# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email gmoula@iitk.ac.in _publ_contact_author_name 'Golam Moula' loop_ _publ_author_name S.Sarkar G.Moula M.Bose B.Maiti data_16mayam _database_code_depnum_ccdc_archive 'CCDC 839360' #TrackingRef 'DMAD Cl.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C24 H20 P), C6 H6 Cl2 Fe Mo O5 S4' _chemical_formula_sum 'C54 H46 Cl2 Fe Mo O5 P2 S4' _chemical_formula_weight 1187.82 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.198(5) _cell_length_b 14.103(5) _cell_length_c 16.253(5) _cell_angle_alpha 92.955(5) _cell_angle_beta 109.280(5) _cell_angle_gamma 100.481(5) _cell_volume 2576.3(16) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.1 _cell_measurement_theta_max 28.4 _exptl_crystal_description needle _exptl_crystal_colour green _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.531 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1212 _exptl_absorpt_coefficient_mu 0.901 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.910 _exptl_absorpt_correction_T_max 0.934 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71069 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX' _diffrn_measurement_method /w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17141 _diffrn_reflns_av_R_equivalents 0.0403 _diffrn_reflns_av_sigmaI/netI 0.1030 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 28.35 _reflns_number_total 12887 _reflns_number_gt 8002 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART 5.628 (Bruker, 2003)' _computing_cell_refinement 'SAINT 6.45 ( Bruker, 2003)' _computing_data_reduction 'SAINT 6.45 (Bruker, 2003)' _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 2.1e, Ortep' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1421P)^2^+9.9670P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12887 _refine_ls_number_parameters 618 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1280 _refine_ls_R_factor_gt 0.0810 _refine_ls_wR_factor_ref 0.2491 _refine_ls_wR_factor_gt 0.2020 _refine_ls_goodness_of_fit_ref 1.167 _refine_ls_restrained_S_all 1.167 _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 0.92247(6) 0.31027(5) 0.20412(4) 0.02036(19) Uani 1 1 d . . . Fe1 Fe 1.15987(10) 0.29819(8) 0.27415(7) 0.0228(3) Uani 1 1 d . . . Cl1 Cl 1.28471(18) 0.36069(15) 0.41097(13) 0.0310(4) Uani 1 1 d . . . Cl2 Cl 1.25929(19) 0.22891(15) 0.20280(15) 0.0339(5) Uani 1 1 d . . . S1 S 0.84584(17) 0.37764(14) 0.06855(13) 0.0238(4) Uani 1 1 d . . . S2 S 0.76031(18) 0.17502(14) 0.12368(13) 0.0257(4) Uani 1 1 d . . . S3 S 1.09115(17) 0.41779(13) 0.20495(13) 0.0225(4) Uani 1 1 d . . . S4 S 1.00266(18) 0.18431(14) 0.26750(14) 0.0266(4) Uani 1 1 d . . . P1 P 0.83240(18) 0.64564(14) 0.28207(13) 0.0212(4) Uani 1 1 d . . . P2 P 0.69494(17) 0.05740(14) 0.69184(13) 0.0213(4) Uani 1 1 d . . . O1 O 0.8731(5) 0.3618(4) 0.2765(4) 0.0284(12) Uani 1 1 d . . . O2 O 0.5294(5) 0.0907(5) -0.0708(4) 0.0360(14) Uani 1 1 d . . . O3 O 0.4682(5) 0.1732(4) 0.0219(4) 0.0301(13) Uani 1 1 d . . . O4 O 0.6921(5) 0.4130(4) -0.0956(4) 0.0324(13) Uani 1 1 d . . . O5 O 0.5240(6) 0.3098(5) -0.1050(4) 0.0425(17) Uani 1 1 d . . . C1 C 0.7033(7) 0.3050(6) 0.0092(5) 0.0266(17) Uani 1 1 d . . . C2 C 0.6679(7) 0.2204(5) 0.0358(5) 0.0247(16) Uani 1 1 d . . . C3 C 0.5485(7) 0.1542(6) -0.0130(5) 0.0248(12) Uani 1 1 d . . . C4 C 0.6307(7) 0.3413(6) -0.0689(5) 0.0248(12) Uani 1 1 d . . . C5 C 0.6244(8) 0.4542(7) -0.1694(6) 0.039(2) Uani 1 1 d . . . H5A H 0.6769 0.5021 -0.1864 0.059 Uiso 1 1 calc R . . H5B H 0.5682 0.4841 -0.1538 0.059 Uiso 1 1 calc R . . H5C H 0.5828 0.4039 -0.2175 0.059 Uiso 1 1 calc R . . C6 C 0.3506(7) 0.1140(7) -0.0188(7) 0.037(2) Uani 1 1 d . . . H6A H 0.3033 0.1234 0.0166 0.056 Uiso 1 1 calc R . . H6B H 0.3554 0.0469 -0.0240 0.056 Uiso 1 1 calc R . . H6C H 0.3148 0.1323 -0.0761 0.056 Uiso 1 1 calc R . . C7 C 0.7134(6) 0.5513(5) 0.2849(5) 0.0215(15) Uani 1 1 d . . . C8 C 0.6667(7) 0.4701(5) 0.2195(6) 0.0267(17) Uani 1 1 d . . . H8 H 0.6931 0.4677 0.1720 0.032 Uiso 1 1 calc R . . C9 C 0.5820(8) 0.3944(6) 0.2261(7) 0.038(2) Uani 1 1 d . . . H9 H 0.5506 0.3411 0.1832 0.045 Uiso 1 1 calc R . . C10 C 0.5437(8) 0.3990(6) 0.2985(7) 0.037(2) Uani 1 1 d . . . H10 H 0.4867 0.3483 0.3035 0.045 Uiso 1 1 calc R . . C11 C 0.5894(8) 0.4774(7) 0.3615(7) 0.038(2) Uani 1 1 d . . . H11 H 0.5623 0.4795 0.4087 0.045 Uiso 1 1 calc R . . C12 C 0.6749(7) 0.5535(6) 0.3566(6) 0.0274(17) Uani 1 1 d . . . H12 H 0.7065 0.6057 0.4007 0.033 Uiso 1 1 calc R . . C13 C 0.7968(7) 0.7635(6) 0.2874(5) 0.0255(17) Uani 1 1 d . . . C14 C 0.6822(7) 0.7757(6) 0.2756(5) 0.0265(17) Uani 1 1 d . . . H14 H 0.6235 0.7233 0.2756 0.032 Uiso 1 1 calc R . . C15 C 0.6564(8) 0.8679(6) 0.2639(6) 0.0333(19) Uani 1 1 d . . . H15 H 0.5798 0.8769 0.2545 0.040 Uiso 1 1 calc R . . C16 C 0.7449(8) 0.9451(6) 0.2661(5) 0.0304(18) Uani 1 1 d . . . H16 H 0.7279 1.0065 0.2592 0.036 Uiso 1 1 calc R . . C17 C 0.8579(8) 0.9326(6) 0.2785(6) 0.0313(19) Uani 1 1 d . . . H17 H 0.9171 0.9853 0.2803 0.038 Uiso 1 1 calc R . . C18 C 0.8837(8) 0.8424(6) 0.2884(5) 0.0270(17) Uani 1 1 d . . . H18 H 0.9601 0.8340 0.2958 0.032 Uiso 1 1 calc R . . C19 C 0.9604(7) 0.6416(5) 0.3772(5) 0.0224(15) Uani 1 1 d . . . C20 C 0.9865(7) 0.7060(5) 0.4526(5) 0.0215(15) Uani 1 1 d . . . H20 H 0.9452 0.7556 0.4511 0.026 Uiso 1 1 calc R . . C21 C 1.0735(7) 0.6959(6) 0.5295(5) 0.0236(16) Uani 1 1 d . . . H21 H 1.0913 0.7386 0.5799 0.028 Uiso 1 1 calc R . . C22 C 1.1342(7) 0.6211(5) 0.5311(5) 0.0257(17) Uani 1 1 d . . . H22 H 1.1921 0.6134 0.5829 0.031 Uiso 1 1 calc R . . C23 C 1.1090(7) 0.5584(6) 0.4560(5) 0.0271(17) Uani 1 1 d . . . H23 H 1.1517 0.5099 0.4573 0.032 Uiso 1 1 calc R . . C24 C 1.0212(7) 0.5672(6) 0.3793(5) 0.0263(17) Uani 1 1 d . . . H24 H 1.0029 0.5236 0.3294 0.032 Uiso 1 1 calc R . . C25 C 0.8560(7) 0.6323(6) 0.1786(5) 0.0273(17) Uani 1 1 d . . . C26 C 0.9621(7) 0.6208(5) 0.1712(6) 0.0254(16) Uani 1 1 d . . . H26 H 1.0242 0.6144 0.2210 0.030 Uiso 1 1 calc R . . C27 C 0.9777(9) 0.6187(6) 0.0910(6) 0.037(2) Uani 1 1 d . . . H27 H 1.0488 0.6089 0.0861 0.045 Uiso 1 1 calc R . . C28 C 0.8858(9) 0.6314(6) 0.0178(6) 0.038(2) Uani 1 1 d . . . H28 H 0.8960 0.6306 -0.0365 0.045 Uiso 1 1 calc R . . C29 C 0.7790(9) 0.6452(6) 0.0237(6) 0.034(2) Uani 1 1 d . . . H29 H 0.7190 0.6546 -0.0262 0.041 Uiso 1 1 calc R . . C30 C 0.7609(9) 0.6451(7) 0.1042(6) 0.037(2) Uani 1 1 d . . . H30 H 0.6891 0.6532 0.1088 0.045 Uiso 1 1 calc R . . C31 C 0.8094(7) 0.0813(5) 0.7977(5) 0.0245(16) Uani 1 1 d . . . C32 C 0.9067(7) 0.0382(6) 0.8135(6) 0.0273(17) Uani 1 1 d . . . H32 H 0.9120 -0.0024 0.7687 0.033 Uiso 1 1 calc R . . C33 C 0.9958(8) 0.0546(7) 0.8946(6) 0.034(2) Uani 1 1 d . . . H33 H 1.0599 0.0242 0.9051 0.041 Uiso 1 1 calc R . . C34 C 0.9881(8) 0.1173(6) 0.9600(6) 0.0310(18) Uani 1 1 d . . . H34 H 1.0490 0.1313 1.0143 0.037 Uiso 1 1 calc R . . C35 C 0.8900(8) 0.1591(6) 0.9448(5) 0.0301(18) Uani 1 1 d . . . H35 H 0.8836 0.1983 0.9900 0.036 Uiso 1 1 calc R . . C36 C 0.8041(7) 0.1436(6) 0.8655(6) 0.0278(17) Uani 1 1 d . . . H36 H 0.7406 0.1745 0.8555 0.033 Uiso 1 1 calc R . . C37 C 0.6475(6) 0.1677(5) 0.6611(5) 0.0204(15) Uani 1 1 d . . . C38 C 0.5310(8) 0.1649(6) 0.6077(5) 0.0289(18) Uani 1 1 d . . . H38 H 0.4742 0.1072 0.5931 0.035 Uiso 1 1 calc R . . C39 C 0.5013(8) 0.2503(6) 0.5767(6) 0.0317(19) Uani 1 1 d . . . H39 H 0.4241 0.2496 0.5405 0.038 Uiso 1 1 calc R . . C40 C 0.5859(8) 0.3366(6) 0.5993(6) 0.0317(19) Uani 1 1 d . . . H40 H 0.5653 0.3927 0.5769 0.038 Uiso 1 1 calc R . . C41 C 0.7010(8) 0.3398(6) 0.6552(6) 0.0311(19) Uani 1 1 d . . . H41 H 0.7567 0.3982 0.6722 0.037 Uiso 1 1 calc R . . C42 C 0.7314(7) 0.2551(6) 0.6849(6) 0.0321(19) Uani 1 1 d . . . H42 H 0.8087 0.2562 0.7212 0.038 Uiso 1 1 calc R . . C43 C 0.7511(7) 0.0138(5) 0.6105(5) 0.0231(16) Uani 1 1 d . . . C44 C 0.7922(7) 0.0768(6) 0.5583(5) 0.0249(16) Uani 1 1 d . . . H44 H 0.7885 0.1420 0.5638 0.030 Uiso 1 1 calc R . . C45 C 0.8379(8) 0.0423(6) 0.4988(6) 0.0306(18) Uani 1 1 d . . . H45 H 0.8635 0.0836 0.4630 0.037 Uiso 1 1 calc R . . C46 C 0.8457(8) -0.0540(7) 0.4926(6) 0.0326(19) Uani 1 1 d . . . H46 H 0.8782 -0.0771 0.4533 0.039 Uiso 1 1 calc R . . C47 C 0.8063(7) -0.1160(6) 0.5439(5) 0.0256(17) Uani 1 1 d . . . H47 H 0.8123 -0.1807 0.5387 0.031 Uiso 1 1 calc R . . C48 C 0.7581(7) -0.0844(5) 0.6024(5) 0.0225(15) Uani 1 1 d . . . H48 H 0.7304 -0.1272 0.6363 0.027 Uiso 1 1 calc R . . C49 C 0.5725(7) -0.0338(5) 0.6928(5) 0.0228(15) Uani 1 1 d . . . C50 C 0.5521(7) -0.0438(6) 0.7721(5) 0.0254(16) Uani 1 1 d . . . H50 H 0.6018 -0.0043 0.8232 0.030 Uiso 1 1 calc R . . C51 C 0.4568(8) -0.1133(7) 0.7732(6) 0.0336(19) Uani 1 1 d . . . H51 H 0.4434 -0.1207 0.8259 0.040 Uiso 1 1 calc R . . C52 C 0.3809(7) -0.1723(6) 0.6977(6) 0.0263(17) Uani 1 1 d . . . H52 H 0.3160 -0.2176 0.6991 0.032 Uiso 1 1 calc R . . C53 C 0.4035(7) -0.1625(6) 0.6190(6) 0.0305(18) Uani 1 1 d . . . H53 H 0.3550 -0.2031 0.5682 0.037 Uiso 1 1 calc R . . C54 C 0.4966(7) -0.0935(6) 0.6169(5) 0.0274(17) Uani 1 1 d . . . H54 H 0.5095 -0.0862 0.5641 0.033 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 0.0212(3) 0.0218(3) 0.0183(3) 0.0020(2) 0.0062(3) 0.0063(2) Fe1 0.0200(6) 0.0238(6) 0.0235(6) 0.0024(4) 0.0053(5) 0.0061(4) Cl1 0.0294(10) 0.0324(10) 0.0248(10) 0.0017(8) 0.0016(8) 0.0064(8) Cl2 0.0299(11) 0.0344(11) 0.0415(12) 0.0004(9) 0.0160(9) 0.0112(9) S1 0.0231(9) 0.0257(10) 0.0191(9) 0.0041(7) 0.0024(7) 0.0049(7) S2 0.0273(10) 0.0266(10) 0.0247(10) 0.0061(8) 0.0109(8) 0.0049(8) S3 0.0230(9) 0.0212(9) 0.0233(10) 0.0057(7) 0.0071(8) 0.0052(7) S4 0.0276(10) 0.0216(9) 0.0304(11) 0.0045(8) 0.0092(8) 0.0062(8) P1 0.0240(10) 0.0202(9) 0.0195(10) 0.0004(7) 0.0079(8) 0.0047(7) P2 0.0220(10) 0.0224(10) 0.0196(10) 0.0015(7) 0.0069(8) 0.0052(7) O1 0.032(3) 0.028(3) 0.024(3) 0.005(2) 0.008(2) 0.004(2) O2 0.032(3) 0.039(4) 0.032(3) -0.005(3) 0.011(3) -0.001(3) O3 0.021(3) 0.037(3) 0.030(3) 0.000(3) 0.009(2) 0.002(2) O4 0.026(3) 0.037(3) 0.031(3) 0.008(3) 0.005(3) 0.007(3) O5 0.036(4) 0.050(4) 0.032(4) 0.019(3) 0.003(3) -0.001(3) C1 0.021(4) 0.033(4) 0.020(4) -0.001(3) -0.001(3) 0.010(3) C2 0.029(4) 0.022(4) 0.031(4) -0.002(3) 0.021(4) 0.006(3) C3 0.022(3) 0.025(3) 0.019(3) 0.000(2) -0.001(2) 0.000(2) C4 0.022(3) 0.025(3) 0.019(3) 0.000(2) -0.001(2) 0.000(2) C5 0.027(5) 0.052(6) 0.036(5) 0.019(4) 0.003(4) 0.015(4) C6 0.020(4) 0.034(5) 0.049(6) 0.001(4) 0.007(4) -0.003(3) C7 0.021(4) 0.023(4) 0.019(4) -0.001(3) 0.005(3) 0.005(3) C8 0.025(4) 0.020(4) 0.030(4) 0.000(3) 0.003(3) 0.004(3) C9 0.028(4) 0.028(4) 0.046(6) 0.001(4) -0.002(4) 0.005(4) C10 0.029(5) 0.024(4) 0.049(6) 0.011(4) 0.002(4) -0.002(3) C11 0.034(5) 0.036(5) 0.051(6) 0.027(4) 0.017(4) 0.016(4) C12 0.023(4) 0.028(4) 0.032(4) 0.005(3) 0.011(3) 0.004(3) C13 0.036(4) 0.030(4) 0.020(4) 0.013(3) 0.014(3) 0.018(3) C14 0.029(4) 0.026(4) 0.022(4) 0.000(3) 0.007(3) 0.001(3) C15 0.031(4) 0.037(5) 0.034(5) 0.007(4) 0.008(4) 0.017(4) C16 0.047(5) 0.027(4) 0.020(4) 0.008(3) 0.013(4) 0.012(4) C17 0.038(5) 0.032(4) 0.029(5) 0.009(4) 0.020(4) 0.003(4) C18 0.031(4) 0.028(4) 0.024(4) 0.007(3) 0.011(3) 0.006(3) C19 0.022(4) 0.023(4) 0.016(4) 0.002(3) 0.003(3) -0.002(3) C20 0.026(4) 0.020(4) 0.021(4) 0.004(3) 0.009(3) 0.009(3) C21 0.035(4) 0.025(4) 0.013(3) 0.001(3) 0.010(3) 0.009(3) C22 0.023(4) 0.024(4) 0.026(4) 0.012(3) 0.002(3) 0.002(3) C23 0.031(4) 0.031(4) 0.026(4) 0.007(3) 0.015(4) 0.014(3) C24 0.030(4) 0.026(4) 0.027(4) 0.002(3) 0.013(3) 0.008(3) C25 0.028(4) 0.031(4) 0.018(4) 0.000(3) 0.005(3) 0.003(3) C26 0.031(4) 0.021(4) 0.029(4) 0.000(3) 0.018(4) 0.005(3) C27 0.052(6) 0.028(5) 0.037(5) 0.000(4) 0.024(5) 0.003(4) C28 0.066(7) 0.025(4) 0.022(4) 0.003(3) 0.016(4) 0.006(4) C29 0.044(5) 0.038(5) 0.022(4) 0.000(4) 0.016(4) 0.006(4) C30 0.041(5) 0.046(5) 0.018(4) 0.001(4) 0.002(4) 0.009(4) C31 0.028(4) 0.019(4) 0.026(4) 0.003(3) 0.010(3) 0.003(3) C32 0.017(4) 0.036(4) 0.027(4) 0.000(3) 0.005(3) 0.007(3) C33 0.035(5) 0.037(5) 0.030(5) 0.011(4) 0.008(4) 0.011(4) C34 0.031(4) 0.038(5) 0.023(4) 0.007(4) 0.010(4) 0.002(4) C35 0.039(5) 0.030(4) 0.015(4) -0.010(3) 0.006(3) 0.000(4) C36 0.030(4) 0.025(4) 0.031(4) -0.002(3) 0.012(4) 0.008(3) C37 0.018(3) 0.022(4) 0.022(4) 0.003(3) 0.007(3) 0.009(3) C38 0.036(5) 0.027(4) 0.020(4) -0.001(3) 0.007(3) 0.004(3) C39 0.039(5) 0.031(4) 0.030(5) 0.007(4) 0.015(4) 0.012(4) C40 0.041(5) 0.025(4) 0.032(5) 0.006(3) 0.014(4) 0.013(4) C41 0.029(4) 0.021(4) 0.039(5) 0.003(3) 0.011(4) -0.002(3) C42 0.018(4) 0.030(4) 0.044(5) -0.003(4) 0.003(4) 0.009(3) C43 0.022(4) 0.023(4) 0.019(4) 0.003(3) 0.003(3) 0.000(3) C44 0.029(4) 0.022(4) 0.028(4) 0.011(3) 0.013(3) 0.008(3) C45 0.039(5) 0.025(4) 0.035(5) 0.001(3) 0.021(4) 0.006(3) C46 0.031(4) 0.043(5) 0.024(4) 0.001(4) 0.008(4) 0.013(4) C47 0.033(4) 0.019(4) 0.032(4) 0.004(3) 0.021(4) 0.008(3) C48 0.032(4) 0.021(4) 0.017(4) 0.006(3) 0.008(3) 0.012(3) C49 0.027(4) 0.017(3) 0.027(4) 0.004(3) 0.010(3) 0.010(3) C50 0.026(4) 0.030(4) 0.025(4) 0.003(3) 0.015(3) 0.007(3) C51 0.033(5) 0.040(5) 0.035(5) 0.012(4) 0.017(4) 0.014(4) C52 0.022(4) 0.025(4) 0.038(5) 0.011(3) 0.014(3) 0.009(3) C53 0.028(4) 0.032(4) 0.031(5) 0.003(4) 0.011(4) 0.004(3) C54 0.033(4) 0.030(4) 0.019(4) 0.002(3) 0.009(3) 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 Mo1 O1 1.677(6) . ? Mo1 S4 2.308(2) . ? Mo1 S3 2.319(2) . ? Mo1 S1 2.410(2) . ? Mo1 S2 2.434(2) . ? Mo1 Fe1 2.7809(17) . ? Fe1 S3 2.214(2) . ? Fe1 S4 2.235(2) . ? Fe1 Cl2 2.239(2) . ? Fe1 Cl1 2.261(2) . ? S1 C1 1.774(8) . ? S2 C2 1.736(9) . ? P1 C7 1.796(8) . ? P1 C13 1.798(8) . ? P1 C25 1.804(8) . ? P1 C19 1.811(8) . ? P2 C49 1.790(8) . ? P2 C31 1.791(8) . ? P2 C37 1.794(7) . ? P2 C43 1.806(8) . ? O2 C3 1.196(10) . ? O3 C3 1.341(10) . ? O3 C6 1.440(9) . ? O4 C4 1.325(9) . ? O4 C5 1.431(10) . ? O5 C4 1.223(9) . ? C1 C2 1.337(11) . ? C1 C4 1.466(11) . ? C2 C3 1.512(11) . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 C12 1.395(11) . ? C7 C8 1.416(11) . ? C8 C9 1.379(12) . ? C8 H8 0.9300 . ? C9 C10 1.404(14) . ? C9 H9 0.9300 . ? C10 C11 1.365(14) . ? C10 H10 0.9300 . ? C11 C12 1.379(11) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C18 1.385(11) . ? C13 C14 1.391(11) . ? C14 C15 1.400(12) . ? C14 H14 0.9300 . ? C15 C16 1.377(12) . ? C15 H15 0.9300 . ? C16 C17 1.371(12) . ? C16 H16 0.9300 . ? C17 C18 1.370(12) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 C24 1.387(11) . ? C19 C20 1.396(10) . ? C20 C21 1.381(11) . ? C20 H20 0.9300 . ? C21 C22 1.391(11) . ? C21 H21 0.9300 . ? C22 C23 1.381(11) . ? C22 H22 0.9300 . ? C23 C24 1.378(11) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 C26 1.375(11) . ? C25 C30 1.420(12) . ? C26 C27 1.377(12) . ? C26 H26 0.9300 . ? C27 C28 1.386(14) . ? C27 H27 0.9300 . ? C28 C29 1.385(13) . ? C28 H28 0.9300 . ? C29 C30 1.396(12) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? C31 C32 1.387(11) . ? C31 C36 1.398(11) . ? C32 C33 1.379(12) . ? C32 H32 0.9300 . ? C33 C34 1.386(12) . ? C33 H33 0.9300 . ? C34 C35 1.384(12) . ? C34 H34 0.9300 . ? C35 C36 1.343(11) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? C37 C38 1.391(11) . ? C37 C42 1.396(11) . ? C38 C39 1.392(12) . ? C38 H38 0.9300 . ? C39 C40 1.388(12) . ? C39 H39 0.9300 . ? C40 C41 1.389(12) . ? C40 H40 0.9300 . ? C41 C42 1.379(12) . ? C41 H41 0.9300 . ? C42 H42 0.9300 . ? C43 C44 1.400(10) . ? C43 C48 1.405(10) . ? C44 C45 1.374(11) . ? C44 H44 0.9300 . ? C45 C46 1.380(12) . ? C45 H45 0.9300 . ? C46 C47 1.370(11) . ? C46 H46 0.9300 . ? C47 C48 1.368(10) . ? C47 H47 0.9300 . ? C48 H48 0.9300 . ? C49 C54 1.393(11) . ? C49 C50 1.402(11) . ? C50 C51 1.383(12) . ? C50 H50 0.9300 . ? C51 C52 1.386(13) . ? C51 H51 0.9300 . ? C52 C53 1.403(12) . ? C52 H52 0.9300 . ? C53 C54 1.366(11) . ? C53 H53 0.9300 . ? C54 H54 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Mo1 S4 106.5(2) . . ? O1 Mo1 S3 106.7(2) . . ? S4 Mo1 S3 101.37(8) . . ? O1 Mo1 S1 106.7(2) . . ? S4 Mo1 S1 145.14(8) . . ? S3 Mo1 S1 79.04(7) . . ? O1 Mo1 S2 104.3(2) . . ? S4 Mo1 S2 80.95(8) . . ? S3 Mo1 S2 146.75(8) . . ? S1 Mo1 S2 80.78(7) . . ? O1 Mo1 Fe1 113.5(2) . . ? S4 Mo1 Fe1 51.06(6) . . ? S3 Mo1 Fe1 50.46(6) . . ? S1 Mo1 Fe1 121.71(6) . . ? S2 Mo1 Fe1 124.71(6) . . ? S3 Fe1 S4 107.19(9) . . ? S3 Fe1 Cl2 110.15(9) . . ? S4 Fe1 Cl2 106.37(9) . . ? S3 Fe1 Cl1 108.46(9) . . ? S4 Fe1 Cl1 115.46(9) . . ? Cl2 Fe1 Cl1 109.14(9) . . ? S3 Fe1 Mo1 53.89(6) . . ? S4 Fe1 Mo1 53.47(6) . . ? Cl2 Fe1 Mo1 125.45(8) . . ? Cl1 Fe1 Mo1 125.39(7) . . ? C1 S1 Mo1 107.3(3) . . ? C2 S2 Mo1 106.5(3) . . ? Fe1 S3 Mo1 75.65(7) . . ? Fe1 S4 Mo1 75.47(7) . . ? C7 P1 C13 111.7(4) . . ? C7 P1 C25 110.8(4) . . ? C13 P1 C25 104.1(4) . . ? C7 P1 C19 106.7(3) . . ? C13 P1 C19 109.2(4) . . ? C25 P1 C19 114.5(4) . . ? C49 P2 C31 110.4(4) . . ? C49 P2 C37 110.7(3) . . ? C31 P2 C37 109.5(4) . . ? C49 P2 C43 108.0(4) . . ? C31 P2 C43 110.2(4) . . ? C37 P2 C43 108.0(4) . . ? C3 O3 C6 115.0(6) . . ? C4 O4 C5 115.5(6) . . ? C2 C1 C4 123.3(7) . . ? C2 C1 S1 119.6(6) . . ? C4 C1 S1 117.1(6) . . ? C1 C2 C3 122.2(8) . . ? C1 C2 S2 122.1(6) . . ? C3 C2 S2 115.5(6) . . ? O2 C3 O3 124.7(7) . . ? O2 C3 C2 125.4(8) . . ? O3 C3 C2 109.8(6) . . ? O5 C4 O4 123.4(7) . . ? O5 C4 C1 123.5(7) . . ? O4 C4 C1 113.2(7) . . ? O4 C5 H5A 109.5 . . ? O4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? O4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? O3 C6 H6A 109.5 . . ? O3 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? O3 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C12 C7 C8 119.6(7) . . ? C12 C7 P1 119.6(6) . . ? C8 C7 P1 120.5(6) . . ? C9 C8 C7 120.0(8) . . ? C9 C8 H8 120.0 . . ? C7 C8 H8 120.0 . . ? C8 C9 C10 119.2(8) . . ? C8 C9 H9 120.4 . . ? C10 C9 H9 120.4 . . ? C11 C10 C9 120.6(8) . . ? C11 C10 H10 119.7 . . ? C9 C10 H10 119.7 . . ? C10 C11 C12 121.2(9) . . ? C10 C11 H11 119.4 . . ? C12 C11 H11 119.4 . . ? C11 C12 C7 119.4(8) . . ? C11 C12 H12 120.3 . . ? C7 C12 H12 120.3 . . ? C18 C13 C14 119.9(7) . . ? C18 C13 P1 116.8(6) . . ? C14 C13 P1 122.4(6) . . ? C13 C14 C15 119.1(8) . . ? C13 C14 H14 120.5 . . ? C15 C14 H14 120.5 . . ? C16 C15 C14 119.8(8) . . ? C16 C15 H15 120.1 . . ? C14 C15 H15 120.1 . . ? C17 C16 C15 120.7(8) . . ? C17 C16 H16 119.6 . . ? C15 C16 H16 119.6 . . ? C18 C17 C16 120.1(8) . . ? C18 C17 H17 120.0 . . ? C16 C17 H17 120.0 . . ? C17 C18 C13 120.5(8) . . ? C17 C18 H18 119.8 . . ? C13 C18 H18 119.8 . . ? C24 C19 C20 120.2(7) . . ? C24 C19 P1 120.2(6) . . ? C20 C19 P1 118.9(6) . . ? C21 C20 C19 120.0(7) . . ? C21 C20 H20 120.0 . . ? C19 C20 H20 120.0 . . ? C20 C21 C22 119.5(7) . . ? C20 C21 H21 120.3 . . ? C22 C21 H21 120.3 . . ? C23 C22 C21 120.3(7) . . ? C23 C22 H22 119.8 . . ? C21 C22 H22 119.8 . . ? C24 C23 C22 120.6(7) . . ? C24 C23 H23 119.7 . . ? C22 C23 H23 119.7 . . ? C23 C24 C19 119.4(7) . . ? C23 C24 H24 120.3 . . ? C19 C24 H24 120.3 . . ? C26 C25 C30 120.8(8) . . ? C26 C25 P1 123.6(6) . . ? C30 C25 P1 115.2(6) . . ? C25 C26 C27 121.0(9) . . ? C25 C26 H26 119.5 . . ? C27 C26 H26 119.5 . . ? C26 C27 C28 118.9(9) . . ? C26 C27 H27 120.5 . . ? C28 C27 H27 120.5 . . ? C29 C28 C27 121.3(8) . . ? C29 C28 H28 119.4 . . ? C27 C28 H28 119.4 . . ? C28 C29 C30 120.4(9) . . ? C28 C29 H29 119.8 . . ? C30 C29 H29 119.8 . . ? C29 C30 C25 117.6(9) . . ? C29 C30 H30 121.2 . . ? C25 C30 H30 121.2 . . ? C32 C31 C36 118.6(8) . . ? C32 C31 P2 119.7(6) . . ? C36 C31 P2 121.7(6) . . ? C33 C32 C31 121.1(8) . . ? C33 C32 H32 119.4 . . ? C31 C32 H32 119.4 . . ? C32 C33 C34 118.7(8) . . ? C32 C33 H33 120.6 . . ? C34 C33 H33 120.6 . . ? C35 C34 C33 120.2(8) . . ? C35 C34 H34 119.9 . . ? C33 C34 H34 119.9 . . ? C36 C35 C34 120.7(8) . . ? C36 C35 H35 119.6 . . ? C34 C35 H35 119.6 . . ? C35 C36 C31 120.6(8) . . ? C35 C36 H36 119.7 . . ? C31 C36 H36 119.7 . . ? C38 C37 C42 120.4(7) . . ? C38 C37 P2 120.4(6) . . ? C42 C37 P2 119.0(6) . . ? C37 C38 C39 118.6(8) . . ? C37 C38 H38 120.7 . . ? C39 C38 H38 120.7 . . ? C40 C39 C38 120.7(8) . . ? C40 C39 H39 119.7 . . ? C38 C39 H39 119.7 . . ? C41 C40 C39 120.6(8) . . ? C41 C40 H40 119.7 . . ? C39 C40 H40 119.7 . . ? C42 C41 C40 118.9(7) . . ? C42 C41 H41 120.5 . . ? C40 C41 H41 120.5 . . ? C41 C42 C37 120.8(7) . . ? C41 C42 H42 119.6 . . ? C37 C42 H42 119.6 . . ? C44 C43 C48 119.7(7) . . ? C44 C43 P2 121.2(6) . . ? C48 C43 P2 119.1(6) . . ? C45 C44 C43 120.0(7) . . ? C45 C44 H44 120.0 . . ? C43 C44 H44 120.0 . . ? C44 C45 C46 119.6(8) . . ? C44 C45 H45 120.2 . . ? C46 C45 H45 120.2 . . ? C47 C46 C45 120.7(8) . . ? C47 C46 H46 119.6 . . ? C45 C46 H46 119.6 . . ? C48 C47 C46 121.1(7) . . ? C48 C47 H47 119.4 . . ? C46 C47 H47 119.4 . . ? C47 C48 C43 118.9(7) . . ? C47 C48 H48 120.6 . . ? C43 C48 H48 120.6 . . ? C54 C49 C50 119.5(7) . . ? C54 C49 P2 121.9(6) . . ? C50 C49 P2 118.6(6) . . ? C51 C50 C49 119.0(8) . . ? C51 C50 H50 120.5 . . ? C49 C50 H50 120.5 . . ? C50 C51 C52 121.5(8) . . ? C50 C51 H51 119.3 . . ? C52 C51 H51 119.3 . . ? C51 C52 C53 118.9(7) . . ? C51 C52 H52 120.5 . . ? C53 C52 H52 120.5 . . ? C54 C53 C52 120.0(8) . . ? C54 C53 H53 120.0 . . ? C52 C53 H53 120.0 . . ? C53 C54 C49 121.0(8) . . ? C53 C54 H54 119.5 . . ? C49 C54 H54 119.5 . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 28.35 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.860 _refine_diff_density_min -0.729 _refine_diff_density_rms 0.244 # Attachment 'TDT Cl.txt' data_24julam _database_code_depnum_ccdc_archive 'CCDC 839362' #TrackingRef 'TDT Cl.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C55 H46 Cl2 Fe Mo O P2 S4' _chemical_formula_sum 'C55 H46 Cl2 Fe Mo O P2 S4' _chemical_formula_weight 1135.79 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 P21/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 11.000(5) _cell_length_b 20.675(5) _cell_length_c 22.984(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 99.197(5) _cell_angle_gamma 90.000(5) _cell_volume 5160(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.462 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2320 _exptl_absorpt_coefficient_mu 0.891 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.958 _exptl_absorpt_correction_T_max 0.982 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32636 _diffrn_reflns_av_R_equivalents 0.0903 _diffrn_reflns_av_sigmaI/netI 0.1270 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 28.33 _reflns_number_total 12704 _reflns_number_gt 7404 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SMART' _computing_structure_solution 'Bruker SMART' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP-3 _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0608P)^2^+8.8694P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0019(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 12704 _refine_ls_number_parameters 596 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1434 _refine_ls_R_factor_gt 0.0754 _refine_ls_wR_factor_ref 0.1906 _refine_ls_wR_factor_gt 0.1450 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _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 C1 C 0.6657(6) 0.7649(3) 0.5411(3) 0.0304(14) Uani 1 1 d . . . C2 C 0.7656(6) 0.7701(3) 0.5871(3) 0.0376(16) Uani 1 1 d . . . H2 H 0.8449 0.7634 0.5791 0.045 Uiso 1 1 calc R . . C3 C 0.7495(7) 0.7850(3) 0.6442(3) 0.0378(17) Uani 1 1 d . . . C4 C 0.6303(7) 0.7965(3) 0.6547(3) 0.0401(17) Uani 1 1 d . . . H4 H 0.6176 0.8077 0.6925 0.048 Uiso 1 1 calc R . . C5 C 0.5310(7) 0.7915(3) 0.6102(3) 0.0413(17) Uani 1 1 d . . . H5 H 0.4522 0.7994 0.6184 0.050 Uiso 1 1 calc R . . C6 C 0.5462(6) 0.7749(3) 0.5532(3) 0.0322(15) Uani 1 1 d . . . C7 C 0.8588(7) 0.7873(4) 0.6935(3) 0.051(2) Uani 1 1 d . . . H7A H 0.9329 0.7784 0.6778 0.077 Uiso 1 1 calc R . . H7B H 0.8484 0.7556 0.7227 0.077 Uiso 1 1 calc R . . H7C H 0.8643 0.8296 0.7110 0.077 Uiso 1 1 calc R . . C8 C 0.9204(5) 0.0881(3) 0.5893(3) 0.0265(13) Uani 1 1 d . . . C9 C 1.0487(5) 0.0884(3) 0.5929(3) 0.0278(14) Uani 1 1 d . . . H9 H 1.0926 0.0499 0.5980 0.033 Uiso 1 1 calc R . . C10 C 1.1100(6) 0.1461(3) 0.5887(3) 0.0333(15) Uani 1 1 d . . . H10 H 1.1953 0.1466 0.5912 0.040 Uiso 1 1 calc R . . C11 C 1.0446(7) 0.2027(3) 0.5809(3) 0.0371(16) Uani 1 1 d . . . H11 H 1.0864 0.2414 0.5783 0.045 Uiso 1 1 calc R . . C12 C 0.9185(6) 0.2035(3) 0.5770(3) 0.0396(17) Uani 1 1 d . . . H12 H 0.8758 0.2424 0.5721 0.047 Uiso 1 1 calc R . . C13 C 0.8559(6) 0.1460(3) 0.5803(3) 0.0355(16) Uani 1 1 d . . . H13 H 0.7705 0.1461 0.5764 0.043 Uiso 1 1 calc R . . C14 C 0.7665(6) 0.0206(3) 0.6625(3) 0.0296(14) Uani 1 1 d . . . C15 C 0.7483(6) 0.0789(3) 0.6897(3) 0.0382(17) Uani 1 1 d . . . H15 H 0.7763 0.1172 0.6751 0.046 Uiso 1 1 calc R . . C16 C 0.6888(7) 0.0806(4) 0.7384(3) 0.0447(18) Uani 1 1 d . . . H16 H 0.6768 0.1198 0.7566 0.054 Uiso 1 1 calc R . . C17 C 0.6471(7) 0.0235(4) 0.7599(3) 0.0451(19) Uani 1 1 d . . . H17 H 0.6054 0.0244 0.7920 0.054 Uiso 1 1 calc R . . C18 C 0.6672(7) -0.0349(3) 0.7338(3) 0.0430(18) Uani 1 1 d . . . H18 H 0.6405 -0.0731 0.7489 0.052 Uiso 1 1 calc R . . C19 C 0.7261(6) -0.0366(3) 0.6859(3) 0.0375(16) Uani 1 1 d . . . H19 H 0.7395 -0.0761 0.6686 0.045 Uiso 1 1 calc R . . C20 C 0.9489(5) -0.0496(3) 0.6104(3) 0.0266(13) Uani 1 1 d . . . C21 C 1.0315(6) -0.0529(3) 0.6630(3) 0.0358(16) Uani 1 1 d . . . H21 H 1.0228 -0.0245 0.6934 0.043 Uiso 1 1 calc R . . C22 C 1.1264(6) -0.0976(3) 0.6707(3) 0.0376(17) Uani 1 1 d . . . H22 H 1.1833 -0.0984 0.7053 0.045 Uiso 1 1 calc R . . C23 C 1.1347(6) -0.1410(3) 0.6262(3) 0.0341(16) Uani 1 1 d . . . H23 H 1.1971 -0.1717 0.6313 0.041 Uiso 1 1 calc R . . C24 C 1.0532(6) -0.1399(3) 0.5746(3) 0.0350(15) Uani 1 1 d . . . H24 H 1.0609 -0.1699 0.5452 0.042 Uiso 1 1 calc R . . C25 C 0.9592(6) -0.0946(3) 0.5658(3) 0.0287(14) Uani 1 1 d . . . H25 H 0.9037 -0.0940 0.5308 0.034 Uiso 1 1 calc R . . C26 C 0.7336(6) -0.0022(3) 0.5328(3) 0.0296(14) Uani 1 1 d . . . C27 C 0.6547(6) -0.0548(3) 0.5313(3) 0.0315(15) Uani 1 1 d . . . H27 H 0.6532 -0.0792 0.5652 0.038 Uiso 1 1 calc R . . C28 C 0.5784(6) -0.0711(3) 0.4795(3) 0.0359(16) Uani 1 1 d . . . H28 H 0.5264 -0.1067 0.4786 0.043 Uiso 1 1 calc R . . C29 C 0.5789(6) -0.0346(3) 0.4288(3) 0.0375(17) Uani 1 1 d . . . H29 H 0.5271 -0.0454 0.3941 0.045 Uiso 1 1 calc R . . C30 C 0.6571(6) 0.0175(4) 0.4304(3) 0.0403(17) Uani 1 1 d . . . H30 H 0.6585 0.0419 0.3965 0.048 Uiso 1 1 calc R . . C31 C 0.7340(6) 0.0342(3) 0.4822(3) 0.0355(16) Uani 1 1 d . . . H31 H 0.7858 0.0698 0.4829 0.043 Uiso 1 1 calc R . . C32 C 0.9532(5) 0.6081(3) 0.5829(3) 0.0289(14) Uani 1 1 d . . . C33 C 0.9818(6) 0.6130(3) 0.5263(3) 0.0337(15) Uani 1 1 d . . . H33 H 0.9377 0.5889 0.4959 0.040 Uiso 1 1 calc R . . C34 C 1.0748(6) 0.6533(3) 0.5149(4) 0.0421(18) Uani 1 1 d . . . H34 H 1.0927 0.6570 0.4768 0.051 Uiso 1 1 calc R . . C35 C 1.1411(6) 0.6881(3) 0.5601(4) 0.0435(19) Uani 1 1 d . . . H35 H 1.2052 0.7145 0.5526 0.052 Uiso 1 1 calc R . . C36 C 1.1136(6) 0.6844(3) 0.6164(4) 0.0453(19) Uani 1 1 d . . . H36 H 1.1586 0.7085 0.6466 0.054 Uiso 1 1 calc R . . C37 C 1.0197(6) 0.6448(3) 0.6281(3) 0.0416(18) Uani 1 1 d . . . H37 H 1.0006 0.6425 0.6660 0.050 Uiso 1 1 calc R . . C38 C 0.7663(5) 0.5790(3) 0.6568(3) 0.0280(14) Uani 1 1 d . . . C39 C 0.6578(6) 0.6147(3) 0.6403(3) 0.0344(15) Uani 1 1 d . . . H39 H 0.6274 0.6214 0.6007 0.041 Uiso 1 1 calc R . . C40 C 0.5958(7) 0.6401(3) 0.6831(3) 0.0421(18) Uani 1 1 d . . . H40 H 0.5235 0.6633 0.6718 0.050 Uiso 1 1 calc R . . C41 C 0.6393(7) 0.6314(3) 0.7413(3) 0.0459(19) Uani 1 1 d . . . H41 H 0.5964 0.6480 0.7697 0.055 Uiso 1 1 calc R . . C42 C 0.7474(8) 0.5977(4) 0.7580(4) 0.062(2) Uani 1 1 d . . . H42 H 0.7780 0.5925 0.7978 0.074 Uiso 1 1 calc R . . C43 C 0.8111(7) 0.5716(4) 0.7163(3) 0.0460(19) Uani 1 1 d . . . H43 H 0.8840 0.5491 0.7282 0.055 Uiso 1 1 calc R . . C44 C 0.9408(5) 0.4800(3) 0.6297(3) 0.0250(13) Uani 1 1 d . . . C45 C 1.0620(6) 0.4740(3) 0.6179(3) 0.0326(15) Uani 1 1 d . . . H45 H 1.0969 0.5068 0.5983 0.039 Uiso 1 1 calc R . . C46 C 1.1283(6) 0.4192(3) 0.6358(3) 0.0367(16) Uani 1 1 d . . . H46 H 1.2084 0.4151 0.6281 0.044 Uiso 1 1 calc R . . C47 C 1.0787(6) 0.3707(3) 0.6646(3) 0.0305(14) Uani 1 1 d . . . H47 H 1.1248 0.3336 0.6755 0.037 Uiso 1 1 calc R . . C48 C 0.9608(5) 0.3758(3) 0.6779(3) 0.0301(14) Uani 1 1 d . . . H48 H 0.9278 0.3428 0.6980 0.036 Uiso 1 1 calc R . . C49 C 0.8919(5) 0.4315(3) 0.6604(3) 0.0261(13) Uani 1 1 d . . . H49 H 0.8129 0.4358 0.6695 0.031 Uiso 1 1 calc R . . C50 C 0.7441(5) 0.5245(3) 0.5372(3) 0.0250(13) Uani 1 1 d . . . C51 C 0.6918(5) 0.5719(3) 0.4971(3) 0.0328(15) Uani 1 1 d . . . H51 H 0.7113 0.6152 0.5041 0.039 Uiso 1 1 calc R . . C52 C 0.6112(6) 0.5540(3) 0.4472(3) 0.0366(16) Uani 1 1 d . . . H52 H 0.5756 0.5854 0.4208 0.044 Uiso 1 1 calc R . . C53 C 0.5840(6) 0.4897(4) 0.4366(3) 0.0352(16) Uani 1 1 d . . . H53 H 0.5316 0.4778 0.4025 0.042 Uiso 1 1 calc R . . C54 C 0.6339(5) 0.4425(3) 0.4763(3) 0.0330(15) Uani 1 1 d . . . H54 H 0.6132 0.3993 0.4693 0.040 Uiso 1 1 calc R . . C55 C 0.7143(5) 0.4599(3) 0.5262(3) 0.0275(14) Uani 1 1 d . . . H55 H 0.7488 0.4283 0.5526 0.033 Uiso 1 1 calc R . . O1 O 0.4765(4) 0.8313(2) 0.3793(2) 0.0411(12) Uani 1 1 d . . . P1 P 0.84003(14) 0.01478(8) 0.59860(7) 0.0265(4) Uani 1 1 d . . . P2 P 0.84907(14) 0.54809(8) 0.60194(7) 0.0261(4) Uani 1 1 d . . . S1 S 0.68800(14) 0.74412(8) 0.46945(7) 0.0314(4) Uani 1 1 d . . . S2 S 0.41994(15) 0.76031(8) 0.49761(8) 0.0351(4) Uani 1 1 d . . . S3 S 0.31151(14) 0.69992(9) 0.37891(8) 0.0369(4) Uani 1 1 d . . . S4 S 0.61361(14) 0.70464(8) 0.34118(8) 0.0334(4) Uani 1 1 d . . . Cl1 Cl 0.34619(17) 0.73585(8) 0.22565(8) 0.0438(4) Uani 1 1 d . . . Cl2 Cl 0.40265(14) 0.57265(8) 0.29011(8) 0.0370(4) Uani 1 1 d . . . Fe1 Fe 0.41957(8) 0.67886(4) 0.30742(4) 0.0279(2) Uani 1 1 d . . . Mo1 Mo 0.49503(5) 0.75469(2) 0.40380(2) 0.02652(15) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.036(3) 0.018(3) 0.033(4) 0.004(3) -0.004(3) -0.003(3) C2 0.043(4) 0.026(3) 0.041(4) 0.005(3) 0.000(3) -0.004(3) C3 0.057(4) 0.022(3) 0.030(4) 0.002(3) -0.009(3) -0.005(3) C4 0.053(4) 0.034(4) 0.034(4) -0.006(3) 0.011(3) -0.008(3) C5 0.052(4) 0.032(4) 0.040(4) 0.001(3) 0.007(3) -0.005(3) C6 0.042(4) 0.024(3) 0.031(4) 0.002(3) 0.008(3) -0.010(3) C7 0.068(5) 0.039(4) 0.043(5) 0.001(3) -0.004(4) -0.006(4) C8 0.029(3) 0.024(3) 0.027(3) 0.001(2) 0.007(3) 0.001(3) C9 0.032(3) 0.020(3) 0.030(4) 0.001(2) 0.001(3) -0.001(3) C10 0.032(3) 0.031(4) 0.038(4) -0.001(3) 0.008(3) 0.001(3) C11 0.051(4) 0.023(3) 0.042(4) 0.002(3) 0.024(3) -0.007(3) C12 0.047(4) 0.026(3) 0.052(5) 0.007(3) 0.025(4) 0.007(3) C13 0.038(4) 0.027(3) 0.043(4) 0.000(3) 0.012(3) 0.006(3) C14 0.029(3) 0.028(3) 0.032(4) 0.001(3) 0.009(3) 0.001(3) C15 0.035(4) 0.028(4) 0.054(5) 0.000(3) 0.015(3) -0.007(3) C16 0.055(5) 0.035(4) 0.050(5) -0.011(3) 0.027(4) -0.005(3) C17 0.053(4) 0.041(4) 0.047(5) -0.004(3) 0.025(4) -0.008(4) C18 0.056(4) 0.033(4) 0.046(5) 0.000(3) 0.027(4) -0.008(3) C19 0.041(4) 0.030(4) 0.044(4) -0.002(3) 0.014(3) -0.002(3) C20 0.031(3) 0.024(3) 0.026(3) 0.006(2) 0.009(3) 0.000(3) C21 0.047(4) 0.024(3) 0.034(4) -0.004(3) 0.000(3) 0.000(3) C22 0.040(4) 0.030(4) 0.039(4) 0.011(3) -0.006(3) -0.001(3) C23 0.030(3) 0.024(3) 0.050(5) 0.006(3) 0.008(3) 0.011(3) C24 0.038(4) 0.034(4) 0.037(4) 0.000(3) 0.017(3) 0.002(3) C25 0.032(3) 0.023(3) 0.032(4) 0.004(3) 0.008(3) -0.002(3) C26 0.030(3) 0.019(3) 0.039(4) -0.003(3) 0.004(3) 0.004(3) C27 0.037(3) 0.023(3) 0.033(4) 0.003(3) 0.001(3) 0.003(3) C28 0.042(4) 0.027(3) 0.037(4) 0.004(3) 0.003(3) 0.001(3) C29 0.028(3) 0.036(4) 0.045(4) -0.003(3) -0.004(3) 0.006(3) C30 0.029(3) 0.051(5) 0.038(4) 0.012(3) -0.002(3) 0.000(3) C31 0.033(3) 0.031(4) 0.041(4) 0.004(3) 0.001(3) -0.011(3) C32 0.027(3) 0.022(3) 0.035(4) 0.003(3) -0.003(3) 0.000(3) C33 0.035(3) 0.031(4) 0.036(4) 0.006(3) 0.010(3) -0.001(3) C34 0.038(4) 0.026(4) 0.067(5) 0.008(3) 0.022(4) 0.004(3) C35 0.024(3) 0.026(4) 0.080(6) 0.011(4) 0.009(4) 0.000(3) C36 0.043(4) 0.027(4) 0.059(5) 0.000(3) -0.013(4) -0.014(3) C37 0.040(4) 0.030(4) 0.050(5) 0.007(3) -0.007(3) -0.004(3) C38 0.029(3) 0.020(3) 0.034(4) 0.000(3) 0.005(3) 0.000(3) C39 0.036(3) 0.026(3) 0.043(4) 0.006(3) 0.012(3) -0.003(3) C40 0.044(4) 0.026(4) 0.059(5) 0.001(3) 0.018(4) 0.002(3) C41 0.058(5) 0.038(4) 0.045(5) -0.011(3) 0.016(4) 0.003(4) C42 0.069(6) 0.077(6) 0.037(5) -0.014(4) 0.000(4) 0.016(5) C43 0.053(4) 0.052(5) 0.029(4) -0.003(3) -0.002(3) 0.017(4) C44 0.028(3) 0.020(3) 0.027(3) 0.001(2) 0.002(3) -0.004(2) C45 0.029(3) 0.039(4) 0.029(4) 0.011(3) 0.005(3) -0.002(3) C46 0.028(3) 0.051(4) 0.033(4) 0.011(3) 0.007(3) 0.006(3) C47 0.037(3) 0.022(3) 0.031(4) 0.002(3) -0.001(3) 0.000(3) C48 0.031(3) 0.029(3) 0.029(4) 0.004(3) 0.002(3) -0.001(3) C49 0.023(3) 0.027(3) 0.028(3) 0.007(3) 0.004(3) -0.003(2) C50 0.023(3) 0.023(3) 0.028(3) 0.008(2) 0.001(3) 0.001(2) C51 0.030(3) 0.036(4) 0.031(4) 0.005(3) 0.002(3) -0.008(3) C52 0.033(3) 0.041(4) 0.034(4) 0.013(3) -0.002(3) -0.003(3) C53 0.032(3) 0.052(4) 0.021(3) -0.003(3) 0.001(3) -0.004(3) C54 0.026(3) 0.036(4) 0.037(4) -0.004(3) 0.005(3) -0.003(3) C55 0.026(3) 0.028(3) 0.029(4) 0.006(3) 0.005(3) 0.001(3) O1 0.059(3) 0.024(2) 0.036(3) 0.000(2) -0.004(2) -0.003(2) P1 0.0263(8) 0.0222(8) 0.0311(9) 0.0011(7) 0.0047(7) 0.0001(6) P2 0.0272(8) 0.0221(8) 0.0278(9) 0.0037(7) 0.0010(7) -0.0024(6) S1 0.0254(7) 0.0289(8) 0.0387(10) 0.0022(7) 0.0015(7) -0.0020(7) S2 0.0301(8) 0.0387(10) 0.0365(10) -0.0009(7) 0.0056(7) -0.0056(7) S3 0.0241(8) 0.0444(10) 0.0429(11) -0.0143(8) 0.0072(7) -0.0044(7) S4 0.0275(8) 0.0331(9) 0.0408(10) -0.0008(7) 0.0086(7) -0.0010(7) Cl1 0.0505(10) 0.0362(9) 0.0400(10) 0.0026(8) -0.0067(8) 0.0023(8) Cl2 0.0336(8) 0.0259(8) 0.0521(11) -0.0042(7) 0.0085(8) 0.0009(7) Fe1 0.0277(4) 0.0242(5) 0.0316(5) -0.0008(4) 0.0041(4) 0.0013(4) Mo1 0.0258(3) 0.0213(3) 0.0317(3) 0.0011(2) 0.0022(2) -0.0006(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C6 1.402(9) . ? C1 C2 1.402(9) . ? C1 S1 1.758(7) . ? C2 C3 1.386(9) . ? C3 C4 1.391(10) . ? C3 C7 1.515(9) . ? C4 C5 1.377(9) . ? C5 C6 1.389(9) . ? C6 S2 1.757(7) . ? C8 C13 1.391(8) . ? C8 C9 1.401(8) . ? C8 P1 1.784(6) . ? C9 C10 1.381(8) . ? C10 C11 1.369(9) . ? C11 C12 1.375(9) . ? C12 C13 1.381(9) . ? C14 C15 1.387(9) . ? C14 C19 1.402(9) . ? C14 P1 1.790(7) . ? C15 C16 1.385(9) . ? C16 C17 1.386(10) . ? C17 C18 1.381(10) . ? C18 C19 1.365(9) . ? C20 C21 1.392(8) . ? C20 C25 1.403(8) . ? C20 P1 1.781(6) . ? C21 C22 1.385(9) . ? C22 C23 1.374(9) . ? C23 C24 1.368(9) . ? C24 C25 1.386(8) . ? C26 C31 1.384(9) . ? C26 C27 1.390(8) . ? C26 P1 1.793(6) . ? C27 C28 1.384(9) . ? C28 C29 1.390(9) . ? C29 C30 1.376(9) . ? C30 C31 1.389(9) . ? C32 C33 1.389(9) . ? C32 C37 1.396(9) . ? C32 P2 1.790(6) . ? C33 C34 1.377(9) . ? C34 C35 1.373(10) . ? C35 C36 1.378(10) . ? C36 C37 1.378(9) . ? C38 C43 1.386(9) . ? C38 C39 1.403(8) . ? C38 P2 1.786(6) . ? C39 C40 1.386(9) . ? C40 C41 1.358(10) . ? C41 C42 1.378(11) . ? C42 C43 1.383(10) . ? C44 C49 1.384(8) . ? C44 C45 1.408(8) . ? C44 P2 1.789(6) . ? C45 C46 1.375(9) . ? C46 C47 1.363(9) . ? C47 C48 1.383(9) . ? C48 C49 1.401(8) . ? C50 C55 1.388(8) . ? C50 C51 1.404(8) . ? C50 P2 1.799(6) . ? C51 C52 1.383(9) . ? C52 C53 1.375(9) . ? C53 C54 1.389(9) . ? C54 C55 1.380(8) . ? O1 Mo1 1.683(4) . ? S1 Mo1 2.4096(18) . ? S2 Mo1 2.4319(19) . ? S3 Fe1 2.220(2) . ? S3 Mo1 2.3056(18) . ? S4 Fe1 2.216(2) . ? S4 Mo1 2.3332(18) . ? Cl1 Fe1 2.256(2) . ? Cl2 Fe1 2.2340(19) . ? Fe1 Mo1 2.7325(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6 C1 C2 119.1(6) . . ? C6 C1 S1 119.8(5) . . ? C2 C1 S1 121.0(5) . . ? C3 C2 C1 121.8(7) . . ? C2 C3 C4 118.0(6) . . ? C2 C3 C7 120.6(7) . . ? C4 C3 C7 121.4(7) . . ? C5 C4 C3 121.1(7) . . ? C4 C5 C6 121.2(7) . . ? C5 C6 C1 118.8(6) . . ? C5 C6 S2 121.8(5) . . ? C1 C6 S2 119.2(5) . . ? C13 C8 C9 119.3(6) . . ? C13 C8 P1 119.9(5) . . ? C9 C8 P1 120.8(5) . . ? C10 C9 C8 119.9(6) . . ? C11 C10 C9 119.6(6) . . ? C10 C11 C12 121.5(6) . . ? C11 C12 C13 119.5(6) . . ? C12 C13 C8 120.1(6) . . ? C15 C14 C19 118.9(6) . . ? C15 C14 P1 123.1(5) . . ? C19 C14 P1 118.1(5) . . ? C16 C15 C14 120.5(6) . . ? C15 C16 C17 119.5(7) . . ? C18 C17 C16 120.4(7) . . ? C19 C18 C17 120.2(7) . . ? C18 C19 C14 120.6(6) . . ? C21 C20 C25 118.9(6) . . ? C21 C20 P1 119.9(5) . . ? C25 C20 P1 121.0(5) . . ? C22 C21 C20 121.2(6) . . ? C23 C22 C21 118.6(6) . . ? C24 C23 C22 121.6(6) . . ? C23 C24 C25 120.5(6) . . ? C24 C25 C20 119.2(6) . . ? C31 C26 C27 119.4(6) . . ? C31 C26 P1 120.9(5) . . ? C27 C26 P1 119.7(5) . . ? C28 C27 C26 120.1(6) . . ? C27 C28 C29 120.4(6) . . ? C30 C29 C28 119.3(6) . . ? C29 C30 C31 120.7(7) . . ? C26 C31 C30 120.1(6) . . ? C33 C32 C37 119.1(6) . . ? C33 C32 P2 122.0(5) . . ? C37 C32 P2 118.3(5) . . ? C34 C33 C32 120.6(7) . . ? C35 C34 C33 119.5(7) . . ? C34 C35 C36 120.8(6) . . ? C37 C36 C35 120.0(7) . . ? C36 C37 C32 119.9(7) . . ? C43 C38 C39 118.4(6) . . ? C43 C38 P2 121.1(5) . . ? C39 C38 P2 120.4(5) . . ? C40 C39 C38 120.1(7) . . ? C41 C40 C39 120.8(7) . . ? C40 C41 C42 119.5(7) . . ? C41 C42 C43 121.0(8) . . ? C42 C43 C38 120.1(7) . . ? C49 C44 C45 119.5(5) . . ? C49 C44 P2 120.6(5) . . ? C45 C44 P2 119.9(5) . . ? C46 C45 C44 119.2(6) . . ? C47 C46 C45 121.2(6) . . ? C46 C47 C48 120.9(6) . . ? C47 C48 C49 118.9(6) . . ? C44 C49 C48 120.3(6) . . ? C55 C50 C51 119.4(6) . . ? C55 C50 P2 120.9(4) . . ? C51 C50 P2 119.7(5) . . ? C52 C51 C50 120.0(6) . . ? C53 C52 C51 119.7(6) . . ? C52 C53 C54 120.8(6) . . ? C55 C54 C53 119.7(6) . . ? C54 C55 C50 120.3(6) . . ? C20 P1 C8 108.6(3) . . ? C20 P1 C14 107.8(3) . . ? C8 P1 C14 109.7(3) . . ? C20 P1 C26 108.4(3) . . ? C8 P1 C26 109.5(3) . . ? C14 P1 C26 112.7(3) . . ? C38 P2 C44 110.6(3) . . ? C38 P2 C32 110.1(3) . . ? C44 P2 C32 106.6(3) . . ? C38 P2 C50 110.4(3) . . ? C44 P2 C50 109.4(3) . . ? C32 P2 C50 109.7(3) . . ? C1 S1 Mo1 108.9(2) . . ? C6 S2 Mo1 108.2(2) . . ? Fe1 S3 Mo1 74.26(6) . . ? Fe1 S4 Mo1 73.78(6) . . ? S4 Fe1 S3 107.06(7) . . ? S4 Fe1 Cl2 110.30(7) . . ? S3 Fe1 Cl2 106.58(7) . . ? S4 Fe1 Cl1 111.25(8) . . ? S3 Fe1 Cl1 110.59(8) . . ? Cl2 Fe1 Cl1 110.89(8) . . ? S4 Fe1 Mo1 55.07(5) . . ? S3 Fe1 Mo1 54.31(5) . . ? Cl2 Fe1 Mo1 135.58(6) . . ? Cl1 Fe1 Mo1 113.43(6) . . ? O1 Mo1 S3 108.95(17) . . ? O1 Mo1 S4 105.12(18) . . ? S3 Mo1 S4 100.53(7) . . ? O1 Mo1 S1 110.04(16) . . ? S3 Mo1 S1 139.43(7) . . ? S4 Mo1 S1 79.79(6) . . ? O1 Mo1 S2 102.23(17) . . ? S3 Mo1 S2 80.53(6) . . ? S4 Mo1 S2 150.54(6) . . ? S1 Mo1 S2 80.75(6) . . ? O1 Mo1 Fe1 105.29(15) . . ? S3 Mo1 Fe1 51.43(5) . . ? S4 Mo1 Fe1 51.15(5) . . ? S1 Mo1 Fe1 125.36(5) . . ? S2 Mo1 Fe1 130.09(5) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 28.33 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.129 _refine_diff_density_min -1.214 _refine_diff_density_rms 0.158 # Attachment 'TDT SPh.txt' data_14augb _database_code_depnum_ccdc_archive 'CCDC 839363' #TrackingRef 'TDT SPh.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C73 H56 Fe Mo N O2 P2 S6' _chemical_formula_sum 'C73 H56 Fe Mo N O2 P2 S6' _chemical_formula_weight 1385.28 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/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 27.668(5) _cell_length_b 15.146(5) _cell_length_c 16.240(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 105.910(5) _cell_angle_gamma 90.000(5) _cell_volume 6545(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour purple _exptl_crystal_size_max 0.94 _exptl_crystal_size_mid 0.61 _exptl_crystal_size_min 0.31 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.406 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2844 _exptl_absorpt_coefficient_mu 0.700 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.605 _exptl_absorpt_correction_T_max 0.805 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'Omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35566 _diffrn_reflns_av_R_equivalents 0.1071 _diffrn_reflns_av_sigmaI/netI 0.1268 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 26.00 _reflns_number_total 12833 _reflns_number_gt 8638 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SMART' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP-3 _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0764P)^2^+13.8167P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12833 _refine_ls_number_parameters 775 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1324 _refine_ls_R_factor_gt 0.0890 _refine_ls_wR_factor_ref 0.2047 _refine_ls_wR_factor_gt 0.1845 _refine_ls_goodness_of_fit_ref 1.096 _refine_ls_restrained_S_all 1.096 _refine_ls_shift/su_max 0.011 _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 C1 C 0.6294(3) -0.6268(4) 0.1361(4) 0.0168(15) Uani 1 1 d . . . C2 C 0.5913(3) -0.5690(4) 0.0931(4) 0.0172(15) Uani 1 1 d . . . C3 C 0.5446(3) -0.5717(4) 0.1098(4) 0.0167(14) Uani 1 1 d . . . H3 H 0.5191 -0.5350 0.0786 0.020 Uiso 1 1 calc R . . C4 C 0.5344(2) -0.6275(4) 0.1715(4) 0.0157(14) Uani 1 1 d . . . C5 C 0.5736(3) -0.6828(4) 0.2160(4) 0.0203(16) Uani 1 1 d . . . H5 H 0.5686 -0.7196 0.2588 0.024 Uiso 1 1 calc R . . C6 C 0.6193(3) -0.6837(4) 0.1975(4) 0.0189(15) Uani 1 1 d . . . H6 H 0.6440 -0.7230 0.2264 0.023 Uiso 1 1 calc R . . C7 C 0.4845(3) -0.6306(4) 0.1896(5) 0.0217(16) Uani 1 1 d . . . H7A H 0.4854 -0.6730 0.2339 0.033 Uiso 1 1 calc R . . H7B H 0.4592 -0.6472 0.1386 0.033 Uiso 1 1 calc R . . H7C H 0.4767 -0.5734 0.2081 0.033 Uiso 1 1 calc R . . C8 C 0.7559(3) -0.6051(4) -0.2713(4) 0.0206(16) Uani 1 1 d . . . C9 C 0.8056(3) -0.5899(4) -0.2249(5) 0.0228(16) Uani 1 1 d . . . H9 H 0.8124 -0.5573 -0.1745 0.027 Uiso 1 1 calc R . . C10 C 0.8449(3) -0.6232(5) -0.2536(5) 0.0331(19) Uani 1 1 d . . . H10 H 0.8780 -0.6132 -0.2222 0.040 Uiso 1 1 calc R . . C11 C 0.8348(3) -0.6712(5) -0.3289(6) 0.036(2) Uani 1 1 d . . . H11 H 0.8610 -0.6928 -0.3487 0.043 Uiso 1 1 calc R . . C12 C 0.7864(3) -0.6865(5) -0.3737(5) 0.034(2) Uani 1 1 d . . . H12 H 0.7798 -0.7184 -0.4245 0.040 Uiso 1 1 calc R . . C13 C 0.7474(3) -0.6567(5) -0.3462(5) 0.0263(17) Uani 1 1 d . . . H13 H 0.7147 -0.6703 -0.3770 0.032 Uiso 1 1 calc R . . C14 C 0.8461(4) -0.4146(6) -0.0536(6) 0.046(2) Uani 1 1 d . . . C15 C 0.8900(4) -0.4218(6) -0.0804(7) 0.050(3) Uani 1 1 d . . . H15 H 0.8877 -0.4124 -0.1379 0.060 Uiso 1 1 calc R . . C16 C 0.9346(4) -0.4415(7) -0.0276(8) 0.063(3) Uani 1 1 d . . . H16 H 0.9622 -0.4513 -0.0487 0.075 Uiso 1 1 calc R . . C17 C 0.9397(5) -0.4474(7) 0.0644(8) 0.070(3) Uani 1 1 d . . . H17 H 0.9709 -0.4546 0.1038 0.084 Uiso 1 1 calc R . . C18 C 0.8968(4) -0.4420(7) 0.0899(7) 0.052(3) Uani 1 1 d . . . H18 H 0.8990 -0.4499 0.1476 0.063 Uiso 1 1 calc R . . C19 C 0.8518(4) -0.4257(6) 0.0358(6) 0.051(3) Uani 1 1 d . . . H19 H 0.8238 -0.4216 0.0567 0.061 Uiso 1 1 calc R . . C20 C 0.6291(3) -0.0989(4) -0.1420(4) 0.0166(14) Uani 1 1 d . . . C21 C 0.6364(2) -0.0462(4) -0.2078(4) 0.0159(14) Uani 1 1 d . . . H21 H 0.6185 0.0061 -0.2223 0.019 Uiso 1 1 calc R . . C22 C 0.6706(2) -0.0721(4) -0.2517(4) 0.0181(15) Uani 1 1 d . . . H22 H 0.6755 -0.0375 -0.2960 0.022 Uiso 1 1 calc R . . C23 C 0.6978(3) -0.1511(4) -0.2286(4) 0.0189(15) Uani 1 1 d . . . H23 H 0.7208 -0.1685 -0.2577 0.023 Uiso 1 1 calc R . . C24 C 0.6905(3) -0.2023(4) -0.1639(4) 0.0195(15) Uani 1 1 d . . . H24 H 0.7086 -0.2544 -0.1493 0.023 Uiso 1 1 calc R . . C25 C 0.6565(2) -0.1774(4) -0.1197(4) 0.0157(14) Uani 1 1 d . . . H25 H 0.6517 -0.2125 -0.0756 0.019 Uiso 1 1 calc R . . C26 C 0.5870(2) -0.1274(4) 0.0037(4) 0.0170(14) Uani 1 1 d . . . C27 C 0.5744(3) -0.2165(4) 0.0010(5) 0.0232(16) Uani 1 1 d . . . H27 H 0.5623 -0.2445 -0.0516 0.028 Uiso 1 1 calc R . . C28 C 0.5796(3) -0.2639(4) 0.0756(4) 0.0231(16) Uani 1 1 d . . . H28 H 0.5721 -0.3238 0.0737 0.028 Uiso 1 1 calc R . . C29 C 0.5963(3) -0.2208(5) 0.1533(5) 0.0226(16) Uani 1 1 d . . . H29 H 0.5985 -0.2518 0.2037 0.027 Uiso 1 1 calc R . . C30 C 0.6097(3) -0.1326(5) 0.1578(5) 0.0233(16) Uani 1 1 d . . . H30 H 0.6216 -0.1046 0.2104 0.028 Uiso 1 1 calc R . . C31 C 0.6051(3) -0.0866(4) 0.0821(4) 0.0201(15) Uani 1 1 d . . . H31 H 0.6143 -0.0274 0.0843 0.024 Uiso 1 1 calc R . . C32 C 0.5205(2) -0.0889(4) -0.1658(4) 0.0155(14) Uani 1 1 d . . . C33 C 0.4792(3) -0.0923(4) -0.1336(5) 0.0210(16) Uani 1 1 d . . . H33 H 0.4833 -0.0898 -0.0748 0.025 Uiso 1 1 calc R . . C34 C 0.4319(3) -0.0995(4) -0.1896(5) 0.0218(16) Uani 1 1 d . . . H34 H 0.4039 -0.1034 -0.1684 0.026 Uiso 1 1 calc R . . C35 C 0.4256(3) -0.1010(4) -0.2768(5) 0.0239(17) Uani 1 1 d . . . H35 H 0.3936 -0.1039 -0.3143 0.029 Uiso 1 1 calc R . . C36 C 0.4665(3) -0.0982(4) -0.3078(5) 0.0219(16) Uani 1 1 d . . . H36 H 0.4620 -0.0996 -0.3667 0.026 Uiso 1 1 calc R . . C37 C 0.5148(3) -0.0935(4) -0.2533(4) 0.0211(16) Uani 1 1 d . . . H37 H 0.5426 -0.0934 -0.2749 0.025 Uiso 1 1 calc R . . C38 C 0.5872(2) 0.0495(4) -0.0725(4) 0.0154(14) Uani 1 1 d . . . C39 C 0.5451(3) 0.1020(4) -0.0818(4) 0.0182(15) Uani 1 1 d . . . H39 H 0.5133 0.0767 -0.0993 0.022 Uiso 1 1 calc R . . C40 C 0.5497(3) 0.1915(4) -0.0653(5) 0.0226(16) Uani 1 1 d . . . H40 H 0.5212 0.2261 -0.0708 0.027 Uiso 1 1 calc R . . C41 C 0.5967(3) 0.2295(5) -0.0407(4) 0.0243(17) Uani 1 1 d . . . H41 H 0.5999 0.2897 -0.0292 0.029 Uiso 1 1 calc R . . C42 C 0.6392(3) 0.1784(5) -0.0329(5) 0.0257(17) Uani 1 1 d . . . H42 H 0.6708 0.2047 -0.0182 0.031 Uiso 1 1 calc R . . C43 C 0.6347(3) 0.0874(4) -0.0470(4) 0.0221(16) Uani 1 1 d . . . H43 H 0.6632 0.0525 -0.0393 0.027 Uiso 1 1 calc R . . C44 C 0.8010(2) -0.1041(4) 0.0314(4) 0.0172(15) Uani 1 1 d . . . C45 C 0.7923(3) -0.1937(4) 0.0128(4) 0.0209(15) Uani 1 1 d . . . H45 H 0.8091 -0.2228 -0.0215 0.025 Uiso 1 1 calc R . . C46 C 0.7581(3) -0.2391(4) 0.0463(5) 0.0229(16) Uani 1 1 d . . . H46 H 0.7512 -0.2983 0.0327 0.028 Uiso 1 1 calc R . . C47 C 0.7346(3) -0.1970(5) 0.0991(5) 0.0278(18) Uani 1 1 d . . . H47 H 0.7124 -0.2282 0.1221 0.033 Uiso 1 1 calc R . . C48 C 0.7434(3) -0.1082(4) 0.1190(5) 0.0242(17) Uani 1 1 d . . . H48 H 0.7273 -0.0804 0.1550 0.029 Uiso 1 1 calc R . . C49 C 0.7764(3) -0.0610(4) 0.0849(5) 0.0238(16) Uani 1 1 d . . . H49 H 0.7821 -0.0014 0.0974 0.029 Uiso 1 1 calc R . . C50 C 0.8560(3) -0.1063(4) -0.0984(5) 0.0230(16) Uani 1 1 d . . . C51 C 0.8982(3) -0.1609(5) -0.0785(5) 0.0317(19) Uani 1 1 d . . . H51 H 0.9198 -0.1627 -0.0234 0.038 Uiso 1 1 calc R . . C52 C 0.9074(3) -0.2132(5) -0.1448(6) 0.042(2) Uani 1 1 d . . . H52 H 0.9352 -0.2502 -0.1329 0.050 Uiso 1 1 calc R . . C53 C 0.8763(3) -0.2102(6) -0.2251(6) 0.043(2) Uani 1 1 d . . . H53 H 0.8830 -0.2444 -0.2683 0.051 Uiso 1 1 calc R . . C54 C 0.8344(3) -0.1560(5) -0.2427(5) 0.036(2) Uani 1 1 d . . . H54 H 0.8127 -0.1544 -0.2978 0.043 Uiso 1 1 calc R . . C55 C 0.8246(3) -0.1045(5) -0.1794(5) 0.0278(17) Uani 1 1 d . . . H55 H 0.7964 -0.0682 -0.1919 0.033 Uiso 1 1 calc R . . C56 C 0.8989(3) -0.0169(4) 0.0652(5) 0.0246(17) Uani 1 1 d . . . C57 C 0.9385(3) 0.0228(5) 0.0407(5) 0.0330(19) Uani 1 1 d . . . H57 H 0.9354 0.0345 -0.0167 0.040 Uiso 1 1 calc R . . C58 C 0.9818(3) 0.0444(6) 0.1019(6) 0.039(2) Uani 1 1 d . . . H58 H 1.0080 0.0718 0.0861 0.047 Uiso 1 1 calc R . . C59 C 0.9867(3) 0.0255(6) 0.1871(6) 0.042(2) Uani 1 1 d . . . H59 H 1.0165 0.0393 0.2281 0.051 Uiso 1 1 calc R . . C60 C 0.9483(3) -0.0131(6) 0.2120(6) 0.041(2) Uani 1 1 d . . . H60 H 0.9519 -0.0241 0.2697 0.050 Uiso 1 1 calc R . . C61 C 0.9039(3) -0.0361(5) 0.1516(5) 0.0307(18) Uani 1 1 d . . . H61 H 0.8781 -0.0636 0.1681 0.037 Uiso 1 1 calc R . . C62 C 0.8101(3) 0.0569(4) -0.0586(4) 0.0215(16) Uani 1 1 d . . . C63 C 0.7593(3) 0.0512(5) -0.1010(5) 0.0240(16) Uani 1 1 d . . . H63 H 0.7427 -0.0025 -0.1029 0.029 Uiso 1 1 calc R . . C64 C 0.7331(3) 0.1250(5) -0.1405(5) 0.0294(18) Uani 1 1 d . . . H64 H 0.6992 0.1208 -0.1698 0.035 Uiso 1 1 calc R . . C65 C 0.7585(3) 0.2059(5) -0.1354(5) 0.0284(18) Uani 1 1 d . . . H65 H 0.7413 0.2558 -0.1614 0.034 Uiso 1 1 calc R . . C66 C 0.8080(3) 0.2118(5) -0.0927(5) 0.0305(19) Uani 1 1 d . . . H66 H 0.8244 0.2657 -0.0900 0.037 Uiso 1 1 calc R . . C67 C 0.8347(3) 0.1379(4) -0.0528(5) 0.0264(17) Uani 1 1 d . . . H67 H 0.8684 0.1428 -0.0226 0.032 Uiso 1 1 calc R . . C68 C 0.8211(3) 0.0952(6) -0.2955(6) 0.050(3) Uani 1 1 d . . . C69 C 0.8699(3) 0.0832(5) -0.2341(6) 0.039(2) Uani 1 1 d . . . C70 C 0.9588(6) 0.3043(10) 0.1372(12) 0.107(5) Uani 1 1 d . . . C71 C 0.9379(5) 0.3095(9) 0.0418(14) 0.112(6) Uani 1 1 d . . . C72 C 0.9625(7) 0.2763(12) -0.0898(12) 0.130(8) Uani 1 1 d . . . C73 C 1.0017(7) 0.2311(12) -0.1235(12) 0.131(7) Uani 1 1 d . . . O1 O 0.72247(18) -0.4273(3) 0.0954(3) 0.0214(11) Uani 1 1 d . . . O2 O 0.9736(4) 0.2664(6) -0.0006(8) 0.112(4) Uani 1 1 d . . . P1 P 0.58127(7) -0.06753(11) -0.09355(11) 0.0150(4) Uani 1 1 d . . . P2 P 0.84179(7) -0.04216(11) -0.01409(12) 0.0200(4) Uani 1 1 d . . . S1 S 0.68667(7) -0.63033(10) 0.11000(11) 0.0175(4) Uani 1 1 d . . . S2 S 0.60266(6) -0.49775(11) 0.01469(11) 0.0178(4) Uani 1 1 d . . . S3 S 0.65980(7) -0.42475(11) -0.10431(11) 0.0186(4) Uani 1 1 d . . . S4 S 0.75156(7) -0.58935(11) -0.01384(11) 0.0219(4) Uani 1 1 d . . . S5 S 0.70267(7) -0.56368(11) -0.24415(11) 0.0205(4) Uani 1 1 d . . . S6 S 0.78832(7) -0.38580(11) -0.12443(12) 0.0239(4) Uani 1 1 d . . . Fe1 Fe 0.72918(4) -0.48965(6) -0.11654(6) 0.0178(2) Uani 1 1 d . . . Mo1 Mo 0.69159(2) -0.50247(4) 0.02310(4) 0.01477(16) Uani 1 1 d . . . N1 N 0.9070(3) 0.0755(5) -0.1836(6) 0.053(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.027(4) 0.010(3) 0.013(3) -0.004(2) 0.005(3) 0.000(3) C2 0.027(4) 0.009(3) 0.014(4) -0.007(2) 0.002(3) -0.003(3) C3 0.022(4) 0.011(3) 0.016(4) 0.002(3) 0.003(3) -0.003(3) C4 0.023(4) 0.010(3) 0.013(3) -0.005(2) 0.003(3) -0.008(3) C5 0.036(4) 0.014(3) 0.011(4) 0.004(3) 0.006(3) 0.002(3) C6 0.033(4) 0.007(3) 0.016(4) 0.002(2) 0.005(3) 0.001(3) C7 0.032(4) 0.014(3) 0.020(4) -0.004(3) 0.008(3) -0.006(3) C8 0.040(5) 0.010(3) 0.013(4) 0.002(3) 0.010(3) -0.002(3) C9 0.027(4) 0.014(3) 0.027(4) 0.000(3) 0.007(3) -0.001(3) C10 0.032(5) 0.032(4) 0.036(5) 0.007(4) 0.010(4) 0.000(4) C11 0.048(5) 0.022(4) 0.047(6) 0.002(4) 0.030(5) 0.007(4) C12 0.055(6) 0.014(4) 0.039(5) -0.008(3) 0.024(5) -0.006(4) C13 0.039(5) 0.020(4) 0.021(4) 0.000(3) 0.009(4) -0.008(3) C14 0.063(6) 0.040(5) 0.038(6) -0.004(4) 0.018(5) -0.007(5) C15 0.048(6) 0.049(6) 0.060(7) -0.009(5) 0.025(5) 0.000(5) C16 0.044(6) 0.068(8) 0.078(9) 0.032(6) 0.022(6) 0.021(5) C17 0.081(9) 0.047(7) 0.079(9) 0.013(6) 0.017(7) 0.010(6) C18 0.046(6) 0.068(7) 0.039(6) -0.001(5) 0.006(5) 0.008(5) C19 0.059(6) 0.048(6) 0.044(6) -0.005(4) 0.008(5) -0.017(5) C20 0.027(4) 0.012(3) 0.010(3) 0.001(2) 0.003(3) 0.001(3) C21 0.017(3) 0.011(3) 0.019(4) 0.003(3) 0.003(3) 0.003(3) C22 0.023(4) 0.022(4) 0.010(3) 0.003(3) 0.006(3) -0.003(3) C23 0.022(4) 0.024(4) 0.014(4) -0.006(3) 0.010(3) 0.000(3) C24 0.021(4) 0.018(4) 0.019(4) -0.005(3) 0.005(3) 0.002(3) C25 0.023(4) 0.010(3) 0.010(3) 0.004(2) -0.003(3) -0.001(3) C26 0.021(4) 0.019(4) 0.009(3) 0.000(3) 0.003(3) 0.003(3) C27 0.040(5) 0.017(4) 0.014(4) -0.005(3) 0.009(3) -0.002(3) C28 0.040(5) 0.012(3) 0.017(4) 0.006(3) 0.008(3) 0.002(3) C29 0.028(4) 0.025(4) 0.015(4) 0.007(3) 0.008(3) 0.007(3) C30 0.032(4) 0.024(4) 0.014(4) 0.002(3) 0.007(3) 0.003(3) C31 0.024(4) 0.016(3) 0.020(4) 0.002(3) 0.007(3) 0.004(3) C32 0.025(4) 0.004(3) 0.018(4) 0.002(2) 0.008(3) 0.002(3) C33 0.030(4) 0.013(3) 0.022(4) -0.009(3) 0.009(3) 0.001(3) C34 0.029(4) 0.004(3) 0.035(4) -0.004(3) 0.013(4) 0.004(3) C35 0.033(4) 0.008(3) 0.026(4) 0.003(3) -0.001(4) -0.001(3) C36 0.039(5) 0.004(3) 0.017(4) 0.002(2) -0.001(3) -0.004(3) C37 0.032(4) 0.013(3) 0.018(4) 0.004(3) 0.006(3) -0.002(3) C38 0.022(4) 0.011(3) 0.011(3) 0.000(2) 0.001(3) 0.002(3) C39 0.028(4) 0.018(3) 0.009(3) -0.005(3) 0.006(3) -0.003(3) C40 0.029(4) 0.017(4) 0.023(4) 0.004(3) 0.010(3) 0.004(3) C41 0.038(5) 0.021(4) 0.012(4) -0.003(3) 0.004(3) 0.004(3) C42 0.031(4) 0.022(4) 0.023(4) -0.009(3) 0.004(3) -0.008(3) C43 0.025(4) 0.022(4) 0.018(4) 0.004(3) 0.004(3) 0.006(3) C44 0.023(4) 0.013(3) 0.013(3) -0.002(3) 0.002(3) -0.001(3) C45 0.030(4) 0.016(3) 0.018(4) 0.003(3) 0.009(3) 0.004(3) C46 0.042(5) 0.010(3) 0.020(4) 0.001(3) 0.014(3) 0.000(3) C47 0.045(5) 0.025(4) 0.015(4) 0.004(3) 0.012(4) -0.003(3) C48 0.035(4) 0.016(4) 0.024(4) 0.002(3) 0.013(4) 0.002(3) C49 0.043(5) 0.012(3) 0.020(4) 0.002(3) 0.013(3) -0.001(3) C50 0.029(4) 0.016(4) 0.027(4) -0.003(3) 0.011(3) -0.004(3) C51 0.035(5) 0.028(4) 0.031(5) 0.000(3) 0.008(4) -0.001(3) C52 0.045(5) 0.031(5) 0.050(6) -0.005(4) 0.014(5) 0.012(4) C53 0.043(5) 0.048(6) 0.041(6) -0.021(4) 0.018(5) 0.000(4) C54 0.045(5) 0.041(5) 0.019(4) -0.013(3) 0.004(4) -0.011(4) C55 0.031(4) 0.024(4) 0.029(5) -0.005(3) 0.009(4) -0.008(3) C56 0.026(4) 0.016(4) 0.032(4) -0.003(3) 0.007(3) 0.004(3) C57 0.037(5) 0.030(4) 0.031(5) -0.009(3) 0.008(4) -0.001(4) C58 0.030(5) 0.034(5) 0.052(6) -0.014(4) 0.008(4) 0.001(4) C59 0.031(5) 0.048(6) 0.037(5) -0.014(4) -0.011(4) 0.002(4) C60 0.041(5) 0.050(6) 0.026(5) -0.005(4) -0.003(4) 0.011(4) C61 0.043(5) 0.027(4) 0.024(4) -0.005(3) 0.012(4) 0.002(4) C62 0.038(4) 0.012(3) 0.014(4) 0.004(3) 0.007(3) 0.002(3) C63 0.034(4) 0.016(4) 0.019(4) 0.000(3) 0.004(3) -0.003(3) C64 0.041(5) 0.026(4) 0.021(4) 0.008(3) 0.008(4) 0.006(3) C65 0.041(5) 0.016(4) 0.027(4) 0.008(3) 0.007(4) -0.001(3) C66 0.050(5) 0.013(4) 0.031(5) 0.000(3) 0.015(4) -0.010(3) C67 0.046(5) 0.015(4) 0.018(4) 0.003(3) 0.008(4) 0.001(3) C68 0.048(6) 0.042(5) 0.043(6) 0.003(4) -0.016(5) -0.004(4) C69 0.038(5) 0.032(5) 0.043(6) 0.002(4) 0.005(5) 0.001(4) C70 0.119(12) 0.085(11) 0.126(15) -0.039(10) 0.047(11) -0.009(9) C71 0.090(11) 0.054(8) 0.185(19) -0.044(10) 0.023(11) 0.008(7) C72 0.157(17) 0.100(13) 0.080(12) 0.019(10) -0.055(12) -0.030(11) C73 0.145(16) 0.097(13) 0.130(16) -0.037(11) 0.004(12) 0.029(11) O1 0.042(3) 0.013(2) 0.012(2) -0.0052(18) 0.014(2) -0.008(2) O2 0.106(8) 0.057(6) 0.147(11) -0.013(6) -0.007(7) 0.005(5) P1 0.0240(10) 0.0105(8) 0.0105(9) -0.0006(6) 0.0047(7) 0.0005(7) P2 0.0268(10) 0.0126(9) 0.0204(10) -0.0010(7) 0.0059(8) -0.0006(7) S1 0.0256(10) 0.0105(8) 0.0162(9) 0.0015(6) 0.0052(8) 0.0011(7) S2 0.0274(9) 0.0118(8) 0.0141(8) 0.0030(6) 0.0056(7) 0.0006(7) S3 0.0277(10) 0.0158(8) 0.0140(9) 0.0044(6) 0.0084(8) 0.0041(7) S4 0.0303(10) 0.0204(9) 0.0165(9) 0.0044(7) 0.0093(8) 0.0092(7) S5 0.0238(10) 0.0227(9) 0.0151(9) -0.0011(7) 0.0054(8) -0.0013(7) S6 0.0306(11) 0.0154(9) 0.0266(10) -0.0001(7) 0.0094(9) -0.0009(7) Fe1 0.0266(6) 0.0143(5) 0.0139(5) 0.0002(4) 0.0082(4) 0.0005(4) Mo1 0.0244(3) 0.0097(3) 0.0105(3) -0.0004(2) 0.0053(2) -0.0009(2) N1 0.043(5) 0.063(6) 0.049(5) 0.002(4) 0.005(4) 0.000(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.400(9) . ? C1 C6 1.404(9) . ? C1 S1 1.749(7) . ? C2 C3 1.394(9) . ? C2 S2 1.761(7) . ? C3 C4 1.397(9) . ? C4 C5 1.403(9) . ? C4 C7 1.490(9) . ? C5 C6 1.377(9) . ? C8 C9 1.393(10) . ? C8 C13 1.409(9) . ? C8 S5 1.764(7) . ? C9 C10 1.391(10) . ? C10 C11 1.383(11) . ? C11 C12 1.359(11) . ? C12 C13 1.353(11) . ? C14 C15 1.402(12) . ? C14 C19 1.425(13) . ? C14 S6 1.749(10) . ? C15 C16 1.330(13) . ? C16 C17 1.464(16) . ? C17 C18 1.361(14) . ? C18 C19 1.336(12) . ? C20 C21 1.392(9) . ? C20 C25 1.402(8) . ? C20 P1 1.780(7) . ? C21 C22 1.387(9) . ? C22 C23 1.409(9) . ? C23 C24 1.366(10) . ? C24 C25 1.384(9) . ? C26 C31 1.380(9) . ? C26 C27 1.392(9) . ? C26 P1 1.789(7) . ? C27 C28 1.382(9) . ? C28 C29 1.383(10) . ? C29 C30 1.383(10) . ? C30 C31 1.387(9) . ? C32 C33 1.380(9) . ? C32 C37 1.388(9) . ? C32 P1 1.796(7) . ? C33 C34 1.380(10) . ? C34 C35 1.379(10) . ? C35 C36 1.358(10) . ? C36 C37 1.387(10) . ? C38 C39 1.386(9) . ? C38 C43 1.388(9) . ? C38 P1 1.804(6) . ? C39 C40 1.381(9) . ? C40 C41 1.376(10) . ? C41 C42 1.386(10) . ? C42 C43 1.397(9) . ? C44 C45 1.397(9) . ? C44 C49 1.402(10) . ? C44 P2 1.777(7) . ? C45 C46 1.396(10) . ? C46 C47 1.368(10) . ? C47 C48 1.388(10) . ? C48 C49 1.387(10) . ? C50 C55 1.363(10) . ? C50 C51 1.394(10) . ? C50 P2 1.809(7) . ? C51 C52 1.413(11) . ? C52 C53 1.353(12) . ? C53 C54 1.384(12) . ? C54 C55 1.377(10) . ? C56 C57 1.399(11) . ? C56 C61 1.402(10) . ? C56 P2 1.785(8) . ? C57 C58 1.371(11) . ? C58 C59 1.383(13) . ? C59 C60 1.368(13) . ? C60 C61 1.389(11) . ? C62 C63 1.388(10) . ? C62 C67 1.393(9) . ? C62 P2 1.787(7) . ? C63 C64 1.391(10) . ? C64 C65 1.404(10) . ? C65 C66 1.358(11) . ? C66 C67 1.398(10) . ? C68 C69 1.453(12) . ? C69 N1 1.131(10) . ? C70 C71 1.50(2) . ? C71 O2 1.501(18) . ? C72 O2 1.404(19) . ? C72 C73 1.51(3) . ? O1 Mo1 1.689(4) . ? S1 Mo1 2.4219(18) . ? S2 Mo1 2.4278(19) . ? S3 Fe1 2.213(2) . ? S3 Mo1 2.3330(18) . ? S4 Fe1 2.209(2) . ? S4 Mo1 2.3217(18) . ? S5 Fe1 2.293(2) . ? S6 Fe1 2.299(2) . ? Fe1 Mo1 2.7486(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 C2 C1 C6 117.9(6) . . ? C2 C1 S1 120.4(5) . . ? C6 C1 S1 121.6(5) . . ? C3 C2 C1 119.8(6) . . ? C3 C2 S2 121.1(5) . . ? C1 C2 S2 119.0(5) . . ? C2 C3 C4 122.5(6) . . ? C3 C4 C5 116.8(6) . . ? C3 C4 C7 122.7(6) . . ? C5 C4 C7 120.5(6) . . ? C6 C5 C4 121.3(6) . . ? C5 C6 C1 121.5(6) . . ? C9 C8 C13 117.6(7) . . ? C9 C8 S5 125.0(5) . . ? C13 C8 S5 117.4(6) . . ? C10 C9 C8 120.4(7) . . ? C11 C10 C9 119.9(8) . . ? C12 C11 C10 119.6(8) . . ? C13 C12 C11 121.6(8) . . ? C12 C13 C8 120.7(7) . . ? C15 C14 C19 116.3(9) . . ? C15 C14 S6 121.9(8) . . ? C19 C14 S6 121.7(8) . . ? C16 C15 C14 123.2(10) . . ? C15 C16 C17 118.9(10) . . ? C18 C17 C16 117.4(11) . . ? C19 C18 C17 122.9(11) . . ? C18 C19 C14 121.0(10) . . ? C21 C20 C25 120.2(6) . . ? C21 C20 P1 117.9(5) . . ? C25 C20 P1 121.7(5) . . ? C22 C21 C20 119.7(6) . . ? C21 C22 C23 119.6(6) . . ? C24 C23 C22 120.4(6) . . ? C23 C24 C25 120.6(6) . . ? C24 C25 C20 119.5(6) . . ? C31 C26 C27 119.1(6) . . ? C31 C26 P1 120.7(5) . . ? C27 C26 P1 120.2(5) . . ? C28 C27 C26 120.7(6) . . ? C27 C28 C29 119.0(6) . . ? C28 C29 C30 121.4(6) . . ? C29 C30 C31 118.7(7) . . ? C26 C31 C30 121.0(6) . . ? C33 C32 C37 120.8(6) . . ? C33 C32 P1 118.9(5) . . ? C37 C32 P1 120.1(5) . . ? C34 C33 C32 119.2(7) . . ? C35 C34 C33 120.4(7) . . ? C36 C35 C34 119.9(7) . . ? C35 C36 C37 121.2(7) . . ? C36 C37 C32 118.4(7) . . ? C39 C38 C43 119.6(6) . . ? C39 C38 P1 120.9(5) . . ? C43 C38 P1 119.5(5) . . ? C40 C39 C38 120.8(7) . . ? C41 C40 C39 119.8(7) . . ? C40 C41 C42 120.3(7) . . ? C41 C42 C43 120.0(7) . . ? C38 C43 C42 119.5(6) . . ? C45 C44 C49 120.1(6) . . ? C45 C44 P2 121.0(5) . . ? C49 C44 P2 118.9(5) . . ? C46 C45 C44 119.3(6) . . ? C47 C46 C45 120.2(7) . . ? C46 C47 C48 120.9(7) . . ? C49 C48 C47 120.0(7) . . ? C48 C49 C44 119.4(6) . . ? C55 C50 C51 120.6(7) . . ? C55 C50 P2 120.3(6) . . ? C51 C50 P2 119.0(6) . . ? C50 C51 C52 117.9(8) . . ? C53 C52 C51 121.1(8) . . ? C52 C53 C54 119.6(8) . . ? C55 C54 C53 120.5(8) . . ? C50 C55 C54 120.3(8) . . ? C57 C56 C61 120.2(7) . . ? C57 C56 P2 119.7(6) . . ? C61 C56 P2 120.2(6) . . ? C58 C57 C56 119.6(8) . . ? C57 C58 C59 120.1(9) . . ? C60 C59 C58 120.9(8) . . ? C59 C60 C61 120.4(8) . . ? C60 C61 C56 118.8(8) . . ? C63 C62 C67 119.9(6) . . ? C63 C62 P2 117.7(5) . . ? C67 C62 P2 122.4(6) . . ? C62 C63 C64 120.5(7) . . ? C63 C64 C65 119.0(7) . . ? C66 C65 C64 120.4(7) . . ? C65 C66 C67 121.0(7) . . ? C62 C67 C66 119.2(7) . . ? N1 C69 C68 176.9(11) . . ? O2 C71 C70 109.5(12) . . ? O2 C72 C73 110.4(15) . . ? C72 O2 C71 116.1(14) . . ? C20 P1 C26 111.0(3) . . ? C20 P1 C32 109.9(3) . . ? C26 P1 C32 109.0(3) . . ? C20 P1 C38 107.8(3) . . ? C26 P1 C38 110.4(3) . . ? C32 P1 C38 108.7(3) . . ? C44 P2 C56 110.6(3) . . ? C44 P2 C62 108.3(3) . . ? C56 P2 C62 110.5(3) . . ? C44 P2 C50 109.0(3) . . ? C56 P2 C50 109.1(3) . . ? C62 P2 C50 109.2(3) . . ? C1 S1 Mo1 108.4(2) . . ? C2 S2 Mo1 108.6(2) . . ? Fe1 S3 Mo1 74.34(6) . . ? Fe1 S4 Mo1 74.65(6) . . ? C8 S5 Fe1 108.5(2) . . ? C14 S6 Fe1 109.2(3) . . ? S4 Fe1 S3 107.84(8) . . ? S4 Fe1 S5 107.59(8) . . ? S3 Fe1 S5 103.18(7) . . ? S4 Fe1 S6 116.96(8) . . ? S3 Fe1 S6 110.44(8) . . ? S5 Fe1 S6 109.91(8) . . ? S4 Fe1 Mo1 54.54(5) . . ? S3 Fe1 Mo1 54.81(5) . . ? S5 Fe1 Mo1 127.71(6) . . ? S6 Fe1 Mo1 122.04(6) . . ? O1 Mo1 S4 107.48(17) . . ? O1 Mo1 S3 105.82(16) . . ? S4 Mo1 S3 100.32(7) . . ? O1 Mo1 S1 103.41(16) . . ? S4 Mo1 S1 81.70(6) . . ? S3 Mo1 S1 148.48(6) . . ? O1 Mo1 S2 109.32(17) . . ? S4 Mo1 S2 141.93(7) . . ? S3 Mo1 S2 78.77(6) . . ? S1 Mo1 S2 80.70(6) . . ? O1 Mo1 Fe1 107.00(16) . . ? S4 Mo1 Fe1 50.81(5) . . ? S3 Mo1 Fe1 50.84(5) . . ? S1 Mo1 Fe1 129.17(5) . . ? S2 Mo1 Fe1 123.94(5) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.911 _refine_diff_density_min -1.316 _refine_diff_density_rms 0.156