# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2002 data_global _journal_name_full 'New J.Chem.(Nouv.J.Chim.)' _audit_creation_date 10-05-02 _journal_coden_Cambridge 0440 loop_ _publ_author_name 'P. Braunstein' 'Nicolas Auvray' 'Stefan Hufner' 'Sanjay Mathur' 'Hao Shen' 'Michael Veith' _publ_contact_author_name 'Pierre Braunstein' _publ_contact_author_address ; Prof P Braunstein Laboratoire de Chimie de Coordination Insitut Le Bel, Universite Louis Pa\steur 4 Rue Blaise Pascal Strasbourg Cedex F-67070 FRANCE ; _publ_contact_author_phone 0390241593 _publ_contact_author_fax 0390241232 _publ_contact_author_email braunst@chimie.u-strasbg.fr _publ_section_title ; Thin films by metal organic deposition of Fe-Mo-S molecular clusters : synthesis and crystal structure of [Cp2MoFe2(m3-S)2(CO)6] ; _publ_requested_category FM _publ_section_references ; Burla, M.C., Camalli, M., Cascarano, G.,Giacovazzo, C., Polidori, G., Spagna, R. &Viterbo, D. (1989). SIR. J. Appl. Cryst. 22, 389-393. A.L. Spek, PLATON 98, Utrecht University, The Netherland, 1998. KappaCCD Operation Manual (1997), Nonius B.V., Delft, The Nederlands. Otwinowski, Z. & Minor, W. (1997), Methods in Enzymology, 276, 307-326. Sheldrick, G.M. (1997). SHELXL97. Program for the refinement of crystal structures. University of Gottingen. Germany. ; data_pbr31 _database_code_CSD 193026 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H10 Fe2 Mo O6 S2' _chemical_formula_sum 'C16 H10 Fe2 Mo O6 S2' _chemical_formula_weight 570.00 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' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.217(5) _cell_length_b 13.703(5) _cell_length_c 16.310(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 92.176(5) _cell_angle_gamma 90.000(5) _cell_volume 1835.1(14) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9471 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.063 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1120 _exptl_absorpt_coefficient_mu 2.491 # Absorption correction _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.698 _exptl_absorpt_correction_T_max 0.783 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _diffrn_reflns_av_R_equivalents 0.036 _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 KappaCCD _diffrn_measurement_method '\p scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4204 _diffrn_reflns_av_sigmaI/netI 0.0809 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 27.48 _reflns_number_total 4203 _reflns_number_gt 3030 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Denzo (Nonius B.V., 1998)' _computing_data_reduction 'Denzo (Nonius B.V., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON 98 (Spek, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0431P)^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 4203 _refine_ls_number_parameters 244 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0522 _refine_ls_R_factor_gt 0.0320 _refine_ls_wR_factor_ref 0.1091 _refine_ls_wR_factor_gt 0.1018 _refine_ls_goodness_of_fit_ref 0.940 _refine_ls_restrained_S_all 0.940 _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 Mo Mo 0.85295(4) 0.43273(3) 0.16604(2) 0.02316(12) Uani 1 1 d . . . Fe1 Fe 1.11038(8) 0.21896(4) 0.11394(4) 0.02569(17) Uani 1 1 d . . . Fe2 Fe 0.87977(8) 0.23220(5) 0.01355(4) 0.02616(17) Uani 1 1 d . . . S1 S 0.85005(14) 0.24793(8) 0.15386(7) 0.0255(2) Uani 1 1 d . . . S2 S 1.02967(13) 0.36568(8) 0.05387(7) 0.0258(2) Uani 1 1 d . . . C12 C 0.5769(5) 0.4384(4) 0.1776(3) 0.0328(11) Uani 1 1 d . . . H12 H 0.5305 0.4056 0.2209 0.039 Uiso 1 1 calc . . . C9 C 1.0504(6) 0.5396(4) 0.2107(3) 0.0390(12) Uani 1 1 d . . . H9 H 1.0842 0.5876 0.1749 0.047 Uiso 1 1 calc . . . C1 C 1.2447(6) 0.2427(3) 0.2001(3) 0.0359(11) Uani 1 1 d . . . O6 O 0.6231(4) 0.3114(3) -0.0971(2) 0.0503(10) Uani 1 1 d . . . O3 O 1.0713(5) 0.0099(3) 0.1447(2) 0.0526(10) Uani 1 1 d . . . C5 C 0.7956(6) 0.1111(4) 0.0149(3) 0.0395(12) Uani 1 1 d . . . O1 O 1.3412(5) 0.2528(3) 0.2529(2) 0.0515(10) Uani 1 1 d . . . O2 O 1.3849(4) 0.1901(3) 0.0067(2) 0.0534(10) Uani 1 1 d . . . C3 C 1.0889(6) 0.0909(4) 0.1319(3) 0.0344(11) Uani 1 1 d . . . O4 O 1.0936(4) 0.1961(3) -0.1232(2) 0.0467(9) Uani 1 1 d . . . C16 C 0.6341(6) 0.5362(4) 0.1781(3) 0.0334(11) Uani 1 1 d . . . H16 H 0.6278 0.5799 0.2214 0.040 Uiso 1 1 calc . . . C10 C 1.1176(5) 0.4460(3) 0.2211(3) 0.0332(11) Uani 1 1 d . . . H10 H 1.2066 0.4219 0.1939 0.040 Uiso 1 1 calc . . . C4 C 1.0074(6) 0.2083(3) -0.0704(3) 0.0323(11) Uani 1 1 d . . . C2 C 1.2765(6) 0.2013(4) 0.0474(3) 0.0348(11) Uani 1 1 d . . . C11 C 1.0289(6) 0.3948(4) 0.2791(3) 0.0369(11) Uani 1 1 d . . . H11 H 1.0494 0.3313 0.2968 0.044 Uiso 1 1 calc . . . C15 C 0.7026(6) 0.5560(3) 0.1012(3) 0.0356(11) Uani 1 1 d . . . H15 H 0.7523 0.6139 0.0861 0.043 Uiso 1 1 calc . . . O5 O 0.7414(5) 0.0351(3) 0.0169(2) 0.0651(13) Uani 1 1 d . . . C6 C 0.7190(6) 0.2825(4) -0.0496(3) 0.0341(11) Uani 1 1 d . . . C14 C 0.6820(6) 0.4728(4) 0.0523(3) 0.0326(11) Uani 1 1 d . . . H14 H 0.7141 0.4664 -0.0015 0.039 Uiso 1 1 calc . . . C8 C 0.9203(6) 0.5465(4) 0.2658(3) 0.0438(13) Uani 1 1 d . . . H8 H 0.8568 0.6016 0.2740 0.053 Uiso 1 1 calc . . . C13 C 0.6043(5) 0.4001(4) 0.0981(3) 0.0326(11) Uani 1 1 d . . . H13 H 0.5759 0.3380 0.0795 0.039 Uiso 1 1 calc . . . C7 C 0.9039(6) 0.4557(4) 0.3057(3) 0.0437(13) Uani 1 1 d . . . H7 H 0.8250 0.4393 0.3428 0.052 Uiso 1 1 calc . . . 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 Mo 0.0247(2) 0.0190(2) 0.0259(2) -0.00137(15) 0.00436(15) -0.00075(15) Fe1 0.0301(4) 0.0220(3) 0.0250(3) 0.0003(3) 0.0015(3) 0.0005(3) Fe2 0.0318(4) 0.0249(3) 0.0218(3) -0.0029(3) 0.0013(3) -0.0022(3) S1 0.0325(6) 0.0209(5) 0.0236(6) -0.0003(4) 0.0054(4) -0.0022(5) S2 0.0298(6) 0.0223(5) 0.0255(6) 0.0010(4) 0.0049(4) -0.0026(4) C12 0.020(2) 0.039(3) 0.040(3) -0.001(2) 0.0093(19) 0.001(2) C9 0.037(3) 0.026(2) 0.053(3) -0.010(2) -0.004(2) -0.008(2) C1 0.046(3) 0.026(2) 0.036(3) 0.003(2) -0.001(2) 0.007(2) O6 0.048(2) 0.064(3) 0.038(2) -0.0097(19) -0.0110(18) 0.014(2) O3 0.079(3) 0.0241(19) 0.056(2) 0.0031(17) 0.018(2) 0.0014(19) C5 0.049(3) 0.039(3) 0.031(3) -0.009(2) 0.005(2) -0.008(3) O1 0.064(3) 0.038(2) 0.051(2) 0.0006(18) -0.025(2) 0.0086(19) O2 0.034(2) 0.065(3) 0.062(3) -0.010(2) 0.0161(19) 0.0002(19) C3 0.039(3) 0.032(3) 0.032(3) -0.003(2) 0.007(2) 0.004(2) O4 0.047(2) 0.062(2) 0.0312(19) -0.0104(18) 0.0052(17) 0.0034(19) C16 0.033(3) 0.031(2) 0.037(3) -0.004(2) 0.007(2) 0.007(2) C10 0.029(2) 0.032(3) 0.038(3) -0.012(2) -0.006(2) 0.001(2) C4 0.038(3) 0.032(3) 0.026(2) -0.002(2) -0.003(2) -0.003(2) C2 0.033(3) 0.031(3) 0.039(3) 0.000(2) -0.003(2) 0.001(2) C11 0.042(3) 0.040(3) 0.028(2) -0.006(2) -0.009(2) 0.001(2) C15 0.035(3) 0.027(2) 0.044(3) 0.007(2) 0.003(2) 0.008(2) O5 0.104(4) 0.038(2) 0.055(3) -0.010(2) 0.023(2) -0.033(2) C6 0.036(3) 0.040(3) 0.027(2) -0.010(2) 0.002(2) 0.000(2) C14 0.030(2) 0.037(3) 0.031(2) 0.003(2) 0.000(2) 0.009(2) C8 0.042(3) 0.038(3) 0.052(3) -0.028(3) -0.003(2) 0.004(2) C13 0.023(2) 0.033(3) 0.042(3) -0.006(2) -0.001(2) 0.004(2) C7 0.045(3) 0.056(3) 0.030(3) -0.013(3) 0.001(2) -0.003(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 Mo C9 2.284(5) . ? Mo C12 2.285(4) . ? Mo C16 2.304(5) . ? Mo C8 2.305(5) . ? Mo C7 2.322(5) . ? Mo C15 2.323(4) . ? Mo C10 2.328(4) . ? Mo C13 2.331(4) . ? Mo C14 2.350(4) . ? Mo C11 2.357(5) . ? Mo S1 2.5402(15) . ? Mo S2 2.5498(13) . ? Fe1 C1 1.783(5) . ? Fe1 C3 1.789(5) . ? Fe1 C2 1.792(5) . ? Fe1 S1 2.2941(18) . ? Fe1 S2 2.3222(14) . ? Fe1 Fe2 2.4636(13) . ? Fe2 C6 1.783(5) . ? Fe2 C4 1.786(5) . ? Fe2 C5 1.799(5) . ? Fe2 S2 2.2877(14) . ? Fe2 S1 2.3207(14) . ? C12 C16 1.420(7) . ? C12 C13 1.425(6) . ? C12 H12 0.9300 . ? C9 C10 1.403(7) . ? C9 C8 1.425(7) . ? C9 H9 0.9300 . ? C1 O1 1.157(6) . ? O6 C6 1.154(6) . ? O3 C3 1.140(6) . ? C5 O5 1.133(6) . ? O2 C2 1.142(6) . ? O4 C4 1.148(5) . ? C16 C15 1.419(7) . ? C16 H16 0.9300 . ? C10 C11 1.404(7) . ? C10 H10 0.9300 . ? C11 C7 1.405(7) . ? C11 H11 0.9300 . ? C15 C14 1.399(7) . ? C15 H15 0.9300 . ? C14 C13 1.412(7) . ? C14 H14 0.9300 . ? C8 C7 1.414(8) . ? C8 H8 0.9300 . ? C13 H13 0.9300 . ? C7 H7 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 C9 Mo C12 130.35(18) . . ? C9 Mo C16 97.23(18) . . ? C12 Mo C16 36.06(17) . . ? C9 Mo C8 36.17(18) . . ? C12 Mo C8 97.55(18) . . ? C16 Mo C8 72.01(17) . . ? C9 Mo C7 60.04(19) . . ? C12 Mo C7 93.26(18) . . ? C16 Mo C7 86.87(18) . . ? C8 Mo C7 35.58(19) . . ? C9 Mo C15 92.20(19) . . ? C12 Mo C15 60.04(17) . . ? C16 Mo C15 35.73(17) . . ? C8 Mo C15 86.49(19) . . ? C7 Mo C15 114.90(19) . . ? C9 Mo C10 35.41(16) . . ? C12 Mo C10 151.80(18) . . ? C16 Mo C10 129.77(17) . . ? C8 Mo C10 58.61(17) . . ? C7 Mo C10 58.67(18) . . ? C15 Mo C10 126.26(18) . . ? C9 Mo C13 150.94(18) . . ? C12 Mo C13 35.95(16) . . ? C16 Mo C13 59.04(17) . . ? C8 Mo C13 130.39(17) . . ? C7 Mo C13 127.93(18) . . ? C15 Mo C13 58.77(17) . . ? C10 Mo C13 170.99(16) . . ? C9 Mo C14 119.91(18) . . ? C12 Mo C14 59.44(16) . . ? C16 Mo C14 58.56(16) . . ? C8 Mo C14 121.31(19) . . ? C7 Mo C14 145.42(18) . . ? C15 Mo C14 34.83(17) . . ? C10 Mo C14 143.92(18) . . ? C13 Mo C14 35.11(16) . . ? C9 Mo C11 58.98(18) . . ? C12 Mo C11 121.61(18) . . ? C16 Mo C11 121.78(17) . . ? C8 Mo C11 58.25(18) . . ? C7 Mo C11 34.94(18) . . ? C15 Mo C11 144.70(18) . . ? C10 Mo C11 34.86(18) . . ? C13 Mo C11 146.12(18) . . ? C14 Mo C11 178.76(17) . . ? C9 Mo S1 131.94(13) . . ? C12 Mo S1 91.93(12) . . ? C16 Mo S1 127.95(13) . . ? C8 Mo S1 136.94(15) . . ? C7 Mo S1 102.27(15) . . ? C15 Mo S1 133.30(13) . . ? C10 Mo S1 96.55(12) . . ? C13 Mo S1 76.47(12) . . ? C14 Mo S1 99.64(12) . . ? C11 Mo S1 81.07(13) . . ? C9 Mo S2 92.47(14) . . ? C12 Mo S2 131.73(13) . . ? C16 Mo S2 138.62(12) . . ? C8 Mo S2 128.46(14) . . ? C7 Mo S2 131.80(14) . . ? C15 Mo S2 104.06(13) . . ? C10 Mo S2 75.88(12) . . ? C13 Mo S2 95.88(12) . . ? C14 Mo S2 81.79(12) . . ? C11 Mo S2 97.62(13) . . ? S1 Mo S2 65.70(4) . . ? C1 Fe1 C3 96.4(2) . . ? C1 Fe1 C2 92.2(2) . . ? C3 Fe1 C2 92.8(2) . . ? C1 Fe1 S1 107.52(17) . . ? C3 Fe1 S1 91.40(16) . . ? C2 Fe1 S1 159.23(16) . . ? C1 Fe1 S2 109.45(16) . . ? C3 Fe1 S2 152.87(16) . . ? C2 Fe1 S2 94.21(16) . . ? S1 Fe1 S2 73.47(4) . . ? C1 Fe1 Fe2 161.40(16) . . ? C3 Fe1 Fe2 95.90(16) . . ? C2 Fe1 Fe2 101.06(16) . . ? S1 Fe1 Fe2 58.26(4) . . ? S2 Fe1 Fe2 57.02(3) . . ? C6 Fe2 C4 94.1(2) . . ? C6 Fe2 C5 95.0(2) . . ? C4 Fe2 C5 94.5(2) . . ? C6 Fe2 S2 103.67(16) . . ? C4 Fe2 S2 92.36(15) . . ? C5 Fe2 S2 159.60(17) . . ? C6 Fe2 S1 115.49(15) . . ? C4 Fe2 S1 149.27(15) . . ? C5 Fe2 S1 91.06(16) . . ? S2 Fe2 S1 73.62(4) . . ? C6 Fe2 Fe1 161.27(16) . . ? C4 Fe2 Fe1 92.09(15) . . ? C5 Fe2 Fe1 102.13(17) . . ? S2 Fe2 Fe1 58.38(4) . . ? S1 Fe2 Fe1 57.21(4) . . ? Fe1 S1 Fe2 64.53(4) . . ? Fe1 S1 Mo 100.87(4) . . ? Fe2 S1 Mo 99.71(4) . . ? Fe2 S2 Fe1 64.60(4) . . ? Fe2 S2 Mo 100.33(5) . . ? Fe1 S2 Mo 99.82(5) . . ? C16 C12 C13 106.7(4) . . ? C16 C12 Mo 72.7(2) . . ? C13 C12 Mo 73.8(2) . . ? C16 C12 H12 126.6 . . ? C13 C12 H12 126.6 . . ? Mo C12 H12 118.9 . . ? C10 C9 C8 106.6(5) . . ? C10 C9 Mo 74.0(3) . . ? C8 C9 Mo 72.7(3) . . ? C10 C9 H9 126.7 . . ? C8 C9 H9 126.7 . . ? Mo C9 H9 118.6 . . ? O1 C1 Fe1 174.2(5) . . ? O5 C5 Fe2 178.9(5) . . ? O3 C3 Fe1 178.0(5) . . ? C15 C16 C12 108.6(4) . . ? C15 C16 Mo 72.9(3) . . ? C12 C16 Mo 71.2(3) . . ? C15 C16 H16 125.7 . . ? C12 C16 H16 125.7 . . ? Mo C16 H16 121.8 . . ? C9 C10 C11 109.0(4) . . ? C9 C10 Mo 70.6(3) . . ? C11 C10 Mo 73.7(3) . . ? C9 C10 H10 125.5 . . ? C11 C10 H10 125.5 . . ? Mo C10 H10 121.9 . . ? O4 C4 Fe2 177.2(4) . . ? O2 C2 Fe1 178.3(4) . . ? C10 C11 C7 108.4(5) . . ? C10 C11 Mo 71.4(3) . . ? C7 C11 Mo 71.2(3) . . ? C10 C11 H11 125.8 . . ? C7 C11 H11 125.8 . . ? Mo C11 H11 123.2 . . ? C14 C15 C16 107.7(4) . . ? C14 C15 Mo 73.6(3) . . ? C16 C15 Mo 71.4(3) . . ? C14 C15 H15 126.1 . . ? C16 C15 H15 126.1 . . ? Mo C15 H15 120.6 . . ? O6 C6 Fe2 173.1(4) . . ? C15 C14 C13 108.7(4) . . ? C15 C14 Mo 71.6(3) . . ? C13 C14 Mo 71.7(3) . . ? C15 C14 H14 125.7 . . ? C13 C14 H14 125.7 . . ? Mo C14 H14 122.7 . . ? C7 C8 C9 108.6(5) . . ? C7 C8 Mo 72.9(3) . . ? C9 C8 Mo 71.1(3) . . ? C7 C8 H8 125.7 . . ? C9 C8 H8 125.7 . . ? Mo C8 H8 122.0 . . ? C14 C13 C12 108.2(4) . . ? C14 C13 Mo 73.2(3) . . ? C12 C13 Mo 70.3(2) . . ? C14 C13 H13 125.9 . . ? C12 C13 H13 125.9 . . ? Mo C13 H13 122.3 . . ? C11 C7 C8 107.2(5) . . ? C11 C7 Mo 73.9(3) . . ? C8 C7 Mo 71.5(3) . . ? C11 C7 H7 126.4 . . ? C8 C7 H7 126.4 . . ? Mo C7 H7 120.1 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Fe1 Fe2 C6 29.0(7) . . . . ? C3 Fe1 Fe2 C6 160.2(5) . . . . ? C2 Fe1 Fe2 C6 -105.8(5) . . . . ? S1 Fe1 Fe2 C6 72.2(5) . . . . ? S2 Fe1 Fe2 C6 -17.9(5) . . . . ? C1 Fe1 Fe2 C4 138.4(5) . . . . ? C3 Fe1 Fe2 C4 -90.4(2) . . . . ? C2 Fe1 Fe2 C4 3.6(2) . . . . ? S1 Fe1 Fe2 C4 -178.37(16) . . . . ? S2 Fe1 Fe2 C4 91.48(16) . . . . ? C1 Fe1 Fe2 C5 -126.6(5) . . . . ? C3 Fe1 Fe2 C5 4.6(2) . . . . ? C2 Fe1 Fe2 C5 98.7(2) . . . . ? S1 Fe1 Fe2 C5 -83.35(17) . . . . ? S2 Fe1 Fe2 C5 -173.50(17) . . . . ? C1 Fe1 Fe2 S2 46.9(5) . . . . ? C3 Fe1 Fe2 S2 178.14(16) . . . . ? C2 Fe1 Fe2 S2 -87.84(17) . . . . ? S1 Fe1 Fe2 S2 90.15(5) . . . . ? C1 Fe1 Fe2 S1 -43.3(5) . . . . ? C3 Fe1 Fe2 S1 87.99(16) . . . . ? C2 Fe1 Fe2 S1 -177.99(17) . . . . ? S2 Fe1 Fe2 S1 -90.15(5) . . . . ? C1 Fe1 S1 Fe2 166.75(16) . . . . ? C3 Fe1 S1 Fe2 -96.08(15) . . . . ? C2 Fe1 S1 Fe2 5.6(5) . . . . ? S2 Fe1 S1 Fe2 61.05(4) . . . . ? C1 Fe1 S1 Mo 71.08(16) . . . . ? C3 Fe1 S1 Mo 168.25(16) . . . . ? C2 Fe1 S1 Mo -90.1(5) . . . . ? S2 Fe1 S1 Mo -34.62(4) . . . . ? Fe2 Fe1 S1 Mo -95.67(4) . . . . ? C6 Fe2 S1 Fe1 -160.20(18) . . . . ? C4 Fe2 S1 Fe1 3.2(3) . . . . ? C5 Fe2 S1 Fe1 103.77(17) . . . . ? S2 Fe2 S1 Fe1 -62.57(5) . . . . ? C6 Fe2 S1 Mo -62.70(18) . . . . ? C4 Fe2 S1 Mo 100.7(3) . . . . ? C5 Fe2 S1 Mo -158.74(17) . . . . ? S2 Fe2 S1 Mo 34.93(5) . . . . ? Fe1 Fe2 S1 Mo 97.49(4) . . . . ? C9 Mo S1 Fe1 -37.0(2) . . . . ? C12 Mo S1 Fe1 168.66(13) . . . . ? C16 Mo S1 Fe1 166.76(15) . . . . ? C8 Mo S1 Fe1 -88.1(2) . . . . ? C7 Mo S1 Fe1 -97.58(14) . . . . ? C15 Mo S1 Fe1 119.58(18) . . . . ? C10 Mo S1 Fe1 -38.29(13) . . . . ? C13 Mo S1 Fe1 135.93(13) . . . . ? C14 Mo S1 Fe1 109.34(13) . . . . ? C11 Mo S1 Fe1 -69.63(14) . . . . ? S2 Mo S1 Fe1 32.97(4) . . . . ? C9 Mo S1 Fe2 -102.73(19) . . . . ? C12 Mo S1 Fe2 102.96(13) . . . . ? C16 Mo S1 Fe2 101.05(16) . . . . ? C8 Mo S1 Fe2 -153.8(2) . . . . ? C7 Mo S1 Fe2 -163.29(14) . . . . ? C15 Mo S1 Fe2 53.87(18) . . . . ? C10 Mo S1 Fe2 -103.99(13) . . . . ? C13 Mo S1 Fe2 70.22(13) . . . . ? C14 Mo S1 Fe2 43.64(12) . . . . ? C11 Mo S1 Fe2 -135.33(14) . . . . ? S2 Mo S1 Fe2 -32.73(4) . . . . ? C6 Fe2 S2 Fe1 174.16(16) . . . . ? C4 Fe2 S2 Fe1 -91.01(15) . . . . ? C5 Fe2 S2 Fe1 18.5(5) . . . . ? S1 Fe2 S2 Fe1 61.20(4) . . . . ? C6 Fe2 S2 Mo 78.11(16) . . . . ? C4 Fe2 S2 Mo 172.95(15) . . . . ? C5 Fe2 S2 Mo -77.5(5) . . . . ? S1 Fe2 S2 Mo -34.85(4) . . . . ? Fe1 Fe2 S2 Mo -96.05(5) . . . . ? C1 Fe1 S2 Fe2 -165.70(18) . . . . ? C3 Fe1 S2 Fe2 -4.1(3) . . . . ? C2 Fe1 S2 Fe2 100.46(16) . . . . ? S1 Fe1 S2 Fe2 -62.51(5) . . . . ? C1 Fe1 S2 Mo -68.85(18) . . . . ? C3 Fe1 S2 Mo 92.8(3) . . . . ? C2 Fe1 S2 Mo -162.69(16) . . . . ? S1 Fe1 S2 Mo 34.34(4) . . . . ? Fe2 Fe1 S2 Mo 96.85(5) . . . . ? C9 Mo S2 Fe2 168.94(14) . . . . ? C12 Mo S2 Fe2 -35.98(17) . . . . ? C16 Mo S2 Fe2 -87.21(19) . . . . ? C8 Mo S2 Fe2 165.04(19) . . . . ? C7 Mo S2 Fe2 118.1(2) . . . . ? C15 Mo S2 Fe2 -98.17(14) . . . . ? C10 Mo S2 Fe2 137.38(13) . . . . ? C13 Mo S2 Fe2 -38.93(13) . . . . ? C14 Mo S2 Fe2 -71.19(13) . . . . ? C11 Mo S2 Fe2 109.91(13) . . . . ? S1 Mo S2 Fe2 33.34(4) . . . . ? C9 Mo S2 Fe1 103.20(14) . . . . ? C12 Mo S2 Fe1 -101.72(17) . . . . ? C16 Mo S2 Fe1 -152.95(18) . . . . ? C8 Mo S2 Fe1 99.30(19) . . . . ? C7 Mo S2 Fe1 52.4(2) . . . . ? C15 Mo S2 Fe1 -163.91(13) . . . . ? C10 Mo S2 Fe1 71.64(13) . . . . ? C13 Mo S2 Fe1 -104.67(13) . . . . ? C14 Mo S2 Fe1 -136.92(13) . . . . ? C11 Mo S2 Fe1 44.17(13) . . . . ? S1 Mo S2 Fe1 -32.40(4) . . . . ? C9 Mo C12 C16 27.6(4) . . . . ? C8 Mo C12 C16 44.7(3) . . . . ? C7 Mo C12 C16 80.1(3) . . . . ? C15 Mo C12 C16 -36.8(3) . . . . ? C10 Mo C12 C16 74.8(5) . . . . ? C13 Mo C12 C16 -113.9(4) . . . . ? C14 Mo C12 C16 -77.4(3) . . . . ? C11 Mo C12 C16 101.9(3) . . . . ? S1 Mo C12 C16 -177.4(3) . . . . ? S2 Mo C12 C16 -118.9(3) . . . . ? C9 Mo C12 C13 141.5(3) . . . . ? C16 Mo C12 C13 113.9(4) . . . . ? C8 Mo C12 C13 158.5(3) . . . . ? C7 Mo C12 C13 -166.0(3) . . . . ? C15 Mo C12 C13 77.0(3) . . . . ? C10 Mo C12 C13 -171.3(3) . . . . ? C14 Mo C12 C13 36.5(3) . . . . ? C11 Mo C12 C13 -144.3(3) . . . . ? S1 Mo C12 C13 -63.6(3) . . . . ? S2 Mo C12 C13 -5.0(4) . . . . ? C12 Mo C9 C10 143.2(3) . . . . ? C16 Mo C9 C10 159.1(3) . . . . ? C8 Mo C9 C10 113.6(5) . . . . ? C7 Mo C9 C10 77.0(3) . . . . ? C15 Mo C9 C10 -165.4(3) . . . . ? C13 Mo C9 C10 -167.9(3) . . . . ? C14 Mo C9 C10 -143.1(3) . . . . ? C11 Mo C9 C10 36.2(3) . . . . ? S1 Mo C9 C10 -2.2(4) . . . . ? S2 Mo C9 C10 -61.2(3) . . . . ? C12 Mo C9 C8 29.5(4) . . . . ? C16 Mo C9 C8 45.5(3) . . . . ? C7 Mo C9 C8 -36.7(3) . . . . ? C15 Mo C9 C8 81.0(3) . . . . ? C10 Mo C9 C8 -113.6(5) . . . . ? C13 Mo C9 C8 78.4(5) . . . . ? C14 Mo C9 C8 103.2(3) . . . . ? C11 Mo C9 C8 -77.4(3) . . . . ? S1 Mo C9 C8 -115.8(3) . . . . ? S2 Mo C9 C8 -174.8(3) . . . . ? C3 Fe1 C1 O1 63(5) . . . . ? C2 Fe1 C1 O1 -30(5) . . . . ? S1 Fe1 C1 O1 156(5) . . . . ? S2 Fe1 C1 O1 -126(5) . . . . ? Fe2 Fe1 C1 O1 -166(4) . . . . ? C6 Fe2 C5 O5 -93(30) . . . . ? C4 Fe2 C5 O5 172(100) . . . . ? S2 Fe2 C5 O5 63(30) . . . . ? S1 Fe2 C5 O5 22(30) . . . . ? Fe1 Fe2 C5 O5 79(30) . . . . ? C1 Fe1 C3 O3 91(14) . . . . ? C2 Fe1 C3 O3 -177(100) . . . . ? S1 Fe1 C3 O3 -17(14) . . . . ? S2 Fe1 C3 O3 -72(14) . . . . ? Fe2 Fe1 C3 O3 -75(14) . . . . ? C13 C12 C16 C15 -2.7(5) . . . . ? Mo C12 C16 C15 63.8(3) . . . . ? C13 C12 C16 Mo -66.5(3) . . . . ? C9 Mo C16 C15 83.7(3) . . . . ? C12 Mo C16 C15 -117.2(4) . . . . ? C8 Mo C16 C15 110.0(3) . . . . ? C7 Mo C16 C15 143.0(3) . . . . ? C10 Mo C16 C15 99.3(3) . . . . ? C13 Mo C16 C15 -78.4(3) . . . . ? C14 Mo C16 C15 -37.1(3) . . . . ? C11 Mo C16 C15 141.5(3) . . . . ? S1 Mo C16 C15 -113.9(3) . . . . ? S2 Mo C16 C15 -18.4(4) . . . . ? C9 Mo C16 C12 -159.2(3) . . . . ? C8 Mo C16 C12 -132.9(3) . . . . ? C7 Mo C16 C12 -99.9(3) . . . . ? C15 Mo C16 C12 117.2(4) . . . . ? C10 Mo C16 C12 -143.6(3) . . . . ? C13 Mo C16 C12 38.8(3) . . . . ? C14 Mo C16 C12 80.1(3) . . . . ? C11 Mo C16 C12 -101.3(3) . . . . ? S1 Mo C16 C12 3.2(3) . . . . ? S2 Mo C16 C12 98.7(3) . . . . ? C8 C9 C10 C11 1.8(5) . . . . ? Mo C9 C10 C11 -64.1(3) . . . . ? C8 C9 C10 Mo 65.9(3) . . . . ? C12 Mo C10 C9 -75.0(5) . . . . ? C16 Mo C10 C9 -27.4(4) . . . . ? C8 Mo C10 C9 -39.3(3) . . . . ? C7 Mo C10 C9 -81.2(3) . . . . ? C15 Mo C10 C9 18.3(4) . . . . ? C13 Mo C10 C9 139.6(11) . . . . ? C14 Mo C10 C9 62.0(4) . . . . ? C11 Mo C10 C9 -117.6(4) . . . . ? S1 Mo C10 C9 178.4(3) . . . . ? S2 Mo C10 C9 115.5(3) . . . . ? C9 Mo C10 C11 117.6(4) . . . . ? C12 Mo C10 C11 42.6(5) . . . . ? C16 Mo C10 C11 90.2(3) . . . . ? C8 Mo C10 C11 78.3(3) . . . . ? C7 Mo C10 C11 36.4(3) . . . . ? C15 Mo C10 C11 135.9(3) . . . . ? C13 Mo C10 C11 -102.8(11) . . . . ? C14 Mo C10 C11 179.6(3) . . . . ? S1 Mo C10 C11 -64.0(3) . . . . ? S2 Mo C10 C11 -126.9(3) . . . . ? C6 Fe2 C4 O4 108(9) . . . . ? C5 Fe2 C4 O4 -157(9) . . . . ? S2 Fe2 C4 O4 4(9) . . . . ? S1 Fe2 C4 O4 -57(9) . . . . ? Fe1 Fe2 C4 O4 -55(9) . . . . ? C1 Fe1 C2 O2 9(16) . . . . ? C3 Fe1 C2 O2 -88(16) . . . . ? S1 Fe1 C2 O2 171(16) . . . . ? S2 Fe1 C2 O2 119(16) . . . . ? Fe2 Fe1 C2 O2 176(100) . . . . ? C9 C10 C11 C7 0.2(5) . . . . ? Mo C10 C11 C7 -61.9(3) . . . . ? C9 C10 C11 Mo 62.1(3) . . . . ? C9 Mo C11 C10 -36.8(3) . . . . ? C12 Mo C11 C10 -157.9(3) . . . . ? C16 Mo C11 C10 -115.3(3) . . . . ? C8 Mo C11 C10 -79.4(3) . . . . ? C7 Mo C11 C10 -117.8(4) . . . . ? C15 Mo C11 C10 -76.3(4) . . . . ? C13 Mo C11 C10 164.1(3) . . . . ? C14 Mo C11 C10 -10(8) . . . . ? S1 Mo C11 C10 115.3(3) . . . . ? S2 Mo C11 C10 51.5(3) . . . . ? C9 Mo C11 C7 81.0(3) . . . . ? C12 Mo C11 C7 -40.1(4) . . . . ? C16 Mo C11 C7 2.5(4) . . . . ? C8 Mo C11 C7 38.3(3) . . . . ? C15 Mo C11 C7 41.5(5) . . . . ? C10 Mo C11 C7 117.8(4) . . . . ? C13 Mo C11 C7 -78.1(4) . . . . ? C14 Mo C11 C7 108(8) . . . . ? S1 Mo C11 C7 -126.9(3) . . . . ? S2 Mo C11 C7 169.3(3) . . . . ? C12 C16 C15 C14 2.4(5) . . . . ? Mo C16 C15 C14 65.2(3) . . . . ? C12 C16 C15 Mo -62.7(3) . . . . ? C9 Mo C15 C14 144.9(3) . . . . ? C12 Mo C15 C14 -78.5(3) . . . . ? C16 Mo C15 C14 -115.7(4) . . . . ? C8 Mo C15 C14 -179.3(3) . . . . ? C7 Mo C15 C14 -157.3(3) . . . . ? C10 Mo C15 C14 134.5(3) . . . . ? C13 Mo C15 C14 -36.5(3) . . . . ? C11 Mo C15 C14 178.0(3) . . . . ? S1 Mo C15 C14 -17.9(4) . . . . ? S2 Mo C15 C14 51.8(3) . . . . ? C9 Mo C15 C16 -99.3(3) . . . . ? C12 Mo C15 C16 37.2(3) . . . . ? C8 Mo C15 C16 -63.6(3) . . . . ? C7 Mo C15 C16 -41.5(3) . . . . ? C10 Mo C15 C16 -109.8(3) . . . . ? C13 Mo C15 C16 79.2(3) . . . . ? C14 Mo C15 C16 115.7(4) . . . . ? C11 Mo C15 C16 -66.3(4) . . . . ? S1 Mo C15 C16 97.9(3) . . . . ? S2 Mo C15 C16 167.6(3) . . . . ? C4 Fe2 C6 O6 11(4) . . . . ? C5 Fe2 C6 O6 -84(4) . . . . ? S2 Fe2 C6 O6 105(4) . . . . ? S1 Fe2 C6 O6 -177(4) . . . . ? Fe1 Fe2 C6 O6 120(4) . . . . ? C16 C15 C14 C13 -1.2(5) . . . . ? Mo C15 C14 C13 62.5(3) . . . . ? C16 C15 C14 Mo -63.7(3) . . . . ? C9 Mo C14 C15 -41.5(4) . . . . ? C12 Mo C14 C15 80.4(3) . . . . ? C16 Mo C14 C15 38.1(3) . . . . ? C8 Mo C14 C15 0.8(4) . . . . ? C7 Mo C14 C15 38.1(5) . . . . ? C10 Mo C14 C15 -77.7(4) . . . . ? C13 Mo C14 C15 117.8(4) . . . . ? C11 Mo C14 C15 -68(8) . . . . ? S1 Mo C14 C15 166.9(3) . . . . ? S2 Mo C14 C15 -129.6(3) . . . . ? C9 Mo C14 C13 -159.2(3) . . . . ? C12 Mo C14 C13 -37.4(3) . . . . ? C16 Mo C14 C13 -79.7(3) . . . . ? C8 Mo C14 C13 -117.0(3) . . . . ? C7 Mo C14 C13 -79.6(4) . . . . ? C15 Mo C14 C13 -117.8(4) . . . . ? C10 Mo C14 C13 164.6(3) . . . . ? C11 Mo C14 C13 174(8) . . . . ? S1 Mo C14 C13 49.2(3) . . . . ? S2 Mo C14 C13 112.7(3) . . . . ? C10 C9 C8 C7 -3.1(6) . . . . ? Mo C9 C8 C7 63.7(4) . . . . ? C10 C9 C8 Mo -66.8(3) . . . . ? C9 Mo C8 C7 -117.3(5) . . . . ? C12 Mo C8 C7 85.0(3) . . . . ? C16 Mo C8 C7 110.8(3) . . . . ? C15 Mo C8 C7 144.2(3) . . . . ? C10 Mo C8 C7 -78.8(3) . . . . ? C13 Mo C8 C7 101.4(4) . . . . ? C14 Mo C8 C7 143.7(3) . . . . ? C11 Mo C8 C7 -37.6(3) . . . . ? S1 Mo C8 C7 -16.0(4) . . . . ? S2 Mo C8 C7 -110.6(3) . . . . ? C12 Mo C8 C9 -157.7(3) . . . . ? C16 Mo C8 C9 -131.9(4) . . . . ? C7 Mo C8 C9 117.3(5) . . . . ? C15 Mo C8 C9 -98.6(3) . . . . ? C10 Mo C8 C9 38.4(3) . . . . ? C13 Mo C8 C9 -141.3(3) . . . . ? C14 Mo C8 C9 -99.0(3) . . . . ? C11 Mo C8 C9 79.6(3) . . . . ? S1 Mo C8 C9 101.2(3) . . . . ? S2 Mo C8 C9 6.6(4) . . . . ? C15 C14 C13 C12 -0.5(5) . . . . ? Mo C14 C13 C12 61.9(3) . . . . ? C15 C14 C13 Mo -62.4(3) . . . . ? C16 C12 C13 C14 2.0(5) . . . . ? Mo C12 C13 C14 -63.8(3) . . . . ? C16 C12 C13 Mo 65.7(3) . . . . ? C9 Mo C13 C14 39.3(5) . . . . ? C12 Mo C13 C14 117.1(4) . . . . ? C16 Mo C13 C14 78.2(3) . . . . ? C8 Mo C13 C14 88.6(4) . . . . ? C7 Mo C13 C14 134.9(3) . . . . ? C15 Mo C13 C14 36.2(3) . . . . ? C10 Mo C13 C14 -90.1(12) . . . . ? C11 Mo C13 C14 -179.8(3) . . . . ? S1 Mo C13 C14 -129.9(3) . . . . ? S2 Mo C13 C14 -66.7(3) . . . . ? C9 Mo C13 C12 -77.8(5) . . . . ? C16 Mo C13 C12 -38.9(3) . . . . ? C8 Mo C13 C12 -28.4(4) . . . . ? C7 Mo C13 C12 17.9(4) . . . . ? C15 Mo C13 C12 -80.9(3) . . . . ? C10 Mo C13 C12 152.8(10) . . . . ? C14 Mo C13 C12 -117.1(4) . . . . ? C11 Mo C13 C12 63.1(4) . . . . ? S1 Mo C13 C12 113.0(3) . . . . ? S2 Mo C13 C12 176.2(3) . . . . ? C10 C11 C7 C8 -2.1(5) . . . . ? Mo C11 C7 C8 -64.2(3) . . . . ? C10 C11 C7 Mo 62.1(3) . . . . ? C9 C8 C7 C11 3.3(6) . . . . ? Mo C8 C7 C11 65.8(3) . . . . ? C9 C8 C7 Mo -62.5(3) . . . . ? C9 Mo C7 C11 -77.7(3) . . . . ? C12 Mo C7 C11 146.6(3) . . . . ? C16 Mo C7 C11 -177.9(3) . . . . ? C8 Mo C7 C11 -114.9(5) . . . . ? C15 Mo C7 C11 -155.0(3) . . . . ? C10 Mo C7 C11 -36.3(3) . . . . ? C13 Mo C7 C11 136.2(3) . . . . ? C14 Mo C7 C11 -177.9(3) . . . . ? S1 Mo C7 C11 53.9(3) . . . . ? S2 Mo C7 C11 -14.3(4) . . . . ? C9 Mo C7 C8 37.3(3) . . . . ? C12 Mo C7 C8 -98.4(3) . . . . ? C16 Mo C7 C8 -62.9(3) . . . . ? C15 Mo C7 C8 -40.1(4) . . . . ? C10 Mo C7 C8 78.6(3) . . . . ? C13 Mo C7 C8 -108.8(3) . . . . ? C14 Mo C7 C8 -63.0(5) . . . . ? C11 Mo C7 C8 114.9(5) . . . . ? S1 Mo C7 C8 168.9(3) . . . . ? S2 Mo C7 C8 100.6(3) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.644 _refine_diff_density_min -0.983 _refine_diff_density_rms 0.171