . ? C101 C102 1.392(9) . ? C102 C103 1.399(8) . ? C103 C104 1.373(10) . ? C104 C105 1.379(10) . ? C105 C106 1.387(9) . ? C111 C112 1.396(8) . ? C111 C116 1.398(7) . ? C112 C113 1.393(8) . ? C113 C114 1.387(8) . ? C114 C115 1.368(9) . ? C115 C116 1.386(9) . ? 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 C12 Os1 C11 95.9(3) . . ? C12 Os1 C13 96.7(3) . . ? C11 Os1 C13 91.8(2) . . ? C12 Os1 P1 99.26(18) . . ? C11 Os1 P1 92.86(18) . . ? C13 Os1 P1 162.78(18) . . ? C12 Os1 Au1 172.30(18) . . ? C11 Os1 Au1 81.18(18) . . ? C13 Os1 Au1 76.32(17) . . ? P1 Os1 Au1 88.03(3) . . ? C12 Os1 Os3 81.5(2) . . ? C11 Os1 Os3 177.28(18) . . ? C13 Os1 Os3 89.29(17) . . ? P1 Os1 Os3 86.82(3) . . ? Au1 Os1 Os3 101.510(9) . . ? C12 Os1 Os2 128.97(19) . . ? C11 Os1 Os2 122.31(18) . . ? C13 Os1 Os2 112.83(17) . . ? P1 Os1 Os2 51.27(3) . . ? Au1 Os1 Os2 57.910(7) . . ? Os3 Os1 Os2 59.395(7) . . ? C22 Os2 C21 95.5(3) . . ? C22 Os2 C23 93.2(2) . . ? C21 Os2 C23 94.8(2) . . ? C22 Os2 P1 94.55(17) . . ? C21 Os2 P1 99.85(18) . . ? C23 Os2 P1 162.67(17) . . ? C22 Os2 Au1 75.48(17) . . ? C21 Os2 Au1 168.4(2) . . ? C23 Os2 Au1 78.75(17) . . ? P1 Os2 Au1 88.23(3) . . ? C22 Os2 Os3 176.64(16) . . ? C21 Os2 Os3 87.3(2) . . ? C23 Os2 Os3 84.69(19) . . ? P1 Os2 Os3 86.79(3) . . ? Au1 Os2 Os3 101.501(9) . . ? C22 Os2 Os1 119.43(17) . . ? C21 Os2 Os1 133.5(2) . . ? C23 Os2 Os1 111.41(17) . . ? P1 Os2 Os1 51.41(3) . . ? Au1 Os2 Os1 58.060(7) . . ? Os3 Os2 Os1 59.236(7) . . ? C32 Os3 C31 101.8(3) . . ? C32 Os3 C34 94.2(3) . . ? C31 Os3 C34 90.9(3) . . ? C32 Os3 C33 88.5(3) . . ? C31 Os3 C33 88.1(3) . . ? C34 Os3 C33 177.3(3) . . ? C32 Os3 Os1 153.4(2) . . ? C31 Os3 Os1 104.8(2) . . ? C34 Os3 Os1 84.62(18) . . ? C33 Os3 Os1 93.20(19) . . ? C32 Os3 Os2 92.0(2) . . ? C31 Os3 Os2 166.1(2) . . ? C34 Os3 Os2 86.04(18) . . ? C33 Os3 Os2 94.30(18) . . ? Os1 Os3 Os2 61.369(7) . . ? P2 Au1 Os2 141.01(4) . . ? P2 Au1 Os1 153.68(4) . . ? Os2 Au1 Os1 64.030(7) . . ? C201 P2 C211 105.8(3) . . ? C201 P2 C221 104.8(3) . . ? C211 P2 C221 104.6(2) . . ? C201 P2 Au1 114.68(19) . . ? C211 P2 Au1 114.96(19) . . ? C221 P2 Au1 111.04(17) . . ? C101 P1 C111 99.5(2) . . ? C101 P1 Os2 121.7(2) . . ? C111 P1 Os2 118.72(17) . . ? C101 P1 Os1 124.14(19) . . ? C111 P1 Os1 116.49(17) . . ? Os2 P1 Os1 77.32(4) . . ? O11 C11 Os1 174.3(6) . . ? O12 C12 Os1 178.6(6) . . ? O13 C13 Os1 176.0(5) . . ? O21 C21 Os2 178.1(6) . . ? O22 C22 Os2 175.3(5) . . ? O23 C23 Os2 175.8(5) . . ? O31 C31 Os3 177.5(7) . . ? O32 C32 Os3 176.7(7) . . ? O33 C33 Os3 169.6(6) . . ? O34 C34 Os3 177.2(6) . . ? C206 C201 C202 118.8(6) . . ? C206 C201 P2 119.6(5) . . ? C202 C201 P2 121.5(5) . . ? C201 C202 C203 119.5(6) . . ? C204 C203 C202 120.1(7) . . ? C203 C204 C205 121.4(6) . . ? C206 C205 C204 118.9(7) . . ? C205 C206 C201 121.3(6) . . ? C212 C211 C216 118.9(5) . . ? C212 C211 P2 122.6(5) . . ? C216 C211 P2 118.5(4) . . ? C213 C212 C211 120.5(6) . . ? C212 C213 C214 120.6(7) . . ? C213 C214 C215 120.3(6) . . ? C214 C215 C216 120.4(6) . . ? C215 C216 C211 119.2(6) . . ? C222 C221 C226 118.2(5) . . ? C222 C221 P2 122.6(4) . . ? C226 C221 P2 119.2(4) . . ? C223 C222 C221 121.1(5) . . ? C222 C223 C224 119.7(6) . . ? C225 C224 C223 119.8(6) . . ? C224 C225 C226 120.5(6) . . ? C225 C226 C221 120.7(5) . . ? C106 C101 C102 118.9(5) . . ? C106 C101 P1 121.4(5) . . ? C102 C101 P1 119.4(4) . . ? C101 C102 C103 119.5(6) . . ? C104 C103 C102 120.6(6) . . ? C103 C104 C105 120.1(6) . . ? C104 C105 C106 119.3(6) . . ? C101 C106 C105 121.6(6) . . ? C112 C111 C116 117.1(5) . . ? C112 C111 P1 120.5(4) . . ? C116 C111 P1 122.4(4) . . ? C111 C112 C113 121.1(5) . . ? C114 C113 C112 119.9(6) . . ? C115 C114 C113 120.0(6) . . ? C114 C115 C116 120.1(6) . . ? C115 C116 C111 121.8(5) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.168 _refine_diff_density_min -3.752 _refine_diff_density_rms 0.236 #===END data_for_complex_11 _database_code_CSD 197614 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H19 Ag O10 Os3 P2' _chemical_formula_weight 1219.81 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' Ag Ag -0.8971 1.1015 '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' Os Os -1.2165 7.6030 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 17.4362(2) _cell_length_b 8.79980(10) _cell_length_c 20.0377(3) _cell_angle_alpha 90.00 _cell_angle_beta 93.0380(10) _cell_angle_gamma 90.00 _cell_volume 3070.17(7) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 40543 _cell_measurement_theta_min 3.02 _cell_measurement_theta_max 27.48 _exptl_crystal_description platelet _exptl_crystal_colour orange _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.639 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2216 _exptl_absorpt_coefficient_mu 13.159 _exptl_absorpt_correction_type SORTAV _exptl_absorpt_correction_T_min 0.3012 _exptl_absorpt_correction_T_max 0.5591 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Nonius Kappa CCD Diffractometer' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 40543 _diffrn_reflns_av_R_equivalents 0.0655 _diffrn_reflns_av_sigmaI/netI 0.0407 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 27.48 _reflns_number_total 7038 _reflns_number_gt 6171 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Kappa CCD control software' _computing_cell_refinement 'Kappa CCD control software' _computing_data_reduction 'Kappa CCD control software' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP 3 (WinGX, L. Farrugia)' _computing_publication_material 'SHELXL-97 (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^)+(0.0958P)^2^+0.7694P] 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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00260(15) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7038 _refine_ls_number_parameters 374 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0578 _refine_ls_R_factor_gt 0.0488 _refine_ls_wR_factor_ref 0.1411 _refine_ls_wR_factor_gt 0.1186 _refine_ls_goodness_of_fit_ref 1.142 _refine_ls_restrained_S_all 1.142 _refine_ls_shift/su_max 0.018 _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 Os2 Os 0.005117(17) 0.09558(3) 0.255789(15) 0.02250(13) Uani 1 1 d . . . Os3 Os 0.059191(17) 0.21888(3) 0.383021(14) 0.02520(13) Uani 1 1 d . . . Os1 Os 0.057875(17) 0.41591(3) 0.266532(15) 0.02287(13) Uani 1 1 d . . . Ag1 Ag 0.12026(3) 0.21429(7) 0.17736(3) 0.02870(17) Uani 1 1 d . . . P2 P 0.17984(12) 0.1603(2) 0.07483(10) 0.0277(4) Uani 1 1 d . . . P1 P -0.06669(11) 0.3219(2) 0.23715(10) 0.0233(4) Uani 1 1 d . . . C23 C -0.0172(5) 0.0206(10) 0.1674(4) 0.0322(18) Uani 1 1 d . . . C22 C -0.0688(5) -0.0175(9) 0.2995(4) 0.0328(18) Uani 1 1 d . . . C21 C 0.0876(5) -0.0490(10) 0.2724(4) 0.0289(17) Uani 1 1 d . . . C33 C -0.0481(5) 0.2596(9) 0.4039(4) 0.0310(17) Uani 1 1 d . . . C34 C 0.0590(5) 0.0301(10) 0.4323(4) 0.0336(18) Uani 1 1 d . . . C32 C 0.0930(5) 0.3562(11) 0.4539(4) 0.039(2) Uani 1 1 d . . . C31 C 0.1642(5) 0.1736(9) 0.3567(4) 0.0318(17) Uani 1 1 d . . . C13 C 0.0344(5) 0.5665(9) 0.3295(5) 0.0327(18) Uani 1 1 d . . . C12 C 0.1676(5) 0.4419(10) 0.2779(5) 0.0351(19) Uani 1 1 d . . . C11 C 0.0572(5) 0.5438(9) 0.1890(4) 0.0326(18) Uani 1 1 d . . . C203 C 0.2720(5) 0.2522(12) 0.0606(5) 0.045(2) Uani 1 1 d . . . H3C H 0.3107 0.2180 0.0945 0.068 Uiso 1 1 calc R . . H3B H 0.2661 0.3627 0.0635 0.068 Uiso 1 1 calc R . . H3A H 0.2883 0.2249 0.0161 0.068 Uiso 1 1 calc R . . C202 C 0.1187(6) 0.2196(11) 0.0042(5) 0.042(2) Uani 1 1 d . . . H2C H 0.0728 0.1552 0.0008 0.063 Uiso 1 1 calc R . . H2B H 0.1466 0.2102 -0.0368 0.063 Uiso 1 1 calc R . . H2A H 0.1034 0.3258 0.0102 0.063 Uiso 1 1 calc R . . C201 C 0.1910(8) -0.0420(11) 0.0545(6) 0.059(3) Uani 1 1 d . . . H1C H 0.2105 -0.0970 0.0943 0.088 Uiso 1 1 calc R . . H1B H 0.2273 -0.0527 0.0191 0.088 Uiso 1 1 calc R . . H1A H 0.1411 -0.0842 0.0391 0.088 Uiso 1 1 calc R . . C117 C -0.1055(4) 0.3564(8) 0.1512(4) 0.0251(15) Uani 1 1 d . . . C118 C -0.0602(5) 0.3291(11) 0.0967(4) 0.0350(18) Uani 1 1 d . . . H18 H -0.0083 0.2982 0.1045 0.042 Uiso 1 1 calc R . . C119 C -0.0901(5) 0.3464(11) 0.0314(4) 0.038(2) Uani 1 1 d . . . H19 H -0.0585 0.3257 -0.0047 0.046 Uiso 1 1 calc R . . C120 C -0.1648(5) 0.3932(9) 0.0182(5) 0.037(2) Uani 1 1 d . . . H20 H -0.1848 0.4041 -0.0265 0.044 Uiso 1 1 calc R . . C121 C -0.2098(5) 0.4237(9) 0.0705(5) 0.037(2) Uani 1 1 d . . . H21 H -0.2612 0.4568 0.0616 0.045 Uiso 1 1 calc R . . C122 C -0.1808(5) 0.4066(8) 0.1380(4) 0.0293(17) Uani 1 1 d . . . H22 H -0.2125 0.4293 0.1738 0.035 Uiso 1 1 calc R . . C111 C -0.1487(4) 0.3768(9) 0.2845(4) 0.0263(16) Uani 1 1 d . . . C112 C -0.2095(5) 0.2745(9) 0.2925(4) 0.0318(18) Uani 1 1 d . . . H12 H -0.2078 0.1753 0.2739 0.038 Uiso 1 1 calc R . . C113 C -0.2721(5) 0.3198(11) 0.3278(4) 0.038(2) Uani 1 1 d . . . H13 H -0.3131 0.2510 0.3337 0.045 Uiso 1 1 calc R . . C114 C -0.2749(5) 0.4638(11) 0.3544(4) 0.037(2) Uani 1 1 d . . . H14 H -0.3185 0.4939 0.3777 0.045 Uiso 1 1 calc R . . C115 C -0.2171(5) 0.5622(10) 0.3479(5) 0.038(2) Uani 1 1 d . . . H15 H -0.2190 0.6600 0.3678 0.045 Uiso 1 1 calc R . . C116 C -0.1536(5) 0.5207(9) 0.3115(4) 0.0303(17) Uani 1 1 d . . . H16 H -0.1137 0.5921 0.3055 0.036 Uiso 1 1 calc R . . O23 O -0.0293(4) -0.0378(9) 0.1163(3) 0.0499(17) Uani 1 1 d . . . O22 O -0.1155(4) -0.0855(7) 0.3261(4) 0.0465(18) Uani 1 1 d . . . O21 O 0.1331(3) -0.1425(7) 0.2818(3) 0.0369(14) Uani 1 1 d . . . O33 O -0.1076(4) 0.2709(8) 0.4224(3) 0.0486(17) Uani 1 1 d . . . O34 O 0.0603(4) -0.0791(7) 0.4607(3) 0.0458(17) Uani 1 1 d . . . O32 O 0.1110(5) 0.4342(10) 0.4973(4) 0.068(2) Uani 1 1 d . . . O31 O 0.2242(3) 0.1421(8) 0.3459(3) 0.0412(15) Uani 1 1 d . . . O13 O 0.0230(4) 0.6584(7) 0.3686(3) 0.0441(16) Uani 1 1 d . . . O12 O 0.2316(4) 0.4703(8) 0.2834(3) 0.0464(16) Uani 1 1 d . . . O11 O 0.0555(5) 0.6260(8) 0.1467(4) 0.0529(18) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Os2 0.0234(2) 0.01748(19) 0.0267(2) -0.00148(10) 0.00215(13) -0.00156(10) Os3 0.0301(2) 0.02153(19) 0.0241(2) 0.00047(11) 0.00236(13) -0.00170(11) Os1 0.0248(2) 0.01814(19) 0.0259(2) 0.00038(10) 0.00287(13) -0.00274(10) Ag1 0.0282(3) 0.0304(3) 0.0279(3) -0.0008(2) 0.0055(2) 0.0010(2) P2 0.0298(10) 0.0239(10) 0.0298(10) -0.0026(8) 0.0048(8) 0.0019(8) P1 0.0245(9) 0.0188(9) 0.0268(10) 0.0000(7) 0.0015(7) -0.0001(7) C23 0.027(4) 0.032(4) 0.038(5) -0.004(4) 0.001(3) 0.001(3) C22 0.035(4) 0.023(4) 0.040(5) -0.001(3) 0.003(4) -0.004(3) C21 0.031(4) 0.026(4) 0.029(4) -0.001(3) 0.003(3) -0.007(3) C33 0.039(5) 0.027(4) 0.027(4) 0.011(3) 0.000(3) 0.007(3) C34 0.031(4) 0.039(5) 0.031(4) -0.002(4) 0.005(3) 0.003(4) C32 0.045(5) 0.038(5) 0.033(5) -0.004(4) 0.003(4) -0.004(4) C31 0.035(5) 0.028(4) 0.033(4) 0.000(3) -0.001(3) -0.009(3) C13 0.028(4) 0.026(4) 0.044(5) -0.002(4) -0.003(4) 0.000(3) C12 0.037(5) 0.023(4) 0.045(5) 0.001(4) -0.003(4) -0.009(3) C11 0.037(5) 0.022(4) 0.039(5) 0.004(3) 0.006(4) -0.003(3) C203 0.028(5) 0.056(6) 0.052(6) 0.004(5) 0.003(4) 0.001(4) C202 0.042(5) 0.047(6) 0.036(5) -0.004(4) -0.004(4) 0.005(4) C201 0.090(9) 0.027(5) 0.059(7) -0.007(5) 0.006(6) 0.007(5) C117 0.026(4) 0.016(3) 0.033(4) 0.002(3) -0.004(3) 0.000(3) C118 0.033(4) 0.041(5) 0.030(4) -0.002(4) -0.001(3) 0.000(4) C119 0.048(5) 0.040(5) 0.026(4) -0.004(4) 0.004(4) 0.008(4) C120 0.042(5) 0.032(4) 0.035(5) 0.002(3) -0.011(4) 0.000(4) C121 0.036(5) 0.026(4) 0.048(5) 0.012(4) -0.012(4) -0.003(3) C122 0.027(4) 0.024(4) 0.037(5) 0.006(3) 0.002(3) 0.001(3) C111 0.020(4) 0.026(4) 0.033(4) 0.004(3) 0.003(3) 0.000(3) C112 0.035(4) 0.027(4) 0.034(4) 0.000(3) -0.001(3) -0.002(3) C113 0.031(4) 0.045(5) 0.038(5) 0.007(4) 0.003(4) -0.002(4) C114 0.031(4) 0.051(6) 0.031(5) 0.005(4) 0.004(4) 0.008(4) C115 0.041(5) 0.028(4) 0.043(5) -0.005(4) 0.001(4) 0.008(4) C116 0.032(4) 0.026(4) 0.033(4) -0.001(3) 0.001(3) 0.003(3) O23 0.045(4) 0.059(4) 0.045(4) -0.025(4) -0.002(3) 0.002(3) O22 0.041(4) 0.034(4) 0.067(5) 0.008(3) 0.020(4) -0.008(3) O21 0.031(3) 0.025(3) 0.055(4) 0.003(3) 0.003(3) 0.009(2) O33 0.044(4) 0.062(5) 0.040(4) 0.014(3) 0.006(3) 0.021(3) O34 0.064(5) 0.034(4) 0.042(4) 0.016(3) 0.017(3) 0.016(3) O32 0.081(6) 0.074(5) 0.049(5) -0.031(4) 0.003(4) -0.020(5) O31 0.028(3) 0.040(4) 0.056(4) -0.004(3) 0.001(3) 0.000(3) O13 0.052(4) 0.029(3) 0.052(4) -0.018(3) 0.009(3) -0.001(3) O12 0.027(3) 0.057(4) 0.056(4) 0.000(3) 0.006(3) -0.012(3) O11 0.067(5) 0.045(4) 0.047(4) 0.019(3) 0.002(4) -0.007(4) _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 Os2 C22 1.881(8) . ? Os2 C23 1.912(8) . ? Os2 C21 1.936(9) . ? Os2 P1 2.3712(19) . ? Os2 Ag1 2.8153(7) . ? Os2 Os3 2.8829(4) . ? Os2 Os1 2.9694(4) . ? Os3 C34 1.933(9) . ? Os3 C32 1.933(9) . ? Os3 C33 1.971(9) . ? Os3 C31 1.974(9) . ? Os3 Os1 2.9068(4) . ? Os1 C13 1.889(9) . ? Os1 C11 1.917(8) . ? Os1 C12 1.928(9) . ? Os1 P1 2.3692(19) . ? Os1 Ag1 2.7802(7) . ? Ag1 P2 2.398(2) . ? P2 C202 1.804(9) . ? P2 C203 1.835(9) . ? P2 C201 1.839(10) . ? P1 C111 1.822(8) . ? P1 C117 1.842(8) . ? C23 O23 1.154(10) . ? C22 O22 1.163(10) . ? C21 O21 1.152(10) . ? C33 O33 1.125(11) . ? C34 O34 1.116(10) . ? C32 O32 1.138(11) . ? C31 O31 1.114(11) . ? C13 O13 1.151(10) . ? C12 O12 1.144(11) . ? C11 O11 1.114(10) . ? C117 C122 1.397(11) . ? C117 C118 1.401(12) . ? C118 C119 1.392(12) . ? C119 C120 1.377(13) . ? C120 C121 1.367(14) . ? C121 C122 1.427(12) . ? C111 C116 1.382(11) . ? C111 C112 1.407(11) . ? C112 C113 1.390(13) . ? C113 C114 1.376(14) . ? C114 C115 1.341(13) . ? C115 C116 1.406(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C22 Os2 C23 97.9(4) . . ? C22 Os2 C21 95.3(3) . . ? C23 Os2 C21 92.6(3) . . ? C22 Os2 P1 98.5(3) . . ? C23 Os2 P1 93.7(3) . . ? C21 Os2 P1 163.8(2) . . ? C22 Os2 Ag1 169.3(3) . . ? C23 Os2 Ag1 74.2(3) . . ? C21 Os2 Ag1 78.1(2) . . ? P1 Os2 Ag1 89.24(5) . . ? C22 Os2 Os3 89.3(3) . . ? C23 Os2 Os3 172.2(2) . . ? C21 Os2 Os3 83.7(2) . . ? P1 Os2 Os3 88.19(5) . . ? Ag1 Os2 Os3 98.308(16) . . ? C22 Os2 Os1 133.3(3) . . ? C23 Os2 Os1 116.2(3) . . ? C21 Os2 Os1 112.8(2) . . ? P1 Os2 Os1 51.18(5) . . ? Ag1 Os2 Os1 57.377(14) . . ? Os3 Os2 Os1 59.541(10) . . ? C34 Os3 C32 99.8(4) . . ? C34 Os3 C33 91.2(3) . . ? C32 Os3 C33 89.2(4) . . ? C34 Os3 C31 89.4(3) . . ? C32 Os3 C31 94.1(4) . . ? C33 Os3 C31 176.5(3) . . ? C34 Os3 Os2 96.8(2) . . ? C32 Os3 Os2 163.3(3) . . ? C33 Os3 Os2 89.2(3) . . ? C31 Os3 Os2 87.3(2) . . ? C34 Os3 Os1 157.3(2) . . ? C32 Os3 Os1 101.9(3) . . ? C33 Os3 Os1 95.5(2) . . ? C31 Os3 Os1 82.7(2) . . ? Os2 Os3 Os1 61.710(10) . . ? C13 Os1 C11 97.9(4) . . ? C13 Os1 C12 95.0(4) . . ? C11 Os1 C12 89.4(4) . . ? C13 Os1 P1 100.5(3) . . ? C11 Os1 P1 92.1(3) . . ? C12 Os1 P1 164.1(3) . . ? C13 Os1 Ag1 169.3(3) . . ? C11 Os1 Ag1 80.8(3) . . ? C12 Os1 Ag1 74.5(3) . . ? P1 Os1 Ag1 90.12(5) . . ? C13 Os1 Os3 82.8(3) . . ? C11 Os1 Os3 179.3(3) . . ? C12 Os1 Os3 90.6(3) . . ? P1 Os1 Os3 87.67(5) . . ? Ag1 Os1 Os3 98.552(16) . . ? C13 Os1 Os2 129.6(3) . . ? C11 Os1 Os2 120.6(3) . . ? C12 Os1 Os2 115.0(3) . . ? P1 Os1 Os2 51.25(5) . . ? Ag1 Os1 Os2 58.524(15) . . ? Os3 Os1 Os2 58.749(10) . . ? P2 Ag1 Os1 151.52(6) . . ? P2 Ag1 Os2 139.35(6) . . ? Os1 Ag1 Os2 64.099(15) . . ? C202 P2 C203 103.7(5) . . ? C202 P2 C201 99.9(5) . . ? C203 P2 C201 106.7(5) . . ? C202 P2 Ag1 110.5(3) . . ? C203 P2 Ag1 118.0(4) . . ? C201 P2 Ag1 116.0(4) . . ? C111 P1 C117 100.6(4) . . ? C111 P1 Os1 120.8(3) . . ? C117 P1 Os1 117.4(3) . . ? C111 P1 Os2 124.3(3) . . ? C117 P1 Os2 116.8(3) . . ? Os1 P1 Os2 77.57(6) . . ? O23 C23 Os2 173.7(8) . . ? O22 C22 Os2 178.7(8) . . ? O21 C21 Os2 175.5(7) . . ? O33 C33 Os3 171.4(7) . . ? O34 C34 Os3 178.8(8) . . ? O32 C32 Os3 177.2(9) . . ? O31 C31 Os3 174.9(8) . . ? O13 C13 Os1 177.4(7) . . ? O12 C12 Os1 174.1(8) . . ? O11 C11 Os1 175.3(8) . . ? C122 C117 C118 118.0(7) . . ? C122 C117 P1 121.6(6) . . ? C118 C117 P1 120.4(6) . . ? C119 C118 C117 121.0(8) . . ? C120 C119 C118 121.1(9) . . ? C121 C120 C119 119.2(8) . . ? C120 C121 C122 121.0(9) . . ? C117 C122 C121 119.7(9) . . ? C116 C111 C112 118.6(7) . . ? C116 C111 P1 120.9(6) . . ? C112 C111 P1 120.5(6) . . ? C113 C112 C111 119.5(8) . . ? C114 C113 C112 120.4(8) . . ? C115 C114 C113 120.9(8) . . ? C114 C115 C116 120.0(8) . . ? C111 C116 C115 120.6(8) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 4.700 _refine_diff_density_min -4.524 _refine_diff_density_rms 0.631 #===END