Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2003 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 loop_ _publ_author_name 'Tony Manning' 'C. John McAdam' 'Anthony J. Palmer' 'Brian H. Robinson' 'Jim Simpson' _publ_contact_author_name 'Prof Tony Manning' _publ_contact_author_address ; Department of Chemistry University College Dublin Belfield Dublin 4 REPUBLIC OF IRELAND ; _publ_contact_author_email ANTHONY.MANNING@UCD.IE _publ_section_title ; The reaction of [{Co(n5-C5H5)}2{Fe(CO)2(PPh3)}(m3-S)(m3-CS)] and related complexes with carbon disulphide. Synthesis, structure and reactivity of [{Co(n5-C5H5)}2{Fe(CO)(L)}(m3-S)(m3-C2S3)] derivatives (L = PR3 and CNR). ; data_fecomi _database_code_CSD 207316 _audit_creation_method SHELXL-97 _publ_section_references ; Hunter K.A. and Simpson, J. (1996) Titan: A molecular graphics program to aid structure solution and refinement with the SHELX suite of programs Siemens Analytical X-ray Instruments, Madison, Wisconsin, USA, (1995) SMART and SAINT: Area detector control and integration software, Sheldrick, G.M. (1996) SADABS A program for empirical absorption correction of area detector data. University of Gottingen, Federal Republic of Germany. Sheldrick, G.M. (1997) SHELXS-97 A program for the solution of crystal structures from diffraction data. University of Gottingen, Federal Republic of Germany. Sheldrick, G.M. (1997) SHELXL-97 A program for the refinement of crystal structures. University of Gottingen, Federal Republic of Germany. 1997. Sheldrick, G. M. (1990). SHELXTL-PC. Programs for crystal structure determination. Siemens Analytical X-ray Instruments Inc., Madison, Wisconsin, USA. ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C32 H28 O P S4 Co2 Fe I, C H Cl3, 0.5(C6 H6)' _chemical_formula_sum 'C36 H32 O P S4 Cl3 Co2 Fe I' _chemical_formula_weight 1046.79 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' 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 12.9130(7) _cell_length_b 20.9619(10) _cell_length_c 16.2086(8) _cell_angle_alpha 90.00 _cell_angle_beta 100.2930(10) _cell_angle_gamma 90.00 _cell_volume 4316.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 300(2) _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 1.60 _cell_measurement_theta_max 23.39 _exptl_crystal_description plate _exptl_crystal_colour 'dark brown' _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.611 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2076 _exptl_absorpt_coefficient_mu 2.250 _exptl_absorpt_correction_type 'Siemens SADABS' _exptl_absorpt_correction_T_min 0.720984 _exptl_absorpt_correction_T_max 1.000000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 300(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 'Siemens SMART CD' _diffrn_measurement_method 'Exposures over 0.3\% \f or \w rotation' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12780 _diffrn_reflns_av_R_equivalents 0.0314 _diffrn_reflns_av_sigmaI/netI 0.0365 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 23.39 _reflns_number_total 4746 _reflns_number_gt 4019 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens 1995)' _computing_cell_refinement 'SAINT (Siemens 1995)' _computing_data_reduction 'SAINT (Siemens 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'TITAN (Hunter & Simpson 1997), SHELXTL-PC (Sheldrick 1976)' _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 w=1/[\s^2^(Fo^2^)+(0.1014P)^2^+18.8032P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4746 _refine_ls_number_parameters 470 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.0672 _refine_ls_R_factor_gt 0.0586 _refine_ls_wR_factor_ref 0.1874 _refine_ls_wR_factor_gt 0.1812 _refine_ls_goodness_of_fit_ref 1.128 _refine_ls_restrained_S_all 1.127 _refine_ls_shift/su_max 0.013 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group I1 I 0.81345(8) 0.07614(4) 0.65204(6) 0.0906(4) Uani 1 d . . . Co1 Co 1.10664(12) 0.16282(6) 0.28043(7) 0.0489(4) Uani 1 d . . . Co2 Co 1.10017(11) 0.14938(5) 0.42853(6) 0.0387(4) Uani 1 d . . . Fe1 Fe 0.95624(11) 0.21504(5) 0.33259(6) 0.0367(4) Uani 1 d . . . S1 S 1.1229(2) 0.23831(10) 0.37141(14) 0.0483(7) Uani 1 d . . . C1 C 1.0021(8) 0.1291(4) 0.3333(5) 0.039(2) Uani 1 d . . . S2 S 0.9236(2) 0.06058(10) 0.31388(14) 0.0495(8) Uani 1 d . . . C2 C 0.8083(8) 0.0942(4) 0.3261(5) 0.046(3) Uani 1 d . . . S3 S 0.6940(3) 0.05041(13) 0.3228(2) 0.0752(10) Uani 1 d . . . C3 C 0.7311(10) -0.0294(4) 0.2978(7) 0.077(4) Uani 1 d . . . H3A H 0.7605 -0.0284 0.2474 0.115 Uiso 1 calc R . . H3B H 0.6701 -0.0564 0.2895 0.115 Uiso 1 calc R . . H3C H 0.7825 -0.0457 0.3430 0.115 Uiso 1 calc R . . S4 S 0.7993(2) 0.17321(10) 0.34171(15) 0.0490(7) Uani 1 d . . . C11 C 1.094(2) 0.1601(15) 0.1526(9) 0.140(10) Uani 1 d . . . H11 H 1.0375 0.1743 0.1135 0.168 Uiso 1 calc R . . C12 C 1.178(2) 0.1954(9) 0.1856(12) 0.119(7) Uani 1 d . . . H12 H 1.1879 0.2383 0.1743 0.143 Uiso 1 calc R . . C13 C 1.2498(12) 0.1571(9) 0.2402(9) 0.093(5) Uani 1 d . . . H13 H 1.3149 0.1693 0.2705 0.112 Uiso 1 calc R . . C14 C 1.2025(17) 0.0966(7) 0.2396(10) 0.091(5) Uani 1 d . . . H14 H 1.2314 0.0613 0.2701 0.109 Uiso 1 calc R . . C15 C 1.106(2) 0.0980(11) 0.1865(15) 0.132(8) Uani 1 d . . . H15 H 1.0585 0.0645 0.1752 0.158 Uiso 1 calc R . . C21 C 1.2100(11) 0.0843(5) 0.4883(6) 0.057(3) Uani 1 d . . . H21 H 1.2587 0.0620 0.4636 0.068 Uiso 1 calc R . . C22 C 1.2278(10) 0.1435(5) 0.5275(6) 0.059(3) Uani 1 d . . . H22 H 1.2897 0.1672 0.5338 0.071 Uiso 1 calc R . . C23 C 1.1347(10) 0.1607(5) 0.5558(5) 0.057(3) Uani 1 d . . . H23 H 1.1243 0.1983 0.5838 0.068 Uiso 1 calc R . . C24 C 1.0574(10) 0.1103(5) 0.5341(6) 0.061(3) Uani 1 d . . . H24 H 0.9894 0.1088 0.5455 0.073 Uiso 1 calc R . . C25 C 1.1082(11) 0.0634(5) 0.4915(6) 0.055(3) Uani 1 d . . . H25 H 1.0784 0.0253 0.4696 0.066 Uiso 1 calc R . . C4 C 0.9121(9) 0.2431(4) 0.2311(5) 0.049(3) Uani 1 d . . . O4 O 0.8833(8) 0.2590(4) 0.1633(4) 0.084(3) Uani 1 d . . . P5 P 0.9098(2) 0.30430(9) 0.39751(12) 0.0377(7) Uani 1 d . . . C31 C 0.9525(8) 0.2990(4) 0.5115(5) 0.041(3) Uani 1 d . . . C32 C 1.0351(9) 0.3348(4) 0.5514(5) 0.050(3) Uani 1 d . . . H32 H 1.0690 0.3629 0.5207 0.060 Uiso 1 calc R . . C33 C 1.0689(10) 0.3295(5) 0.6384(6) 0.064(3) Uani 1 d . . . H33 H 1.1250 0.3539 0.6655 0.077 Uiso 1 calc R . . C34 C 1.0180(11) 0.2876(5) 0.6831(6) 0.070(4) Uani 1 d . . . H34 H 1.0386 0.2847 0.7409 0.084 Uiso 1 calc R . . C35 C 0.9366(10) 0.2498(5) 0.6428(6) 0.062(3) Uani 1 d . . . H35 H 0.9035 0.2210 0.6732 0.074 Uiso 1 calc R . . C36 C 0.9046(9) 0.2554(4) 0.5565(5) 0.054(3) Uani 1 d . . . H36 H 0.8507 0.2297 0.5289 0.064 Uiso 1 calc R . . C41 C 0.7702(8) 0.3243(4) 0.3816(5) 0.043(3) Uani 1 d . . . C42 C 0.7120(10) 0.3363(5) 0.4447(6) 0.053(3) Uani 1 d . . . H42 H 0.7437 0.3309 0.5005 0.064 Uiso 1 calc R . . C43 C 0.6116(12) 0.3554(7) 0.4267(7) 0.080(4) Uani 1 d . . . H43 H 0.5752 0.3627 0.4704 0.096 Uiso 1 calc R . . C44 C 0.5605(10) 0.3644(5) 0.3452(7) 0.067(3) Uani 1 d . . . H44 H 0.4906 0.3777 0.3337 0.081 Uiso 1 calc R . . C45 C 0.6163(10) 0.3532(4) 0.2809(6) 0.053(3) Uani 1 d . . . H45 H 0.5843 0.3595 0.2254 0.064 Uiso 1 calc R . . C46 C 0.7176(9) 0.3330(4) 0.2991(5) 0.046(3) Uani 1 d . . . H46 H 0.7532 0.3245 0.2552 0.055 Uiso 1 calc R . . C51 C 0.9627(8) 0.3806(4) 0.3682(5) 0.047(3) Uani 1 d . . . C52 C 1.0293(9) 0.3855(4) 0.3085(6) 0.053(3) Uani 1 d . . . H52 H 1.0499 0.3488 0.2834 0.063 Uiso 1 calc R . . C53 C 1.0637(10) 0.4436(5) 0.2874(7) 0.068(3) Uani 1 d . . . H53 H 1.1066 0.4463 0.2471 0.082 Uiso 1 calc R . . C54 C 1.0361(10) 0.4983(5) 0.3245(7) 0.072(4) Uani 1 d . . . H54 H 1.0619 0.5376 0.3106 0.087 Uiso 1 calc R . . C55 C 0.9695(11) 0.4950(4) 0.3830(6) 0.069(4) Uani 1 d . . . H55 H 0.9496 0.5321 0.4074 0.082 Uiso 1 calc R . . C56 C 0.9328(9) 0.4365(4) 0.4048(5) 0.050(3) Uani 1 d . . . H56 H 0.8882 0.4343 0.4438 0.060 Uiso 1 calc R . . C60 C 0.569(2) 0.1199(12) 0.4998(12) 0.163(9) Uani 1 d . . . H60 H 0.6401 0.1021 0.5123 0.195 Uiso 1 calc R . . Cl1 Cl 0.5033(5) 0.1240(5) 0.5847(3) 0.203(4) Uani 1 d . . . Cl2 Cl 0.4687(6) 0.0708(5) 0.4213(5) 0.231(4) Uani 1 d . . . Cl3 Cl 0.5586(11) 0.1908(5) 0.4515(7) 0.309(6) Uani 1 d . . . C61 C 0.8149(16) 0.0994(8) 0.0774(11) 0.047(4) Uani 0.50 d PU . . H61 H 0.8112 0.1136 0.1312 0.056 Uiso 0.50 calc PR . . C62 C 0.8093(16) 0.1413(8) 0.0125(11) 0.046(4) Uani 0.50 d PU . . H62 H 0.8057 0.1849 0.0227 0.055 Uiso 0.50 calc PR . . C63 C 0.8090(14) 0.1204(8) -0.0668(9) 0.036(4) Uani 0.50 d PU . . H63 H 0.8040 0.1494 -0.1107 0.043 Uiso 0.50 calc PR . . C64 C 0.8155(15) 0.0600(8) -0.0813(10) 0.040(4) Uani 0.50 d PU . . H64 H 0.8117 0.0458 -0.1362 0.048 Uiso 0.50 calc PR . . C65 C 0.8273(18) 0.0180(10) -0.0197(13) 0.063(6) Uani 0.50 d PU . . H65 H 0.8367 -0.0249 -0.0311 0.076 Uiso 0.50 calc PR . . C66 C 0.8259(17) 0.0371(9) 0.0617(11) 0.053(5) Uani 0.50 d PU . . H66 H 0.8325 0.0073 0.1048 0.064 Uiso 0.50 calc PR . . 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 I1 0.0835(10) 0.0913(6) 0.1041(7) -0.0161(5) 0.0358(6) -0.0174(5) Co1 0.0504(13) 0.0607(7) 0.0389(6) 0.0012(5) 0.0171(6) 0.0057(7) Co2 0.0411(11) 0.0420(6) 0.0321(6) -0.0009(4) 0.0044(5) 0.0015(5) Fe1 0.0450(12) 0.0346(6) 0.0297(6) -0.0014(4) 0.0046(5) 0.0005(5) S1 0.045(2) 0.0457(12) 0.0528(13) 0.0032(9) 0.0061(12) -0.0045(11) C1 0.047(8) 0.036(4) 0.031(4) -0.002(3) 0.001(4) 0.005(4) S2 0.055(2) 0.0392(11) 0.0517(13) -0.0082(9) 0.0016(12) 0.0008(11) C2 0.055(9) 0.038(4) 0.043(5) -0.001(3) 0.003(4) -0.006(4) S3 0.066(3) 0.0535(15) 0.105(2) -0.0111(14) 0.0114(18) -0.0151(14) C3 0.092(11) 0.043(5) 0.084(7) 0.003(5) -0.017(7) -0.018(6) S4 0.045(2) 0.0389(11) 0.0631(14) -0.0093(9) 0.0089(12) -0.0015(11) C11 0.16(3) 0.21(3) 0.054(8) -0.005(12) 0.032(11) 0.10(2) C12 0.17(2) 0.119(13) 0.087(11) 0.033(10) 0.079(13) 0.021(14) C13 0.055(13) 0.143(14) 0.092(10) -0.005(9) 0.040(8) 0.023(10) C14 0.122(17) 0.087(9) 0.086(10) 0.009(7) 0.076(11) 0.041(10) C15 0.13(2) 0.163(18) 0.128(16) -0.098(15) 0.092(15) -0.045(16) C21 0.064(12) 0.061(6) 0.048(5) 0.004(4) 0.015(5) 0.020(6) C22 0.037(10) 0.081(7) 0.051(5) 0.007(5) -0.011(5) -0.005(6) C23 0.070(11) 0.064(6) 0.034(5) -0.002(4) 0.003(5) 0.017(6) C24 0.058(10) 0.082(7) 0.042(5) 0.021(5) 0.006(5) 0.001(6) C25 0.064(12) 0.052(5) 0.046(5) 0.005(4) 0.003(5) -0.002(6) C4 0.068(9) 0.047(5) 0.030(5) 0.000(4) 0.002(4) 0.004(5) O4 0.126(8) 0.079(5) 0.042(4) 0.006(3) 0.002(4) 0.024(5) P5 0.048(2) 0.0344(10) 0.0290(10) -0.0011(8) 0.0018(10) 0.0006(10) C31 0.055(8) 0.038(4) 0.027(4) -0.003(3) -0.002(4) 0.006(4) C32 0.060(9) 0.041(5) 0.043(5) -0.001(4) -0.004(5) 0.006(5) C33 0.080(10) 0.048(5) 0.053(6) -0.005(4) -0.017(6) 0.010(5) C34 0.109(12) 0.057(6) 0.037(5) -0.006(5) -0.006(6) 0.034(7) C35 0.075(10) 0.070(6) 0.042(5) 0.008(5) 0.015(5) 0.022(6) C36 0.067(9) 0.051(5) 0.040(5) 0.000(4) 0.003(5) 0.006(5) C41 0.062(9) 0.035(4) 0.032(4) -0.002(3) 0.004(4) -0.004(4) C42 0.025(10) 0.096(7) 0.041(5) 0.006(5) 0.011(5) 0.025(6) C43 0.046(12) 0.146(12) 0.052(6) 0.005(6) 0.020(6) 0.031(9) C44 0.044(10) 0.082(7) 0.074(7) 0.007(6) 0.005(6) 0.015(6) C45 0.057(11) 0.058(5) 0.042(5) -0.002(4) 0.003(5) 0.002(6) C46 0.039(10) 0.055(5) 0.041(5) -0.004(4) 0.001(5) 0.007(5) C51 0.061(9) 0.034(4) 0.040(5) 0.001(3) -0.010(5) -0.005(4) C52 0.053(9) 0.051(5) 0.055(6) 0.007(4) 0.015(5) 0.004(5) C53 0.068(11) 0.066(7) 0.072(7) 0.017(5) 0.017(6) -0.010(6) C54 0.068(11) 0.054(6) 0.085(8) 0.014(5) -0.014(7) -0.016(6) C55 0.103(11) 0.038(5) 0.058(6) -0.006(4) -0.005(6) -0.005(6) C56 0.063(9) 0.043(5) 0.045(5) 0.000(4) 0.008(5) 0.003(5) C60 0.19(2) 0.21(2) 0.102(13) 0.034(14) 0.065(14) 0.021(19) Cl1 0.124(6) 0.380(11) 0.110(4) -0.014(5) 0.031(3) 0.074(6) Cl2 0.126(6) 0.373(12) 0.204(7) -0.111(7) 0.058(5) -0.032(6) Cl3 0.419(17) 0.264(11) 0.277(11) 0.084(9) 0.153(11) 0.013(11) C61 0.043(7) 0.055(6) 0.041(6) -0.008(4) 0.007(4) 0.005(5) C62 0.043(6) 0.042(5) 0.050(6) -0.010(4) 0.002(4) 0.007(4) C63 0.027(6) 0.044(5) 0.036(5) 0.003(4) 0.007(4) 0.003(4) C64 0.038(6) 0.046(5) 0.035(5) -0.009(4) 0.008(4) 0.000(4) C65 0.065(7) 0.060(7) 0.066(7) -0.006(5) 0.013(5) -0.003(5) C66 0.052(7) 0.058(6) 0.052(6) 0.004(4) 0.011(5) -0.002(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 C1 1.862(10) . ? Co1 C15 2.041(13) . ? Co1 C12 2.048(15) . ? Co1 C11 2.051(15) . ? Co1 C14 2.047(12) . ? Co1 C13 2.071(14) . ? Co1 S1 2.148(3) . ? Co1 Co2 2.4333(15) . ? Co1 Fe1 2.5042(19) . ? Co2 C1 1.862(8) . ? Co2 C23 2.045(9) . ? Co2 C24 2.060(10) . ? Co2 C25 2.065(9) . ? Co2 C21 2.079(10) . ? Co2 C22 2.089(10) . ? Co2 S1 2.125(2) . ? Co2 Fe1 2.5950(16) . ? Fe1 C4 1.743(8) . ? Fe1 C1 1.895(8) . ? Fe1 S1 2.187(3) . ? Fe1 S4 2.238(3) . ? Fe1 P5 2.279(2) . ? C1 S2 1.754(9) . ? S2 C2 1.691(11) . ? C2 S4 1.682(8) . ? C2 S3 1.732(10) . ? S3 C3 1.805(11) . ? C11 C12 1.34(3) . ? C11 C15 1.41(3) . ? C12 C13 1.41(2) . ? C13 C14 1.41(2) . ? C14 C15 1.38(3) . ? C21 C25 1.395(15) . ? C21 C22 1.395(14) . ? C22 C23 1.408(15) . ? C23 C24 1.454(15) . ? C24 C25 1.426(15) . ? C4 O4 1.145(10) . ? P5 C41 1.824(11) . ? P5 C31 1.835(7) . ? P5 C51 1.835(9) . ? C31 C32 1.368(13) . ? C31 C36 1.382(13) . ? C32 C33 1.404(13) . ? C33 C34 1.377(16) . ? C34 C35 1.383(16) . ? C35 C36 1.391(12) . ? C41 C42 1.397(14) . ? C41 C46 1.399(12) . ? C42 C43 1.338(15) . ? C43 C44 1.381(15) . ? C44 C45 1.390(15) . ? C45 C46 1.355(14) . ? C51 C56 1.398(12) . ? C51 C52 1.410(14) . ? C52 C53 1.361(14) . ? C53 C54 1.371(16) . ? C54 C55 1.391(16) . ? C55 C56 1.383(14) . ? C60 Cl3 1.68(2) . ? C60 Cl1 1.742(18) . ? C60 Cl2 1.94(3) . ? C61 C66 1.34(3) . ? C61 C62 1.36(2) . ? C62 C63 1.36(2) . ? C63 C64 1.29(2) . ? C64 C65 1.32(3) . ? C65 C66 1.38(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Co1 C15 100.7(6) . . ? C1 Co1 C12 159.1(8) . . ? C15 Co1 C12 66.6(8) . . ? C1 Co1 C11 121.6(10) . . ? C15 Co1 C11 40.3(8) . . ? C12 Co1 C11 38.3(8) . . ? C1 Co1 C14 114.9(5) . . ? C15 Co1 C14 39.5(7) . . ? C12 Co1 C14 66.6(6) . . ? C11 Co1 C14 66.2(7) . . ? C1 Co1 C13 152.1(6) . . ? C15 Co1 C13 67.0(7) . . ? C12 Co1 C13 40.0(7) . . ? C11 Co1 C13 65.9(8) . . ? C14 Co1 C13 40.0(6) . . ? C1 Co1 S1 87.3(2) . . ? C15 Co1 S1 171.9(5) . . ? C12 Co1 S1 105.5(6) . . ? C11 Co1 S1 134.0(9) . . ? C14 Co1 S1 137.0(7) . . ? C13 Co1 S1 106.0(5) . . ? C1 Co1 Co2 49.2(2) . . ? C15 Co1 Co2 131.6(8) . . ? C12 Co1 Co2 151.5(8) . . ? C11 Co1 Co2 169.6(10) . . ? C14 Co1 Co2 111.7(4) . . ? C13 Co1 Co2 119.6(4) . . ? S1 Co1 Co2 54.85(7) . . ? C1 Co1 Fe1 48.8(2) . . ? C15 Co1 Fe1 130.1(8) . . ? C12 Co1 Fe1 126.1(6) . . ? C11 Co1 Fe1 115.4(6) . . ? C14 Co1 Fe1 162.9(6) . . ? C13 Co1 Fe1 157.1(5) . . ? S1 Co1 Fe1 55.44(8) . . ? Co2 Co1 Fe1 63.39(5) . . ? C1 Co2 C23 148.9(5) . . ? C1 Co2 C24 110.8(4) . . ? C23 Co2 C24 41.5(4) . . ? C1 Co2 C25 100.2(4) . . ? C23 Co2 C25 67.7(4) . . ? C24 Co2 C25 40.4(4) . . ? C1 Co2 C21 122.9(4) . . ? C23 Co2 C21 66.3(4) . . ? C24 Co2 C21 67.2(5) . . ? C25 Co2 C21 39.3(4) . . ? C1 Co2 C22 161.8(4) . . ? C23 Co2 C22 39.8(4) . . ? C24 Co2 C22 68.3(5) . . ? C25 Co2 C22 66.8(4) . . ? C21 Co2 C22 39.1(4) . . ? C1 Co2 S1 88.0(3) . . ? C23 Co2 S1 108.4(3) . . ? C24 Co2 S1 142.1(3) . . ? C25 Co2 S1 169.3(4) . . ? C21 Co2 S1 130.0(4) . . ? C22 Co2 S1 103.6(3) . . ? C1 Co2 Co1 49.2(3) . . ? C23 Co2 Co1 160.4(4) . . ? C24 Co2 Co1 158.0(3) . . ? C25 Co2 Co1 125.5(3) . . ? C21 Co2 Co1 113.3(3) . . ? C22 Co2 Co1 127.1(4) . . ? S1 Co2 Co1 55.73(7) . . ? C1 Co2 Fe1 46.8(2) . . ? C23 Co2 Fe1 123.1(3) . . ? C24 Co2 Fe1 116.1(3) . . ? C25 Co2 Fe1 136.6(4) . . ? C21 Co2 Fe1 169.5(3) . . ? C22 Co2 Fe1 151.0(3) . . ? S1 Co2 Fe1 54.10(8) . . ? Co1 Co2 Fe1 59.64(5) . . ? C4 Fe1 C1 112.1(4) . . ? C4 Fe1 S1 109.6(4) . . ? C1 Fe1 S1 85.4(3) . . ? C4 Fe1 S4 92.7(4) . . ? C1 Fe1 S4 85.0(3) . . ? S1 Fe1 S4 157.67(10) . . ? C4 Fe1 P5 95.2(3) . . ? C1 Fe1 P5 152.3(2) . . ? S1 Fe1 P5 90.60(10) . . ? S4 Fe1 P5 88.57(10) . . ? C4 Fe1 Co1 88.4(3) . . ? C1 Fe1 Co1 47.6(3) . . ? S1 Fe1 Co1 53.98(8) . . ? S4 Fe1 Co1 128.12(8) . . ? P5 Fe1 Co1 143.00(9) . . ? C4 Fe1 Co2 145.3(3) . . ? C1 Fe1 Co2 45.8(2) . . ? S1 Fe1 Co2 51.92(7) . . ? S4 Fe1 Co2 108.23(8) . . ? P5 Fe1 Co2 112.22(7) . . ? Co1 Fe1 Co2 56.97(5) . . ? Co2 S1 Co1 69.43(8) . . ? Co2 S1 Fe1 73.98(9) . . ? Co1 S1 Fe1 70.58(9) . . ? S2 C1 Co2 128.4(4) . . ? S2 C1 Co1 132.1(5) . . ? Co2 C1 Co1 81.6(4) . . ? S2 C1 Fe1 127.4(6) . . ? Co2 C1 Fe1 87.4(3) . . ? Co1 C1 Fe1 83.6(3) . . ? C2 S2 C1 97.5(4) . . ? S4 C2 S2 121.0(6) . . ? S4 C2 S3 116.4(6) . . ? S2 C2 S3 122.6(5) . . ? C2 S3 C3 103.9(5) . . ? C2 S4 Fe1 106.7(4) . . ? C12 C11 C15 109(2) . . ? C12 C11 Co1 70.8(10) . . ? C15 C11 Co1 69.4(9) . . ? C11 C12 C13 109.1(18) . . ? C11 C12 Co1 71.0(11) . . ? C13 C12 Co1 70.9(8) . . ? C14 C13 C12 106.0(16) . . ? C14 C13 Co1 69.1(8) . . ? C12 C13 Co1 69.1(9) . . ? C15 C14 C13 109.0(15) . . ? C15 C14 Co1 70.0(8) . . ? C13 C14 Co1 70.9(7) . . ? C14 C15 C11 106.6(18) . . ? C14 C15 Co1 70.5(8) . . ? C11 C15 Co1 70.2(9) . . ? C25 C21 C22 110.0(10) . . ? C25 C21 Co2 69.8(6) . . ? C22 C21 Co2 70.8(6) . . ? C21 C22 C23 107.2(11) . . ? C21 C22 Co2 70.1(6) . . ? C23 C22 Co2 68.4(6) . . ? C22 C23 C24 108.9(9) . . ? C22 C23 Co2 71.8(6) . . ? C24 C23 Co2 69.8(5) . . ? C25 C24 C23 105.3(11) . . ? C25 C24 Co2 70.0(6) . . ? C23 C24 Co2 68.7(5) . . ? C21 C25 C24 108.7(10) . . ? C21 C25 Co2 70.9(6) . . ? C24 C25 Co2 69.6(5) . . ? O4 C4 Fe1 177.2(8) . . ? C41 P5 C31 105.6(4) . . ? C41 P5 C51 99.6(4) . . ? C31 P5 C51 104.7(4) . . ? C41 P5 Fe1 117.3(3) . . ? C31 P5 Fe1 111.0(3) . . ? C51 P5 Fe1 117.1(3) . . ? C32 C31 C36 119.9(8) . . ? C32 C31 P5 120.8(7) . . ? C36 C31 P5 119.2(7) . . ? C31 C32 C33 120.5(10) . . ? C34 C33 C32 119.1(10) . . ? C33 C34 C35 120.7(9) . . ? C34 C35 C36 119.4(10) . . ? C31 C36 C35 120.3(10) . . ? C42 C41 C46 116.4(10) . . ? C42 C41 P5 125.8(7) . . ? C46 C41 P5 117.7(8) . . ? C43 C42 C41 121.4(9) . . ? C42 C43 C44 121.9(11) . . ? C43 C44 C45 118.1(12) . . ? C46 C45 C44 120.0(9) . . ? C45 C46 C41 122.2(9) . . ? C56 C51 C52 118.6(8) . . ? C56 C51 P5 118.5(8) . . ? C52 C51 P5 122.8(7) . . ? C53 C52 C51 120.3(10) . . ? C52 C53 C54 121.1(11) . . ? C53 C54 C55 119.8(10) . . ? C56 C55 C54 120.1(10) . . ? C55 C56 C51 120.1(10) . . ? Cl3 C60 Cl1 108.4(14) . . ? Cl3 C60 Cl2 100.1(12) . . ? Cl1 C60 Cl2 100.6(12) . . ? C66 C61 C62 118.2(16) . . ? C61 C62 C63 120.9(16) . . ? C64 C63 C62 120.0(16) . . ? C63 C64 C65 121.2(16) . . ? C64 C65 C66 120.7(19) . . ? C61 C66 C65 118.9(18) . . ? _diffrn_measured_fraction_theta_max 0.729 _diffrn_reflns_theta_full 23.39 _diffrn_measured_fraction_theta_full 0.729 _refine_diff_density_max 1.023 _refine_diff_density_min -0.640 _refine_diff_density_rms 0.132 data_fecos _database_code_CSD 215760 _audit_creation_method SHELXL-96 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C43 H37 Co2 Fe O P S4' _chemical_formula_weight 902.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? 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 9.853(13) _cell_length_b 19.97(2) _cell_length_c 20.61(2) _cell_angle_alpha 90.00 _cell_angle_beta 91.79(4) _cell_angle_gamma 90.00 _cell_volume 4055(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 20 _cell_measurement_theta_min 4 _cell_measurement_theta_max 11 _exptl_crystal_description plate _exptl_crystal_colour 'dark brown' _exptl_crystal_size_max 0.95 _exptl_crystal_size_mid 0.65 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.478 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1848 _exptl_absorpt_coefficient_mu 1.440 _exptl_absorpt_correction_type 'empirical \y scans' _exptl_absorpt_correction_T_min 0.419 _exptl_absorpt_correction_T_max 0.925 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 1 _diffrn_reflns_number 6687 _diffrn_reflns_av_R_equivalents 0.1296 _diffrn_reflns_av_sigmaI/netI 0.1813 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 25.01 _reflns_number_total 6380 _reflns_number_gt 2930 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens XSCANS' _computing_structure_solution SHELXS-86 _computing_structure_refinement SHELXL-96 _computing_molecular_graphics SHELXTL-PC _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 w=1/[\s^2^(Fo^2^)+(0.0887P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6380 _refine_ls_number_parameters 469 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1488 _refine_ls_R_factor_gt 0.0692 _refine_ls_wR_factor_ref 0.1823 _refine_ls_wR_factor_gt 0.1575 _refine_ls_goodness_of_fit_ref 0.832 _refine_ls_restrained_S_all 0.832 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S1 S 0.3180(2) 0.18339(12) 0.18213(13) 0.0300(6) Uani 1 d . . . C1 C 0.3068(9) 0.3084(5) 0.2442(5) 0.035(3) Uani 1 d . . . S2 S 0.2994(3) 0.38683(13) 0.28440(14) 0.0403(7) Uani 1 d . . . C2 C 0.2987(8) 0.4398(5) 0.2179(6) 0.036(3) Uani 1 d . . . S3 S 0.2743(3) 0.52254(13) 0.22640(16) 0.0453(8) Uani 1 d . . . S4 S 0.3213(2) 0.40112(12) 0.14190(14) 0.0323(6) Uani 1 d . . . Co1 Co 0.17151(12) 0.24263(6) 0.23344(7) 0.0266(3) Uani 1 d . . . C13 C -0.0245(11) 0.2656(12) 0.2053(9) 0.096(7) Uani 1 d . . . H13 H -0.0486 0.2902 0.1684 0.115 Uiso 1 calc R . . C14 C -0.0074(14) 0.1956(12) 0.2084(10) 0.096(7) Uani 1 d . . . H14 H -0.0143 0.1664 0.1734 0.115 Uiso 1 calc R . . C15 C 0.0194(13) 0.1786(7) 0.2678(9) 0.071(5) Uani 1 d . . . H15 H 0.0251 0.1345 0.2821 0.085 Uiso 1 calc R . . C11 C 0.0401(10) 0.2372(7) 0.3107(6) 0.053(3) Uani 1 d . . . H11 H 0.0698 0.2392 0.3539 0.064 Uiso 1 calc R . . C12 C 0.0008(11) 0.2910(6) 0.2663(7) 0.053(4) Uani 1 d . . . H12 H -0.0061 0.3359 0.2777 0.064 Uiso 1 calc R . . Co2 Co 0.41293(13) 0.23315(7) 0.26638(7) 0.0320(4) Uani 1 d . . . C21 C 0.6086(11) 0.1980(6) 0.2886(6) 0.055(4) Uani 1 d . . . H21 H 0.6737 0.1871 0.2587 0.066 Uiso 1 calc R . . C22 C 0.5902(12) 0.2623(7) 0.3159(6) 0.055(3) Uani 1 d . . . H22 H 0.6400 0.3007 0.3071 0.066 Uiso 1 calc R . . C23 C 0.4819(12) 0.2573(6) 0.3590(6) 0.052(3) Uani 1 d U . . H23 H 0.4479 0.2918 0.3842 0.062 Uiso 1 calc R . . C24 C 0.4341(12) 0.1902(6) 0.3572(6) 0.055(3) Uani 1 d . . . H24 H 0.3625 0.1737 0.3809 0.066 Uiso 1 calc R . . C25 C 0.5115(12) 0.1525(6) 0.3140(6) 0.051(3) Uani 1 d . . . H25 H 0.5017 0.1073 0.3041 0.061 Uiso 1 calc R . . Fe1 Fe 0.36237(13) 0.28910(7) 0.15975(7) 0.0244(3) Uani 1 d . . . C3 C 0.5387(11) 0.2966(5) 0.1514(5) 0.034(2) Uani 1 d . . . O3 O 0.6575(6) 0.3012(4) 0.1526(4) 0.051(2) Uani 1 d . . . P1 P 0.3131(2) 0.27108(12) 0.05127(13) 0.0245(6) Uani 1 d . . . C31 C 0.3610(9) 0.3369(5) -0.0083(5) 0.028(2) Uani 1 d . . . C32 C 0.2900(10) 0.3517(5) -0.0625(5) 0.036(3) Uani 1 d . . . H32 H 0.2075 0.3302 -0.0708 0.043 Uiso 1 calc R . . C33 C 0.3356(10) 0.3992(5) -0.1081(6) 0.039(3) Uani 1 d . . . H33 H 0.2834 0.4086 -0.1453 0.047 Uiso 1 calc R . . C34 C 0.4555(12) 0.4305(6) -0.0969(6) 0.048(3) Uani 1 d . . . H34 H 0.4868 0.4613 -0.1268 0.058 Uiso 1 calc R . . C35 C 0.5329(13) 0.4169(7) -0.0403(7) 0.073(5) Uani 1 d . . . H35 H 0.6144 0.4392 -0.0320 0.087 Uiso 1 calc R . . C36 C 0.4867(10) 0.3692(6) 0.0039(6) 0.058(4) Uani 1 d . . . H36 H 0.5385 0.3590 0.0410 0.069 Uiso 1 calc R . . C41 C 0.1273(8) 0.2597(5) 0.0388(5) 0.028(2) Uani 1 d . . . C42 C 0.0679(9) 0.1959(5) 0.0331(4) 0.027(2) Uani 1 d . . . H42 H 0.1234 0.1582 0.0325 0.032 Uiso 1 calc R . . C43 C -0.0711(10) 0.1880(5) 0.0282(5) 0.036(3) Uani 1 d . . . H43 H -0.1081 0.1452 0.0267 0.044 Uiso 1 calc R . . C44 C -0.1562(9) 0.2431(5) 0.0256(5) 0.037(3) Uani 1 d . . . H44 H -0.2497 0.2380 0.0207 0.044 Uiso 1 calc R . . C45 C -0.0976(9) 0.3067(5) 0.0305(5) 0.034(3) Uani 1 d . . . H45 H -0.1536 0.3442 0.0311 0.041 Uiso 1 calc R . . C46 C 0.0392(9) 0.3152(5) 0.0346(5) 0.032(2) Uani 1 d . . . H46 H 0.0752 0.3582 0.0345 0.038 Uiso 1 calc R . . C51 C 0.3885(9) 0.1968(5) 0.0127(5) 0.031(2) Uani 1 d . . . C52 C 0.4919(10) 0.1592(5) 0.0429(5) 0.040(3) Uani 1 d . . . H52 H 0.5223 0.1702 0.0847 0.048 Uiso 1 calc R . . C53 C 0.5503(11) 0.1054(5) 0.0110(7) 0.051(3) Uani 1 d . . . H53 H 0.6197 0.0815 0.0321 0.061 Uiso 1 calc R . . C54 C 0.5096(11) 0.0867(6) -0.0493(6) 0.044(3) Uani 1 d . . . H54 H 0.5521 0.0511 -0.0695 0.053 Uiso 1 calc R . . C55 C 0.4017(11) 0.1214(5) -0.0821(6) 0.045(3) Uani 1 d . . . H55 H 0.3697 0.1081 -0.1230 0.054 Uiso 1 calc R . . C56 C 0.3448(10) 0.1771(5) -0.0500(5) 0.032(2) Uani 1 d . . . H56 H 0.2762 0.2013 -0.0713 0.039 Uiso 1 calc R . . C1B1 C 0.8958(13) 0.5267(7) 0.2989(8) 0.075(5) Uani 1 d . . . H1B1 H 0.9713 0.5478 0.3178 0.090 Uiso 1 calc R . . C1B2 C 0.9095(12) 0.4765(7) 0.2538(8) 0.070(5) Uani 1 d . . . H1B2 H 0.9962 0.4637 0.2422 0.083 Uiso 1 calc R . . C1B3 C 0.7998(11) 0.4449(6) 0.2253(7) 0.055(4) Uani 1 d . . . H1B3 H 0.8132 0.4103 0.1959 0.066 Uiso 1 calc R . . C1B4 C 0.6689(12) 0.4639(7) 0.2397(7) 0.058(4) Uani 1 d . . . H1B4 H 0.5940 0.4443 0.2187 0.070 Uiso 1 calc R . . C1B5 C 0.6526(13) 0.5134(8) 0.2868(8) 0.074(5) Uani 1 d . . . H1B5 H 0.5658 0.5253 0.2990 0.088 Uiso 1 calc R . . C1B6 C 0.7644(15) 0.5448(7) 0.3153(7) 0.071(4) Uani 1 d . . . H1B6 H 0.7518 0.5784 0.3458 0.085 Uiso 1 calc R . . C2B1 C -0.0677(15) -0.0279(6) 0.0514(7) 0.065(4) Uani 1 d . . . H2B1 H -0.1127 -0.0463 0.0861 0.078 Uiso 1 calc R . . C2B2 C 0.0651(17) -0.0085(6) 0.0591(8) 0.078(5) Uani 1 d . . . H2B2 H 0.1097 -0.0145 0.0991 0.093 Uiso 1 calc R . . C2B3 C 0.1349(12) 0.0203(5) 0.0079(7) 0.052(3) Uani 1 d . . . H2B3 H 0.2247 0.0339 0.0138 0.063 Uiso 1 calc R . . C3B1 C 0.0961(13) 0.5121(6) 0.0471(7) 0.059(4) Uani 1 d . . . H3B1 H 0.1632 0.5200 0.0789 0.071 Uiso 1 calc R . . C3B2 C 0.1302(13) 0.5048(7) -0.0181(9) 0.084(6) Uani 1 d . . . H3B2 H 0.2203 0.5086 -0.0299 0.100 Uiso 1 calc R . . C3B3 C 0.0347(16) 0.4924(6) -0.0628(7) 0.064(4) Uani 1 d . . . H3B3 H 0.0584 0.4867 -0.1057 0.077 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1 0.0412(14) 0.0294(13) 0.0193(16) -0.0033(11) 0.0020(11) 0.0079(11) C1 0.038(6) 0.049(7) 0.018(6) -0.006(5) -0.008(4) 0.001(5) S2 0.0590(17) 0.0364(15) 0.0261(18) -0.0111(12) 0.0103(13) -0.0014(13) C2 0.015(5) 0.046(6) 0.049(8) -0.004(5) 0.005(4) -0.009(4) S3 0.0477(16) 0.0309(15) 0.058(2) -0.0122(14) 0.0112(14) -0.0014(12) S4 0.0394(14) 0.0269(13) 0.0308(18) 0.0009(11) 0.0024(11) 0.0008(11) Co1 0.0321(7) 0.0311(8) 0.0170(8) 0.0037(6) 0.0094(5) 0.0020(6) C13 0.017(6) 0.20(2) 0.067(13) 0.069(14) 0.021(6) 0.028(9) C14 0.052(9) 0.17(2) 0.070(15) -0.050(13) 0.041(9) -0.043(11) C15 0.062(8) 0.050(8) 0.105(15) 0.004(9) 0.064(9) -0.006(6) C11 0.044(6) 0.090(10) 0.026(8) 0.013(7) 0.010(5) 0.002(6) C12 0.059(8) 0.038(7) 0.064(11) 0.005(7) 0.027(7) 0.022(6) Co2 0.0391(8) 0.0424(8) 0.0142(9) 0.0032(6) -0.0010(6) 0.0041(6) C21 0.054(7) 0.058(9) 0.055(10) 0.006(7) 0.006(6) 0.006(6) C22 0.061(8) 0.069(9) 0.035(9) -0.007(7) -0.011(6) -0.019(7) C23 0.071(6) 0.061(7) 0.022(6) -0.015(5) -0.014(5) 0.006(5) C24 0.064(8) 0.062(9) 0.037(9) 0.008(7) -0.003(6) 0.007(6) C25 0.088(9) 0.041(7) 0.021(8) 0.003(5) -0.023(6) 0.021(6) Fe1 0.0315(7) 0.0287(8) 0.0132(8) 0.0003(6) 0.0031(6) -0.0003(6) C3 0.058(7) 0.040(6) 0.003(5) 0.005(4) 0.002(5) 0.006(5) O3 0.019(4) 0.086(6) 0.049(6) 0.010(4) 0.004(3) 0.003(4) P1 0.0250(12) 0.0336(14) 0.0149(15) -0.0018(11) 0.0022(10) -0.0014(10) C31 0.033(5) 0.033(6) 0.019(7) -0.002(4) 0.006(4) -0.007(4) C32 0.043(6) 0.055(7) 0.010(6) -0.003(5) -0.001(5) -0.020(5) C33 0.051(7) 0.038(6) 0.029(8) 0.006(5) 0.010(5) -0.008(5) C34 0.071(8) 0.060(8) 0.016(7) 0.004(6) 0.021(6) -0.009(6) C35 0.066(8) 0.097(11) 0.053(11) 0.019(8) -0.008(7) -0.061(8) C36 0.039(6) 0.094(10) 0.039(9) 0.027(7) -0.016(5) -0.021(6) C41 0.023(4) 0.042(6) 0.019(6) 0.000(4) 0.006(4) -0.006(4) C42 0.035(5) 0.034(6) 0.012(6) 0.010(4) 0.002(4) 0.005(4) C43 0.048(6) 0.039(6) 0.023(7) 0.001(5) 0.000(5) -0.013(5) C44 0.025(5) 0.058(7) 0.026(7) -0.001(5) 0.005(4) -0.012(5) C45 0.032(5) 0.039(6) 0.031(7) 0.004(5) 0.008(5) 0.014(4) C46 0.038(5) 0.033(6) 0.024(7) -0.004(5) 0.006(4) -0.003(5) C51 0.032(5) 0.036(6) 0.027(7) 0.002(5) 0.008(4) 0.004(4) C52 0.057(7) 0.038(6) 0.027(7) 0.005(5) 0.021(5) 0.004(5) C53 0.048(7) 0.032(6) 0.072(11) -0.009(6) 0.012(6) 0.005(5) C54 0.051(7) 0.045(7) 0.037(9) -0.013(6) 0.011(6) 0.010(5) C55 0.065(8) 0.030(6) 0.042(8) -0.002(5) 0.023(6) -0.008(5) C56 0.044(6) 0.032(6) 0.022(7) 0.002(5) 0.010(5) 0.010(5) C1B1 0.055(9) 0.063(10) 0.105(15) 0.033(9) -0.028(8) -0.021(7) C1B2 0.042(7) 0.060(9) 0.108(15) 0.033(9) 0.018(8) -0.003(7) C1B3 0.050(7) 0.049(8) 0.066(11) 0.020(7) 0.003(7) -0.001(6) C1B4 0.049(7) 0.071(9) 0.054(11) 0.011(8) -0.008(6) -0.002(7) C1B5 0.044(7) 0.096(12) 0.082(14) 0.033(9) 0.021(8) 0.009(7) C1B6 0.091(11) 0.057(9) 0.066(12) 0.006(8) 0.001(8) -0.003(8) C2B1 0.097(11) 0.055(9) 0.045(11) 0.003(7) 0.026(8) -0.016(8) C2B2 0.136(14) 0.031(7) 0.066(12) 0.010(7) -0.001(10) -0.002(8) C2B3 0.059(8) 0.035(7) 0.063(11) -0.010(6) 0.007(7) 0.005(6) C3B1 0.066(9) 0.043(7) 0.065(12) -0.026(7) -0.044(7) 0.019(6) C3B2 0.050(8) 0.077(10) 0.126(17) -0.058(10) 0.032(9) -0.011(7) C3B3 0.096(11) 0.059(9) 0.038(10) -0.009(7) 0.015(8) -0.029(8) _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 S1 Co1 2.168(3) . ? S1 Co2 2.186(3) . ? S1 Fe1 2.208(4) . ? C1 S2 1.774(10) . ? C1 Co2 1.880(10) . ? C1 Co1 1.881(10) . ? C1 Fe1 1.881(11) . ? S2 C2 1.731(11) . ? C2 S3 1.680(11) . ? C2 S4 1.768(11) . ? S4 Fe1 2.301(4) . ? Co1 C13 2.051(12) . ? Co1 C14 2.049(14) . ? Co1 C12 2.072(10) . ? Co1 C11 2.086(11) . ? Co1 C15 2.110(11) . ? Co1 Co2 2.461(4) . ? Co1 Fe1 2.624(3) . ? C13 C12 1.37(2) . ? C13 C14 1.41(2) . ? C14 C15 1.29(2) . ? C15 C11 1.478(18) . ? C11 C12 1.455(16) . ? Co2 C24 2.064(12) . ? Co2 C23 2.064(12) . ? Co2 C22 2.079(11) . ? Co2 C21 2.088(11) . ? Co2 C25 2.109(11) . ? Co2 Fe1 2.502(3) . ? C21 C22 1.416(16) . ? C21 C25 1.431(16) . ? C22 C23 1.414(16) . ? C23 C24 1.421(16) . ? C24 C25 1.409(16) . ? Fe1 C3 1.758(11) . ? Fe1 P1 2.302(4) . ? C3 O3 1.173(11) . ? P1 C51 1.850(10) . ? P1 C41 1.854(9) . ? P1 C31 1.869(10) . ? C31 C32 1.334(14) . ? C31 C36 1.413(13) . ? C32 C33 1.416(13) . ? C33 C34 1.351(14) . ? C34 C35 1.401(17) . ? C35 C36 1.403(16) . ? C41 C42 1.407(12) . ? C41 C46 1.410(13) . ? C42 C43 1.379(12) . ? C43 C44 1.383(13) . ? C44 C45 1.399(13) . ? C45 C46 1.358(12) . ? C51 C52 1.397(14) . ? C51 C56 1.407(14) . ? C52 C53 1.394(14) . ? C53 C54 1.347(16) . ? C54 C55 1.422(15) . ? C55 C56 1.418(13) . ? C1B1 C1B2 1.38(2) . ? C1B1 C1B6 1.395(18) . ? C1B2 C1B3 1.368(17) . ? C1B3 C1B4 1.386(15) . ? C1B4 C1B5 1.397(19) . ? C1B5 C1B6 1.382(19) . ? C2B1 C2B2 1.369(18) . ? C2B1 C2B3 1.380(18) 3 ? C2B2 C2B3 1.401(18) . ? C2B3 C2B1 1.380(18) 3 ? C3B1 C3B3 1.342(16) 3_565 ? C3B1 C3B2 1.40(2) . ? C3B2 C3B3 1.318(19) . ? C3B3 C3B1 1.342(16) 3_565 ? 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 Co1 S1 Co2 68.83(12) . . ? Co1 S1 Fe1 73.68(11) . . ? Co2 S1 Fe1 69.43(10) . . ? S2 C1 Co2 128.6(6) . . ? S2 C1 Co1 129.2(5) . . ? Co2 C1 Co1 81.7(4) . . ? S2 C1 Fe1 129.1(6) . . ? Co2 C1 Fe1 83.4(4) . . ? Co1 C1 Fe1 88.4(4) . . ? C2 S2 C1 99.7(5) . . ? S3 C2 S2 121.1(7) . . ? S3 C2 S4 123.0(7) . . ? S2 C2 S4 115.9(6) . . ? C2 S4 Fe1 108.1(4) . . ? C1 Co1 C13 122.3(7) . . ? C1 Co1 C14 162.1(8) . . ? C13 Co1 C14 40.2(6) . . ? C1 Co1 C12 102.4(5) . . ? C13 Co1 C12 38.9(6) . . ? C14 Co1 C12 66.2(6) . . ? C1 Co1 C11 113.6(5) . . ? C13 Co1 C11 68.1(5) . . ? C14 Co1 C11 67.6(6) . . ? C12 Co1 C11 41.0(5) . . ? C1 Co1 C15 153.2(6) . . ? C13 Co1 C15 63.8(6) . . ? C14 Co1 C15 36.1(6) . . ? C12 Co1 C15 65.2(5) . . ? C11 Co1 C15 41.2(5) . . ? C1 Co1 S1 87.6(3) . . ? C13 Co1 S1 128.3(6) . . ? C14 Co1 S1 102.0(5) . . ? C12 Co1 S1 166.9(4) . . ? C11 Co1 S1 141.5(4) . . ? C15 Co1 S1 108.9(4) . . ? C1 Co1 Co2 49.1(3) . . ? C13 Co1 Co2 171.5(7) . . ? C14 Co1 Co2 148.3(7) . . ? C12 Co1 Co2 137.1(4) . . ? C11 Co1 Co2 113.8(3) . . ? C15 Co1 Co2 123.5(5) . . ? S1 Co1 Co2 55.93(10) . . ? C1 Co1 Fe1 45.8(3) . . ? C13 Co1 Fe1 116.3(4) . . ? C14 Co1 Fe1 130.0(5) . . ? C12 Co1 Fe1 128.9(3) . . ? C11 Co1 Fe1 159.0(4) . . ? C15 Co1 Fe1 159.8(5) . . ? S1 Co1 Fe1 53.86(10) . . ? Co2 Co1 Fe1 58.86(9) . . ? C12 C13 C14 107.8(13) . . ? C12 C13 Co1 71.4(7) . . ? C14 C13 Co1 69.8(8) . . ? C15 C14 C13 109.0(15) . . ? C15 C14 Co1 74.5(9) . . ? C13 C14 Co1 70.0(8) . . ? C14 C15 C11 112.3(14) . . ? C14 C15 Co1 69.4(8) . . ? C11 C15 Co1 68.5(6) . . ? C12 C11 C15 100.4(12) . . ? C12 C11 Co1 69.0(6) . . ? C15 C11 Co1 70.2(7) . . ? C13 C12 C11 109.9(12) . . ? C13 C12 Co1 69.7(7) . . ? C11 C12 Co1 70.0(6) . . ? C1 Co2 C24 126.4(5) . . ? C1 Co2 C23 101.7(5) . . ? C24 Co2 C23 40.3(5) . . ? C1 Co2 C22 110.3(5) . . ? C24 Co2 C22 67.2(5) . . ? C23 Co2 C22 39.9(5) . . ? C1 Co2 C21 145.5(5) . . ? C24 Co2 C21 66.1(5) . . ? C23 Co2 C21 66.5(5) . . ? C22 Co2 C21 39.7(4) . . ? C1 Co2 C25 165.8(5) . . ? C24 Co2 C25 39.4(4) . . ? C23 Co2 C25 67.3(5) . . ? C22 Co2 C25 67.5(5) . . ? C21 Co2 C25 39.9(4) . . ? C1 Co2 S1 87.1(3) . . ? C24 Co2 S1 124.1(4) . . ? C23 Co2 S1 164.1(4) . . ? C22 Co2 S1 148.2(4) . . ? C21 Co2 S1 113.0(4) . . ? C25 Co2 S1 101.6(4) . . ? C1 Co2 Co1 49.2(3) . . ? C24 Co2 Co1 110.6(3) . . ? C23 Co2 Co1 121.6(3) . . ? C22 Co2 Co1 154.7(4) . . ? C21 Co2 Co1 164.6(4) . . ? C25 Co2 Co1 127.9(4) . . ? S1 Co2 Co1 55.24(8) . . ? C1 Co2 Fe1 48.3(3) . . ? C24 Co2 Fe1 173.8(3) . . ? C23 Co2 Fe1 139.4(4) . . ? C22 Co2 Fe1 116.6(4) . . ? C21 Co2 Fe1 120.0(4) . . ? C25 Co2 Fe1 145.8(3) . . ? S1 Co2 Fe1 55.71(11) . . ? Co1 Co2 Fe1 63.83(6) . . ? C22 C21 C25 109.6(11) . . ? C22 C21 Co2 69.8(7) . . ? C25 C21 Co2 70.8(6) . . ? C21 C22 C23 107.1(11) . . ? C21 C22 Co2 70.5(7) . . ? C23 C22 Co2 69.5(6) . . ? C22 C23 C24 107.8(11) . . ? C22 C23 Co2 70.6(7) . . ? C24 C23 Co2 69.8(7) . . ? C25 C24 C23 109.6(11) . . ? C25 C24 Co2 72.0(7) . . ? C23 C24 Co2 69.9(7) . . ? C24 C25 C21 105.8(11) . . ? C24 C25 Co2 68.6(7) . . ? C21 C25 Co2 69.3(6) . . ? C3 Fe1 C1 113.0(4) . . ? C3 Fe1 S1 107.7(3) . . ? C1 Fe1 S1 86.4(3) . . ? C3 Fe1 S4 94.1(3) . . ? C1 Fe1 S4 83.9(3) . . ? S1 Fe1 S4 158.18(11) . . ? C3 Fe1 P1 95.6(3) . . ? C1 Fe1 P1 150.8(3) . . ? S1 Fe1 P1 90.94(11) . . ? S4 Fe1 P1 88.05(11) . . ? C3 Fe1 Co2 87.3(3) . . ? C1 Fe1 Co2 48.3(3) . . ? S1 Fe1 Co2 54.87(8) . . ? S4 Fe1 Co2 127.14(10) . . ? P1 Fe1 Co2 144.47(11) . . ? C3 Fe1 Co1 144.6(3) . . ? C1 Fe1 Co1 45.8(3) . . ? S1 Fe1 Co1 52.45(7) . . ? S4 Fe1 Co1 108.12(9) . . ? P1 Fe1 Co1 111.95(10) . . ? Co2 Fe1 Co1 57.31(8) . . ? O3 C3 Fe1 173.2(9) . . ? C51 P1 C41 104.5(4) . . ? C51 P1 C31 99.7(4) . . ? C41 P1 C31 105.3(4) . . ? C51 P1 Fe1 117.9(4) . . ? C41 P1 Fe1 109.4(3) . . ? C31 P1 Fe1 118.6(3) . . ? C32 C31 C36 118.7(9) . . ? C32 C31 P1 124.8(7) . . ? C36 C31 P1 116.3(8) . . ? C31 C32 C33 122.4(10) . . ? C34 C33 C32 119.4(11) . . ? C33 C34 C35 120.2(10) . . ? C34 C35 C36 119.6(10) . . ? C35 C36 C31 119.7(11) . . ? C42 C41 C46 117.0(8) . . ? C42 C41 P1 122.0(7) . . ? C46 C41 P1 121.0(7) . . ? C43 C42 C41 121.3(9) . . ? C42 C43 C44 120.8(9) . . ? C43 C44 C45 118.2(9) . . ? C46 C45 C44 121.6(9) . . ? C45 C46 C41 120.9(9) . . ? C52 C51 C56 117.2(9) . . ? C52 C51 P1 122.5(8) . . ? C56 C51 P1 120.3(7) . . ? C53 C52 C51 120.7(11) . . ? C54 C53 C52 122.3(12) . . ? C53 C54 C55 120.0(10) . . ? C56 C55 C54 117.5(11) . . ? C51 C56 C55 122.3(10) . . ? C1B2 C1B1 C1B6 117.6(13) . . ? C1B3 C1B2 C1B1 122.2(12) . . ? C1B2 C1B3 C1B4 120.6(14) . . ? C1B3 C1B4 C1B5 118.1(12) . . ? C1B6 C1B5 C1B4 120.6(13) . . ? C1B5 C1B6 C1B1 120.8(15) . . ? C2B2 C2B1 C2B3 120.2(12) . 3 ? C2B1 C2B2 C2B3 121.2(14) . . ? C2B1 C2B3 C2B2 118.6(13) 3 . ? C3B3 C3B1 C3B2 119.0(11) 3_565 . ? C3B3 C3B2 C3B1 120.0(12) . . ? C3B2 C3B3 C3B1 121.0(14) . 3_565 ? _diffrn_measured_fraction_theta_max 0.864 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.864 _refine_diff_density_max 1.482 _refine_diff_density_min -0.620 _refine_diff_density_rms 0.131