Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Dr Graeme Hogarth' _publ_contact_author_address ; Department of Chemistry University College London 20 Gordon Street LONDON WC1H OAJ U.K. ; _publ_contact_author_email G.HOGARTH@UCL.AC.UK _publ_section_title ; Regioselective and reversible carbon-nitrogen bond formation: Synthesis, structure and reactivity of ureato-bridged complexes [Mo2(NAr)2( -X){ -ArNC(O)NAr}(S2CNR2)2] (Ar = Ph, p-tol; X = S, NAr; R = Me, Et, Pr) ; loop_ _publ_author_name 'Graeme Hogarth' 'Idris Richards' data_str712 _database_code_depnum_ccdc_archive 'CCDC 253354' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H34 Mo2 N4 S7' _chemical_formula_weight 794.85 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 18.516(4) _cell_length_b 12.012(2) _cell_length_c 14.994(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.13(3) _cell_angle_gamma 90.00 _cell_volume 3334.9(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 15 _cell_measurement_theta_max 25 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.583 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1608 _exptl_absorpt_coefficient_mu 1.211 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.741 _exptl_absorpt_correction_T_max 0.988 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nicolet R3' _diffrn_measurement_method omega-2theta _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 2980 _diffrn_reflns_av_R_equivalents 0.0231 _diffrn_reflns_av_sigmaI/netI 0.0387 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.72 _diffrn_reflns_theta_max 25.11 _reflns_number_total 2886 _reflns_number_gt 2104 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Nicolet R3' _computing_cell_refinement 'Nicolet R3' _computing_data_reduction XDISK _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XP _computing_publication_material CIFTAB _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^)+(0.0358P)^2^+29.1176P] 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 2886 _refine_ls_number_parameters 172 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0776 _refine_ls_R_factor_gt 0.0539 _refine_ls_wR_factor_ref 0.1319 _refine_ls_wR_factor_gt 0.1147 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_restrained_S_all 1.084 _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 0.44152(3) 0.21377(5) 0.19142(4) 0.0492(2) Uani 1 1 d . . . S1 S 0.41760(12) 0.1335(2) 0.04096(15) 0.0852(8) Uani 1 1 d . . . S2 S 0.31919(10) 0.12544(18) 0.18874(14) 0.0651(5) Uani 1 1 d . . . S3 S 0.56492(10) 0.20000(18) 0.14997(13) 0.0624(5) Uani 1 1 d . . . S4 S 0.5323(2) 0.0566(3) 0.1920(3) 0.0645(10) Uani 0.50 1 d P . . N1 N 0.2847(3) 0.0536(5) 0.0231(4) 0.0657(17) Uani 1 1 d . . . N2 N 0.4253(3) 0.3540(5) 0.1743(4) 0.0604(16) Uani 1 1 d . . . C1 C 0.3329(4) 0.0989(6) 0.0761(5) 0.0568(17) Uani 1 1 d . . . C2 C 0.3024(5) 0.0265(7) -0.0717(5) 0.069(2) Uani 1 1 d . . . H2A H 0.2735 -0.0350 -0.0917 0.080 Uiso 1 1 d R . . H2B H 0.3524 0.0061 -0.0767 0.080 Uiso 1 1 d R . . C3 C 0.2889(7) 0.1264(9) -0.1305(7) 0.113(4) Uani 1 1 d . . . H3A H 0.3000 0.1105 -0.1917 0.080 Uiso 1 1 d R . . H3B H 0.2389 0.1459 -0.1253 0.080 Uiso 1 1 d R . . H3C H 0.3182 0.1873 -0.1102 0.080 Uiso 1 1 d R . . C4 C 0.2103(4) 0.0264(9) 0.0544(7) 0.089(3) Uani 1 1 d . . . H4A H 0.1765 0.0296 0.0059 0.080 Uiso 1 1 d R . . H4B H 0.1923 0.0747 0.1003 0.080 Uiso 1 1 d R . . C5 C 0.2035(6) -0.0941(11) 0.0764(8) 0.134(5) Uani 1 1 d . . . H5A H 0.1552 -0.1126 0.0943 0.080 Uiso 1 1 d R . . H5B H 0.2191 -0.1450 0.0310 0.080 Uiso 1 1 d R . . H5C H 0.2353 -0.0991 0.1269 0.080 Uiso 1 1 d R . . C10 C 0.4250(4) 0.4695(6) 0.1645(5) 0.0516(16) Uani 1 1 d . . . C11 C 0.3703(4) 0.5346(6) 0.1982(5) 0.064(2) Uani 1 1 d . . . H11A H 0.3306 0.4989 0.2279 0.080 Uiso 1 1 d R . . C12 C 0.3702(5) 0.6490(7) 0.1873(6) 0.072(2) Uani 1 1 d . . . H12A H 0.3331 0.6934 0.2144 0.080 Uiso 1 1 d R . . C13 C 0.4247(5) 0.7000(6) 0.1405(7) 0.078(2) Uani 1 1 d . . . C14 C 0.4793(5) 0.6366(7) 0.1072(7) 0.098(3) Uani 1 1 d . . . H14A H 0.5181 0.6717 0.0756 0.080 Uiso 1 1 d R . . C15 C 0.4804(5) 0.5219(7) 0.1181(7) 0.082(3) Uani 1 1 d . . . H15A H 0.5187 0.4783 0.0929 0.080 Uiso 1 1 d R . . C16 C 0.4248(7) 0.8248(7) 0.1265(9) 0.121(4) Uani 1 1 d . . . H16A H 0.4662 0.8465 0.0922 0.080 Uiso 1 1 d R . . H16B H 0.3816 0.8441 0.0946 0.080 Uiso 1 1 d R . . H16C H 0.4255 0.8626 0.1829 0.080 Uiso 1 1 d 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 Mo 0.0454(3) 0.0379(3) 0.0644(4) 0.0050(3) 0.0013(2) -0.0012(3) S1 0.0712(14) 0.116(2) 0.0690(13) -0.0130(13) 0.0140(10) -0.0385(14) S2 0.0456(10) 0.0753(13) 0.0742(12) -0.0055(10) 0.0092(9) -0.0088(9) S3 0.0481(10) 0.0743(13) 0.0648(11) 0.0012(10) 0.0094(8) -0.0087(9) S4 0.060(2) 0.048(2) 0.085(3) -0.0065(19) 0.0138(19) -0.0058(17) N1 0.057(4) 0.065(4) 0.075(4) -0.001(3) -0.002(3) -0.006(3) N2 0.061(4) 0.048(3) 0.073(4) 0.014(3) -0.005(3) 0.003(3) C1 0.051(4) 0.045(4) 0.074(5) 0.004(4) -0.001(3) -0.003(3) C2 0.070(5) 0.062(5) 0.076(5) -0.014(4) -0.006(4) -0.004(4) C3 0.151(10) 0.098(8) 0.090(7) 0.021(6) -0.028(7) -0.023(8) C4 0.056(5) 0.119(9) 0.092(6) -0.018(6) -0.009(4) -0.013(5) C5 0.117(9) 0.146(12) 0.140(11) -0.035(9) 0.032(8) -0.078(9) C10 0.047(4) 0.044(4) 0.065(4) 0.000(3) 0.001(3) -0.004(3) C11 0.065(5) 0.055(4) 0.072(5) 0.010(4) 0.014(4) 0.001(4) C12 0.074(5) 0.054(5) 0.089(6) -0.006(4) 0.019(4) 0.009(4) C13 0.087(6) 0.037(4) 0.109(7) 0.008(4) 0.026(5) 0.003(4) C14 0.091(7) 0.051(5) 0.152(9) 0.012(6) 0.054(6) -0.014(5) C15 0.073(5) 0.047(4) 0.125(8) 0.003(5) 0.038(5) 0.009(4) C16 0.144(10) 0.032(4) 0.186(12) -0.001(6) 0.051(9) -0.004(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo N2 1.731(6) . ? Mo S3 2.3750(19) . ? Mo S3 2.387(2) 2_655 ? Mo S1 2.492(2) . ? Mo S2 2.502(2) . ? Mo S4 2.528(4) . ? Mo S4 2.618(4) 2_655 ? Mo Mo 2.7854(15) 2_655 ? S1 C1 1.707(7) . ? S2 C1 1.738(8) . ? S3 S4 1.932(4) . ? S3 Mo 2.387(2) 2_655 ? S4 S4 2.114(8) 2_655 ? S4 Mo 2.618(4) 2_655 ? N1 C1 1.312(9) . ? N1 C4 1.492(10) . ? N1 C2 1.496(10) . ? N2 C10 1.395(9) . ? C2 C3 1.509(12) . ? C4 C5 1.490(15) . ? C10 C11 1.376(10) . ? C10 C15 1.392(10) . ? C11 C12 1.385(10) . ? C12 C13 1.374(11) . ? C13 C14 1.361(12) . ? C13 C16 1.514(11) . ? C14 C15 1.388(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 N2 Mo S3 101.3(2) . . ? N2 Mo S3 101.9(2) . 2_655 ? S3 Mo S3 107.83(6) . 2_655 ? N2 Mo S1 102.2(2) . . ? S3 Mo S1 84.57(8) . . ? S3 Mo S1 149.98(8) 2_655 . ? N2 Mo S2 104.7(2) . . ? S3 Mo S2 146.92(8) . . ? S3 Mo S2 86.52(7) 2_655 . ? S1 Mo S2 70.26(7) . . ? N2 Mo S4 147.5(2) . . ? S3 Mo S4 46.28(10) . . ? S3 Mo S4 88.84(11) 2_655 . ? S1 Mo S4 80.26(12) . . ? S2 Mo S4 106.57(10) . . ? N2 Mo S4 146.4(2) . 2_655 ? S3 Mo S4 87.00(10) . 2_655 ? S3 Mo S4 45.11(10) 2_655 2_655 ? S1 Mo S4 110.96(12) . 2_655 ? S2 Mo S4 82.59(11) . 2_655 ? S4 Mo S4 48.46(17) . 2_655 ? N2 Mo Mo 103.2(2) . 2_655 ? S3 Mo Mo 54.41(5) . 2_655 ? S3 Mo Mo 54.00(5) 2_655 2_655 ? S1 Mo Mo 135.02(7) . 2_655 ? S2 Mo Mo 135.46(6) . 2_655 ? S4 Mo Mo 58.80(10) . 2_655 ? S4 Mo Mo 55.69(9) 2_655 2_655 ? C1 S1 Mo 88.6(3) . . ? C1 S2 Mo 87.7(2) . . ? S4 S3 Mo 71.04(13) . . ? S4 S3 Mo 73.78(14) . 2_655 ? Mo S3 Mo 71.59(6) . 2_655 ? S3 S4 S4 116.50(13) . 2_655 ? S3 S4 Mo 62.68(13) . . ? S4 S4 Mo 67.99(14) 2_655 . ? S3 S4 Mo 61.10(12) . 2_655 ? S4 S4 Mo 63.54(15) 2_655 2_655 ? Mo S4 Mo 65.51(10) . 2_655 ? C1 N1 C4 121.8(7) . . ? C1 N1 C2 121.0(6) . . ? C4 N1 C2 117.2(6) . . ? C10 N2 Mo 169.9(5) . . ? N1 C1 S1 122.6(6) . . ? N1 C1 S2 124.3(6) . . ? S1 C1 S2 113.1(4) . . ? N1 C2 C3 110.3(7) . . ? C5 C4 N1 111.1(8) . . ? C11 C10 C15 118.1(6) . . ? C11 C10 N2 121.9(6) . . ? C15 C10 N2 120.0(6) . . ? C10 C11 C12 121.4(7) . . ? C13 C12 C11 120.1(7) . . ? C14 C13 C12 119.0(7) . . ? C14 C13 C16 120.1(8) . . ? C12 C13 C16 120.9(8) . . ? C13 C14 C15 121.6(8) . . ? C14 C15 C10 119.8(7) . . ? 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 N2 Mo S1 C1 -97.6(3) . . . . ? S3 Mo S1 C1 162.0(3) . . . . ? S3 Mo S1 C1 45.3(3) 2_655 . . . ? S2 Mo S1 C1 3.8(3) . . . . ? S4 Mo S1 C1 115.5(3) . . . . ? S4 Mo S1 C1 77.3(3) 2_655 . . . ? Mo Mo S1 C1 139.2(2) 2_655 . . . ? N2 Mo S2 C1 94.2(3) . . . . ? S3 Mo S2 C1 -46.5(3) . . . . ? S3 Mo S2 C1 -164.4(2) 2_655 . . . ? S1 Mo S2 C1 -3.8(2) . . . . ? S4 Mo S2 C1 -76.7(3) . . . . ? S4 Mo S2 C1 -119.2(3) 2_655 . . . ? Mo Mo S2 C1 -138.7(2) 2_655 . . . ? N2 Mo S3 S4 176.9(3) . . . . ? S3 Mo S3 S4 70.30(17) 2_655 . . . ? S1 Mo S3 S4 -81.71(16) . . . . ? S2 Mo S3 S4 -41.8(2) . . . . ? S4 Mo S3 S4 29.7(2) 2_655 . . . ? Mo Mo S3 S4 78.64(15) 2_655 . . . ? N2 Mo S3 Mo 98.2(2) . . . 2_655 ? S3 Mo S3 Mo -8.34(11) 2_655 . . 2_655 ? S1 Mo S3 Mo -160.35(8) . . . 2_655 ? S2 Mo S3 Mo -120.47(12) . . . 2_655 ? S4 Mo S3 Mo -78.64(15) . . . 2_655 ? S4 Mo S3 Mo -48.95(10) 2_655 . . 2_655 ? Mo S3 S4 S4 -43.2(3) . . . 2_655 ? Mo S3 S4 S4 32.4(3) 2_655 . . 2_655 ? Mo S3 S4 Mo 75.65(7) 2_655 . . . ? Mo S3 S4 Mo -75.65(7) . . . 2_655 ? N2 Mo S4 S3 -5.7(5) . . . . ? S3 Mo S4 S3 -116.30(13) 2_655 . . . ? S1 Mo S4 S3 91.79(13) . . . . ? S2 Mo S4 S3 157.68(11) . . . . ? S4 Mo S4 S3 -138.6(3) 2_655 . . . ? Mo Mo S4 S3 -68.76(11) 2_655 . . . ? N2 Mo S4 S4 132.9(4) . . . 2_655 ? S3 Mo S4 S4 138.6(3) . . . 2_655 ? S3 Mo S4 S4 22.34(18) 2_655 . . 2_655 ? S1 Mo S4 S4 -129.57(19) . . . 2_655 ? S2 Mo S4 S4 -63.7(2) . . . 2_655 ? Mo Mo S4 S4 69.88(19) 2_655 . . 2_655 ? N2 Mo S4 Mo 63.0(4) . . . 2_655 ? S3 Mo S4 Mo 68.76(11) . . . 2_655 ? S3 Mo S4 Mo -47.55(8) 2_655 . . 2_655 ? S1 Mo S4 Mo 160.55(9) . . . 2_655 ? S2 Mo S4 Mo -133.57(7) . . . 2_655 ? S4 Mo S4 Mo -69.88(19) 2_655 . . 2_655 ? S3 Mo N2 C10 -31(3) . . . . ? S3 Mo N2 C10 80(3) 2_655 . . . ? S1 Mo N2 C10 -118(3) . . . . ? S2 Mo N2 C10 170(3) . . . . ? S4 Mo N2 C10 -27(3) . . . . ? S4 Mo N2 C10 71(3) 2_655 . . . ? Mo Mo N2 C10 25(3) 2_655 . . . ? C4 N1 C1 S1 -178.5(7) . . . . ? C2 N1 C1 S1 1.8(10) . . . . ? C4 N1 C1 S2 3.8(11) . . . . ? C2 N1 C1 S2 -175.9(6) . . . . ? Mo S1 C1 N1 176.4(6) . . . . ? Mo S1 C1 S2 -5.6(4) . . . . ? Mo S2 C1 N1 -176.5(6) . . . . ? Mo S2 C1 S1 5.6(4) . . . . ? C1 N1 C2 C3 -86.9(9) . . . . ? C4 N1 C2 C3 93.3(9) . . . . ? C1 N1 C4 C5 -99.9(10) . . . . ? C2 N1 C4 C5 79.8(10) . . . . ? Mo N2 C10 C11 -135(3) . . . . ? Mo N2 C10 C15 46(4) . . . . ? C15 C10 C11 C12 -0.6(13) . . . . ? N2 C10 C11 C12 -179.3(8) . . . . ? C10 C11 C12 C13 1.3(14) . . . . ? C11 C12 C13 C14 -1.6(15) . . . . ? C11 C12 C13 C16 179.0(10) . . . . ? C12 C13 C14 C15 1.1(18) . . . . ? C16 C13 C14 C15 -179.4(11) . . . . ? C13 C14 C15 C10 -0.4(18) . . . . ? C11 C10 C15 C14 0.2(14) . . . . ? N2 C10 C15 C14 178.9(9) . . . . ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 25.11 _diffrn_measured_fraction_theta_full 0.969 _refine_diff_density_max 1.059 _refine_diff_density_min -0.745 _refine_diff_density_rms 0.102 data_str0018 _database_code_depnum_ccdc_archive 'CCDC 253355' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H48 Mo2 N7 O S4' _chemical_formula_weight 1023.02 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 35.949(2) _cell_length_b 16.1750(11) _cell_length_c 17.8306(12) _cell_angle_alpha 90.00 _cell_angle_beta 112.9570(10) _cell_angle_gamma 90.00 _cell_volume 9546.8(11) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description rod _exptl_crystal_colour red _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.424 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4184 _exptl_absorpt_coefficient_mu 0.741 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8969 _exptl_absorpt_correction_T_max 0.9853 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29627 _diffrn_reflns_av_R_equivalents 0.0723 _diffrn_reflns_av_sigmaI/netI 0.1160 _diffrn_reflns_limit_h_min -47 _diffrn_reflns_limit_h_max 43 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 28.30 _reflns_number_total 11157 _reflns_number_gt 5984 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1013P)^2^+17.7215P] 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 11157 _refine_ls_number_parameters 576 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1573 _refine_ls_R_factor_gt 0.0804 _refine_ls_wR_factor_ref 0.2296 _refine_ls_wR_factor_gt 0.1942 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.016 _refine_ls_shift/su_mean 0.002 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 0.114524(17) 0.33212(4) 0.04045(4) 0.04127(19) Uani 1 1 d . . . Mo2 Mo 0.114237(18) 0.19007(4) 0.10868(4) 0.0524(2) Uani 1 1 d . . . S1 S 0.13997(6) 0.37678(14) -0.06361(12) 0.0590(5) Uani 1 1 d . . . S2 S 0.14605(6) 0.47388(13) 0.07601(14) 0.0628(6) Uani 1 1 d . . . S3 S 0.14450(8) 0.06176(16) 0.0822(2) 0.0926(9) Uani 1 1 d . . . S4 S 0.14888(8) 0.1168(2) 0.24164(18) 0.1024(10) Uani 1 1 d . . . N1 N 0.1723(2) 0.5287(5) -0.0367(5) 0.077(2) Uani 1 1 d . . . N2 N 0.1862(3) -0.0242(7) 0.2166(7) 0.118(3) Uani 1 1 d . . . N3 N 0.11933(17) 0.3107(3) 0.1636(4) 0.0481(14) Uani 1 1 d . . . N4 N 0.17320(16) 0.2738(3) 0.1445(3) 0.0457(14) Uani 1 1 d . . . N5 N 0.06392(17) 0.3586(4) -0.0026(3) 0.0473(14) Uani 1 1 d . . . N6 N 0.11265(16) 0.2184(4) 0.0001(3) 0.0519(15) Uani 1 1 d . . . N7 N 0.06478(18) 0.1669(4) 0.0936(4) 0.0589(16) Uani 1 1 d . . . O1 O 0.18283(15) 0.3350(4) 0.2701(3) 0.0702(16) Uani 1 1 d . . . C1 C 0.1551(2) 0.4679(5) -0.0109(5) 0.0550(19) Uani 1 1 d . . . C2 C 0.1836(3) 0.6073(6) 0.0093(7) 0.096(3) Uani 1 1 d . . . H2A H 0.1877 0.5975 0.0668 0.115 Uiso 1 1 calc R . . H2B H 0.2094 0.6278 0.0083 0.115 Uiso 1 1 calc R . . C3 C 0.1526(5) 0.6683(9) -0.0257(13) 0.206(10) Uani 1 1 d . . . H3A H 0.1465 0.6734 -0.0841 0.310 Uiso 1 1 calc R . . H3B H 0.1620 0.7217 0.0010 0.310 Uiso 1 1 calc R . . H3C H 0.1282 0.6515 -0.0179 0.310 Uiso 1 1 calc R . . C4 C 0.1794(5) 0.5226(9) -0.1105(6) 0.149(7) Uani 1 1 d . . . H4A H 0.1762 0.5777 -0.1367 0.179 Uiso 1 1 calc R . . H4B H 0.1595 0.4845 -0.1490 0.179 Uiso 1 1 calc R . . C5 C 0.2226(5) 0.4901(11) -0.0900(11) 0.193(9) Uani 1 1 d . . . H5A H 0.2422 0.5341 -0.0638 0.289 Uiso 1 1 calc R . . H5B H 0.2254 0.4729 -0.1403 0.289 Uiso 1 1 calc R . . H5C H 0.2278 0.4428 -0.0530 0.289 Uiso 1 1 calc R . . C6 C 0.1592(3) 0.0469(6) 0.1727(9) 0.102(4) Uani 1 1 d . . . C7 C 0.2028(6) -0.0819(9) 0.1680(11) 0.166(7) Uani 1 1 d . . . H7A H 0.2283 -0.1085 0.2044 0.200 Uiso 1 1 calc R . . H7B H 0.2080 -0.0507 0.1253 0.200 Uiso 1 1 calc R . . C8 C 0.1678(6) -0.1504(10) 0.1276(13) 0.189(8) Uani 1 1 d . . . H8A H 0.1655 -0.1852 0.1706 0.283 Uiso 1 1 calc R . . H8B H 0.1748 -0.1849 0.0897 0.283 Uiso 1 1 calc R . . H8C H 0.1420 -0.1225 0.0981 0.283 Uiso 1 1 calc R . . C9 C 0.2004(4) -0.0366(10) 0.2984(8) 0.143(6) Uani 1 1 d . . . H9 H 0.1851 -0.0617 0.3253 0.172 Uiso 1 1 calc R . . C10 C 0.2428(5) -0.0062(10) 0.3413(11) 0.258(14) Uani 1 1 d . . . H10A H 0.2617 -0.0499 0.3416 0.387 Uiso 1 1 calc R . . H10B H 0.2473 0.0088 0.3974 0.387 Uiso 1 1 calc R . . H10C H 0.2471 0.0424 0.3128 0.387 Uiso 1 1 calc R . . C11 C 0.1631(2) 0.3098(5) 0.2026(5) 0.0516(18) Uani 1 1 d . . . C20 C 0.0978(2) 0.3515(5) 0.2071(4) 0.0522(19) Uani 1 1 d . . . C21 C 0.0913(3) 0.4309(7) 0.2036(6) 0.091(3) Uani 1 1 d . . . H21 H 0.0999 0.4637 0.1691 0.110 Uiso 1 1 calc R . . C22 C 0.0725(3) 0.4689(7) 0.2483(6) 0.098(4) Uani 1 1 d . . . H22 H 0.0682 0.5268 0.2425 0.118 Uiso 1 1 calc R . . C23 C 0.0603(2) 0.4288(9) 0.2987(5) 0.089(4) Uani 1 1 d . . . C24 C 0.0677(6) 0.3447(11) 0.3043(11) 0.182(8) Uani 1 1 d . . . H24 H 0.0613 0.3130 0.3426 0.218 Uiso 1 1 calc R . . C25 C 0.0839(5) 0.3063(8) 0.2562(8) 0.143(6) Uani 1 1 d . . . H25 H 0.0857 0.2477 0.2566 0.171 Uiso 1 1 calc R . . C26 C 0.0421(3) 0.4726(9) 0.3506(7) 0.140(6) Uani 1 1 d . . . H26A H 0.0636 0.4897 0.4019 0.210 Uiso 1 1 calc R . . H26B H 0.0235 0.4352 0.3620 0.210 Uiso 1 1 calc R . . H26C H 0.0273 0.5215 0.3216 0.210 Uiso 1 1 calc R . . C30 C 0.21306(19) 0.2530(4) 0.1589(4) 0.0474(17) Uani 1 1 d . . . C31 C 0.2392(2) 0.2134(5) 0.2301(5) 0.065(2) Uani 1 1 d . . . H31 H 0.2303 0.2021 0.2727 0.078 Uiso 1 1 calc R . . C32 C 0.2775(2) 0.1910(5) 0.2387(6) 0.070(2) Uani 1 1 d . . . H32 H 0.2946 0.1639 0.2871 0.085 Uiso 1 1 calc R . . C33 C 0.2913(2) 0.2066(6) 0.1798(6) 0.075(3) Uani 1 1 d . . . H33 H 0.3180 0.1908 0.1870 0.091 Uiso 1 1 calc R . . C34 C 0.2664(3) 0.2458(6) 0.1088(5) 0.077(3) Uani 1 1 d . . . H34 H 0.2759 0.2573 0.0671 0.093 Uiso 1 1 calc R . . C35 C 0.2276(2) 0.2683(5) 0.0991(5) 0.062(2) Uani 1 1 d . . . H35 H 0.2106 0.2949 0.0501 0.074 Uiso 1 1 calc R . . C40 C 0.0224(2) 0.3549(5) -0.0422(4) 0.0491(17) Uani 1 1 d . . . C41 C 0.0060(2) 0.3124(5) -0.1161(5) 0.065(2) Uani 1 1 d . . . H41 H 0.0232 0.2877 -0.1388 0.079 Uiso 1 1 calc R . . C42 C -0.0353(3) 0.3066(6) -0.1557(6) 0.076(3) Uani 1 1 d . . . H42 H -0.0462 0.2756 -0.2048 0.092 Uiso 1 1 calc R . . C43 C -0.0611(2) 0.3440(6) -0.1267(7) 0.080(3) Uani 1 1 d . . . C44 C -0.0445(2) 0.3872(6) -0.0542(6) 0.081(3) Uani 1 1 d . . . H44 H -0.0620 0.4137 -0.0331 0.098 Uiso 1 1 calc R . . C45 C -0.0028(2) 0.3927(6) -0.0115(5) 0.068(2) Uani 1 1 d . . . H45 H 0.0080 0.4224 0.0384 0.081 Uiso 1 1 calc R . . C46 C -0.1066(3) 0.3374(7) -0.1701(8) 0.121(5) Uani 1 1 d . . . H46A H -0.1133 0.3112 -0.2233 0.181 Uiso 1 1 calc R . . H46B H -0.1186 0.3928 -0.1776 0.181 Uiso 1 1 calc R . . H46C H -0.1174 0.3038 -0.1373 0.181 Uiso 1 1 calc R . . C50 C 0.0254(3) 0.1535(5) 0.0890(7) 0.072(3) Uani 1 1 d . . . C51 C -0.0072(5) 0.1662(15) 0.0329(12) 0.078(6) Uani 0.50 1 d P . . C81 C 0.0038(5) 0.0834(11) 0.0343(10) 0.064(4) Uani 0.50 1 d P . . C52 C -0.0454(6) 0.1490(19) 0.0346(14) 0.084(6) Uani 0.50 1 d P . . C82 C -0.0371(6) 0.0681(15) 0.0279(14) 0.092(7) Uani 0.50 1 d P . . C53 C -0.0520(3) 0.1249(8) 0.0854(13) 0.121(5) Uani 1 1 d . . . C54 C -0.0160(6) 0.1220(16) 0.1809(14) 0.107(8) Uani 0.50 1 d P . . C84 C -0.0370(8) 0.1949(18) 0.098(3) 0.136(12) Uani 0.50 1 d P . . C55 C 0.0226(6) 0.1358(16) 0.1750(14) 0.105(7) Uani 0.50 1 d P . . C85 C 0.0054(7) 0.2067(12) 0.109(2) 0.107(8) Uani 0.50 1 d P . . C56 C -0.0929(3) 0.1055(8) 0.0891(10) 0.147(6) Uani 1 1 d . . . H56A H -0.1121 0.0885 0.0351 0.221 Uiso 1 1 calc R . . H56B H -0.1032 0.1549 0.1066 0.221 Uiso 1 1 calc R . . H56C H -0.0897 0.0606 0.1281 0.221 Uiso 1 1 calc R . . C60 C 0.1018(2) 0.1788(4) -0.0758(4) 0.0507(18) Uani 1 1 d . . . C61 C 0.0679(3) 0.1309(6) -0.1051(6) 0.082(3) Uani 1 1 d . . . H61 H 0.0521 0.1239 -0.0735 0.099 Uiso 1 1 calc R . . C62 C 0.0560(3) 0.0920(7) -0.1811(6) 0.090(3) Uani 1 1 d . . . H62 H 0.0322 0.0593 -0.2001 0.108 Uiso 1 1 calc R . . C63 C 0.0774(3) 0.0997(6) -0.2281(5) 0.073(3) Uani 1 1 d . . . C64 C 0.1119(3) 0.1465(6) -0.1986(6) 0.086(3) Uani 1 1 d . . . H64 H 0.1274 0.1532 -0.2308 0.103 Uiso 1 1 calc R . . C65 C 0.1249(3) 0.1849(6) -0.1214(6) 0.078(3) Uani 1 1 d . . . H65 H 0.1496 0.2149 -0.1012 0.094 Uiso 1 1 calc R . . C66 C 0.0633(3) 0.0596(7) -0.3108(6) 0.105(4) Uani 1 1 d . . . H66A H 0.0646 0.0998 -0.3508 0.158 Uiso 1 1 calc R . . H66B H 0.0354 0.0404 -0.3266 0.158 Uiso 1 1 calc R . . H66C H 0.0808 0.0124 -0.3087 0.158 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 0.0311(3) 0.0549(4) 0.0366(3) -0.0026(3) 0.0119(2) -0.0003(3) Mo2 0.0363(4) 0.0551(4) 0.0575(4) 0.0052(3) 0.0094(3) -0.0019(3) S1 0.0479(11) 0.0891(15) 0.0425(11) 0.0011(10) 0.0204(9) -0.0046(10) S2 0.0639(13) 0.0628(12) 0.0755(15) -0.0102(11) 0.0423(12) -0.0104(10) S3 0.0712(17) 0.0725(16) 0.118(2) -0.0008(16) 0.0194(16) 0.0109(12) S4 0.0672(16) 0.125(2) 0.0871(19) 0.0549(17) 0.0004(14) -0.0136(15) N1 0.055(4) 0.092(6) 0.076(5) 0.025(4) 0.017(4) -0.012(4) N2 0.082(7) 0.132(9) 0.117(9) 0.019(7) 0.014(6) 0.001(6) N3 0.038(3) 0.061(4) 0.043(3) -0.002(3) 0.015(3) 0.002(3) N4 0.036(3) 0.053(3) 0.047(3) -0.003(3) 0.015(3) -0.003(3) N5 0.042(3) 0.060(4) 0.042(3) 0.003(3) 0.018(3) -0.004(3) N6 0.040(3) 0.073(4) 0.044(4) -0.011(3) 0.018(3) -0.005(3) N7 0.044(4) 0.061(4) 0.066(4) 0.006(3) 0.016(3) -0.005(3) O1 0.045(3) 0.119(5) 0.041(3) -0.020(3) 0.010(3) -0.001(3) C1 0.042(4) 0.072(5) 0.054(5) 0.019(4) 0.022(4) 0.001(4) C2 0.083(7) 0.087(7) 0.110(9) 0.024(7) 0.030(6) -0.020(6) C3 0.160(16) 0.094(10) 0.30(3) 0.051(13) 0.026(16) 0.021(10) C4 0.223(16) 0.182(13) 0.062(7) -0.014(8) 0.076(9) -0.131(13) C5 0.199(16) 0.242(19) 0.230(19) -0.120(15) 0.185(16) -0.137(15) C6 0.091(8) 0.061(6) 0.189(14) -0.043(7) 0.093(9) -0.019(5) C7 0.196(18) 0.120(12) 0.219(19) 0.037(12) 0.120(16) 0.047(12) C8 0.23(2) 0.128(13) 0.26(2) 0.047(14) 0.150(19) 0.010(14) C9 0.084(8) 0.210(15) 0.089(9) 0.033(9) -0.016(7) -0.068(9) C10 0.198(18) 0.163(15) 0.23(2) 0.104(14) -0.113(15) -0.088(13) C11 0.038(4) 0.068(5) 0.040(4) 0.002(4) 0.005(3) 0.005(3) C20 0.039(4) 0.084(6) 0.036(4) -0.012(4) 0.016(3) -0.001(4) C21 0.103(8) 0.115(8) 0.082(7) 0.039(6) 0.064(6) 0.057(6) C22 0.100(8) 0.127(9) 0.090(7) 0.033(7) 0.061(7) 0.063(7) C23 0.042(5) 0.183(12) 0.046(5) -0.032(6) 0.023(4) 0.001(6) C24 0.27(2) 0.163(14) 0.214(18) -0.077(13) 0.211(18) -0.076(14) C25 0.244(17) 0.116(9) 0.147(12) -0.044(8) 0.161(13) -0.060(10) C26 0.071(7) 0.263(17) 0.108(9) -0.096(10) 0.059(7) -0.048(9) C30 0.032(4) 0.059(4) 0.045(4) -0.013(3) 0.008(3) -0.005(3) C31 0.040(4) 0.092(6) 0.055(5) 0.012(4) 0.008(4) 0.001(4) C32 0.044(5) 0.084(6) 0.064(6) 0.000(5) -0.001(4) 0.009(4) C33 0.038(5) 0.118(8) 0.067(6) -0.014(5) 0.017(4) 0.011(5) C34 0.053(5) 0.121(8) 0.057(5) -0.009(5) 0.020(4) 0.013(5) C35 0.039(4) 0.086(6) 0.051(5) -0.006(4) 0.007(4) 0.012(4) C40 0.039(4) 0.062(5) 0.044(4) 0.011(3) 0.012(3) 0.004(3) C41 0.040(4) 0.083(6) 0.057(5) -0.007(4) 0.002(4) 0.004(4) C42 0.063(6) 0.079(6) 0.073(6) -0.014(5) 0.011(5) 0.002(5) C43 0.033(4) 0.080(6) 0.102(8) -0.005(6) -0.002(5) -0.012(4) C44 0.043(5) 0.109(8) 0.088(7) -0.018(6) 0.021(5) 0.004(5) C45 0.036(4) 0.093(6) 0.071(6) -0.009(5) 0.019(4) -0.003(4) C46 0.041(5) 0.132(10) 0.145(11) -0.019(8) -0.012(6) -0.001(6) C50 0.045(5) 0.053(5) 0.121(8) 0.019(5) 0.035(6) -0.003(4) C51 0.039(10) 0.126(18) 0.065(12) 0.020(12) 0.014(9) -0.023(10) C81 0.060(10) 0.077(12) 0.049(10) 0.007(9) 0.013(8) -0.022(9) C52 0.039(11) 0.12(2) 0.081(15) 0.019(15) 0.012(10) -0.002(12) C82 0.047(11) 0.115(18) 0.109(17) 0.038(14) 0.023(11) -0.006(11) C53 0.062(7) 0.087(9) 0.230(18) 0.010(10) 0.074(10) -0.004(6) C54 0.046(12) 0.14(2) 0.113(18) 0.039(15) 0.005(11) -0.010(12) C84 0.086(18) 0.14(2) 0.22(4) -0.06(2) 0.10(2) -0.035(16) C55 0.057(12) 0.14(2) 0.095(16) 0.023(15) -0.001(11) -0.021(12) C85 0.099(17) 0.060(12) 0.19(3) -0.022(15) 0.090(19) -0.021(12) C56 0.079(8) 0.114(9) 0.274(19) -0.005(11) 0.097(11) -0.005(7) C60 0.034(4) 0.063(5) 0.046(4) -0.012(3) 0.005(3) 0.005(3) C61 0.065(6) 0.098(7) 0.092(7) -0.041(6) 0.040(5) -0.025(5) C62 0.068(6) 0.112(8) 0.085(7) -0.029(6) 0.027(6) -0.014(6) C63 0.062(6) 0.087(6) 0.055(6) -0.012(5) 0.005(5) 0.019(5) C64 0.088(7) 0.105(8) 0.070(6) -0.020(6) 0.037(6) 0.020(6) C65 0.059(5) 0.115(8) 0.067(6) -0.025(5) 0.030(5) -0.006(5) C66 0.107(9) 0.121(9) 0.067(7) -0.032(6) 0.011(6) 0.016(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 N5 1.730(6) . ? Mo1 N6 1.966(6) . ? Mo1 N3 2.163(6) . ? Mo1 N4 2.394(5) . ? Mo1 S1 2.475(2) . ? Mo1 S2 2.527(2) . ? Mo1 Mo2 2.6018(9) . ? Mo2 N7 1.732(6) . ? Mo2 N6 1.969(6) . ? Mo2 N3 2.159(6) . ? Mo2 N4 2.383(5) . ? Mo2 S3 2.473(3) . ? Mo2 S4 2.504(2) . ? S1 C1 1.719(9) . ? S2 C1 1.706(8) . ? S3 C6 1.508(15) . ? S4 C6 1.813(10) . ? N1 C1 1.334(9) . ? N1 C4 1.439(13) . ? N1 C2 1.481(12) . ? N2 C9 1.358(15) . ? N2 C6 1.512(15) . ? N2 C7 1.544(17) . ? N3 C20 1.450(9) . ? N3 C11 1.451(9) . ? N4 C11 1.355(9) . ? N4 C30 1.395(8) . ? N5 C40 1.382(8) . ? N6 C60 1.408(9) . ? N7 C50 1.401(9) . ? O1 C11 1.206(8) . ? C2 C3 1.437(16) . ? C4 C5 1.54(2) . ? C7 C8 1.62(2) . ? C9 C10 1.497(17) . ? C20 C21 1.302(12) . ? C20 C25 1.376(13) . ? C21 C22 1.374(12) . ? C22 C23 1.315(14) . ? C23 C24 1.383(19) . ? C23 C26 1.503(12) . ? C24 C25 1.360(16) . ? C30 C35 1.380(10) . ? C30 C31 1.405(10) . ? C31 C32 1.375(11) . ? C32 C33 1.349(13) . ? C33 C34 1.387(12) . ? C34 C35 1.387(10) . ? C40 C45 1.372(10) . ? C40 C41 1.396(11) . ? C41 C42 1.375(11) . ? C42 C43 1.368(13) . ? C43 C44 1.383(13) . ? C43 C46 1.516(12) . ? C44 C45 1.395(11) . ? C50 C51 1.225(19) . ? C50 C85 1.26(2) . ? C50 C81 1.500(19) . ? C50 C55 1.60(3) . ? C51 C52 1.41(3) . ? C52 C53 1.09(2) . ? C53 C56 1.531(14) . ? C53 C54 1.69(3) . ? C54 C55 1.45(3) . ? C81 C82 1.45(2) . ? C84 C85 1.47(3) . ? C60 C61 1.365(10) . ? C60 C65 1.374(11) . ? C61 C62 1.402(12) . ? C62 C63 1.346(13) . ? C63 C64 1.370(13) . ? C63 C66 1.506(12) . ? C64 C65 1.413(12) . ? 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 N5 Mo1 N6 100.9(3) . . ? N5 Mo1 N3 98.3(2) . . ? N6 Mo1 N3 101.5(2) . . ? N5 Mo1 N4 153.9(2) . . ? N6 Mo1 N4 79.0(2) . . ? N3 Mo1 N4 56.8(2) . . ? N5 Mo1 S1 103.12(18) . . ? N6 Mo1 S1 88.19(17) . . ? N3 Mo1 S1 154.37(16) . . ? N4 Mo1 S1 102.98(14) . . ? N5 Mo1 S2 100.2(2) . . ? N6 Mo1 S2 152.69(16) . . ? N3 Mo1 S2 92.30(16) . . ? N4 Mo1 S2 89.41(14) . . ? S1 Mo1 S2 70.27(7) . . ? N5 Mo1 Mo2 103.36(18) . . ? N6 Mo1 Mo2 48.66(17) . . ? N3 Mo1 Mo2 52.92(15) . . ? N4 Mo1 Mo2 56.80(13) . . ? S1 Mo1 Mo2 132.72(6) . . ? S2 Mo1 Mo2 140.11(6) . . ? N7 Mo2 N6 105.3(3) . . ? N7 Mo2 N3 99.6(3) . . ? N6 Mo2 N3 101.6(2) . . ? N7 Mo2 N4 156.4(3) . . ? N6 Mo2 N4 79.2(2) . . ? N3 Mo2 N4 57.0(2) . . ? N7 Mo2 S3 106.9(2) . . ? N6 Mo2 S3 81.6(2) . . ? N3 Mo2 S3 151.59(16) . . ? N4 Mo2 S3 96.70(15) . . ? N7 Mo2 S4 98.4(2) . . ? N6 Mo2 S4 148.67(19) . . ? N3 Mo2 S4 94.30(17) . . ? N4 Mo2 S4 87.30(15) . . ? S3 Mo2 S4 71.98(12) . . ? N7 Mo2 Mo1 108.0(2) . . ? N6 Mo2 Mo1 48.56(18) . . ? N3 Mo2 Mo1 53.05(15) . . ? N4 Mo2 Mo1 57.19(14) . . ? S3 Mo2 Mo1 124.72(9) . . ? S4 Mo2 Mo1 140.27(8) . . ? C1 S1 Mo1 88.4(2) . . ? C1 S2 Mo1 86.9(3) . . ? C6 S3 Mo2 85.8(4) . . ? C6 S4 Mo2 79.1(5) . . ? C1 N1 C4 122.5(9) . . ? C1 N1 C2 120.4(8) . . ? C4 N1 C2 117.1(8) . . ? C9 N2 C6 124.4(13) . . ? C9 N2 C7 116.7(12) . . ? C6 N2 C7 118.6(11) . . ? C20 N3 C11 117.0(6) . . ? C20 N3 Mo2 133.3(5) . . ? C11 N3 Mo2 95.3(4) . . ? C20 N3 Mo1 128.5(5) . . ? C11 N3 Mo1 97.5(4) . . ? Mo2 N3 Mo1 74.03(18) . . ? C11 N4 C30 121.7(6) . . ? C11 N4 Mo2 88.5(4) . . ? C30 N4 Mo2 130.9(4) . . ? C11 N4 Mo1 90.3(4) . . ? C30 N4 Mo1 140.3(4) . . ? Mo2 N4 Mo1 66.01(14) . . ? C40 N5 Mo1 162.9(5) . . ? C60 N6 Mo1 137.3(5) . . ? C60 N6 Mo2 136.9(5) . . ? Mo1 N6 Mo2 82.8(2) . . ? C50 N7 Mo2 173.7(7) . . ? N1 C1 S2 123.3(7) . . ? N1 C1 S1 122.3(6) . . ? S2 C1 S1 114.4(4) . . ? C3 C2 N1 110.5(10) . . ? N1 C4 C5 109.2(11) . . ? S3 C6 N2 124.2(8) . . ? S3 C6 S4 123.1(8) . . ? N2 C6 S4 112.5(10) . . ? N2 C7 C8 105.0(13) . . ? N2 C9 C10 112.4(13) . . ? O1 C11 N4 132.8(7) . . ? O1 C11 N3 125.5(7) . . ? N4 C11 N3 101.7(6) . . ? C21 C20 C25 116.8(8) . . ? C21 C20 N3 123.1(7) . . ? C25 C20 N3 120.0(9) . . ? C20 C21 C22 122.2(9) . . ? C23 C22 C21 123.2(11) . . ? C22 C23 C24 115.3(9) . . ? C22 C23 C26 122.1(13) . . ? C24 C23 C26 122.5(12) . . ? C25 C24 C23 121.4(13) . . ? C24 C25 C20 120.7(12) . . ? C35 C30 N4 119.1(6) . . ? C35 C30 C31 117.4(7) . . ? N4 C30 C31 123.5(7) . . ? C32 C31 C30 120.5(8) . . ? C33 C32 C31 121.5(8) . . ? C32 C33 C34 119.5(8) . . ? C33 C34 C35 119.6(8) . . ? C30 C35 C34 121.5(8) . . ? C45 C40 N5 121.8(7) . . ? C45 C40 C41 119.6(7) . . ? N5 C40 C41 118.5(7) . . ? C42 C41 C40 119.5(8) . . ? C43 C42 C41 122.0(9) . . ? C42 C43 C44 117.9(8) . . ? C42 C43 C46 122.2(10) . . ? C44 C43 C46 119.9(10) . . ? C43 C44 C45 121.5(8) . . ? C40 C45 C44 119.3(8) . . ? C51 C50 C85 69.1(17) . . ? C51 C50 N7 130.1(12) . . ? C85 C50 N7 123.5(12) . . ? C51 C50 C81 60.5(14) . . ? C85 C50 C81 119.4(15) . . ? N7 C50 C81 114.4(10) . . ? C51 C50 C55 114.4(13) . . ? C85 C50 C55 66.1(17) . . ? N7 C50 C55 114.3(10) . . ? C50 C51 C52 125.4(17) . . ? C53 C52 C51 128(2) . . ? C52 C53 C56 129(2) . . ? C84 C53 C82 114(2) . . ? C52 C53 C54 121.1(17) . . ? C56 C53 C54 108.7(16) . . ? C55 C54 C53 107.5(18) . . ? C53 C84 C85 120(2) . . ? C54 C55 C50 121.2(16) . . ? C50 C85 C84 123.5(19) . . ? C61 C60 C65 118.0(8) . . ? C61 C60 N6 119.8(7) . . ? C65 C60 N6 122.2(7) . . ? C60 C61 C62 121.0(9) . . ? C63 C62 C61 121.8(9) . . ? C62 C63 C64 117.6(9) . . ? C62 C63 C66 120.9(10) . . ? C64 C63 C66 121.5(10) . . ? C63 C64 C65 121.5(9) . . ? C60 C65 C64 119.9(9) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N5 Mo1 Mo2 N7 -1.9(3) . . . . ? N6 Mo1 Mo2 N7 -94.7(3) . . . . ? N3 Mo1 Mo2 N7 88.5(3) . . . . ? N4 Mo1 Mo2 N7 159.5(3) . . . . ? S1 Mo1 Mo2 N7 -124.3(2) . . . . ? S2 Mo1 Mo2 N7 122.8(2) . . . . ? N5 Mo1 Mo2 N6 92.9(3) . . . . ? N3 Mo1 Mo2 N6 -176.8(3) . . . . ? N4 Mo1 Mo2 N6 -105.8(3) . . . . ? S1 Mo1 Mo2 N6 -29.6(2) . . . . ? S2 Mo1 Mo2 N6 -142.5(2) . . . . ? N5 Mo1 Mo2 N3 -90.4(3) . . . . ? N6 Mo1 Mo2 N3 176.8(3) . . . . ? N4 Mo1 Mo2 N3 71.0(2) . . . . ? S1 Mo1 Mo2 N3 147.2(2) . . . . ? S2 Mo1 Mo2 N3 34.3(2) . . . . ? N5 Mo1 Mo2 N4 -161.4(2) . . . . ? N6 Mo1 Mo2 N4 105.8(3) . . . . ? N3 Mo1 Mo2 N4 -71.0(2) . . . . ? S1 Mo1 Mo2 N4 76.18(17) . . . . ? S2 Mo1 Mo2 N4 -36.67(18) . . . . ? N5 Mo1 Mo2 S3 124.8(2) . . . . ? N6 Mo1 Mo2 S3 31.9(2) . . . . ? N3 Mo1 Mo2 S3 -144.9(2) . . . . ? N4 Mo1 Mo2 S3 -73.87(18) . . . . ? S1 Mo1 Mo2 S3 2.31(11) . . . . ? S2 Mo1 Mo2 S3 -110.54(12) . . . . ? N5 Mo1 Mo2 S4 -131.0(2) . . . . ? N6 Mo1 Mo2 S4 136.1(3) . . . . ? N3 Mo1 Mo2 S4 -40.7(2) . . . . ? N4 Mo1 Mo2 S4 30.3(2) . . . . ? S1 Mo1 Mo2 S4 106.49(15) . . . . ? S2 Mo1 Mo2 S4 -6.37(16) . . . . ? N5 Mo1 S1 C1 95.3(3) . . . . ? N6 Mo1 S1 C1 -163.9(3) . . . . ? N3 Mo1 S1 C1 -50.5(4) . . . . ? N4 Mo1 S1 C1 -85.6(3) . . . . ? S2 Mo1 S1 C1 -1.0(2) . . . . ? Mo2 Mo1 S1 C1 -142.1(2) . . . . ? N5 Mo1 S2 C1 -99.4(3) . . . . ? N6 Mo1 S2 C1 40.9(5) . . . . ? N3 Mo1 S2 C1 161.8(3) . . . . ? N4 Mo1 S2 C1 105.0(3) . . . . ? S1 Mo1 S2 C1 1.0(3) . . . . ? Mo2 Mo1 S2 C1 135.0(2) . . . . ? N7 Mo2 S3 C6 -93.8(4) . . . . ? N6 Mo2 S3 C6 162.7(4) . . . . ? N3 Mo2 S3 C6 63.9(5) . . . . ? N4 Mo2 S3 C6 84.7(4) . . . . ? S4 Mo2 S3 C6 -0.3(4) . . . . ? Mo1 Mo2 S3 C6 139.1(4) . . . . ? N7 Mo2 S4 C6 105.3(4) . . . . ? N6 Mo2 S4 C6 -33.7(5) . . . . ? N3 Mo2 S4 C6 -154.3(3) . . . . ? N4 Mo2 S4 C6 -97.7(3) . . . . ? S3 Mo2 S4 C6 0.2(3) . . . . ? Mo1 Mo2 S4 C6 -122.9(3) . . . . ? N7 Mo2 N3 C20 22.8(7) . . . . ? N6 Mo2 N3 C20 130.8(6) . . . . ? N4 Mo2 N3 C20 -160.4(7) . . . . ? S3 Mo2 N3 C20 -135.5(5) . . . . ? S4 Mo2 N3 C20 -76.4(6) . . . . ? Mo1 Mo2 N3 C20 128.3(7) . . . . ? N7 Mo2 N3 C11 158.3(4) . . . . ? N6 Mo2 N3 C11 -93.8(4) . . . . ? N4 Mo2 N3 C11 -24.9(4) . . . . ? S3 Mo2 N3 C11 -0.1(6) . . . . ? S4 Mo2 N3 C11 59.0(4) . . . . ? Mo1 Mo2 N3 C11 -96.3(4) . . . . ? N7 Mo2 N3 Mo1 -105.4(2) . . . . ? N6 Mo2 N3 Mo1 2.5(2) . . . . ? N4 Mo2 N3 Mo1 71.3(2) . . . . ? S3 Mo2 N3 Mo1 96.2(3) . . . . ? S4 Mo2 N3 Mo1 155.30(13) . . . . ? N5 Mo1 N3 C20 -32.6(6) . . . . ? N6 Mo1 N3 C20 -135.6(6) . . . . ? N4 Mo1 N3 C20 155.9(6) . . . . ? S1 Mo1 N3 C20 113.9(6) . . . . ? S2 Mo1 N3 C20 68.1(6) . . . . ? Mo2 Mo1 N3 C20 -133.1(6) . . . . ? N5 Mo1 N3 C11 -166.1(4) . . . . ? N6 Mo1 N3 C11 90.9(4) . . . . ? N4 Mo1 N3 C11 22.4(4) . . . . ? S1 Mo1 N3 C11 -19.6(6) . . . . ? S2 Mo1 N3 C11 -65.4(4) . . . . ? Mo2 Mo1 N3 C11 93.4(4) . . . . ? N5 Mo1 N3 Mo2 100.5(2) . . . . ? N6 Mo1 N3 Mo2 -2.5(2) . . . . ? N4 Mo1 N3 Mo2 -71.0(2) . . . . ? S1 Mo1 N3 Mo2 -113.0(3) . . . . ? S2 Mo1 N3 Mo2 -158.78(12) . . . . ? N7 Mo2 N4 C11 34.7(8) . . . . ? N6 Mo2 N4 C11 138.3(4) . . . . ? N3 Mo2 N4 C11 26.7(4) . . . . ? S3 Mo2 N4 C11 -141.6(4) . . . . ? S4 Mo2 N4 C11 -70.2(4) . . . . ? Mo1 Mo2 N4 C11 91.0(4) . . . . ? N7 Mo2 N4 C30 167.0(7) . . . . ? N6 Mo2 N4 C30 -89.4(6) . . . . ? N3 Mo2 N4 C30 159.0(7) . . . . ? S3 Mo2 N4 C30 -9.4(6) . . . . ? S4 Mo2 N4 C30 62.1(6) . . . . ? Mo1 Mo2 N4 C30 -136.7(6) . . . . ? N7 Mo2 N4 Mo1 -56.3(7) . . . . ? N6 Mo2 N4 Mo1 47.26(19) . . . . ? N3 Mo2 N4 Mo1 -64.3(2) . . . . ? S3 Mo2 N4 Mo1 127.34(12) . . . . ? S4 Mo2 N4 Mo1 -161.16(13) . . . . ? N5 Mo1 N4 C11 -43.2(7) . . . . ? N6 Mo1 N4 C11 -135.6(4) . . . . ? N3 Mo1 N4 C11 -23.8(4) . . . . ? S1 Mo1 N4 C11 138.9(4) . . . . ? S2 Mo1 N4 C11 69.3(4) . . . . ? Mo2 Mo1 N4 C11 -88.2(4) . . . . ? N5 Mo1 N4 C30 170.8(7) . . . . ? N6 Mo1 N4 C30 78.4(7) . . . . ? N3 Mo1 N4 C30 -169.8(8) . . . . ? S1 Mo1 N4 C30 -7.1(7) . . . . ? S2 Mo1 N4 C30 -76.7(7) . . . . ? Mo2 Mo1 N4 C30 125.8(7) . . . . ? N5 Mo1 N4 Mo2 45.0(6) . . . . ? N6 Mo1 N4 Mo2 -47.40(18) . . . . ? N3 Mo1 N4 Mo2 64.3(2) . . . . ? S1 Mo1 N4 Mo2 -132.93(9) . . . . ? S2 Mo1 N4 Mo2 157.48(10) . . . . ? N6 Mo1 N5 C40 10.4(17) . . . . ? N3 Mo1 N5 C40 -93.1(16) . . . . ? N4 Mo1 N5 C40 -76.8(18) . . . . ? S1 Mo1 N5 C40 101.1(16) . . . . ? S2 Mo1 N5 C40 173.0(16) . . . . ? Mo2 Mo1 N5 C40 -39.4(17) . . . . ? N5 Mo1 N6 C60 63.1(7) . . . . ? N3 Mo1 N6 C60 164.0(7) . . . . ? N4 Mo1 N6 C60 -143.5(7) . . . . ? S1 Mo1 N6 C60 -39.9(7) . . . . ? S2 Mo1 N6 C60 -77.0(8) . . . . ? Mo2 Mo1 N6 C60 161.4(8) . . . . ? N5 Mo1 N6 Mo2 -98.3(2) . . . . ? N3 Mo1 N6 Mo2 2.6(2) . . . . ? N4 Mo1 N6 Mo2 55.11(18) . . . . ? S1 Mo1 N6 Mo2 158.71(15) . . . . ? S2 Mo1 N6 Mo2 121.6(3) . . . . ? N7 Mo2 N6 C60 -60.8(7) . . . . ? N3 Mo2 N6 C60 -164.2(6) . . . . ? N4 Mo2 N6 C60 143.0(7) . . . . ? S3 Mo2 N6 C60 44.5(6) . . . . ? S4 Mo2 N6 C60 76.9(7) . . . . ? Mo1 Mo2 N6 C60 -161.5(8) . . . . ? N7 Mo2 N6 Mo1 100.8(3) . . . . ? N3 Mo2 N6 Mo1 -2.6(2) . . . . ? N4 Mo2 N6 Mo1 -55.43(19) . . . . ? S3 Mo2 N6 Mo1 -153.95(17) . . . . ? S4 Mo2 N6 Mo1 -121.5(3) . . . . ? N6 Mo2 N7 C50 -135(5) . . . . ? N3 Mo2 N7 C50 -30(5) . . . . ? N4 Mo2 N7 C50 -37(6) . . . . ? S3 Mo2 N7 C50 139(5) . . . . ? S4 Mo2 N7 C50 66(5) . . . . ? Mo1 Mo2 N7 C50 -84(5) . . . . ? C4 N1 C1 S2 -179.5(10) . . . . ? C2 N1 C1 S2 -1.6(11) . . . . ? C4 N1 C1 S1 0.1(13) . . . . ? C2 N1 C1 S1 178.0(6) . . . . ? Mo1 S2 C1 N1 178.2(7) . . . . ? Mo1 S2 C1 S1 -1.5(4) . . . . ? Mo1 S1 C1 N1 -178.1(6) . . . . ? Mo1 S1 C1 S2 1.5(4) . . . . ? C1 N1 C2 C3 -96.7(13) . . . . ? C4 N1 C2 C3 81.3(15) . . . . ? C1 N1 C4 C5 -93.6(11) . . . . ? C2 N1 C4 C5 88.4(12) . . . . ? Mo2 S3 C6 N2 -175.5(8) . . . . ? Mo2 S3 C6 S4 0.4(6) . . . . ? C9 N2 C6 S3 178.2(9) . . . . ? C7 N2 C6 S3 5.1(15) . . . . ? C9 N2 C6 S4 1.9(13) . . . . ? C7 N2 C6 S4 -171.2(10) . . . . ? Mo2 S4 C6 S3 -0.4(6) . . . . ? Mo2 S4 C6 N2 175.9(7) . . . . ? C9 N2 C7 C8 100.8(14) . . . . ? C6 N2 C7 C8 -85.6(14) . . . . ? C6 N2 C9 C10 -99.0(17) . . . . ? C7 N2 C9 C10 74.2(18) . . . . ? C30 N4 C11 O1 5.2(13) . . . . ? Mo2 N4 C11 O1 144.1(9) . . . . ? Mo1 N4 C11 O1 -149.9(9) . . . . ? C30 N4 C11 N3 -173.9(6) . . . . ? Mo2 N4 C11 N3 -35.0(5) . . . . ? Mo1 N4 C11 N3 31.0(5) . . . . ? C20 N3 C11 O1 5.3(11) . . . . ? Mo2 N3 C11 O1 -139.7(8) . . . . ? Mo1 N3 C11 O1 145.8(7) . . . . ? C20 N3 C11 N4 -175.5(6) . . . . ? Mo2 N3 C11 N4 39.5(5) . . . . ? Mo1 N3 C11 N4 -35.1(5) . . . . ? C11 N3 C20 C21 84.3(10) . . . . ? Mo2 N3 C20 C21 -147.3(8) . . . . ? Mo1 N3 C20 C21 -41.9(11) . . . . ? C11 N3 C20 C25 -94.3(11) . . . . ? Mo2 N3 C20 C25 34.0(12) . . . . ? Mo1 N3 C20 C25 139.5(9) . . . . ? C25 C20 C21 C22 1.8(17) . . . . ? N3 C20 C21 C22 -176.9(9) . . . . ? C20 C21 C22 C23 1.1(18) . . . . ? C21 C22 C23 C24 0.2(18) . . . . ? C21 C22 C23 C26 176.2(10) . . . . ? C22 C23 C24 C25 -5(2) . . . . ? C26 C23 C24 C25 179.5(14) . . . . ? C23 C24 C25 C20 8(3) . . . . ? C21 C20 C25 C24 -6(2) . . . . ? N3 C20 C25 C24 172.7(14) . . . . ? C11 N4 C30 C35 -138.0(7) . . . . ? Mo2 N4 C30 C35 102.4(8) . . . . ? Mo1 N4 C30 C35 0.9(11) . . . . ? C11 N4 C30 C31 45.0(10) . . . . ? Mo2 N4 C30 C31 -74.6(9) . . . . ? Mo1 N4 C30 C31 -176.2(6) . . . . ? C35 C30 C31 C32 -0.3(12) . . . . ? N4 C30 C31 C32 176.8(7) . . . . ? C30 C31 C32 C33 0.5(14) . . . . ? C31 C32 C33 C34 -0.3(14) . . . . ? C32 C33 C34 C35 -0.2(14) . . . . ? N4 C30 C35 C34 -177.4(7) . . . . ? C31 C30 C35 C34 -0.2(12) . . . . ? C33 C34 C35 C30 0.4(14) . . . . ? Mo1 N5 C40 C45 133.8(15) . . . . ? Mo1 N5 C40 C41 -47.3(19) . . . . ? C45 C40 C41 C42 -2.2(12) . . . . ? N5 C40 C41 C42 178.8(7) . . . . ? C40 C41 C42 C43 2.6(14) . . . . ? C41 C42 C43 C44 -1.4(15) . . . . ? C41 C42 C43 C46 -179.7(10) . . . . ? C42 C43 C44 C45 -0.1(15) . . . . ? C46 C43 C44 C45 178.2(10) . . . . ? N5 C40 C45 C44 179.7(8) . . . . ? C41 C40 C45 C44 0.8(13) . . . . ? C43 C44 C45 C40 0.4(15) . . . . ? Mo2 N7 C50 C51 124(5) . . . . ? Mo2 N7 C50 C85 34(6) . . . . ? Mo2 N7 C50 C81 -165(5) . . . . ? Mo2 N7 C50 C55 -43(6) . . . . ? N7 C50 C51 C81 98.2(16) . . . . ? C55 C50 C51 C81 -95.3(16) . . . . ? N7 C50 C51 C52 179(2) . . . . ? C55 C50 C51 C52 -14(3) . . . . ? C50 C51 C52 C53 3(5) . . . . ? C51 C52 C53 C56 -180(2) . . . . ? C51 C52 C53 C54 13(5) . . . . ? C52 C53 C54 C55 -14(3) . . . . ? C56 C53 C54 C55 176.8(17) . . . . ? C53 C54 C55 C85 42(2) . . . . ? C53 C54 C55 C50 2(3) . . . . ? C51 C50 C55 C54 10(3) . . . . ? N7 C50 C55 C54 179.0(19) . . . . ? Mo1 N6 C60 C61 -110.2(9) . . . . ? Mo2 N6 C60 C61 42.2(11) . . . . ? Mo1 N6 C60 C65 71.3(10) . . . . ? Mo2 N6 C60 C65 -136.3(7) . . . . ? C65 C60 C61 C62 -2.7(14) . . . . ? N6 C60 C61 C62 178.8(9) . . . . ? C60 C61 C62 C63 0.4(16) . . . . ? C61 C62 C63 C64 0.7(16) . . . . ? C61 C62 C63 C66 -178.0(10) . . . . ? C62 C63 C64 C65 0.6(15) . . . . ? C66 C63 C64 C65 179.3(9) . . . . ? C61 C60 C65 C64 3.9(14) . . . . ? N6 C60 C65 C64 -177.6(8) . . . . ? C63 C64 C65 C60 -2.9(15) . . . . ? _diffrn_measured_fraction_theta_max 0.940 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.512 _refine_diff_density_min -1.086 _refine_diff_density_rms 0.119 data_str0033 _database_code_depnum_ccdc_archive 'CCDC 253356' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C43 H55 Mo2 N6 O S5' _chemical_formula_weight 1024.11 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P1bar loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.9948(9) _cell_length_b 13.0247(9) _cell_length_c 16.4809(11) _cell_angle_alpha 88.1540(10) _cell_angle_beta 69.8280(10) _cell_angle_gamma 65.0950(10) _cell_volume 2353.8(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.445 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1054 _exptl_absorpt_coefficient_mu 0.794 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9108 _exptl_absorpt_correction_T_max 0.9320 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20955 _diffrn_reflns_av_R_equivalents 0.0219 _diffrn_reflns_av_sigmaI/netI 0.0395 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 28.26 _reflns_number_total 10851 _reflns_number_gt 7712 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0609P)^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 10851 _refine_ls_number_parameters 521 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0728 _refine_ls_R_factor_gt 0.0486 _refine_ls_wR_factor_ref 0.1226 _refine_ls_wR_factor_gt 0.1102 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _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 Mo1 Mo 1.03274(3) 0.26265(2) 0.28069(2) 0.05739(10) Uani 1 1 d . . . Mo2 Mo 0.86188(3) 0.26610(2) 0.22348(2) 0.05890(10) Uani 1 1 d . . . S1 S 1.15926(9) 0.12805(7) 0.35742(7) 0.0677(2) Uani 1 1 d . . . S2 S 1.00746(9) 0.36765(7) 0.41248(6) 0.0705(3) Uani 1 1 d . . . S3 S 0.75578(8) 0.14271(8) 0.22599(7) 0.0741(3) Uani 1 1 d . . . S4 S 0.64040(9) 0.38572(8) 0.26845(7) 0.0764(3) Uani 1 1 d . . . S5 S 0.86065(9) 0.42786(7) 0.28299(7) 0.0701(3) Uani 1 1 d . . . N1 N 1.1096(3) 0.2278(2) 0.5144(2) 0.0691(8) Uani 1 1 d . . . N2 N 0.5132(3) 0.2625(3) 0.2810(2) 0.0804(9) Uani 1 1 d . . . N3 N 0.8803(2) 0.2038(2) 0.35430(18) 0.0559(6) Uani 1 1 d . . . N4 N 1.0217(2) 0.1189(2) 0.22863(18) 0.0550(6) Uani 1 1 d . . . N5 N 1.1427(3) 0.2814(2) 0.19402(19) 0.0629(7) Uani 1 1 d . . . N6 N 0.9235(3) 0.2677(2) 0.11282(19) 0.0650(7) Uani 1 1 d . . . O1 O 0.9754(2) 0.00247(19) 0.33427(17) 0.0730(7) Uani 1 1 d . . . C1 C 1.0962(3) 0.2395(3) 0.4389(2) 0.0626(9) Uani 1 1 d . . . C2 C 1.1752(4) 0.1132(3) 0.5361(3) 0.0774(11) Uani 1 1 d . . . H2A H 1.1383 0.1123 0.5981 0.093 Uiso 1 1 calc R . . H2B H 1.1654 0.0577 0.5054 0.093 Uiso 1 1 calc R . . C3 C 1.3065(4) 0.0785(4) 0.5134(3) 0.0955(13) Uani 1 1 d . . . H3A H 1.3175 0.1328 0.5445 0.115 Uiso 1 1 calc R . . H3B H 1.3445 0.0784 0.4514 0.115 Uiso 1 1 calc R . . C4 C 1.3669(5) -0.0402(4) 0.5375(4) 0.129(2) Uani 1 1 d . . . H4A H 1.3279 -0.0403 0.5987 0.193 Uiso 1 1 calc R . . H4B H 1.4516 -0.0608 0.5244 0.193 Uiso 1 1 calc R . . H4C H 1.3592 -0.0944 0.5046 0.193 Uiso 1 1 calc R . . C5 C 1.0570(4) 0.3269(4) 0.5802(3) 0.0905(13) Uani 1 1 d . . . H5A H 1.0588 0.3923 0.5510 0.109 Uiso 1 1 calc R . . H5B H 1.1071 0.3116 0.6153 0.109 Uiso 1 1 calc R . . C6 C 0.9233(6) 0.3576(5) 0.6416(4) 0.136(2) Uani 1 1 d . . . H6A H 0.8835 0.4388 0.6618 0.164 Uiso 1 1 calc R . . H6B H 0.8823 0.3446 0.6066 0.164 Uiso 1 1 calc R . . C7 C 0.9028(7) 0.3016(6) 0.7144(4) 0.155(2) Uani 1 1 d . . . H7A H 0.9683 0.2466 0.7260 0.185 Uiso 1 1 calc R . . H7B H 0.8234 0.3191 0.7515 0.185 Uiso 1 1 calc R . . C8 C 0.6209(3) 0.2642(3) 0.2608(2) 0.0694(10) Uani 1 1 d . . . C9 C 0.3979(4) 0.3690(4) 0.3145(3) 0.1020(15) Uani 1 1 d . . . H9A H 0.3486 0.3739 0.2804 0.122 Uiso 1 1 calc R . . H9B H 0.4167 0.4341 0.3067 0.122 Uiso 1 1 calc R . . C10 C 0.3241(5) 0.3753(5) 0.4108(4) 0.131(2) Uani 1 1 d . . . H10A H 0.2524 0.4483 0.4282 0.157 Uiso 1 1 calc R . . H10B H 0.2960 0.3164 0.4161 0.157 Uiso 1 1 calc R . . C11 C 0.3822(6) 0.3636(5) 0.4701(4) 0.135(2) Uani 1 1 d . . . H11A H 0.4422 0.2860 0.4625 0.202 Uiso 1 1 calc R . . H11B H 0.3231 0.3831 0.5285 0.202 Uiso 1 1 calc R . . H11C H 0.4213 0.4135 0.4602 0.202 Uiso 1 1 calc R . . C12 C 0.5032(4) 0.1568(4) 0.2705(3) 0.0907(13) Uani 1 1 d . . . H12A H 0.4279 0.1625 0.3145 0.109 Uiso 1 1 calc R . . H12B H 0.5702 0.0943 0.2805 0.109 Uiso 1 1 calc R . . C13 C 0.5047(5) 0.1296(5) 0.1817(4) 0.1237(19) Uani 1 1 d . . . H13A H 0.4371 0.1916 0.1720 0.148 Uiso 1 1 calc R . . H13B H 0.5795 0.1250 0.1377 0.148 Uiso 1 1 calc R . . C14 C 0.4961(5) 0.0207(6) 0.1709(4) 0.149(2) Uani 1 1 d . . . H14A H 0.5664 -0.0420 0.1754 0.224 Uiso 1 1 calc R . . H14B H 0.4926 0.0104 0.1146 0.224 Uiso 1 1 calc R . . H14C H 0.4238 0.0235 0.2155 0.224 Uiso 1 1 calc R . . C15 C 0.9586(3) 0.0953(3) 0.3119(2) 0.0587(8) Uani 1 1 d . . . C20 C 0.8080(3) 0.2215(3) 0.4447(2) 0.0630(9) Uani 1 1 d . . . C21 C 0.8526(4) 0.1549(3) 0.5031(3) 0.0730(10) Uani 1 1 d . . . H21 H 0.9316 0.0967 0.4834 0.088 Uiso 1 1 calc R . . C22 C 0.7805(5) 0.1743(4) 0.5901(3) 0.0940(14) Uani 1 1 d . . . H22 H 0.8115 0.1287 0.6285 0.113 Uiso 1 1 calc R . . C23 C 0.6644(5) 0.2595(4) 0.6210(3) 0.0997(15) Uani 1 1 d . . . C24 C 0.6221(4) 0.3275(4) 0.5640(3) 0.0999(15) Uani 1 1 d . . . H24 H 0.5440 0.3872 0.5845 0.120 Uiso 1 1 calc R . . C25 C 0.6930(4) 0.3095(3) 0.4761(3) 0.0796(11) Uani 1 1 d . . . H25 H 0.6625 0.3571 0.4385 0.096 Uiso 1 1 calc R . . C26 C 0.5902(8) 0.2717(7) 0.7122(5) 0.203(4) Uani 1 1 d . . . H26A H 0.5983 0.3254 0.7453 0.304 Uiso 1 1 calc R . . H26B H 0.6169 0.1990 0.7333 0.304 Uiso 1 1 calc R . . H26C H 0.5064 0.2989 0.7186 0.304 Uiso 1 1 calc R . . C30 C 1.1102(3) 0.0220(3) 0.1655(2) 0.0594(8) Uani 1 1 d . . . C31 C 1.2303(3) 0.0015(3) 0.1304(3) 0.0763(11) Uani 1 1 d . . . H31 H 1.2547 0.0527 0.1465 0.092 Uiso 1 1 calc R . . C32 C 1.3157(4) -0.0951(4) 0.0711(3) 0.0964(14) Uani 1 1 d . . . H32 H 1.3972 -0.1088 0.0488 0.116 Uiso 1 1 calc R . . C33 C 1.2815(4) -0.1702(4) 0.0453(3) 0.0864(12) Uani 1 1 d . . . C34 C 1.1616(4) -0.1487(3) 0.0799(3) 0.0855(12) Uani 1 1 d . . . H34 H 1.1373 -0.1993 0.0626 0.103 Uiso 1 1 calc R . . C35 C 1.0760(3) -0.0547(3) 0.1395(3) 0.0764(11) Uani 1 1 d . . . H35 H 0.9950 -0.0426 0.1624 0.092 Uiso 1 1 calc R . . C36 C 1.3653(7) -0.2747(7) -0.0150(5) 0.193(3) Uani 1 1 d . . . H36A H 1.4469 -0.2948 -0.0185 0.290 Uiso 1 1 calc R . . H36B H 1.3607 -0.2630 -0.0717 0.290 Uiso 1 1 calc R . . H36C H 1.3435 -0.3353 0.0055 0.290 Uiso 1 1 calc R . . C40 C 1.2108(3) 0.3158(3) 0.1248(2) 0.0649(9) Uani 1 1 d . . . C41 C 1.2191(4) 0.4150(4) 0.1401(3) 0.0954(14) Uani 1 1 d . . . H41 H 1.1798 0.4552 0.1960 0.114 Uiso 1 1 calc R . . C42 C 1.2840(6) 0.4549(5) 0.0745(4) 0.146(2) Uani 1 1 d . . . H42 H 1.2910 0.5206 0.0859 0.175 Uiso 1 1 calc R . . C43 C 1.3397(6) 0.3968(7) -0.0099(4) 0.133(2) Uani 1 1 d . . . C44 C 1.3313(5) 0.3002(6) -0.0249(3) 0.1188(19) Uani 1 1 d . . . H44 H 1.3686 0.2611 -0.0811 0.143 Uiso 1 1 calc R . . C45 C 1.2682(4) 0.2589(5) 0.0419(3) 0.0981(14) Uani 1 1 d . . . H45 H 1.2644 0.1913 0.0306 0.118 Uiso 1 1 calc R . . C46 C 1.4124(9) 0.4441(8) -0.0861(5) 0.252(5) Uani 1 1 d . . . H46A H 1.3881 0.5231 -0.0690 0.378 Uiso 1 1 calc R . . H46B H 1.3952 0.4368 -0.1372 0.378 Uiso 1 1 calc R . . H46C H 1.4981 0.4013 -0.0985 0.378 Uiso 1 1 calc R . . C50 C 0.9954(3) 0.2616(3) 0.0266(2) 0.0613(8) Uani 1 1 d . . . C51 C 0.9860(4) 0.3600(3) -0.0099(3) 0.0750(10) Uani 1 1 d . . . H51 H 0.9301 0.4306 0.0230 0.090 Uiso 1 1 calc R . . C52 C 1.0590(4) 0.3551(4) -0.0950(3) 0.0860(12) Uani 1 1 d . . . H52 H 1.0511 0.4226 -0.1187 0.103 Uiso 1 1 calc R . . C53 C 1.1434(4) 0.2518(4) -0.1459(3) 0.0803(11) Uani 1 1 d . . . C54 C 1.1499(4) 0.1539(4) -0.1091(3) 0.0769(11) Uani 1 1 d . . . H54 H 1.2051 0.0835 -0.1426 0.092 Uiso 1 1 calc R . . C55 C 1.0785(4) 0.1559(3) -0.0251(3) 0.0711(10) Uani 1 1 d . . . H55 H 1.0848 0.0881 -0.0025 0.085 Uiso 1 1 calc R . . C56 C 1.2270(5) 0.2454(5) -0.2372(3) 0.1159(17) Uani 1 1 d . . . H56A H 1.2934 0.2588 -0.2354 0.174 Uiso 1 1 calc R . . H56B H 1.1826 0.3023 -0.2664 0.174 Uiso 1 1 calc R . . H56C H 1.2583 0.1710 -0.2682 0.174 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 0.06049(19) 0.04584(16) 0.0654(2) 0.00552(13) -0.01963(14) -0.02538(14) Mo2 0.05459(18) 0.04792(17) 0.0673(2) 0.00755(13) -0.02075(15) -0.01738(13) S1 0.0692(6) 0.0506(5) 0.0813(6) 0.0022(4) -0.0307(5) -0.0214(4) S2 0.0894(7) 0.0478(5) 0.0756(6) 0.0046(4) -0.0314(5) -0.0300(5) S3 0.0557(5) 0.0602(5) 0.1030(8) 0.0022(5) -0.0312(5) -0.0199(4) S4 0.0602(5) 0.0569(5) 0.0910(7) 0.0140(5) -0.0221(5) -0.0113(4) S5 0.0784(6) 0.0433(5) 0.0795(6) 0.0105(4) -0.0245(5) -0.0220(4) N1 0.087(2) 0.0621(18) 0.071(2) 0.0170(15) -0.0307(17) -0.0426(17) N2 0.0566(18) 0.093(2) 0.085(2) 0.0164(18) -0.0279(17) -0.0249(18) N3 0.0571(16) 0.0425(14) 0.0641(17) 0.0073(12) -0.0185(14) -0.0210(12) N4 0.0509(15) 0.0453(14) 0.0668(18) 0.0048(12) -0.0214(13) -0.0192(12) N5 0.0646(17) 0.0592(17) 0.0686(19) 0.0066(14) -0.0235(15) -0.0310(14) N6 0.0612(17) 0.0608(17) 0.072(2) 0.0050(14) -0.0268(15) -0.0232(14) O1 0.0787(16) 0.0441(13) 0.0894(18) 0.0129(12) -0.0230(14) -0.0270(12) C1 0.067(2) 0.059(2) 0.068(2) 0.0064(17) -0.0206(18) -0.0358(18) C2 0.092(3) 0.076(3) 0.081(3) 0.028(2) -0.039(2) -0.047(2) C3 0.100(3) 0.090(3) 0.121(4) 0.042(3) -0.056(3) -0.054(3) C4 0.113(4) 0.099(4) 0.209(6) 0.073(4) -0.089(4) -0.057(3) C5 0.120(4) 0.082(3) 0.075(3) 0.007(2) -0.032(3) -0.051(3) C6 0.180(6) 0.108(4) 0.099(4) 0.003(3) -0.041(4) -0.050(4) C7 0.155(6) 0.141(6) 0.133(5) 0.032(5) -0.028(5) -0.054(5) C8 0.058(2) 0.071(2) 0.070(2) 0.0136(18) -0.0238(18) -0.0198(18) C9 0.055(2) 0.105(4) 0.114(4) 0.022(3) -0.028(3) -0.008(2) C10 0.075(3) 0.133(5) 0.132(5) 0.010(4) -0.020(4) -0.010(3) C11 0.131(5) 0.112(4) 0.118(5) 0.010(4) -0.023(4) -0.033(4) C12 0.070(3) 0.104(3) 0.103(3) 0.013(3) -0.031(2) -0.042(2) C13 0.114(4) 0.149(5) 0.120(4) 0.000(4) -0.061(4) -0.051(4) C14 0.103(4) 0.183(6) 0.177(6) -0.031(5) -0.051(4) -0.072(4) C15 0.0582(19) 0.0489(19) 0.075(2) 0.0057(16) -0.0291(18) -0.0248(16) C20 0.069(2) 0.0441(18) 0.072(2) 0.0069(16) -0.0175(19) -0.0267(17) C21 0.088(3) 0.051(2) 0.079(3) 0.0138(18) -0.028(2) -0.031(2) C22 0.132(4) 0.074(3) 0.079(3) 0.022(2) -0.033(3) -0.054(3) C23 0.116(4) 0.085(3) 0.069(3) 0.010(2) -0.005(3) -0.040(3) C24 0.089(3) 0.081(3) 0.083(3) 0.000(2) 0.001(3) -0.019(2) C25 0.082(3) 0.062(2) 0.078(3) 0.0065(19) -0.017(2) -0.024(2) C26 0.220(8) 0.183(8) 0.117(5) 0.002(5) 0.007(6) -0.061(7) C30 0.058(2) 0.0469(18) 0.069(2) 0.0028(15) -0.0275(17) -0.0145(15) C31 0.059(2) 0.072(2) 0.090(3) -0.016(2) -0.020(2) -0.0255(19) C32 0.063(2) 0.093(3) 0.109(4) -0.032(3) -0.012(2) -0.024(2) C33 0.083(3) 0.066(2) 0.083(3) -0.020(2) -0.026(2) -0.010(2) C34 0.086(3) 0.063(2) 0.105(3) -0.014(2) -0.044(3) -0.022(2) C35 0.063(2) 0.062(2) 0.100(3) -0.007(2) -0.034(2) -0.0197(19) C36 0.179(7) 0.184(8) 0.189(8) 0.007(6) -0.042(6) -0.073(6) C40 0.058(2) 0.074(2) 0.063(2) 0.0154(19) -0.0247(18) -0.0282(18) C41 0.118(4) 0.082(3) 0.079(3) 0.017(2) -0.017(3) -0.052(3) C42 0.184(6) 0.114(5) 0.130(5) 0.035(4) -0.013(5) -0.093(5) C43 0.162(6) 0.165(6) 0.084(4) 0.055(4) -0.030(4) -0.095(5) C44 0.114(4) 0.180(6) 0.059(3) 0.010(3) -0.017(3) -0.073(4) C45 0.100(3) 0.127(4) 0.075(3) 0.000(3) -0.026(3) -0.060(3) C46 0.321(12) 0.310(12) 0.146(7) 0.111(7) -0.022(7) -0.212(11) C50 0.063(2) 0.067(2) 0.059(2) 0.0038(17) -0.0295(18) -0.0270(18) C51 0.085(3) 0.059(2) 0.075(3) 0.0016(19) -0.029(2) -0.024(2) C52 0.105(3) 0.077(3) 0.074(3) 0.018(2) -0.035(3) -0.037(3) C53 0.089(3) 0.090(3) 0.065(3) 0.011(2) -0.034(2) -0.037(2) C54 0.075(3) 0.077(3) 0.072(3) -0.009(2) -0.027(2) -0.026(2) C55 0.078(2) 0.062(2) 0.079(3) 0.0060(19) -0.034(2) -0.031(2) C56 0.123(4) 0.130(4) 0.068(3) 0.015(3) -0.025(3) -0.040(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 N5 1.733(3) . ? Mo1 N4 2.162(3) . ? Mo1 S5 2.3509(10) . ? Mo1 N3 2.354(3) . ? Mo1 S2 2.4529(10) . ? Mo1 S1 2.4978(10) . ? Mo1 Mo2 2.6793(5) . ? Mo2 N6 1.724(3) . ? Mo2 N4 2.180(2) . ? Mo2 N3 2.333(3) . ? Mo2 S5 2.3442(10) . ? Mo2 S4 2.4672(10) . ? Mo2 S3 2.5115(10) . ? S1 C1 1.716(4) . ? S2 C1 1.727(4) . ? S3 C8 1.712(4) . ? S4 C8 1.720(4) . ? N1 C1 1.311(4) . ? N1 C5 1.465(5) . ? N1 C2 1.478(5) . ? N2 C8 1.332(5) . ? N2 C12 1.456(5) . ? N2 C9 1.484(5) . ? N3 C15 1.373(4) . ? N3 C20 1.425(4) . ? N4 C30 1.427(4) . ? N4 C15 1.436(4) . ? N5 C40 1.375(4) . ? N6 C50 1.389(4) . ? O1 C15 1.204(4) . ? C2 C3 1.475(5) . ? C3 C4 1.522(6) . ? C5 C6 1.559(8) . ? C6 C7 1.388(8) . ? C9 C10 1.529(7) . ? C10 C11 1.398(7) . ? C12 C13 1.509(6) . ? C13 C14 1.491(8) . ? C20 C25 1.369(5) . ? C20 C21 1.387(5) . ? C21 C22 1.377(6) . ? C22 C23 1.365(6) . ? C23 C24 1.364(7) . ? C23 C26 1.450(8) . ? C24 C25 1.386(6) . ? C30 C31 1.371(5) . ? C30 C35 1.383(5) . ? C31 C32 1.387(5) . ? C32 C33 1.364(6) . ? C33 C34 1.364(6) . ? C33 C36 1.455(8) . ? C34 C35 1.369(5) . ? C40 C45 1.368(5) . ? C40 C41 1.379(5) . ? C41 C42 1.363(7) . ? C42 C43 1.393(8) . ? C43 C44 1.346(8) . ? C43 C46 1.571(8) . ? C44 C45 1.373(7) . ? C50 C51 1.375(5) . ? C50 C55 1.405(5) . ? C51 C52 1.382(5) . ? C52 C53 1.382(5) . ? C53 C54 1.378(6) . ? C53 C56 1.502(6) . ? C54 C55 1.369(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N5 Mo1 N4 103.08(12) . . ? N5 Mo1 S5 99.00(10) . . ? N4 Mo1 S5 107.28(7) . . ? N5 Mo1 N3 158.44(12) . . ? N4 Mo1 N3 57.19(10) . . ? S5 Mo1 N3 80.90(7) . . ? N5 Mo1 S2 107.30(9) . . ? N4 Mo1 S2 145.66(8) . . ? S5 Mo1 S2 83.56(4) . . ? N3 Mo1 S2 94.15(7) . . ? N5 Mo1 S1 101.56(10) . . ? N4 Mo1 S1 87.94(7) . . ? S5 Mo1 S1 150.86(4) . . ? N3 Mo1 S1 87.30(7) . . ? S2 Mo1 S1 70.75(3) . . ? N5 Mo1 Mo2 107.47(9) . . ? N4 Mo1 Mo2 52.21(7) . . ? S5 Mo1 Mo2 55.09(3) . . ? N3 Mo1 Mo2 54.77(7) . . ? S2 Mo1 Mo2 129.01(3) . . ? S1 Mo1 Mo2 134.60(2) . . ? N6 Mo2 N4 95.05(12) . . ? N6 Mo2 N3 151.51(11) . . ? N4 Mo2 N3 57.30(10) . . ? N6 Mo2 S5 102.72(10) . . ? N4 Mo2 S5 106.89(7) . . ? N3 Mo2 S5 81.48(7) . . ? N6 Mo2 S4 106.37(9) . . ? N4 Mo2 S4 153.43(8) . . ? N3 Mo2 S4 102.08(7) . . ? S5 Mo2 S4 83.91(4) . . ? N6 Mo2 S3 100.57(10) . . ? N4 Mo2 S3 90.95(7) . . ? N3 Mo2 S3 87.68(7) . . ? S5 Mo2 S3 149.07(4) . . ? S4 Mo2 S3 70.11(3) . . ? N6 Mo2 Mo1 103.42(9) . . ? N4 Mo2 Mo1 51.59(7) . . ? N3 Mo2 Mo1 55.51(6) . . ? S5 Mo2 Mo1 55.32(3) . . ? S4 Mo2 Mo1 133.77(3) . . ? S3 Mo2 Mo1 136.63(3) . . ? C1 S1 Mo1 87.35(13) . . ? C1 S2 Mo1 88.58(12) . . ? C8 S3 Mo2 87.86(14) . . ? C8 S4 Mo2 89.14(13) . . ? Mo2 S5 Mo1 69.59(3) . . ? C1 N1 C5 121.0(3) . . ? C1 N1 C2 120.5(3) . . ? C5 N1 C2 118.5(3) . . ? C8 N2 C12 121.8(3) . . ? C8 N2 C9 121.2(4) . . ? C12 N2 C9 117.1(4) . . ? C15 N3 C20 120.3(3) . . ? C15 N3 Mo2 90.3(2) . . ? C20 N3 Mo2 140.0(2) . . ? C15 N3 Mo1 88.87(19) . . ? C20 N3 Mo1 130.2(2) . . ? Mo2 N3 Mo1 69.72(7) . . ? C30 N4 C15 116.1(3) . . ? C30 N4 Mo1 132.2(2) . . ? C15 N4 Mo1 95.21(18) . . ? C30 N4 Mo2 130.9(2) . . ? C15 N4 Mo2 94.95(18) . . ? Mo1 N4 Mo2 76.19(8) . . ? C40 N5 Mo1 168.6(3) . . ? C50 N6 Mo2 168.2(2) . . ? N1 C1 S1 123.6(3) . . ? N1 C1 S2 123.6(3) . . ? S1 C1 S2 112.7(2) . . ? C3 C2 N1 113.6(3) . . ? C2 C3 C4 110.2(4) . . ? N1 C5 C6 113.5(4) . . ? C7 C6 C5 119.2(6) . . ? N2 C8 S3 122.7(3) . . ? N2 C8 S4 124.5(3) . . ? S3 C8 S4 112.9(2) . . ? N2 C9 C10 112.9(4) . . ? C11 C10 C9 117.6(5) . . ? N2 C12 C13 113.5(4) . . ? C14 C13 C12 113.4(5) . . ? O1 C15 N3 132.4(3) . . ? O1 C15 N4 126.6(3) . . ? N3 C15 N4 101.0(3) . . ? C25 C20 C21 118.5(4) . . ? C25 C20 N3 119.6(3) . . ? C21 C20 N3 121.8(3) . . ? C22 C21 C20 120.4(4) . . ? C23 C22 C21 121.1(4) . . ? C24 C23 C22 118.4(4) . . ? C24 C23 C26 122.9(6) . . ? C22 C23 C26 118.7(6) . . ? C23 C24 C25 121.5(4) . . ? C20 C25 C24 120.0(4) . . ? C31 C30 C35 118.6(3) . . ? C31 C30 N4 121.3(3) . . ? C35 C30 N4 120.1(3) . . ? C30 C31 C32 120.5(4) . . ? C33 C32 C31 120.7(4) . . ? C34 C33 C32 118.4(4) . . ? C34 C33 C36 117.3(5) . . ? C32 C33 C36 124.3(5) . . ? C33 C34 C35 121.9(4) . . ? C34 C35 C30 119.9(4) . . ? C45 C40 N5 123.9(4) . . ? C45 C40 C41 118.5(4) . . ? N5 C40 C41 117.7(4) . . ? C42 C41 C40 120.9(5) . . ? C41 C42 C43 119.7(6) . . ? C44 C43 C42 119.4(5) . . ? C44 C43 C46 120.8(7) . . ? C42 C43 C46 119.8(7) . . ? C43 C44 C45 120.6(5) . . ? C40 C45 C44 120.8(5) . . ? C51 C50 N6 120.0(3) . . ? C51 C50 C55 118.7(4) . . ? N6 C50 C55 121.3(3) . . ? C50 C51 C52 120.6(4) . . ? C51 C52 C53 121.4(4) . . ? C54 C53 C52 117.4(4) . . ? C54 C53 C56 120.7(4) . . ? C52 C53 C56 121.9(4) . . ? C55 C54 C53 122.6(4) . . ? C54 C55 C50 119.3(4) . . ? 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 N5 Mo1 Mo2 N6 7.45(13) . . . . ? N4 Mo1 Mo2 N6 -85.77(13) . . . . ? S5 Mo1 Mo2 N6 96.32(10) . . . . ? N3 Mo1 Mo2 N6 -158.80(12) . . . . ? S2 Mo1 Mo2 N6 138.46(10) . . . . ? S1 Mo1 Mo2 N6 -119.82(10) . . . . ? N5 Mo1 Mo2 N4 93.22(14) . . . . ? S5 Mo1 Mo2 N4 -177.91(9) . . . . ? N3 Mo1 Mo2 N4 -73.03(12) . . . . ? S2 Mo1 Mo2 N4 -135.77(10) . . . . ? S1 Mo1 Mo2 N4 -34.05(10) . . . . ? N5 Mo1 Mo2 N3 166.25(12) . . . . ? N4 Mo1 Mo2 N3 73.03(12) . . . . ? S5 Mo1 Mo2 N3 -104.88(8) . . . . ? S2 Mo1 Mo2 N3 -62.73(8) . . . . ? S1 Mo1 Mo2 N3 38.98(8) . . . . ? N5 Mo1 Mo2 S5 -88.87(10) . . . . ? N4 Mo1 Mo2 S5 177.91(9) . . . . ? N3 Mo1 Mo2 S5 104.88(8) . . . . ? S2 Mo1 Mo2 S5 42.14(4) . . . . ? S1 Mo1 Mo2 S5 143.86(5) . . . . ? N5 Mo1 Mo2 S4 -121.59(10) . . . . ? N4 Mo1 Mo2 S4 145.19(10) . . . . ? S5 Mo1 Mo2 S4 -32.72(5) . . . . ? N3 Mo1 Mo2 S4 72.16(8) . . . . ? S2 Mo1 Mo2 S4 9.42(5) . . . . ? S1 Mo1 Mo2 S4 111.14(5) . . . . ? N5 Mo1 Mo2 S3 129.27(10) . . . . ? N4 Mo1 Mo2 S3 36.05(10) . . . . ? S5 Mo1 Mo2 S3 -141.87(5) . . . . ? N3 Mo1 Mo2 S3 -36.99(9) . . . . ? S2 Mo1 Mo2 S3 -99.72(5) . . . . ? S1 Mo1 Mo2 S3 2.00(6) . . . . ? N5 Mo1 S1 C1 109.34(15) . . . . ? N4 Mo1 S1 C1 -147.73(14) . . . . ? S5 Mo1 S1 C1 -24.67(14) . . . . ? N3 Mo1 S1 C1 -90.49(13) . . . . ? S2 Mo1 S1 C1 4.86(11) . . . . ? Mo2 Mo1 S1 C1 -121.45(11) . . . . ? N5 Mo1 S2 C1 -101.35(15) . . . . ? N4 Mo1 S2 C1 49.82(17) . . . . ? S5 Mo1 S2 C1 161.20(12) . . . . ? N3 Mo1 S2 C1 80.85(13) . . . . ? S1 Mo1 S2 C1 -4.83(12) . . . . ? Mo2 Mo1 S2 C1 127.57(11) . . . . ? N6 Mo2 S3 C8 -105.01(16) . . . . ? N4 Mo2 S3 C8 159.68(15) . . . . ? N3 Mo2 S3 C8 102.46(14) . . . . ? S5 Mo2 S3 C8 33.31(15) . . . . ? S4 Mo2 S3 C8 -1.27(13) . . . . ? Mo1 Mo2 S3 C8 132.21(13) . . . . ? N6 Mo2 S4 C8 96.83(16) . . . . ? N4 Mo2 S4 C8 -45.6(2) . . . . ? N3 Mo2 S4 C8 -81.76(14) . . . . ? S5 Mo2 S4 C8 -161.67(13) . . . . ? S3 Mo2 S4 C8 1.27(13) . . . . ? Mo1 Mo2 S4 C8 -135.12(13) . . . . ? N6 Mo2 S5 Mo1 -97.65(10) . . . . ? N4 Mo2 S5 Mo1 1.71(8) . . . . ? N3 Mo2 S5 Mo1 53.66(7) . . . . ? S4 Mo2 S5 Mo1 156.89(3) . . . . ? S3 Mo2 S5 Mo1 124.42(6) . . . . ? N5 Mo1 S5 Mo2 105.08(10) . . . . ? N4 Mo1 S5 Mo2 -1.73(8) . . . . ? N3 Mo1 S5 Mo2 -53.09(7) . . . . ? S2 Mo1 S5 Mo2 -148.35(3) . . . . ? S1 Mo1 S5 Mo2 -120.43(6) . . . . ? N6 Mo2 N3 C15 -41.2(3) . . . . ? N4 Mo2 N3 C15 -25.75(17) . . . . ? S5 Mo2 N3 C15 -142.19(18) . . . . ? S4 Mo2 N3 C15 135.96(17) . . . . ? S3 Mo2 N3 C15 66.87(17) . . . . ? Mo1 Mo2 N3 C15 -88.71(18) . . . . ? N6 Mo2 N3 C20 176.5(3) . . . . ? N4 Mo2 N3 C20 -168.0(3) . . . . ? S5 Mo2 N3 C20 75.5(3) . . . . ? S4 Mo2 N3 C20 -6.3(3) . . . . ? S3 Mo2 N3 C20 -75.4(3) . . . . ? Mo1 Mo2 N3 C20 129.0(3) . . . . ? N6 Mo2 N3 Mo1 47.5(2) . . . . ? N4 Mo2 N3 Mo1 62.96(9) . . . . ? S5 Mo2 N3 Mo1 -53.48(5) . . . . ? S4 Mo2 N3 Mo1 -135.33(5) . . . . ? S3 Mo2 N3 Mo1 155.58(5) . . . . ? N5 Mo1 N3 C15 52.6(4) . . . . ? N4 Mo1 N3 C15 26.61(18) . . . . ? S5 Mo1 N3 C15 144.07(19) . . . . ? S2 Mo1 N3 C15 -133.14(18) . . . . ? S1 Mo1 N3 C15 -62.67(18) . . . . ? Mo2 Mo1 N3 C15 90.69(19) . . . . ? N5 Mo1 N3 C20 -177.2(3) . . . . ? N4 Mo1 N3 C20 156.8(3) . . . . ? S5 Mo1 N3 C20 -85.8(3) . . . . ? S2 Mo1 N3 C20 -3.0(3) . . . . ? S1 Mo1 N3 C20 67.5(3) . . . . ? Mo2 Mo1 N3 C20 -139.2(3) . . . . ? N5 Mo1 N3 Mo2 -38.1(3) . . . . ? N4 Mo1 N3 Mo2 -64.07(9) . . . . ? S5 Mo1 N3 Mo2 53.38(5) . . . . ? S2 Mo1 N3 Mo2 136.17(5) . . . . ? S1 Mo1 N3 Mo2 -153.36(5) . . . . ? N5 Mo1 N4 C30 31.2(3) . . . . ? S5 Mo1 N4 C30 135.2(3) . . . . ? N3 Mo1 N4 C30 -158.3(3) . . . . ? S2 Mo1 N4 C30 -120.5(3) . . . . ? S1 Mo1 N4 C30 -70.1(3) . . . . ? Mo2 Mo1 N4 C30 133.4(3) . . . . ? N5 Mo1 N4 C15 164.06(19) . . . . ? S5 Mo1 N4 C15 -92.03(17) . . . . ? N3 Mo1 N4 C15 -25.46(17) . . . . ? S2 Mo1 N4 C15 12.3(2) . . . . ? S1 Mo1 N4 C15 62.66(17) . . . . ? Mo2 Mo1 N4 C15 -93.83(18) . . . . ? N5 Mo1 N4 Mo2 -102.12(11) . . . . ? S5 Mo1 N4 Mo2 1.79(8) . . . . ? N3 Mo1 N4 Mo2 68.37(9) . . . . ? S2 Mo1 N4 Mo2 106.09(11) . . . . ? S1 Mo1 N4 Mo2 156.49(6) . . . . ? N6 Mo2 N4 C30 -31.4(3) . . . . ? N3 Mo2 N4 C30 155.9(3) . . . . ? S5 Mo2 N4 C30 -136.4(3) . . . . ? S4 Mo2 N4 C30 112.6(3) . . . . ? S3 Mo2 N4 C30 69.3(3) . . . . ? Mo1 Mo2 N4 C30 -134.6(3) . . . . ? N6 Mo2 N4 C15 -162.70(19) . . . . ? N3 Mo2 N4 C15 24.63(16) . . . . ? S5 Mo2 N4 C15 92.37(17) . . . . ? S4 Mo2 N4 C15 -18.7(3) . . . . ? S3 Mo2 N4 C15 -62.00(17) . . . . ? Mo1 Mo2 N4 C15 94.16(18) . . . . ? N6 Mo2 N4 Mo1 103.14(11) . . . . ? N3 Mo2 N4 Mo1 -69.53(9) . . . . ? S5 Mo2 N4 Mo1 -1.80(8) . . . . ? S4 Mo2 N4 Mo1 -112.84(14) . . . . ? S3 Mo2 N4 Mo1 -156.17(6) . . . . ? N4 Mo1 N5 C40 110.7(13) . . . . ? S5 Mo1 N5 C40 0.5(13) . . . . ? N3 Mo1 N5 C40 88.5(14) . . . . ? S2 Mo1 N5 C40 -85.5(13) . . . . ? S1 Mo1 N5 C40 -158.7(13) . . . . ? Mo2 Mo1 N5 C40 56.6(13) . . . . ? N4 Mo2 N6 C50 -34.5(12) . . . . ? N3 Mo2 N6 C50 -21.5(14) . . . . ? S5 Mo2 N6 C50 74.1(12) . . . . ? S4 Mo2 N6 C50 161.4(12) . . . . ? S3 Mo2 N6 C50 -126.4(12) . . . . ? Mo1 Mo2 N6 C50 17.2(12) . . . . ? C5 N1 C1 S1 177.9(3) . . . . ? C2 N1 C1 S1 -4.1(5) . . . . ? C5 N1 C1 S2 -5.2(5) . . . . ? C2 N1 C1 S2 172.8(3) . . . . ? Mo1 S1 C1 N1 170.2(3) . . . . ? Mo1 S1 C1 S2 -7.07(17) . . . . ? Mo1 S2 C1 N1 -170.0(3) . . . . ? Mo1 S2 C1 S1 7.20(17) . . . . ? C1 N1 C2 C3 92.3(5) . . . . ? C5 N1 C2 C3 -89.7(5) . . . . ? N1 C2 C3 C4 -179.8(4) . . . . ? C1 N1 C5 C6 88.0(5) . . . . ? C2 N1 C5 C6 -90.1(5) . . . . ? N1 C5 C6 C7 84.9(7) . . . . ? C12 N2 C8 S3 -3.2(5) . . . . ? C9 N2 C8 S3 177.5(3) . . . . ? C12 N2 C8 S4 178.0(3) . . . . ? C9 N2 C8 S4 -1.3(6) . . . . ? Mo2 S3 C8 N2 -177.0(3) . . . . ? Mo2 S3 C8 S4 1.87(19) . . . . ? Mo2 S4 C8 N2 177.0(3) . . . . ? Mo2 S4 C8 S3 -1.90(19) . . . . ? C8 N2 C9 C10 -109.7(5) . . . . ? C12 N2 C9 C10 70.9(6) . . . . ? N2 C9 C10 C11 55.4(7) . . . . ? C8 N2 C12 C13 -89.5(5) . . . . ? C9 N2 C12 C13 89.9(5) . . . . ? N2 C12 C13 C14 179.2(4) . . . . ? C20 N3 C15 O1 6.9(6) . . . . ? Mo2 N3 C15 O1 -146.0(4) . . . . ? Mo1 N3 C15 O1 144.3(4) . . . . ? C20 N3 C15 N4 -172.7(3) . . . . ? Mo2 N3 C15 N4 34.4(2) . . . . ? Mo1 N3 C15 N4 -35.3(2) . . . . ? C30 N4 C15 O1 2.3(5) . . . . ? Mo1 N4 C15 O1 -140.5(3) . . . . ? Mo2 N4 C15 O1 143.0(3) . . . . ? C30 N4 C15 N3 -178.1(3) . . . . ? Mo1 N4 C15 N3 39.1(2) . . . . ? Mo2 N4 C15 N3 -37.4(2) . . . . ? C15 N3 C20 C25 -145.3(3) . . . . ? Mo2 N3 C20 C25 -10.4(5) . . . . ? Mo1 N3 C20 C25 97.0(4) . . . . ? C15 N3 C20 C21 37.5(5) . . . . ? Mo2 N3 C20 C21 172.3(3) . . . . ? Mo1 N3 C20 C21 -80.2(4) . . . . ? C25 C20 C21 C22 2.5(6) . . . . ? N3 C20 C21 C22 179.8(3) . . . . ? C20 C21 C22 C23 -0.3(6) . . . . ? C21 C22 C23 C24 -1.8(7) . . . . ? C21 C22 C23 C26 176.4(5) . . . . ? C22 C23 C24 C25 1.9(8) . . . . ? C26 C23 C24 C25 -176.3(6) . . . . ? C21 C20 C25 C24 -2.5(6) . . . . ? N3 C20 C25 C24 -179.9(4) . . . . ? C23 C24 C25 C20 0.3(7) . . . . ? C15 N4 C30 C31 -120.0(4) . . . . ? Mo1 N4 C30 C31 5.5(5) . . . . ? Mo2 N4 C30 C31 116.5(3) . . . . ? C15 N4 C30 C35 58.9(4) . . . . ? Mo1 N4 C30 C35 -175.6(3) . . . . ? Mo2 N4 C30 C35 -64.6(4) . . . . ? C35 C30 C31 C32 -0.9(6) . . . . ? N4 C30 C31 C32 178.0(4) . . . . ? C30 C31 C32 C33 1.3(7) . . . . ? C31 C32 C33 C34 -0.8(7) . . . . ? C31 C32 C33 C36 -178.6(6) . . . . ? C32 C33 C34 C35 -0.2(7) . . . . ? C36 C33 C34 C35 177.8(5) . . . . ? C33 C34 C35 C30 0.6(7) . . . . ? C31 C30 C35 C34 0.0(6) . . . . ? N4 C30 C35 C34 -178.9(4) . . . . ? Mo1 N5 C40 C45 -113.6(13) . . . . ? Mo1 N5 C40 C41 64.9(14) . . . . ? C45 C40 C41 C42 -0.7(7) . . . . ? N5 C40 C41 C42 -179.3(5) . . . . ? C40 C41 C42 C43 2.0(10) . . . . ? C41 C42 C43 C44 -1.7(11) . . . . ? C41 C42 C43 C46 178.7(7) . . . . ? C42 C43 C44 C45 0.2(10) . . . . ? C46 C43 C44 C45 179.7(6) . . . . ? N5 C40 C45 C44 177.7(4) . . . . ? C41 C40 C45 C44 -0.8(7) . . . . ? C43 C44 C45 C40 1.1(9) . . . . ? Mo2 N6 C50 C51 -108.2(12) . . . . ? Mo2 N6 C50 C55 71.9(13) . . . . ? N6 C50 C51 C52 178.6(3) . . . . ? C55 C50 C51 C52 -1.5(6) . . . . ? C50 C51 C52 C53 -0.3(6) . . . . ? C51 C52 C53 C54 1.6(6) . . . . ? C51 C52 C53 C56 -177.3(4) . . . . ? C52 C53 C54 C55 -1.2(6) . . . . ? C56 C53 C54 C55 177.7(4) . . . . ? C53 C54 C55 C50 -0.5(6) . . . . ? C51 C50 C55 C54 1.8(5) . . . . ? N6 C50 C55 C54 -178.2(3) . . . . ? _diffrn_measured_fraction_theta_max 0.929 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.694 _refine_diff_density_min -0.379 _refine_diff_density_rms 0.072 data_str0032 _database_code_depnum_ccdc_archive 'CCDC 253357' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H42 Mo2 N4 S6' _chemical_formula_weight 818.90 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 tetragonal _symmetry_space_group_name_H-M P4(3)2(1)2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y+1/2, x+1/2, z+3/4' 'y+1/2, -x+1/2, z+1/4' '-x+1/2, y+1/2, -z+3/4' 'x+1/2, -y+1/2, -z+1/4' 'y, x, -z' '-y, -x, -z+1/2' _cell_length_a 12.4558(5) _cell_length_b 12.4558(5) _cell_length_c 49.648(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7702.8(6) _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 block _exptl_crystal_colour red _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.412 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3344 _exptl_absorpt_coefficient_mu 0.999 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8895 _exptl_absorpt_correction_T_max 0.9067 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 68980 _diffrn_reflns_av_R_equivalents 0.0501 _diffrn_reflns_av_sigmaI/netI 0.0366 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -63 _diffrn_reflns_limit_l_max 63 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 28.32 _reflns_number_total 9229 _reflns_number_gt 7565 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0477P)^2^+3.5531P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(5) _refine_ls_number_reflns 9229 _refine_ls_number_parameters 356 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0625 _refine_ls_R_factor_gt 0.0472 _refine_ls_wR_factor_ref 0.1057 _refine_ls_wR_factor_gt 0.1000 _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_restrained_S_all 1.092 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.89465(3) 0.93404(3) 0.036353(7) 0.04659(10) Uani 1 1 d . . . Mo2 Mo 0.88514(4) 0.71186(3) 0.021273(7) 0.04817(10) Uani 1 1 d . . . S1 S 1.01040(13) 1.09988(12) 0.03469(3) 0.0749(4) Uani 1 1 d . . . S2 S 0.78873(14) 1.09498(11) 0.05185(3) 0.0734(4) Uani 1 1 d . . . S3 S 0.98236(15) 0.56119(13) -0.00205(3) 0.0809(5) Uani 1 1 d . . . S4 S 0.76117(15) 0.55626(12) 0.01436(3) 0.0772(4) Uani 1 1 d . . . S5 S 0.73848(9) 0.82654(9) 0.03143(2) 0.0482(3) Uani 1 1 d . . . S6 S 1.02319(9) 0.83642(10) 0.01084(2) 0.0514(3) Uani 1 1 d . . . N1 N 0.9140(6) 1.2688(4) 0.05762(10) 0.099(2) Uani 1 1 d . . . N2 N 0.8582(6) 0.3865(4) -0.00780(10) 0.104(2) Uani 1 1 d . . . N3 N 0.9354(3) 0.9110(3) 0.06903(7) 0.0539(9) Uani 1 1 d . . . N4 N 0.9280(4) 0.6722(3) 0.05281(8) 0.0583(10) Uani 1 1 d . . . C1 C 0.9060(6) 1.1655(4) 0.04934(10) 0.0791(19) Uani 1 1 d . . . C2 C 1.0156(8) 1.3278(6) 0.05473(15) 0.123(3) Uani 1 1 d . . . H2A H 1.0001 1.4040 0.0537 0.148 Uiso 1 1 calc R . . H2B H 1.0494 1.3069 0.0379 0.148 Uiso 1 1 calc R . . C3 C 1.0927(10) 1.3086(7) 0.0773(2) 0.176(6) Uani 1 1 d . . . H3A H 1.1026 1.2321 0.0800 0.212 Uiso 1 1 calc R . . H3B H 1.0647 1.3390 0.0939 0.212 Uiso 1 1 calc R . . C4 C 1.2039(12) 1.3631(12) 0.0700(3) 0.278(10) Uani 1 1 d . . . H4A H 1.2538 1.3524 0.0845 0.416 Uiso 1 1 calc R . . H4B H 1.1934 1.4387 0.0672 0.416 Uiso 1 1 calc R . . H4C H 1.2320 1.3314 0.0538 0.416 Uiso 1 1 calc R . . C5 C 0.8247(9) 1.3218(6) 0.07057(17) 0.131(3) Uani 1 1 d . . . H5A H 0.7573 1.2905 0.0648 0.157 Uiso 1 1 calc R . . H5B H 0.8243 1.3978 0.0662 0.157 Uiso 1 1 calc R . . C6 C 0.8428(13) 1.3035(14) 0.1040(2) 0.254(9) Uani 1 1 d . . . H6A H 0.8638 1.2309 0.1088 0.305 Uiso 1 1 calc R . . H6B H 0.8904 1.3557 0.1122 0.305 Uiso 1 1 calc R . . C7 C 0.728(2) 1.326(2) 0.1085(6) 0.456(18) Uiso 1 1 d . . . H7A H 0.7126 1.3225 0.1274 0.685 Uiso 1 1 calc R . . H7B H 0.6854 1.2738 0.0991 0.685 Uiso 1 1 calc R . . H7C H 0.7113 1.3965 0.1019 0.685 Uiso 1 1 calc R . . C8 C 0.8686(6) 0.4895(4) 0.00060(10) 0.0813(19) Uani 1 1 d . . . C9 C 0.9497(9) 0.3319(6) -0.02035(15) 0.130(3) Uani 1 1 d . . . H9A H 1.0158 0.3604 -0.0128 0.156 Uiso 1 1 calc R . . H9B H 0.9466 0.2560 -0.0160 0.156 Uiso 1 1 calc R . . C10 C 0.9521(12) 0.3443(10) -0.04954(17) 0.187(6) Uani 1 1 d . . . H10A H 0.9411 0.4192 -0.0541 0.225 Uiso 1 1 calc R . . H10B H 0.8941 0.3030 -0.0575 0.225 Uiso 1 1 calc R . . C11 C 1.0559(12) 0.3076(11) -0.0609(2) 0.215(7) Uani 1 1 d . . . H11A H 1.0551 0.3165 -0.0801 0.323 Uiso 1 1 calc R . . H11B H 1.0665 0.2331 -0.0566 0.323 Uiso 1 1 calc R . . H11C H 1.1133 0.3492 -0.0533 0.323 Uiso 1 1 calc R . . C12 C 0.7602(9) 0.3276(6) -0.00452(18) 0.133(4) Uani 1 1 d . . . H12A H 0.7269 0.3490 0.0123 0.160 Uiso 1 1 calc R . . H12B H 0.7772 0.2517 -0.0032 0.160 Uiso 1 1 calc R . . C13 C 0.6820(11) 0.3428(9) -0.0265(2) 0.182(5) Uani 1 1 d . . . H13A H 0.7074 0.3063 -0.0426 0.218 Uiso 1 1 calc R . . H13B H 0.6760 0.4187 -0.0306 0.218 Uiso 1 1 calc R . . C14 C 0.5737(13) 0.2996(14) -0.0188(4) 0.293(10) Uani 1 1 d . . . H14A H 0.5239 0.3120 -0.0332 0.440 Uiso 1 1 calc R . . H14B H 0.5490 0.3352 -0.0028 0.440 Uiso 1 1 calc R . . H14C H 0.5792 0.2238 -0.0155 0.440 Uiso 1 1 calc R . . C20 C 0.9708(4) 0.9154(4) 0.09533(9) 0.0602(13) Uani 1 1 d . . . C21 C 1.0738(7) 0.9020(13) 0.10076(14) 0.205(7) Uani 1 1 d . . . H21A H 1.1230 0.8872 0.0872 0.246 Uiso 1 1 calc R . . C22 C 1.1060(8) 0.9108(17) 0.12731(18) 0.285(12) Uani 1 1 d . . . H22A H 1.1796 0.9144 0.1304 0.342 Uiso 1 1 calc R . . C23 C 1.0459(8) 0.9143(9) 0.14810(14) 0.133(3) Uani 1 1 d . . . C24 C 0.9490(8) 0.9227(12) 0.14237(14) 0.193(7) Uani 1 1 d . . . H24A H 0.9002 0.9310 0.1564 0.232 Uiso 1 1 calc R . . C25 C 0.9093(7) 0.9202(12) 0.11593(13) 0.195(7) Uani 1 1 d . . . H25A H 0.8354 0.9222 0.1133 0.234 Uiso 1 1 calc R . . C26 C 1.0874(10) 0.9157(14) 0.17747(16) 0.239(8) Uani 1 1 d . . . H26A H 1.0279 0.9234 0.1896 0.358 Uiso 1 1 calc R . . H26B H 1.1360 0.9748 0.1798 0.358 Uiso 1 1 calc R . . H26C H 1.1242 0.8496 0.1812 0.358 Uiso 1 1 calc R . . C30 C 0.9698(5) 0.6438(4) 0.07739(9) 0.0607(13) Uani 1 1 d . . . C31 C 1.0756(7) 0.6304(11) 0.08027(15) 0.162(5) Uani 1 1 d . . . H31A H 1.1211 0.6365 0.0655 0.195 Uiso 1 1 calc R . . C32 C 1.1157(8) 0.6078(15) 0.1052(2) 0.235(9) Uani 1 1 d . . . H32A H 1.1900 0.6031 0.1068 0.282 Uiso 1 1 calc R . . C33 C 1.0586(8) 0.5920(8) 0.12699(13) 0.115(3) Uani 1 1 d . . . C34 C 0.9537(8) 0.6052(9) 0.12405(13) 0.137(4) Uani 1 1 d . . . H34A H 0.9093 0.5978 0.1390 0.164 Uiso 1 1 calc R . . C35 C 0.9085(6) 0.6296(8) 0.09944(12) 0.122(3) Uani 1 1 d . . . H35A H 0.8344 0.6365 0.0981 0.147 Uiso 1 1 calc R . . C36 C 1.1069(9) 0.5676(14) 0.15459(17) 0.247(9) Uani 1 1 d . . . H36A H 1.1832 0.5589 0.1529 0.370 Uiso 1 1 calc R . . H36B H 1.0761 0.5026 0.1616 0.370 Uiso 1 1 calc R . . H36C H 1.0919 0.6258 0.1667 0.370 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 0.0601(2) 0.0472(2) 0.03248(16) -0.00111(15) -0.00440(16) -0.00454(17) Mo2 0.0663(3) 0.0453(2) 0.03291(16) 0.00102(15) -0.00087(17) -0.00161(18) S1 0.0924(10) 0.0657(8) 0.0666(8) -0.0019(7) -0.0118(7) -0.0260(8) S2 0.1026(11) 0.0602(8) 0.0574(7) -0.0092(6) 0.0089(7) 0.0094(8) S3 0.1121(13) 0.0652(9) 0.0655(8) -0.0071(7) 0.0003(8) 0.0272(9) S4 0.1150(13) 0.0613(8) 0.0553(7) -0.0036(6) 0.0074(7) -0.0283(8) S5 0.0553(6) 0.0558(6) 0.0335(5) -0.0012(4) 0.0059(4) -0.0066(5) S6 0.0492(6) 0.0632(7) 0.0417(5) 0.0033(5) -0.0035(5) -0.0009(5) N1 0.171(6) 0.057(3) 0.069(3) -0.006(2) -0.026(4) -0.005(4) N2 0.192(7) 0.051(3) 0.069(3) -0.003(2) -0.015(4) 0.005(4) N3 0.069(2) 0.056(2) 0.0365(17) -0.0038(16) -0.0057(17) -0.0048(18) N4 0.083(3) 0.045(2) 0.047(2) -0.0011(17) 0.000(2) 0.000(2) C1 0.142(6) 0.056(3) 0.039(2) 0.004(2) -0.018(3) -0.026(3) C2 0.208(9) 0.060(4) 0.101(5) 0.009(4) -0.052(6) -0.045(5) C3 0.274(15) 0.094(6) 0.162(9) 0.020(6) -0.115(10) -0.055(8) C4 0.256(17) 0.204(15) 0.37(2) 0.082(15) -0.148(17) -0.121(13) C5 0.216(10) 0.069(4) 0.108(6) -0.010(4) -0.007(6) 0.031(6) C6 0.268(19) 0.35(2) 0.147(10) -0.146(12) 0.049(11) 0.020(16) C8 0.148(6) 0.049(3) 0.047(3) 0.004(2) -0.007(3) 0.006(3) C9 0.243(11) 0.062(4) 0.085(5) -0.018(4) -0.009(6) 0.046(6) C10 0.302(16) 0.183(11) 0.077(5) -0.015(6) 0.017(8) 0.102(11) C11 0.295(18) 0.232(15) 0.119(8) -0.021(9) 0.029(10) 0.098(14) C12 0.226(11) 0.059(4) 0.116(6) -0.008(4) -0.026(7) -0.036(6) C13 0.239(14) 0.142(9) 0.164(10) -0.009(7) -0.090(10) -0.052(9) C14 0.202(16) 0.28(2) 0.39(3) -0.023(19) -0.066(16) -0.083(16) C20 0.076(3) 0.070(3) 0.034(2) -0.002(2) -0.012(2) -0.016(3) C21 0.089(6) 0.48(2) 0.049(4) -0.001(8) -0.012(4) -0.027(10) C22 0.093(6) 0.69(4) 0.070(5) 0.014(12) -0.032(5) -0.066(14) C23 0.132(7) 0.215(11) 0.052(4) 0.006(5) -0.028(4) -0.031(7) C24 0.116(7) 0.43(2) 0.039(3) -0.016(7) -0.011(4) 0.043(10) C25 0.087(5) 0.46(2) 0.043(3) -0.032(7) -0.005(3) 0.033(9) C26 0.199(12) 0.45(2) 0.066(5) 0.022(9) -0.062(6) -0.069(13) C30 0.087(4) 0.048(3) 0.046(3) 0.004(2) -0.010(2) 0.004(2) C31 0.097(6) 0.324(15) 0.066(4) 0.048(7) -0.002(4) 0.053(8) C32 0.096(6) 0.51(3) 0.097(6) 0.074(11) -0.011(6) 0.077(12) C33 0.122(6) 0.169(8) 0.053(4) 0.026(4) -0.023(4) 0.018(6) C34 0.135(7) 0.227(11) 0.049(3) 0.040(5) -0.019(4) -0.036(8) C35 0.100(5) 0.216(9) 0.052(3) 0.045(5) -0.010(3) -0.035(6) C36 0.166(10) 0.50(3) 0.072(5) 0.072(10) -0.031(6) 0.084(14) _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 N3 1.724(3) . ? Mo1 S5 2.3741(12) . ? Mo1 S6 2.3764(13) . ? Mo1 S2 2.5201(14) . ? Mo1 S1 2.5204(14) . ? Mo1 S6 2.6923(11) 7 ? Mo1 Mo2 2.8694(5) . ? Mo2 N4 1.726(4) . ? Mo2 S5 2.3732(12) . ? Mo2 S6 2.3733(12) . ? Mo2 S4 2.5017(14) . ? Mo2 S3 2.5158(15) . ? Mo2 S5 2.7368(11) 7 ? S1 C1 1.699(7) . ? S2 C1 1.709(7) . ? S3 C8 1.680(7) . ? S4 C8 1.717(7) . ? S5 Mo2 2.7368(11) 7 ? S6 Mo1 2.6923(11) 7 ? N1 C1 1.354(7) . ? N1 C5 1.445(10) . ? N1 C2 1.470(10) . ? N2 C8 1.355(7) . ? N2 C12 1.434(10) . ? N2 C9 1.467(11) . ? N3 C20 1.380(5) . ? N4 C30 1.373(6) . ? C2 C3 1.496(11) . ? C3 C4 1.585(17) . ? C5 C6 1.689(15) . ? C6 C7 1.47(3) . ? C9 C10 1.458(10) . ? C10 C11 1.483(15) . ? C12 C13 1.475(13) . ? C13 C14 1.502(17) . ? C20 C25 1.279(8) . ? C20 C21 1.321(10) . ? C21 C22 1.382(10) . ? C22 C23 1.276(12) . ? C23 C24 1.244(12) . ? C23 C26 1.547(9) . ? C24 C25 1.403(9) . ? C30 C31 1.336(9) . ? C30 C35 1.346(8) . ? C31 C32 1.363(10) . ? C32 C33 1.312(12) . ? C33 C34 1.325(12) . ? C33 C36 1.527(9) . ? C34 C35 1.379(9) . ? 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 N3 Mo1 S5 104.12(13) . . ? N3 Mo1 S6 102.61(14) . . ? S5 Mo1 S6 102.04(4) . . ? N3 Mo1 S2 89.95(13) . . ? S5 Mo1 S2 92.93(5) . . ? S6 Mo1 S2 157.30(5) . . ? N3 Mo1 S1 89.94(13) . . ? S5 Mo1 S1 158.06(5) . . ? S6 Mo1 S1 90.94(5) . . ? S2 Mo1 S1 69.98(5) . . ? N3 Mo1 S6 165.23(13) . 7 ? S5 Mo1 S6 85.55(4) . 7 ? S6 Mo1 S6 85.91(4) . 7 ? S2 Mo1 S6 78.26(4) . 7 ? S1 Mo1 S6 77.74(4) . 7 ? N3 Mo1 Mo2 95.57(12) . . ? S5 Mo1 Mo2 52.80(3) . . ? S6 Mo1 Mo2 52.78(3) . . ? S2 Mo1 Mo2 145.61(4) . . ? S1 Mo1 Mo2 143.66(4) . . ? S6 Mo1 Mo2 99.19(3) 7 . ? N4 Mo2 S5 102.56(14) . . ? N4 Mo2 S6 99.26(15) . . ? S5 Mo2 S6 102.16(4) . . ? N4 Mo2 S4 95.37(14) . . ? S5 Mo2 S4 91.17(5) . . ? S6 Mo2 S4 157.48(4) . . ? N4 Mo2 S3 93.16(13) . . ? S5 Mo2 S3 156.54(5) . . ? S6 Mo2 S3 92.20(5) . . ? S4 Mo2 S3 69.88(6) . . ? N4 Mo2 S5 169.83(13) . 7 ? S5 Mo2 S5 85.70(4) . 7 ? S6 Mo2 S5 84.57(4) . 7 ? S4 Mo2 S5 78.35(4) . 7 ? S3 Mo2 S5 77.22(4) . 7 ? N4 Mo2 Mo1 91.52(13) . . ? S5 Mo2 Mo1 52.83(3) . . ? S6 Mo2 Mo1 52.88(3) . . ? S4 Mo2 Mo1 143.95(5) . . ? S3 Mo2 Mo1 145.05(5) . . ? S5 Mo2 Mo1 98.26(3) 7 . ? C1 S1 Mo1 86.71(19) . . ? C1 S2 Mo1 86.5(2) . . ? C8 S3 Mo2 87.4(2) . . ? C8 S4 Mo2 87.1(2) . . ? Mo2 S5 Mo1 74.37(4) . . ? Mo2 S5 Mo2 92.90(4) . 7 ? Mo1 S5 Mo2 92.71(4) . 7 ? Mo2 S6 Mo1 74.33(4) . . ? Mo2 S6 Mo1 93.86(4) . 7 ? Mo1 S6 Mo1 92.76(4) . 7 ? C1 N1 C5 120.8(7) . . ? C1 N1 C2 120.6(7) . . ? C5 N1 C2 118.5(6) . . ? C8 N2 C12 122.1(7) . . ? C8 N2 C9 119.7(7) . . ? C12 N2 C9 118.2(6) . . ? C20 N3 Mo1 168.1(3) . . ? C30 N4 Mo2 175.6(4) . . ? N1 C1 S1 122.0(6) . . ? N1 C1 S2 121.9(6) . . ? S1 C1 S2 116.0(3) . . ? N1 C2 C3 113.6(7) . . ? C2 C3 C4 108.7(9) . . ? N1 C5 C6 105.8(8) . . ? C7 C6 C5 89.7(16) . . ? N2 C8 S3 124.0(6) . . ? N2 C8 S4 120.4(6) . . ? S3 C8 S4 115.5(3) . . ? C10 C9 N2 112.9(8) . . ? C9 C10 C11 111.3(10) . . ? N2 C12 C13 114.3(8) . . ? C12 C13 C14 111.0(12) . . ? C25 C20 C21 115.1(6) . . ? C25 C20 N3 124.5(6) . . ? C21 C20 N3 119.9(5) . . ? C20 C21 C22 117.8(8) . . ? C23 C22 C21 127.2(9) . . ? C24 C23 C22 112.8(7) . . ? C24 C23 C26 122.6(9) . . ? C22 C23 C26 124.5(10) . . ? C23 C24 C25 123.7(8) . . ? C20 C25 C24 122.5(8) . . ? C31 C30 C35 117.1(6) . . ? C31 C30 N4 120.1(6) . . ? C35 C30 N4 122.8(6) . . ? C30 C31 C32 119.0(8) . . ? C33 C32 C31 125.5(9) . . ? C32 C33 C34 115.2(7) . . ? C32 C33 C36 123.9(9) . . ? C34 C33 C36 120.8(8) . . ? C33 C34 C35 121.8(8) . . ? C30 C35 C34 121.2(8) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Mo1 Mo2 N4 -1.1(2) . . . . ? S5 Mo1 Mo2 N4 -104.64(15) . . . . ? S6 Mo1 Mo2 N4 100.48(15) . . . . ? S2 Mo1 Mo2 N4 -99.23(16) . . . . ? S1 Mo1 Mo2 N4 96.39(16) . . . . ? S6 Mo1 Mo2 N4 178.15(15) 7 . . . ? N3 Mo1 Mo2 S5 103.52(14) . . . . ? S6 Mo1 Mo2 S5 -154.87(5) . . . . ? S2 Mo1 Mo2 S5 5.41(7) . . . . ? S1 Mo1 Mo2 S5 -158.96(7) . . . . ? S6 Mo1 Mo2 S5 -77.20(4) 7 . . . ? N3 Mo1 Mo2 S6 -101.61(14) . . . . ? S5 Mo1 Mo2 S6 154.87(5) . . . . ? S2 Mo1 Mo2 S6 160.29(7) . . . . ? S1 Mo1 Mo2 S6 -4.09(7) . . . . ? S6 Mo1 Mo2 S6 77.67(4) 7 . . . ? N3 Mo1 Mo2 S4 100.15(15) . . . . ? S5 Mo1 Mo2 S4 -3.37(7) . . . . ? S6 Mo1 Mo2 S4 -158.24(7) . . . . ? S2 Mo1 Mo2 S4 2.04(9) . . . . ? S1 Mo1 Mo2 S4 -162.33(8) . . . . ? S6 Mo1 Mo2 S4 -80.57(7) 7 . . . ? N3 Mo1 Mo2 S3 -98.85(15) . . . . ? S5 Mo1 Mo2 S3 157.64(8) . . . . ? S6 Mo1 Mo2 S3 2.76(7) . . . . ? S2 Mo1 Mo2 S3 163.05(9) . . . . ? S1 Mo1 Mo2 S3 -1.33(10) . . . . ? S6 Mo1 Mo2 S3 80.43(7) 7 . . . ? N3 Mo1 Mo2 S5 -178.32(14) . . . 7 ? S5 Mo1 Mo2 S5 78.16(4) . . . 7 ? S6 Mo1 Mo2 S5 -76.71(4) . . . 7 ? S2 Mo1 Mo2 S5 83.57(7) . . . 7 ? S1 Mo1 Mo2 S5 -80.80(7) . . . 7 ? S6 Mo1 Mo2 S5 0.96(4) 7 . . 7 ? N3 Mo1 S1 C1 -84.4(2) . . . . ? S5 Mo1 S1 C1 46.2(2) . . . . ? S6 Mo1 S1 C1 173.00(18) . . . . ? S2 Mo1 S1 C1 5.57(18) . . . . ? S6 Mo1 S1 C1 87.39(18) 7 . . . ? Mo2 Mo1 S1 C1 176.26(17) . . . . ? N3 Mo1 S2 C1 84.4(2) . . . . ? S5 Mo1 S2 C1 -171.45(17) . . . . ? S6 Mo1 S2 C1 -39.9(2) . . . . ? S1 Mo1 S2 C1 -5.54(17) . . . . ? S6 Mo1 S2 C1 -86.61(17) 7 . . . ? Mo2 Mo1 S2 C1 -175.76(16) . . . . ? N4 Mo2 S3 C8 92.3(2) . . . . ? S5 Mo2 S3 C8 -40.1(2) . . . . ? S6 Mo2 S3 C8 -168.27(19) . . . . ? S4 Mo2 S3 C8 -2.25(19) . . . . ? S5 Mo2 S3 C8 -84.35(19) 7 . . . ? Mo1 Mo2 S3 C8 -170.48(18) . . . . ? N4 Mo2 S4 C8 -89.2(2) . . . . ? S5 Mo2 S4 C8 168.06(18) . . . . ? S6 Mo2 S4 C8 41.2(2) . . . . ? S3 Mo2 S4 C8 2.20(18) . . . . ? S5 Mo2 S4 C8 82.70(18) 7 . . . ? Mo1 Mo2 S4 C8 170.75(17) . . . . ? N4 Mo2 S5 Mo1 82.25(14) . . . . ? S6 Mo2 S5 Mo1 -20.27(4) . . . . ? S4 Mo2 S5 Mo1 178.02(4) . . . . ? S3 Mo2 S5 Mo1 -146.80(11) . . . . ? S5 Mo2 S5 Mo1 -103.76(3) 7 . . . ? N4 Mo2 S5 Mo2 174.25(14) . . . 7 ? S6 Mo2 S5 Mo2 71.74(4) . . . 7 ? S4 Mo2 S5 Mo2 -89.98(4) . . . 7 ? S3 Mo2 S5 Mo2 -54.80(13) . . . 7 ? S5 Mo2 S5 Mo2 -11.75(5) 7 . . 7 ? Mo1 Mo2 S5 Mo2 92.00(3) . . . 7 ? N3 Mo1 S5 Mo2 -86.26(13) . . . . ? S6 Mo1 S5 Mo2 20.23(4) . . . . ? S2 Mo1 S5 Mo2 -176.94(4) . . . . ? S1 Mo1 S5 Mo2 145.30(11) . . . . ? S6 Mo1 S5 Mo2 105.08(3) 7 . . . ? N3 Mo1 S5 Mo2 -178.51(14) . . . 7 ? S6 Mo1 S5 Mo2 -72.03(4) . . . 7 ? S2 Mo1 S5 Mo2 90.80(4) . . . 7 ? S1 Mo1 S5 Mo2 53.05(13) . . . 7 ? S6 Mo1 S5 Mo2 12.82(4) 7 . . 7 ? Mo2 Mo1 S5 Mo2 -92.25(3) . . . 7 ? N4 Mo2 S6 Mo1 -84.85(13) . . . . ? S5 Mo2 S6 Mo1 20.25(4) . . . . ? S4 Mo2 S6 Mo1 145.28(13) . . . . ? S3 Mo2 S6 Mo1 -178.42(4) . . . . ? S5 Mo2 S6 Mo1 104.65(3) 7 . . . ? N4 Mo2 S6 Mo1 -176.64(13) . . . 7 ? S5 Mo2 S6 Mo1 -71.54(4) . . . 7 ? S4 Mo2 S6 Mo1 53.50(15) . . . 7 ? S3 Mo2 S6 Mo1 89.79(5) . . . 7 ? S5 Mo2 S6 Mo1 12.86(4) 7 . . 7 ? Mo1 Mo2 S6 Mo1 -91.79(4) . . . 7 ? N3 Mo1 S6 Mo2 87.43(13) . . . . ? S5 Mo1 S6 Mo2 -20.23(4) . . . . ? S2 Mo1 S6 Mo2 -150.42(12) . . . . ? S1 Mo1 S6 Mo2 177.58(4) . . . . ? S6 Mo1 S6 Mo2 -104.79(3) 7 . . . ? N3 Mo1 S6 Mo1 -179.34(13) . . . 7 ? S5 Mo1 S6 Mo1 73.00(4) . . . 7 ? S2 Mo1 S6 Mo1 -57.18(14) . . . 7 ? S1 Mo1 S6 Mo1 -89.19(5) . . . 7 ? S6 Mo1 S6 Mo1 -11.56(5) 7 . . 7 ? Mo2 Mo1 S6 Mo1 93.23(4) . . . 7 ? S5 Mo1 N3 C20 -135.7(18) . . . . ? S6 Mo1 N3 C20 118.3(18) . . . . ? S2 Mo1 N3 C20 -42.7(19) . . . . ? S1 Mo1 N3 C20 27.3(19) . . . . ? S6 Mo1 N3 C20 -6(2) 7 . . . ? Mo2 Mo1 N3 C20 171.3(18) . . . . ? S5 Mo2 N4 C30 -123(5) . . . . ? S6 Mo2 N4 C30 -18(5) . . . . ? S4 Mo2 N4 C30 144(5) . . . . ? S3 Mo2 N4 C30 74(5) . . . . ? S5 Mo2 N4 C30 93(5) 7 . . . ? Mo1 Mo2 N4 C30 -71(5) . . . . ? C5 N1 C1 S1 -178.6(5) . . . . ? C2 N1 C1 S1 -1.4(8) . . . . ? C5 N1 C1 S2 3.9(8) . . . . ? C2 N1 C1 S2 -178.9(5) . . . . ? Mo1 S1 C1 N1 173.7(4) . . . . ? Mo1 S1 C1 S2 -8.6(3) . . . . ? Mo1 S2 C1 N1 -173.7(4) . . . . ? Mo1 S2 C1 S1 8.6(3) . . . . ? C1 N1 C2 C3 -84.2(9) . . . . ? C5 N1 C2 C3 93.1(9) . . . . ? N1 C2 C3 C4 172.3(10) . . . . ? C1 N1 C5 C6 92.7(9) . . . . ? C2 N1 C5 C6 -84.5(9) . . . . ? N1 C5 C6 C7 -159.8(15) . . . . ? C12 N2 C8 S3 178.4(5) . . . . ? C9 N2 C8 S3 -0.7(8) . . . . ? C12 N2 C8 S4 -2.9(9) . . . . ? C9 N2 C8 S4 177.9(5) . . . . ? Mo2 S3 C8 N2 -177.9(5) . . . . ? Mo2 S3 C8 S4 3.4(3) . . . . ? Mo2 S4 C8 N2 177.8(5) . . . . ? Mo2 S4 C8 S3 -3.4(3) . . . . ? C8 N2 C9 C10 -90.8(10) . . . . ? C12 N2 C9 C10 90.0(10) . . . . ? N2 C9 C10 C11 168.5(10) . . . . ? C8 N2 C12 C13 86.3(10) . . . . ? C9 N2 C12 C13 -94.5(9) . . . . ? N2 C12 C13 C14 -167.2(11) . . . . ? Mo1 N3 C20 C25 95(2) . . . . ? Mo1 N3 C20 C21 -93(2) . . . . ? C25 C20 C21 C22 -9(2) . . . . ? N3 C20 C21 C22 177.8(13) . . . . ? C20 C21 C22 C23 12(3) . . . . ? C21 C22 C23 C24 -9(3) . . . . ? C21 C22 C23 C26 175.2(17) . . . . ? C22 C23 C24 C25 5(2) . . . . ? C26 C23 C24 C25 -179.1(14) . . . . ? C21 C20 C25 C24 6(2) . . . . ? N3 C20 C25 C24 178.9(11) . . . . ? C23 C24 C25 C20 -4(3) . . . . ? Mo2 N4 C30 C31 -22(5) . . . . ? Mo2 N4 C30 C35 157(4) . . . . ? C35 C30 C31 C32 -2.6(17) . . . . ? N4 C30 C31 C32 176.6(12) . . . . ? C30 C31 C32 C33 4(3) . . . . ? C31 C32 C33 C34 -4(2) . . . . ? C31 C32 C33 C36 -179.5(16) . . . . ? C32 C33 C34 C35 2.4(19) . . . . ? C36 C33 C34 C35 178.6(12) . . . . ? C31 C30 C35 C34 1.7(14) . . . . ? N4 C30 C35 C34 -177.4(8) . . . . ? C33 C34 C35 C30 -1.7(17) . . . . ? _diffrn_measured_fraction_theta_max 0.964 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.512 _refine_diff_density_min -0.356 _refine_diff_density_rms 0.076