Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Prof Jaehong Han' _publ_contact_author_address ; Department of Biotechnology Chung-Ang University Nae-Ri 72-1 Anseong-Si Gyeonggi-Do 456-756 KOREA ; _publ_contact_author_email JAEHONGH@CAU.AC.KR _publ_section_title ; Synthesis and Structure of the MFe2(u-S)2 clusters (M=Mo or Fe) ; loop_ _publ_author_name 'Jaehong Han' D.Coucouvanis data_comp_1 _database_code_depnum_ccdc_archive 'CCDC 258776' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H30 Cl4 Fe2 Mo O7 P2 S2' _chemical_formula_weight 881.96 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 15.17260(10) _cell_length_b 14.1221(2) _cell_length_c 30.99230(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6640.69(11) _cell_formula_units_Z 8 _cell_measurement_temperature 158(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.44 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.764 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3536 _exptl_absorpt_coefficient_mu 1.816 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 158(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 65299 _diffrn_reflns_av_R_equivalents 0.0287 _diffrn_reflns_av_sigmaI/netI 0.0172 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 2.37 _diffrn_reflns_theta_max 29.32 _reflns_number_total 8569 _reflns_number_gt 7899 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.0240P)^2^+12.6255P] 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 8569 _refine_ls_number_parameters 361 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0384 _refine_ls_R_factor_gt 0.0339 _refine_ls_wR_factor_ref 0.0777 _refine_ls_wR_factor_gt 0.0754 _refine_ls_goodness_of_fit_ref 1.170 _refine_ls_restrained_S_all 1.170 _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 Mo1 Mo 0.151146(13) 0.311796(14) 0.406399(6) 0.01724(5) Uani 1 1 d . . . Fe1 Fe 0.27658(2) 0.25400(2) 0.331711(11) 0.01656(7) Uani 1 1 d . . . Fe2 Fe 0.33402(2) 0.31189(2) 0.405693(11) 0.01849(8) Uani 1 1 d . . . S1 S 0.24582(4) 0.39838(4) 0.361425(19) 0.01788(11) Uani 1 1 d . . . S2 S 0.24818(4) 0.18437(4) 0.396815(19) 0.01923(11) Uani 1 1 d . . . Cl1 Cl -0.09631(5) 0.07601(5) 0.41047(3) 0.03485(15) Uani 1 1 d . . . Cl2 Cl -0.27789(4) 0.17085(5) 0.38544(2) 0.03388(15) Uani 1 1 d . . . Cl3 Cl -0.28084(4) 0.37965(5) 0.35069(2) 0.03219(15) Uani 1 1 d . . . Cl4 Cl -0.10003(4) 0.49022(4) 0.33891(2) 0.02537(12) Uani 1 1 d . . . P1 P 0.16780(4) 0.19969(4) 0.28946(2) 0.01786(12) Uani 1 1 d . . . P2 P 0.41625(4) 0.21892(5) 0.44955(2) 0.02419(14) Uani 1 1 d . . . O1 O 0.14784(12) 0.35266(14) 0.45756(6) 0.0275(4) Uani 1 1 d . . . O2 O 0.05617(12) 0.21106(13) 0.40274(6) 0.0231(4) Uani 1 1 d . . . O3 O 0.05378(11) 0.38290(12) 0.37511(6) 0.0200(3) Uani 1 1 d . . . O4 O 0.35453(16) 0.35680(17) 0.25923(7) 0.0424(5) Uani 1 1 d . . . O5 O 0.39944(16) 0.09736(17) 0.31759(7) 0.0443(6) Uani 1 1 d . . . O6 O 0.33233(16) 0.46236(18) 0.47151(9) 0.0503(7) Uani 1 1 d . . . O7 O 0.49226(14) 0.35943(19) 0.35572(8) 0.0452(6) Uani 1 1 d . . . C1 C -0.02344(15) 0.24468(17) 0.39135(8) 0.0192(4) Uani 1 1 d . . . C2 C -0.10085(17) 0.19187(18) 0.39265(8) 0.0223(5) Uani 1 1 d . . . C3 C -0.18086(16) 0.23390(18) 0.37991(8) 0.0222(5) Uani 1 1 d . . . C4 C -0.18180(16) 0.32655(19) 0.36454(8) 0.0218(5) Uani 1 1 d . . . C5 C -0.10313(15) 0.37818(17) 0.36132(7) 0.0187(4) Uani 1 1 d . . . C6 C -0.02471(15) 0.33836(17) 0.37606(7) 0.0181(4) Uani 1 1 d . . . C7 C 0.32339(18) 0.31773(19) 0.28779(9) 0.0258(5) Uani 1 1 d . . . C8 C 0.34903(18) 0.1566(2) 0.32260(8) 0.0270(5) Uani 1 1 d . . . C9 C 0.33418(18) 0.4026(2) 0.44656(10) 0.0318(6) Uani 1 1 d . . . C10 C 0.43101(17) 0.3401(2) 0.37556(9) 0.0288(6) Uani 1 1 d . . . C11 C 0.19913(18) 0.17004(19) 0.23382(8) 0.0261(5) Uani 1 1 d . . . H11A H 0.1461 0.1461 0.2187 0.031 Uiso 1 1 calc R . . H11B H 0.2174 0.2291 0.2191 0.031 Uiso 1 1 calc R . . C12 C 0.2725(2) 0.0974(2) 0.22841(10) 0.0389(7) Uani 1 1 d . . . H12A H 0.2840 0.0874 0.1976 0.047 Uiso 1 1 calc R . . H12B H 0.2546 0.0374 0.2417 0.047 Uiso 1 1 calc R . . H12C H 0.3262 0.1206 0.2425 0.047 Uiso 1 1 calc R . . C13 C 0.07550(17) 0.28070(19) 0.27946(8) 0.0251(5) Uani 1 1 d . . . H13A H 0.0375 0.2530 0.2568 0.030 Uiso 1 1 calc R . . H13B H 0.0398 0.2853 0.3061 0.030 Uiso 1 1 calc R . . C14 C 0.1018(2) 0.3801(2) 0.26563(10) 0.0346(6) Uani 1 1 d . . . H14A H 0.0487 0.4183 0.2610 0.041 Uiso 1 1 calc R . . H14B H 0.1357 0.3768 0.2387 0.041 Uiso 1 1 calc R . . H14C H 0.1380 0.4092 0.2882 0.041 Uiso 1 1 calc R . . C15 C 0.11584(19) 0.09256(19) 0.31115(9) 0.0278(5) Uani 1 1 d . . . H15A H 0.1592 0.0402 0.3098 0.033 Uiso 1 1 calc R . . H15B H 0.1019 0.1036 0.3419 0.033 Uiso 1 1 calc R . . C16 C 0.0317(2) 0.0606(3) 0.28832(12) 0.0487(9) Uani 1 1 d . . . H16A H 0.0090 0.0032 0.3022 0.058 Uiso 1 1 calc R . . H16B H 0.0447 0.0471 0.2580 0.058 Uiso 1 1 calc R . . H16C H -0.0127 0.1108 0.2901 0.058 Uiso 1 1 calc R . . C17 C 0.3543(2) 0.1397(3) 0.48762(11) 0.0429(8) Uani 1 1 d . . . H17A H 0.3266 0.0882 0.4707 0.051 Uiso 1 1 calc R . . H17B H 0.3970 0.1102 0.5077 0.051 Uiso 1 1 calc R . . C18 C 0.2854(2) 0.1869(4) 0.51329(11) 0.0589(12) Uani 1 1 d . . . H18A H 0.2562 0.1402 0.5318 0.071 Uiso 1 1 calc R . . H18B H 0.2419 0.2155 0.4939 0.071 Uiso 1 1 calc R . . H18C H 0.3122 0.2363 0.5312 0.071 Uiso 1 1 calc R . . C19 C 0.4829(2) 0.1334(2) 0.42003(9) 0.0334(6) Uani 1 1 d . . . H19A H 0.4434 0.0965 0.4009 0.040 Uiso 1 1 calc R . . H19B H 0.5243 0.1686 0.4013 0.040 Uiso 1 1 calc R . . C20 C 0.5363(2) 0.0634(2) 0.44742(9) 0.0359(7) Uani 1 1 d . . . H20A H 0.5698 0.0213 0.4284 0.043 Uiso 1 1 calc R . . H20B H 0.4961 0.0259 0.4653 0.043 Uiso 1 1 calc R . . H20C H 0.5770 0.0985 0.4660 0.043 Uiso 1 1 calc R . . C21 C 0.4881(2) 0.2811(2) 0.48652(11) 0.0419(7) Uani 1 1 d . . . H21A H 0.4510 0.3137 0.5082 0.050 Uiso 1 1 calc R . . H21B H 0.5243 0.2338 0.5020 0.050 Uiso 1 1 calc R . . C22 C 0.5497(2) 0.3539(3) 0.46645(14) 0.0601(11) Uani 1 1 d . . . H22A H 0.5856 0.3832 0.4891 0.072 Uiso 1 1 calc R . . H22B H 0.5150 0.4027 0.4518 0.072 Uiso 1 1 calc R . . H22C H 0.5884 0.3225 0.4455 0.072 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 Mo1 0.01545(9) 0.02007(10) 0.01620(10) -0.00067(7) 0.00014(7) 0.00066(7) Fe1 0.01577(15) 0.01841(16) 0.01550(15) -0.00124(12) -0.00199(11) 0.00165(12) Fe2 0.01604(15) 0.02180(17) 0.01764(16) -0.00212(13) -0.00401(12) 0.00101(13) S1 0.0155(2) 0.0173(2) 0.0209(3) 0.0000(2) -0.0010(2) 0.0000(2) S2 0.0184(3) 0.0198(3) 0.0194(3) 0.0019(2) -0.0028(2) 0.0016(2) Cl1 0.0353(4) 0.0238(3) 0.0454(4) 0.0066(3) -0.0029(3) -0.0081(3) Cl2 0.0224(3) 0.0419(4) 0.0374(4) -0.0004(3) -0.0006(3) -0.0138(3) Cl3 0.0171(3) 0.0401(4) 0.0394(4) -0.0024(3) -0.0055(2) 0.0029(3) Cl4 0.0245(3) 0.0230(3) 0.0286(3) 0.0025(2) -0.0035(2) 0.0030(2) P1 0.0196(3) 0.0166(3) 0.0173(3) -0.0010(2) -0.0047(2) 0.0017(2) P2 0.0246(3) 0.0313(3) 0.0167(3) -0.0025(2) -0.0061(2) 0.0069(3) O1 0.0265(9) 0.0348(10) 0.0214(9) -0.0045(8) 0.0027(7) 0.0012(8) O2 0.0191(8) 0.0219(8) 0.0283(9) 0.0038(7) -0.0015(7) -0.0003(7) O3 0.0148(7) 0.0196(8) 0.0256(9) 0.0004(7) -0.0008(6) -0.0006(6) O4 0.0475(13) 0.0468(13) 0.0329(12) 0.0052(10) 0.0131(10) -0.0095(11) O5 0.0470(13) 0.0509(13) 0.0349(12) -0.0145(10) -0.0142(10) 0.0307(11) O6 0.0469(14) 0.0466(14) 0.0574(16) -0.0305(12) -0.0197(12) 0.0088(11) O7 0.0227(10) 0.0689(17) 0.0441(13) 0.0172(12) 0.0006(9) -0.0070(10) C1 0.0191(11) 0.0199(11) 0.0186(11) -0.0016(9) 0.0013(8) -0.0008(9) C2 0.0241(12) 0.0219(11) 0.0209(11) -0.0005(9) 0.0012(9) -0.0047(9) C3 0.0173(10) 0.0279(12) 0.0212(11) -0.0052(9) 0.0010(9) -0.0073(9) C4 0.0164(10) 0.0302(13) 0.0189(11) -0.0050(9) -0.0010(8) 0.0008(9) C5 0.0188(10) 0.0208(11) 0.0165(10) -0.0026(8) 0.0004(8) 0.0003(9) C6 0.0175(10) 0.0198(11) 0.0169(10) -0.0020(8) 0.0015(8) -0.0009(8) C7 0.0247(12) 0.0279(13) 0.0249(12) -0.0042(10) 0.0004(10) -0.0008(10) C8 0.0274(13) 0.0339(14) 0.0199(12) -0.0041(10) -0.0069(10) 0.0069(11) C9 0.0258(13) 0.0342(14) 0.0355(15) -0.0081(12) -0.0116(11) 0.0058(11) C10 0.0207(12) 0.0359(14) 0.0299(13) 0.0058(11) -0.0080(10) -0.0013(11) C11 0.0291(13) 0.0297(13) 0.0196(11) -0.0051(10) -0.0048(10) 0.0063(11) C12 0.0385(16) 0.0501(18) 0.0280(14) -0.0149(13) -0.0062(12) 0.0180(14) C13 0.0230(12) 0.0290(13) 0.0233(12) -0.0023(10) -0.0051(9) 0.0074(10) C14 0.0450(17) 0.0273(13) 0.0313(14) 0.0040(11) -0.0075(12) 0.0126(12) C15 0.0352(14) 0.0232(12) 0.0249(13) 0.0013(10) -0.0081(11) -0.0063(11) C16 0.055(2) 0.0475(19) 0.0438(19) 0.0078(15) -0.0207(16) -0.0307(17) C17 0.0394(17) 0.057(2) 0.0328(16) 0.0144(15) -0.0051(13) 0.0006(15) C18 0.0398(18) 0.108(4) 0.0294(17) 0.015(2) -0.0003(14) -0.013(2) C19 0.0419(16) 0.0367(15) 0.0215(13) -0.0019(11) -0.0052(11) 0.0159(13) C20 0.0460(17) 0.0382(16) 0.0234(13) 0.0004(11) -0.0049(12) 0.0188(14) C21 0.0390(17) 0.0449(18) 0.0416(18) -0.0083(14) -0.0168(14) 0.0078(14) C22 0.0307(17) 0.082(3) 0.068(3) 0.015(2) -0.0205(17) -0.0153(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 O1 1.6882(19) . ? Mo1 O2 2.0282(18) . ? Mo1 O3 2.0325(17) . ? Mo1 S2 2.3440(6) . ? Mo1 S1 2.3455(6) . ? Mo1 Fe2 2.7747(4) . ? Fe1 C7 1.780(3) . ? Fe1 C8 1.783(3) . ? Fe1 P1 2.2420(7) . ? Fe1 S1 2.2854(7) . ? Fe1 S2 2.2856(7) . ? Fe1 Fe2 2.5856(5) . ? Fe2 C10 1.788(3) . ? Fe2 C9 1.801(3) . ? Fe2 S2 2.2394(7) . ? Fe2 P2 2.2645(7) . ? Fe2 S1 2.2726(7) . ? Cl1 C2 1.728(3) . ? Cl2 C3 1.729(2) . ? Cl3 C4 1.733(3) . ? Cl4 C5 1.729(2) . ? P1 C15 1.834(3) . ? P1 C13 1.835(3) . ? P1 C11 1.837(3) . ? P2 C21 1.809(3) . ? P2 C19 1.822(3) . ? P2 C17 1.878(3) . ? O2 C1 1.345(3) . ? O3 C6 1.347(3) . ? O4 C7 1.145(3) . ? O5 C8 1.145(3) . ? O6 C9 1.145(4) . ? O7 C10 1.147(3) . ? C1 C2 1.392(3) . ? C1 C6 1.405(3) . ? C2 C3 1.408(4) . ? C3 C4 1.393(4) . ? C4 C5 1.402(3) . ? C5 C6 1.393(3) . ? C11 C12 1.524(4) . ? C13 C14 1.521(4) . ? C15 C16 1.528(4) . ? C17 C18 1.473(5) . ? C19 C20 1.533(4) . ? C21 C22 1.522(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Mo1 O2 105.73(8) . . ? O1 Mo1 O3 104.94(8) . . ? O2 Mo1 O3 78.66(7) . . ? O1 Mo1 S2 113.58(7) . . ? O2 Mo1 S2 84.30(5) . . ? O3 Mo1 S2 140.84(5) . . ? O1 Mo1 S1 113.46(7) . . ? O2 Mo1 S1 140.14(5) . . ? O3 Mo1 S1 84.49(5) . . ? S2 Mo1 S1 86.57(2) . . ? O1 Mo1 Fe2 92.12(6) . . ? O2 Mo1 Fe2 135.27(5) . . ? O3 Mo1 Fe2 136.28(5) . . ? S2 Mo1 Fe2 51.044(17) . . ? S1 Mo1 Fe2 51.876(16) . . ? C7 Fe1 C8 91.31(13) . . ? C7 Fe1 P1 91.15(9) . . ? C8 Fe1 P1 95.60(9) . . ? C7 Fe1 S1 86.47(9) . . ? C8 Fe1 S1 151.37(9) . . ? P1 Fe1 S1 112.97(2) . . ? C7 Fe1 S2 165.47(9) . . ? C8 Fe1 S2 85.65(9) . . ? P1 Fe1 S2 103.28(3) . . ? S1 Fe1 S2 89.41(2) . . ? C7 Fe1 Fe2 112.57(9) . . ? C8 Fe1 Fe2 100.16(8) . . ? P1 Fe1 Fe2 150.95(2) . . ? S1 Fe1 Fe2 55.207(18) . . ? S2 Fe1 Fe2 54.318(18) . . ? C10 Fe2 C9 101.99(14) . . ? C10 Fe2 S2 126.42(10) . . ? C9 Fe2 S2 131.22(10) . . ? C10 Fe2 P2 89.39(9) . . ? C9 Fe2 P2 89.40(9) . . ? S2 Fe2 P2 85.86(3) . . ? C10 Fe2 S1 92.84(9) . . ? C9 Fe2 S1 92.47(9) . . ? S2 Fe2 S1 90.89(2) . . ? P2 Fe2 S1 176.74(3) . . ? C10 Fe2 Fe1 83.38(9) . . ? C9 Fe2 Fe1 148.08(9) . . ? S2 Fe2 Fe1 55.996(18) . . ? P2 Fe2 Fe1 122.32(2) . . ? S1 Fe2 Fe1 55.674(18) . . ? C10 Fe2 Mo1 145.82(8) . . ? C9 Fe2 Mo1 89.78(9) . . ? S2 Fe2 Mo1 54.484(17) . . ? P2 Fe2 Mo1 123.09(2) . . ? S1 Fe2 Mo1 54.283(16) . . ? Fe1 Fe2 Mo1 70.718(12) . . ? Fe2 S1 Fe1 69.12(2) . . ? Fe2 S1 Mo1 73.84(2) . . ? Fe1 S1 Mo1 84.23(2) . . ? Fe2 S2 Fe1 69.69(2) . . ? Fe2 S2 Mo1 74.47(2) . . ? Fe1 S2 Mo1 84.26(2) . . ? C15 P1 C13 104.37(13) . . ? C15 P1 C11 105.50(13) . . ? C13 P1 C11 100.43(12) . . ? C15 P1 Fe1 112.62(9) . . ? C13 P1 Fe1 116.57(9) . . ? C11 P1 Fe1 115.84(9) . . ? C21 P2 C19 107.80(15) . . ? C21 P2 C17 101.13(17) . . ? C19 P2 C17 101.43(16) . . ? C21 P2 Fe2 115.50(12) . . ? C19 P2 Fe2 112.89(9) . . ? C17 P2 Fe2 116.53(11) . . ? C1 O2 Mo1 113.90(15) . . ? C6 O3 Mo1 113.66(14) . . ? O2 C1 C2 124.1(2) . . ? O2 C1 C6 115.7(2) . . ? C2 C1 C6 120.2(2) . . ? C1 C2 C3 119.6(2) . . ? C1 C2 Cl1 118.9(2) . . ? C3 C2 Cl1 121.54(19) . . ? C4 C3 C2 120.1(2) . . ? C4 C3 Cl2 120.60(19) . . ? C2 C3 Cl2 119.3(2) . . ? C3 C4 C5 120.3(2) . . ? C3 C4 Cl3 120.01(19) . . ? C5 C4 Cl3 119.7(2) . . ? C6 C5 C4 119.6(2) . . ? C6 C5 Cl4 118.56(18) . . ? C4 C5 Cl4 121.85(19) . . ? O3 C6 C5 124.0(2) . . ? O3 C6 C1 115.8(2) . . ? C5 C6 C1 120.2(2) . . ? O4 C7 Fe1 178.4(3) . . ? O5 C8 Fe1 176.1(3) . . ? O6 C9 Fe2 177.4(3) . . ? O7 C10 Fe2 178.6(3) . . ? C12 C11 P1 116.49(19) . . ? C14 C13 P1 115.00(19) . . ? C16 C15 P1 115.7(2) . . ? C18 C17 P2 115.2(3) . . ? C20 C19 P2 116.2(2) . . ? C22 C21 P2 116.1(3) . . ? _diffrn_measured_fraction_theta_max 0.942 _diffrn_reflns_theta_full 29.32 _diffrn_measured_fraction_theta_full 0.942 _refine_diff_density_max 1.423 _refine_diff_density_min -0.641 _refine_diff_density_rms 0.091 data_compoundII _database_code_depnum_ccdc_archive 'CCDC 258777' _audit_creation_method SHELXL-97 _chemical_name_systematic ; (Cl4-cat)Mo(O)Fe2S2(PnPR3)2(CO)4 ; _chemical_name_common (Cl4-cat)Mo(O)Fe2S2(PnPR3)2(CO)4 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H49 Cl4 Fe2 Mo O7 P2 S2' _chemical_formula_weight 1009.20 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 9.4995(4) _cell_length_b 14.0311(5) _cell_length_c 16.7235(6) _cell_angle_alpha 103.6170(10) _cell_angle_beta 100.9500(10) _cell_angle_gamma 94.6490(10) _cell_volume 2108.39(14) _cell_formula_units_Z 2 _cell_measurement_temperature 158(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour black _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.590 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1030 _exptl_absorpt_coefficient_mu 1.441 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 158(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14750 _diffrn_reflns_av_R_equivalents 0.1553 _diffrn_reflns_av_sigmaI/netI 0.2402 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.28 _diffrn_reflns_theta_max 23.27 _reflns_number_total 6035 _reflns_number_gt 2779 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART CCD' _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _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^)+(0.1793P)^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 6035 _refine_ls_number_parameters 272 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2164 _refine_ls_R_factor_gt 0.1149 _refine_ls_wR_factor_ref 0.3231 _refine_ls_wR_factor_gt 0.2684 _refine_ls_goodness_of_fit_ref 0.941 _refine_ls_restrained_S_all 0.941 _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 Mo1 Mo -0.36619(17) -0.74833(12) -0.33962(10) 0.0271(5) Uani 1 1 d . . . Fe2 Fe -0.3655(3) -0.67930(19) -0.48658(16) 0.0236(7) Uani 1 1 d . . . Fe1 Fe -0.1231(3) -0.61584(19) -0.37991(16) 0.0253(7) Uani 1 1 d . . . S2 S -0.3438(5) -0.5858(4) -0.3538(3) 0.0271(12) Uani 1 1 d . . . S1 S -0.2163(5) -0.7785(3) -0.4368(3) 0.0257(12) Uani 1 1 d . . . Cl1 Cl -0.0815(5) -0.9587(4) -0.1814(3) 0.0368(13) Uani 1 1 d . . . Cl2 Cl -0.0905(6) -0.9016(4) 0.0123(3) 0.0433(14) Uani 1 1 d . . . Cl3 Cl -0.2563(6) -0.7287(4) 0.0823(3) 0.0416(14) Uani 1 1 d . . . Cl4 Cl -0.4088(6) -0.6096(4) -0.0405(3) 0.0433(14) Uani 1 1 d . . . P2 P -0.4502(5) -0.8027(4) -0.6027(3) 0.0282(13) Uani 1 1 d . . . P1 P 0.0393(5) -0.6077(4) -0.2622(3) 0.0290(13) Uani 1 1 d . . . O1 O -0.5319(13) -0.8130(9) -0.3841(7) 0.032(3) Uiso 1 1 d . . . O2 O -0.2456(12) -0.8332(8) -0.2773(7) 0.023(3) Uiso 1 1 d . . . O3 O -0.3700(13) -0.6846(8) -0.2179(7) 0.025(3) Uiso 1 1 d . . . O4 O 0.0893(14) -0.6659(10) -0.4841(8) 0.044(4) Uani 1 1 d . . . O5 O -0.0681(15) -0.4012(10) -0.3542(8) 0.043(4) Uani 1 1 d . . . O7 O -0.2230(14) -0.5635(10) -0.5792(8) 0.039(4) Uani 1 1 d . . . O6 O -0.6351(13) -0.5951(10) -0.5197(9) 0.043(4) Uani 1 1 d . . . C1 C -0.2460(19) -0.8127(12) -0.1958(10) 0.023(4) Uiso 1 1 d . . . C2 C -0.174(2) -0.8638(13) -0.1416(11) 0.028(5) Uiso 1 1 d . . . C3 C -0.176(2) -0.8381(13) -0.0548(11) 0.026(4) Uiso 1 1 d . . . C4 C -0.251(2) -0.7597(13) -0.0230(11) 0.028(5) Uiso 1 1 d . . . C5 C -0.318(2) -0.7072(13) -0.0762(11) 0.025(4) Uiso 1 1 d . . . C6 C -0.3143(19) -0.7352(13) -0.1626(11) 0.025(4) Uiso 1 1 d . . . C7 C 0.009(2) -0.6468(15) -0.4440(13) 0.040(5) Uiso 1 1 d . . . C8 C -0.087(2) -0.4862(14) -0.3657(11) 0.027(5) Uiso 1 1 d . . . C9 C -0.532(2) -0.6286(14) -0.5079(11) 0.031(5) Uiso 1 1 d . . . C10 C -0.273(2) -0.6073(13) -0.5404(11) 0.026(4) Uiso 1 1 d . . . C11 C -0.572(2) -0.9044(14) -0.5884(13) 0.042(6) Uiso 1 1 d . . . H11A H -0.5864 -0.9614 -0.6384 0.050 Uiso 1 1 calc R . . H11B H -0.5245 -0.9260 -0.5387 0.050 Uiso 1 1 calc R . . C12 C -0.722(2) -0.8734(15) -0.5757(13) 0.043(6) Uiso 1 1 d . . . H12A H -0.7075 -0.8128 -0.5290 0.051 Uiso 1 1 calc R . . H12B H -0.7740 -0.8586 -0.6276 0.051 Uiso 1 1 calc R . . C13 C -0.811(2) -0.9553(15) -0.5556(13) 0.050(6) Uiso 1 1 d . . . H13A H -0.9050 -0.9348 -0.5480 0.076 Uiso 1 1 calc R . . H13B H -0.7602 -0.9692 -0.5037 0.076 Uiso 1 1 calc R . . H13C H -0.8263 -1.0151 -0.6022 0.076 Uiso 1 1 calc R . . C14 C -0.556(2) -0.7588(13) -0.6867(11) 0.035(5) Uiso 1 1 d . . . H14A H -0.6393 -0.7311 -0.6665 0.042 Uiso 1 1 calc R . . H14B H -0.4952 -0.7039 -0.6967 0.042 Uiso 1 1 calc R . . C15 C -0.613(2) -0.8337(16) -0.7696(13) 0.050(6) Uiso 1 1 d . . . H15A H -0.6579 -0.8948 -0.7597 0.060 Uiso 1 1 calc R . . H15B H -0.5317 -0.8507 -0.7972 0.060 Uiso 1 1 calc R . . C16 C -0.727(2) -0.7935(16) -0.8288(13) 0.055(6) Uiso 1 1 d . . . H16A H -0.7634 -0.8445 -0.8817 0.082 Uiso 1 1 calc R . . H16B H -0.6811 -0.7346 -0.8407 0.082 Uiso 1 1 calc R . . H16C H -0.8067 -0.7762 -0.8014 0.082 Uiso 1 1 calc R . . C17 C -0.315(2) -0.8691(14) -0.6495(12) 0.039(5) Uiso 1 1 d . . . H17A H -0.2585 -0.8983 -0.6076 0.047 Uiso 1 1 calc R . . H17B H -0.3654 -0.9238 -0.6983 0.047 Uiso 1 1 calc R . . C18 C -0.210(2) -0.7992(13) -0.6793(11) 0.031(5) Uiso 1 1 d . . . H18A H -0.2666 -0.7645 -0.7169 0.037 Uiso 1 1 calc R . . H18B H -0.1514 -0.7487 -0.6298 0.037 Uiso 1 1 calc R . . C19 C -0.108(3) -0.8601(17) -0.7268(14) 0.062(7) Uiso 1 1 d . . . H19A H -0.0426 -0.8157 -0.7445 0.092 Uiso 1 1 calc R . . H19B H -0.1664 -0.9089 -0.7766 0.092 Uiso 1 1 calc R . . H19C H -0.0522 -0.8942 -0.6895 0.092 Uiso 1 1 calc R . . C20 C -0.017(2) -0.5547(13) -0.1637(11) 0.033(5) Uiso 1 1 d . . . H20A H -0.0915 -0.6035 -0.1563 0.040 Uiso 1 1 calc R . . H20B H 0.0675 -0.5460 -0.1165 0.040 Uiso 1 1 calc R . . C21 C -0.076(2) -0.4584(14) -0.1562(12) 0.042(6) Uiso 1 1 d . . . H21A H -0.1719 -0.4686 -0.1949 0.050 Uiso 1 1 calc R . . H21B H -0.0107 -0.4116 -0.1730 0.050 Uiso 1 1 calc R . . C22 C -0.091(2) -0.4137(15) -0.0649(12) 0.046(6) Uiso 1 1 d . . . H22A H -0.1288 -0.3504 -0.0614 0.069 Uiso 1 1 calc R . . H22B H 0.0045 -0.4032 -0.0268 0.069 Uiso 1 1 calc R . . H22C H -0.1569 -0.4593 -0.0488 0.069 Uiso 1 1 calc R . . C23 C 0.2063(19) -0.5266(13) -0.2579(11) 0.027(5) Uiso 1 1 d . . . H23A H 0.2339 -0.5454 -0.3131 0.033 Uiso 1 1 calc R . . H23B H 0.1848 -0.4575 -0.2490 0.033 Uiso 1 1 calc R . . C24 C 0.333(2) -0.5307(14) -0.1904(11) 0.035(5) Uiso 1 1 d . . . H24A H 0.3614 -0.5980 -0.2017 0.042 Uiso 1 1 calc R . . H24B H 0.3043 -0.5167 -0.1352 0.042 Uiso 1 1 calc R . . C25 C 0.466(2) -0.4528(14) -0.1864(12) 0.039(5) Uiso 1 1 d . . . H25A H 0.5476 -0.4579 -0.1425 0.059 Uiso 1 1 calc R . . H25B H 0.4389 -0.3859 -0.1731 0.059 Uiso 1 1 calc R . . H25C H 0.4942 -0.4665 -0.2410 0.059 Uiso 1 1 calc R . . C26 C 0.098(2) -0.7221(13) -0.2470(11) 0.030(5) Uiso 1 1 d . . . H26A H 0.1705 -0.7071 -0.1931 0.036 Uiso 1 1 calc R . . H26B H 0.0143 -0.7644 -0.2411 0.036 Uiso 1 1 calc R . . C27 C 0.166(2) -0.7837(14) -0.3175(12) 0.041(5) Uiso 1 1 d . . . H27A H 0.0930 -0.8037 -0.3711 0.049 Uiso 1 1 calc R . . H27B H 0.2483 -0.7417 -0.3259 0.049 Uiso 1 1 calc R . . C28 C 0.220(2) -0.8757(15) -0.2959(13) 0.054(6) Uiso 1 1 d . . . H28A H 0.2611 -0.9119 -0.3416 0.081 Uiso 1 1 calc R . . H28B H 0.1387 -0.9183 -0.2885 0.081 Uiso 1 1 calc R . . H28C H 0.2940 -0.8564 -0.2435 0.081 Uiso 1 1 calc R . . C29 C 0.464(3) 0.0411(17) 0.0046(15) 0.068(8) Uiso 1 1 d . . . H29A H 0.5331 0.0973 0.0426 0.082 Uiso 1 1 calc R . . H29B H 0.3866 0.0290 0.0347 0.082 Uiso 1 1 calc R . . C30 C 0.393(3) 0.077(2) -0.0730(17) 0.097(10) Uiso 1 1 d . . . H30A H 0.4681 0.0894 -0.1042 0.116 Uiso 1 1 calc R . . H30B H 0.3198 0.0226 -0.1109 0.116 Uiso 1 1 calc R . . C31 C 0.321(3) 0.168(2) -0.0517(18) 0.102(10) Uiso 1 1 d . . . H31A H 0.2800 0.1862 -0.1036 0.153 Uiso 1 1 calc R . . H31B H 0.3932 0.2228 -0.0150 0.153 Uiso 1 1 calc R . . H31C H 0.2442 0.1559 -0.0225 0.153 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 Mo1 0.0126(10) 0.0380(11) 0.0341(11) 0.0105(8) 0.0150(8) -0.0050(8) Fe2 0.0111(15) 0.0300(16) 0.0326(16) 0.0090(13) 0.0125(12) -0.0023(12) Fe1 0.0118(15) 0.0344(17) 0.0322(17) 0.0096(13) 0.0119(13) -0.0028(13) S2 0.018(3) 0.034(3) 0.034(3) 0.009(2) 0.017(2) 0.002(2) S1 0.016(3) 0.034(3) 0.032(3) 0.011(2) 0.013(2) 0.003(2) Cl1 0.030(3) 0.038(3) 0.051(3) 0.018(3) 0.021(3) 0.004(2) Cl2 0.029(3) 0.058(4) 0.050(3) 0.022(3) 0.017(3) 0.000(3) Cl3 0.037(3) 0.059(4) 0.032(3) 0.014(3) 0.015(3) 0.001(3) Cl4 0.049(4) 0.054(4) 0.038(3) 0.016(3) 0.027(3) 0.016(3) P2 0.015(3) 0.030(3) 0.039(3) 0.006(2) 0.013(2) -0.003(2) P1 0.011(3) 0.043(3) 0.037(3) 0.015(3) 0.013(2) -0.004(2) O4 0.025(8) 0.062(10) 0.046(9) 0.007(7) 0.029(7) -0.012(7) O5 0.040(9) 0.032(9) 0.060(10) 0.019(7) 0.010(7) 0.005(7) O7 0.023(8) 0.058(9) 0.040(8) 0.028(7) 0.005(7) -0.007(7) O6 0.012(8) 0.054(10) 0.064(10) 0.024(8) 0.002(7) 0.004(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 O1 1.691(13) . ? Mo1 O3 2.029(11) . ? Mo1 O2 2.042(11) . ? Mo1 S2 2.345(5) . ? Mo1 S1 2.346(5) . ? Mo1 Fe2 2.847(3) . ? Fe2 C10 1.786(19) . ? Fe2 C9 1.79(2) . ? Fe2 P2 2.239(6) . ? Fe2 S1 2.249(5) . ? Fe2 S2 2.260(5) . ? Fe2 Fe1 2.576(4) . ? Fe1 C8 1.774(19) . ? Fe1 C7 1.81(2) . ? Fe1 P1 2.231(6) . ? Fe1 S2 2.274(5) . ? Fe1 S1 2.287(5) . ? Cl1 C2 1.729(18) . ? Cl2 C3 1.718(18) . ? Cl3 C4 1.721(18) . ? Cl4 C5 1.727(17) . ? P2 C14 1.825(18) . ? P2 C17 1.831(19) . ? P2 C11 1.85(2) . ? P1 C26 1.801(17) . ? P1 C20 1.838(18) . ? P1 C23 1.855(18) . ? O2 C1 1.326(18) . ? O3 C6 1.349(19) . ? O4 C7 1.12(2) . ? O5 C8 1.16(2) . ? O7 C10 1.13(2) . ? O6 C9 1.13(2) . ? C1 C6 1.37(2) . ? C1 C2 1.40(2) . ? C2 C3 1.41(2) . ? C3 C4 1.42(2) . ? C4 C5 1.38(2) . ? C5 C6 1.41(2) . ? C11 C12 1.56(3) . ? C12 C13 1.51(3) . ? C14 C15 1.50(2) . ? C15 C16 1.55(3) . ? C17 C18 1.57(3) . ? C18 C19 1.55(3) . ? C20 C21 1.49(2) . ? C21 C22 1.55(2) . ? C23 C24 1.50(2) . ? C24 C25 1.58(3) . ? C26 C27 1.57(2) . ? C27 C28 1.52(3) . ? C29 C29 1.38(4) 2_655 ? C29 C30 1.55(3) . ? C30 C31 1.51(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Mo1 O3 106.3(5) . . ? O1 Mo1 O2 108.2(5) . . ? O3 Mo1 O2 78.2(4) . . ? O1 Mo1 S2 114.0(4) . . ? O3 Mo1 S2 85.0(3) . . ? O2 Mo1 S2 137.5(4) . . ? O1 Mo1 S1 109.2(4) . . ? O3 Mo1 S1 144.2(4) . . ? O2 Mo1 S1 86.0(3) . . ? S2 Mo1 S1 85.36(16) . . ? O1 Mo1 Fe2 90.3(4) . . ? O3 Mo1 Fe2 135.2(3) . . ? O2 Mo1 Fe2 136.1(3) . . ? S2 Mo1 Fe2 50.47(13) . . ? S1 Mo1 Fe2 50.20(13) . . ? C10 Fe2 C9 94.4(8) . . ? C10 Fe2 P2 93.4(6) . . ? C9 Fe2 P2 88.6(6) . . ? C10 Fe2 S1 109.1(6) . . ? C9 Fe2 S1 156.4(6) . . ? P2 Fe2 S1 88.7(2) . . ? C10 Fe2 S2 107.1(6) . . ? C9 Fe2 S2 84.5(6) . . ? P2 Fe2 S2 158.8(2) . . ? S1 Fe2 S2 89.71(19) . . ? C10 Fe2 Fe1 78.4(6) . . ? C9 Fe2 Fe1 133.7(6) . . ? P2 Fe2 Fe1 137.04(17) . . ? S1 Fe2 Fe1 56.08(15) . . ? S2 Fe2 Fe1 55.62(14) . . ? C10 Fe2 Mo1 148.3(6) . . ? C9 Fe2 Mo1 106.3(6) . . ? P2 Fe2 Mo1 110.42(16) . . ? S1 Fe2 Mo1 53.27(13) . . ? S2 Fe2 Mo1 53.18(13) . . ? Fe1 Fe2 Mo1 70.02(9) . . ? C8 Fe1 C7 95.2(9) . . ? C8 Fe1 P1 91.1(6) . . ? C7 Fe1 P1 91.6(7) . . ? C8 Fe1 S2 85.7(6) . . ? C7 Fe1 S2 156.3(7) . . ? P1 Fe1 S2 112.1(2) . . ? C8 Fe1 S1 161.7(6) . . ? C7 Fe1 S1 83.4(7) . . ? P1 Fe1 S1 107.3(2) . . ? S2 Fe1 S1 88.42(19) . . ? C8 Fe1 Fe2 108.3(6) . . ? C7 Fe1 Fe2 102.7(7) . . ? P1 Fe1 Fe2 154.50(18) . . ? S2 Fe1 Fe2 55.11(15) . . ? S1 Fe1 Fe2 54.70(14) . . ? Fe2 S2 Fe1 69.27(15) . . ? Fe2 S2 Mo1 76.35(16) . . ? Fe1 S2 Mo1 84.94(17) . . ? Fe2 S1 Fe1 69.23(16) . . ? Fe2 S1 Mo1 76.53(15) . . ? Fe1 S1 Mo1 84.63(17) . . ? C14 P2 C17 105.7(9) . . ? C14 P2 C11 105.2(9) . . ? C17 P2 C11 102.1(9) . . ? C14 P2 Fe2 111.4(6) . . ? C17 P2 Fe2 116.5(7) . . ? C11 P2 Fe2 114.7(7) . . ? C26 P1 C20 103.1(8) . . ? C26 P1 C23 105.4(8) . . ? C20 P1 C23 104.8(9) . . ? C26 P1 Fe1 117.1(6) . . ? C20 P1 Fe1 115.2(6) . . ? C23 P1 Fe1 110.0(6) . . ? C1 O2 Mo1 113.1(10) . . ? C6 O3 Mo1 114.5(10) . . ? O2 C1 C6 118.5(15) . . ? O2 C1 C2 122.8(15) . . ? C6 C1 C2 118.6(16) . . ? C1 C2 C3 120.7(16) . . ? C1 C2 Cl1 119.4(13) . . ? C3 C2 Cl1 119.9(13) . . ? C2 C3 C4 119.3(16) . . ? C2 C3 Cl2 121.2(13) . . ? C4 C3 Cl2 119.5(14) . . ? C5 C4 C3 119.7(16) . . ? C5 C4 Cl3 120.4(14) . . ? C3 C4 Cl3 119.8(14) . . ? C4 C5 C6 119.3(16) . . ? C4 C5 Cl4 121.8(14) . . ? C6 C5 Cl4 118.9(13) . . ? O3 C6 C1 114.7(15) . . ? O3 C6 C5 123.0(15) . . ? C1 C6 C5 122.2(16) . . ? O4 C7 Fe1 180(2) . . ? O5 C8 Fe1 176.9(17) . . ? O6 C9 Fe2 178.4(19) . . ? O7 C10 Fe2 174.9(17) . . ? C12 C11 P2 112.5(14) . . ? C13 C12 C11 110.5(17) . . ? C15 C14 P2 116.7(13) . . ? C14 C15 C16 111.4(17) . . ? C18 C17 P2 111.9(13) . . ? C19 C18 C17 110.2(16) . . ? C21 C20 P1 117.0(13) . . ? C20 C21 C22 110.9(15) . . ? C24 C23 P1 114.6(12) . . ? C23 C24 C25 111.1(15) . . ? C27 C26 P1 116.9(12) . . ? C28 C27 C26 112.3(16) . . ? C29 C29 C30 121(3) 2_655 . ? C31 C30 C29 114(2) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 23.27 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 2.556 _refine_diff_density_min -2.418 _refine_diff_density_rms 0.313 #===END data_comp_3 _database_code_depnum_ccdc_archive 'CCDC 258778' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H30 Cl8 Fe4 Mo2 O16 P2 S4' _chemical_formula_weight 1583.64 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' 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.0059(5) _cell_length_b 16.1615(6) _cell_length_c 14.0452(5) _cell_angle_alpha 90.00 _cell_angle_beta 103.9990(10) _cell_angle_gamma 90.00 _cell_volume 2644.30(18) _cell_formula_units_Z 2 _cell_measurement_temperature 158(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description rhombic _exptl_crystal_colour brown _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.989 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1560 _exptl_absorpt_coefficient_mu 2.213 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 158(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21176 _diffrn_reflns_av_R_equivalents 0.1013 _diffrn_reflns_av_sigmaI/netI 0.0818 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.37 _diffrn_reflns_theta_max 24.71 _reflns_number_total 4468 _reflns_number_gt 3067 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.0713P)^2^+5.6268P] 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 4468 _refine_ls_number_parameters 316 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1121 _refine_ls_R_factor_gt 0.0704 _refine_ls_wR_factor_ref 0.1602 _refine_ls_wR_factor_gt 0.1422 _refine_ls_goodness_of_fit_ref 1.111 _refine_ls_restrained_S_all 1.111 _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 Mo1 Mo 0.90364(7) 0.05310(5) 0.77159(6) 0.0291(2) Uani 1 1 d . . . Fe1 Fe 0.88028(11) -0.12597(8) 0.72897(10) 0.0300(3) Uani 1 1 d . . . Fe2 Fe 1.08367(11) -0.06006(8) 0.77773(9) 0.0284(3) Uani 1 1 d . . . Cl1 Cl 0.5796(2) 0.18289(15) 0.51631(17) 0.0410(6) Uani 1 1 d . . . Cl2 Cl 0.3823(2) 0.24708(15) 0.61092(18) 0.0413(6) Uani 1 1 d . . . Cl3 Cl 0.3853(2) 0.19778(16) 0.82899(18) 0.0427(6) Uani 1 1 d . . . Cl4 Cl 0.5971(2) 0.09838(16) 0.95555(18) 0.0424(6) Uani 1 1 d . . . S1 S 0.9597(2) -0.06078(14) 0.87607(16) 0.0295(5) Uani 1 1 d . . . S2 S 0.95029(19) -0.02374(14) 0.64584(16) 0.0295(5) Uani 1 1 d . . . P1 P 1.2005(2) -0.07123(14) 0.67142(17) 0.0287(6) Uani 1 1 d . . . O1 O 0.9951(5) 0.1337(4) 0.8039(5) 0.0356(16) Uani 1 1 d . . . O2 O 0.7695(5) 0.0962(4) 0.6644(4) 0.0311(14) Uani 1 1 d . . . O3 O 0.7779(5) 0.0651(4) 0.8459(4) 0.0324(15) Uani 1 1 d . . . O4 O 0.8987(6) -0.2772(4) 0.8511(5) 0.0483(18) Uani 1 1 d . . . O5 O 0.8582(6) -0.2291(4) 0.5532(5) 0.0470(18) Uani 1 1 d . . . O6 O 0.6327(6) -0.0888(4) 0.6953(6) 0.0506(19) Uani 1 1 d . . . O7 O 1.1790(6) -0.2181(4) 0.8668(5) 0.0437(17) Uani 1 1 d . . . O8 O 1.2339(6) 0.0585(4) 0.9079(5) 0.0520(19) Uani 1 1 d . . . C1 C 0.6778(7) 0.1235(5) 0.6955(7) 0.028(2) Uani 1 1 d . . . C2 C 0.5859(7) 0.1639(5) 0.6386(6) 0.028(2) Uani 1 1 d . . . C3 C 0.4948(8) 0.1892(5) 0.6800(7) 0.031(2) Uani 1 1 d . . . C4 C 0.5003(7) 0.1715(5) 0.7786(6) 0.027(2) Uani 1 1 d . . . C5 C 0.5938(8) 0.1267(5) 0.8369(7) 0.031(2) Uani 1 1 d . . . C6 C 0.6829(7) 0.1051(5) 0.7960(7) 0.029(2) Uani 1 1 d . . . C8 C 0.8914(8) -0.2197(6) 0.8039(7) 0.037(2) Uani 1 1 d . . . C7 C 0.8677(8) -0.1876(6) 0.6198(7) 0.033(2) Uani 1 1 d . . . C9 C 0.7265(9) -0.1036(6) 0.7086(7) 0.037(2) Uani 1 1 d . . . C10 C 1.1439(8) -0.1573(6) 0.8317(7) 0.034(2) Uani 1 1 d . . . C11 C 1.1801(9) 0.0111(7) 0.8539(8) 0.043(3) Uani 1 1 d . . . C12 C 1.1453(8) -0.1378(5) 0.5642(6) 0.029(2) Uani 1 1 d . . . H12A H 1.0665 -0.1198 0.5317 0.035 Uiso 1 1 calc R . . H12B H 1.1936 -0.1299 0.5169 0.035 Uiso 1 1 calc R . . C13 C 1.1429(9) -0.2292(5) 0.5883(7) 0.037(2) Uani 1 1 d . . . H13A H 1.1125 -0.2606 0.5278 0.045 Uiso 1 1 calc R . . H13B H 1.0938 -0.2380 0.6338 0.045 Uiso 1 1 calc R . . H13C H 1.2210 -0.2482 0.6187 0.045 Uiso 1 1 calc R . . C14 C 1.2284(8) 0.0299(5) 0.6200(6) 0.031(2) Uani 1 1 d . . . H14A H 1.1547 0.0522 0.5808 0.038 Uiso 1 1 calc R . . H14B H 1.2573 0.0687 0.6750 0.038 Uiso 1 1 calc R . . C15 C 1.3141(8) 0.0280(6) 0.5553(7) 0.038(2) Uani 1 1 d . . . H15A H 1.3236 0.0840 0.5315 0.046 Uiso 1 1 calc R . . H15B H 1.2854 -0.0088 0.4992 0.046 Uiso 1 1 calc R . . H15C H 1.3883 0.0076 0.5936 0.046 Uiso 1 1 calc R . . C16 C 1.3418(8) -0.1143(6) 0.7245(7) 0.035(2) Uani 1 1 d . . . H16A H 1.3318 -0.1688 0.7534 0.042 Uiso 1 1 calc R . . H16B H 1.3810 -0.1237 0.6711 0.042 Uiso 1 1 calc R . . C17 C 1.4194(8) -0.0617(7) 0.8029(7) 0.047(3) Uani 1 1 d . . . H17A H 1.4931 -0.0899 0.8269 0.056 Uiso 1 1 calc R . . H17B H 1.3829 -0.0532 0.8575 0.056 Uiso 1 1 calc R . . H17C H 1.4323 -0.0080 0.7749 0.056 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 Mo1 0.0275(5) 0.0176(4) 0.0416(5) 0.0011(4) 0.0075(4) 0.0033(3) Fe1 0.0308(8) 0.0213(7) 0.0377(8) 0.0004(6) 0.0080(6) 0.0015(6) Fe2 0.0264(7) 0.0214(7) 0.0369(8) 0.0030(6) 0.0067(6) 0.0031(6) Cl1 0.0404(15) 0.0377(14) 0.0431(14) 0.0080(11) 0.0066(12) 0.0092(11) Cl2 0.0345(14) 0.0311(13) 0.0536(16) 0.0019(12) 0.0013(12) 0.0099(11) Cl3 0.0333(14) 0.0415(15) 0.0539(16) -0.0088(12) 0.0116(12) 0.0063(12) Cl4 0.0419(15) 0.0424(15) 0.0427(15) 0.0007(12) 0.0096(12) 0.0061(12) S1 0.0308(13) 0.0237(12) 0.0338(12) 0.0019(10) 0.0074(10) 0.0028(10) S2 0.0302(13) 0.0212(12) 0.0360(13) 0.0038(10) 0.0060(11) 0.0045(10) P1 0.0309(14) 0.0180(12) 0.0362(13) 0.0050(10) 0.0060(11) 0.0034(10) O1 0.026(4) 0.022(3) 0.056(4) -0.006(3) 0.006(3) 0.002(3) O2 0.030(4) 0.024(3) 0.038(4) 0.004(3) 0.006(3) 0.003(3) O3 0.034(4) 0.022(3) 0.041(4) -0.003(3) 0.009(3) 0.001(3) O4 0.068(5) 0.028(4) 0.051(4) 0.009(4) 0.018(4) -0.003(4) O5 0.047(5) 0.040(4) 0.048(4) -0.007(4) 0.000(4) 0.004(4) O6 0.030(4) 0.037(4) 0.082(6) -0.005(4) 0.011(4) 0.000(3) O7 0.039(4) 0.036(4) 0.055(4) 0.017(4) 0.010(3) 0.007(3) O8 0.048(5) 0.040(4) 0.063(5) -0.006(4) 0.004(4) 0.000(4) C1 0.020(5) 0.018(4) 0.045(6) -0.006(4) 0.006(4) -0.005(4) C2 0.025(5) 0.019(5) 0.039(5) 0.001(4) 0.005(4) -0.004(4) C3 0.031(5) 0.011(4) 0.045(6) -0.006(4) -0.003(4) -0.003(4) C4 0.020(5) 0.024(5) 0.034(5) -0.003(4) -0.003(4) 0.002(4) C5 0.032(5) 0.020(5) 0.040(5) -0.002(4) 0.010(4) 0.000(4) C6 0.018(5) 0.019(5) 0.047(6) 0.002(4) 0.000(4) -0.003(4) C8 0.037(6) 0.034(6) 0.038(6) -0.005(5) 0.008(5) 0.000(5) C7 0.035(6) 0.024(5) 0.042(6) 0.002(5) 0.011(5) -0.002(4) C9 0.041(7) 0.021(5) 0.050(6) 0.007(4) 0.013(5) 0.000(5) C10 0.036(6) 0.037(6) 0.034(5) 0.007(5) 0.017(5) 0.006(5) C11 0.042(7) 0.035(6) 0.053(7) 0.001(5) 0.015(5) 0.012(5) C12 0.033(6) 0.020(5) 0.037(5) 0.002(4) 0.012(4) -0.001(4) C13 0.052(7) 0.013(5) 0.047(6) -0.002(4) 0.013(5) 0.003(4) C14 0.037(6) 0.022(5) 0.030(5) 0.000(4) -0.001(4) -0.003(4) C15 0.041(6) 0.024(5) 0.050(6) 0.005(5) 0.012(5) 0.001(4) C16 0.039(6) 0.025(5) 0.038(6) 0.007(4) 0.003(5) 0.009(4) C17 0.037(6) 0.053(7) 0.046(6) 0.004(5) 0.001(5) 0.012(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 Mo1 O1 1.694(6) . ? Mo1 O3 2.042(6) . ? Mo1 O2 2.042(6) . ? Mo1 S2 2.335(2) . ? Mo1 S1 2.349(2) . ? Mo1 Fe2 2.8166(14) . ? Mo1 Fe1 2.9547(15) . ? Fe1 C7 1.804(10) . ? Fe1 C8 1.832(11) . ? Fe1 C9 1.834(11) . ? Fe1 S2 2.297(3) . ? Fe1 S1 2.310(3) . ? Fe1 Fe2 2.5995(18) . ? Fe2 C11 1.791(12) . ? Fe2 C10 1.817(10) . ? Fe2 S2 2.215(3) . ? Fe2 S1 2.262(2) . ? Fe2 P1 2.290(3) . ? Cl1 C2 1.728(9) . ? Cl2 C3 1.735(9) . ? Cl3 C4 1.749(9) . ? Cl4 C5 1.719(9) . ? P1 C16 1.818(9) . ? P1 C12 1.839(9) . ? P1 C14 1.850(9) . ? O2 C1 1.353(10) . ? O3 C6 1.349(10) . ? O4 C8 1.132(11) . ? O5 C7 1.134(10) . ? O6 C9 1.123(11) . ? O7 C10 1.134(10) . ? O8 C11 1.158(12) . ? C1 C2 1.362(12) . ? C1 C6 1.430(12) . ? C2 C3 1.417(12) . ? C3 C4 1.400(12) . ? C4 C5 1.417(12) . ? C5 C6 1.376(12) . ? C12 C13 1.518(11) . ? C14 C15 1.530(12) . ? C16 C17 1.518(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Mo1 O3 107.6(3) . . ? O1 Mo1 O2 106.2(3) . . ? O3 Mo1 O2 78.2(2) . . ? O1 Mo1 S2 110.7(2) . . ? O3 Mo1 S2 141.21(18) . . ? O2 Mo1 S2 85.12(17) . . ? O1 Mo1 S1 111.5(2) . . ? O3 Mo1 S1 83.74(18) . . ? O2 Mo1 S1 141.59(18) . . ? S2 Mo1 S1 88.34(8) . . ? O1 Mo1 Fe2 92.8(2) . . ? O3 Mo1 Fe2 134.68(17) . . ? O2 Mo1 Fe2 134.96(17) . . ? S2 Mo1 Fe2 49.85(6) . . ? S1 Mo1 Fe2 50.97(6) . . ? O1 Mo1 Fe1 146.2(2) . . ? O3 Mo1 Fe1 98.69(16) . . ? O2 Mo1 Fe1 99.54(17) . . ? S2 Mo1 Fe1 49.79(6) . . ? S1 Mo1 Fe1 50.05(6) . . ? Fe2 Mo1 Fe1 53.48(4) . . ? C7 Fe1 C8 90.6(4) . . ? C7 Fe1 C9 95.8(4) . . ? C8 Fe1 C9 100.6(4) . . ? C7 Fe1 S2 86.0(3) . . ? C8 Fe1 S2 154.5(3) . . ? C9 Fe1 S2 104.9(3) . . ? C7 Fe1 S1 160.7(3) . . ? C8 Fe1 S1 84.6(3) . . ? C9 Fe1 S1 103.4(3) . . ? S2 Fe1 S1 90.23(9) . . ? C7 Fe1 Fe2 109.3(3) . . ? C8 Fe1 Fe2 104.8(3) . . ? C9 Fe1 Fe2 143.7(3) . . ? S2 Fe1 Fe2 53.35(7) . . ? S1 Fe1 Fe2 54.50(7) . . ? C7 Fe1 Mo1 134.2(3) . . ? C8 Fe1 Mo1 134.7(3) . . ? C9 Fe1 Mo1 83.2(3) . . ? S2 Fe1 Mo1 50.94(6) . . ? S1 Fe1 Mo1 51.22(6) . . ? Fe2 Fe1 Mo1 60.54(4) . . ? C11 Fe2 C10 99.9(4) . . ? C11 Fe2 S2 124.2(3) . . ? C10 Fe2 S2 135.4(3) . . ? C11 Fe2 S1 93.7(3) . . ? C10 Fe2 S1 89.7(3) . . ? S2 Fe2 S1 93.59(9) . . ? C11 Fe2 P1 91.7(3) . . ? C10 Fe2 P1 87.6(3) . . ? S2 Fe2 P1 84.75(9) . . ? S1 Fe2 P1 174.29(10) . . ? C11 Fe2 Fe1 148.3(3) . . ? C10 Fe2 Fe1 90.5(3) . . ? S2 Fe2 Fe1 56.30(7) . . ? S1 Fe2 Fe1 56.21(7) . . ? P1 Fe2 Fe1 118.72(8) . . ? C11 Fe2 Mo1 89.0(3) . . ? C10 Fe2 Mo1 143.1(3) . . ? S2 Fe2 Mo1 53.70(7) . . ? S1 Fe2 Mo1 53.75(6) . . ? P1 Fe2 Mo1 128.16(8) . . ? Fe1 Fe2 Mo1 65.98(4) . . ? Fe2 S1 Fe1 69.29(8) . . ? Fe2 S1 Mo1 75.28(8) . . ? Fe1 S1 Mo1 78.73(8) . . ? Fe2 S2 Fe1 70.35(8) . . ? Fe2 S2 Mo1 76.44(8) . . ? Fe1 S2 Mo1 79.27(8) . . ? C16 P1 C12 103.2(4) . . ? C16 P1 C14 105.0(4) . . ? C12 P1 C14 105.1(4) . . ? C16 P1 Fe2 114.9(3) . . ? C12 P1 Fe2 115.1(3) . . ? C14 P1 Fe2 112.5(3) . . ? C1 O2 Mo1 115.6(5) . . ? C6 O3 Mo1 114.6(5) . . ? O2 C1 C2 125.0(8) . . ? O2 C1 C6 114.0(7) . . ? C2 C1 C6 121.0(8) . . ? C1 C2 C3 119.5(8) . . ? C1 C2 Cl1 120.2(7) . . ? C3 C2 Cl1 120.3(7) . . ? C4 C3 C2 119.4(8) . . ? C4 C3 Cl2 120.5(7) . . ? C2 C3 Cl2 120.0(7) . . ? C3 C4 C5 121.1(8) . . ? C3 C4 Cl3 119.8(7) . . ? C5 C4 Cl3 118.9(7) . . ? C6 C5 C4 118.4(8) . . ? C6 C5 Cl4 119.9(7) . . ? C4 C5 Cl4 121.7(7) . . ? O3 C6 C5 123.3(8) . . ? O3 C6 C1 116.2(7) . . ? C5 C6 C1 120.5(8) . . ? O4 C8 Fe1 179.2(9) . . ? O5 C7 Fe1 177.1(8) . . ? O6 C9 Fe1 178.9(9) . . ? O7 C10 Fe2 177.9(8) . . ? O8 C11 Fe2 173.2(9) . . ? C13 C12 P1 114.2(6) . . ? C15 C14 P1 115.2(6) . . ? C17 C16 P1 115.6(7) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 24.71 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.151 _refine_diff_density_min -1.234 _refine_diff_density_rms 0.163 data_compoundIV _database_code_depnum_ccdc_archive 'CCDC 258779' _audit_creation_method SHELXL-97 _chemical_name_systematic ; (Cl4-cat)2MoFe2S2(depe)2(CO)2 ; _chemical_name_common (Cl4-cat)2MoFe2S2(depe)2(CO)2 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C41 H63 Cl8 Fe2 Mo O7 P4 S2' _chemical_formula_weight 1347.15 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.4024(3) _cell_length_b 19.8815(5) _cell_length_c 22.3725(7) _cell_angle_alpha 90.00 _cell_angle_beta 106.3570(10) _cell_angle_gamma 90.00 _cell_volume 5293.3(2) _cell_formula_units_Z 4 _cell_measurement_temperature 178(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description rhombic _exptl_crystal_colour black _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.690 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2748 _exptl_absorpt_coefficient_mu 1.424 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 178(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 'SMART CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 47262 _diffrn_reflns_av_R_equivalents 0.0510 _diffrn_reflns_av_sigmaI/netI 0.0423 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 26.44 _reflns_number_total 10827 _reflns_number_gt 8492 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.0633P)^2^+28.9046P] 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 10827 _refine_ls_number_parameters 574 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.0831 _refine_ls_R_factor_gt 0.0621 _refine_ls_wR_factor_ref 0.1626 _refine_ls_wR_factor_gt 0.1501 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.061 _refine_ls_shift/su_max 0.019 _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 Mo1 Mo 0.09990(4) 0.54253(2) 0.31012(2) 0.02447(12) Uani 1 1 d . . . Fe1 Fe 0.06271(7) 0.39667(4) 0.28892(3) 0.02910(19) Uani 1 1 d . . . Fe2 Fe 0.23236(7) 0.44030(4) 0.37943(3) 0.02796(18) Uani 1 1 d . . . Cl1 Cl -0.01471(18) 0.61237(10) 0.08429(7) 0.0587(5) Uani 1 1 d . . . Cl2 Cl -0.27370(19) 0.64456(10) 0.03539(9) 0.0713(6) Uani 1 1 d . . . Cl3 Cl -0.42270(16) 0.63666(11) 0.12601(12) 0.0783(7) Uani 1 1 d . . . Cl4 Cl -0.31331(14) 0.59965(10) 0.26732(10) 0.0595(5) Uani 1 1 d . . . Cl5 Cl 0.44180(16) 0.68374(11) 0.31556(11) 0.0726(6) Uani 1 1 d . . . Cl6 Cl 0.48157(19) 0.79700(10) 0.41968(14) 0.0983(10) Uani 1 1 d . . . Cl7 Cl 0.3295(2) 0.80063(11) 0.50989(13) 0.1002(10) Uani 1 1 d . . . Cl8 Cl 0.1376(2) 0.69336(12) 0.49545(10) 0.0785(7) Uani 1 1 d . . . S1 S 0.20357(12) 0.45831(7) 0.27826(6) 0.0298(3) Uani 1 1 d . . . S2 S 0.05161(11) 0.45696(7) 0.36983(6) 0.0279(3) Uani 1 1 d . . . P1 P -0.11507(16) 0.36458(10) 0.27505(9) 0.0505(5) Uani 1 1 d . . . P2 P 0.02657(18) 0.37068(8) 0.18762(7) 0.0475(5) Uani 1 1 d . . . P3 P 0.38445(14) 0.37950(10) 0.37757(9) 0.0467(4) Uani 1 1 d . . . P4 P 0.24551(14) 0.38874(8) 0.47017(7) 0.0368(4) Uani 1 1 d . . . O1 O 0.0548(3) 0.57277(19) 0.22026(17) 0.0319(8) Uani 1 1 d . . . O2 O -0.0657(3) 0.5680(2) 0.29346(17) 0.0325(8) Uani 1 1 d . . . O3 O 0.2397(3) 0.5988(2) 0.31199(18) 0.0349(9) Uani 1 1 d . . . O4 O 0.1171(3) 0.6023(2) 0.38620(18) 0.0356(9) Uani 1 1 d . . . O5 O 0.1449(5) 0.2639(2) 0.3334(2) 0.0547(13) Uani 1 1 d . . . O6 O 0.3755(4) 0.5447(2) 0.4505(2) 0.0462(11) Uani 1 1 d . . . C1 C 0.1139(6) 0.3166(3) 0.3156(3) 0.0392(14) Uani 1 1 d . . . C2 C 0.3172(5) 0.5041(3) 0.4214(3) 0.0368(13) Uani 1 1 d . . . C3 C -0.0532(5) 0.5891(3) 0.1953(3) 0.0328(12) Uani 1 1 d . . . C4 C -0.1004(5) 0.6072(3) 0.1332(3) 0.0398(14) Uani 1 1 d . . . C5 C -0.2144(6) 0.6222(3) 0.1123(3) 0.0498(18) Uani 1 1 d . . . C6 C -0.2807(5) 0.6193(3) 0.1529(3) 0.0489(17) Uani 1 1 d . . . C7 C -0.2330(5) 0.6028(3) 0.2150(3) 0.0413(15) Uani 1 1 d . . . C8 C -0.1191(5) 0.5861(3) 0.2357(3) 0.0337(12) Uani 1 1 d . . . C9 C 0.2676(5) 0.6451(3) 0.3566(3) 0.0398(14) Uani 1 1 d . . . C10 C 0.3577(6) 0.6894(3) 0.3652(4) 0.0527(19) Uani 1 1 d . . . C11 C 0.3766(6) 0.7380(3) 0.4128(4) 0.063(3) Uani 1 1 d . . . C12 C 0.3095(7) 0.7395(3) 0.4524(4) 0.065(3) Uani 1 1 d . . . C13 C 0.2213(6) 0.6930(3) 0.4461(3) 0.0537(19) Uani 1 1 d . . . C14 C 0.1985(5) 0.6467(3) 0.3972(3) 0.0402(15) Uani 1 1 d . . . C15 C -0.1154(9) 0.3281(5) 0.1612(4) 0.087(3) Uani 1 1 d . . . H15A H -0.1718 0.3606 0.1375 0.105 Uiso 1 1 calc R . . H15B H -0.1115 0.2903 0.1330 0.105 Uiso 1 1 calc R . . C16 C -0.1509(8) 0.3026(4) 0.2137(4) 0.073(3) Uani 1 1 d . . . H16A H -0.1124 0.2596 0.2285 0.087 Uiso 1 1 calc R . . H16B H -0.2330 0.2945 0.2010 0.087 Uiso 1 1 calc R . . C17 C -0.2198(6) 0.4326(4) 0.2488(4) 0.065(2) Uani 1 1 d . . . H17A H -0.2153 0.4621 0.2851 0.078 Uiso 1 1 calc R . . H17B H -0.1957 0.4599 0.2178 0.078 Uiso 1 1 calc R . . C18 C -0.3399(7) 0.4154(6) 0.2209(5) 0.087(3) Uani 1 1 d . . . H18A H -0.3839 0.4568 0.2102 0.105 Uiso 1 1 calc R . . H18B H -0.3672 0.3895 0.2510 0.105 Uiso 1 1 calc R . . H18C H -0.3479 0.3885 0.1832 0.105 Uiso 1 1 calc R . . C19 C 0.1272(11) 0.3172(5) 0.1649(4) 0.102(4) Uani 1 1 d . . . H19A H 0.1145 0.3209 0.1193 0.122 Uiso 1 1 calc R . . H19B H 0.2039 0.3339 0.1853 0.122 Uiso 1 1 calc R . . C20 C 0.1206(18) 0.2428(6) 0.1817(5) 0.202(11) Uani 1 1 d . . . H20A H 0.1781 0.2173 0.1689 0.242 Uiso 1 1 calc R . . H20B H 0.0461 0.2251 0.1601 0.242 Uiso 1 1 calc R . . H20C H 0.1336 0.2384 0.2268 0.242 Uiso 1 1 calc R . . C21 C 0.0065(7) 0.4401(3) 0.1328(3) 0.0501(17) Uani 1 1 d . . . H21A H -0.0514 0.4704 0.1407 0.060 Uiso 1 1 calc R . . H21B H 0.0776 0.4658 0.1418 0.060 Uiso 1 1 calc R . . C22 C -0.0286(9) 0.4215(4) 0.0637(3) 0.070(2) Uani 1 1 d . . . H22A H -0.0369 0.4625 0.0385 0.084 Uiso 1 1 calc R . . H22B H -0.1004 0.3973 0.0536 0.084 Uiso 1 1 calc R . . H22C H 0.0290 0.3926 0.0547 0.084 Uiso 1 1 calc R . . C23 C -0.1548(10) 0.3257(6) 0.3409(5) 0.096(4) Uani 1 1 d . . . H23A H -0.1011 0.3420 0.3799 0.116 Uiso 1 1 calc R . . H23B H -0.2297 0.3434 0.3403 0.116 Uiso 1 1 calc R . . C24 C -0.1594(17) 0.2556(6) 0.3449(7) 0.169(8) Uani 1 1 d . . . H24A H -0.1820 0.2431 0.3820 0.203 Uiso 1 1 calc R . . H24B H -0.0851 0.2367 0.3478 0.203 Uiso 1 1 calc R . . H24C H -0.2142 0.2380 0.3076 0.203 Uiso 1 1 calc R . . C25 C 0.4174(7) 0.3192(5) 0.4427(5) 0.079(3) Uani 1 1 d . . . H25A H 0.3733 0.2775 0.4304 0.095 Uiso 1 1 calc R . . H25B H 0.4983 0.3075 0.4544 0.095 Uiso 1 1 calc R . . C26 C 0.3884(6) 0.3515(5) 0.4966(4) 0.068(3) Uani 1 1 d . . . H26A H 0.4439 0.3870 0.5147 0.081 Uiso 1 1 calc R . . H26B H 0.3910 0.3175 0.5293 0.081 Uiso 1 1 calc R . . C27 C 0.2490(9) 0.4421(5) 0.5363(3) 0.074(3) Uani 1 1 d . . . H27A H 0.2625 0.4130 0.5736 0.089 Uiso 1 1 calc R . . H27B H 0.3147 0.4724 0.5428 0.089 Uiso 1 1 calc R . . C28 C 0.1498(10) 0.4840(7) 0.5337(4) 0.109(5) Uani 1 1 d . . . H28A H 0.1635 0.5107 0.5720 0.131 Uiso 1 1 calc R . . H28B H 0.0842 0.4551 0.5297 0.131 Uiso 1 1 calc R . . H28C H 0.1357 0.5143 0.4977 0.131 Uiso 1 1 calc R . . C29 C 0.5132(6) 0.4300(5) 0.3902(4) 0.061(2) Uani 1 1 d . . . H29A H 0.5277 0.4534 0.4308 0.074 Uiso 1 1 calc R . . H29B H 0.5774 0.3995 0.3926 0.074 Uiso 1 1 calc R . . C30 C 0.5075(6) 0.4821(5) 0.3393(3) 0.063(2) Uani 1 1 d . . . H30A H 0.5783 0.5071 0.3487 0.075 Uiso 1 1 calc R . . H30B H 0.4454 0.5133 0.3374 0.075 Uiso 1 1 calc R . . H30C H 0.4949 0.4593 0.2990 0.075 Uiso 1 1 calc R . . C31 C 0.1517(6) 0.3195(4) 0.4712(3) 0.0495(17) Uani 1 1 d . . . H31A H 0.0737 0.3354 0.4530 0.059 Uiso 1 1 calc R . . H31B H 0.1660 0.2837 0.4436 0.059 Uiso 1 1 calc R . . C32 C 0.1594(7) 0.2880(5) 0.5350(4) 0.073(3) Uani 1 1 d . . . H32A H 0.1051 0.2511 0.5298 0.088 Uiso 1 1 calc R . . H32B H 0.1426 0.3222 0.5626 0.088 Uiso 1 1 calc R . . H32C H 0.2354 0.2705 0.5533 0.088 Uiso 1 1 calc R . . C33 C 0.3831(7) 0.3272(5) 0.3095(5) 0.078(3) Uani 1 1 d . . . H33A H 0.3228 0.2933 0.3042 0.094 Uiso 1 1 calc R . . H33B H 0.3635 0.3563 0.2720 0.094 Uiso 1 1 calc R . . C34 C 0.4933(9) 0.2905(5) 0.3121(6) 0.096(4) Uani 1 1 d . . . H34A H 0.4839 0.2642 0.2739 0.115 Uiso 1 1 calc R . . H34B H 0.5128 0.2602 0.3482 0.115 Uiso 1 1 calc R . . H34C H 0.5536 0.3234 0.3160 0.115 Uiso 1 1 calc R . . C35 C 0.3502(8) 0.9741(3) 0.4332(4) 0.070(2) Uani 1 1 d D . . H35A H 0.3097 1.0036 0.4553 0.084 Uiso 1 1 calc R . . H35B H 0.3576 1.0012 0.3974 0.084 Uiso 1 1 calc R . . C36 C 0.4683(9) 0.9744(5) 0.4761(6) 0.122(5) Uani 1 1 d D . . H36A H 0.5165 0.9681 0.4480 0.147 Uiso 1 1 calc R . . H36B H 0.4739 0.9320 0.4999 0.147 Uiso 1 1 calc R . . C37 C 0.2640(12) 0.9247(8) 0.4033(8) 0.159 Uiso 1 1 d D . . H37A H 0.2033 0.9472 0.3720 0.147 Uiso 1 1 calc R . . H37B H 0.2336 0.9038 0.4348 0.147 Uiso 1 1 calc R . . H37C H 0.2975 0.8899 0.3830 0.147 Uiso 1 1 calc R . . O7 O 0.6487(7) -0.0271(5) 0.3406(4) 0.116(3) Uani 1 1 d D . . C38 C 0.656(2) -0.0268(12) 0.4061(8) 0.44(3) Uani 1 1 d D . . H38A H 0.6868 -0.0699 0.4260 0.527 Uiso 1 1 calc R . . H38B H 0.5821 -0.0186 0.4130 0.527 Uiso 1 1 calc R . . C39 C 0.738(2) 0.0318(13) 0.4319(8) 0.44(3) Uani 1 1 d D . . H39A H 0.7302 0.0469 0.4726 0.527 Uiso 1 1 calc R . . H39B H 0.8167 0.0172 0.4377 0.527 Uiso 1 1 calc R . . C40 C 0.7082(8) 0.0897(8) 0.3842(7) 0.167(8) Uani 1 1 d D . . H40A H 0.7755 0.1150 0.3816 0.200 Uiso 1 1 calc R . . H40B H 0.6524 0.1210 0.3929 0.200 Uiso 1 1 calc R . . C41 C 0.6559(14) 0.0451(7) 0.3231(6) 0.175(9) Uani 1 1 d D . . H41A H 0.5799 0.0619 0.3012 0.211 Uiso 1 1 calc R . . H41B H 0.7035 0.0490 0.2945 0.211 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 Mo1 0.0247(2) 0.0271(2) 0.0193(2) -0.00132(17) 0.00250(16) -0.00142(18) Fe1 0.0388(4) 0.0269(4) 0.0201(4) -0.0027(3) 0.0058(3) -0.0043(3) Fe2 0.0296(4) 0.0308(4) 0.0216(4) 0.0018(3) 0.0040(3) 0.0015(3) Cl1 0.0764(12) 0.0676(12) 0.0284(8) 0.0120(8) 0.0087(8) 0.0028(10) Cl2 0.0786(14) 0.0595(11) 0.0467(10) 0.0105(8) -0.0297(9) 0.0011(10) Cl3 0.0357(9) 0.0705(13) 0.1037(17) 0.0099(12) -0.0213(10) 0.0085(9) Cl4 0.0311(8) 0.0646(11) 0.0831(13) 0.0044(10) 0.0164(8) 0.0058(8) Cl5 0.0473(10) 0.0752(13) 0.0835(14) 0.0338(11) -0.0009(9) -0.0256(9) Cl6 0.0658(13) 0.0403(10) 0.139(2) 0.0192(12) -0.0521(14) -0.0218(9) Cl7 0.0916(16) 0.0503(11) 0.1077(19) -0.0418(12) -0.0552(14) 0.0190(11) Cl8 0.0804(14) 0.0857(15) 0.0553(12) -0.0410(11) -0.0038(10) 0.0192(12) S1 0.0341(7) 0.0336(7) 0.0234(6) 0.0011(5) 0.0110(5) 0.0019(6) S2 0.0299(7) 0.0331(7) 0.0209(6) -0.0016(5) 0.0077(5) -0.0016(5) P1 0.0514(11) 0.0519(10) 0.0437(10) -0.0081(8) 0.0059(8) -0.0259(9) P2 0.0840(13) 0.0335(8) 0.0219(7) -0.0057(6) 0.0100(8) -0.0082(8) P3 0.0342(9) 0.0536(10) 0.0536(10) 0.0164(8) 0.0144(8) 0.0121(8) P4 0.0440(9) 0.0406(8) 0.0223(7) 0.0049(6) 0.0036(6) 0.0016(7) O1 0.032(2) 0.036(2) 0.0256(19) 0.0038(16) 0.0046(16) 0.0006(17) O2 0.0261(19) 0.038(2) 0.031(2) 0.0012(17) 0.0039(16) 0.0000(16) O3 0.033(2) 0.035(2) 0.032(2) 0.0048(17) 0.0010(17) -0.0081(17) O4 0.034(2) 0.038(2) 0.030(2) -0.0093(17) -0.0004(17) 0.0030(17) O5 0.083(4) 0.032(2) 0.046(3) 0.007(2) 0.012(3) 0.009(2) O6 0.045(3) 0.041(2) 0.038(2) 0.0039(19) -0.011(2) -0.009(2) C1 0.058(4) 0.032(3) 0.027(3) -0.002(2) 0.012(3) -0.001(3) C2 0.035(3) 0.036(3) 0.032(3) 0.013(2) -0.003(2) 0.002(3) C3 0.036(3) 0.027(3) 0.029(3) 0.001(2) -0.002(2) -0.003(2) C4 0.045(4) 0.035(3) 0.031(3) 0.000(2) -0.003(3) -0.002(3) C5 0.054(4) 0.032(3) 0.042(4) 0.002(3) -0.022(3) -0.007(3) C6 0.035(3) 0.039(4) 0.058(4) 0.001(3) -0.012(3) -0.003(3) C7 0.028(3) 0.032(3) 0.058(4) 0.002(3) 0.001(3) -0.003(2) C8 0.030(3) 0.028(3) 0.037(3) 0.000(2) 0.001(2) -0.001(2) C9 0.035(3) 0.030(3) 0.041(3) 0.006(2) -0.012(3) 0.000(2) C10 0.040(4) 0.035(3) 0.065(5) 0.019(3) -0.016(3) -0.006(3) C11 0.042(4) 0.024(3) 0.089(6) 0.010(3) -0.037(4) -0.002(3) C12 0.052(5) 0.033(4) 0.074(5) -0.015(3) -0.040(4) 0.011(3) C13 0.054(4) 0.042(4) 0.045(4) -0.015(3) -0.018(3) 0.014(3) C14 0.039(3) 0.030(3) 0.037(3) -0.002(2) -0.013(3) 0.010(3) C15 0.125(9) 0.076(6) 0.046(5) -0.015(4) 0.000(5) -0.052(6) C16 0.078(6) 0.060(5) 0.072(6) -0.029(4) 0.008(5) -0.030(4) C17 0.046(4) 0.072(5) 0.075(6) -0.015(4) 0.012(4) -0.004(4) C18 0.054(5) 0.093(7) 0.106(8) -0.012(6) 0.009(5) -0.002(5) C19 0.175(11) 0.091(7) 0.033(4) -0.010(4) 0.020(5) 0.078(7) C20 0.45(3) 0.099(9) 0.050(6) 0.009(6) 0.056(11) 0.141(15) C21 0.073(5) 0.047(4) 0.025(3) -0.001(3) 0.006(3) 0.003(3) C22 0.119(7) 0.063(5) 0.021(3) 0.002(3) 0.008(4) 0.004(5) C23 0.111(8) 0.112(8) 0.071(6) 0.004(6) 0.033(6) -0.069(7) C24 0.34(3) 0.075(8) 0.143(13) 0.041(8) 0.149(16) 0.026(12) C25 0.053(5) 0.091(7) 0.101(7) 0.059(6) 0.036(5) 0.039(5) C26 0.042(4) 0.091(6) 0.059(5) 0.049(5) -0.005(3) 0.005(4) C27 0.113(8) 0.077(6) 0.028(4) 0.001(4) 0.014(4) 0.000(5) C28 0.133(10) 0.156(11) 0.040(5) -0.008(6) 0.028(5) 0.078(9) C29 0.036(4) 0.098(6) 0.051(4) 0.017(4) 0.012(3) -0.006(4) C30 0.050(4) 0.096(6) 0.042(4) 0.013(4) 0.015(3) -0.021(4) C31 0.045(4) 0.065(5) 0.034(3) 0.017(3) 0.003(3) -0.010(3) C32 0.063(5) 0.101(7) 0.049(5) 0.035(5) 0.008(4) -0.012(5) C33 0.064(5) 0.074(6) 0.107(7) -0.014(5) 0.042(5) 0.020(4) C34 0.093(7) 0.079(7) 0.148(10) 0.006(7) 0.085(8) 0.028(6) C35 0.103(7) 0.025(3) 0.075(6) 0.009(3) 0.014(5) 0.009(4) C36 0.114(10) 0.057(6) 0.160(13) -0.001(7) -0.021(9) 0.005(6) O7 0.112(6) 0.141(8) 0.121(7) 0.006(6) 0.077(6) -0.003(6) C38 0.16(2) 0.75(8) 0.41(4) 0.23(4) 0.08(3) -0.03(3) C39 0.16(2) 0.75(8) 0.41(4) 0.23(4) 0.08(3) -0.03(3) C40 0.024(4) 0.36(3) 0.128(11) -0.078(14) 0.036(6) -0.024(9) C41 0.225(19) 0.22(2) 0.110(11) 0.040(12) 0.102(13) 0.147(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 O1 2.021(4) . ? Mo1 O4 2.038(4) . ? Mo1 O2 2.044(4) . ? Mo1 O3 2.053(4) . ? Mo1 S1 2.3411(14) . ? Mo1 S2 2.3426(14) . ? Mo1 Fe2 2.7927(9) . ? Mo1 Fe1 2.9537(9) . ? Fe1 C1 1.754(6) . ? Fe1 S1 2.2013(16) . ? Fe1 S2 2.2075(15) . ? Fe1 P1 2.231(2) . ? Fe1 P2 2.2432(17) . ? Fe1 Fe2 2.6230(11) . ? Fe2 C2 1.744(6) . ? Fe2 S2 2.2158(15) . ? Fe2 S1 2.2189(15) . ? Fe2 P4 2.2387(16) . ? Fe2 P3 2.2506(18) . ? Cl1 C4 1.729(7) . ? Cl2 C5 1.729(6) . ? Cl3 C6 1.728(7) . ? Cl4 C7 1.739(7) . ? Cl5 C10 1.728(9) . ? Cl6 C11 1.726(7) . ? Cl7 C12 1.736(8) . ? Cl8 C13 1.715(9) . ? P1 C16 1.804(8) . ? P1 C23 1.850(9) . ? P1 C17 1.853(9) . ? P2 C21 1.815(7) . ? P2 C19 1.818(9) . ? P2 C15 1.893(9) . ? P3 C29 1.840(8) . ? P3 C33 1.841(9) . ? P3 C25 1.842(8) . ? P4 C31 1.806(7) . ? P4 C27 1.812(8) . ? P4 C26 1.857(7) . ? O1 C3 1.338(7) . ? O2 C8 1.326(7) . ? O3 C9 1.331(7) . ? O4 C14 1.310(7) . ? O5 C1 1.148(7) . ? O6 C2 1.154(7) . ? C3 C8 1.379(8) . ? C3 C4 1.396(8) . ? C4 C5 1.390(9) . ? C5 C6 1.387(11) . ? C6 C7 1.387(9) . ? C7 C8 1.397(8) . ? C9 C10 1.393(9) . ? C9 C14 1.414(10) . ? C10 C11 1.408(11) . ? C11 C12 1.377(13) . ? C12 C13 1.409(11) . ? C13 C14 1.396(9) . ? C15 C16 1.457(12) . ? C17 C18 1.483(11) . ? C19 C20 1.534(17) . ? C21 C22 1.530(9) . ? C23 C24 1.398(15) . ? C25 C26 1.497(13) . ? C27 C28 1.473(13) . ? C29 C30 1.527(10) . ? C31 C32 1.537(9) . ? C33 C34 1.536(11) . ? C35 C37 1.468(12) . ? C35 C36 1.509(11) . ? C36 C36 1.524(14) 3_676 ? O7 C38 1.442(13) . ? O7 C41 1.497(11) . ? C38 C39 1.545(17) . ? C39 C40 1.541(17) . ? C40 C41 1.604(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Mo1 O4 126.30(16) . . ? O1 Mo1 O2 76.25(15) . . ? O4 Mo1 O2 82.63(15) . . ? O1 Mo1 O3 81.60(15) . . ? O4 Mo1 O3 77.04(17) . . ? O2 Mo1 O3 131.89(16) . . ? O1 Mo1 S1 86.09(12) . . ? O4 Mo1 S1 137.25(11) . . ? O2 Mo1 S1 136.96(12) . . ? O3 Mo1 S1 82.12(12) . . ? O1 Mo1 S2 137.71(12) . . ? O4 Mo1 S2 86.04(12) . . ? O2 Mo1 S2 83.03(11) . . ? O3 Mo1 S2 137.21(11) . . ? S1 Mo1 S2 84.54(5) . . ? O1 Mo1 Fe2 136.37(11) . . ? O4 Mo1 Fe2 93.09(11) . . ? O2 Mo1 Fe2 133.22(11) . . ? O3 Mo1 Fe2 91.37(11) . . ? S1 Mo1 Fe2 50.28(4) . . ? S2 Mo1 Fe2 50.19(4) . . ? O1 Mo1 Fe1 98.36(11) . . ? O4 Mo1 Fe1 133.00(12) . . ? O2 Mo1 Fe1 96.33(11) . . ? O3 Mo1 Fe1 129.11(12) . . ? S1 Mo1 Fe1 47.41(4) . . ? S2 Mo1 Fe1 47.56(4) . . ? Fe2 Mo1 Fe1 54.23(2) . . ? C1 Fe1 S1 108.7(2) . . ? C1 Fe1 S2 108.25(19) . . ? S1 Fe1 S2 91.21(6) . . ? C1 Fe1 P1 92.1(2) . . ? S1 Fe1 P1 158.02(7) . . ? S2 Fe1 P1 88.97(7) . . ? C1 Fe1 P2 94.91(19) . . ? S1 Fe1 P2 87.57(7) . . ? S2 Fe1 P2 155.88(7) . . ? P1 Fe1 P2 83.41(8) . . ? C1 Fe1 Fe2 84.4(2) . . ? S1 Fe1 Fe2 53.91(4) . . ? S2 Fe1 Fe2 53.78(4) . . ? P1 Fe1 Fe2 138.44(6) . . ? P2 Fe1 Fe2 138.13(7) . . ? C1 Fe1 Mo1 144.2(2) . . ? S1 Fe1 Mo1 51.53(4) . . ? S2 Fe1 Mo1 51.55(4) . . ? P1 Fe1 Mo1 113.99(6) . . ? P2 Fe1 Mo1 111.47(5) . . ? Fe2 Fe1 Mo1 59.75(2) . . ? C2 Fe2 S2 112.6(2) . . ? C2 Fe2 S1 109.31(19) . . ? S2 Fe2 S1 90.53(6) . . ? C2 Fe2 P4 88.08(19) . . ? S2 Fe2 P4 88.26(6) . . ? S1 Fe2 P4 161.54(7) . . ? C2 Fe2 P3 91.1(2) . . ? S2 Fe2 P3 155.34(7) . . ? S1 Fe2 P3 87.87(6) . . ? P4 Fe2 P3 85.60(7) . . ? C2 Fe2 Fe1 152.52(18) . . ? S2 Fe2 Fe1 53.48(4) . . ? S1 Fe2 Fe1 53.29(4) . . ? P4 Fe2 Fe1 112.73(5) . . ? P3 Fe2 Fe1 107.60(6) . . ? C2 Fe2 Mo1 86.59(18) . . ? S2 Fe2 Mo1 54.31(4) . . ? S1 Fe2 Mo1 54.25(4) . . ? P4 Fe2 Mo1 135.89(6) . . ? P3 Fe2 Mo1 138.22(6) . . ? Fe1 Fe2 Mo1 66.02(3) . . ? Fe1 S1 Fe2 72.80(5) . . ? Fe1 S1 Mo1 81.06(5) . . ? Fe2 S1 Mo1 75.48(5) . . ? Fe1 S2 Fe2 72.74(5) . . ? Fe1 S2 Mo1 80.90(5) . . ? Fe2 S2 Mo1 75.50(5) . . ? C16 P1 C23 104.9(5) . . ? C16 P1 C17 104.9(4) . . ? C23 P1 C17 103.8(5) . . ? C16 P1 Fe1 108.8(3) . . ? C23 P1 Fe1 118.9(4) . . ? C17 P1 Fe1 114.4(3) . . ? C21 P2 C19 103.3(4) . . ? C21 P2 C15 101.0(4) . . ? C19 P2 C15 107.6(5) . . ? C21 P2 Fe1 117.2(2) . . ? C19 P2 Fe1 117.4(3) . . ? C15 P2 Fe1 108.8(3) . . ? C29 P3 C33 103.9(4) . . ? C29 P3 C25 104.1(4) . . ? C33 P3 C25 103.7(5) . . ? C29 P3 Fe2 113.6(3) . . ? C33 P3 Fe2 120.4(3) . . ? C25 P3 Fe2 109.6(3) . . ? C31 P4 C27 107.6(4) . . ? C31 P4 C26 104.6(4) . . ? C27 P4 C26 99.9(4) . . ? C31 P4 Fe2 118.6(2) . . ? C27 P4 Fe2 116.8(3) . . ? C26 P4 Fe2 106.9(2) . . ? C3 O1 Mo1 116.8(3) . . ? C8 O2 Mo1 116.5(4) . . ? C9 O3 Mo1 115.6(4) . . ? C14 O4 Mo1 116.3(4) . . ? O5 C1 Fe1 178.4(6) . . ? O6 C2 Fe2 177.6(5) . . ? O1 C3 C8 115.2(5) . . ? O1 C3 C4 124.6(6) . . ? C8 C3 C4 120.3(6) . . ? C5 C4 C3 119.4(6) . . ? C5 C4 Cl1 121.5(5) . . ? C3 C4 Cl1 119.1(5) . . ? C6 C5 C4 120.4(6) . . ? C6 C5 Cl2 119.8(5) . . ? C4 C5 Cl2 119.8(6) . . ? C7 C6 C5 120.0(6) . . ? C7 C6 Cl3 120.1(6) . . ? C5 C6 Cl3 119.9(5) . . ? C6 C7 C8 119.7(6) . . ? C6 C7 Cl4 121.3(5) . . ? C8 C7 Cl4 119.0(5) . . ? O2 C8 C3 115.1(5) . . ? O2 C8 C7 124.7(6) . . ? C3 C8 C7 120.2(6) . . ? O3 C9 C10 124.8(7) . . ? O3 C9 C14 114.9(5) . . ? C10 C9 C14 120.4(6) . . ? C9 C10 C11 119.7(8) . . ? C9 C10 Cl5 118.4(6) . . ? C11 C10 Cl5 121.9(6) . . ? C12 C11 C10 119.9(7) . . ? C12 C11 Cl6 120.4(6) . . ? C10 C11 Cl6 119.7(8) . . ? C11 C12 C13 121.0(7) . . ? C11 C12 Cl7 120.4(6) . . ? C13 C12 Cl7 118.6(8) . . ? C14 C13 C12 119.4(8) . . ? C14 C13 Cl8 118.8(6) . . ? C12 C13 Cl8 121.7(6) . . ? O4 C14 C13 124.5(7) . . ? O4 C14 C9 116.0(5) . . ? C13 C14 C9 119.5(6) . . ? C16 C15 P2 111.6(6) . . ? C15 C16 P1 108.1(6) . . ? C18 C17 P1 119.7(7) . . ? C20 C19 P2 114.1(10) . . ? C22 C21 P2 116.4(5) . . ? C24 C23 P1 119.5(9) . . ? C26 C25 P3 108.0(6) . . ? C25 C26 P4 109.8(5) . . ? C28 C27 P4 118.1(7) . . ? C30 C29 P3 113.5(5) . . ? C32 C31 P4 116.8(5) . . ? C34 C33 P3 115.9(8) . . ? C37 C35 C36 138.1(9) . . ? C35 C36 C36 131.8(12) . 3_676 ? C38 O7 C41 105.6(10) . . ? O7 C38 C39 103.4(11) . . ? C40 C39 C38 107.5(11) . . ? C39 C40 C41 97.9(9) . . ? O7 C41 C40 110.3(8) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.44 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.409 _refine_diff_density_min -2.286 _refine_diff_density_rms 0.123 #===END data_comp_5 _database_code_depnum_ccdc_archive 'CCDC 258780' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C43 H66 Fe3 O7 P2 S2' _chemical_formula_weight 988.57 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' Fe Fe 0.3463 0.8444 '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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pna2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' _cell_length_a 19.17360(10) _cell_length_b 11.19000(10) _cell_length_c 21.82370(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4682.33(5) _cell_formula_units_Z 4 _cell_measurement_temperature 158(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description rhombic _exptl_crystal_colour black _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.402 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2080 _exptl_absorpt_coefficient_mu 1.121 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.8238 _exptl_absorpt_correction_T_max 0.8773 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 158(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41028 _diffrn_reflns_av_R_equivalents 0.1225 _diffrn_reflns_av_sigmaI/netI 0.1083 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.30 _diffrn_reflns_theta_max 26.75 _reflns_number_total 9585 _reflns_number_gt 7319 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _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^)+(0.0057P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.005(13) _refine_ls_number_reflns 9585 _refine_ls_number_parameters 514 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0747 _refine_ls_R_factor_gt 0.0504 _refine_ls_wR_factor_ref 0.0839 _refine_ls_wR_factor_gt 0.0767 _refine_ls_goodness_of_fit_ref 0.954 _refine_ls_restrained_S_all 0.954 _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 0.60676(3) 0.35734(6) -0.07654(2) 0.01713(15) Uani 1 1 d . . . Fe2 Fe 0.61284(4) 0.55227(6) -0.01266(3) 0.02195(16) Uani 1 1 d . . . Fe3 Fe 0.64958(3) 0.40584(6) 0.07654(3) 0.01746(14) Uani 1 1 d . . . S2 S 0.69812(6) 0.41082(11) -0.01774(5) 0.0202(2) Uani 1 1 d . . . S1 S 0.55499(6) 0.38401(10) 0.01544(4) 0.0167(2) Uani 1 1 d . . . P1 P 0.61937(6) 0.15742(11) -0.08639(5) 0.0158(3) Uani 1 1 d . . . P2 P 0.59107(6) 0.45497(11) 0.16665(5) 0.0172(3) Uani 1 1 d . . . O1 O 0.78591(18) 0.4800(4) 0.12302(14) 0.0452(11) Uani 1 1 d . . . O2 O 0.67197(18) 0.1581(3) 0.11320(14) 0.0335(9) Uani 1 1 d . . . O3 O 0.69184(18) 0.4243(3) -0.18283(13) 0.0334(9) Uani 1 1 d . . . O4 O 0.47459(17) 0.3779(3) -0.14373(13) 0.0304(8) Uani 1 1 d . . . O5 O 0.6118(3) 0.6576(4) -0.13596(15) 0.0639(14) Uani 1 1 d . . . O6 O 0.7191(2) 0.7128(4) 0.03890(18) 0.0564(12) Uani 1 1 d . . . O7 O 0.4838(2) 0.6768(3) 0.02012(16) 0.0415(10) Uani 1 1 d . . . C1 C 0.7306(3) 0.4556(5) 0.10686(19) 0.0264(12) Uani 1 1 d . . . C2 C 0.6620(2) 0.2579(5) 0.09857(18) 0.0220(11) Uani 1 1 d . . . C3 C 0.6580(2) 0.3925(4) -0.14213(19) 0.0223(11) Uani 1 1 d . . . C4 C 0.5260(2) 0.3662(4) -0.11719(18) 0.0202(11) Uani 1 1 d . . . C5 C 0.6122(3) 0.6107(4) -0.0897(2) 0.0352(13) Uani 1 1 d . . . C6 C 0.6770(3) 0.6502(5) 0.0200(2) 0.0358(13) Uani 1 1 d . . . C7 C 0.5347(3) 0.6302(4) 0.0077(2) 0.0265(12) Uani 1 1 d . . . C8 C 0.6226(2) 0.0979(4) -0.16755(17) 0.0164(10) Uani 1 1 d . . . H8 H 0.6721 0.1083 -0.1812 0.020 Uiso 1 1 calc R . . C9 C 0.6079(2) -0.0362(4) -0.17246(18) 0.0213(11) Uani 1 1 d . . . H9A H 0.6382 -0.0799 -0.1434 0.026 Uiso 1 1 calc R . . H9B H 0.5588 -0.0518 -0.1609 0.026 Uiso 1 1 calc R . . C10 C 0.6207(3) -0.0828(4) -0.23740(18) 0.0257(12) Uani 1 1 d . . . H10A H 0.6708 -0.0742 -0.2477 0.031 Uiso 1 1 calc R . . H10B H 0.6087 -0.1687 -0.2394 0.031 Uiso 1 1 calc R . . C11 C 0.5770(3) -0.0139(5) -0.28404(19) 0.0257(12) Uani 1 1 d . . . H11A H 0.5881 -0.0423 -0.3259 0.031 Uiso 1 1 calc R . . H11B H 0.5269 -0.0291 -0.2764 0.031 Uiso 1 1 calc R . . C12 C 0.5914(3) 0.1192(5) -0.27969(17) 0.0268(12) Uani 1 1 d . . . H12A H 0.5610 0.1622 -0.3090 0.032 Uiso 1 1 calc R . . H12B H 0.6404 0.1348 -0.2913 0.032 Uiso 1 1 calc R . . C13 C 0.5782(2) 0.1676(4) -0.21434(17) 0.0223(11) Uani 1 1 d . . . H13A H 0.5904 0.2535 -0.2126 0.027 Uiso 1 1 calc R . . H13B H 0.5282 0.1593 -0.2040 0.027 Uiso 1 1 calc R . . C14 C 0.7043(2) 0.1104(4) -0.05254(17) 0.0152(10) Uani 1 1 d . . . H14 H 0.7054 0.1476 -0.0109 0.018 Uiso 1 1 calc R . . C15 C 0.7663(2) 0.1649(4) -0.08691(19) 0.0223(11) Uani 1 1 d . . . H15A H 0.7566 0.2501 -0.0958 0.027 Uiso 1 1 calc R . . H15B H 0.7727 0.1229 -0.1264 0.027 Uiso 1 1 calc R . . C16 C 0.8334(2) 0.1551(5) -0.0489(2) 0.0252(11) Uani 1 1 d . . . H16A H 0.8728 0.1901 -0.0721 0.030 Uiso 1 1 calc R . . H16B H 0.8279 0.2007 -0.0103 0.030 Uiso 1 1 calc R . . C17 C 0.8492(3) 0.0245(5) -0.0341(2) 0.0296(12) Uani 1 1 d . . . H17A H 0.8610 -0.0186 -0.0724 0.035 Uiso 1 1 calc R . . H17B H 0.8900 0.0201 -0.0064 0.035 Uiso 1 1 calc R . . C18 C 0.7867(2) -0.0351(5) -0.0037(2) 0.0324(13) Uani 1 1 d . . . H18A H 0.7790 0.0015 0.0370 0.039 Uiso 1 1 calc R . . H18B H 0.7970 -0.1209 0.0026 0.039 Uiso 1 1 calc R . . C19 C 0.7197(2) -0.0230(4) -0.0420(2) 0.0243(11) Uani 1 1 d . . . H19A H 0.6802 -0.0608 -0.0201 0.029 Uiso 1 1 calc R . . H19B H 0.7257 -0.0639 -0.0819 0.029 Uiso 1 1 calc R . . C20 C 0.5515(2) 0.0631(4) -0.04896(17) 0.0183(11) Uani 1 1 d . . . H20 H 0.5607 -0.0216 -0.0611 0.022 Uiso 1 1 calc R . . C21 C 0.5542(2) 0.0687(4) 0.02192(17) 0.0227(11) Uani 1 1 d . . . H21A H 0.6011 0.0442 0.0362 0.027 Uiso 1 1 calc R . . H21B H 0.5460 0.1519 0.0356 0.027 Uiso 1 1 calc R . . C22 C 0.4991(2) -0.0135(4) 0.04986(19) 0.0271(12) Uani 1 1 d . . . H22A H 0.5110 -0.0975 0.0401 0.033 Uiso 1 1 calc R . . H22B H 0.4998 -0.0047 0.0950 0.033 Uiso 1 1 calc R . . C23 C 0.4262(3) 0.0136(6) 0.0264(2) 0.0381(14) Uani 1 1 d . . . H23A H 0.4118 0.0938 0.0408 0.046 Uiso 1 1 calc R . . H23B H 0.3930 -0.0456 0.0433 0.046 Uiso 1 1 calc R . . C24 C 0.4231(3) 0.0101(5) -0.0436(2) 0.0302(13) Uani 1 1 d . . . H24A H 0.3761 0.0344 -0.0576 0.036 Uiso 1 1 calc R . . H24B H 0.4317 -0.0725 -0.0581 0.036 Uiso 1 1 calc R . . C25 C 0.4783(2) 0.0949(5) -0.0710(2) 0.0241(11) Uani 1 1 d . . . H25A H 0.4767 0.0901 -0.1163 0.029 Uiso 1 1 calc R . . H25B H 0.4673 0.1782 -0.0590 0.029 Uiso 1 1 calc R . . C26 C 0.6067(3) 0.6060(4) 0.20175(18) 0.0214(11) Uani 1 1 d . . . H26 H 0.5737 0.6140 0.2370 0.026 Uiso 1 1 calc R . . C27 C 0.6803(3) 0.6233(5) 0.2273(2) 0.0382(14) Uani 1 1 d . . . H27A H 0.7148 0.6114 0.1941 0.046 Uiso 1 1 calc R . . H27B H 0.6893 0.5627 0.2594 0.046 Uiso 1 1 calc R . . C28 C 0.6894(3) 0.7489(5) 0.2547(2) 0.0386(14) Uani 1 1 d . . . H28A H 0.6575 0.7584 0.2901 0.046 Uiso 1 1 calc R . . H28B H 0.7378 0.7584 0.2697 0.046 Uiso 1 1 calc R . . C29 C 0.6739(3) 0.8448(5) 0.2076(2) 0.0384(14) Uani 1 1 d . . . H29A H 0.6793 0.9248 0.2264 0.046 Uiso 1 1 calc R . . H29B H 0.7072 0.8385 0.1731 0.046 Uiso 1 1 calc R . . C30 C 0.6001(3) 0.8297(5) 0.1842(2) 0.0351(13) Uani 1 1 d . . . H30A H 0.5904 0.8913 0.1528 0.042 Uiso 1 1 calc R . . H30B H 0.5669 0.8414 0.2184 0.042 Uiso 1 1 calc R . . C31 C 0.5894(2) 0.7062(4) 0.1566(2) 0.0255(11) Uani 1 1 d . . . H31A H 0.6194 0.6979 0.1198 0.031 Uiso 1 1 calc R . . H31B H 0.5403 0.6980 0.1433 0.031 Uiso 1 1 calc R . . C32 C 0.4942(2) 0.4528(4) 0.15575(17) 0.0177(10) Uani 1 1 d . . . H32 H 0.4865 0.4859 0.1137 0.021 Uiso 1 1 calc R . . C33 C 0.4479(2) 0.5287(5) 0.19765(19) 0.0246(11) Uani 1 1 d . . . H33A H 0.4663 0.6112 0.1997 0.030 Uiso 1 1 calc R . . H33B H 0.4482 0.4949 0.2396 0.030 Uiso 1 1 calc R . . C34 C 0.3727(2) 0.5304(5) 0.1726(2) 0.0269(12) Uani 1 1 d . . . H34A H 0.3431 0.5803 0.1995 0.032 Uiso 1 1 calc R . . H34B H 0.3725 0.5663 0.1311 0.032 Uiso 1 1 calc R . . C35 C 0.3430(3) 0.4055(5) 0.1694(2) 0.0333(13) Uani 1 1 d . . . H35A H 0.2959 0.4085 0.1509 0.040 Uiso 1 1 calc R . . H35B H 0.3384 0.3729 0.2114 0.040 Uiso 1 1 calc R . . C36 C 0.3895(2) 0.3230(5) 0.1314(2) 0.0276(12) Uani 1 1 d . . . H36A H 0.3711 0.2405 0.1338 0.033 Uiso 1 1 calc R . . H36B H 0.3877 0.3484 0.0879 0.033 Uiso 1 1 calc R . . C37 C 0.4653(2) 0.3235(4) 0.15296(19) 0.0206(10) Uani 1 1 d . . . H37A H 0.4940 0.2753 0.1245 0.025 Uiso 1 1 calc R . . H37B H 0.4682 0.2865 0.1941 0.025 Uiso 1 1 calc R . . C38 C 0.6093(2) 0.3433(4) 0.22821(17) 0.0202(10) Uani 1 1 d . . . H38 H 0.5893 0.2665 0.2127 0.024 Uiso 1 1 calc R . . C39 C 0.5717(2) 0.3663(5) 0.29018(18) 0.0254(12) Uani 1 1 d . . . H39A H 0.5917 0.4383 0.3099 0.030 Uiso 1 1 calc R . . H39B H 0.5216 0.3813 0.2826 0.030 Uiso 1 1 calc R . . C41 C 0.6563(3) 0.2255(5) 0.3431(2) 0.0357(14) Uani 1 1 d . . . H41A H 0.6796 0.2902 0.3663 0.043 Uiso 1 1 calc R . . H41B H 0.6591 0.1514 0.3677 0.043 Uiso 1 1 calc R . . C42 C 0.6940(3) 0.2068(5) 0.2827(2) 0.0277(12) Uani 1 1 d . . . H42A H 0.6746 0.1356 0.2618 0.033 Uiso 1 1 calc R . . H42B H 0.7441 0.1921 0.2906 0.033 Uiso 1 1 calc R . . C43 C 0.6860(2) 0.3155(4) 0.24148(18) 0.0205(11) Uani 1 1 d . . . H43A H 0.7107 0.3009 0.2024 0.025 Uiso 1 1 calc R . . H43B H 0.7079 0.3855 0.2615 0.025 Uiso 1 1 calc R . . C40 C 0.5800(3) 0.2582(5) 0.3332(2) 0.0361(14) Uani 1 1 d . . . H40A H 0.5583 0.2768 0.3732 0.043 Uiso 1 1 calc R . . H40B H 0.5551 0.1887 0.3155 0.043 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 0.0217(3) 0.0148(4) 0.0149(3) -0.0001(3) 0.0013(3) 0.0018(3) Fe2 0.0315(4) 0.0131(4) 0.0213(3) -0.0005(3) 0.0042(3) -0.0017(3) Fe3 0.0175(3) 0.0188(4) 0.0161(3) -0.0019(3) 0.0006(3) -0.0018(3) S2 0.0176(6) 0.0227(7) 0.0204(5) -0.0022(5) 0.0042(5) -0.0034(5) S1 0.0191(6) 0.0147(7) 0.0163(5) -0.0015(5) 0.0010(5) 0.0007(5) P1 0.0160(6) 0.0159(6) 0.0155(5) -0.0004(5) -0.0001(5) 0.0018(5) P2 0.0188(6) 0.0164(7) 0.0164(5) -0.0019(5) -0.0003(5) -0.0018(5) O1 0.024(2) 0.077(3) 0.034(2) -0.008(2) 0.0006(17) -0.017(2) O2 0.044(2) 0.023(2) 0.0339(18) -0.0070(16) -0.0146(17) 0.0093(18) O3 0.040(2) 0.035(3) 0.0246(16) 0.0058(16) 0.0135(16) 0.0021(19) O4 0.0247(19) 0.037(2) 0.0297(17) 0.0046(16) -0.0069(16) 0.0080(17) O5 0.126(4) 0.039(3) 0.027(2) 0.0143(18) 0.015(2) 0.022(3) O6 0.054(3) 0.047(3) 0.068(3) -0.013(2) 0.007(2) -0.028(2) O7 0.045(2) 0.021(2) 0.058(2) -0.0089(18) 0.001(2) 0.010(2) C1 0.021(3) 0.040(4) 0.018(2) -0.008(2) 0.005(2) -0.010(2) C2 0.017(3) 0.030(3) 0.019(2) -0.007(2) -0.0005(18) -0.003(2) C3 0.025(3) 0.020(3) 0.021(2) 0.000(2) -0.003(2) 0.007(2) C4 0.027(3) 0.020(3) 0.014(2) 0.0000(19) 0.003(2) 0.004(2) C5 0.061(4) 0.003(3) 0.041(3) -0.007(2) 0.006(3) 0.005(3) C6 0.041(3) 0.029(3) 0.038(3) -0.002(3) 0.008(3) -0.004(3) C7 0.043(3) 0.009(3) 0.028(2) -0.0053(19) -0.005(2) -0.011(2) C8 0.017(2) 0.015(3) 0.018(2) -0.0025(18) 0.0008(18) 0.000(2) C9 0.024(3) 0.017(3) 0.023(2) -0.0062(19) -0.004(2) 0.000(2) C10 0.031(3) 0.022(3) 0.024(2) -0.010(2) -0.003(2) 0.004(2) C11 0.027(3) 0.028(3) 0.023(2) -0.008(2) 0.001(2) 0.006(2) C12 0.028(3) 0.037(4) 0.016(2) -0.004(2) -0.003(2) 0.007(2) C13 0.028(3) 0.019(3) 0.020(2) -0.0011(19) 0.000(2) 0.002(2) C14 0.012(2) 0.015(3) 0.019(2) -0.0006(19) 0.0007(17) 0.007(2) C15 0.021(2) 0.025(3) 0.021(2) -0.002(2) 0.005(2) 0.001(2) C16 0.019(3) 0.024(3) 0.033(2) -0.002(2) 0.004(2) -0.001(2) C17 0.021(3) 0.026(3) 0.041(3) 0.001(2) -0.008(2) -0.002(2) C18 0.025(3) 0.027(3) 0.045(3) 0.010(2) -0.009(2) 0.003(2) C19 0.024(3) 0.015(3) 0.035(3) 0.005(2) -0.001(2) 0.005(2) C20 0.012(2) 0.021(3) 0.022(2) -0.0034(19) 0.0043(18) -0.001(2) C21 0.030(3) 0.023(3) 0.014(2) 0.0031(19) 0.003(2) -0.001(2) C22 0.035(3) 0.021(3) 0.025(2) -0.002(2) 0.013(2) -0.004(2) C23 0.031(3) 0.042(4) 0.041(3) 0.000(3) 0.014(3) -0.004(3) C24 0.016(3) 0.035(4) 0.040(3) -0.006(2) 0.002(2) -0.006(2) C25 0.018(2) 0.031(3) 0.023(2) -0.002(2) -0.001(2) 0.003(2) C26 0.029(3) 0.016(3) 0.019(2) -0.0061(19) -0.001(2) 0.000(2) C27 0.043(4) 0.017(3) 0.054(3) -0.004(2) -0.025(3) -0.002(3) C28 0.044(4) 0.021(3) 0.051(3) -0.002(2) -0.023(3) -0.003(3) C29 0.046(4) 0.021(3) 0.048(3) -0.007(3) -0.006(3) -0.004(3) C30 0.050(4) 0.015(3) 0.040(3) 0.000(2) -0.013(3) 0.003(3) C31 0.025(3) 0.021(3) 0.030(2) 0.000(2) -0.004(2) 0.004(2) C32 0.013(2) 0.022(3) 0.017(2) 0.0009(19) 0.0014(18) -0.002(2) C33 0.020(3) 0.029(3) 0.025(2) -0.011(2) 0.006(2) -0.004(2) C34 0.022(3) 0.030(3) 0.028(2) -0.002(2) 0.006(2) 0.005(2) C35 0.022(3) 0.044(4) 0.034(3) 0.002(3) -0.006(2) 0.000(3) C36 0.025(3) 0.029(3) 0.029(2) 0.001(2) -0.006(2) -0.008(2) C37 0.026(3) 0.013(3) 0.023(2) -0.0019(19) 0.005(2) -0.004(2) C38 0.025(3) 0.015(3) 0.021(2) -0.0030(18) 0.001(2) 0.002(2) C39 0.021(3) 0.032(3) 0.023(2) 0.003(2) 0.004(2) 0.006(2) C41 0.039(3) 0.035(4) 0.033(3) 0.015(2) 0.005(2) 0.005(3) C42 0.027(3) 0.024(3) 0.032(3) 0.001(2) 0.001(2) 0.004(2) C43 0.024(3) 0.018(3) 0.020(2) 0.0000(19) 0.005(2) 0.001(2) C40 0.033(3) 0.042(4) 0.033(3) 0.011(2) 0.015(2) 0.005(3) _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 C3 1.780(5) . ? Fe1 C4 1.788(5) . ? Fe1 S2 2.2524(13) . ? Fe1 S1 2.2590(11) . ? Fe1 P1 2.2604(13) . ? Fe1 Fe2 2.5914(9) . ? Fe2 C7 1.790(6) . ? Fe2 C6 1.795(6) . ? Fe2 C5 1.803(5) . ? Fe2 S1 2.2697(13) . ? Fe2 S2 2.2786(14) . ? Fe2 Fe3 2.6402(9) . ? Fe3 C2 1.740(5) . ? Fe3 C1 1.778(5) . ? Fe3 S2 2.2590(12) . ? Fe3 S1 2.2642(12) . ? Fe3 P2 2.3297(12) . ? P1 C14 1.863(4) . ? P1 C20 1.864(4) . ? P1 C8 1.893(4) . ? P2 C38 1.868(4) . ? P2 C32 1.873(4) . ? P2 C26 1.880(5) . ? O1 C1 1.150(5) . ? O2 C2 1.177(6) . ? O3 C3 1.156(5) . ? O4 C4 1.150(5) . ? O5 C5 1.138(5) . ? O6 C6 1.146(6) . ? O7 C7 1.139(6) . ? C8 C9 1.531(6) . ? C8 C13 1.541(6) . ? C9 C10 1.530(6) . ? C10 C11 1.528(6) . ? C11 C12 1.518(7) . ? C12 C13 1.546(5) . ? C14 C15 1.533(6) . ? C14 C19 1.539(6) . ? C15 C16 1.534(6) . ? C16 C17 1.528(7) . ? C17 C18 1.524(6) . ? C18 C19 1.539(6) . ? C20 C25 1.527(6) . ? C20 C21 1.549(5) . ? C21 C22 1.528(6) . ? C22 C23 1.521(6) . ? C23 C24 1.530(6) . ? C24 C25 1.543(6) . ? C26 C31 1.529(6) . ? C26 C27 1.531(7) . ? C27 C28 1.537(7) . ? C28 C29 1.515(7) . ? C29 C30 1.513(7) . ? C30 C31 1.522(7) . ? C32 C33 1.531(6) . ? C32 C37 1.551(6) . ? C33 C34 1.542(6) . ? C34 C35 1.510(7) . ? C35 C36 1.528(7) . ? C36 C37 1.527(6) . ? C38 C43 1.530(6) . ? C38 C39 1.554(5) . ? C39 C40 1.540(7) . ? C41 C42 1.517(6) . ? C41 C40 1.523(7) . ? C42 C43 1.520(6) . ? 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 Fe1 C4 93.83(19) . . ? C3 Fe1 S2 88.29(15) . . ? C4 Fe1 S2 160.35(15) . . ? C3 Fe1 S1 158.07(16) . . ? C4 Fe1 S1 93.03(13) . . ? S2 Fe1 S1 78.49(4) . . ? C3 Fe1 P1 94.79(16) . . ? C4 Fe1 P1 95.77(15) . . ? S2 Fe1 P1 103.53(5) . . ? S1 Fe1 P1 105.21(5) . . ? C3 Fe1 Fe2 102.79(16) . . ? C4 Fe1 Fe2 105.02(15) . . ? S2 Fe1 Fe2 55.59(4) . . ? S1 Fe1 Fe2 55.29(3) . . ? P1 Fe1 Fe2 151.58(4) . . ? C7 Fe2 C6 100.2(2) . . ? C7 Fe2 C5 92.8(2) . . ? C6 Fe2 C5 98.8(2) . . ? C7 Fe2 S1 85.86(15) . . ? C6 Fe2 S1 137.23(16) . . ? C5 Fe2 S1 123.34(17) . . ? C7 Fe2 S2 162.06(16) . . ? C6 Fe2 S2 87.24(18) . . ? C5 Fe2 S2 102.20(17) . . ? S1 Fe2 S2 77.73(4) . . ? C7 Fe2 Fe1 120.38(15) . . ? C6 Fe2 Fe1 139.34(18) . . ? C5 Fe2 Fe1 78.68(15) . . ? S1 Fe2 Fe1 54.90(3) . . ? S2 Fe2 Fe1 54.64(3) . . ? C7 Fe2 Fe3 110.05(15) . . ? C6 Fe2 Fe3 84.46(17) . . ? C5 Fe2 Fe3 156.06(16) . . ? S1 Fe2 Fe3 54.29(3) . . ? S2 Fe2 Fe3 54.07(3) . . ? Fe1 Fe2 Fe3 83.47(3) . . ? C2 Fe3 C1 94.3(2) . . ? C2 Fe3 S2 102.63(14) . . ? C1 Fe3 S2 88.35(14) . . ? C2 Fe3 S1 99.78(15) . . ? C1 Fe3 S1 162.33(16) . . ? S2 Fe3 S1 78.25(4) . . ? C2 Fe3 P2 93.28(14) . . ? C1 Fe3 P2 91.87(14) . . ? S2 Fe3 P2 164.03(5) . . ? S1 Fe3 P2 97.87(4) . . ? C2 Fe3 Fe2 146.16(14) . . ? C1 Fe3 Fe2 108.25(17) . . ? S2 Fe3 Fe2 54.77(4) . . ? S1 Fe3 Fe2 54.48(3) . . ? P2 Fe3 Fe2 110.33(4) . . ? Fe1 S2 Fe3 101.06(5) . . ? Fe1 S2 Fe2 69.77(4) . . ? Fe3 S2 Fe2 71.16(4) . . ? Fe1 S1 Fe3 100.70(5) . . ? Fe1 S1 Fe2 69.81(4) . . ? Fe3 S1 Fe2 71.23(4) . . ? C14 P1 C20 106.0(2) . . ? C14 P1 C8 104.06(19) . . ? C20 P1 C8 103.5(2) . . ? C14 P1 Fe1 109.57(15) . . ? C20 P1 Fe1 116.37(15) . . ? C8 P1 Fe1 116.14(14) . . ? C38 P2 C32 105.6(2) . . ? C38 P2 C26 106.2(2) . . ? C32 P2 C26 102.8(2) . . ? C38 P2 Fe3 111.03(14) . . ? C32 P2 Fe3 111.56(13) . . ? C26 P2 Fe3 118.65(15) . . ? O1 C1 Fe3 173.6(4) . . ? O2 C2 Fe3 178.5(4) . . ? O3 C3 Fe1 174.7(4) . . ? O4 C4 Fe1 176.6(4) . . ? O5 C5 Fe2 173.8(4) . . ? O6 C6 Fe2 177.6(5) . . ? O7 C7 Fe2 178.0(4) . . ? C9 C8 C13 110.3(3) . . ? C9 C8 P1 113.8(3) . . ? C13 C8 P1 115.1(3) . . ? C10 C9 C8 111.6(4) . . ? C11 C10 C9 110.9(4) . . ? C12 C11 C10 110.7(4) . . ? C11 C12 C13 111.8(4) . . ? C8 C13 C12 110.1(4) . . ? C15 C14 C19 108.1(4) . . ? C15 C14 P1 111.8(3) . . ? C19 C14 P1 120.0(3) . . ? C14 C15 C16 110.9(3) . . ? C17 C16 C15 110.5(4) . . ? C18 C17 C16 110.7(4) . . ? C17 C18 C19 112.5(4) . . ? C18 C19 C14 109.1(4) . . ? C25 C20 C21 109.7(4) . . ? C25 C20 P1 111.8(3) . . ? C21 C20 P1 113.0(3) . . ? C22 C21 C20 110.5(4) . . ? C23 C22 C21 112.4(4) . . ? C22 C23 C24 111.6(4) . . ? C23 C24 C25 110.1(4) . . ? C20 C25 C24 111.4(4) . . ? C31 C26 C27 110.0(4) . . ? C31 C26 P2 111.2(3) . . ? C27 C26 P2 114.2(3) . . ? C26 C27 C28 111.2(4) . . ? C29 C28 C27 111.2(4) . . ? C30 C29 C28 109.4(5) . . ? C29 C30 C31 111.2(4) . . ? C30 C31 C26 112.4(4) . . ? C33 C32 C37 109.5(3) . . ? C33 C32 P2 119.5(3) . . ? C37 C32 P2 111.8(3) . . ? C32 C33 C34 109.7(3) . . ? C35 C34 C33 111.0(4) . . ? C34 C35 C36 111.3(4) . . ? C37 C36 C35 112.7(4) . . ? C36 C37 C32 110.8(4) . . ? C43 C38 C39 108.4(3) . . ? C43 C38 P2 116.9(3) . . ? C39 C38 P2 115.3(3) . . ? C40 C39 C38 110.6(4) . . ? C42 C41 C40 111.6(4) . . ? C41 C42 C43 110.8(4) . . ? C42 C43 C38 111.8(4) . . ? C41 C40 C39 111.9(4) . . ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 26.75 _diffrn_measured_fraction_theta_full 0.969 _refine_diff_density_max 0.615 _refine_diff_density_min -0.567 _refine_diff_density_rms 0.095