# Supplementary Material (ESI) for New Journal of Chemistry # This journal is (c) The Royal Society of Chemistry and The Centre National de la Recherche Scientifique, 2010 data_global _journal_name_full 'New J.Chem.' _journal_coden_Cambridge 0440 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Shariff Kabir' _publ_contact_author_email 'skabir ju@yahoo.com' _publ_section_title ; The rational synthesis of tetranuclear heterometallic butterfly clusters: reactions of [M2(CO)6(\^I -pyS)2] (M = Re, Mn) with group VIII metal carbonyls ; _publ_author_name 'Shariff Kabir' # Attachment '- Compound 11.cif' data_dth1sb _database_code_depnum_ccdc_archive 'CCDC 721479' #TrackingRef '- Compound 11.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H34 N O11 Os3 P2 Re S' _chemical_formula_weight 1699.60 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -5.2083 5.8923 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Os Os -4.9801 6.2216 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/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 13.7860(3) _cell_length_b 21.2076(4) _cell_length_c 16.8447(4) _cell_angle_alpha 90.00 _cell_angle_beta 92.3630(10) _cell_angle_gamma 90.00 _cell_volume 4920.66(18) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9926 _cell_measurement_theta_min 3 _cell_measurement_theta_max 67 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.294 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3160 _exptl_absorpt_coefficient_mu 20.497 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.0566 _exptl_absorpt_correction_T_max 0.1828 _exptl_absorpt_process_details ; Numerical (based on real shape of the crystal) absorption correction followed by: SADABS. Program for empirical absorption correction of area-detector data. University of Goetingen. Germany. Sheldrick, G. M. 1996 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX2 CCD detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 40725 _diffrn_reflns_av_R_equivalents 0.0405 _diffrn_reflns_av_sigmaI/netI 0.0280 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.21 _diffrn_reflns_theta_max 68.03 _reflns_number_total 8654 _reflns_number_gt 8047 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2-2008.5-0 (Bruker, 2008)' _computing_cell_refinement 'SAINT v7.56A (Bruker, 2008)' _computing_data_reduction 'SADABS-2008/1 (Bruker, 2008)' _computing_structure_solution 'XS/SHELXTL-2008/1 (Bruker, 2008)' _computing_structure_refinement 'SHELXL-2008/4(Bruker, 2008)' _computing_molecular_graphics 'XP v5.1 (Bruker, 1998)' _computing_publication_material 'XCIF-2008/2 (Bruker, 2008)' _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^)+(0.0349P)^2^+15.5173P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.000025(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 8654 _refine_ls_number_parameters 641 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0298 _refine_ls_R_factor_gt 0.0266 _refine_ls_wR_factor_ref 0.0656 _refine_ls_wR_factor_gt 0.0641 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.020 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Os1 Os 0.490935(15) 0.223584(9) 0.593551(13) 0.01582(6) Uani 1 1 d . . . Os2 Os 0.281898(15) 0.219434(9) 0.572997(13) 0.01484(6) Uani 1 1 d . . . Os3 Os 0.369577(15) 0.325882(10) 0.642958(13) 0.01685(6) Uani 1 1 d . . . Re1 Re 0.185638(16) 0.339821(10) 0.550930(14) 0.01777(6) Uani 1 1 d . . . S1 S 0.27524(9) 0.24845(5) 0.71075(7) 0.0166(2) Uani 1 1 d . . . P1 P 0.66110(9) 0.23474(6) 0.60583(8) 0.0175(3) Uani 1 1 d . . . P2 P 0.25493(9) 0.11079(6) 0.60113(8) 0.0166(3) Uani 1 1 d . . . O1 O 0.4919(3) 0.19009(17) 0.7712(2) 0.0247(8) Uani 1 1 d . . . O2 O 0.5193(3) 0.09350(17) 0.5233(2) 0.0264(8) Uani 1 1 d . . . O3 O 0.5003(3) 0.2958(2) 0.4356(2) 0.0328(9) Uani 1 1 d . . . O4 O 0.3339(3) 0.19656(19) 0.4020(2) 0.0271(9) Uani 1 1 d . . . O5 O 0.0766(3) 0.20079(17) 0.5053(3) 0.0288(9) Uani 1 1 d . . . O6 O 0.2638(3) 0.44197(18) 0.7003(3) 0.0309(9) Uani 1 1 d . . . O7 O 0.4813(3) 0.41201(19) 0.5338(3) 0.0362(10) Uani 1 1 d . . . O8 O 0.5051(3) 0.33312(18) 0.7912(2) 0.0261(8) Uani 1 1 d . . . O9 O 0.2998(3) 0.3628(2) 0.4003(3) 0.0407(11) Uani 1 1 d . . . O10 O 0.1289(3) 0.47906(18) 0.5568(3) 0.0377(10) Uani 1 1 d . . . O11 O 0.0016(3) 0.32703(19) 0.4452(3) 0.0313(9) Uani 1 1 d . . . N1 N 0.1173(3) 0.31876(19) 0.6655(3) 0.0182(9) Uani 1 1 d . . . C1 C 0.4869(4) 0.2000(2) 0.7049(3) 0.0199(11) Uani 1 1 d . . . C2 C 0.5087(4) 0.1423(2) 0.5500(3) 0.0204(11) Uani 1 1 d . . . C3 C 0.4933(4) 0.2682(2) 0.4929(3) 0.0213(11) Uani 1 1 d . . . C4 C 0.3171(4) 0.2057(2) 0.4673(3) 0.0207(11) Uani 1 1 d . . . C5 C 0.1499(4) 0.2168(2) 0.5357(3) 0.0186(11) Uani 1 1 d . . . C6 C 0.2941(4) 0.3971(2) 0.6734(3) 0.0233(11) Uani 1 1 d . . . C7 C 0.4414(4) 0.3783(2) 0.5735(3) 0.0230(11) Uani 1 1 d . . . C8 C 0.4596(4) 0.3302(2) 0.7336(4) 0.0235(12) Uani 1 1 d . . . C9 C 0.2573(4) 0.3546(3) 0.4566(3) 0.0273(12) Uani 1 1 d . . . C10 C 0.1508(4) 0.4271(2) 0.5543(3) 0.0250(12) Uani 1 1 d . . . C11 C 0.0701(4) 0.3318(2) 0.4860(3) 0.0222(11) Uani 1 1 d . . . C12 C 0.1616(4) 0.2850(2) 0.7246(3) 0.0193(11) Uani 1 1 d . . . C13 C 0.1189(4) 0.2762(2) 0.7976(3) 0.0212(11) Uani 1 1 d . . . H13A H 0.1517 0.2523 0.8381 0.025 Uiso 1 1 calc R . . C14 C 0.0294(4) 0.3022(3) 0.8112(4) 0.0269(12) Uani 1 1 d . . . H14A H 0.0005 0.2975 0.8611 0.032 Uiso 1 1 calc R . . C15 C -0.0176(4) 0.3354(2) 0.7494(4) 0.0261(12) Uani 1 1 d . . . H15A H -0.0803 0.3529 0.7558 0.031 Uiso 1 1 calc R . . C16 C 0.0286(4) 0.3426(2) 0.6787(3) 0.0235(11) Uani 1 1 d . . . H16A H -0.0039 0.3656 0.6371 0.028 Uiso 1 1 calc R . . C17 C 0.7108(4) 0.1992(2) 0.6980(3) 0.0202(11) Uani 1 1 d . . . C18 C 0.6939(4) 0.1344(2) 0.7083(3) 0.0265(12) Uani 1 1 d . . . H18A H 0.6602 0.1111 0.6677 0.032 Uiso 1 1 calc R . . C19 C 0.7261(4) 0.1044(3) 0.7774(4) 0.0283(12) Uani 1 1 d . . . H19A H 0.7151 0.0605 0.7842 0.034 Uiso 1 1 calc R . . C20 C 0.7744(4) 0.1385(3) 0.8365(4) 0.0298(13) Uani 1 1 d . . . H20A H 0.7955 0.1181 0.8844 0.036 Uiso 1 1 calc R . . C21 C 0.7922(4) 0.2016(3) 0.8271(3) 0.0300(13) Uani 1 1 d . . . H21A H 0.8264 0.2244 0.8679 0.036 Uiso 1 1 calc R . . C22 C 0.7604(4) 0.2324(3) 0.7579(3) 0.0244(11) Uani 1 1 d . . . H22A H 0.7727 0.2761 0.7517 0.029 Uiso 1 1 calc R . . C23 C 0.7270(4) 0.1921(2) 0.5306(3) 0.0200(11) Uani 1 1 d . . . C24 C 0.6873(4) 0.1787(2) 0.4560(3) 0.0240(11) Uani 1 1 d . . . H24A H 0.6247 0.1945 0.4412 0.029 Uiso 1 1 calc R . . C25 C 0.7368(4) 0.1427(2) 0.4018(3) 0.0266(12) Uani 1 1 d . . . H25A H 0.7074 0.1333 0.3511 0.032 Uiso 1 1 calc R . . C26 C 0.8292(4) 0.1205(2) 0.4220(4) 0.0294(13) Uani 1 1 d . . . H26A H 0.8633 0.0959 0.3852 0.035 Uiso 1 1 calc R . . C27 C 0.8715(4) 0.1345(2) 0.4958(4) 0.0269(12) Uani 1 1 d . . . H27A H 0.9352 0.1199 0.5094 0.032 Uiso 1 1 calc R . . C28 C 0.8213(4) 0.1696(2) 0.5498(4) 0.0252(12) Uani 1 1 d . . . H28A H 0.8507 0.1787 0.6005 0.030 Uiso 1 1 calc R . . C29 C 0.7141(4) 0.3140(2) 0.6039(3) 0.0197(11) Uani 1 1 d . . . C30 C 0.7858(4) 0.3306(2) 0.5526(3) 0.0245(11) Uani 1 1 d . . . H30A H 0.8113 0.2998 0.5181 0.029 Uiso 1 1 calc R . . C31 C 0.8209(4) 0.3925(3) 0.5516(3) 0.0263(12) Uani 1 1 d . . . H31A H 0.8687 0.4039 0.5151 0.032 Uiso 1 1 calc R . . C32 C 0.7867(4) 0.4371(3) 0.6030(4) 0.0290(13) Uani 1 1 d . . . H32A H 0.8111 0.4790 0.6025 0.035 Uiso 1 1 calc R . . C33 C 0.7165(4) 0.4203(3) 0.6555(4) 0.0338(14) Uani 1 1 d . . . H33A H 0.6929 0.4506 0.6914 0.041 Uiso 1 1 calc R . . C34 C 0.6808(4) 0.3600(3) 0.6557(4) 0.0286(13) Uani 1 1 d . . . H34A H 0.6324 0.3492 0.6918 0.034 Uiso 1 1 calc R . . C35 C 0.1531(4) 0.0947(2) 0.6673(3) 0.0196(10) Uani 1 1 d . . . C36 C 0.0850(4) 0.1393(2) 0.6857(3) 0.0235(11) Uani 1 1 d . . . H36A H 0.0883 0.1803 0.6632 0.028 Uiso 1 1 calc R . . C37 C 0.0118(4) 0.1253(3) 0.7366(4) 0.0271(12) Uani 1 1 d . . . H37A H -0.0342 0.1567 0.7490 0.032 Uiso 1 1 calc R . . C38 C 0.0052(4) 0.0661(3) 0.7695(3) 0.0275(12) Uani 1 1 d . . . H38A H -0.0440 0.0570 0.8057 0.033 Uiso 1 1 calc R . . C39 C 0.0708(4) 0.0199(2) 0.7494(3) 0.0242(12) Uani 1 1 d . . . H39A H 0.0653 -0.0215 0.7702 0.029 Uiso 1 1 calc R . . C40 C 0.1448(4) 0.0343(2) 0.6989(3) 0.0231(11) Uani 1 1 d . . . H40A H 0.1902 0.0026 0.6858 0.028 Uiso 1 1 calc R . . C41 C 0.2207(4) 0.0675(2) 0.5098(3) 0.0201(11) Uani 1 1 d . . . C42 C 0.1249(4) 0.0516(2) 0.4925(3) 0.0225(11) Uani 1 1 d . . . H42A H 0.0769 0.0597 0.5301 0.027 Uiso 1 1 calc R . . C43 C 0.0990(4) 0.0239(3) 0.4200(4) 0.0284(13) Uani 1 1 d . . . H43A H 0.0329 0.0136 0.4080 0.034 Uiso 1 1 calc R . . C44 C 0.1679(4) 0.0112(3) 0.3656(4) 0.0288(13) Uani 1 1 d . . . H44A H 0.1497 -0.0082 0.3164 0.035 Uiso 1 1 calc R . . C45 C 0.2648(4) 0.0268(3) 0.3830(4) 0.0276(12) Uani 1 1 d . . . H45A H 0.3129 0.0173 0.3461 0.033 Uiso 1 1 calc R . . C46 C 0.2904(4) 0.0559(2) 0.4537(3) 0.0246(12) Uani 1 1 d . . . H46A H 0.3559 0.0682 0.4644 0.030 Uiso 1 1 calc R . . C47 C 0.3478(4) 0.0625(2) 0.6537(3) 0.0205(11) Uani 1 1 d . . . C48 C 0.3937(4) 0.0108(2) 0.6210(4) 0.0238(11) Uani 1 1 d . . . H48A H 0.3767 -0.0020 0.5682 0.029 Uiso 1 1 calc R . . C49 C 0.4644(4) -0.0224(2) 0.6651(4) 0.0268(12) Uani 1 1 d . . . H49A H 0.4956 -0.0576 0.6425 0.032 Uiso 1 1 calc R . . C50 C 0.4892(4) -0.0037(3) 0.7425(4) 0.0271(12) Uani 1 1 d . . . H50A H 0.5387 -0.0254 0.7724 0.033 Uiso 1 1 calc R . . C51 C 0.4411(4) 0.0469(2) 0.7760(3) 0.0248(12) Uani 1 1 d . . . H51A H 0.4565 0.0588 0.8294 0.030 Uiso 1 1 calc R . . C52 C 0.3714(4) 0.0798(2) 0.7321(3) 0.0215(11) Uani 1 1 d . . . H52A H 0.3392 0.1145 0.7553 0.026 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 0.01232(11) 0.01694(11) 0.01805(12) -0.00061(8) -0.00114(8) -0.00054(8) Os2 0.01218(11) 0.01420(11) 0.01796(12) -0.00082(7) -0.00152(8) -0.00035(7) Os3 0.01441(11) 0.01491(11) 0.02113(12) -0.00156(8) -0.00029(9) -0.00195(8) Re1 0.01665(12) 0.01664(11) 0.01993(13) 0.00194(8) -0.00049(9) 0.00123(8) S1 0.0142(6) 0.0158(5) 0.0197(6) 0.0001(4) -0.0009(5) 0.0007(4) P1 0.0150(6) 0.0169(6) 0.0205(7) -0.0017(5) -0.0010(5) -0.0011(5) P2 0.0136(6) 0.0148(6) 0.0212(7) -0.0019(5) -0.0014(5) 0.0002(5) O1 0.028(2) 0.0248(19) 0.022(2) 0.0014(15) -0.0009(16) 0.0002(16) O2 0.024(2) 0.023(2) 0.031(2) -0.0069(16) 0.0016(17) -0.0040(15) O3 0.036(2) 0.039(2) 0.024(2) 0.0057(18) 0.0034(18) 0.0054(19) O4 0.025(2) 0.039(2) 0.017(2) -0.0020(16) 0.0012(16) 0.0015(17) O5 0.018(2) 0.0207(18) 0.046(3) 0.0006(17) -0.0104(18) 0.0006(15) O6 0.028(2) 0.025(2) 0.040(2) -0.0111(17) -0.0034(18) 0.0043(17) O7 0.045(3) 0.030(2) 0.035(3) 0.0015(18) 0.009(2) -0.0134(19) O8 0.024(2) 0.030(2) 0.024(2) -0.0057(15) -0.0031(17) -0.0039(16) O9 0.041(3) 0.050(3) 0.031(3) 0.011(2) 0.010(2) 0.003(2) O10 0.051(3) 0.017(2) 0.045(3) 0.0058(17) 0.001(2) 0.0080(18) O11 0.026(2) 0.034(2) 0.032(2) 0.0017(17) -0.0106(19) 0.0032(17) N1 0.022(2) 0.017(2) 0.016(2) 0.0022(16) 0.0012(17) -0.0016(17) C1 0.014(3) 0.016(2) 0.030(3) -0.001(2) 0.001(2) -0.0034(19) C2 0.015(3) 0.019(3) 0.027(3) -0.001(2) 0.001(2) 0.001(2) C3 0.017(3) 0.028(3) 0.019(3) 0.001(2) 0.000(2) 0.001(2) C4 0.012(3) 0.020(2) 0.029(3) 0.004(2) -0.004(2) 0.000(2) C5 0.015(3) 0.019(2) 0.022(3) -0.0008(19) -0.004(2) 0.0026(19) C6 0.014(3) 0.019(3) 0.037(3) -0.003(2) -0.001(2) 0.001(2) C7 0.020(3) 0.024(3) 0.025(3) 0.001(2) 0.000(2) -0.006(2) C8 0.016(3) 0.018(2) 0.037(4) 0.000(2) 0.006(2) -0.004(2) C9 0.031(3) 0.027(3) 0.024(3) 0.003(2) 0.000(3) 0.002(2) C10 0.029(3) 0.023(3) 0.022(3) 0.005(2) 0.004(2) 0.000(2) C11 0.020(3) 0.020(3) 0.027(3) 0.004(2) -0.002(2) 0.005(2) C12 0.018(3) 0.011(2) 0.028(3) -0.0051(19) -0.002(2) -0.0017(19) C13 0.017(3) 0.021(3) 0.026(3) 0.000(2) 0.001(2) -0.002(2) C14 0.025(3) 0.027(3) 0.028(3) -0.002(2) 0.005(2) 0.000(2) C15 0.022(3) 0.023(3) 0.033(3) -0.006(2) 0.001(2) 0.005(2) C16 0.021(3) 0.018(2) 0.032(3) 0.000(2) -0.002(2) 0.004(2) C17 0.016(3) 0.022(3) 0.022(3) -0.001(2) -0.002(2) 0.003(2) C18 0.028(3) 0.021(3) 0.030(3) 0.000(2) -0.005(2) 0.000(2) C19 0.026(3) 0.027(3) 0.031(3) 0.004(2) 0.001(2) 0.005(2) C20 0.031(3) 0.033(3) 0.025(3) 0.003(2) 0.000(2) 0.012(2) C21 0.030(3) 0.038(3) 0.022(3) -0.003(2) -0.006(2) -0.001(3) C22 0.022(3) 0.026(3) 0.025(3) -0.001(2) 0.002(2) 0.000(2) C23 0.019(3) 0.016(2) 0.026(3) -0.0009(19) 0.006(2) -0.0072(19) C24 0.019(3) 0.022(3) 0.031(3) 0.000(2) 0.005(2) 0.000(2) C25 0.034(3) 0.020(3) 0.026(3) -0.001(2) 0.006(2) -0.003(2) C26 0.036(3) 0.020(3) 0.033(3) -0.004(2) 0.013(3) -0.002(2) C27 0.018(3) 0.020(3) 0.043(4) -0.003(2) 0.004(2) 0.001(2) C28 0.017(3) 0.022(3) 0.036(3) -0.004(2) -0.002(2) -0.001(2) C29 0.017(3) 0.018(2) 0.023(3) 0.0013(19) -0.006(2) -0.0026(19) C30 0.030(3) 0.021(3) 0.023(3) -0.005(2) 0.000(2) -0.001(2) C31 0.028(3) 0.030(3) 0.020(3) 0.007(2) -0.004(2) -0.008(2) C32 0.025(3) 0.020(3) 0.041(4) -0.001(2) -0.010(3) -0.005(2) C33 0.023(3) 0.031(3) 0.048(4) -0.016(3) 0.002(3) -0.006(2) C34 0.015(3) 0.031(3) 0.041(4) -0.008(2) 0.006(2) -0.003(2) C35 0.018(3) 0.020(2) 0.021(3) -0.0044(19) -0.003(2) -0.005(2) C36 0.021(3) 0.017(2) 0.032(3) -0.002(2) -0.002(2) -0.001(2) C37 0.021(3) 0.026(3) 0.035(3) -0.006(2) 0.002(2) -0.001(2) C38 0.023(3) 0.034(3) 0.025(3) 0.001(2) 0.004(2) -0.012(2) C39 0.022(3) 0.021(3) 0.029(3) 0.005(2) -0.004(2) -0.005(2) C40 0.020(3) 0.022(3) 0.027(3) 0.000(2) 0.000(2) 0.000(2) C41 0.023(3) 0.015(2) 0.023(3) -0.0031(19) 0.000(2) 0.002(2) C42 0.020(3) 0.021(2) 0.026(3) -0.002(2) -0.001(2) 0.002(2) C43 0.018(3) 0.031(3) 0.036(3) -0.001(2) -0.003(2) -0.007(2) C44 0.027(3) 0.030(3) 0.029(3) -0.010(2) -0.007(2) -0.004(2) C45 0.026(3) 0.024(3) 0.033(3) -0.007(2) 0.002(2) -0.002(2) C46 0.017(3) 0.024(3) 0.032(3) -0.003(2) -0.004(2) -0.002(2) C47 0.015(3) 0.018(2) 0.028(3) 0.003(2) -0.003(2) 0.0014(19) C48 0.017(3) 0.025(3) 0.030(3) 0.001(2) 0.000(2) -0.002(2) C49 0.023(3) 0.020(3) 0.037(3) 0.003(2) 0.002(2) 0.008(2) C50 0.019(3) 0.025(3) 0.037(3) 0.009(2) -0.004(2) 0.002(2) C51 0.023(3) 0.024(3) 0.027(3) 0.007(2) -0.005(2) -0.004(2) C52 0.018(3) 0.016(2) 0.030(3) 0.001(2) 0.000(2) 0.000(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 C2 1.894(5) . ? Os1 C3 1.943(5) . ? Os1 C1 1.945(6) . ? Os1 P1 2.3584(13) . ? Os1 Os3 2.8833(3) . ? Os1 Os2 2.8896(3) . ? Os2 C4 1.887(6) . ? Os2 C5 1.902(5) . ? Os2 P2 2.3847(12) . ? Os2 S1 2.4060(12) . ? Os2 Os3 2.7980(3) . ? Os2 Re1 2.8943(3) . ? Os3 C6 1.916(5) . ? Os3 C7 1.919(5) . ? Os3 C8 1.929(6) . ? Os3 S1 2.4113(12) . ? Os3 Re1 2.9320(3) . ? Re1 C11 1.903(6) . ? Re1 C10 1.914(5) . ? Re1 C9 1.931(6) . ? Re1 N1 2.227(4) . ? S1 C12 1.771(5) . ? P1 C23 1.829(5) . ? P1 C17 1.833(5) . ? P1 C29 1.834(5) . ? P2 C41 1.836(5) . ? P2 C47 1.837(5) . ? P2 C35 1.860(5) . ? O1 C1 1.136(7) . ? O2 C2 1.140(6) . ? O3 C3 1.136(7) . ? O4 C4 1.150(7) . ? O5 C5 1.164(6) . ? O6 C6 1.140(6) . ? O7 C7 1.136(7) . ? O8 C8 1.136(7) . ? O9 C9 1.148(7) . ? O10 C10 1.144(7) . ? O11 C11 1.149(7) . ? N1 C16 1.350(7) . ? N1 C12 1.352(7) . ? C12 C13 1.398(8) . ? C13 C14 1.379(8) . ? C13 H13A 0.9500 . ? C14 C15 1.395(8) . ? C14 H14A 0.9500 . ? C15 C16 1.381(8) . ? C15 H15A 0.9500 . ? C16 H16A 0.9500 . ? C17 C22 1.388(8) . ? C17 C18 1.405(7) . ? C18 C19 1.384(8) . ? C18 H18A 0.9500 . ? C19 C20 1.379(8) . ? C19 H19A 0.9500 . ? C20 C21 1.370(9) . ? C20 H20A 0.9500 . ? C21 C22 1.389(8) . ? C21 H21A 0.9500 . ? C22 H22A 0.9500 . ? C23 C24 1.379(8) . ? C23 C28 1.409(8) . ? C24 C25 1.390(8) . ? C24 H24A 0.9500 . ? C25 C26 1.387(9) . ? C25 H25A 0.9500 . ? C26 C27 1.383(9) . ? C26 H26A 0.9500 . ? C27 C28 1.384(8) . ? C27 H27A 0.9500 . ? C28 H28A 0.9500 . ? C29 C30 1.385(8) . ? C29 C34 1.397(8) . ? C30 C31 1.401(7) . ? C30 H30A 0.9500 . ? C31 C32 1.379(8) . ? C31 H31A 0.9500 . ? C32 C33 1.384(9) . ? C32 H32A 0.9500 . ? C33 C34 1.369(8) . ? C33 H33A 0.9500 . ? C34 H34A 0.9500 . ? C35 C36 1.377(7) . ? C35 C40 1.395(7) . ? C36 C37 1.383(8) . ? C36 H36A 0.9500 . ? C37 C38 1.377(8) . ? C37 H37A 0.9500 . ? C38 C39 1.384(8) . ? C38 H38A 0.9500 . ? C39 C40 1.388(8) . ? C39 H39A 0.9500 . ? C40 H40A 0.9500 . ? C41 C42 1.382(8) . ? C41 C46 1.399(8) . ? C42 C43 1.389(8) . ? C42 H42A 0.9500 . ? C43 C44 1.374(8) . ? C43 H43A 0.9500 . ? C44 C45 1.395(8) . ? C44 H44A 0.9500 . ? C45 C46 1.374(8) . ? C45 H45A 0.9500 . ? C46 H46A 0.9500 . ? C47 C48 1.392(7) . ? C47 C52 1.396(8) . ? C48 C49 1.392(8) . ? C48 H48A 0.9500 . ? C49 C50 1.391(8) . ? C49 H49A 0.9500 . ? C50 C51 1.391(8) . ? C50 H50A 0.9500 . ? C51 C52 1.379(7) . ? C51 H51A 0.9500 . ? C52 H52A 0.9500 . ? 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 95.6(2) . . ? C2 Os1 C1 98.6(2) . . ? C3 Os1 C1 165.7(2) . . ? C2 Os1 P1 88.92(16) . . ? C3 Os1 P1 88.56(16) . . ? C1 Os1 P1 90.54(15) . . ? C2 Os1 Os3 151.98(15) . . ? C3 Os1 Os3 85.19(16) . . ? C1 Os1 Os3 82.81(15) . . ? P1 Os1 Os3 119.09(3) . . ? C2 Os1 Os2 94.02(15) . . ? C3 Os1 Os2 87.89(16) . . ? C1 Os1 Os2 92.26(15) . . ? P1 Os1 Os2 175.59(3) . . ? Os3 Os1 Os2 57.982(7) . . ? C4 Os2 C5 87.9(2) . . ? C4 Os2 P2 94.94(16) . . ? C5 Os2 P2 83.24(15) . . ? C4 Os2 S1 166.13(16) . . ? C5 Os2 S1 104.59(16) . . ? P2 Os2 S1 92.47(4) . . ? C4 Os2 Os3 113.50(15) . . ? C5 Os2 Os3 123.62(14) . . ? P2 Os2 Os3 139.83(3) . . ? S1 Os2 Os3 54.58(3) . . ? C4 Os2 Os1 79.83(15) . . ? C5 Os2 Os1 167.61(16) . . ? P2 Os2 Os1 99.70(3) . . ? S1 Os2 Os1 87.37(3) . . ? Os3 Os2 Os1 60.895(7) . . ? C4 Os2 Re1 98.62(15) . . ? C5 Os2 Re1 63.64(14) . . ? P2 Os2 Re1 143.46(3) . . ? S1 Os2 Re1 82.11(3) . . ? Os3 Os2 Re1 61.978(8) . . ? Os1 Os2 Re1 115.991(9) . . ? C6 Os3 C7 90.3(2) . . ? C6 Os3 C8 95.1(2) . . ? C7 Os3 C8 97.1(2) . . ? C6 Os3 S1 95.80(17) . . ? C7 Os3 S1 170.21(16) . . ? C8 Os3 S1 89.97(15) . . ? C6 Os3 Os2 121.26(16) . . ? C7 Os3 Os2 115.82(16) . . ? C8 Os3 Os2 128.62(15) . . ? S1 Os3 Os2 54.40(3) . . ? C6 Os3 Os1 176.75(16) . . ? C7 Os3 Os1 86.56(16) . . ? C8 Os3 Os1 84.39(16) . . ? S1 Os3 Os1 87.42(3) . . ? Os2 Os3 Os1 61.123(7) . . ? C6 Os3 Re1 66.08(16) . . ? C7 Os3 Re1 94.35(16) . . ? C8 Os3 Re1 158.06(16) . . ? S1 Os3 Re1 81.22(3) . . ? Os2 Os3 Re1 60.624(7) . . ? Os1 Os3 Re1 115.008(9) . . ? C11 Re1 C10 84.2(2) . . ? C11 Re1 C9 89.2(2) . . ? C10 Re1 C9 90.3(2) . . ? C11 Re1 N1 96.1(2) . . ? C10 Re1 N1 93.0(2) . . ? C9 Re1 N1 174.0(2) . . ? C11 Re1 Os2 111.30(15) . . ? C10 Re1 Os2 164.50(18) . . ? C9 Re1 Os2 90.07(17) . . ? N1 Re1 Os2 85.41(11) . . ? C11 Re1 Os3 168.62(15) . . ? C10 Re1 Os3 107.11(18) . . ? C9 Re1 Os3 89.45(18) . . ? N1 Re1 Os3 84.80(11) . . ? Os2 Re1 Os3 57.397(7) . . ? C12 S1 Os2 107.93(18) . . ? C12 S1 Os3 105.15(17) . . ? Os2 S1 Os3 71.02(3) . . ? C23 P1 C17 101.8(2) . . ? C23 P1 C29 103.4(2) . . ? C17 P1 C29 104.9(2) . . ? C23 P1 Os1 114.23(17) . . ? C17 P1 Os1 111.61(18) . . ? C29 P1 Os1 119.06(17) . . ? C41 P2 C47 106.0(2) . . ? C41 P2 C35 103.7(2) . . ? C47 P2 C35 97.9(2) . . ? C41 P2 Os2 110.69(17) . . ? C47 P2 Os2 121.49(17) . . ? C35 P2 Os2 115.06(16) . . ? C16 N1 C12 117.5(5) . . ? C16 N1 Re1 119.1(3) . . ? C12 N1 Re1 123.3(4) . . ? O1 C1 Os1 173.3(4) . . ? O2 C2 Os1 179.6(5) . . ? O3 C3 Os1 175.7(5) . . ? O4 C4 Os2 176.6(5) . . ? O5 C5 Os2 162.8(4) . . ? O6 C6 Os3 167.4(5) . . ? O7 C7 Os3 176.4(5) . . ? O8 C8 Os3 173.5(5) . . ? O9 C9 Re1 179.4(5) . . ? O10 C10 Re1 179.1(5) . . ? O11 C11 Re1 178.4(5) . . ? N1 C12 C13 121.6(5) . . ? N1 C12 S1 120.7(4) . . ? C13 C12 S1 117.7(4) . . ? C14 C13 C12 120.4(5) . . ? C14 C13 H13A 119.8 . . ? C12 C13 H13A 119.8 . . ? C13 C14 C15 118.0(5) . . ? C13 C14 H14A 121.0 . . ? C15 C14 H14A 121.0 . . ? C16 C15 C14 118.9(5) . . ? C16 C15 H15A 120.6 . . ? C14 C15 H15A 120.6 . . ? N1 C16 C15 123.6(5) . . ? N1 C16 H16A 118.2 . . ? C15 C16 H16A 118.2 . . ? C22 C17 C18 119.0(5) . . ? C22 C17 P1 124.3(4) . . ? C18 C17 P1 116.6(4) . . ? C19 C18 C17 120.3(5) . . ? C19 C18 H18A 119.9 . . ? C17 C18 H18A 119.9 . . ? C20 C19 C18 119.6(5) . . ? C20 C19 H19A 120.2 . . ? C18 C19 H19A 120.2 . . ? C21 C20 C19 120.8(5) . . ? C21 C20 H20A 119.6 . . ? C19 C20 H20A 119.6 . . ? C20 C21 C22 120.3(5) . . ? C20 C21 H21A 119.9 . . ? C22 C21 H21A 119.9 . . ? C17 C22 C21 120.0(5) . . ? C17 C22 H22A 120.0 . . ? C21 C22 H22A 120.0 . . ? C24 C23 C28 117.9(5) . . ? C24 C23 P1 122.9(4) . . ? C28 C23 P1 119.2(4) . . ? C23 C24 C25 121.6(5) . . ? C23 C24 H24A 119.2 . . ? C25 C24 H24A 119.2 . . ? C26 C25 C24 119.7(5) . . ? C26 C25 H25A 120.1 . . ? C24 C25 H25A 120.1 . . ? C27 C26 C25 119.8(5) . . ? C27 C26 H26A 120.1 . . ? C25 C26 H26A 120.1 . . ? C26 C27 C28 120.2(5) . . ? C26 C27 H27A 119.9 . . ? C28 C27 H27A 119.9 . . ? C27 C28 C23 120.8(5) . . ? C27 C28 H28A 119.6 . . ? C23 C28 H28A 119.6 . . ? C30 C29 C34 118.2(5) . . ? C30 C29 P1 122.6(4) . . ? C34 C29 P1 119.2(4) . . ? C29 C30 C31 120.1(5) . . ? C29 C30 H30A 120.0 . . ? C31 C30 H30A 120.0 . . ? C32 C31 C30 120.5(5) . . ? C32 C31 H31A 119.7 . . ? C30 C31 H31A 119.7 . . ? C31 C32 C33 119.4(5) . . ? C31 C32 H32A 120.3 . . ? C33 C32 H32A 120.3 . . ? C34 C33 C32 120.2(5) . . ? C34 C33 H33A 119.9 . . ? C32 C33 H33A 119.9 . . ? C33 C34 C29 121.5(5) . . ? C33 C34 H34A 119.2 . . ? C29 C34 H34A 119.2 . . ? C36 C35 C40 118.6(5) . . ? C36 C35 P2 123.2(4) . . ? C40 C35 P2 118.2(4) . . ? C35 C36 C37 120.9(5) . . ? C35 C36 H36A 119.6 . . ? C37 C36 H36A 119.6 . . ? C38 C37 C36 120.6(5) . . ? C38 C37 H37A 119.7 . . ? C36 C37 H37A 119.7 . . ? C37 C38 C39 119.4(5) . . ? C37 C38 H38A 120.3 . . ? C39 C38 H38A 120.3 . . ? C38 C39 C40 119.9(5) . . ? C38 C39 H39A 120.0 . . ? C40 C39 H39A 120.0 . . ? C39 C40 C35 120.6(5) . . ? C39 C40 H40A 119.7 . . ? C35 C40 H40A 119.7 . . ? C42 C41 C46 119.4(5) . . ? C42 C41 P2 120.6(4) . . ? C46 C41 P2 119.6(4) . . ? C41 C42 C43 119.9(5) . . ? C41 C42 H42A 120.1 . . ? C43 C42 H42A 120.1 . . ? C44 C43 C42 120.6(5) . . ? C44 C43 H43A 119.7 . . ? C42 C43 H43A 119.7 . . ? C43 C44 C45 119.7(5) . . ? C43 C44 H44A 120.1 . . ? C45 C44 H44A 120.1 . . ? C46 C45 C44 119.9(5) . . ? C46 C45 H45A 120.1 . . ? C44 C45 H45A 120.1 . . ? C45 C46 C41 120.4(5) . . ? C45 C46 H46A 119.8 . . ? C41 C46 H46A 119.8 . . ? C48 C47 C52 119.3(5) . . ? C48 C47 P2 124.6(4) . . ? C52 C47 P2 116.1(4) . . ? C47 C48 C49 120.4(5) . . ? C47 C48 H48A 119.8 . . ? C49 C48 H48A 119.8 . . ? C50 C49 C48 119.7(5) . . ? C50 C49 H49A 120.1 . . ? C48 C49 H49A 120.1 . . ? C51 C50 C49 119.8(5) . . ? C51 C50 H50A 120.1 . . ? C49 C50 H50A 120.1 . . ? C52 C51 C50 120.4(5) . . ? C52 C51 H51A 119.8 . . ? C50 C51 H51A 119.8 . . ? C51 C52 C47 120.3(5) . . ? C51 C52 H52A 119.9 . . ? C47 C52 H52A 119.9 . . ? 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 C4 -56.9(2) . . . . ? C3 Os1 Os2 C4 38.6(2) . . . . ? C1 Os1 Os2 C4 -155.6(2) . . . . ? P1 Os1 Os2 C4 75.0(5) . . . . ? Os3 Os1 Os2 C4 124.29(15) . . . . ? C2 Os1 Os2 C5 -66.3(7) . . . . ? C3 Os1 Os2 C5 29.2(7) . . . . ? C1 Os1 Os2 C5 -165.1(7) . . . . ? P1 Os1 Os2 C5 65.5(8) . . . . ? Os3 Os1 Os2 C5 114.8(7) . . . . ? C2 Os1 Os2 P2 36.47(17) . . . . ? C3 Os1 Os2 P2 131.98(16) . . . . ? C1 Os1 Os2 P2 -62.31(15) . . . . ? P1 Os1 Os2 P2 168.3(4) . . . . ? Os3 Os1 Os2 P2 -142.38(3) . . . . ? C2 Os1 Os2 S1 128.52(17) . . . . ? C3 Os1 Os2 S1 -135.97(16) . . . . ? C1 Os1 Os2 S1 29.75(15) . . . . ? P1 Os1 Os2 S1 -99.6(4) . . . . ? Os3 Os1 Os2 S1 -50.32(3) . . . . ? C2 Os1 Os2 Os3 178.84(16) . . . . ? C3 Os1 Os2 Os3 -85.65(16) . . . . ? C1 Os1 Os2 Os3 80.07(14) . . . . ? P1 Os1 Os2 Os3 -49.3(4) . . . . ? C2 Os1 Os2 Re1 -151.57(16) . . . . ? C3 Os1 Os2 Re1 -56.06(16) . . . . ? C1 Os1 Os2 Re1 109.65(14) . . . . ? P1 Os1 Os2 Re1 -19.7(4) . . . . ? Os3 Os1 Os2 Re1 29.585(10) . . . . ? C4 Os2 Os3 C6 115.0(3) . . . . ? C5 Os2 Os3 C6 11.0(3) . . . . ? P2 Os2 Os3 C6 -113.7(2) . . . . ? S1 Os2 Os3 C6 -73.2(2) . . . . ? Os1 Os2 Os3 C6 177.4(2) . . . . ? Re1 Os2 Os3 C6 27.6(2) . . . . ? C4 Os2 Os3 C7 7.5(2) . . . . ? C5 Os2 Os3 C7 -96.5(3) . . . . ? P2 Os2 Os3 C7 138.82(19) . . . . ? S1 Os2 Os3 C7 179.31(19) . . . . ? Os1 Os2 Os3 C7 69.94(18) . . . . ? Re1 Os2 Os3 C7 -79.88(18) . . . . ? C4 Os2 Os3 C8 -116.8(3) . . . . ? C5 Os2 Os3 C8 139.2(3) . . . . ? P2 Os2 Os3 C8 14.6(2) . . . . ? S1 Os2 Os3 C8 55.1(2) . . . . ? Os1 Os2 Os3 C8 -54.3(2) . . . . ? Re1 Os2 Os3 C8 155.9(2) . . . . ? C4 Os2 Os3 S1 -171.83(17) . . . . ? C5 Os2 Os3 S1 84.2(2) . . . . ? P2 Os2 Os3 S1 -40.49(6) . . . . ? Os1 Os2 Os3 S1 -109.36(3) . . . . ? Re1 Os2 Os3 S1 100.82(3) . . . . ? C4 Os2 Os3 Os1 -62.46(16) . . . . ? C5 Os2 Os3 Os1 -166.48(19) . . . . ? P2 Os2 Os3 Os1 68.87(5) . . . . ? S1 Os2 Os3 Os1 109.36(3) . . . . ? Re1 Os2 Os3 Os1 -149.820(10) . . . . ? C4 Os2 Os3 Re1 87.36(16) . . . . ? C5 Os2 Os3 Re1 -16.66(19) . . . . ? P2 Os2 Os3 Re1 -141.31(5) . . . . ? S1 Os2 Os3 Re1 -100.82(3) . . . . ? Os1 Os2 Os3 Re1 149.820(10) . . . . ? C2 Os1 Os3 C6 -140(3) . . . . ? C3 Os1 Os3 C6 -47(3) . . . . ? C1 Os1 Os3 C6 125(3) . . . . ? P1 Os1 Os3 C6 38(3) . . . . ? Os2 Os1 Os3 C6 -138(3) . . . . ? C2 Os1 Os3 C7 -124.6(4) . . . . ? C3 Os1 Os3 C7 -31.6(2) . . . . ? C1 Os1 Os3 C7 140.7(2) . . . . ? P1 Os1 Os3 C7 54.07(17) . . . . ? Os2 Os1 Os3 C7 -122.11(16) . . . . ? C2 Os1 Os3 C8 137.9(4) . . . . ? C3 Os1 Os3 C8 -129.1(2) . . . . ? C1 Os1 Os3 C8 43.2(2) . . . . ? P1 Os1 Os3 C8 -43.44(16) . . . . ? Os2 Os1 Os3 C8 140.39(15) . . . . ? C2 Os1 Os3 S1 47.7(3) . . . . ? C3 Os1 Os3 S1 140.68(16) . . . . ? C1 Os1 Os3 S1 -47.06(15) . . . . ? P1 Os1 Os3 S1 -133.66(5) . . . . ? Os2 Os1 Os3 S1 50.17(3) . . . . ? C2 Os1 Os3 Os2 -2.5(3) . . . . ? C3 Os1 Os3 Os2 90.51(16) . . . . ? C1 Os1 Os3 Os2 -97.23(15) . . . . ? P1 Os1 Os3 Os2 176.18(4) . . . . ? C2 Os1 Os3 Re1 -31.4(3) . . . . ? C3 Os1 Os3 Re1 61.61(16) . . . . ? C1 Os1 Os3 Re1 -126.13(15) . . . . ? P1 Os1 Os3 Re1 147.27(4) . . . . ? Os2 Os1 Os3 Re1 -28.908(9) . . . . ? C4 Os2 Re1 C11 66.4(2) . . . . ? C5 Os2 Re1 C11 -17.0(3) . . . . ? P2 Os2 Re1 C11 -44.16(19) . . . . ? S1 Os2 Re1 C11 -127.60(18) . . . . ? Os3 Os2 Re1 C11 178.48(18) . . . . ? Os1 Os2 Re1 C11 149.23(18) . . . . ? C4 Os2 Re1 C10 -114.2(6) . . . . ? C5 Os2 Re1 C10 162.5(6) . . . . ? P2 Os2 Re1 C10 135.3(6) . . . . ? S1 Os2 Re1 C10 51.8(6) . . . . ? Os3 Os2 Re1 C10 -2.1(6) . . . . ? Os1 Os2 Re1 C10 -31.3(6) . . . . ? C4 Os2 Re1 C9 -22.8(2) . . . . ? C5 Os2 Re1 C9 -106.1(3) . . . . ? P2 Os2 Re1 C9 -133.33(18) . . . . ? S1 Os2 Re1 C9 143.22(18) . . . . ? Os3 Os2 Re1 C9 89.31(18) . . . . ? Os1 Os2 Re1 C9 60.06(18) . . . . ? C4 Os2 Re1 N1 161.15(19) . . . . ? C5 Os2 Re1 N1 77.8(2) . . . . ? P2 Os2 Re1 N1 50.60(12) . . . . ? S1 Os2 Re1 N1 -32.84(11) . . . . ? Os3 Os2 Re1 N1 -86.76(11) . . . . ? Os1 Os2 Re1 N1 -116.01(11) . . . . ? C4 Os2 Re1 Os3 -112.09(15) . . . . ? C5 Os2 Re1 Os3 164.55(18) . . . . ? P2 Os2 Re1 Os3 137.36(6) . . . . ? S1 Os2 Re1 Os3 53.91(3) . . . . ? Os1 Os2 Re1 Os3 -29.253(9) . . . . ? C6 Os3 Re1 C11 -161.5(9) . . . . ? C7 Os3 Re1 C11 110.1(9) . . . . ? C8 Os3 Re1 C11 -128.5(9) . . . . ? S1 Os3 Re1 C11 -61.1(8) . . . . ? Os2 Os3 Re1 C11 -7.2(8) . . . . ? Os1 Os3 Re1 C11 21.9(8) . . . . ? C6 Os3 Re1 C10 25.1(3) . . . . ? C7 Os3 Re1 C10 -63.3(2) . . . . ? C8 Os3 Re1 C10 58.1(4) . . . . ? S1 Os3 Re1 C10 125.50(18) . . . . ? Os2 Os3 Re1 C10 179.42(17) . . . . ? Os1 Os3 Re1 C10 -151.52(17) . . . . ? C6 Os3 Re1 C9 115.3(2) . . . . ? C7 Os3 Re1 C9 26.9(2) . . . . ? C8 Os3 Re1 C9 148.3(4) . . . . ? S1 Os3 Re1 C9 -144.35(17) . . . . ? Os2 Os3 Re1 C9 -90.43(17) . . . . ? Os1 Os3 Re1 C9 -61.37(17) . . . . ? C6 Os3 Re1 N1 -66.4(2) . . . . ? C7 Os3 Re1 N1 -154.83(19) . . . . ? C8 Os3 Re1 N1 -33.4(4) . . . . ? S1 Os3 Re1 N1 33.96(11) . . . . ? Os2 Os3 Re1 N1 87.87(10) . . . . ? Os1 Os3 Re1 N1 116.93(10) . . . . ? C6 Os3 Re1 Os2 -154.30(18) . . . . ? C7 Os3 Re1 Os2 117.29(16) . . . . ? C8 Os3 Re1 Os2 -121.3(4) . . . . ? S1 Os3 Re1 Os2 -53.92(3) . . . . ? Os1 Os3 Re1 Os2 29.061(9) . . . . ? C4 Os2 S1 C12 133.3(7) . . . . ? C5 Os2 S1 C12 -20.8(2) . . . . ? P2 Os2 S1 C12 -104.47(17) . . . . ? Os3 Os2 S1 C12 100.32(17) . . . . ? Os1 Os2 S1 C12 155.93(17) . . . . ? Re1 Os2 S1 C12 39.23(17) . . . . ? C4 Os2 S1 Os3 32.9(6) . . . . ? C5 Os2 S1 Os3 -121.14(15) . . . . ? P2 Os2 S1 Os3 155.21(4) . . . . ? Os1 Os2 S1 Os3 55.61(2) . . . . ? Re1 Os2 S1 Os3 -61.090(19) . . . . ? C6 Os3 S1 C12 20.5(2) . . . . ? C7 Os3 S1 C12 -107.8(10) . . . . ? C8 Os3 S1 C12 115.7(2) . . . . ? Os2 Os3 S1 C12 -104.13(18) . . . . ? Os1 Os3 S1 C12 -159.92(18) . . . . ? Re1 Os3 S1 C12 -44.12(18) . . . . ? C6 Os3 S1 Os2 124.67(17) . . . . ? C7 Os3 S1 Os2 -3.7(10) . . . . ? C8 Os3 S1 Os2 -140.17(16) . . . . ? Os1 Os3 S1 Os2 -55.79(2) . . . . ? Re1 Os3 S1 Os2 60.01(2) . . . . ? C2 Os1 P1 C23 30.3(2) . . . . ? C3 Os1 P1 C23 -65.4(2) . . . . ? C1 Os1 P1 C23 128.9(2) . . . . ? Os3 Os1 P1 C23 -149.05(18) . . . . ? Os2 Os1 P1 C23 -101.7(5) . . . . ? C2 Os1 P1 C17 -84.5(2) . . . . ? C3 Os1 P1 C17 179.8(2) . . . . ? C1 Os1 P1 C17 14.1(2) . . . . ? Os3 Os1 P1 C17 96.13(18) . . . . ? Os2 Os1 P1 C17 143.5(4) . . . . ? C2 Os1 P1 C29 153.1(3) . . . . ? C3 Os1 P1 C29 57.4(3) . . . . ? C1 Os1 P1 C29 -108.4(2) . . . . ? Os3 Os1 P1 C29 -26.3(2) . . . . ? Os2 Os1 P1 C29 21.1(5) . . . . ? C4 Os2 P2 C41 -27.0(2) . . . . ? C5 Os2 P2 C41 60.4(2) . . . . ? S1 Os2 P2 C41 164.76(19) . . . . ? Os3 Os2 P2 C41 -163.25(18) . . . . ? Os1 Os2 P2 C41 -107.48(18) . . . . ? Re1 Os2 P2 C41 84.71(19) . . . . ? C4 Os2 P2 C47 98.2(3) . . . . ? C5 Os2 P2 C47 -174.4(3) . . . . ? S1 Os2 P2 C47 -70.0(2) . . . . ? Os3 Os2 P2 C47 -38.0(2) . . . . ? Os1 Os2 P2 C47 17.7(2) . . . . ? Re1 Os2 P2 C47 -150.1(2) . . . . ? C4 Os2 P2 C35 -144.1(2) . . . . ? C5 Os2 P2 C35 -56.7(2) . . . . ? S1 Os2 P2 C35 47.67(19) . . . . ? Os3 Os2 P2 C35 79.65(19) . . . . ? Os1 Os2 P2 C35 135.43(18) . . . . ? Re1 Os2 P2 C35 -32.4(2) . . . . ? C11 Re1 N1 C16 -40.0(4) . . . . ? C10 Re1 N1 C16 44.5(4) . . . . ? C9 Re1 N1 C16 167.9(18) . . . . ? Os2 Re1 N1 C16 -151.0(4) . . . . ? Os3 Re1 N1 C16 151.4(4) . . . . ? C11 Re1 N1 C12 142.6(4) . . . . ? C10 Re1 N1 C12 -132.9(4) . . . . ? C9 Re1 N1 C12 -9(2) . . . . ? Os2 Re1 N1 C12 31.6(4) . . . . ? Os3 Re1 N1 C12 -26.0(4) . . . . ? C2 Os1 C1 O1 122(4) . . . . ? C3 Os1 C1 O1 -53(4) . . . . ? P1 Os1 C1 O1 33(4) . . . . ? Os3 Os1 C1 O1 -86(4) . . . . ? Os2 Os1 C1 O1 -144(4) . . . . ? C3 Os1 C2 O2 -9(64) . . . . ? C1 Os1 C2 O2 172(100) . . . . ? P1 Os1 C2 O2 -97(64) . . . . ? Os3 Os1 C2 O2 81(65) . . . . ? Os2 Os1 C2 O2 79(64) . . . . ? C2 Os1 C3 O3 -109(7) . . . . ? C1 Os1 C3 O3 66(7) . . . . ? P1 Os1 C3 O3 -20(7) . . . . ? Os3 Os1 C3 O3 99(7) . . . . ? Os2 Os1 C3 O3 157(7) . . . . ? C5 Os2 C4 O4 -12(8) . . . . ? P2 Os2 C4 O4 71(8) . . . . ? S1 Os2 C4 O4 -167(7) . . . . ? Os3 Os2 C4 O4 -138(8) . . . . ? Os1 Os2 C4 O4 170(8) . . . . ? Re1 Os2 C4 O4 -75(8) . . . . ? C4 Os2 C5 O5 54.0(16) . . . . ? P2 Os2 C5 O5 -41.2(15) . . . . ? S1 Os2 C5 O5 -132.0(15) . . . . ? Os3 Os2 C5 O5 171.1(15) . . . . ? Os1 Os2 C5 O5 63.4(19) . . . . ? Re1 Os2 C5 O5 154.7(16) . . . . ? C7 Os3 C6 O6 -80(2) . . . . ? C8 Os3 C6 O6 18(2) . . . . ? S1 Os3 C6 O6 108(2) . . . . ? Os2 Os3 C6 O6 160(2) . . . . ? Os1 Os3 C6 O6 -64(5) . . . . ? Re1 Os3 C6 O6 -174(2) . . . . ? C6 Os3 C7 O7 4(8) . . . . ? C8 Os3 C7 O7 -91(8) . . . . ? S1 Os3 C7 O7 133(8) . . . . ? Os2 Os3 C7 O7 130(8) . . . . ? Os1 Os3 C7 O7 -175(8) . . . . ? Re1 Os3 C7 O7 70(8) . . . . ? C6 Os3 C8 O8 49(4) . . . . ? C7 Os3 C8 O8 140(4) . . . . ? S1 Os3 C8 O8 -47(4) . . . . ? Os2 Os3 C8 O8 -89(4) . . . . ? Os1 Os3 C8 O8 -134(4) . . . . ? Re1 Os3 C8 O8 19(4) . . . . ? C11 Re1 C9 O9 -69(61) . . . . ? C10 Re1 C9 O9 -153(61) . . . . ? N1 Re1 C9 O9 83(61) . . . . ? Os2 Re1 C9 O9 42(61) . . . . ? Os3 Re1 C9 O9 99(61) . . . . ? C11 Re1 C10 O10 58(38) . . . . ? C9 Re1 C10 O10 147(38) . . . . ? N1 Re1 C10 O10 -38(38) . . . . ? Os2 Re1 C10 O10 -122(38) . . . . ? Os3 Re1 C10 O10 -123(38) . . . . ? C10 Re1 C11 O11 95(16) . . . . ? C9 Re1 C11 O11 5(16) . . . . ? N1 Re1 C11 O11 -172(100) . . . . ? Os2 Re1 C11 O11 -85(16) . . . . ? Os3 Re1 C11 O11 -78(16) . . . . ? C16 N1 C12 C13 -1.6(7) . . . . ? Re1 N1 C12 C13 175.8(4) . . . . ? C16 N1 C12 S1 176.7(4) . . . . ? Re1 N1 C12 S1 -5.9(5) . . . . ? Os2 S1 C12 N1 -31.5(4) . . . . ? Os3 S1 C12 N1 43.1(4) . . . . ? Os2 S1 C12 C13 146.9(4) . . . . ? Os3 S1 C12 C13 -138.6(4) . . . . ? N1 C12 C13 C14 0.0(8) . . . . ? S1 C12 C13 C14 -178.3(4) . . . . ? C12 C13 C14 C15 1.8(8) . . . . ? C13 C14 C15 C16 -2.0(8) . . . . ? C12 N1 C16 C15 1.4(8) . . . . ? Re1 N1 C16 C15 -176.1(4) . . . . ? C14 C15 C16 N1 0.4(8) . . . . ? C23 P1 C17 C22 119.3(5) . . . . ? C29 P1 C17 C22 11.8(5) . . . . ? Os1 P1 C17 C22 -118.5(4) . . . . ? C23 P1 C17 C18 -62.8(5) . . . . ? C29 P1 C17 C18 -170.3(4) . . . . ? Os1 P1 C17 C18 59.5(4) . . . . ? C22 C17 C18 C19 0.2(8) . . . . ? P1 C17 C18 C19 -177.8(4) . . . . ? C17 C18 C19 C20 0.5(9) . . . . ? C18 C19 C20 C21 -1.1(9) . . . . ? C19 C20 C21 C22 1.0(9) . . . . ? C18 C17 C22 C21 -0.4(8) . . . . ? P1 C17 C22 C21 177.6(4) . . . . ? C20 C21 C22 C17 -0.3(9) . . . . ? C17 P1 C23 C24 147.9(4) . . . . ? C29 P1 C23 C24 -103.4(4) . . . . ? Os1 P1 C23 C24 27.5(5) . . . . ? C17 P1 C23 C28 -29.7(5) . . . . ? C29 P1 C23 C28 78.9(4) . . . . ? Os1 P1 C23 C28 -150.2(4) . . . . ? C28 C23 C24 C25 1.9(8) . . . . ? P1 C23 C24 C25 -175.8(4) . . . . ? C23 C24 C25 C26 -1.4(8) . . . . ? C24 C25 C26 C27 -0.1(8) . . . . ? C25 C26 C27 C28 1.0(8) . . . . ? C26 C27 C28 C23 -0.4(8) . . . . ? C24 C23 C28 C27 -1.0(8) . . . . ? P1 C23 C28 C27 176.8(4) . . . . ? C23 P1 C29 C30 1.0(5) . . . . ? C17 P1 C29 C30 107.3(5) . . . . ? Os1 P1 C29 C30 -126.9(4) . . . . ? C23 P1 C29 C34 -179.4(4) . . . . ? C17 P1 C29 C34 -73.1(5) . . . . ? Os1 P1 C29 C34 52.6(5) . . . . ? C34 C29 C30 C31 -2.1(8) . . . . ? P1 C29 C30 C31 177.4(4) . . . . ? C29 C30 C31 C32 2.0(9) . . . . ? C30 C31 C32 C33 -0.6(9) . . . . ? C31 C32 C33 C34 -0.5(9) . . . . ? C32 C33 C34 C29 0.3(10) . . . . ? C30 C29 C34 C33 1.0(9) . . . . ? P1 C29 C34 C33 -178.6(5) . . . . ? C41 P2 C35 C36 -107.8(5) . . . . ? C47 P2 C35 C36 143.6(5) . . . . ? Os2 P2 C35 C36 13.2(5) . . . . ? C41 P2 C35 C40 71.3(5) . . . . ? C47 P2 C35 C40 -37.3(5) . . . . ? Os2 P2 C35 C40 -167.7(4) . . . . ? C40 C35 C36 C37 2.2(8) . . . . ? P2 C35 C36 C37 -178.7(4) . . . . ? C35 C36 C37 C38 -0.5(9) . . . . ? C36 C37 C38 C39 -1.9(9) . . . . ? C37 C38 C39 C40 2.5(9) . . . . ? C38 C39 C40 C35 -0.7(8) . . . . ? C36 C35 C40 C39 -1.6(8) . . . . ? P2 C35 C40 C39 179.2(4) . . . . ? C47 P2 C41 C42 124.3(4) . . . . ? C35 P2 C41 C42 21.8(5) . . . . ? Os2 P2 C41 C42 -102.1(4) . . . . ? C47 P2 C41 C46 -61.9(5) . . . . ? C35 P2 C41 C46 -164.4(4) . . . . ? Os2 P2 C41 C46 71.7(4) . . . . ? C46 C41 C42 C43 0.5(8) . . . . ? P2 C41 C42 C43 174.3(4) . . . . ? C41 C42 C43 C44 1.0(8) . . . . ? C42 C43 C44 C45 -0.6(9) . . . . ? C43 C44 C45 C46 -1.3(9) . . . . ? C44 C45 C46 C41 2.8(8) . . . . ? C42 C41 C46 C45 -2.4(8) . . . . ? P2 C41 C46 C45 -176.3(4) . . . . ? C41 P2 C47 C48 11.2(5) . . . . ? C35 P2 C47 C48 117.9(5) . . . . ? Os2 P2 C47 C48 -116.2(4) . . . . ? C41 P2 C47 C52 -168.0(4) . . . . ? C35 P2 C47 C52 -61.3(4) . . . . ? Os2 P2 C47 C52 64.7(4) . . . . ? C52 C47 C48 C49 -1.8(8) . . . . ? P2 C47 C48 C49 179.0(4) . . . . ? C47 C48 C49 C50 0.1(8) . . . . ? C48 C49 C50 C51 1.8(8) . . . . ? C49 C50 C51 C52 -2.1(8) . . . . ? C50 C51 C52 C47 0.4(8) . . . . ? C48 C47 C52 C51 1.6(8) . . . . ? P2 C47 C52 C51 -179.2(4) . . . . ? _diffrn_measured_fraction_theta_max 0.964 _diffrn_reflns_theta_full 68.03 _diffrn_measured_fraction_theta_full 0.964 _refine_diff_density_max 1.421 _refine_diff_density_min -0.817 _refine_diff_density_rms 0.135 # Attachment '- Compound 4.CIF' data_comp4 _database_code_depnum_ccdc_archive 'CCDC 748072' #TrackingRef '- Compound 4.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H4 Mn N O13 Os3 S' _chemical_formula_sum 'C18 H4 Mn N O13 Os3 S' _chemical_formula_weight 1099.82 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' N N 0.0061 0.0033 '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' S S 0.1246 0.1234 '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' Os Os -1.2165 7.6030 '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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.4909(3) _cell_length_b 10.1166(9) _cell_length_c 15.1573(11) _cell_angle_alpha 70.739(5) _cell_angle_beta 83.786(4) _cell_angle_gamma 88.325(6) _cell_volume 1221.87(15) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 4427 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description Block _exptl_crystal_colour Red _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.989 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 984 _exptl_absorpt_coefficient_mu 16.205 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.1948 _exptl_absorpt_correction_T_max 0.1948 _exptl_absorpt_process_details ; [North et al. (1968) Acta. Cryst. A24, 351] ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf-Nonius CAD4' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4822 _diffrn_reflns_av_R_equivalents 0.0164 _diffrn_reflns_av_sigmaI/netI 0.0362 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.43 _diffrn_reflns_theta_max 25.29 _reflns_number_total 4427 _reflns_number_gt 3671 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 Express (Enraf Nonius, 1994)' _computing_cell_refinement 'CAD4 Express (Enraf Nonius, 1994)' _computing_data_reduction 'CAD4 Express (Enraf Nonius, 1994)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0382P)^2^+1.7180P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4427 _refine_ls_number_parameters 334 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0387 _refine_ls_R_factor_gt 0.0267 _refine_ls_wR_factor_ref 0.0695 _refine_ls_wR_factor_gt 0.0672 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Os1 Os 0.28183(4) 0.77343(3) 0.12092(2) 0.03599(10) Uani 1 1 d . . . Os2 Os 0.17915(3) 0.48825(3) 0.175082(19) 0.02888(9) Uani 1 1 d . . . Os3 Os 0.35751(3) 0.56967(3) 0.292605(19) 0.02642(9) Uani 1 1 d . . . Mn1 Mn 0.15998(13) 0.32507(11) 0.36649(7) 0.0276(2) Uani 1 1 d . . . S1 S 0.4552(2) 0.4405(2) 0.19047(12) 0.0300(4) Uani 1 1 d . . . O1 O 0.5873(10) 0.7019(9) 0.0156(5) 0.090(3) Uani 1 1 d . . . O2 O 0.1440(13) 0.9145(10) -0.0643(6) 0.099(3) Uani 1 1 d . . . O3 O 0.4356(11) 1.0315(8) 0.1335(6) 0.086(3) Uani 1 1 d . . . O4 O -0.0209(8) 0.8280(8) 0.2354(5) 0.0628(19) Uani 1 1 d . . . O5 O 0.1765(8) 0.7333(7) 0.4074(4) 0.0527(16) Uani 1 1 d . . . O6 O 0.6399(8) 0.7634(7) 0.2640(6) 0.064(2) Uani 1 1 d . . . O7 O 0.5018(9) 0.3708(7) 0.4628(5) 0.064(2) Uani 1 1 d . . . O8 O -0.1666(8) 0.5688(9) 0.1923(6) 0.079(2) Uani 1 1 d . . . O9 O 0.1856(9) 0.5660(8) -0.0375(4) 0.065(2) Uani 1 1 d . . . O10 O 0.0871(10) 0.1926(8) 0.1923(5) 0.074(2) Uani 1 1 d . . . O11 O -0.0959(8) 0.5079(7) 0.4028(5) 0.0593(18) Uani 1 1 d . . . O12 O -0.0868(10) 0.1076(8) 0.4086(6) 0.080(2) Uani 1 1 d . . . O13 O 0.1893(8) 0.2116(7) 0.5694(4) 0.0551(17) Uani 1 1 d . . . N1 N 0.3523(8) 0.2084(6) 0.3327(4) 0.0326(14) Uani 1 1 d . . . C1 C 0.4780(12) 0.7232(10) 0.0556(6) 0.055(3) Uani 1 1 d . . . C2 C 0.1911(13) 0.8625(11) 0.0051(7) 0.059(3) Uani 1 1 d . . . C3 C 0.3789(13) 0.9357(10) 0.1289(7) 0.056(3) Uani 1 1 d . . . C4 C 0.0890(12) 0.8040(9) 0.1951(6) 0.044(2) Uani 1 1 d . . . C5 C 0.2424(9) 0.6706(9) 0.3642(5) 0.0364(18) Uani 1 1 d . . . C6 C 0.5366(10) 0.6915(9) 0.2714(6) 0.041(2) Uani 1 1 d . . . C7 C 0.4350(11) 0.4369(8) 0.4010(6) 0.0395(19) Uani 1 1 d . . . C8 C -0.0353(10) 0.5423(10) 0.1849(6) 0.044(2) Uani 1 1 d . . . C9 C 0.1882(10) 0.5374(10) 0.0416(6) 0.042(2) Uani 1 1 d . . . C10 C 0.1231(11) 0.2999(9) 0.1952(6) 0.043(2) Uani 1 1 d . . . C11 C 0.0062(10) 0.4403(9) 0.3877(5) 0.0384(19) Uani 1 1 d . . . C12 C 0.0117(11) 0.1928(9) 0.3896(6) 0.043(2) Uani 1 1 d . . . C13 C 0.1772(10) 0.2555(9) 0.4905(6) 0.042(2) Uani 1 1 d . . . C14 C 0.4700(9) 0.2649(8) 0.2644(5) 0.0305(16) Uani 1 1 d . . . C15 C 0.6048(10) 0.1924(8) 0.2486(6) 0.0394(19) Uani 1 1 d . . . H15 H 0.6832 0.2352 0.2006 0.047 Uiso 1 1 calc R . . C16 C 0.6214(12) 0.0549(9) 0.3055(6) 0.048(2) Uani 1 1 d . . . H16 H 0.7125 0.0047 0.2980 0.058 Uiso 1 1 calc R . . C17 C 0.4971(12) -0.0063(9) 0.3744(6) 0.049(2) Uani 1 1 d . . . H17 H 0.5023 -0.0994 0.4123 0.059 Uiso 1 1 calc R . . C18 C 0.3683(11) 0.0730(8) 0.3850(6) 0.041(2) Uani 1 1 d . . . H18 H 0.2866 0.0311 0.4311 0.050 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 0.04087(19) 0.02976(17) 0.03113(16) -0.00209(12) -0.00279(13) 0.00135(14) Os2 0.02862(16) 0.03198(17) 0.02702(15) -0.01050(12) -0.00481(11) 0.00119(12) Os3 0.02785(16) 0.02270(15) 0.02826(15) -0.00712(11) -0.00486(11) -0.00041(12) Mn1 0.0290(6) 0.0222(6) 0.0277(5) -0.0042(4) 0.0018(4) -0.0022(5) S1 0.0289(10) 0.0278(10) 0.0310(9) -0.0078(8) -0.0001(7) 0.0025(8) O1 0.090(6) 0.076(6) 0.066(5) 0.012(4) 0.039(5) 0.017(5) O2 0.135(8) 0.097(7) 0.057(5) -0.006(5) -0.044(5) 0.024(6) O3 0.118(7) 0.047(5) 0.089(6) -0.011(4) -0.027(5) -0.026(5) O4 0.049(4) 0.069(5) 0.071(5) -0.027(4) -0.002(3) 0.017(4) O5 0.056(4) 0.058(4) 0.053(4) -0.031(3) 0.000(3) 0.004(3) O6 0.034(4) 0.055(4) 0.114(6) -0.040(4) -0.006(4) -0.010(3) O7 0.083(5) 0.045(4) 0.060(4) -0.003(3) -0.039(4) 0.001(4) O8 0.040(4) 0.115(7) 0.113(6) -0.079(6) -0.019(4) 0.017(4) O9 0.075(5) 0.090(6) 0.031(3) -0.019(3) -0.010(3) 0.002(4) O10 0.106(7) 0.054(5) 0.069(5) -0.025(4) -0.022(4) -0.013(4) O11 0.050(4) 0.057(4) 0.065(4) -0.017(3) 0.006(3) 0.019(3) O12 0.072(5) 0.069(5) 0.087(6) -0.007(4) -0.014(4) -0.032(5) O13 0.070(5) 0.059(4) 0.032(3) -0.009(3) -0.009(3) 0.018(4) N1 0.036(4) 0.023(3) 0.037(3) -0.009(3) 0.002(3) -0.001(3) C1 0.060(6) 0.051(6) 0.037(5) 0.003(4) 0.012(4) -0.002(5) C2 0.066(7) 0.054(6) 0.050(6) -0.010(5) -0.010(5) 0.010(5) C3 0.072(7) 0.037(5) 0.048(5) 0.001(4) -0.004(5) -0.013(5) C4 0.056(6) 0.029(4) 0.043(5) -0.006(4) -0.008(4) 0.009(4) C5 0.031(4) 0.037(5) 0.037(4) -0.007(4) -0.004(3) -0.003(4) C6 0.040(5) 0.032(5) 0.058(5) -0.024(4) -0.006(4) 0.006(4) C7 0.054(5) 0.026(4) 0.043(5) -0.014(4) -0.014(4) -0.001(4) C8 0.033(5) 0.064(6) 0.048(5) -0.032(5) -0.011(4) -0.004(4) C9 0.037(5) 0.053(6) 0.035(5) -0.015(4) 0.001(3) -0.001(4) C10 0.047(5) 0.040(5) 0.046(5) -0.017(4) -0.018(4) 0.003(4) C11 0.041(5) 0.042(5) 0.027(4) -0.005(3) -0.004(3) -0.003(4) C12 0.040(5) 0.036(5) 0.046(5) -0.005(4) -0.003(4) -0.006(4) C13 0.044(5) 0.037(5) 0.042(5) -0.012(4) 0.003(4) 0.005(4) C14 0.030(4) 0.028(4) 0.036(4) -0.013(3) -0.008(3) -0.003(3) C15 0.043(5) 0.031(4) 0.043(4) -0.012(4) -0.003(4) 0.014(4) C16 0.059(6) 0.036(5) 0.053(5) -0.019(4) -0.014(4) 0.017(4) C17 0.073(7) 0.021(4) 0.053(5) -0.009(4) -0.017(5) 0.014(4) C18 0.055(5) 0.027(4) 0.040(4) -0.008(3) -0.005(4) 0.000(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 Os1 C1 1.985(10) . ? Os1 C2 1.922(10) . ? Os1 C3 1.903(10) . ? Os1 C4 1.960(10) . ? Os1 Os3 2.8600(5) . ? Os1 Os2 2.8613(5) . ? Os2 C8 1.890(9) . ? Os2 C10 1.894(9) . ? Os2 C9 1.911(8) . ? Os2 S1 2.4001(19) . ? Os2 Os3 2.7874(4) . ? Os2 Mn1 2.8147(11) . ? Os3 C5 1.902(8) . ? Os3 C7 1.914(8) . ? Os3 C6 1.918(9) . ? Os3 S1 2.4051(18) . ? Os3 Mn1 2.8632(11) . ? Mn1 C12 1.787(9) . ? Mn1 C13 1.797(9) . ? Mn1 C11 1.799(9) . ? Mn1 N1 2.104(6) . ? S1 C14 1.769(8) . ? O1 C1 1.108(11) . ? O2 C2 1.121(12) . ? O3 C3 1.120(11) . ? O4 C4 1.125(11) . ? O5 C5 1.148(10) . ? O6 C6 1.129(10) . ? O7 C7 1.152(10) . ? O8 C8 1.141(10) . ? O9 C9 1.139(10) . ? O10 C10 1.153(10) . ? O11 C11 1.139(10) . ? O12 C12 1.163(10) . ? O13 C13 1.146(10) . ? N1 C14 1.348(10) . ? N1 C18 1.349(10) . ? C14 C15 1.384(11) . ? C15 C16 1.386(12) . ? C15 H15 0.9300 . ? C16 C17 1.400(13) . ? C16 H16 0.9300 . ? C17 C18 1.364(12) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3 Os1 C2 97.3(4) . . ? C3 Os1 C4 91.2(4) . . ? C2 Os1 C4 91.7(4) . . ? C3 Os1 C1 92.1(5) . . ? C2 Os1 C1 92.7(4) . . ? C4 Os1 C1 174.1(4) . . ? C3 Os1 Os3 100.5(3) . . ? C2 Os1 Os3 162.0(3) . . ? C4 Os1 Os3 85.3(2) . . ? C1 Os1 Os3 89.3(3) . . ? C3 Os1 Os2 158.8(3) . . ? C2 Os1 Os2 103.8(3) . . ? C4 Os1 Os2 86.4(3) . . ? C1 Os1 Os2 88.8(3) . . ? Os3 Os1 Os2 58.313(11) . . ? C8 Os2 C10 92.3(4) . . ? C8 Os2 C9 92.2(4) . . ? C10 Os2 C9 92.9(4) . . ? C8 Os2 S1 167.2(2) . . ? C10 Os2 S1 94.8(3) . . ? C9 Os2 S1 98.1(3) . . ? C8 Os2 Os3 112.6(2) . . ? C10 Os2 Os3 123.6(2) . . ? C9 Os2 Os3 132.9(3) . . ? S1 Os2 Os3 54.63(4) . . ? C8 Os2 Mn1 92.4(3) . . ? C10 Os2 Mn1 68.0(2) . . ? C9 Os2 Mn1 160.6(3) . . ? S1 Os2 Mn1 80.42(5) . . ? Os3 Os2 Mn1 61.47(2) . . ? C8 Os2 Os1 91.1(3) . . ? C10 Os2 Os1 172.5(3) . . ? C9 Os2 Os1 80.3(3) . . ? S1 Os2 Os1 83.22(5) . . ? Os3 Os2 Os1 60.820(12) . . ? Mn1 Os2 Os1 118.52(3) . . ? C5 Os3 C7 93.2(3) . . ? C5 Os3 C6 90.3(3) . . ? C7 Os3 C6 92.5(4) . . ? C5 Os3 S1 169.0(2) . . ? C7 Os3 S1 93.5(2) . . ? C6 Os3 S1 98.1(2) . . ? C5 Os3 Os2 114.5(2) . . ? C7 Os3 Os2 122.0(2) . . ? C6 Os3 Os2 134.0(3) . . ? S1 Os3 Os2 54.46(5) . . ? C5 Os3 Os1 91.1(2) . . ? C7 Os3 Os1 172.9(3) . . ? C6 Os3 Os1 81.8(3) . . ? S1 Os3 Os1 83.16(5) . . ? Os2 Os3 Os1 60.866(12) . . ? C5 Os3 Mn1 95.0(2) . . ? C7 Os3 Mn1 68.3(3) . . ? C6 Os3 Mn1 160.3(3) . . ? S1 Os3 Mn1 79.34(5) . . ? Os2 Os3 Mn1 59.73(2) . . ? Os1 Os3 Mn1 116.96(3) . . ? C12 Mn1 C13 85.1(4) . . ? C12 Mn1 C11 88.1(4) . . ? C13 Mn1 C11 89.8(4) . . ? C12 Mn1 N1 97.0(3) . . ? C13 Mn1 N1 93.3(3) . . ? C11 Mn1 N1 174.2(3) . . ? C12 Mn1 Os2 108.9(3) . . ? C13 Mn1 Os2 165.7(3) . . ? C11 Mn1 Os2 87.8(2) . . ? N1 Mn1 Os2 88.02(17) . . ? C12 Mn1 Os3 166.6(3) . . ? C13 Mn1 Os3 107.0(3) . . ? C11 Mn1 Os3 86.1(3) . . ? N1 Mn1 Os3 88.30(17) . . ? Os2 Mn1 Os3 58.80(2) . . ? C14 S1 Os2 107.3(3) . . ? C14 S1 Os3 105.6(2) . . ? Os2 S1 Os3 70.91(5) . . ? C14 N1 C18 116.7(7) . . ? C14 N1 Mn1 123.1(5) . . ? C18 N1 Mn1 120.0(5) . . ? O1 C1 Os1 176.3(9) . . ? O2 C2 Os1 177.2(11) . . ? O3 C3 Os1 179.7(11) . . ? O4 C4 Os1 176.7(8) . . ? O5 C5 Os3 178.2(7) . . ? O6 C6 Os3 176.0(8) . . ? O7 C7 Os3 169.3(8) . . ? O8 C8 Os2 177.0(9) . . ? O9 C9 Os2 176.6(8) . . ? O10 C10 Os2 169.1(8) . . ? O11 C11 Mn1 176.7(8) . . ? O12 C12 Mn1 176.9(9) . . ? O13 C13 Mn1 179.5(9) . . ? N1 C14 C15 123.2(7) . . ? N1 C14 S1 119.5(6) . . ? C15 C14 S1 117.3(6) . . ? C14 C15 C16 119.1(8) . . ? C14 C15 H15 120.5 . . ? C16 C15 H15 120.5 . . ? C15 C16 C17 118.1(8) . . ? C15 C16 H16 120.9 . . ? C17 C16 H16 120.9 . . ? C18 C17 C16 118.9(8) . . ? C18 C17 H17 120.6 . . ? C16 C17 H17 120.6 . . ? N1 C18 C17 123.9(8) . . ? N1 C18 H18 118.0 . . ? C17 C18 H18 118.0 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.29 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.087 _refine_diff_density_min -1.417 _refine_diff_density_rms 0.188 # Attachment '- Compound 6.CIF' data_comp6 _database_code_depnum_ccdc_archive 'CCDC 748073' #TrackingRef '- Compound 6.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H4 Mn N O13 Ru3 S' _chemical_formula_sum 'C18 H4 Mn N O13 Ru3 S' _chemical_formula_weight 832.43 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' N N 0.0061 0.0033 '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' S S 0.1246 0.1234 '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' Ru Ru -1.2594 0.8363 '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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.5181(3) _cell_length_b 10.1387(4) _cell_length_c 15.1751(6) _cell_angle_alpha 70.434(2) _cell_angle_beta 83.813(3) _cell_angle_gamma 88.009(5) _cell_volume 1227.69(8) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 4386 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description Block _exptl_crystal_colour 'Deep Red' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.252 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 792 _exptl_absorpt_coefficient_mu 2.464 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.6386 _exptl_absorpt_correction_T_max 0.6654 _exptl_absorpt_process_details ; [North et al. (1968) Acta. Cryst. A24, 351] ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf-Nonius CAD4' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 4708 _diffrn_reflns_av_R_equivalents 0.0688 _diffrn_reflns_av_sigmaI/netI 0.0279 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 25.16 _reflns_number_total 4386 _reflns_number_gt 3893 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 Express (Enraf Nonius, 1994)' _computing_cell_refinement 'CAD4 Express (Enraf Nonius, 1994)' _computing_data_reduction 'CAD4 Express (Enraf Nonius, 1994)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0490P)^2^+0.1282P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4386 _refine_ls_number_parameters 334 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0335 _refine_ls_R_factor_gt 0.0270 _refine_ls_wR_factor_ref 0.0744 _refine_ls_wR_factor_gt 0.0716 _refine_ls_goodness_of_fit_ref 1.125 _refine_ls_restrained_S_all 1.125 _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 Ru1 Ru 0.28103(3) 0.77084(3) 0.121577(18) 0.03874(9) Uani 1 1 d . . . Ru2 Ru 0.17864(3) 0.48933(3) 0.174927(16) 0.03168(9) Uani 1 1 d . . . Ru3 Ru 0.35665(3) 0.56904(2) 0.292956(16) 0.02960(9) Uani 1 1 d . . . Mn1 Mn 0.15868(6) 0.32464(5) 0.36562(3) 0.03423(12) Uani 1 1 d . . . S1 S 0.45104(9) 0.44208(8) 0.19163(5) 0.03353(17) Uani 1 1 d . . . O1 O 0.5881(5) 0.7045(4) 0.0164(3) 0.0958(13) Uani 1 1 d . . . O2 O 0.1414(6) 0.9178(5) -0.0627(3) 0.1086(15) Uani 1 1 d . . . O3 O 0.4287(6) 1.0290(4) 0.1375(3) 0.0994(14) Uani 1 1 d . . . O4 O -0.0201(4) 0.8209(4) 0.2366(2) 0.0692(8) Uani 1 1 d . . . O5 O 0.1793(4) 0.7313(3) 0.4088(2) 0.0611(7) Uani 1 1 d . . . O6 O 0.6393(3) 0.7604(3) 0.2645(3) 0.0679(8) Uani 1 1 d . . . O7 O 0.4993(4) 0.3699(3) 0.4631(2) 0.0660(8) Uani 1 1 d . . . O8 O -0.1670(3) 0.5710(5) 0.1877(3) 0.0887(12) Uani 1 1 d . . . O9 O 0.1874(4) 0.5675(4) -0.03813(19) 0.0698(9) Uani 1 1 d . . . O10 O 0.0837(5) 0.1962(3) 0.1909(2) 0.0802(10) Uani 1 1 d . . . O11 O -0.0955(3) 0.5106(3) 0.4006(2) 0.0613(7) Uani 1 1 d . . . O12 O -0.0866(4) 0.1103(4) 0.4091(3) 0.0818(10) Uani 1 1 d . . . O13 O 0.1848(4) 0.2091(3) 0.56861(19) 0.0610(7) Uani 1 1 d . . . N1 N 0.3502(3) 0.2084(3) 0.33338(18) 0.0352(6) Uani 1 1 d . . . C1 C 0.4764(5) 0.7218(4) 0.0576(3) 0.0578(10) Uani 1 1 d . . . C2 C 0.1920(6) 0.8622(5) 0.0053(3) 0.0633(11) Uani 1 1 d . . . C3 C 0.3737(6) 0.9326(4) 0.1317(3) 0.0593(11) Uani 1 1 d . . . C4 C 0.0900(5) 0.7935(4) 0.1971(3) 0.0479(8) Uani 1 1 d . . . C5 C 0.2404(4) 0.6694(4) 0.3643(2) 0.0397(7) Uani 1 1 d . . . C6 C 0.5351(4) 0.6903(4) 0.2719(3) 0.0417(8) Uani 1 1 d . . . C7 C 0.4332(5) 0.4354(4) 0.4018(2) 0.0435(8) Uani 1 1 d . . . C8 C -0.0364(5) 0.5444(5) 0.1848(3) 0.0508(9) Uani 1 1 d . . . C9 C 0.1891(4) 0.5428(4) 0.0408(3) 0.0465(8) Uani 1 1 d . . . C10 C 0.1205(5) 0.3005(4) 0.1946(3) 0.0479(8) Uani 1 1 d . . . C11 C 0.0060(4) 0.4425(4) 0.3852(2) 0.0435(8) Uani 1 1 d . . . C12 C 0.0119(5) 0.1920(4) 0.3904(3) 0.0487(9) Uani 1 1 d . . . C13 C 0.1758(4) 0.2559(4) 0.4899(3) 0.0418(8) Uani 1 1 d . . . C14 C 0.4674(4) 0.2658(3) 0.2655(2) 0.0339(7) Uani 1 1 d . . . C15 C 0.6030(4) 0.1936(4) 0.2507(3) 0.0437(8) Uani 1 1 d . . . H15 H 0.6823 0.2373 0.2038 0.052 Uiso 1 1 calc R . . C16 C 0.6189(5) 0.0564(4) 0.3064(3) 0.0486(9) Uani 1 1 d . . . H16 H 0.7100 0.0066 0.2988 0.058 Uiso 1 1 calc R . . C17 C 0.4977(5) -0.0058(4) 0.3735(3) 0.0502(9) Uani 1 1 d . . . H17 H 0.5039 -0.0995 0.4103 0.060 Uiso 1 1 calc R . . C18 C 0.3679(5) 0.0723(4) 0.3854(2) 0.0447(8) Uani 1 1 d . . . H18 H 0.2874 0.0294 0.4317 0.054 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 Ru1 0.04336(17) 0.03429(15) 0.03250(15) -0.00372(11) -0.00274(12) 0.00249(12) Ru2 0.03179(15) 0.03691(15) 0.02833(14) -0.01301(11) -0.00553(10) 0.00262(11) Ru3 0.03107(15) 0.02863(14) 0.02955(14) -0.00969(10) -0.00530(10) 0.00059(10) Mn1 0.0348(3) 0.0315(2) 0.0332(2) -0.0084(2) 0.0026(2) -0.0005(2) S1 0.0320(4) 0.0338(4) 0.0328(4) -0.0098(3) 0.0000(3) 0.0035(3) O1 0.089(3) 0.080(2) 0.078(2) 0.0104(19) 0.038(2) 0.025(2) O2 0.153(4) 0.108(3) 0.062(2) -0.015(2) -0.051(3) 0.038(3) O3 0.145(4) 0.054(2) 0.096(3) -0.0081(19) -0.040(3) -0.028(2) O4 0.0525(18) 0.087(2) 0.0658(19) -0.0267(17) 0.0010(15) 0.0165(16) O5 0.0623(18) 0.0718(19) 0.0588(17) -0.0379(16) 0.0019(14) 0.0080(15) O6 0.0425(16) 0.0596(17) 0.112(3) -0.0443(18) -0.0005(16) -0.0099(14) O7 0.081(2) 0.0496(16) 0.0644(18) -0.0053(14) -0.0419(17) 0.0002(15) O8 0.0389(17) 0.145(3) 0.122(3) -0.094(3) -0.0224(18) 0.0255(19) O9 0.083(2) 0.095(2) 0.0337(15) -0.0250(15) -0.0068(14) 0.0014(18) O10 0.116(3) 0.0565(19) 0.079(2) -0.0316(17) -0.021(2) -0.0202(19) O11 0.0556(17) 0.0595(17) 0.0628(17) -0.0183(14) 0.0093(14) 0.0137(14) O12 0.075(2) 0.077(2) 0.088(2) -0.0178(19) -0.0084(18) -0.0372(19) O13 0.073(2) 0.0666(18) 0.0392(15) -0.0134(13) -0.0072(13) 0.0184(15) N1 0.0371(14) 0.0314(13) 0.0376(14) -0.0125(11) -0.0024(11) 0.0013(11) C1 0.058(2) 0.049(2) 0.046(2) 0.0066(17) 0.0066(19) 0.0038(18) C2 0.077(3) 0.061(3) 0.047(2) -0.010(2) -0.014(2) 0.012(2) C3 0.075(3) 0.042(2) 0.053(2) -0.0028(18) -0.011(2) -0.009(2) C4 0.050(2) 0.049(2) 0.0406(19) -0.0082(16) -0.0093(17) 0.0052(17) C5 0.0394(18) 0.0419(18) 0.0372(17) -0.0116(15) -0.0054(14) -0.0030(15) C6 0.0355(18) 0.0383(17) 0.055(2) -0.0204(16) -0.0029(15) 0.0035(15) C7 0.057(2) 0.0345(17) 0.0422(19) -0.0135(15) -0.0182(17) 0.0006(15) C8 0.047(2) 0.068(3) 0.050(2) -0.035(2) -0.0118(17) 0.0045(18) C9 0.0443(19) 0.056(2) 0.042(2) -0.0198(17) -0.0063(15) 0.0041(16) C10 0.051(2) 0.050(2) 0.047(2) -0.0193(17) -0.0115(17) -0.0038(17) C11 0.046(2) 0.0408(18) 0.0382(18) -0.0080(15) 0.0021(15) -0.0001(16) C12 0.049(2) 0.047(2) 0.048(2) -0.0127(17) -0.0031(17) -0.0052(18) C13 0.0412(19) 0.0394(18) 0.045(2) -0.0158(15) 0.0009(15) 0.0046(15) C14 0.0365(17) 0.0323(16) 0.0359(16) -0.0146(13) -0.0084(13) 0.0052(13) C15 0.0398(19) 0.047(2) 0.0473(19) -0.0201(16) -0.0031(15) 0.0055(15) C16 0.049(2) 0.0417(19) 0.060(2) -0.0224(18) -0.0130(18) 0.0165(16) C17 0.063(2) 0.0339(17) 0.054(2) -0.0140(16) -0.0135(19) 0.0114(16) C18 0.057(2) 0.0327(17) 0.0420(19) -0.0094(14) -0.0041(16) 0.0013(15) _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 Ru1 C1 1.969(4) . ? Ru1 C2 1.921(4) . ? Ru1 C3 1.903(4) . ? Ru1 C4 1.939(4) . ? Ru1 Ru2 2.8347(4) . ? Ru1 Ru3 2.8408(4) . ? Ru2 C8 1.901(4) . ? Ru2 C10 1.910(4) . ? Ru2 C9 1.916(4) . ? Ru2 S1 2.3761(8) . ? Ru2 Ru3 2.7929(3) . ? Ru2 Mn1 2.8050(5) . ? Ru3 C5 1.904(4) . ? Ru3 C7 1.913(3) . ? Ru3 C6 1.919(3) . ? Ru3 S1 2.3780(8) . ? Ru3 Mn1 2.8739(6) . ? Mn1 C12 1.786(4) . ? Mn1 C13 1.798(4) . ? Mn1 C11 1.804(4) . ? Mn1 N1 2.090(3) . ? S1 C14 1.773(3) . ? O1 C1 1.122(5) . ? O2 C2 1.122(5) . ? O3 C3 1.132(5) . ? O4 C4 1.135(5) . ? O5 C5 1.143(4) . ? O6 C6 1.130(4) . ? O7 C7 1.139(4) . ? O8 C8 1.135(5) . ? O9 C9 1.140(4) . ? O10 C10 1.134(5) . ? O11 C11 1.141(5) . ? O12 C12 1.144(5) . ? O13 C13 1.139(4) . ? N1 C14 1.347(4) . ? N1 C18 1.354(4) . ? C14 C15 1.384(5) . ? C15 C16 1.375(5) . ? C15 H15 0.9300 . ? C16 C17 1.374(5) . ? C16 H16 0.9300 . ? C17 C18 1.369(5) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3 Ru1 C2 97.12(19) . . ? C3 Ru1 C4 91.67(19) . . ? C2 Ru1 C4 93.05(19) . . ? C3 Ru1 C1 92.8(2) . . ? C2 Ru1 C1 92.82(19) . . ? C4 Ru1 C1 172.11(15) . . ? C3 Ru1 Ru2 158.55(12) . . ? C2 Ru1 Ru2 104.09(15) . . ? C4 Ru1 Ru2 84.11(12) . . ? C1 Ru1 Ru2 89.36(12) . . ? C3 Ru1 Ru3 99.70(12) . . ? C2 Ru1 Ru3 162.91(15) . . ? C4 Ru1 Ru3 83.53(11) . . ? C1 Ru1 Ru3 89.33(11) . . ? Ru2 Ru1 Ru3 58.957(9) . . ? C8 Ru2 C10 91.78(18) . . ? C8 Ru2 C9 92.35(16) . . ? C10 Ru2 C9 93.67(16) . . ? C8 Ru2 S1 166.52(11) . . ? C10 Ru2 S1 95.70(12) . . ? C9 Ru2 S1 98.34(11) . . ? C8 Ru2 Ru3 112.51(11) . . ? C10 Ru2 Ru3 124.10(11) . . ? C9 Ru2 Ru3 132.03(11) . . ? S1 Ru2 Ru3 54.05(2) . . ? C8 Ru2 Mn1 92.16(12) . . ? C10 Ru2 Mn1 68.05(11) . . ? C9 Ru2 Mn1 161.30(12) . . ? S1 Ru2 Mn1 80.32(2) . . ? Ru3 Ru2 Mn1 61.778(13) . . ? C8 Ru2 Ru1 91.32(13) . . ? C10 Ru2 Ru1 172.45(12) . . ? C9 Ru2 Ru1 79.32(12) . . ? S1 Ru2 Ru1 82.66(2) . . ? Ru3 Ru2 Ru1 60.630(9) . . ? Mn1 Ru2 Ru1 118.702(14) . . ? C5 Ru3 C7 93.11(15) . . ? C5 Ru3 C6 90.64(14) . . ? C7 Ru3 C6 92.71(15) . . ? C5 Ru3 S1 168.13(10) . . ? C7 Ru3 S1 93.97(11) . . ? C6 Ru3 S1 98.51(10) . . ? C5 Ru3 Ru2 114.15(10) . . ? C7 Ru3 Ru2 121.95(10) . . ? C6 Ru3 Ru2 133.99(11) . . ? S1 Ru3 Ru2 53.99(2) . . ? C5 Ru3 Ru1 91.38(10) . . ? C7 Ru3 Ru1 173.13(12) . . ? C6 Ru3 Ru1 82.04(11) . . ? S1 Ru3 Ru1 82.50(2) . . ? Ru2 Ru3 Ru1 60.413(9) . . ? C5 Ru3 Mn1 94.93(10) . . ? C7 Ru3 Mn1 68.57(11) . . ? C6 Ru3 Mn1 160.69(11) . . ? S1 Ru3 Mn1 78.86(2) . . ? Ru2 Ru3 Mn1 59.318(12) . . ? Ru1 Ru3 Mn1 116.211(14) . . ? C12 Mn1 C13 84.62(17) . . ? C12 Mn1 C11 88.87(17) . . ? C13 Mn1 C11 89.99(16) . . ? C12 Mn1 N1 97.08(15) . . ? C13 Mn1 N1 93.27(13) . . ? C11 Mn1 N1 173.46(13) . . ? C12 Mn1 Ru2 110.02(13) . . ? C13 Mn1 Ru2 164.96(12) . . ? C11 Mn1 Ru2 87.00(11) . . ? N1 Mn1 Ru2 88.40(7) . . ? C12 Mn1 Ru3 167.75(13) . . ? C13 Mn1 Ru3 106.18(11) . . ? C11 Mn1 Ru3 85.44(11) . . ? N1 Mn1 Ru3 88.20(7) . . ? Ru2 Mn1 Ru3 58.904(12) . . ? C14 S1 Ru2 107.53(11) . . ? C14 S1 Ru3 105.76(11) . . ? Ru2 S1 Ru3 71.96(2) . . ? C14 N1 C18 116.5(3) . . ? C14 N1 Mn1 122.6(2) . . ? C18 N1 Mn1 120.8(2) . . ? O1 C1 Ru1 174.5(4) . . ? O2 C2 Ru1 178.7(5) . . ? O3 C3 Ru1 179.8(5) . . ? O4 C4 Ru1 173.0(4) . . ? O5 C5 Ru3 175.7(3) . . ? O6 C6 Ru3 176.3(4) . . ? O7 C7 Ru3 168.9(3) . . ? O8 C8 Ru2 175.3(3) . . ? O9 C9 Ru2 175.1(4) . . ? O10 C10 Ru2 168.7(3) . . ? O11 C11 Mn1 176.2(3) . . ? O12 C12 Mn1 176.5(4) . . ? O13 C13 Mn1 178.1(3) . . ? N1 C14 C15 122.9(3) . . ? N1 C14 S1 119.4(2) . . ? C15 C14 S1 117.6(3) . . ? C16 C15 C14 119.1(4) . . ? C16 C15 H15 120.5 . . ? C14 C15 H15 120.5 . . ? C17 C16 C15 118.9(3) . . ? C17 C16 H16 120.6 . . ? C15 C16 H16 120.6 . . ? C18 C17 C16 119.0(3) . . ? C18 C17 H17 120.5 . . ? C16 C17 H17 120.5 . . ? N1 C18 C17 123.6(4) . . ? N1 C18 H18 118.2 . . ? C17 C18 H18 118.2 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.16 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.549 _refine_diff_density_min -1.170 _refine_diff_density_rms 0.190 # Attachment '- Compound 7.CIF' data_comp7 _database_code_depnum_ccdc_archive 'CCDC 748074' #TrackingRef '- Compound 7.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H8 N2 O12 Ru4 S' _chemical_formula_sum 'C22 H8 N2 O12 Ru4 S' _chemical_formula_weight 928.64 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' N N 0.0061 0.0033 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' 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 9.40890(10) _cell_length_b 19.4738(2) _cell_length_c 15.7618(10) _cell_angle_alpha 90.00 _cell_angle_beta 92.6190(10) _cell_angle_gamma 90.00 _cell_volume 2884.97(19) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7743 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.138 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1768 _exptl_absorpt_coefficient_mu 2.188 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8109 _exptl_absorpt_correction_T_max 0.8109 _exptl_absorpt_process_details ; [Blessing, Acta Cryst. (1995)] ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 94388 _diffrn_reflns_av_R_equivalents 0.0615 _diffrn_reflns_av_sigmaI/netI 0.0301 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 29.11 _reflns_number_total 7743 _reflns_number_gt 5736 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'DENZO (Otwinowski & Minor, 1997) and COLLECT (Hooft, 1998)' _computing_cell_refinement 'DENZO and COLLECT' _computing_data_reduction 'DENZO and COLLECT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 for windows (Farrugia, 1997)' _computing_publication_material 'WinGX (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0312P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7743 _refine_ls_number_parameters 360 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0506 _refine_ls_R_factor_gt 0.0285 _refine_ls_wR_factor_ref 0.0621 _refine_ls_wR_factor_gt 0.0567 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _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 Ru1 Ru 0.45067(2) 0.229329(11) 0.598203(13) 0.04389(6) Uani 1 1 d . . . Ru2 Ru 0.22007(2) 0.245444(10) 0.694255(12) 0.04126(6) Uani 1 1 d . . . Ru3 Ru 0.42192(2) 0.441939(11) 0.658940(13) 0.04733(7) Uani 1 1 d . . . Ru4 Ru 0.55623(2) 0.381655(11) 0.796123(13) 0.04362(6) Uani 1 1 d . . . S1 S 0.41376(6) 0.32321(3) 0.69059(4) 0.03937(14) Uani 1 1 d . . . O1 O 0.7615(3) 0.22719(16) 0.5501(2) 0.1123(10) Uani 1 1 d . . . O2 O 0.3519(3) 0.10146(11) 0.50367(15) 0.0827(7) Uani 1 1 d . . . O3 O 0.3462(3) 0.31917(12) 0.44927(14) 0.0827(7) Uani 1 1 d . . . O4 O 0.0662(3) 0.11823(13) 0.62747(17) 0.0999(9) Uani 1 1 d . . . O5 O 0.0403(2) 0.33851(11) 0.57700(13) 0.0713(6) Uani 1 1 d . . . O6 O 0.0571(3) 0.28090(15) 0.85236(15) 0.0976(8) Uani 1 1 d . . . O7 O 0.6502(3) 0.40807(14) 0.53443(18) 0.1034(9) Uani 1 1 d . . . O8 O 0.1852(3) 0.47118(12) 0.52370(16) 0.0973(9) Uani 1 1 d . . . O9 O 0.5194(3) 0.58935(12) 0.68772(16) 0.0922(8) Uani 1 1 d . . . O10 O 0.8243(3) 0.33341(19) 0.7139(2) 0.1312(12) Uani 1 1 d . . . O11 O 0.6989(3) 0.50861(12) 0.87194(16) 0.0870(7) Uani 1 1 d . . . O12 O 0.5773(3) 0.28295(13) 0.94727(14) 0.0891(8) Uani 1 1 d . . . N1A N 0.3712(3) 0.18352(11) 0.76101(14) 0.0476(4) Uani 0.616(15) 1 d P . . C13A C 0.3712(3) 0.18352(11) 0.76101(14) 0.0476(4) Uani 0.384(15) 1 d P . . N1B N 0.4843(3) 0.17528(11) 0.71309(15) 0.0476(4) Uani 0.384(15) 1 d P . . C13B C 0.4843(3) 0.17528(11) 0.71309(15) 0.0476(4) Uani 0.616(15) 1 d P . . N2A N 0.3603(2) 0.42036(11) 0.83142(15) 0.0459(4) Uani 0.519(15) 1 d P . . C18A C 0.3603(2) 0.42036(11) 0.83142(15) 0.0459(4) Uani 0.481(15) 1 d P . . N2B N 0.2916(3) 0.44846(11) 0.76339(15) 0.0459(4) Uani 0.481(15) 1 d P . . C18B C 0.2916(3) 0.44846(11) 0.76339(15) 0.0459(4) Uani 0.519(15) 1 d P . . C1 C 0.6482(4) 0.22911(17) 0.5698(2) 0.0667(8) Uani 1 1 d . . . C2 C 0.3910(3) 0.14841(15) 0.54089(17) 0.0556(7) Uani 1 1 d . . . C3 C 0.3856(3) 0.28525(15) 0.50314(17) 0.0547(7) Uani 1 1 d . . . C4 C 0.1215(3) 0.16579(16) 0.65416(19) 0.0614(8) Uani 1 1 d . . . C5 C 0.1060(3) 0.30361(14) 0.61991(16) 0.0488(6) Uani 1 1 d . . . C6 C 0.1172(3) 0.26793(15) 0.79375(19) 0.0575(7) Uani 1 1 d . . . C7 C 0.5661(4) 0.42303(17) 0.5802(2) 0.0698(9) Uani 1 1 d . . . C8 C 0.2711(4) 0.45935(14) 0.57399(19) 0.0645(8) Uani 1 1 d . . . C9 C 0.4832(3) 0.53426(16) 0.67748(18) 0.0620(8) Uani 1 1 d . . . C10 C 0.7267(3) 0.35135(19) 0.7444(2) 0.0744(9) Uani 1 1 d . . . C11 C 0.6462(3) 0.46095(16) 0.84465(19) 0.0588(7) Uani 1 1 d . . . C12 C 0.5716(3) 0.31855(15) 0.89132(18) 0.0558(7) Uani 1 1 d . . . C14 C 0.5982(3) 0.13784(15) 0.7440(2) 0.0640(8) Uani 1 1 d . . . H14 H 0.6790 0.1323 0.7106 0.077 Uiso 1 1 calc R . . C15 C 0.5965(4) 0.10791(15) 0.8238(2) 0.0723(10) Uani 1 1 d . . . H15 H 0.6754 0.0817 0.8451 0.087 Uiso 1 1 calc R . . C16 C 0.4808(4) 0.11646(14) 0.8715(2) 0.0688(9) Uani 1 1 d . . . H16 H 0.4784 0.0965 0.9264 0.083 Uiso 1 1 calc R . . C17 C 0.3676(3) 0.15426(14) 0.83945(17) 0.0584(7) Uani 1 1 d . . . H17 H 0.2861 0.1601 0.8721 0.070 Uiso 1 1 calc R . . C19 C 0.1579(3) 0.47516(15) 0.7711(2) 0.0637(8) Uani 1 1 d . . . H19 H 0.1080 0.4938 0.7227 0.076 Uiso 1 1 calc R . . C20 C 0.0954(3) 0.47533(18) 0.8479(2) 0.0753(9) Uani 1 1 d . . . H20 H 0.0031 0.4943 0.8528 0.090 Uiso 1 1 calc R . . C21 C 0.1664(4) 0.44806(17) 0.9174(2) 0.0709(9) Uani 1 1 d . . . H21 H 0.1243 0.4479 0.9710 0.085 Uiso 1 1 calc R . . C22 C 0.3000(3) 0.42084(14) 0.90860(18) 0.0583(7) Uani 1 1 d . . . H22 H 0.3507 0.4022 0.9567 0.070 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 Ru1 0.04316(12) 0.04966(13) 0.03904(11) -0.00239(9) 0.00405(9) 0.00135(9) Ru2 0.03875(12) 0.04821(12) 0.03687(11) 0.00516(8) 0.00219(9) -0.00333(9) Ru3 0.05367(14) 0.04509(13) 0.04291(12) 0.00904(9) -0.00128(10) -0.00734(9) Ru4 0.03696(12) 0.05168(13) 0.04186(12) 0.00113(9) -0.00219(9) -0.00023(9) S1 0.0391(3) 0.0424(3) 0.0366(3) 0.0025(2) 0.0020(3) -0.0016(3) O1 0.0575(17) 0.147(3) 0.135(2) -0.037(2) 0.0313(17) -0.0009(16) O2 0.0992(19) 0.0634(14) 0.0841(16) -0.0187(12) -0.0119(14) -0.0040(12) O3 0.0935(18) 0.0981(17) 0.0560(13) 0.0226(13) -0.0010(12) 0.0062(14) O4 0.115(2) 0.0865(18) 0.0976(19) -0.0060(14) -0.0065(16) -0.0492(16) O5 0.0633(14) 0.0827(15) 0.0672(13) 0.0190(12) -0.0054(11) 0.0101(11) O6 0.096(2) 0.136(2) 0.0629(15) -0.0019(15) 0.0370(14) -0.0067(17) O7 0.119(2) 0.105(2) 0.0902(19) 0.0102(15) 0.0522(18) -0.0226(17) O8 0.113(2) 0.0828(16) 0.0910(17) 0.0242(14) -0.0511(16) -0.0194(14) O9 0.125(2) 0.0581(14) 0.0943(18) -0.0027(12) 0.0195(16) -0.0336(14) O10 0.0562(17) 0.221(4) 0.118(2) -0.025(2) 0.0200(16) 0.038(2) O11 0.0831(17) 0.0679(14) 0.1072(19) -0.0045(13) -0.0251(15) -0.0202(13) O12 0.110(2) 0.0862(16) 0.0690(15) 0.0282(13) -0.0226(14) -0.0013(14) N1A 0.0528(10) 0.0435(9) 0.0455(10) 0.0015(7) -0.0074(7) 0.0005(8) C13A 0.0528(10) 0.0435(9) 0.0455(10) 0.0015(7) -0.0074(7) 0.0005(8) N1B 0.0528(10) 0.0435(9) 0.0455(10) 0.0015(7) -0.0074(7) 0.0005(8) C13B 0.0528(10) 0.0435(9) 0.0455(10) 0.0015(7) -0.0074(7) 0.0005(8) N2A 0.0445(10) 0.0450(9) 0.0482(10) -0.0006(7) 0.0007(8) 0.0003(7) C18A 0.0445(10) 0.0450(9) 0.0482(10) -0.0006(7) 0.0007(8) 0.0003(7) N2B 0.0445(10) 0.0450(9) 0.0482(10) -0.0006(7) 0.0007(8) 0.0003(7) C18B 0.0445(10) 0.0450(9) 0.0482(10) -0.0006(7) 0.0007(8) 0.0003(7) C1 0.0513(19) 0.084(2) 0.066(2) -0.0167(16) 0.0100(16) 0.0003(16) C2 0.0613(18) 0.0546(17) 0.0507(16) -0.0009(13) 0.0000(14) 0.0081(14) C3 0.0569(18) 0.0636(18) 0.0443(15) -0.0030(13) 0.0103(13) -0.0047(14) C4 0.0590(19) 0.0667(19) 0.0585(17) 0.0093(15) 0.0015(15) -0.0148(15) C5 0.0421(15) 0.0610(17) 0.0438(14) -0.0003(13) 0.0066(12) -0.0037(13) C6 0.0538(18) 0.0727(19) 0.0463(16) 0.0095(14) 0.0059(14) -0.0040(14) C7 0.085(2) 0.067(2) 0.0581(19) 0.0118(16) 0.0149(18) -0.0232(18) C8 0.084(2) 0.0500(17) 0.0580(18) 0.0129(14) -0.0101(17) -0.0129(15) C9 0.074(2) 0.0586(19) 0.0541(17) 0.0092(14) 0.0065(15) -0.0107(16) C10 0.0462(18) 0.107(3) 0.069(2) -0.0028(19) -0.0017(16) 0.0090(18) C11 0.0470(17) 0.0628(19) 0.0655(19) 0.0054(15) -0.0083(14) -0.0036(14) C12 0.0553(18) 0.0598(17) 0.0512(17) -0.0003(14) -0.0108(14) 0.0030(13) C14 0.0588(19) 0.0588(17) 0.073(2) -0.0039(15) -0.0148(16) 0.0081(15) C15 0.077(2) 0.0557(18) 0.081(2) 0.0027(16) -0.033(2) 0.0071(16) C16 0.097(3) 0.0513(18) 0.0557(18) 0.0078(14) -0.0283(19) -0.0068(17) C17 0.078(2) 0.0527(16) 0.0436(15) 0.0056(13) -0.0072(14) -0.0090(15) C19 0.0527(18) 0.0592(18) 0.079(2) 0.0046(16) -0.0019(16) 0.0112(14) C20 0.0477(19) 0.078(2) 0.101(3) -0.012(2) 0.0149(19) 0.0141(16) C21 0.061(2) 0.079(2) 0.074(2) -0.0067(17) 0.0249(18) 0.0036(17) C22 0.0625(19) 0.0598(17) 0.0535(17) 0.0012(13) 0.0125(15) -0.0002(15) _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 Ru1 C1 1.931(3) . ? Ru1 C2 1.889(3) . ? Ru1 C3 1.929(3) . ? Ru1 N1B 2.106(2) . ? Ru1 S1 2.3727(6) . ? Ru1 Ru2 2.7200(3) . ? Ru2 C4 1.900(3) . ? Ru2 C5 1.922(3) . ? Ru2 C6 1.931(3) . ? Ru2 N1A 2.109(2) . ? Ru2 S1 2.3722(6) . ? Ru3 C7 1.916(4) . ? Ru3 C8 1.936(3) . ? Ru3 C9 1.907(3) . ? Ru3 N2B 2.101(2) . ? Ru3 S1 2.3673(6) . ? Ru3 Ru4 2.7204(3) . ? Ru4 C10 1.925(3) . ? Ru4 C11 1.904(3) . ? Ru4 C12 1.940(3) . ? Ru4 N2A 2.090(2) . ? Ru4 S1 2.3781(6) . ? O1 C1 1.125(4) . ? O2 C2 1.138(3) . ? O3 C3 1.125(3) . ? O4 C4 1.134(3) . ? O5 C5 1.124(3) . ? O6 C6 1.133(3) . ? O7 C7 1.133(4) . ? O8 C8 1.130(3) . ? O9 C9 1.135(3) . ? O10 C10 1.112(4) . ? O11 C11 1.128(3) . ? O12 C12 1.121(3) . ? N1A N1B 1.342(3) . ? N1B C14 1.368(4) . ? N2A N2B 1.343(3) . ? N2A C22 1.366(4) . ? C14 C15 1.388(4) . ? C14 H14 0.9500 . ? C15 C16 1.361(5) . ? C15 H15 0.9500 . ? C16 C17 1.372(4) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C19 C20 1.369(4) . ? C19 H19 0.9500 . ? C20 C21 1.364(5) . ? C20 H20 0.9500 . ? C21 C22 1.377(4) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? 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 Ru1 C2 98.94(13) . . ? C1 Ru1 C3 95.49(13) . . ? C2 Ru1 C3 91.30(11) . . ? C2 Ru1 N1B 91.37(10) . . ? C3 Ru1 N1B 168.48(11) . . ? C1 Ru1 N1B 95.16(12) . . ? C1 Ru1 S1 108.26(9) . . ? C2 Ru1 S1 152.58(9) . . ? C3 Ru1 S1 89.52(8) . . ? N1B Ru1 S1 82.98(7) . . ? C1 Ru1 Ru2 158.39(9) . . ? C2 Ru1 Ru2 97.77(9) . . ? C3 Ru1 Ru2 97.73(8) . . ? N1B Ru1 Ru2 70.81(7) . . ? S1 Ru1 Ru2 55.015(16) . . ? C4 Ru2 C5 91.60(12) . . ? C4 Ru2 C6 101.55(13) . . ? C5 Ru2 C6 94.29(11) . . ? C4 Ru2 N1A 90.39(11) . . ? C5 Ru2 N1A 170.54(10) . . ? C6 Ru2 N1A 94.37(11) . . ? C4 Ru2 S1 151.23(10) . . ? C5 Ru2 S1 90.98(8) . . ? C6 Ru2 S1 106.82(9) . . ? N1A Ru2 S1 82.87(6) . . ? C4 Ru2 Ru1 96.32(9) . . ? C5 Ru2 Ru1 99.56(8) . . ? C6 Ru2 Ru1 157.03(9) . . ? N1A Ru2 Ru1 71.02(7) . . ? S1 Ru2 Ru1 55.031(16) . . ? C7 Ru3 C8 95.95(14) . . ? C7 Ru3 C9 93.59(13) . . ? C8 Ru3 C9 98.50(12) . . ? C9 Ru3 N2B 90.35(11) . . ? C7 Ru3 N2B 167.21(12) . . ? C8 Ru3 N2B 95.50(12) . . ? C9 Ru3 S1 154.32(9) . . ? C7 Ru3 S1 88.83(9) . . ? C8 Ru3 S1 106.68(8) . . ? N2B Ru3 S1 82.42(6) . . ? C9 Ru3 Ru4 99.14(9) . . ? C7 Ru3 Ru4 96.62(10) . . ? C8 Ru3 Ru4 157.59(9) . . ? N2B Ru3 Ru4 70.72(6) . . ? S1 Ru3 Ru4 55.208(15) . . ? C11 Ru4 C10 93.16(14) . . ? C11 Ru4 C12 100.77(12) . . ? C10 Ru4 C12 95.69(13) . . ? C11 Ru4 N2A 88.96(11) . . ? C10 Ru4 N2A 170.17(12) . . ? C12 Ru4 N2A 93.33(11) . . ? C10 Ru4 S1 90.62(10) . . ? C11 Ru4 S1 153.50(9) . . ? C12 Ru4 S1 104.93(8) . . ? N2A Ru4 S1 83.28(6) . . ? C11 Ru4 Ru3 98.69(8) . . ? C10 Ru4 Ru3 99.29(10) . . ? C12 Ru4 Ru3 154.66(8) . . ? N2A Ru4 Ru3 70.89(6) . . ? S1 Ru4 Ru3 54.835(15) . . ? Ru3 S1 Ru2 131.37(3) . . ? Ru3 S1 Ru1 128.04(3) . . ? Ru2 S1 Ru1 69.954(18) . . ? Ru3 S1 Ru4 69.958(17) . . ? Ru2 S1 Ru4 134.23(3) . . ? Ru1 S1 Ru4 134.78(3) . . ? N1B N1A Ru2 108.74(16) . . ? N1A N1B C14 119.5(2) . . ? N1A N1B Ru1 109.42(16) . . ? C14 N1B Ru1 131.1(2) . . ? N2B N2A C22 120.2(2) . . ? N2B N2A Ru4 109.44(17) . . ? C22 N2A Ru4 130.3(2) . . ? N2A N2B Ru3 108.89(17) . . ? O1 C1 Ru1 176.8(3) . . ? O2 C2 Ru1 176.9(3) . . ? O3 C3 Ru1 178.0(3) . . ? O4 C4 Ru2 177.2(3) . . ? O5 C5 Ru2 178.9(3) . . ? O6 C6 Ru2 179.7(3) . . ? O7 C7 Ru3 176.2(3) . . ? O8 C8 Ru3 178.0(3) . . ? O9 C9 Ru3 179.4(3) . . ? O10 C10 Ru4 179.2(4) . . ? O11 C11 Ru4 178.6(3) . . ? O12 C12 Ru4 178.0(3) . . ? N1B C14 C15 120.4(3) . . ? N1B C14 H14 119.8 . . ? C15 C14 H14 119.8 . . ? C16 C15 C14 119.5(3) . . ? C16 C15 H15 120.3 . . ? C14 C15 H15 120.3 . . ? C15 C16 C17 119.3(3) . . ? C15 C16 H16 120.4 . . ? C17 C16 H16 120.4 . . ? C16 C17 H17 119.7 . . ? C20 C19 H19 119.6 . . ? C21 C20 C19 119.6(3) . . ? C21 C20 H20 120.2 . . ? C19 C20 H20 120.2 . . ? C20 C21 C22 119.0(3) . . ? C20 C21 H21 120.5 . . ? C22 C21 H21 120.5 . . ? N2A C22 C21 120.7(3) . . ? N2A C22 H22 119.6 . . ? C21 C22 H22 119.6 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 29.11 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.385 _refine_diff_density_min -0.641 _refine_diff_density_rms 0.108 # Attachment '- Compound 8.cif' data_dth1ra _database_code_depnum_ccdc_archive 'CCDC 748075' #TrackingRef '- Compound 8.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H8 Fe2 N2 O13 Re2 S2' _chemical_formula_weight 1068.53 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -5.2083 5.8923 '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 10.44650(10) _cell_length_b 15.4234(2) _cell_length_c 18.4256(2) _cell_angle_alpha 86.7550(10) _cell_angle_beta 84.1080(10) _cell_angle_gamma 88.2370(10) _cell_volume 2947.39(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9967 _cell_measurement_theta_min 3 _cell_measurement_theta_max 67 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.408 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1992 _exptl_absorpt_coefficient_mu 25.339 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.0729 _exptl_absorpt_correction_T_max 0.0878 _exptl_absorpt_process_details ; Numerical (based on real shape of the crystal) absorption correction followed by: SADABS. Program for empirical absorption correction of area-detector data. University of Goetingen. Germany. Sheldrick, G. M. 1996 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX2 CCD detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 24513 _diffrn_reflns_av_R_equivalents 0.0283 _diffrn_reflns_av_sigmaI/netI 0.0290 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.87 _diffrn_reflns_theta_max 67.95 _reflns_number_total 10065 _reflns_number_gt 9567 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2-2008.5-0 (Bruker, 2008)' _computing_cell_refinement 'SAINT v7.56A (Bruker, 2008)' _computing_data_reduction 'SADABS-2008/1 (Bruker, 2008)' _computing_structure_solution 'XS/SHELXTL-2008/1 (Bruker, 2008)' _computing_structure_refinement 'SHELXL-2008/4(Bruker, 2008)' _computing_molecular_graphics 'XP v5.1 (Bruker, 1998)' _computing_publication_material 'XCIF-2008/2 (Bruker, 2008)' _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^)+(0.0384P)^2^+6.8087P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.000041(9) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 10065 _refine_ls_number_parameters 794 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0295 _refine_ls_R_factor_gt 0.0275 _refine_ls_wR_factor_ref 0.0715 _refine_ls_wR_factor_gt 0.0705 _refine_ls_goodness_of_fit_ref 1.095 _refine_ls_restrained_S_all 1.095 _refine_ls_shift/su_max 0.004 _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 Re1 Re 0.60301(2) 0.879615(13) 0.655988(12) 0.01951(7) Uani 1 1 d . . . Re2 Re 0.480734(19) 0.752959(13) 0.506409(11) 0.01769(7) Uani 1 1 d . . . Fe1 Fe 0.76532(7) 0.62688(5) 0.63063(4) 0.01894(16) Uani 1 1 d . . . Fe2 Fe 0.88213(7) 0.72766(5) 0.53080(4) 0.02041(16) Uani 1 1 d . . . S1 S 0.39267(11) 0.83911(7) 0.61519(7) 0.0206(2) Uani 1 1 d . . . S2 S 0.67575(11) 0.75049(7) 0.57985(6) 0.0176(2) Uani 1 1 d . . . O1 O 0.8436(4) 0.9617(3) 0.7034(3) 0.0399(10) Uani 1 1 d . . . O2 O 0.4562(4) 1.0169(3) 0.7486(2) 0.0335(9) Uani 1 1 d . . . O3 O 0.5741(4) 0.7457(2) 0.7906(2) 0.0280(8) Uani 1 1 d . . . O4 O 0.6481(4) 1.0059(3) 0.5173(2) 0.0372(9) Uani 1 1 d . . . O5 O 0.5369(4) 0.6080(2) 0.3998(2) 0.0298(8) Uani 1 1 d . . . O6 O 0.2339(4) 0.7926(3) 0.4327(2) 0.0379(10) Uani 1 1 d . . . O7 O 0.6186(4) 0.8801(3) 0.3918(2) 0.0371(9) Uani 1 1 d . . . O8 O 0.5961(4) 0.5579(3) 0.7575(2) 0.0352(9) Uani 1 1 d . . . O9 O 0.9733(4) 0.4943(3) 0.6325(3) 0.0412(10) Uani 1 1 d . . . O10 O 0.6472(4) 0.5212(2) 0.5307(2) 0.0322(9) Uani 1 1 d . . . O11 O 0.9541(5) 0.9015(3) 0.4688(3) 0.0432(10) Uani 1 1 d . . . O12 O 1.1242(4) 0.6272(3) 0.5131(2) 0.0357(9) Uani 1 1 d . . . O13 O 0.8104(4) 0.6601(3) 0.3938(2) 0.0328(9) Uani 1 1 d . . . N1 N 0.3889(4) 0.6755(3) 0.5978(2) 0.0182(8) Uani 1 1 d . . . N2 N 0.8676(4) 0.7063(3) 0.6804(2) 0.0250(9) Uani 1 1 d . . . C1 C 0.7603(5) 0.9257(3) 0.6850(3) 0.0253(11) Uani 1 1 d . . . C2 C 0.5111(5) 0.9680(4) 0.7123(3) 0.0275(12) Uani 1 1 d . . . C3 C 0.5842(5) 0.7942(3) 0.7428(3) 0.0209(10) Uani 1 1 d . . . C4 C 0.6294(5) 0.9598(3) 0.5661(3) 0.0247(11) Uani 1 1 d . . . C5 C 0.5207(5) 0.6630(3) 0.4402(3) 0.0220(10) Uani 1 1 d . . . C6 C 0.3246(5) 0.7755(4) 0.4603(3) 0.0238(11) Uani 1 1 d . . . C7 C 0.5666(5) 0.8330(3) 0.4350(3) 0.0236(11) Uani 1 1 d . . . C8 C 0.6594(5) 0.5872(3) 0.7101(3) 0.0242(11) Uani 1 1 d . . . C9 C 0.8936(5) 0.5464(4) 0.6327(3) 0.0272(11) Uani 1 1 d . . . C10 C 0.6927(5) 0.5639(3) 0.5688(3) 0.0231(11) Uani 1 1 d . . . C11 C 0.9257(5) 0.8345(4) 0.4919(3) 0.0281(11) Uani 1 1 d . . . C12 C 1.0317(5) 0.6670(3) 0.5194(3) 0.0262(11) Uani 1 1 d . . . C13 C 0.8332(5) 0.6859(3) 0.4475(3) 0.0253(11) Uani 1 1 d . . . C14 C 0.3582(4) 0.7314(3) 0.6516(3) 0.0206(10) Uani 1 1 d . . . C15 C 0.3034(5) 0.7065(3) 0.7200(3) 0.0232(10) Uani 1 1 d . . . H15A H 0.2887 0.7467 0.7574 0.028 Uiso 1 1 calc R . . C16 C 0.2699(5) 0.6197(3) 0.7326(3) 0.0232(10) Uani 1 1 d . . . H16A H 0.2294 0.5999 0.7789 0.028 Uiso 1 1 calc R . . C17 C 0.2959(5) 0.5627(3) 0.6776(3) 0.0235(10) Uani 1 1 d . . . H17A H 0.2715 0.5038 0.6852 0.028 Uiso 1 1 calc R . . C18 C 0.3578(5) 0.5923(3) 0.6112(3) 0.0209(10) Uani 1 1 d . . . H18A H 0.3789 0.5523 0.5741 0.025 Uiso 1 1 calc R . . C19 C 0.9342(4) 0.7553(3) 0.6277(3) 0.0217(10) Uani 1 1 d . . . C20 C 1.0244(5) 0.8124(4) 0.6464(3) 0.0292(12) Uani 1 1 d . . . H20A H 1.0742 0.8457 0.6094 0.035 Uiso 1 1 calc R . . C21 C 1.0410(5) 0.8203(4) 0.7189(4) 0.0362(14) Uani 1 1 d . . . H21A H 1.1014 0.8600 0.7319 0.043 Uiso 1 1 calc R . . C22 C 0.9702(6) 0.7708(4) 0.7729(3) 0.0365(14) Uani 1 1 d . . . H22A H 0.9800 0.7767 0.8230 0.044 Uiso 1 1 calc R . . C23 C 0.8851(5) 0.7127(4) 0.7520(3) 0.0290(12) Uani 1 1 d . . . H23A H 0.8380 0.6767 0.7881 0.035 Uiso 1 1 calc R . . Re1A Re -0.27547(2) 1.085950(13) 0.889853(11) 0.01982(7) Uani 1 1 d . . . Re2A Re -0.43396(2) 1.271271(14) 0.997555(12) 0.02105(7) Uani 1 1 d . . . Fe1A Fe -0.13777(8) 1.34271(5) 0.83467(4) 0.02282(17) Uani 1 1 d . . . Fe2A Fe -0.02621(8) 1.27630(5) 0.94432(4) 0.02278(17) Uani 1 1 d . . . S1A S -0.49780(11) 1.14374(7) 0.93002(6) 0.0215(2) Uani 1 1 d . . . S2A S -0.22541(11) 1.24059(7) 0.91854(6) 0.0189(2) Uani 1 1 d . . . O1A O -0.0197(4) 0.9904(3) 0.8438(2) 0.0348(9) Uani 1 1 d . . . O2A O -0.3918(5) 0.9094(2) 0.8705(2) 0.0388(10) Uani 1 1 d . . . O3A O -0.2978(4) 1.1457(3) 0.7261(2) 0.0310(8) Uani 1 1 d . . . O4A O -0.2355(4) 1.0266(3) 1.0520(2) 0.0383(10) Uani 1 1 d . . . O5A O -0.3926(4) 1.4484(3) 1.0581(3) 0.0479(12) Uani 1 1 d . . . O6A O -0.7064(4) 1.2849(3) 1.0762(2) 0.0358(9) Uani 1 1 d . . . O7A O -0.3215(4) 1.1861(3) 1.1325(2) 0.0405(10) Uani 1 1 d . . . O8A O -0.2823(4) 1.3623(3) 0.7041(2) 0.0383(10) Uani 1 1 d . . . O9A O 0.0730(5) 1.4597(3) 0.7860(3) 0.0489(12) Uani 1 1 d . . . O10A O -0.2663(5) 1.4909(3) 0.9077(3) 0.0465(11) Uani 1 1 d . . . O11A O 0.0715(6) 1.1294(3) 1.0323(3) 0.0571(14) Uani 1 1 d . . . O12A O 0.2066(4) 1.3794(3) 0.9260(3) 0.0422(10) Uani 1 1 d . . . O13A O -0.1197(5) 1.3796(4) 1.0703(3) 0.0520(12) Uani 1 1 d . . . N1A N -0.5042(4) 1.3073(3) 0.8929(2) 0.0223(9) Uani 1 1 d . . . N2A N -0.0258(4) 1.2467(3) 0.7987(2) 0.0270(9) Uani 1 1 d . . . C1A C -0.1081(5) 1.0304(3) 0.8610(3) 0.0264(11) Uani 1 1 d . . . C2A C -0.3479(6) 0.9746(3) 0.8775(3) 0.0289(12) Uani 1 1 d . . . C3A C -0.2909(5) 1.1245(3) 0.7850(3) 0.0228(10) Uani 1 1 d . . . C4A C -0.2517(5) 1.0493(3) 0.9946(3) 0.0251(11) Uani 1 1 d . . . C5A C -0.4032(5) 1.3817(4) 1.0332(3) 0.0338(13) Uani 1 1 d . . . C6A C -0.6056(5) 1.2791(4) 1.0482(3) 0.0264(11) Uani 1 1 d . . . C7A C -0.3651(5) 1.2178(4) 1.0823(3) 0.0286(12) Uani 1 1 d . . . C8A C -0.2304(5) 1.3524(4) 0.7562(3) 0.0296(12) Uani 1 1 d . . . C9A C -0.0085(6) 1.4149(4) 0.8046(3) 0.0340(13) Uani 1 1 d . . . C10A C -0.2200(5) 1.4307(4) 0.8813(3) 0.0318(13) Uani 1 1 d . . . C11A C 0.0299(6) 1.1872(4) 1.0003(3) 0.0364(13) Uani 1 1 d . . . C12A C 0.1158(6) 1.3396(4) 0.9322(3) 0.0316(12) Uani 1 1 d . . . C13A C -0.0885(5) 1.3403(4) 1.0202(3) 0.0329(13) Uani 1 1 d . . . C14A C -0.5276(5) 1.2303(3) 0.8653(3) 0.0215(10) Uani 1 1 d . . . C15A C -0.5729(5) 1.2250(4) 0.7983(3) 0.0269(11) Uani 1 1 d . . . H15B H -0.5877 1.1702 0.7799 0.032 Uiso 1 1 calc R . . C16A C -0.5962(5) 1.3014(4) 0.7582(3) 0.0305(12) Uani 1 1 d . . . H16B H -0.6291 1.2998 0.7122 0.037 Uiso 1 1 calc R . . C17A C -0.5717(5) 1.3793(4) 0.7854(3) 0.0316(12) Uani 1 1 d . . . H17B H -0.5866 1.4320 0.7580 0.038 Uiso 1 1 calc R . . C18A C -0.5250(5) 1.3813(3) 0.8533(3) 0.0266(11) Uani 1 1 d . . . H18B H -0.5075 1.4354 0.8718 0.032 Uiso 1 1 calc R . . C19A C 0.0389(5) 1.2165(3) 0.8550(3) 0.0239(10) Uani 1 1 d . . . C20A C 0.1369(5) 1.1542(4) 0.8422(3) 0.0295(12) Uani 1 1 d . . . H20B H 0.1867 1.1341 0.8804 0.035 Uiso 1 1 calc R . . C21A C 0.1616(6) 1.1213(4) 0.7727(4) 0.0374(14) Uani 1 1 d . . . H21B H 0.2274 1.0782 0.7642 0.045 Uiso 1 1 calc R . . C22A C 0.0918(6) 1.1508(4) 0.7167(3) 0.0371(14) Uani 1 1 d . . . H22B H 0.1066 1.1273 0.6699 0.045 Uiso 1 1 calc R . . C23A C -0.0015(6) 1.2163(4) 0.7304(3) 0.0339(13) Uani 1 1 d . . . H23B H -0.0483 1.2398 0.6919 0.041 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 Re1 0.01972(11) 0.01361(11) 0.02529(12) -0.00273(9) -0.00219(8) 0.00080(8) Re2 0.01882(11) 0.01549(11) 0.01832(11) 0.00288(8) -0.00195(8) -0.00013(8) Fe1 0.0218(4) 0.0158(4) 0.0193(4) 0.0000(3) -0.0037(3) 0.0026(3) Fe2 0.0190(4) 0.0184(4) 0.0232(4) 0.0000(3) 0.0000(3) 0.0008(3) S1 0.0202(5) 0.0150(5) 0.0261(6) 0.0009(5) -0.0015(4) 0.0012(4) S2 0.0183(5) 0.0139(5) 0.0204(5) -0.0004(4) -0.0015(4) 0.0011(4) O1 0.028(2) 0.036(2) 0.059(3) -0.015(2) -0.0091(19) -0.0021(18) O2 0.032(2) 0.0253(19) 0.044(2) -0.0156(19) -0.0039(18) 0.0081(17) O3 0.036(2) 0.0257(19) 0.0223(18) -0.0051(17) -0.0014(15) 0.0053(16) O4 0.043(2) 0.024(2) 0.043(2) 0.0075(19) -0.0038(19) 0.0003(18) O5 0.044(2) 0.0225(19) 0.0230(18) -0.0035(16) -0.0037(16) -0.0015(17) O6 0.028(2) 0.053(3) 0.033(2) 0.0138(19) -0.0086(17) -0.0014(19) O7 0.040(2) 0.033(2) 0.034(2) 0.0106(19) 0.0099(18) -0.0042(18) O8 0.043(2) 0.028(2) 0.032(2) 0.0042(18) 0.0068(18) -0.0060(18) O9 0.036(2) 0.033(2) 0.053(3) 0.005(2) -0.0054(19) 0.0163(19) O10 0.044(2) 0.0233(19) 0.031(2) -0.0071(17) -0.0096(18) -0.0010(17) O11 0.052(3) 0.029(2) 0.048(3) 0.008(2) -0.003(2) -0.009(2) O12 0.0238(19) 0.036(2) 0.046(2) -0.0016(19) -0.0012(17) 0.0067(17) O13 0.033(2) 0.040(2) 0.026(2) -0.0082(18) -0.0019(16) -0.0010(18) N1 0.0180(19) 0.019(2) 0.0172(19) 0.0035(16) -0.0005(15) -0.0005(16) N2 0.023(2) 0.026(2) 0.026(2) -0.0023(19) -0.0078(17) 0.0061(18) C1 0.025(3) 0.017(2) 0.035(3) -0.011(2) -0.006(2) 0.003(2) C2 0.025(3) 0.024(3) 0.034(3) -0.001(2) -0.009(2) -0.003(2) C3 0.022(2) 0.020(2) 0.021(2) -0.008(2) -0.0031(19) 0.001(2) C4 0.027(3) 0.013(2) 0.034(3) 0.002(2) -0.006(2) -0.001(2) C5 0.021(2) 0.021(2) 0.023(2) 0.008(2) -0.0041(19) -0.0028(19) C6 0.017(2) 0.032(3) 0.021(2) 0.005(2) 0.0001(19) -0.001(2) C7 0.027(2) 0.017(2) 0.026(3) 0.002(2) -0.001(2) 0.004(2) C8 0.028(3) 0.018(2) 0.027(3) -0.003(2) -0.006(2) 0.002(2) C9 0.031(3) 0.026(3) 0.025(3) 0.003(2) -0.005(2) 0.000(2) C10 0.026(2) 0.020(2) 0.022(2) 0.005(2) -0.001(2) 0.006(2) C11 0.026(3) 0.027(3) 0.032(3) 0.002(2) -0.003(2) -0.002(2) C12 0.026(3) 0.026(3) 0.027(3) -0.003(2) -0.001(2) -0.002(2) C13 0.022(2) 0.023(2) 0.029(3) 0.006(2) 0.002(2) 0.003(2) C14 0.017(2) 0.018(2) 0.027(2) -0.002(2) -0.0051(19) 0.0001(19) C15 0.022(2) 0.022(2) 0.026(3) -0.004(2) -0.003(2) 0.002(2) C16 0.022(2) 0.027(3) 0.019(2) 0.006(2) 0.0005(19) -0.003(2) C17 0.029(3) 0.016(2) 0.025(3) 0.002(2) -0.002(2) -0.002(2) C18 0.024(2) 0.016(2) 0.023(2) -0.001(2) -0.0057(19) -0.0014(19) C19 0.016(2) 0.020(2) 0.030(3) -0.007(2) -0.0037(19) 0.0071(19) C20 0.019(2) 0.024(3) 0.044(3) -0.001(2) -0.006(2) 0.001(2) C21 0.022(3) 0.037(3) 0.053(4) -0.015(3) -0.017(3) 0.004(2) C22 0.032(3) 0.046(3) 0.035(3) -0.016(3) -0.014(2) 0.010(3) C23 0.024(3) 0.035(3) 0.028(3) -0.007(2) -0.003(2) 0.005(2) Re1A 0.02676(12) 0.01291(11) 0.01945(11) 0.00097(8) -0.00174(8) -0.00058(8) Re2A 0.02191(12) 0.02131(12) 0.01950(11) -0.00348(9) 0.00116(8) -0.00045(9) Fe1A 0.0232(4) 0.0174(4) 0.0268(4) 0.0048(3) -0.0003(3) -0.0028(3) Fe2A 0.0223(4) 0.0220(4) 0.0239(4) 0.0000(3) -0.0018(3) -0.0021(3) S1A 0.0246(6) 0.0169(5) 0.0226(6) 0.0032(5) -0.0016(5) -0.0042(5) S2A 0.0207(5) 0.0150(5) 0.0205(5) -0.0001(4) 0.0006(4) -0.0016(4) O1A 0.037(2) 0.025(2) 0.040(2) 0.0014(18) 0.0049(18) 0.0027(18) O2A 0.061(3) 0.020(2) 0.035(2) 0.0005(17) -0.007(2) -0.0136(19) O3A 0.040(2) 0.033(2) 0.0193(19) 0.0022(16) -0.0028(16) 0.0024(17) O4A 0.059(3) 0.031(2) 0.024(2) 0.0028(17) -0.0098(19) 0.007(2) O5A 0.041(2) 0.039(3) 0.066(3) -0.030(2) -0.003(2) 0.003(2) O6A 0.024(2) 0.053(3) 0.028(2) 0.0015(19) 0.0021(16) 0.0036(18) O7A 0.048(2) 0.048(3) 0.027(2) -0.0112(19) -0.0092(18) 0.016(2) O8A 0.039(2) 0.040(2) 0.037(2) 0.0031(19) -0.0095(19) 0.0013(19) O9A 0.048(3) 0.049(3) 0.049(3) 0.017(2) -0.005(2) -0.029(2) O10A 0.051(3) 0.026(2) 0.062(3) -0.006(2) -0.003(2) 0.001(2) O11A 0.081(4) 0.045(3) 0.044(3) 0.013(2) -0.010(3) 0.017(3) O12A 0.031(2) 0.045(2) 0.052(3) -0.001(2) -0.0061(19) -0.014(2) O13A 0.046(3) 0.069(3) 0.043(3) -0.029(3) -0.003(2) -0.002(2) N1A 0.022(2) 0.020(2) 0.025(2) -0.0029(18) 0.0006(17) 0.0008(17) N2A 0.025(2) 0.029(2) 0.025(2) -0.0009(19) 0.0025(18) -0.0005(18) C1A 0.030(3) 0.018(2) 0.030(3) 0.004(2) 0.001(2) 0.003(2) C2A 0.043(3) 0.019(3) 0.024(3) 0.002(2) -0.002(2) -0.001(2) C3A 0.025(2) 0.015(2) 0.028(3) -0.003(2) 0.002(2) -0.0013(19) C4A 0.033(3) 0.016(2) 0.026(3) 0.000(2) -0.003(2) 0.000(2) C5A 0.026(3) 0.038(3) 0.037(3) -0.016(3) 0.002(2) 0.004(2) C6A 0.025(3) 0.033(3) 0.020(2) 0.000(2) 0.001(2) -0.002(2) C7A 0.030(3) 0.036(3) 0.020(3) -0.009(2) 0.001(2) 0.006(2) C8A 0.027(3) 0.025(3) 0.036(3) 0.000(2) 0.003(2) -0.003(2) C9A 0.040(3) 0.028(3) 0.033(3) 0.008(2) -0.008(3) -0.005(3) C10A 0.030(3) 0.023(3) 0.042(3) 0.005(3) -0.006(2) -0.008(2) C11A 0.042(3) 0.035(3) 0.032(3) -0.003(3) -0.003(3) -0.001(3) C12A 0.034(3) 0.031(3) 0.030(3) -0.003(2) -0.002(2) -0.003(3) C13A 0.025(3) 0.037(3) 0.039(3) -0.006(3) -0.009(2) -0.007(2) C14A 0.022(2) 0.017(2) 0.024(2) 0.002(2) 0.0041(19) -0.0039(19) C15A 0.027(3) 0.027(3) 0.026(3) 0.001(2) -0.003(2) -0.004(2) C16A 0.029(3) 0.035(3) 0.027(3) 0.007(2) -0.003(2) -0.004(2) C17A 0.028(3) 0.024(3) 0.041(3) 0.010(2) -0.004(2) -0.001(2) C18A 0.024(2) 0.018(2) 0.038(3) 0.002(2) -0.003(2) 0.004(2) C19A 0.023(2) 0.021(2) 0.027(3) 0.002(2) 0.002(2) -0.005(2) C20A 0.022(3) 0.027(3) 0.039(3) -0.001(2) -0.001(2) -0.003(2) C21A 0.027(3) 0.035(3) 0.050(4) -0.007(3) 0.006(3) -0.003(2) C22A 0.030(3) 0.047(4) 0.033(3) -0.008(3) 0.011(2) -0.007(3) C23A 0.030(3) 0.039(3) 0.030(3) 0.000(3) 0.009(2) -0.004(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 Re1 C2 1.932(6) . ? Re1 C1 1.946(5) . ? Re1 C4 2.010(5) . ? Re1 C3 2.011(5) . ? Re1 S1 2.5021(12) . ? Re1 S2 2.5527(11) . ? Re2 C5 1.907(5) . ? Re2 C7 1.924(5) . ? Re2 C6 1.929(5) . ? Re2 N1 2.167(4) . ? Re2 S1 2.5450(12) . ? Re2 S2 2.5569(11) . ? Fe1 C10 1.779(6) . ? Fe1 C9 1.800(5) . ? Fe1 C8 1.831(5) . ? Fe1 N2 1.974(4) . ? Fe1 S2 2.2921(13) . ? Fe1 Fe2 2.5731(11) . ? Fe2 C12 1.796(5) . ? Fe2 C11 1.811(6) . ? Fe2 C13 1.824(6) . ? Fe2 C19 1.991(5) . ? Fe2 S2 2.2756(13) . ? S1 C14 1.788(5) . ? O1 C1 1.136(7) . ? O2 C2 1.139(7) . ? O3 C3 1.121(6) . ? O4 C4 1.120(6) . ? O5 C5 1.158(6) . ? O6 C6 1.138(6) . ? O7 C7 1.151(6) . ? O8 C8 1.122(7) . ? O9 C9 1.138(7) . ? O10 C10 1.137(7) . ? O11 C11 1.132(7) . ? O12 C12 1.129(7) . ? O13 C13 1.137(7) . ? N1 C18 1.337(6) . ? N1 C14 1.358(7) . ? N2 C19 1.345(7) . ? N2 C23 1.359(7) . ? C14 C15 1.370(7) . ? C15 C16 1.396(7) . ? C15 H15A 0.9500 . ? C16 C17 1.380(8) . ? C16 H16A 0.9500 . ? C17 C18 1.385(7) . ? C17 H17A 0.9500 . ? C18 H18A 0.9500 . ? C19 C20 1.391(8) . ? C20 C21 1.377(9) . ? C20 H20A 0.9500 . ? C21 C22 1.385(9) . ? C21 H21A 0.9500 . ? C22 C23 1.378(9) . ? C22 H22A 0.9500 . ? C23 H23A 0.9500 . ? Re1A C2A 1.932(6) . ? Re1A C1A 1.960(5) . ? Re1A C3A 2.010(5) . ? Re1A C4A 2.017(5) . ? Re1A S1A 2.5162(12) . ? Re1A S2A 2.5530(11) . ? Re2A C5A 1.908(6) . ? Re2A C7A 1.919(5) . ? Re2A C6A 1.938(5) . ? Re2A N1A 2.171(4) . ? Re2A S1A 2.5279(12) . ? Re2A S2A 2.5404(12) . ? Fe1A C10A 1.796(6) . ? Fe1A C9A 1.800(6) . ? Fe1A C8A 1.817(6) . ? Fe1A N2A 1.961(5) . ? Fe1A S2A 2.2869(13) . ? Fe1A Fe2A 2.5817(11) . ? Fe2A C12A 1.789(6) . ? Fe2A C11A 1.792(6) . ? Fe2A C13A 1.812(6) . ? Fe2A C19A 1.981(5) . ? Fe2A S2A 2.2721(14) . ? S1A C14A 1.780(5) . ? O1A C1A 1.122(6) . ? O2A C2A 1.137(7) . ? O3A C3A 1.124(6) . ? O4A C4A 1.124(6) . ? O5A C5A 1.161(7) . ? O6A C6A 1.128(6) . ? O7A C7A 1.151(7) . ? O8A C8A 1.150(7) . ? O9A C9A 1.128(7) . ? O10A C10A 1.143(7) . ? O11A C11A 1.140(8) . ? O12A C12A 1.137(7) . ? O13A C13A 1.147(7) . ? N1A C18A 1.343(7) . ? N1A C14A 1.357(7) . ? N2A C19A 1.349(7) . ? N2A C23A 1.365(7) . ? C14A C15A 1.374(7) . ? C15A C16A 1.384(8) . ? C15A H15B 0.9500 . ? C16A C17A 1.369(8) . ? C16A H16B 0.9500 . ? C17A C18A 1.390(8) . ? C17A H17B 0.9500 . ? C18A H18B 0.9500 . ? C19A C20A 1.393(8) . ? C20A C21A 1.400(9) . ? C20A H20B 0.9500 . ? C21A C22A 1.373(9) . ? C21A H21B 0.9500 . ? C22A C23A 1.397(9) . ? C22A H22B 0.9500 . ? C23A H23B 0.9500 . ? 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 Re1 C1 86.9(2) . . ? C2 Re1 C4 92.7(2) . . ? C1 Re1 C4 86.8(2) . . ? C2 Re1 C3 90.7(2) . . ? C1 Re1 C3 92.8(2) . . ? C4 Re1 C3 176.5(2) . . ? C2 Re1 S1 88.24(16) . . ? C1 Re1 S1 173.05(15) . . ? C4 Re1 S1 88.46(15) . . ? C3 Re1 S1 92.29(14) . . ? C2 Re1 S2 167.58(16) . . ? C1 Re1 S2 105.32(15) . . ? C4 Re1 S2 89.98(15) . . ? C3 Re1 S2 86.78(14) . . ? S1 Re1 S2 79.71(4) . . ? C5 Re2 C7 88.5(2) . . ? C5 Re2 C6 87.6(2) . . ? C7 Re2 C6 88.6(2) . . ? C5 Re2 N1 98.74(18) . . ? C7 Re2 N1 172.15(19) . . ? C6 Re2 N1 94.67(18) . . ? C5 Re2 S1 163.90(15) . . ? C7 Re2 S1 107.51(16) . . ? C6 Re2 S1 91.14(16) . . ? N1 Re2 S1 65.36(11) . . ? C5 Re2 S2 103.44(15) . . ? C7 Re2 S2 89.75(16) . . ? C6 Re2 S2 168.84(17) . . ? N1 Re2 S2 85.66(11) . . ? S1 Re2 S2 78.83(4) . . ? C10 Fe1 C9 89.0(2) . . ? C10 Fe1 C8 93.7(2) . . ? C9 Fe1 C8 99.7(2) . . ? C10 Fe1 N2 167.9(2) . . ? C9 Fe1 N2 89.6(2) . . ? C8 Fe1 N2 98.4(2) . . ? C10 Fe1 S2 89.77(16) . . ? C9 Fe1 S2 150.87(18) . . ? C8 Fe1 S2 109.39(16) . . ? N2 Fe1 S2 85.59(13) . . ? C10 Fe1 Fe2 95.18(16) . . ? C9 Fe1 Fe2 95.74(17) . . ? C8 Fe1 Fe2 162.27(16) . . ? N2 Fe1 Fe2 73.01(13) . . ? S2 Fe1 Fe2 55.41(4) . . ? C12 Fe2 C11 102.8(2) . . ? C12 Fe2 C13 90.6(2) . . ? C11 Fe2 C13 96.6(2) . . ? C12 Fe2 C19 85.9(2) . . ? C11 Fe2 C19 91.6(2) . . ? C13 Fe2 C19 171.6(2) . . ? C12 Fe2 S2 153.89(18) . . ? C11 Fe2 S2 102.36(18) . . ? C13 Fe2 S2 93.42(16) . . ? C19 Fe2 S2 86.44(14) . . ? C12 Fe2 Fe1 97.92(17) . . ? C11 Fe2 Fe1 151.80(19) . . ? C13 Fe2 Fe1 102.14(16) . . ? C19 Fe2 Fe1 70.83(15) . . ? S2 Fe2 Fe1 56.02(4) . . ? C14 S1 Re1 107.79(16) . . ? C14 S1 Re2 80.19(17) . . ? Re1 S1 Re2 98.09(4) . . ? Fe2 S2 Fe1 68.57(4) . . ? Fe2 S2 Re1 123.62(5) . . ? Fe1 S2 Re1 121.73(5) . . ? Fe2 S2 Re2 123.88(5) . . ? Fe1 S2 Re2 124.29(5) . . ? Re1 S2 Re2 96.49(4) . . ? C18 N1 C14 118.2(4) . . ? C18 N1 Re2 136.2(3) . . ? C14 N1 Re2 105.6(3) . . ? C19 N2 C23 121.2(5) . . ? C19 N2 Fe1 106.6(3) . . ? C23 N2 Fe1 132.0(4) . . ? O1 C1 Re1 171.6(4) . . ? O2 C2 Re1 176.3(5) . . ? O3 C3 Re1 179.0(4) . . ? O4 C4 Re1 177.2(5) . . ? O5 C5 Re2 175.8(4) . . ? O6 C6 Re2 177.0(5) . . ? O7 C7 Re2 179.2(5) . . ? O8 C8 Fe1 175.8(5) . . ? O9 C9 Fe1 178.1(5) . . ? O10 C10 Fe1 177.8(4) . . ? O11 C11 Fe2 178.7(5) . . ? O12 C12 Fe2 178.3(5) . . ? O13 C13 Fe2 175.8(5) . . ? N1 C14 C15 123.6(5) . . ? N1 C14 S1 108.4(3) . . ? C15 C14 S1 127.9(4) . . ? C14 C15 C16 117.3(5) . . ? C14 C15 H15A 121.4 . . ? C16 C15 H15A 121.4 . . ? C17 C16 C15 119.7(5) . . ? C17 C16 H16A 120.2 . . ? C15 C16 H16A 120.2 . . ? C16 C17 C18 119.3(5) . . ? C16 C17 H17A 120.4 . . ? C18 C17 H17A 120.4 . . ? N1 C18 C17 121.8(5) . . ? N1 C18 H18A 119.1 . . ? C17 C18 H18A 119.1 . . ? N2 C19 C20 119.6(5) . . ? N2 C19 Fe2 109.4(3) . . ? C20 C19 Fe2 131.1(4) . . ? C21 C20 C19 119.5(5) . . ? C21 C20 H20A 120.2 . . ? C19 C20 H20A 120.2 . . ? C20 C21 C22 120.4(5) . . ? C20 C21 H21A 119.8 . . ? C22 C21 H21A 119.8 . . ? C23 C22 C21 118.3(5) . . ? C23 C22 H22A 120.9 . . ? C21 C22 H22A 120.9 . . ? N2 C23 C22 120.9(5) . . ? N2 C23 H23A 119.5 . . ? C22 C23 H23A 119.5 . . ? C2A Re1A C1A 86.0(2) . . ? C2A Re1A C3A 92.0(2) . . ? C1A Re1A C3A 89.9(2) . . ? C2A Re1A C4A 89.9(2) . . ? C1A Re1A C4A 88.3(2) . . ? C3A Re1A C4A 177.4(2) . . ? C2A Re1A S1A 89.13(18) . . ? C1A Re1A S1A 174.81(15) . . ? C3A Re1A S1A 92.22(15) . . ? C4A Re1A S1A 89.71(16) . . ? C2A Re1A S2A 168.32(17) . . ? C1A Re1A S2A 105.38(16) . . ? C3A Re1A S2A 90.49(14) . . ? C4A Re1A S2A 88.10(15) . . ? S1A Re1A S2A 79.36(4) . . ? C5A Re2A C7A 88.4(3) . . ? C5A Re2A C6A 87.6(2) . . ? C7A Re2A C6A 92.1(2) . . ? C5A Re2A N1A 102.1(2) . . ? C7A Re2A N1A 168.8(2) . . ? C6A Re2A N1A 92.04(19) . . ? C5A Re2A S1A 167.89(19) . . ? C7A Re2A S1A 103.60(17) . . ? C6A Re2A S1A 90.50(17) . . ? N1A Re2A S1A 66.00(12) . . ? C5A Re2A S2A 102.04(17) . . ? C7A Re2A S2A 91.33(16) . . ? C6A Re2A S2A 169.82(17) . . ? N1A Re2A S2A 82.94(11) . . ? S1A Re2A S2A 79.37(4) . . ? C10A Fe1A C9A 88.6(3) . . ? C10A Fe1A C8A 95.5(3) . . ? C9A Fe1A C8A 100.7(3) . . ? C10A Fe1A N2A 169.0(2) . . ? C9A Fe1A N2A 88.0(2) . . ? C8A Fe1A N2A 95.4(2) . . ? C10A Fe1A S2A 92.74(18) . . ? C9A Fe1A S2A 149.06(19) . . ? C8A Fe1A S2A 109.92(18) . . ? N2A Fe1A S2A 84.87(14) . . ? C10A Fe1A Fe2A 96.83(19) . . ? C9A Fe1A Fe2A 93.90(18) . . ? C8A Fe1A Fe2A 161.08(18) . . ? N2A Fe1A Fe2A 72.95(13) . . ? S2A Fe1A Fe2A 55.24(4) . . ? C12A Fe2A C11A 99.5(3) . . ? C12A Fe2A C13A 89.9(3) . . ? C11A Fe2A C13A 95.1(3) . . ? C12A Fe2A C19A 88.2(2) . . ? C11A Fe2A C19A 90.5(2) . . ? C13A Fe2A C19A 174.4(2) . . ? C12A Fe2A S2A 153.89(19) . . ? C11A Fe2A S2A 105.9(2) . . ? C13A Fe2A S2A 93.38(18) . . ? C19A Fe2A S2A 85.98(15) . . ? C12A Fe2A Fe1A 98.35(19) . . ? C11A Fe2A Fe1A 153.4(2) . . ? C13A Fe2A Fe1A 104.53(19) . . ? C19A Fe2A Fe1A 70.51(15) . . ? S2A Fe2A Fe1A 55.78(4) . . ? C14A S1A Re1A 105.31(16) . . ? C14A S1A Re2A 80.00(17) . . ? Re1A S1A Re2A 98.15(4) . . ? Fe2A S2A Fe1A 68.98(4) . . ? Fe2A S2A Re2A 125.18(5) . . ? Fe1A S2A Re2A 121.33(5) . . ? Fe2A S2A Re1A 121.53(5) . . ? Fe1A S2A Re1A 124.61(5) . . ? Re2A S2A Re1A 96.88(4) . . ? C18A N1A C14A 119.1(4) . . ? C18A N1A Re2A 136.7(4) . . ? C14A N1A Re2A 104.2(3) . . ? C19A N2A C23A 122.3(5) . . ? C19A N2A Fe1A 106.6(3) . . ? C23A N2A Fe1A 130.9(4) . . ? O1A C1A Re1A 172.3(5) . . ? O2A C2A Re1A 179.3(6) . . ? O3A C3A Re1A 179.0(5) . . ? O4A C4A Re1A 177.6(5) . . ? O5A C5A Re2A 175.1(5) . . ? O6A C6A Re2A 178.2(5) . . ? O7A C7A Re2A 178.7(5) . . ? O8A C8A Fe1A 175.1(5) . . ? O9A C9A Fe1A 179.5(6) . . ? O10A C10A Fe1A 174.8(5) . . ? O11A C11A Fe2A 175.6(6) . . ? O12A C12A Fe2A 178.5(5) . . ? O13A C13A Fe2A 175.1(5) . . ? N1A C14A C15A 122.4(5) . . ? N1A C14A S1A 109.7(4) . . ? C15A C14A S1A 127.9(4) . . ? C14A C15A C16A 118.3(5) . . ? C14A C15A H15B 120.8 . . ? C16A C15A H15B 120.8 . . ? C17A C16A C15A 119.6(5) . . ? C17A C16A H16B 120.2 . . ? C15A C16A H16B 120.2 . . ? C16A C17A C18A 119.9(5) . . ? C16A C17A H17B 120.0 . . ? C18A C17A H17B 120.0 . . ? N1A C18A C17A 120.6(5) . . ? N1A C18A H18B 119.7 . . ? C17A C18A H18B 119.7 . . ? N2A C19A C20A 118.7(5) . . ? N2A C19A Fe2A 109.7(4) . . ? C20A C19A Fe2A 131.7(4) . . ? C19A C20A C21A 119.7(5) . . ? C19A C20A H20B 120.2 . . ? C21A C20A H20B 120.2 . . ? C22A C21A C20A 120.8(6) . . ? C22A C21A H21B 119.6 . . ? C20A C21A H21B 119.6 . . ? C21A C22A C23A 118.1(6) . . ? C21A C22A H22B 120.9 . . ? C23A C22A H22B 120.9 . . ? N2A C23A C22A 120.3(6) . . ? N2A C23A H23B 119.8 . . ? C22A C23A H23B 119.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C10 Fe1 Fe2 C12 -92.1(2) . . . . ? C9 Fe1 Fe2 C12 -2.6(2) . . . . ? C8 Fe1 Fe2 C12 148.1(6) . . . . ? N2 Fe1 Fe2 C12 85.2(2) . . . . ? S2 Fe1 Fe2 C12 -178.27(18) . . . . ? C10 Fe1 Fe2 C11 130.8(4) . . . . ? C9 Fe1 Fe2 C11 -139.6(4) . . . . ? C8 Fe1 Fe2 C11 11.0(7) . . . . ? N2 Fe1 Fe2 C11 -51.8(4) . . . . ? S2 Fe1 Fe2 C11 44.7(4) . . . . ? C10 Fe1 Fe2 C13 0.2(2) . . . . ? C9 Fe1 Fe2 C13 89.8(2) . . . . ? C8 Fe1 Fe2 C13 -119.6(6) . . . . ? N2 Fe1 Fe2 C13 177.6(2) . . . . ? S2 Fe1 Fe2 C13 -85.91(17) . . . . ? C10 Fe1 Fe2 C19 -175.0(2) . . . . ? C9 Fe1 Fe2 C19 -85.4(2) . . . . ? C8 Fe1 Fe2 C19 65.3(6) . . . . ? N2 Fe1 Fe2 C19 2.43(19) . . . . ? S2 Fe1 Fe2 C19 98.92(14) . . . . ? C10 Fe1 Fe2 S2 86.13(16) . . . . ? C9 Fe1 Fe2 S2 175.68(18) . . . . ? C8 Fe1 Fe2 S2 -33.7(5) . . . . ? N2 Fe1 Fe2 S2 -96.49(13) . . . . ? C2 Re1 S1 C14 -114.7(2) . . . . ? C1 Re1 S1 C14 -160.9(14) . . . . ? C4 Re1 S1 C14 152.6(2) . . . . ? C3 Re1 S1 C14 -24.0(2) . . . . ? S2 Re1 S1 C14 62.30(18) . . . . ? C2 Re1 S1 Re2 163.10(16) . . . . ? C1 Re1 S1 Re2 116.9(14) . . . . ? C4 Re1 S1 Re2 70.32(15) . . . . ? C3 Re1 S1 Re2 -106.25(14) . . . . ? S2 Re1 S1 Re2 -19.94(4) . . . . ? C5 Re2 S1 C14 13.0(5) . . . . ? C7 Re2 S1 C14 -173.0(2) . . . . ? C6 Re2 S1 C14 98.1(2) . . . . ? N1 Re2 S1 C14 3.52(19) . . . . ? S2 Re2 S1 C14 -86.81(16) . . . . ? C5 Re2 S1 Re1 119.8(5) . . . . ? C7 Re2 S1 Re1 -66.19(16) . . . . ? C6 Re2 S1 Re1 -155.09(15) . . . . ? N1 Re2 S1 Re1 110.30(12) . . . . ? S2 Re2 S1 Re1 19.97(4) . . . . ? C12 Fe2 S2 Fe1 3.9(4) . . . . ? C11 Fe2 S2 Fe1 -160.11(19) . . . . ? C13 Fe2 S2 Fe1 102.34(16) . . . . ? C19 Fe2 S2 Fe1 -69.22(15) . . . . ? C12 Fe2 S2 Re1 118.6(4) . . . . ? C11 Fe2 S2 Re1 -45.43(19) . . . . ? C13 Fe2 S2 Re1 -142.98(17) . . . . ? C19 Fe2 S2 Re1 45.46(15) . . . . ? Fe1 Fe2 S2 Re1 114.68(6) . . . . ? C12 Fe2 S2 Re2 -113.8(4) . . . . ? C11 Fe2 S2 Re2 82.15(19) . . . . ? C13 Fe2 S2 Re2 -15.40(17) . . . . ? C19 Fe2 S2 Re2 173.03(15) . . . . ? Fe1 Fe2 S2 Re2 -117.74(6) . . . . ? C10 Fe1 S2 Fe2 -96.46(17) . . . . ? C9 Fe1 S2 Fe2 -8.9(4) . . . . ? C8 Fe1 S2 Fe2 169.69(17) . . . . ? N2 Fe1 S2 Fe2 72.37(13) . . . . ? C10 Fe1 S2 Re1 146.38(17) . . . . ? C9 Fe1 S2 Re1 -126.0(4) . . . . ? C8 Fe1 S2 Re1 52.53(18) . . . . ? N2 Fe1 S2 Re1 -44.79(14) . . . . ? Fe2 Fe1 S2 Re1 -117.16(6) . . . . ? C10 Fe1 S2 Re2 20.75(17) . . . . ? C9 Fe1 S2 Re2 108.3(4) . . . . ? C8 Fe1 S2 Re2 -73.10(18) . . . . ? N2 Fe1 S2 Re2 -170.42(14) . . . . ? Fe2 Fe1 S2 Re2 117.21(7) . . . . ? C2 Re1 S2 Fe2 172.6(7) . . . . ? C1 Re1 S2 Fe2 -16.78(18) . . . . ? C4 Re1 S2 Fe2 69.87(16) . . . . ? C3 Re1 S2 Fe2 -108.78(15) . . . . ? S1 Re1 S2 Fe2 158.30(6) . . . . ? C2 Re1 S2 Fe1 -103.5(8) . . . . ? C1 Re1 S2 Fe1 67.21(18) . . . . ? C4 Re1 S2 Fe1 153.85(16) . . . . ? C3 Re1 S2 Fe1 -24.80(15) . . . . ? S1 Re1 S2 Fe1 -117.71(6) . . . . ? C2 Re1 S2 Re2 34.0(8) . . . . ? C1 Re1 S2 Re2 -155.31(17) . . . . ? C4 Re1 S2 Re2 -68.67(15) . . . . ? C3 Re1 S2 Re2 112.69(14) . . . . ? S1 Re1 S2 Re2 19.77(4) . . . . ? C5 Re2 S2 Fe2 38.46(16) . . . . ? C7 Re2 S2 Fe2 -49.95(16) . . . . ? C6 Re2 S2 Fe2 -131.4(8) . . . . ? N1 Re2 S2 Fe2 136.43(12) . . . . ? S1 Re2 S2 Fe2 -157.86(6) . . . . ? C5 Re2 S2 Fe1 -47.25(16) . . . . ? C7 Re2 S2 Fe1 -135.66(16) . . . . ? C6 Re2 S2 Fe1 142.9(8) . . . . ? N1 Re2 S2 Fe1 50.71(12) . . . . ? S1 Re2 S2 Fe1 116.43(6) . . . . ? C5 Re2 S2 Re1 176.84(15) . . . . ? C7 Re2 S2 Re1 88.43(15) . . . . ? C6 Re2 S2 Re1 6.9(8) . . . . ? N1 Re2 S2 Re1 -85.20(11) . . . . ? S1 Re2 S2 Re1 -19.48(4) . . . . ? C5 Re2 N1 C18 -2.7(5) . . . . ? C7 Re2 N1 C18 -160.1(12) . . . . ? C6 Re2 N1 C18 85.5(5) . . . . ? S1 Re2 N1 C18 174.6(5) . . . . ? S2 Re2 N1 C18 -105.7(5) . . . . ? C5 Re2 N1 C14 177.9(3) . . . . ? C7 Re2 N1 C14 20.6(14) . . . . ? C6 Re2 N1 C14 -93.9(3) . . . . ? S1 Re2 N1 C14 -4.7(3) . . . . ? S2 Re2 N1 C14 74.9(3) . . . . ? C10 Fe1 N2 C19 9.0(11) . . . . ? C9 Fe1 N2 C19 92.6(3) . . . . ? C8 Fe1 N2 C19 -167.7(3) . . . . ? S2 Fe1 N2 C19 -58.7(3) . . . . ? Fe2 Fe1 N2 C19 -3.5(3) . . . . ? C10 Fe1 N2 C23 -165.7(8) . . . . ? C9 Fe1 N2 C23 -82.2(5) . . . . ? C8 Fe1 N2 C23 17.6(5) . . . . ? S2 Fe1 N2 C23 126.6(5) . . . . ? Fe2 Fe1 N2 C23 -178.3(5) . . . . ? C2 Re1 C1 O1 -22(4) . . . . ? C4 Re1 C1 O1 71(4) . . . . ? C3 Re1 C1 O1 -112(4) . . . . ? S1 Re1 C1 O1 24(5) . . . . ? S2 Re1 C1 O1 160(3) . . . . ? C1 Re1 C2 O2 -95(7) . . . . ? C4 Re1 C2 O2 179(100) . . . . ? C3 Re1 C2 O2 -2(7) . . . . ? S1 Re1 C2 O2 90(7) . . . . ? S2 Re1 C2 O2 76(7) . . . . ? C2 Re1 C3 O3 162(26) . . . . ? C1 Re1 C3 O3 -111(26) . . . . ? C4 Re1 C3 O3 -28(28) . . . . ? S1 Re1 C3 O3 74(26) . . . . ? S2 Re1 C3 O3 -5(26) . . . . ? C2 Re1 C4 O4 79(10) . . . . ? C1 Re1 C4 O4 -7(10) . . . . ? C3 Re1 C4 O4 -90(10) . . . . ? S1 Re1 C4 O4 168(10) . . . . ? S2 Re1 C4 O4 -113(10) . . . . ? C7 Re2 C5 O5 -115(6) . . . . ? C6 Re2 C5 O5 -26(6) . . . . ? N1 Re2 C5 O5 68(6) . . . . ? S1 Re2 C5 O5 60(6) . . . . ? S2 Re2 C5 O5 156(6) . . . . ? C5 Re2 C6 O6 -128(9) . . . . ? C7 Re2 C6 O6 -40(9) . . . . ? N1 Re2 C6 O6 133(9) . . . . ? S1 Re2 C6 O6 68(9) . . . . ? S2 Re2 C6 O6 42(9) . . . . ? C5 Re2 C7 O7 -17(40) . . . . ? C6 Re2 C7 O7 -104(40) . . . . ? N1 Re2 C7 O7 141(39) . . . . ? S1 Re2 C7 O7 165(40) . . . . ? S2 Re2 C7 O7 87(40) . . . . ? C10 Fe1 C8 O8 49(6) . . . . ? C9 Fe1 C8 O8 -40(7) . . . . ? N2 Fe1 C8 O8 -131(6) . . . . ? S2 Fe1 C8 O8 141(6) . . . . ? Fe2 Fe1 C8 O8 169(6) . . . . ? C10 Fe1 C9 O9 6(16) . . . . ? C8 Fe1 C9 O9 100(16) . . . . ? N2 Fe1 C9 O9 -162(16) . . . . ? S2 Fe1 C9 O9 -82(16) . . . . ? Fe2 Fe1 C9 O9 -89(16) . . . . ? C9 Fe1 C10 O10 43(12) . . . . ? C8 Fe1 C10 O10 -56(12) . . . . ? N2 Fe1 C10 O10 127(12) . . . . ? S2 Fe1 C10 O10 -166(12) . . . . ? Fe2 Fe1 C10 O10 139(12) . . . . ? C12 Fe2 C11 O11 -74(25) . . . . ? C13 Fe2 C11 O11 -166(25) . . . . ? C19 Fe2 C11 O11 12(25) . . . . ? S2 Fe2 C11 O11 99(25) . . . . ? Fe1 Fe2 C11 O11 62(25) . . . . ? C11 Fe2 C12 O12 179(100) . . . . ? C13 Fe2 C12 O12 -84(17) . . . . ? C19 Fe2 C12 O12 88(17) . . . . ? S2 Fe2 C12 O12 15(18) . . . . ? Fe1 Fe2 C12 O12 18(17) . . . . ? C12 Fe2 C13 O13 -37(6) . . . . ? C11 Fe2 C13 O13 66(6) . . . . ? C19 Fe2 C13 O13 -102(6) . . . . ? S2 Fe2 C13 O13 169(6) . . . . ? Fe1 Fe2 C13 O13 -135(6) . . . . ? C18 N1 C14 C15 3.5(7) . . . . ? Re2 N1 C14 C15 -176.9(4) . . . . ? C18 N1 C14 S1 -173.0(3) . . . . ? Re2 N1 C14 S1 6.5(3) . . . . ? Re1 S1 C14 N1 -100.8(3) . . . . ? Re2 S1 C14 N1 -5.4(3) . . . . ? Re1 S1 C14 C15 82.8(5) . . . . ? Re2 S1 C14 C15 178.2(5) . . . . ? N1 C14 C15 C16 -4.5(7) . . . . ? S1 C14 C15 C16 171.4(4) . . . . ? C14 C15 C16 C17 1.8(7) . . . . ? C15 C16 C17 C18 1.6(7) . . . . ? C14 N1 C18 C17 0.1(7) . . . . ? Re2 N1 C18 C17 -179.2(4) . . . . ? C16 C17 C18 N1 -2.6(8) . . . . ? C23 N2 C19 C20 1.2(7) . . . . ? Fe1 N2 C19 C20 -174.2(4) . . . . ? C23 N2 C19 Fe2 -179.9(4) . . . . ? Fe1 N2 C19 Fe2 4.6(4) . . . . ? C12 Fe2 C19 N2 -103.5(4) . . . . ? C11 Fe2 C19 N2 153.8(4) . . . . ? C13 Fe2 C19 N2 -37.8(16) . . . . ? S2 Fe2 C19 N2 51.6(3) . . . . ? Fe1 Fe2 C19 N2 -3.6(3) . . . . ? C12 Fe2 C19 C20 75.2(5) . . . . ? C11 Fe2 C19 C20 -27.5(5) . . . . ? C13 Fe2 C19 C20 140.9(13) . . . . ? S2 Fe2 C19 C20 -129.8(5) . . . . ? Fe1 Fe2 C19 C20 175.1(5) . . . . ? N2 C19 C20 C21 -2.3(7) . . . . ? Fe2 C19 C20 C21 179.1(4) . . . . ? C19 C20 C21 C22 1.1(8) . . . . ? C20 C21 C22 C23 1.2(8) . . . . ? C19 N2 C23 C22 1.1(8) . . . . ? Fe1 N2 C23 C22 175.2(4) . . . . ? C21 C22 C23 N2 -2.3(8) . . . . ? C10A Fe1A Fe2A C12A -87.6(3) . . . . ? C9A Fe1A Fe2A C12A 1.4(3) . . . . ? C8A Fe1A Fe2A C12A 142.0(6) . . . . ? N2A Fe1A Fe2A C12A 88.1(2) . . . . ? S2A Fe1A Fe2A C12A -176.2(2) . . . . ? C10A Fe1A Fe2A C11A 140.6(5) . . . . ? C9A Fe1A Fe2A C11A -130.4(5) . . . . ? C8A Fe1A Fe2A C11A 10.3(7) . . . . ? N2A Fe1A Fe2A C11A -43.7(5) . . . . ? S2A Fe1A Fe2A C11A 52.0(5) . . . . ? C10A Fe1A Fe2A C13A 4.5(3) . . . . ? C9A Fe1A Fe2A C13A 93.5(3) . . . . ? C8A Fe1A Fe2A C13A -125.9(6) . . . . ? N2A Fe1A Fe2A C13A -179.8(2) . . . . ? S2A Fe1A Fe2A C13A -84.11(19) . . . . ? C10A Fe1A Fe2A C19A -172.7(2) . . . . ? C9A Fe1A Fe2A C19A -83.7(3) . . . . ? C8A Fe1A Fe2A C19A 56.9(6) . . . . ? N2A Fe1A Fe2A C19A 3.0(2) . . . . ? S2A Fe1A Fe2A C19A 98.67(16) . . . . ? C10A Fe1A Fe2A S2A 88.60(18) . . . . ? C9A Fe1A Fe2A S2A 177.6(2) . . . . ? C8A Fe1A Fe2A S2A -41.8(5) . . . . ? N2A Fe1A Fe2A S2A -95.68(14) . . . . ? C2A Re1A S1A C14A -119.1(2) . . . . ? C1A Re1A S1A C14A -141.1(18) . . . . ? C3A Re1A S1A C14A -27.2(2) . . . . ? C4A Re1A S1A C14A 151.0(2) . . . . ? S2A Re1A S1A C14A 62.87(18) . . . . ? C2A Re1A S1A Re2A 159.07(16) . . . . ? C1A Re1A S1A Re2A 137.1(18) . . . . ? C3A Re1A S1A Re2A -109.01(14) . . . . ? C4A Re1A S1A Re2A 69.20(15) . . . . ? S2A Re1A S1A Re2A -18.92(4) . . . . ? C5A Re2A S1A C14A 12.7(8) . . . . ? C7A Re2A S1A C14A -174.0(2) . . . . ? C6A Re2A S1A C14A 93.7(2) . . . . ? N1A Re2A S1A C14A 1.7(2) . . . . ? S2A Re2A S1A C14A -85.20(16) . . . . ? C5A Re2A S1A Re1A 116.9(8) . . . . ? C7A Re2A S1A Re1A -69.77(17) . . . . ? C6A Re2A S1A Re1A -162.03(16) . . . . ? N1A Re2A S1A Re1A 105.96(12) . . . . ? S2A Re2A S1A Re1A 19.02(4) . . . . ? C12A Fe2A S2A Fe1A 8.6(4) . . . . ? C11A Fe2A S2A Fe1A -158.4(2) . . . . ? C13A Fe2A S2A Fe1A 105.3(2) . . . . ? C19A Fe2A S2A Fe1A -69.10(15) . . . . ? C12A Fe2A S2A Re2A -105.7(4) . . . . ? C11A Fe2A S2A Re2A 87.3(2) . . . . ? C13A Fe2A S2A Re2A -8.9(2) . . . . ? C19A Fe2A S2A Re2A 176.65(15) . . . . ? Fe1A Fe2A S2A Re2A -114.24(7) . . . . ? C12A Fe2A S2A Re1A 127.1(4) . . . . ? C11A Fe2A S2A Re1A -39.9(2) . . . . ? C13A Fe2A S2A Re1A -136.1(2) . . . . ? C19A Fe2A S2A Re1A 49.46(16) . . . . ? Fe1A Fe2A S2A Re1A 118.56(6) . . . . ? C10A Fe1A S2A Fe2A -96.41(18) . . . . ? C9A Fe1A S2A Fe2A -4.6(4) . . . . ? C8A Fe1A S2A Fe2A 166.72(19) . . . . ? N2A Fe1A S2A Fe2A 72.78(14) . . . . ? C10A Fe1A S2A Re2A 22.84(19) . . . . ? C9A Fe1A S2A Re2A 114.6(4) . . . . ? C8A Fe1A S2A Re2A -74.0(2) . . . . ? N2A Fe1A S2A Re2A -167.97(14) . . . . ? Fe2A Fe1A S2A Re2A 119.25(7) . . . . ? C10A Fe1A S2A Re1A 149.04(19) . . . . ? C9A Fe1A S2A Re1A -119.2(4) . . . . ? C8A Fe1A S2A Re1A 52.2(2) . . . . ? N2A Fe1A S2A Re1A -41.77(15) . . . . ? Fe2A Fe1A S2A Re1A -114.55(7) . . . . ? C5A Re2A S2A Fe2A 36.7(2) . . . . ? C7A Re2A S2A Fe2A -51.94(18) . . . . ? C6A Re2A S2A Fe2A -161.5(9) . . . . ? N1A Re2A S2A Fe2A 137.66(13) . . . . ? S1A Re2A S2A Fe2A -155.53(7) . . . . ? C5A Re2A S2A Fe1A -48.4(2) . . . . ? C7A Re2A S2A Fe1A -137.08(18) . . . . ? C6A Re2A S2A Fe1A 113.4(9) . . . . ? N1A Re2A S2A Fe1A 52.52(13) . . . . ? S1A Re2A S2A Fe1A 119.33(6) . . . . ? C5A Re2A S2A Re1A 173.59(19) . . . . ? C7A Re2A S2A Re1A 84.91(18) . . . . ? C6A Re2A S2A Re1A -24.6(9) . . . . ? N1A Re2A S2A Re1A -85.49(12) . . . . ? S1A Re2A S2A Re1A -18.68(4) . . . . ? C2A Re1A S2A Fe2A 147.8(8) . . . . ? C1A Re1A S2A Fe2A -20.03(17) . . . . ? C3A Re1A S2A Fe2A -110.05(15) . . . . ? C4A Re1A S2A Fe2A 67.72(16) . . . . ? S1A Re1A S2A Fe2A 157.79(6) . . . . ? C2A Re1A S2A Fe1A -127.2(8) . . . . ? C1A Re1A S2A Fe1A 64.93(17) . . . . ? C3A Re1A S2A Fe1A -25.09(15) . . . . ? C4A Re1A S2A Fe1A 152.69(16) . . . . ? S1A Re1A S2A Fe1A -117.25(7) . . . . ? C2A Re1A S2A Re2A 8.8(8) . . . . ? C1A Re1A S2A Re2A -159.05(16) . . . . ? C3A Re1A S2A Re2A 110.93(15) . . . . ? C4A Re1A S2A Re2A -71.29(16) . . . . ? S1A Re1A S2A Re2A 18.77(4) . . . . ? C5A Re2A N1A C18A 1.4(5) . . . . ? C7A Re2A N1A C18A -158.9(10) . . . . ? C6A Re2A N1A C18A 89.5(5) . . . . ? S1A Re2A N1A C18A 179.1(5) . . . . ? S2A Re2A N1A C18A -99.4(5) . . . . ? C5A Re2A N1A C14A -180.0(3) . . . . ? C7A Re2A N1A C14A 19.7(12) . . . . ? C6A Re2A N1A C14A -92.0(3) . . . . ? S1A Re2A N1A C14A -2.3(3) . . . . ? S2A Re2A N1A C14A 79.2(3) . . . . ? C10A Fe1A N2A C19A 18.4(13) . . . . ? C9A Fe1A N2A C19A 90.4(4) . . . . ? C8A Fe1A N2A C19A -169.1(4) . . . . ? S2A Fe1A N2A C19A -59.5(3) . . . . ? Fe2A Fe1A N2A C19A -4.3(3) . . . . ? C10A Fe1A N2A C23A -155.8(10) . . . . ? C9A Fe1A N2A C23A -83.8(5) . . . . ? C8A Fe1A N2A C23A 16.7(5) . . . . ? S2A Fe1A N2A C23A 126.3(5) . . . . ? Fe2A Fe1A N2A C23A -178.5(5) . . . . ? C2A Re1A C1A O1A 1(4) . . . . ? C3A Re1A C1A O1A -91(4) . . . . ? C4A Re1A C1A O1A 91(4) . . . . ? S1A Re1A C1A O1A 23(5) . . . . ? S2A Re1A C1A O1A 178(100) . . . . ? C1A Re1A C2A O2A 178(100) . . . . ? C3A Re1A C2A O2A -92(37) . . . . ? C4A Re1A C2A O2A 90(37) . . . . ? S1A Re1A C2A O2A 0(37) . . . . ? S2A Re1A C2A O2A 10(38) . . . . ? C2A Re1A C3A O3A -93(28) . . . . ? C1A Re1A C3A O3A -7(28) . . . . ? C4A Re1A C3A O3A 40(30) . . . . ? S1A Re1A C3A O3A 177(100) . . . . ? S2A Re1A C3A O3A 98(28) . . . . ? C2A Re1A C4A O4A 63(12) . . . . ? C1A Re1A C4A O4A -23(12) . . . . ? C3A Re1A C4A O4A -71(13) . . . . ? S1A Re1A C4A O4A 152(12) . . . . ? S2A Re1A C4A O4A -129(12) . . . . ? C7A Re2A C5A O5A -81(7) . . . . ? C6A Re2A C5A O5A 11(7) . . . . ? N1A Re2A C5A O5A 102(7) . . . . ? S1A Re2A C5A O5A 92(7) . . . . ? S2A Re2A C5A O5A -172(7) . . . . ? C5A Re2A C6A O6A 81(18) . . . . ? C7A Re2A C6A O6A 169(18) . . . . ? N1A Re2A C6A O6A -21(18) . . . . ? S1A Re2A C6A O6A -87(18) . . . . ? S2A Re2A C6A O6A -81(18) . . . . ? C5A Re2A C7A O7A -76(22) . . . . ? C6A Re2A C7A O7A -164(22) . . . . ? N1A Re2A C7A O7A 85(22) . . . . ? S1A Re2A C7A O7A 105(22) . . . . ? S2A Re2A C7A O7A 26(22) . . . . ? C10A Fe1A C8A O8A 93(6) . . . . ? C9A Fe1A C8A O8A 3(6) . . . . ? N2A Fe1A C8A O8A -86(6) . . . . ? S2A Fe1A C8A O8A -172(6) . . . . ? Fe2A Fe1A C8A O8A -137(6) . . . . ? C10A Fe1A C9A O9A 115(94) . . . . ? C8A Fe1A C9A O9A -150(94) . . . . ? N2A Fe1A C9A O9A -55(94) . . . . ? S2A Fe1A C9A O9A 22(94) . . . . ? Fe2A Fe1A C9A O9A 18(94) . . . . ? C9A Fe1A C10A O10A 17(6) . . . . ? C8A Fe1A C10A O10A -83(6) . . . . ? N2A Fe1A C10A O10A 89(6) . . . . ? S2A Fe1A C10A O10A 167(6) . . . . ? Fe2A Fe1A C10A O10A 111(6) . . . . ? C12A Fe2A C11A O11A -61(8) . . . . ? C13A Fe2A C11A O11A -151(8) . . . . ? C19A Fe2A C11A O11A 28(8) . . . . ? S2A Fe2A C11A O11A 114(8) . . . . ? Fe1A Fe2A C11A O11A 71(8) . . . . ? C11A Fe2A C12A O12A -38(22) . . . . ? C13A Fe2A C12A O12A 57(22) . . . . ? C19A Fe2A C12A O12A -128(22) . . . . ? S2A Fe2A C12A O12A 155(22) . . . . ? Fe1A Fe2A C12A O12A 162(22) . . . . ? C12A Fe2A C13A O13A -52(7) . . . . ? C11A Fe2A C13A O13A 47(7) . . . . ? C19A Fe2A C13A O13A -123(6) . . . . ? S2A Fe2A C13A O13A 153(7) . . . . ? Fe1A Fe2A C13A O13A -151(7) . . . . ? C18A N1A C14A C15A -0.5(7) . . . . ? Re2A N1A C14A C15A -179.4(4) . . . . ? C18A N1A C14A S1A -177.9(4) . . . . ? Re2A N1A C14A S1A 3.2(4) . . . . ? Re1A S1A C14A N1A -98.5(3) . . . . ? Re2A S1A C14A N1A -2.7(3) . . . . ? Re1A S1A C14A C15A 84.3(5) . . . . ? Re2A S1A C14A C15A -179.9(5) . . . . ? N1A C14A C15A C16A -0.6(8) . . . . ? S1A C14A C15A C16A 176.3(4) . . . . ? C14A C15A C16A C17A 1.2(8) . . . . ? C15A C16A C17A C18A -0.7(8) . . . . ? C14A N1A C18A C17A 1.0(7) . . . . ? Re2A N1A C18A C17A 179.5(4) . . . . ? C16A C17A C18A N1A -0.4(8) . . . . ? C23A N2A C19A C20A 2.2(8) . . . . ? Fe1A N2A C19A C20A -172.6(4) . . . . ? C23A N2A C19A Fe2A -179.5(4) . . . . ? Fe1A N2A C19A Fe2A 5.7(4) . . . . ? C12A Fe2A C19A N2A -103.9(4) . . . . ? C11A Fe2A C19A N2A 156.6(4) . . . . ? C13A Fe2A C19A N2A -33(3) . . . . ? S2A Fe2A C19A N2A 50.6(3) . . . . ? Fe1A Fe2A C19A N2A -4.4(3) . . . . ? C12A Fe2A C19A C20A 74.1(5) . . . . ? C11A Fe2A C19A C20A -25.4(5) . . . . ? C13A Fe2A C19A C20A 145(2) . . . . ? S2A Fe2A C19A C20A -131.3(5) . . . . ? Fe1A Fe2A C19A C20A 173.6(5) . . . . ? N2A C19A C20A C21A -3.2(8) . . . . ? Fe2A C19A C20A C21A 178.9(4) . . . . ? C19A C20A C21A C22A 1.1(9) . . . . ? C20A C21A C22A C23A 2.0(9) . . . . ? C19A N2A C23A C22A 0.9(8) . . . . ? Fe1A N2A C23A C22A 174.4(4) . . . . ? C21A C22A C23A N2A -3.0(9) . . . . ? _diffrn_measured_fraction_theta_max 0.937 _diffrn_reflns_theta_full 67.95 _diffrn_measured_fraction_theta_full 0.937 _refine_diff_density_max 1.298 _refine_diff_density_min -0.993 _refine_diff_density_rms 0.131 # Attachment '- Compound 9.CIF' data_comp9 _database_code_depnum_ccdc_archive 'CCDC 748076' #TrackingRef '- Compound 9.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H8 Fe4 N2 O12 S' _chemical_formula_sum 'C22 H8 Fe4 N2 O12 S' _chemical_formula_weight 747.76 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' N N 0.0061 0.0033 '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' S S 0.1246 0.1234 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' 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 9.1790(9) _cell_length_b 19.723(2) _cell_length_c 15.1253(15) _cell_angle_alpha 90.00 _cell_angle_beta 91.587(8) _cell_angle_gamma 90.00 _cell_volume 2737.2(5) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 4897 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description Block _exptl_crystal_colour Red _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.815 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1480 _exptl_absorpt_coefficient_mu 2.218 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6070 _exptl_absorpt_correction_T_max 0.6411 _exptl_absorpt_process_details ; [Blessing, Acta Cryst. (1995)] ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'Nonius KappaCCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 5165 _diffrn_reflns_av_R_equivalents 0.0152 _diffrn_reflns_av_sigmaI/netI 0.0647 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 25.17 _reflns_number_total 4897 _reflns_number_gt 3227 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'DENZO (Otwinowski & Minor, 1997) and COLLECT (Hooft, 1998)' _computing_cell_refinement 'DENZO and COLLECT' _computing_data_reduction 'DENZO and COLLECT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 for windows (Farrugia, 1997)' _computing_publication_material 'WinGX (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0348P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4897 _refine_ls_number_parameters 360 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0734 _refine_ls_R_factor_gt 0.0354 _refine_ls_wR_factor_ref 0.0782 _refine_ls_wR_factor_gt 0.0721 _refine_ls_goodness_of_fit_ref 0.944 _refine_ls_restrained_S_all 0.944 _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 Fe1 Fe 0.44622(6) 0.23434(3) 0.59619(3) 0.03916(15) Uani 1 1 d . . . Fe2 Fe 0.22123(5) 0.25141(3) 0.69468(3) 0.03710(14) Uani 1 1 d . . . Fe3 Fe 0.42622(6) 0.43296(3) 0.65426(4) 0.04442(16) Uani 1 1 d . . . Fe4 Fe 0.54773(6) 0.37471(3) 0.79145(4) 0.04139(15) Uani 1 1 d . . . S1 S 0.41174(9) 0.32266(4) 0.68557(6) 0.0338(2) Uani 1 1 d . . . O1 O 0.7535(4) 0.22852(18) 0.5472(2) 0.0924(12) Uani 1 1 d . . . O2 O 0.3453(4) 0.10940(15) 0.5103(2) 0.0798(10) Uani 1 1 d . . . O3 O 0.3513(3) 0.31540(15) 0.4417(2) 0.0712(9) Uani 1 1 d . . . O4 O 0.0550(4) 0.13276(17) 0.6315(2) 0.0931(12) Uani 1 1 d . . . O5 O 0.0462(3) 0.33980(15) 0.57832(19) 0.0648(8) Uani 1 1 d . . . O6 O 0.0631(4) 0.29270(17) 0.8525(2) 0.0809(10) Uani 1 1 d . . . O7 O 0.6573(4) 0.40237(17) 0.5290(3) 0.0954(12) Uani 1 1 d . . . O8 O 0.2006(4) 0.46561(16) 0.5191(2) 0.0900(12) Uani 1 1 d . . . O9 O 0.5259(4) 0.57198(15) 0.6884(2) 0.0915(12) Uani 1 1 d . . . O10 O 0.8122(4) 0.3234(2) 0.7132(3) 0.1211(16) Uani 1 1 d . . . O11 O 0.6965(4) 0.49564(17) 0.8626(3) 0.0936(12) Uani 1 1 d . . . O12 O 0.5678(4) 0.27978(15) 0.9415(2) 0.0758(10) Uani 1 1 d . . . N1A N 0.3617(3) 0.19096(14) 0.75863(19) 0.0406(6) Uani 0.874(19) 1 d P . . C13A C 0.3617(3) 0.19096(14) 0.75863(19) 0.0406(6) Uani 0.126(19) 1 d P . . N1B N 0.4790(4) 0.18300(16) 0.7076(2) 0.0406(6) Uani 0.126(19) 1 d P . . C13B C 0.4790(4) 0.18300(16) 0.7076(2) 0.0406(6) Uani 0.874(19) 1 d P . . N2A N 0.3606(3) 0.41521(15) 0.8278(2) 0.0433(6) Uani 0.82(2) 1 d P . . C18A C 0.3606(3) 0.41521(15) 0.8278(2) 0.0433(6) Uani 0.18(2) 1 d P . . N2B N 0.2961(4) 0.44346(17) 0.7563(2) 0.0433(6) Uani 0.18(2) 1 d P . . C18B C 0.2961(4) 0.44346(17) 0.7563(2) 0.0433(6) Uani 0.82(2) 1 d P . . C1 C 0.6345(5) 0.2318(2) 0.5668(3) 0.0549(11) Uani 1 1 d . . . C2 C 0.3846(5) 0.1579(2) 0.5450(3) 0.0504(10) Uani 1 1 d . . . C3 C 0.3858(4) 0.28415(19) 0.5003(3) 0.0458(10) Uani 1 1 d . . . C4 C 0.1205(4) 0.1781(2) 0.6569(3) 0.0547(11) Uani 1 1 d . . . C5 C 0.1152(4) 0.3051(2) 0.6230(3) 0.0440(9) Uani 1 1 d . . . C6 C 0.1238(4) 0.2767(2) 0.7919(3) 0.0491(10) Uani 1 1 d . . . C7 C 0.5692(5) 0.4152(2) 0.5770(3) 0.0616(12) Uani 1 1 d . . . C8 C 0.2871(5) 0.4515(2) 0.5710(3) 0.0602(12) Uani 1 1 d . . . C9 C 0.4888(5) 0.5176(2) 0.6752(3) 0.0596(12) Uani 1 1 d . . . C10 C 0.7098(5) 0.3439(3) 0.7433(3) 0.0681(13) Uani 1 1 d . . . C11 C 0.6386(5) 0.4491(2) 0.8347(3) 0.0601(12) Uani 1 1 d . . . C12 C 0.5592(4) 0.3159(2) 0.8829(3) 0.0498(10) Uani 1 1 d . . . C14 C 0.5926(4) 0.14287(19) 0.7390(3) 0.0550(11) Uani 1 1 d . . . H14 H 0.6744 0.1368 0.7050 0.066 Uiso 1 1 calc R . . C15 C 0.5856(5) 0.1116(2) 0.8208(3) 0.0647(13) Uani 1 1 d . . . H15 H 0.6629 0.0852 0.8419 0.078 Uiso 1 1 calc R . . C16 C 0.4645(6) 0.11987(19) 0.8706(3) 0.0608(12) Uani 1 1 d . . . H16 H 0.4578 0.0984 0.9251 0.073 Uiso 1 1 calc R . . C17 C 0.3534(5) 0.16027(18) 0.8387(2) 0.0519(10) Uani 1 1 d . . . H17 H 0.2713 0.1667 0.8724 0.062 Uiso 1 1 calc R . . C19 C 0.1628(5) 0.4745(2) 0.7648(3) 0.0615(12) Uani 1 1 d . . . H19 H 0.1158 0.4935 0.7155 0.074 Uiso 1 1 calc R . . C20 C 0.0988(5) 0.4775(2) 0.8461(4) 0.0712(14) Uani 1 1 d . . . H20 H 0.0082 0.4980 0.8516 0.085 Uiso 1 1 calc R . . C21 C 0.1695(5) 0.4502(2) 0.9185(3) 0.0695(13) Uani 1 1 d . . . H21 H 0.1285 0.4527 0.9740 0.083 Uiso 1 1 calc R . . C22 C 0.3009(5) 0.41923(19) 0.9083(3) 0.0546(11) Uani 1 1 d . . . H22 H 0.3499 0.4007 0.9573 0.066 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 Fe1 0.0407(3) 0.0439(3) 0.0330(3) -0.0004(2) 0.0033(2) 0.0017(2) Fe2 0.0343(3) 0.0452(3) 0.0318(3) 0.0055(2) 0.0010(2) -0.0038(2) Fe3 0.0538(4) 0.0408(3) 0.0385(3) 0.0067(2) -0.0008(3) -0.0079(3) Fe4 0.0347(3) 0.0515(3) 0.0378(3) -0.0004(3) -0.0027(2) -0.0019(2) S1 0.0334(5) 0.0379(5) 0.0301(5) 0.0028(4) 0.0016(4) -0.0012(4) O1 0.051(2) 0.125(3) 0.103(3) -0.017(2) 0.025(2) 0.006(2) O2 0.104(3) 0.056(2) 0.079(2) -0.0159(18) -0.010(2) -0.0074(18) O3 0.090(2) 0.075(2) 0.0481(19) 0.0223(16) -0.0034(17) 0.0051(18) O4 0.107(3) 0.083(2) 0.088(3) -0.001(2) -0.014(2) -0.051(2) O5 0.0576(19) 0.077(2) 0.0592(19) 0.0185(17) -0.0062(16) 0.0109(16) O6 0.082(2) 0.110(3) 0.052(2) -0.003(2) 0.0271(18) -0.001(2) O7 0.108(3) 0.091(3) 0.090(3) 0.004(2) 0.053(2) -0.020(2) O8 0.114(3) 0.068(2) 0.085(3) 0.0231(19) -0.049(2) -0.014(2) O9 0.132(3) 0.054(2) 0.088(3) -0.0017(18) 0.004(2) -0.034(2) O10 0.045(2) 0.225(5) 0.095(3) -0.031(3) 0.008(2) 0.027(3) O11 0.090(3) 0.075(2) 0.114(3) -0.006(2) -0.035(2) -0.032(2) O12 0.096(3) 0.071(2) 0.059(2) 0.0161(18) -0.0163(19) 0.0049(18) N1A 0.0472(15) 0.0374(12) 0.0367(15) 0.0035(11) -0.0057(11) -0.0010(12) C13A 0.0472(15) 0.0374(12) 0.0367(15) 0.0035(11) -0.0057(11) -0.0010(12) N1B 0.0472(15) 0.0374(12) 0.0367(15) 0.0035(11) -0.0057(11) -0.0010(12) C13B 0.0472(15) 0.0374(12) 0.0367(15) 0.0035(11) -0.0057(11) -0.0010(12) N2A 0.0442(15) 0.0404(14) 0.0452(15) -0.0009(11) 0.0004(12) 0.0013(11) C18A 0.0442(15) 0.0404(14) 0.0452(15) -0.0009(11) 0.0004(12) 0.0013(11) N2B 0.0442(15) 0.0404(14) 0.0452(15) -0.0009(11) 0.0004(12) 0.0013(11) C18B 0.0442(15) 0.0404(14) 0.0452(15) -0.0009(11) 0.0004(12) 0.0013(11) C1 0.054(3) 0.062(3) 0.050(3) -0.004(2) 0.009(2) 0.002(2) C2 0.061(3) 0.052(3) 0.039(2) 0.003(2) 0.000(2) 0.004(2) C3 0.050(2) 0.048(2) 0.040(2) -0.002(2) 0.010(2) -0.0023(19) C4 0.056(3) 0.061(3) 0.046(3) 0.010(2) -0.002(2) -0.012(2) C5 0.034(2) 0.058(2) 0.040(2) 0.0031(19) 0.0037(18) -0.0034(19) C6 0.043(2) 0.065(3) 0.040(2) 0.009(2) 0.000(2) -0.003(2) C7 0.075(3) 0.057(3) 0.053(3) 0.008(2) 0.015(3) -0.019(2) C8 0.084(4) 0.040(2) 0.055(3) 0.008(2) -0.010(3) -0.016(2) C9 0.068(3) 0.056(3) 0.055(3) 0.004(2) -0.001(2) -0.012(2) C10 0.038(3) 0.107(4) 0.059(3) -0.003(3) 0.001(2) -0.001(3) C11 0.055(3) 0.066(3) 0.058(3) 0.001(2) -0.011(2) -0.004(2) C12 0.050(3) 0.054(2) 0.045(3) -0.008(2) -0.011(2) 0.000(2) C14 0.054(3) 0.048(2) 0.062(3) -0.003(2) -0.011(2) 0.009(2) C15 0.077(3) 0.044(3) 0.070(3) 0.012(2) -0.033(3) 0.002(2) C16 0.093(4) 0.044(2) 0.044(3) 0.011(2) -0.025(3) -0.011(2) C17 0.074(3) 0.047(2) 0.034(2) 0.0070(19) -0.005(2) -0.006(2) C19 0.061(3) 0.052(3) 0.071(3) 0.004(2) -0.003(3) 0.016(2) C20 0.057(3) 0.069(3) 0.087(4) -0.009(3) 0.013(3) 0.017(2) C21 0.071(3) 0.072(3) 0.067(3) -0.016(3) 0.029(3) 0.003(3) C22 0.062(3) 0.059(3) 0.044(3) 0.000(2) 0.011(2) -0.001(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 Fe1 C1 1.797(4) . ? Fe1 C2 1.781(4) . ? Fe1 C3 1.825(4) . ? Fe1 N1B 1.982(3) . ? Fe1 S1 2.2330(10) . ? Fe1 Fe2 2.6015(8) . ? Fe2 C4 1.801(4) . ? Fe2 C5 1.785(4) . ? Fe2 C6 1.812(4) . ? Fe2 N1A 1.987(3) . ? Fe2 S1 2.2505(10) . ? Fe3 C7 1.816(5) . ? Fe3 C8 1.806(5) . ? Fe3 C9 1.791(4) . ? Fe3 N2B 1.988(4) . ? Fe3 S1 2.2312(10) . ? Fe3 Fe4 2.5965(8) . ? Fe4 C10 1.781(5) . ? Fe4 C11 1.802(5) . ? Fe4 C12 1.807(4) . ? Fe4 N2A 1.986(3) . ? Fe4 S1 2.2508(10) . ? O1 C1 1.142(5) . ? O2 C2 1.144(4) . ? O3 C3 1.119(4) . ? O4 C4 1.139(4) . ? O5 C5 1.142(4) . ? O6 C6 1.131(4) . ? O7 C7 1.129(5) . ? O8 C8 1.135(5) . ? O9 C9 1.141(4) . ? O10 C10 1.131(5) . ? O11 C11 1.135(5) . ? O12 C12 1.137(4) . ? N1A N1B 1.351(4) . ? N1B C14 1.383(5) . ? N2A N2B 1.340(5) . ? N2A C22 1.351(5) . ? C14 C15 1.385(6) . ? C14 H14 0.9300 . ? C15 C16 1.370(6) . ? C15 H15 0.9300 . ? C16 C17 1.372(6) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C19 C20 1.378(6) . ? C19 H19 0.9300 . ? C20 C21 1.368(6) . ? C20 H20 0.9300 . ? C21 C22 1.365(6) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? 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 Fe1 C1 99.50(19) . . ? C2 Fe1 C3 91.40(17) . . ? C1 Fe1 C3 95.26(18) . . ? C2 Fe1 N1B 88.63(15) . . ? C1 Fe1 N1B 94.13(17) . . ? C3 Fe1 N1B 170.47(16) . . ? C2 Fe1 S1 151.11(13) . . ? C1 Fe1 S1 108.94(14) . . ? C3 Fe1 S1 90.92(12) . . ? N1B Fe1 S1 84.51(10) . . ? C2 Fe1 Fe2 96.38(13) . . ? C1 Fe1 Fe2 158.33(14) . . ? C3 Fe1 Fe2 99.01(12) . . ? N1B Fe1 Fe2 71.53(11) . . ? S1 Fe1 Fe2 54.85(3) . . ? C5 Fe2 C4 90.97(18) . . ? C5 Fe2 C6 93.30(17) . . ? C4 Fe2 C6 102.58(18) . . ? C5 Fe2 N1A 170.73(15) . . ? C4 Fe2 N1A 89.60(15) . . ? C6 Fe2 N1A 95.60(15) . . ? C5 Fe2 S1 90.23(12) . . ? C4 Fe2 S1 151.03(14) . . ? C6 Fe2 S1 106.25(13) . . ? N1A Fe2 S1 84.83(9) . . ? C5 Fe2 Fe1 99.02(12) . . ? C4 Fe2 Fe1 97.06(14) . . ? C6 Fe2 Fe1 156.60(13) . . ? N1A Fe2 Fe1 71.73(9) . . ? S1 Fe2 Fe1 54.22(3) . . ? C9 Fe3 C8 98.72(19) . . ? C9 Fe3 C7 93.46(19) . . ? C8 Fe3 C7 95.7(2) . . ? C9 Fe3 N2B 87.81(17) . . ? C8 Fe3 N2B 95.28(18) . . ? C7 Fe3 N2B 168.59(18) . . ? C9 Fe3 S1 153.12(14) . . ? C8 Fe3 S1 107.49(12) . . ? C7 Fe3 S1 89.81(13) . . ? N2B Fe3 S1 84.04(10) . . ? C9 Fe3 Fe4 98.18(14) . . ? C8 Fe3 Fe4 157.94(13) . . ? C7 Fe3 Fe4 97.29(15) . . ? N2B Fe3 Fe4 71.32(11) . . ? S1 Fe3 Fe4 54.95(3) . . ? C10 Fe4 C11 92.5(2) . . ? C10 Fe4 C12 93.6(2) . . ? C11 Fe4 C12 103.21(18) . . ? C10 Fe4 N2A 171.53(18) . . ? C11 Fe4 N2A 88.13(17) . . ? C12 Fe4 N2A 94.52(16) . . ? C10 Fe4 S1 90.36(15) . . ? C11 Fe4 S1 150.68(14) . . ? C12 Fe4 S1 105.73(12) . . ? N2A Fe4 S1 85.04(9) . . ? C10 Fe4 Fe3 99.75(15) . . ? C11 Fe4 Fe3 96.56(14) . . ? C12 Fe4 Fe3 155.62(12) . . ? N2A Fe4 Fe3 71.79(10) . . ? S1 Fe4 Fe3 54.25(3) . . ? Fe3 S1 Fe1 128.45(4) . . ? Fe3 S1 Fe2 132.28(4) . . ? Fe1 S1 Fe2 70.93(3) . . ? Fe3 S1 Fe4 70.80(3) . . ? Fe1 S1 Fe4 134.55(4) . . ? Fe2 S1 Fe4 131.13(4) . . ? N1B N1A Fe2 107.9(2) . . ? N1A N1B C14 118.4(3) . . ? N1A N1B Fe1 108.8(2) . . ? C14 N1B Fe1 132.8(3) . . ? N2B N2A C22 121.5(3) . . ? N2B N2A Fe4 108.0(2) . . ? C22 N2A Fe4 130.4(3) . . ? N2A N2B Fe3 108.8(2) . . ? O1 C1 Fe1 178.1(4) . . ? O2 C2 Fe1 178.5(4) . . ? O3 C3 Fe1 178.6(4) . . ? O4 C4 Fe2 178.3(4) . . ? O5 C5 Fe2 178.8(4) . . ? O6 C6 Fe2 179.7(4) . . ? O7 C7 Fe3 178.2(4) . . ? O8 C8 Fe3 177.5(4) . . ? O9 C9 Fe3 178.6(4) . . ? O10 C10 Fe4 178.9(5) . . ? O11 C11 Fe4 179.4(4) . . ? O12 C12 Fe4 178.6(4) . . ? N1B C14 C15 120.6(4) . . ? N1B C14 H14 119.7 . . ? C15 C14 H14 119.7 . . ? C16 C15 C14 119.8(4) . . ? C16 C15 H15 120.1 . . ? C14 C15 H15 120.1 . . ? C15 C16 C17 118.9(4) . . ? C15 C16 H16 120.6 . . ? C17 C16 H16 120.6 . . ? C16 C17 H17 119.6 . . ? C20 C19 H19 119.9 . . ? C21 C20 C19 119.5(4) . . ? C21 C20 H20 120.2 . . ? C19 C20 H20 120.2 . . ? C22 C21 C20 119.1(4) . . ? C22 C21 H21 120.4 . . ? C20 C21 H21 120.4 . . ? N2A C22 C21 120.6(4) . . ? N2A C22 H22 119.7 . . ? C21 C22 H22 119.7 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.17 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.347 _refine_diff_density_min -0.331 _refine_diff_density_rms 0.074 # Attachment '- Compound 10.cif' data_dthf _database_code_depnum_ccdc_archive 'CCDC 748077' #TrackingRef '- Compound 10.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H19 N O12 Os3 P Re S' _chemical_formula_weight 1465.34 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' N N 0.0061 0.0033 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -1.0185 7.2310 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 2(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 13.1359(13) _cell_length_b 15.1378(15) _cell_length_c 18.6633(19) _cell_angle_alpha 90.00 _cell_angle_beta 98.3000(10) _cell_angle_gamma 90.00 _cell_volume 3672.3(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8212 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 31.5 _exptl_crystal_description prism _exptl_crystal_colour purple-red _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.650 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2664 _exptl_absorpt_coefficient_mu 13.797 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.0923 _exptl_absorpt_correction_T_max 0.5756 _exptl_absorpt_process_details ; Numerical (based on real shape of the crystal) absorption correction followed by: SADABS. Program for empirical absorption correction of area-detector data. University of Goetingen. Germany. Sheldrick, G. M. 1996 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 APEX2 CCD detector' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 60539 _diffrn_reflns_av_R_equivalents 0.0315 _diffrn_reflns_av_sigmaI/netI 0.0233 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 32.02 _reflns_number_total 12142 _reflns_number_gt 10783 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 v2.0-2 (Bruker, 2005)' _computing_cell_refinement 'SAINT v7.23A (Bruker, 2005)' _computing_data_reduction 'SADABS-2004/1 (Bruker, 2005)' _computing_structure_solution 'XS/SHELXTL v6.12 (Bruker, 2001)' _computing_structure_refinement 'XL/SHELXTL v6.10 (Bruker, 2001)' _computing_molecular_graphics 'XP v5.1 (Bruker, 1998)' _computing_publication_material 'XCIF v6.12 (Bruker, 2001)' _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^)+(0.0214P)^2^+3.0630P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12142 _refine_ls_number_parameters 487 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0246 _refine_ls_R_factor_gt 0.0195 _refine_ls_wR_factor_ref 0.0443 _refine_ls_wR_factor_gt 0.0430 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 0.005 _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 0.132605(8) 0.764523(6) 0.169797(5) 0.01221(2) Uani 1 1 d . . . Os3 Os 0.352791(8) 0.768338(7) 0.195489(5) 0.01490(3) Uani 1 1 d . . . Os2 Os 0.246465(8) 0.716260(7) 0.308018(5) 0.01258(2) Uani 1 1 d . . . Re1 Re 0.451344(8) 0.645880(7) 0.302930(6) 0.01684(3) Uani 1 1 d . . . S1 S 0.33598(5) 0.85397(4) 0.30109(4) 0.01555(12) Uani 1 1 d . . . P1 P -0.04592(5) 0.74555(4) 0.16351(4) 0.01221(12) Uani 1 1 d . . . O1 O 0.15479(17) 0.56734(14) 0.13504(11) 0.0227(4) Uani 1 1 d . . . O2 O 0.1161(2) 0.95156(14) 0.23204(13) 0.0320(5) Uani 1 1 d . . . O3 O 0.12037(18) 0.81709(15) 0.01221(11) 0.0270(5) Uani 1 1 d . . . O4 O 0.15408(18) 0.53168(14) 0.29035(12) 0.0257(5) Uani 1 1 d . . . O5 O 0.07929(16) 0.81203(15) 0.37660(12) 0.0232(4) Uani 1 1 d . . . O6 O 0.34583(17) 0.67466(16) 0.46223(11) 0.0259(5) Uani 1 1 d . . . O7 O 0.3083(2) 0.93450(16) 0.10324(13) 0.0343(6) Uani 1 1 d . . . O8 O 0.3566(2) 0.63574(17) 0.07316(13) 0.0348(6) Uani 1 1 d . . . O9 O 0.58453(18) 0.79410(18) 0.20533(14) 0.0355(6) Uani 1 1 d . . . O10 O 0.50080(19) 0.51393(17) 0.42652(14) 0.0363(6) Uani 1 1 d . . . O11 O 0.6592(2) 0.59645(19) 0.25895(16) 0.0418(7) Uani 1 1 d . . . O12 O 0.35938(19) 0.48910(16) 0.21186(14) 0.0336(5) Uani 1 1 d . . . N1 N 0.50460(18) 0.76570(16) 0.36742(13) 0.0172(5) Uani 1 1 d . . . C1 C 0.1485(2) 0.64043(18) 0.14870(14) 0.0160(5) Uani 1 1 d . . . C2 C 0.1246(2) 0.88284(19) 0.20928(15) 0.0199(5) Uani 1 1 d . . . C3 C 0.1217(2) 0.79735(18) 0.07145(15) 0.0179(5) Uani 1 1 d . . . C4 C 0.1876(2) 0.60183(18) 0.29618(14) 0.0172(5) Uani 1 1 d . . . C5 C 0.1359(2) 0.77327(18) 0.34826(15) 0.0174(5) Uani 1 1 d . . . C6 C 0.3171(2) 0.68675(19) 0.40188(15) 0.0180(5) Uani 1 1 d . . . C7 C 0.3242(2) 0.8706(2) 0.13464(16) 0.0238(6) Uani 1 1 d . . . C8 C 0.3526(2) 0.6848(2) 0.11959(17) 0.0243(6) Uani 1 1 d . . . C9 C 0.4996(3) 0.7790(2) 0.20634(16) 0.0245(6) Uani 1 1 d . . . C10 C 0.4833(2) 0.5652(2) 0.38087(17) 0.0235(6) Uani 1 1 d . . . C11 C 0.5821(3) 0.6160(2) 0.27690(18) 0.0266(6) Uani 1 1 d . . . C12 C 0.3937(2) 0.5483(2) 0.24521(17) 0.0233(6) Uani 1 1 d . . . C13 C 0.4532(2) 0.84369(19) 0.36116(15) 0.0179(5) Uani 1 1 d . . . C14 C 0.4884(2) 0.9181(2) 0.40081(16) 0.0213(6) Uani 1 1 d . . . H14A H 0.4518 0.9723 0.3940 0.026 Uiso 1 1 calc R . . C15 C 0.5774(2) 0.9123(2) 0.45031(17) 0.0257(6) Uani 1 1 d . . . H15A H 0.6030 0.9625 0.4778 0.031 Uiso 1 1 calc R . . C16 C 0.6285(2) 0.8320(2) 0.45903(17) 0.0257(6) Uani 1 1 d . . . H16A H 0.6885 0.8257 0.4937 0.031 Uiso 1 1 calc R . . C17 C 0.5907(2) 0.7614(2) 0.41664(16) 0.0222(6) Uani 1 1 d . . . H17A H 0.6270 0.7070 0.4223 0.027 Uiso 1 1 calc R . . C18 C -0.0922(2) 0.73547(17) 0.25056(14) 0.0146(5) Uani 1 1 d . . . C19 C -0.1461(2) 0.80350(19) 0.27884(15) 0.0180(5) Uani 1 1 d . . . H19A H -0.1632 0.8556 0.2513 0.022 Uiso 1 1 calc R . . C20 C -0.1747(2) 0.7949(2) 0.34722(16) 0.0231(6) Uani 1 1 d . . . H20A H -0.2117 0.8412 0.3662 0.028 Uiso 1 1 calc R . . C21 C -0.1497(2) 0.7196(2) 0.38796(16) 0.0245(6) Uani 1 1 d . . . H21A H -0.1691 0.7144 0.4349 0.029 Uiso 1 1 calc R . . C22 C -0.0965(2) 0.6518(2) 0.36014(15) 0.0206(6) Uani 1 1 d . . . H22A H -0.0800 0.5998 0.3879 0.025 Uiso 1 1 calc R . . C23 C -0.0671(2) 0.65945(18) 0.29197(14) 0.0160(5) Uani 1 1 d . . . H23A H -0.0298 0.6130 0.2734 0.019 Uiso 1 1 calc R . . C24 C -0.1286(2) 0.83043(18) 0.11578(14) 0.0159(5) Uani 1 1 d . . . C25 C -0.0913(2) 0.90454(18) 0.08442(15) 0.0196(5) Uani 1 1 d . . . H25A H -0.0193 0.9146 0.0893 0.024 Uiso 1 1 calc R . . C26 C -0.1591(3) 0.9645(2) 0.04573(17) 0.0263(7) Uani 1 1 d . . . H26A H -0.1330 1.0144 0.0234 0.032 Uiso 1 1 calc R . . C27 C -0.2637(3) 0.9512(2) 0.03993(16) 0.0266(7) Uani 1 1 d . . . H27A H -0.3097 0.9925 0.0143 0.032 Uiso 1 1 calc R . . C28 C -0.3019(3) 0.8777(2) 0.07126(16) 0.0247(6) Uani 1 1 d . . . H28A H -0.3741 0.8689 0.0672 0.030 Uiso 1 1 calc R . . C29 C -0.2354(2) 0.81733(19) 0.10837(15) 0.0195(5) Uani 1 1 d . . . H29A H -0.2621 0.7665 0.1290 0.023 Uiso 1 1 calc R . . C30 C -0.0956(2) 0.64832(17) 0.11156(14) 0.0139(5) Uani 1 1 d . . . C31 C -0.0658(2) 0.63564(18) 0.04328(15) 0.0165(5) Uani 1 1 d . . . H31A H -0.0191 0.6758 0.0262 0.020 Uiso 1 1 calc R . . C32 C -0.1039(2) 0.56487(19) 0.00022(15) 0.0186(5) Uani 1 1 d . . . H32A H -0.0846 0.5575 -0.0465 0.022 Uiso 1 1 calc R . . C33 C -0.1702(2) 0.50489(19) 0.02552(16) 0.0203(6) Uani 1 1 d . . . H33A H -0.1944 0.4552 -0.0031 0.024 Uiso 1 1 calc R . . C34 C -0.2011(2) 0.51784(19) 0.09260(16) 0.0199(6) Uani 1 1 d . . . H34A H -0.2478 0.4775 0.1094 0.024 Uiso 1 1 calc R . . C35 C -0.1646(2) 0.58892(18) 0.13562(15) 0.0173(5) Uani 1 1 d . . . H35A H -0.1866 0.5972 0.1815 0.021 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 0.01354(5) 0.01212(5) 0.01089(4) -0.00084(3) 0.00150(3) -0.00166(3) Os3 0.01392(5) 0.01902(5) 0.01227(5) -0.00146(4) 0.00364(4) -0.00360(4) Os2 0.01183(5) 0.01466(5) 0.01144(4) 0.00001(3) 0.00233(3) -0.00075(3) Re1 0.01366(5) 0.01862(5) 0.01829(5) -0.00243(4) 0.00242(4) 0.00101(4) S1 0.0149(3) 0.0164(3) 0.0152(3) -0.0019(2) 0.0021(2) -0.0024(2) P1 0.0137(3) 0.0120(3) 0.0111(3) 0.0000(2) 0.0021(2) -0.0002(2) O1 0.0282(11) 0.0184(10) 0.0206(10) -0.0048(8) -0.0002(9) 0.0011(8) O2 0.0418(14) 0.0178(10) 0.0324(13) -0.0062(9) -0.0082(11) 0.0039(10) O3 0.0348(13) 0.0289(12) 0.0179(10) 0.0016(9) 0.0053(9) -0.0060(10) O4 0.0322(12) 0.0192(10) 0.0259(11) 0.0000(8) 0.0053(9) -0.0050(9) O5 0.0209(11) 0.0260(11) 0.0237(11) -0.0062(8) 0.0072(9) 0.0019(9) O6 0.0244(11) 0.0369(12) 0.0157(10) 0.0030(9) 0.0010(8) 0.0034(10) O7 0.0409(15) 0.0322(13) 0.0290(12) 0.0150(10) 0.0028(11) -0.0106(11) O8 0.0354(14) 0.0409(14) 0.0309(13) -0.0179(11) 0.0137(11) -0.0074(11) O9 0.0183(11) 0.0515(16) 0.0379(14) 0.0028(12) 0.0077(10) -0.0077(11) O10 0.0297(13) 0.0398(14) 0.0399(14) 0.0161(12) 0.0073(11) 0.0077(11) O11 0.0287(13) 0.0486(16) 0.0530(17) -0.0044(13) 0.0227(12) 0.0068(12) O12 0.0321(13) 0.0283(12) 0.0391(14) -0.0130(10) 0.0013(11) 0.0008(10) N1 0.0151(11) 0.0214(11) 0.0154(11) -0.0011(9) 0.0032(9) -0.0028(9) C1 0.0127(12) 0.0222(13) 0.0132(12) -0.0005(10) 0.0017(9) -0.0004(10) C2 0.0203(14) 0.0193(13) 0.0183(13) 0.0021(10) -0.0038(11) -0.0009(11) C3 0.0192(13) 0.0164(12) 0.0182(13) 0.0001(10) 0.0028(10) -0.0034(10) C4 0.0171(13) 0.0205(13) 0.0145(12) 0.0023(10) 0.0041(10) 0.0023(10) C5 0.0165(13) 0.0206(13) 0.0144(12) 0.0003(10) 0.0003(10) -0.0027(10) C6 0.0144(12) 0.0215(13) 0.0183(13) -0.0008(10) 0.0032(10) -0.0029(10) C7 0.0241(15) 0.0307(16) 0.0172(13) -0.0020(12) 0.0050(11) -0.0099(12) C8 0.0202(14) 0.0306(16) 0.0228(14) -0.0020(12) 0.0048(12) -0.0049(12) C9 0.0241(15) 0.0327(16) 0.0177(14) -0.0009(12) 0.0072(12) -0.0025(12) C10 0.0143(13) 0.0293(15) 0.0281(15) -0.0010(12) 0.0069(11) -0.0004(11) C11 0.0245(16) 0.0268(15) 0.0294(16) -0.0032(13) 0.0070(13) -0.0003(12) C12 0.0208(14) 0.0206(14) 0.0287(16) -0.0015(12) 0.0046(12) 0.0043(11) C13 0.0144(13) 0.0224(13) 0.0173(13) -0.0011(10) 0.0042(10) -0.0032(10) C14 0.0204(14) 0.0239(14) 0.0198(13) -0.0048(11) 0.0036(11) -0.0035(11) C15 0.0241(15) 0.0304(16) 0.0223(14) -0.0077(12) 0.0019(12) -0.0063(12) C16 0.0180(14) 0.0371(17) 0.0210(14) -0.0022(13) -0.0009(11) -0.0031(12) C17 0.0150(13) 0.0295(15) 0.0219(14) -0.0002(12) 0.0017(11) -0.0027(11) C18 0.0145(12) 0.0164(12) 0.0125(11) -0.0005(9) 0.0006(9) -0.0012(9) C19 0.0200(13) 0.0189(13) 0.0157(12) -0.0014(10) 0.0043(10) 0.0028(10) C20 0.0229(15) 0.0288(15) 0.0183(13) -0.0047(11) 0.0056(11) 0.0021(12) C21 0.0231(15) 0.0352(17) 0.0157(13) 0.0002(12) 0.0044(11) -0.0048(13) C22 0.0226(14) 0.0258(14) 0.0131(12) 0.0037(10) 0.0012(11) -0.0052(11) C23 0.0166(13) 0.0170(12) 0.0136(12) 0.0003(9) -0.0001(10) -0.0006(10) C24 0.0187(13) 0.0154(12) 0.0135(12) 0.0012(9) 0.0021(10) 0.0034(10) C25 0.0233(14) 0.0173(13) 0.0181(13) 0.0023(10) 0.0028(11) -0.0003(11) C26 0.0388(19) 0.0194(14) 0.0208(14) 0.0062(11) 0.0049(13) 0.0043(13) C27 0.0352(18) 0.0250(15) 0.0185(14) 0.0034(11) 0.0003(12) 0.0132(13) C28 0.0225(15) 0.0291(15) 0.0216(14) 0.0003(12) 0.0003(12) 0.0088(12) C29 0.0196(14) 0.0200(13) 0.0185(13) 0.0015(10) 0.0016(11) 0.0021(11) C30 0.0132(12) 0.0132(11) 0.0146(12) 0.0002(9) -0.0007(9) 0.0003(9) C31 0.0152(12) 0.0182(12) 0.0156(12) -0.0007(10) 0.0009(10) -0.0032(10) C32 0.0191(13) 0.0213(13) 0.0152(12) -0.0026(10) 0.0015(10) 0.0005(10) C33 0.0201(14) 0.0198(13) 0.0195(13) -0.0056(10) -0.0026(11) -0.0019(11) C34 0.0194(14) 0.0186(13) 0.0213(14) 0.0015(10) 0.0007(11) -0.0049(10) C35 0.0191(13) 0.0183(12) 0.0142(12) 0.0018(10) 0.0015(10) -0.0003(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Os1 C3 1.887(3) . ? Os1 C1 1.937(3) . ? Os1 C2 1.945(3) . ? Os1 P1 2.3487(7) . ? Os1 Os3 2.8633(3) . ? Os1 Os2 2.8830(3) . ? Os3 C8 1.899(3) . ? Os3 C9 1.916(3) . ? Os3 C7 1.924(3) . ? Os3 S1 2.3956(7) . ? Os3 Os2 2.7982(2) . ? Os3 Re1 2.8955(2) . ? Os2 C4 1.897(3) . ? Os2 C6 1.913(3) . ? Os2 C5 1.932(3) . ? Os2 S1 2.4060(7) . ? Os2 Re1 2.9087(3) . ? Re1 C10 1.899(3) . ? Re1 C11 1.905(3) . ? Re1 C12 1.918(3) . ? Re1 N1 2.233(2) . ? S1 C13 1.776(3) . ? P1 C18 1.821(3) . ? P1 C24 1.829(3) . ? P1 C30 1.830(3) . ? O1 C1 1.141(3) . ? O2 C2 1.135(4) . ? O3 C3 1.143(3) . ? O4 C4 1.149(3) . ? O5 C5 1.136(3) . ? O6 C6 1.150(3) . ? O7 C7 1.135(4) . ? O8 C8 1.148(4) . ? O9 C9 1.142(4) . ? O10 C10 1.151(4) . ? O11 C11 1.151(4) . ? O12 C12 1.146(4) . ? N1 C17 1.351(4) . ? N1 C13 1.357(4) . ? C13 C14 1.390(4) . ? C14 C15 1.384(4) . ? C15 C16 1.387(5) . ? C16 C17 1.378(4) . ? C18 C19 1.396(4) . ? C18 C23 1.399(4) . ? C19 C20 1.387(4) . ? C20 C21 1.384(4) . ? C21 C22 1.384(4) . ? C22 C23 1.387(4) . ? C24 C25 1.387(4) . ? C24 C29 1.404(4) . ? C25 C26 1.397(4) . ? C26 C27 1.378(5) . ? C27 C28 1.384(5) . ? C28 C29 1.380(4) . ? C30 C35 1.396(4) . ? C30 C31 1.399(4) . ? C31 C32 1.388(4) . ? C32 C33 1.387(4) . ? C33 C34 1.385(4) . ? C34 C35 1.386(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 C3 Os1 C1 93.03(12) . . ? C3 Os1 C2 97.20(12) . . ? C1 Os1 C2 169.51(11) . . ? C3 Os1 P1 92.79(9) . . ? C1 Os1 P1 90.42(8) . . ? C2 Os1 P1 91.35(9) . . ? C3 Os1 Os3 95.19(9) . . ? C1 Os1 Os3 85.28(8) . . ? C2 Os1 Os3 91.50(9) . . ? P1 Os1 Os3 171.120(17) . . ? C3 Os1 Os2 153.35(9) . . ? C1 Os1 Os2 83.05(8) . . ? C2 Os1 Os2 86.77(8) . . ? P1 Os1 Os2 113.516(17) . . ? Os3 Os1 Os2 58.281(4) . . ? C8 Os3 C9 91.60(13) . . ? C8 Os3 C7 96.68(13) . . ? C9 Os3 C7 95.91(13) . . ? C8 Os3 S1 169.67(9) . . ? C9 Os3 S1 94.50(9) . . ? C7 Os3 S1 90.98(9) . . ? C8 Os3 Os2 115.15(9) . . ? C9 Os3 Os2 123.22(9) . . ? C7 Os3 Os2 126.39(9) . . ? S1 Os3 Os2 54.528(17) . . ? C8 Os3 Os1 88.22(9) . . ? C9 Os3 Os1 174.93(10) . . ? C7 Os3 Os1 79.09(9) . . ? S1 Os3 Os1 86.437(17) . . ? Os2 Os3 Os1 61.211(6) . . ? C8 Os3 Re1 92.43(10) . . ? C9 Os3 Re1 68.78(10) . . ? C7 Os3 Re1 162.44(9) . . ? S1 Os3 Re1 82.054(18) . . ? Os2 Os3 Re1 61.416(7) . . ? Os1 Os3 Re1 116.289(5) . . ? C4 Os2 C6 91.66(12) . . ? C4 Os2 C5 97.84(12) . . ? C6 Os2 C5 92.32(12) . . ? C4 Os2 S1 168.28(8) . . ? C6 Os2 S1 94.33(9) . . ? C5 Os2 S1 91.97(8) . . ? C4 Os2 Os3 114.15(8) . . ? C6 Os2 Os3 121.64(8) . . ? C5 Os2 Os3 130.58(8) . . ? S1 Os2 Os3 54.182(16) . . ? C4 Os2 Os1 88.68(8) . . ? C6 Os2 Os1 177.31(9) . . ? C5 Os2 Os1 84.99(8) . . ? S1 Os2 Os1 85.802(17) . . ? Os3 Os2 Os1 60.508(8) . . ? C4 Os2 Re1 91.45(8) . . ? C6 Os2 Re1 67.41(8) . . ? C5 Os2 Re1 158.00(8) . . ? S1 Os2 Re1 81.599(18) . . ? Os3 Os2 Re1 60.940(5) . . ? Os1 Os2 Re1 115.248(6) . . ? C10 Re1 C11 86.25(13) . . ? C10 Re1 C12 87.75(14) . . ? C11 Re1 C12 88.35(13) . . ? C10 Re1 N1 95.29(11) . . ? C11 Re1 N1 96.13(12) . . ? C12 Re1 N1 174.73(11) . . ? C10 Re1 Os3 165.79(9) . . ? C11 Re1 Os3 107.75(10) . . ? C12 Re1 Os3 90.18(9) . . ? N1 Re1 Os3 85.83(6) . . ? C10 Re1 Os2 108.30(9) . . ? C11 Re1 Os2 165.35(10) . . ? C12 Re1 Os2 90.46(9) . . ? N1 Re1 Os2 84.50(6) . . ? Os3 Re1 Os2 57.644(5) . . ? C13 S1 Os3 107.31(10) . . ? C13 S1 Os2 106.03(10) . . ? Os3 S1 Os2 71.290(19) . . ? C18 P1 C24 104.01(12) . . ? C18 P1 C30 105.41(12) . . ? C24 P1 C30 99.53(12) . . ? C18 P1 Os1 115.15(9) . . ? C24 P1 Os1 117.19(9) . . ? C30 P1 Os1 113.71(9) . . ? C17 N1 C13 117.2(3) . . ? C17 N1 Re1 119.6(2) . . ? C13 N1 Re1 123.17(19) . . ? O1 C1 Os1 177.8(3) . . ? O2 C2 Os1 177.5(3) . . ? O3 C3 Os1 176.6(3) . . ? O4 C4 Os2 178.1(3) . . ? O5 C5 Os2 172.3(2) . . ? O6 C6 Os2 169.0(3) . . ? O7 C7 Os3 175.0(3) . . ? O8 C8 Os3 176.9(3) . . ? O9 C9 Os3 170.3(3) . . ? O10 C10 Re1 177.5(3) . . ? O11 C11 Re1 177.5(3) . . ? O12 C12 Re1 178.7(3) . . ? N1 C13 C14 122.4(3) . . ? N1 C13 S1 120.4(2) . . ? C14 C13 S1 117.2(2) . . ? C15 C14 C13 119.2(3) . . ? C14 C15 C16 118.8(3) . . ? C17 C16 C15 119.0(3) . . ? N1 C17 C16 123.4(3) . . ? C19 C18 C23 119.4(2) . . ? C19 C18 P1 121.9(2) . . ? C23 C18 P1 118.6(2) . . ? C20 C19 C18 119.9(3) . . ? C21 C20 C19 120.6(3) . . ? C20 C21 C22 119.8(3) . . ? C21 C22 C23 120.3(3) . . ? C22 C23 C18 120.0(3) . . ? C25 C24 C29 118.8(3) . . ? C25 C24 P1 123.6(2) . . ? C29 C24 P1 117.6(2) . . ? C24 C25 C26 120.4(3) . . ? C27 C26 C25 120.0(3) . . ? C26 C27 C28 120.2(3) . . ? C29 C28 C27 120.2(3) . . ? C28 C29 C24 120.5(3) . . ? C35 C30 C31 119.0(2) . . ? C35 C30 P1 123.1(2) . . ? C31 C30 P1 117.9(2) . . ? C32 C31 C30 120.5(3) . . ? C33 C32 C31 120.0(3) . . ? C34 C33 C32 119.7(3) . . ? C33 C34 C35 120.8(3) . . ? C34 C35 C30 120.0(3) . . ? _diffrn_measured_fraction_theta_max 0.951 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.619 _refine_diff_density_min -0.821 _refine_diff_density_rms 0.149 # Attachment '- Compound 3.CIF' data_str0730 _database_code_depnum_ccdc_archive 'CCDC 748787' #TrackingRef '- Compound 3.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H4 N O13 Os3 Re S' _chemical_formula_weight 1231.08 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -1.0185 7.2310 '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' _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 8.4394(15) _cell_length_b 10.1739(18) _cell_length_c 15.109(3) _cell_angle_alpha 70.584(2) _cell_angle_beta 84.140(3) _cell_angle_gamma 88.119(3) _cell_volume 1217.1(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(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 0.32 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.359 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1084 _exptl_absorpt_coefficient_mu 20.718 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.0578 _exptl_absorpt_correction_T_max 0.1181 _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 SMART APEX diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13410 _diffrn_reflns_av_R_equivalents 0.0520 _diffrn_reflns_av_sigmaI/netI 0.0587 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.44 _diffrn_reflns_theta_max 28.25 _reflns_number_total 5623 _reflns_number_gt 5184 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0661P)^2^+22.9220P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5623 _refine_ls_number_parameters 274 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0507 _refine_ls_R_factor_gt 0.0467 _refine_ls_wR_factor_ref 0.1330 _refine_ls_wR_factor_gt 0.1293 _refine_ls_goodness_of_fit_ref 1.134 _refine_ls_restrained_S_all 1.134 _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 0.28840(5) 0.77324(4) 0.11647(3) 0.01262(13) Uani 1 1 d . . . Os2 Os 0.18090(5) 0.49205(4) 0.17114(3) 0.00982(12) Uani 1 1 d . . . Os3 Os 0.35961(5) 0.57057(4) 0.29029(3) 0.00875(12) Uani 1 1 d . . . Re3 Re 0.14744(5) 0.32643(4) 0.36835(3) 0.01028(12) Uani 1 1 d . . . S1 S 0.4583(3) 0.4410(3) 0.18942(19) 0.0101(5) Uani 1 1 d . . . N1 N 0.3579(11) 0.2064(10) 0.3326(7) 0.0118(18) Uiso 1 1 d . . . O1 O 0.5980(13) 0.6982(11) 0.0145(8) 0.038(3) Uani 1 1 d . . . O2 O 0.1484(15) 0.9174(14) -0.0694(7) 0.042(3) Uani 1 1 d . . . O3 O 0.4459(14) 1.0269(12) 0.1321(8) 0.037(3) Uiso 1 1 d . . . O4 O -0.0183(13) 0.8301(11) 0.2285(7) 0.030(2) Uani 1 1 d . . . O5 O 0.1686(11) 0.7352(10) 0.4027(7) 0.0226(19) Uani 1 1 d . . . O6 O 0.6436(11) 0.7644(10) 0.2638(8) 0.027(2) Uani 1 1 d . . . O7 O 0.4976(12) 0.3718(9) 0.4654(7) 0.024(2) Uani 1 1 d . . . O8 O -0.1664(11) 0.5753(12) 0.1886(8) 0.030(2) Uani 1 1 d . . . O9 O 0.1810(12) 0.5694(11) -0.0426(7) 0.027(2) Uani 1 1 d . . . O10 O 0.0837(16) 0.1974(11) 0.1881(8) 0.039(3) Uani 1 1 d . . . O11 O -0.1311(11) 0.5049(9) 0.4104(7) 0.027(2) Uani 1 1 d . . . O12 O -0.0979(13) 0.0943(12) 0.4087(8) 0.034(2) Uiso 1 1 d . . . O13 O 0.1864(12) 0.2074(9) 0.5791(7) 0.024(2) Uani 1 1 d . . . C1 C 0.4809(19) 0.7220(14) 0.0522(10) 0.028(3) Uani 1 1 d . . . C2 C 0.2019(18) 0.8611(13) -0.0015(9) 0.025(3) Uani 1 1 d . . . C3 C 0.3870(19) 0.9294(14) 0.1251(11) 0.031(3) Uani 1 1 d . . . C4 C 0.0939(14) 0.8074(12) 0.1894(8) 0.014(2) Uiso 1 1 d . . . C5 C 0.2386(14) 0.6724(13) 0.3604(8) 0.016(2) Uani 1 1 d . . . C6 C 0.5410(15) 0.6911(13) 0.2722(9) 0.017(2) Uani 1 1 d . . . C7 C 0.4343(14) 0.4396(12) 0.4005(9) 0.016(2) Uani 1 1 d . . . C8 C -0.0348(15) 0.5472(12) 0.1821(9) 0.017(2) Uani 1 1 d . . . C9 C 0.1880(14) 0.5418(13) 0.0368(9) 0.016(2) Uiso 1 1 d . . . C10 C 0.1166(17) 0.3012(14) 0.1920(9) 0.024(3) Uani 1 1 d . . . C11 C -0.0258(14) 0.4423(13) 0.3940(8) 0.016(2) Uiso 1 1 d . . . C12 C -0.0009(13) 0.1782(12) 0.3945(8) 0.012(2) Uiso 1 1 d . . . C13 C 0.1719(13) 0.2525(13) 0.5001(9) 0.016(2) Uani 1 1 d . . . C14 C 0.4740(13) 0.2653(12) 0.2632(8) 0.013(2) Uiso 1 1 d . . . C15 C 0.6108(14) 0.1930(12) 0.2475(8) 0.015(2) Uiso 1 1 d . . . H15A H 0.6925 0.2383 0.2000 0.018 Uiso 1 1 calc R . . C16 C 0.6269(15) 0.0559(13) 0.3012(9) 0.018(2) Uiso 1 1 d . . . H16A H 0.7193 0.0047 0.2914 0.021 Uiso 1 1 calc R . . C17 C 0.5009(15) -0.0088(14) 0.3726(9) 0.019(2) Uiso 1 1 d . . . H17A H 0.5071 -0.1041 0.4101 0.023 Uiso 1 1 calc R . . C18 C 0.3719(16) 0.0703(14) 0.3852(9) 0.021(2) Uiso 1 1 d . . . H18A H 0.2889 0.0283 0.4328 0.025 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 0.0173(2) 0.0042(2) 0.0125(2) 0.00208(16) 0.00055(16) -0.00317(16) Os2 0.0129(2) 0.0054(2) 0.0105(2) -0.00166(16) -0.00048(15) -0.00260(15) Os3 0.0121(2) 0.00212(19) 0.0109(2) -0.00062(15) 0.00000(15) -0.00317(15) Re3 0.0136(2) 0.0030(2) 0.0120(2) -0.00032(16) 0.00249(16) -0.00342(15) S1 0.0153(12) 0.0028(10) 0.0096(12) 0.0005(9) 0.0032(9) -0.0026(9) O1 0.037(6) 0.019(5) 0.031(6) 0.021(4) 0.014(5) 0.005(4) O2 0.048(7) 0.055(8) 0.016(5) 0.001(5) -0.018(5) -0.001(6) O4 0.035(6) 0.034(6) 0.018(5) -0.007(4) 0.005(4) 0.009(4) O5 0.019(4) 0.028(5) 0.025(5) -0.016(4) 0.005(4) 0.001(4) O6 0.023(5) 0.016(4) 0.045(6) -0.013(4) -0.006(4) -0.008(4) O7 0.030(5) 0.011(4) 0.026(5) 0.003(4) -0.014(4) -0.005(4) O8 0.014(4) 0.044(6) 0.041(6) -0.027(5) -0.003(4) 0.003(4) O9 0.035(5) 0.025(5) 0.022(5) -0.008(4) -0.002(4) -0.009(4) O10 0.069(8) 0.017(5) 0.036(6) -0.014(5) -0.002(6) -0.020(5) O11 0.026(5) 0.013(4) 0.037(6) -0.007(4) 0.009(4) 0.007(4) O13 0.039(6) 0.009(4) 0.020(5) -0.001(4) 0.002(4) -0.002(4) C1 0.040(8) 0.016(6) 0.019(7) 0.004(5) 0.004(6) -0.002(6) C2 0.040(8) 0.014(6) 0.013(6) 0.005(5) 0.000(5) -0.014(5) C3 0.043(9) 0.011(6) 0.029(8) 0.009(5) -0.013(6) -0.016(6) C5 0.015(5) 0.020(6) 0.009(5) 0.000(4) -0.002(4) 0.004(5) C6 0.019(6) 0.014(5) 0.019(6) -0.008(5) 0.005(5) -0.002(5) C7 0.017(6) 0.007(5) 0.024(6) -0.006(5) -0.008(5) 0.005(4) C8 0.019(6) 0.010(5) 0.027(6) -0.011(5) -0.006(5) 0.002(4) C10 0.029(7) 0.023(7) 0.021(7) -0.006(5) -0.016(5) 0.009(5) C13 0.005(5) 0.016(5) 0.024(6) -0.004(5) 0.000(4) 0.001(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 Os1 C3 1.866(13) . ? Os1 C2 1.917(13) . ? Os1 C1 1.953(15) . ? Os1 C4 1.969(12) . ? Os1 Os2 2.8524(7) . ? Os1 Os3 2.8549(7) . ? Os2 C8 1.894(12) . ? Os2 C9 1.917(12) . ? Os2 C10 1.947(14) . ? Os2 S1 2.405(3) . ? Os2 Os3 2.7827(7) . ? Os2 Re3 2.8842(7) . ? Os3 C7 1.905(12) . ? Os3 C5 1.918(12) . ? Os3 C6 1.933(12) . ? Os3 S1 2.400(3) . ? Os3 Re3 2.9461(7) . ? Re3 C12 1.904(11) . ? Re3 C13 1.911(13) . ? Re3 C11 1.937(12) . ? Re3 N1 2.244(9) . ? S1 C14 1.774(12) . ? N1 C14 1.353(14) . ? N1 C18 1.356(16) . ? O1 C1 1.150(18) . ? O2 C2 1.127(17) . ? O3 C3 1.163(17) . ? O4 C4 1.123(15) . ? O5 C5 1.155(15) . ? O6 C6 1.131(15) . ? O7 C7 1.165(15) . ? O8 C8 1.141(15) . ? O9 C9 1.145(15) . ? O10 C10 1.122(17) . ? O11 C11 1.132(15) . ? O12 C12 1.155(16) . ? O13 C13 1.145(16) . ? C14 C15 1.391(16) . ? C15 C16 1.371(17) . ? C16 C17 1.438(17) . ? C17 C18 1.368(18) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3 Os1 C2 98.0(6) . . ? C3 Os1 C1 92.0(7) . . ? C2 Os1 C1 91.0(6) . . ? C3 Os1 C4 91.2(6) . . ? C2 Os1 C4 92.6(6) . . ? C1 Os1 C4 174.8(5) . . ? C3 Os1 Os2 158.4(4) . . ? C2 Os1 Os2 103.6(4) . . ? C1 Os1 Os2 89.1(4) . . ? C4 Os1 Os2 86.4(3) . . ? C3 Os1 Os3 100.0(4) . . ? C2 Os1 Os3 161.9(4) . . ? C1 Os1 Os3 90.3(4) . . ? C4 Os1 Os3 85.1(3) . . ? Os2 Os1 Os3 58.363(15) . . ? C8 Os2 C9 92.6(5) . . ? C8 Os2 C10 90.9(5) . . ? C9 Os2 C10 92.9(5) . . ? C8 Os2 S1 166.0(4) . . ? C9 Os2 S1 99.1(4) . . ? C10 Os2 S1 96.0(4) . . ? C8 Os2 Os3 111.7(3) . . ? C9 Os2 Os3 133.5(4) . . ? C10 Os2 Os3 124.2(4) . . ? S1 Os2 Os3 54.52(6) . . ? C8 Os2 Os1 91.7(4) . . ? C9 Os2 Os1 80.1(4) . . ? C10 Os2 Os1 172.6(4) . . ? S1 Os2 Os1 82.90(6) . . ? Os3 Os2 Os1 60.865(16) . . ? C8 Os2 Re3 89.3(4) . . ? C9 Os2 Re3 160.5(4) . . ? C10 Os2 Re3 67.6(4) . . ? S1 Os2 Re3 82.15(6) . . ? Os3 Os2 Re3 62.619(18) . . ? Os1 Os2 Re3 119.238(19) . . ? C7 Os3 C5 93.0(5) . . ? C7 Os3 C6 91.9(5) . . ? C5 Os3 C6 90.6(5) . . ? C7 Os3 S1 94.2(4) . . ? C5 Os3 S1 167.8(4) . . ? C6 Os3 S1 98.9(3) . . ? C7 Os3 Os2 122.5(3) . . ? C5 Os3 Os2 113.1(4) . . ? C6 Os3 Os2 134.9(4) . . ? S1 Os3 Os2 54.70(7) . . ? C7 Os3 Os1 172.9(4) . . ? C5 Os3 Os1 91.0(3) . . ? C6 Os3 Os1 82.1(4) . . ? S1 Os3 Os1 82.93(7) . . ? Os2 Os3 Os1 60.773(18) . . ? C7 Os3 Re3 68.6(4) . . ? C5 Os3 Re3 92.6(4) . . ? C6 Os3 Re3 160.4(4) . . ? S1 Os3 Re3 80.93(6) . . ? Os2 Os3 Re3 60.376(17) . . ? Os1 Os3 Re3 117.09(2) . . ? C12 Re3 C13 84.6(5) . . ? C12 Re3 C11 88.7(5) . . ? C13 Re3 C11 89.7(5) . . ? C12 Re3 N1 95.1(4) . . ? C13 Re3 N1 92.2(4) . . ? C11 Re3 N1 175.9(4) . . ? C12 Re3 Os2 111.9(3) . . ? C13 Re3 Os2 163.4(4) . . ? C11 Re3 Os2 91.5(4) . . ? N1 Re3 Os2 85.7(2) . . ? C12 Re3 Os3 168.9(3) . . ? C13 Re3 Os3 106.5(4) . . ? C11 Re3 Os3 90.9(4) . . ? N1 Re3 Os3 85.0(2) . . ? Os2 Re3 Os3 57.005(14) . . ? C14 S1 Os3 106.5(4) . . ? C14 S1 Os2 108.0(4) . . ? Os3 S1 Os2 70.78(7) . . ? C14 N1 C18 118.7(10) . . ? C14 N1 Re3 122.8(7) . . ? C18 N1 Re3 118.4(8) . . ? O1 C1 Os1 176.3(13) . . ? O2 C2 Os1 176.9(14) . . ? O3 C3 Os1 178.5(16) . . ? O4 C4 Os1 177.9(11) . . ? O5 C5 Os3 178.6(11) . . ? O6 C6 Os3 177.1(11) . . ? O7 C7 Os3 170.6(11) . . ? O8 C8 Os2 177.2(11) . . ? O9 C9 Os2 175.2(11) . . ? O10 C10 Os2 168.5(12) . . ? O11 C11 Re3 177.0(11) . . ? O12 C12 Re3 175.9(10) . . ? O13 C13 Re3 179.6(11) . . ? N1 C14 C15 122.1(11) . . ? N1 C14 S1 120.6(8) . . ? C15 C14 S1 117.2(9) . . ? C16 C15 C14 119.5(11) . . ? C15 C16 C17 118.6(11) . . ? C18 C17 C16 118.4(12) . . ? N1 C18 C17 122.6(12) . . ? 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 C3 Os1 Os2 C8 111.6(15) . . . . ? C2 Os1 Os2 C8 -64.3(6) . . . . ? C1 Os1 Os2 C8 -155.1(6) . . . . ? C4 Os1 Os2 C8 27.5(5) . . . . ? Os3 Os1 Os2 C8 114.0(4) . . . . ? C3 Os1 Os2 C9 -156.1(15) . . . . ? C2 Os1 Os2 C9 28.0(6) . . . . ? C1 Os1 Os2 C9 -62.8(6) . . . . ? C4 Os1 Os2 C9 119.8(5) . . . . ? Os3 Os1 Os2 C9 -153.7(4) . . . . ? C3 Os1 Os2 C10 -137(3) . . . . ? C2 Os1 Os2 C10 47(3) . . . . ? C1 Os1 Os2 C10 -44(3) . . . . ? C4 Os1 Os2 C10 139(3) . . . . ? Os3 Os1 Os2 C10 -135(3) . . . . ? C3 Os1 Os2 S1 -55.5(15) . . . . ? C2 Os1 Os2 S1 128.6(5) . . . . ? C1 Os1 Os2 S1 37.8(4) . . . . ? C4 Os1 Os2 S1 -139.5(3) . . . . ? Os3 Os1 Os2 S1 -53.12(6) . . . . ? C3 Os1 Os2 Os3 -2.4(15) . . . . ? C2 Os1 Os2 Os3 -178.3(5) . . . . ? C1 Os1 Os2 Os3 90.9(4) . . . . ? C4 Os1 Os2 Os3 -86.4(3) . . . . ? C3 Os1 Os2 Re3 21.4(15) . . . . ? C2 Os1 Os2 Re3 -154.5(5) . . . . ? C1 Os1 Os2 Re3 114.7(4) . . . . ? C4 Os1 Os2 Re3 -62.7(3) . . . . ? Os3 Os1 Os2 Re3 23.74(2) . . . . ? C8 Os2 Os3 C7 108.0(6) . . . . ? C9 Os2 Os3 C7 -135.7(7) . . . . ? C10 Os2 Os3 C7 1.0(7) . . . . ? S1 Os2 Os3 C7 -69.7(4) . . . . ? Os1 Os2 Os3 C7 -172.7(4) . . . . ? Re3 Os2 Os3 C7 30.6(4) . . . . ? C8 Os2 Os3 C5 -2.0(6) . . . . ? C9 Os2 Os3 C5 114.3(6) . . . . ? C10 Os2 Os3 C5 -108.9(6) . . . . ? S1 Os2 Os3 C5 -179.7(4) . . . . ? Os1 Os2 Os3 C5 77.4(4) . . . . ? Re3 Os2 Os3 C5 -79.3(4) . . . . ? C8 Os2 Os3 C6 -118.2(7) . . . . ? C9 Os2 Os3 C6 -1.9(7) . . . . ? C10 Os2 Os3 C6 134.8(7) . . . . ? S1 Os2 Os3 C6 64.1(5) . . . . ? Os1 Os2 Os3 C6 -38.8(5) . . . . ? Re3 Os2 Os3 C6 164.5(5) . . . . ? C8 Os2 Os3 S1 177.7(4) . . . . ? C9 Os2 Os3 S1 -66.0(5) . . . . ? C10 Os2 Os3 S1 70.8(5) . . . . ? Os1 Os2 Os3 S1 -102.91(8) . . . . ? Re3 Os2 Os3 S1 100.39(8) . . . . ? C8 Os2 Os3 Os1 -79.4(4) . . . . ? C9 Os2 Os3 Os1 36.9(5) . . . . ? C10 Os2 Os3 Os1 173.7(5) . . . . ? S1 Os2 Os3 Os1 102.91(8) . . . . ? Re3 Os2 Os3 Os1 -156.70(2) . . . . ? C8 Os2 Os3 Re3 77.3(4) . . . . ? C9 Os2 Os3 Re3 -166.4(5) . . . . ? C10 Os2 Os3 Re3 -29.6(5) . . . . ? S1 Os2 Os3 Re3 -100.39(8) . . . . ? Os1 Os2 Os3 Re3 156.70(2) . . . . ? C3 Os1 Os3 C7 -61(3) . . . . ? C2 Os1 Os3 C7 125(3) . . . . ? C1 Os1 Os3 C7 31(3) . . . . ? C4 Os1 Os3 C7 -152(3) . . . . ? Os2 Os1 Os3 C7 120(3) . . . . ? C3 Os1 Os3 C5 63.0(7) . . . . ? C2 Os1 Os3 C5 -110.7(15) . . . . ? C1 Os1 Os3 C5 155.1(6) . . . . ? C4 Os1 Os3 C5 -27.4(5) . . . . ? Os2 Os1 Os3 C5 -116.2(4) . . . . ? C3 Os1 Os3 C6 -27.5(7) . . . . ? C2 Os1 Os3 C6 158.8(15) . . . . ? C1 Os1 Os3 C6 64.6(6) . . . . ? C4 Os1 Os3 C6 -117.9(5) . . . . ? Os2 Os1 Os3 C6 153.3(3) . . . . ? C3 Os1 Os3 S1 -127.6(6) . . . . ? C2 Os1 Os3 S1 58.7(15) . . . . ? C1 Os1 Os3 S1 -35.5(5) . . . . ? C4 Os1 Os3 S1 142.1(3) . . . . ? Os2 Os1 Os3 S1 53.28(7) . . . . ? C3 Os1 Os3 Os2 179.1(6) . . . . ? C2 Os1 Os3 Os2 5.4(15) . . . . ? C1 Os1 Os3 Os2 -88.8(4) . . . . ? C4 Os1 Os3 Os2 88.8(3) . . . . ? C3 Os1 Os3 Re3 156.4(6) . . . . ? C2 Os1 Os3 Re3 -17.3(15) . . . . ? C1 Os1 Os3 Re3 -111.5(4) . . . . ? C4 Os1 Os3 Re3 66.1(3) . . . . ? Os2 Os1 Os3 Re3 -22.719(19) . . . . ? C8 Os2 Re3 C12 64.4(5) . . . . ? C9 Os2 Re3 C12 -31.4(11) . . . . ? C10 Os2 Re3 C12 -26.9(6) . . . . ? S1 Os2 Re3 C12 -126.7(4) . . . . ? Os3 Os2 Re3 C12 179.4(4) . . . . ? Os1 Os2 Re3 C12 156.0(4) . . . . ? C8 Os2 Re3 C13 -118.7(12) . . . . ? C9 Os2 Re3 C13 145.5(16) . . . . ? C10 Os2 Re3 C13 150.0(13) . . . . ? S1 Os2 Re3 C13 50.2(12) . . . . ? Os3 Os2 Re3 C13 -3.7(12) . . . . ? Os1 Os2 Re3 C13 -27.1(12) . . . . ? C8 Os2 Re3 C11 -24.8(5) . . . . ? C9 Os2 Re3 C11 -120.7(11) . . . . ? C10 Os2 Re3 C11 -116.1(6) . . . . ? S1 Os2 Re3 C11 144.1(4) . . . . ? Os3 Os2 Re3 C11 90.1(4) . . . . ? Os1 Os2 Re3 C11 66.8(4) . . . . ? C8 Os2 Re3 N1 158.2(4) . . . . ? C9 Os2 Re3 N1 62.4(11) . . . . ? C10 Os2 Re3 N1 66.9(5) . . . . ? S1 Os2 Re3 N1 -32.9(2) . . . . ? Os3 Os2 Re3 N1 -86.9(2) . . . . ? Os1 Os2 Re3 N1 -110.2(2) . . . . ? C8 Os2 Re3 Os3 -114.9(3) . . . . ? C9 Os2 Re3 Os3 149.2(11) . . . . ? C10 Os2 Re3 Os3 153.8(4) . . . . ? S1 Os2 Re3 Os3 53.95(6) . . . . ? Os1 Os2 Re3 Os3 -23.33(2) . . . . ? C7 Os3 Re3 C12 -155.6(18) . . . . ? C5 Os3 Re3 C12 112.1(17) . . . . ? C6 Os3 Re3 C12 -149(2) . . . . ? S1 Os3 Re3 C12 -57.5(17) . . . . ? Os2 Os3 Re3 C12 -3.1(17) . . . . ? Os1 Os3 Re3 C12 19.7(17) . . . . ? C7 Os3 Re3 C13 26.4(5) . . . . ? C5 Os3 Re3 C13 -65.9(5) . . . . ? C6 Os3 Re3 C13 33.4(11) . . . . ? S1 Os3 Re3 C13 124.5(4) . . . . ? Os2 Os3 Re3 C13 178.9(4) . . . . ? Os1 Os3 Re3 C13 -158.3(4) . . . . ? C7 Os3 Re3 C11 116.3(5) . . . . ? C5 Os3 Re3 C11 24.1(5) . . . . ? C6 Os3 Re3 C11 123.3(11) . . . . ? S1 Os3 Re3 C11 -145.6(4) . . . . ? Os2 Os3 Re3 C11 -91.2(3) . . . . ? Os1 Os3 Re3 C11 -68.4(3) . . . . ? C7 Os3 Re3 N1 -64.5(5) . . . . ? C5 Os3 Re3 N1 -156.7(4) . . . . ? C6 Os3 Re3 N1 -57.4(10) . . . . ? S1 Os3 Re3 N1 33.7(2) . . . . ? Os2 Os3 Re3 N1 88.1(2) . . . . ? Os1 Os3 Re3 N1 110.9(2) . . . . ? C7 Os3 Re3 Os2 -152.5(4) . . . . ? C5 Os3 Re3 Os2 115.2(3) . . . . ? C6 Os3 Re3 Os2 -145.5(10) . . . . ? S1 Os3 Re3 Os2 -54.38(7) . . . . ? Os1 Os3 Re3 Os2 22.813(19) . . . . ? C7 Os3 S1 C14 23.7(5) . . . . ? C5 Os3 S1 C14 -102.4(18) . . . . ? C6 Os3 S1 C14 116.4(6) . . . . ? Os2 Os3 S1 C14 -103.8(4) . . . . ? Os1 Os3 S1 C14 -162.8(4) . . . . ? Re3 Os3 S1 C14 -43.8(4) . . . . ? C7 Os3 S1 Os2 127.5(4) . . . . ? C5 Os3 S1 Os2 1.4(17) . . . . ? C6 Os3 S1 Os2 -139.8(4) . . . . ? Os1 Os3 S1 Os2 -59.00(4) . . . . ? Re3 Os3 S1 Os2 59.98(4) . . . . ? C8 Os2 S1 C14 92.8(16) . . . . ? C9 Os2 S1 C14 -120.5(5) . . . . ? C10 Os2 S1 C14 -26.6(6) . . . . ? Os3 Os2 S1 C14 101.7(4) . . . . ? Os1 Os2 S1 C14 160.7(4) . . . . ? Re3 Os2 S1 C14 39.8(4) . . . . ? C8 Os2 S1 Os3 -8.9(16) . . . . ? C9 Os2 S1 Os3 137.8(4) . . . . ? C10 Os2 S1 Os3 -128.2(4) . . . . ? Os1 Os2 S1 Os3 59.09(4) . . . . ? Re3 Os2 S1 Os3 -61.84(4) . . . . ? C12 Re3 N1 C14 142.7(9) . . . . ? C13 Re3 N1 C14 -132.5(9) . . . . ? C11 Re3 N1 C14 -16(6) . . . . ? Os2 Re3 N1 C14 31.0(8) . . . . ? Os3 Re3 N1 C14 -26.2(8) . . . . ? C12 Re3 N1 C18 -39.8(9) . . . . ? C13 Re3 N1 C18 45.0(9) . . . . ? C11 Re3 N1 C18 162(6) . . . . ? Os2 Re3 N1 C18 -151.4(9) . . . . ? Os3 Re3 N1 C18 151.3(9) . . . . ? C3 Os1 C1 O1 -3(20) . . . . ? C2 Os1 C1 O1 95(20) . . . . ? C4 Os1 C1 O1 -131(18) . . . . ? Os2 Os1 C1 O1 -162(20) . . . . ? Os3 Os1 C1 O1 -103(20) . . . . ? C3 Os1 C2 O2 -49(24) . . . . ? C1 Os1 C2 O2 -141(24) . . . . ? C4 Os1 C2 O2 43(24) . . . . ? Os2 Os1 C2 O2 130(24) . . . . ? Os3 Os1 C2 O2 125(23) . . . . ? C2 Os1 C3 O3 106(52) . . . . ? C1 Os1 C3 O3 -162(52) . . . . ? C4 Os1 C3 O3 14(52) . . . . ? Os2 Os1 C3 O3 -69(53) . . . . ? Os3 Os1 C3 O3 -72(52) . . . . ? C3 Os1 C4 O4 78(31) . . . . ? C2 Os1 C4 O4 -21(31) . . . . ? C1 Os1 C4 O4 -154(28) . . . . ? Os2 Os1 C4 O4 -124(31) . . . . ? Os3 Os1 C4 O4 178(100) . . . . ? C7 Os3 C5 O5 83(45) . . . . ? C6 Os3 C5 O5 -9(45) . . . . ? S1 Os3 C5 O5 -151(43) . . . . ? Os2 Os3 C5 O5 -150(44) . . . . ? Os1 Os3 C5 O5 -91(45) . . . . ? Re3 Os3 C5 O5 151(45) . . . . ? C7 Os3 C6 O6 -90(25) . . . . ? C5 Os3 C6 O6 3(25) . . . . ? S1 Os3 C6 O6 176(25) . . . . ? Os2 Os3 C6 O6 128(25) . . . . ? Os1 Os3 C6 O6 94(25) . . . . ? Re3 Os3 C6 O6 -96(25) . . . . ? C5 Os3 C7 O7 -92(7) . . . . ? C6 Os3 C7 O7 -1(7) . . . . ? S1 Os3 C7 O7 98(7) . . . . ? Os2 Os3 C7 O7 148(6) . . . . ? Os1 Os3 C7 O7 32(9) . . . . ? Re3 Os3 C7 O7 176(7) . . . . ? C9 Os2 C8 O8 82(25) . . . . ? C10 Os2 C8 O8 -11(25) . . . . ? S1 Os2 C8 O8 -131(24) . . . . ? Os3 Os2 C8 O8 -139(25) . . . . ? Os1 Os2 C8 O8 162(25) . . . . ? Re3 Os2 C8 O8 -79(25) . . . . ? C8 Os2 C9 O9 -30(13) . . . . ? C10 Os2 C9 O9 61(13) . . . . ? S1 Os2 C9 O9 158(13) . . . . ? Os3 Os2 C9 O9 -154(13) . . . . ? Os1 Os2 C9 O9 -121(13) . . . . ? Re3 Os2 C9 O9 65(14) . . . . ? C8 Os2 C10 O10 99(6) . . . . ? C9 Os2 C10 O10 6(6) . . . . ? S1 Os2 C10 O10 -93(6) . . . . ? Os3 Os2 C10 O10 -144(6) . . . . ? Os1 Os2 C10 O10 -12(9) . . . . ? Re3 Os2 C10 O10 -172(7) . . . . ? C12 Re3 C11 O11 9(21) . . . . ? C13 Re3 C11 O11 -76(21) . . . . ? N1 Re3 C11 O11 167(17) . . . . ? Os2 Re3 C11 O11 121(21) . . . . ? Os3 Re3 C11 O11 178(100) . . . . ? C13 Re3 C12 O12 117(15) . . . . ? C11 Re3 C12 O12 27(15) . . . . ? N1 Re3 C12 O12 -152(15) . . . . ? Os2 Re3 C12 O12 -64(15) . . . . ? Os3 Re3 C12 O12 -61(15) . . . . ? C12 Re3 C13 O13 36(100) . . . . ? C11 Re3 C13 O13 125(100) . . . . ? N1 Re3 C13 O13 -59(100) . . . . ? Os2 Re3 C13 O13 -141(100) . . . . ? Os3 Re3 C13 O13 -144(100) . . . . ? C18 N1 C14 C15 -3.5(16) . . . . ? Re3 N1 C14 C15 174.0(8) . . . . ? C18 N1 C14 S1 177.7(9) . . . . ? Re3 N1 C14 S1 -4.8(12) . . . . ? Os3 S1 C14 N1 42.3(10) . . . . ? Os2 S1 C14 N1 -32.4(10) . . . . ? Os3 S1 C14 C15 -136.6(8) . . . . ? Os2 S1 C14 C15 148.8(8) . . . . ? N1 C14 C15 C16 2.7(17) . . . . ? S1 C14 C15 C16 -178.5(9) . . . . ? C14 C15 C16 C17 -0.2(17) . . . . ? C15 C16 C17 C18 -1.4(18) . . . . ? C14 N1 C18 C17 1.8(18) . . . . ? Re3 N1 C18 C17 -175.8(9) . . . . ? C16 C17 C18 N1 0.6(19) . . . . ? _diffrn_measured_fraction_theta_max 0.933 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 2.977 _refine_diff_density_min -3.554 _refine_diff_density_rms 0.545