# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_7mayc _database_code_depnum_ccdc_archive 'CCDC 781139' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H36 N, C14 H9 Mo N4 O S3' _chemical_formula_sum 'C30 H45 Mo N5 O S3' _chemical_formula_weight 683.83 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 Orthorhombic _symmetry_space_group_name_H-M Pca21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y, z+1/2' 'x+1/2, -y, z' _cell_length_a 21.844(5) _cell_length_b 9.699(5) _cell_length_c 16.066(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 90.000(5) _cell_angle_gamma 90.000(5) _cell_volume 3404(2) _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 'rectangular block' _exptl_crystal_colour blue _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.334 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1432 _exptl_absorpt_coefficient_mu 0.599 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.965 _exptl_absorpt_correction_T_max 0.988 _exptl_absorpt_process_details 'SADABS (Bruker, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD Area Detector' _diffrn_measurement_method /w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21170 _diffrn_reflns_av_R_equivalents 0.0746 _diffrn_reflns_av_sigmaI/netI 0.0735 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 28.35 _reflns_number_total 7845 _reflns_number_gt 6551 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART 5.628 (Bruker, 2003)' _computing_cell_refinement 'SAINT 6.45 ( Bruker, 2003)' _computing_data_reduction 'SAINT 6.45 ( Bruker, 2003)' _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 3.1e, Ortep' _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^)+(0.1341P)^2^+4.0552P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.06(7) _refine_ls_number_reflns 7845 _refine_ls_number_parameters 361 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0797 _refine_ls_R_factor_gt 0.0556 _refine_ls_wR_factor_ref 0.2120 _refine_ls_wR_factor_gt 0.1452 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.091 _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 0.91516(2) 0.01847(5) 0.33730(5) 0.02204(16) Uani 1 1 d . . . S1 S 0.82203(8) -0.03824(18) 0.41602(12) 0.0289(4) Uani 1 1 d . . . H1 H 0.8242 -0.1562 0.4383 0.043 Uiso 1 1 calc R . . S2 S 0.86030(7) 0.21870(17) 0.29188(12) 0.0288(3) Uani 1 1 d . . . S3 S 1.00600(6) 0.14725(15) 0.30134(11) 0.0233(3) Uani 1 1 d . . . O1 O 0.9138(2) -0.0923(5) 0.2568(3) 0.0290(11) Uani 1 1 d . . . N1 N 0.9428(2) 0.1023(6) 0.4667(3) 0.0248(11) Uani 1 1 d . . . N2 N 0.9592(3) -0.1465(5) 0.4093(4) 0.0274(12) Uani 1 1 d . . . N3 N 0.8795(4) 0.5564(8) 0.1843(5) 0.0477(18) Uani 1 1 d . . . N4 N 1.0596(3) 0.4723(6) 0.2032(5) 0.0370(15) Uani 1 1 d . . . N5 N 0.7249(2) -0.1783(6) 0.1785(4) 0.0270(12) Uani 1 1 d . . . C1 C 0.9168(3) 0.3282(8) 0.2520(5) 0.0291(15) Uani 1 1 d . . . C2 C 0.9780(3) 0.3006(7) 0.2557(4) 0.0267(13) Uani 1 1 d . . . C3 C 0.8966(4) 0.4563(7) 0.2150(5) 0.0343(16) Uani 1 1 d . . . C4 C 1.0216(3) 0.3971(7) 0.2268(4) 0.0292(14) Uani 1 1 d . . . C5 C 0.9360(3) 0.2339(7) 0.4895(4) 0.0277(13) Uani 1 1 d . . . H5 H 0.9169 0.2937 0.4525 0.033 Uiso 1 1 calc R . . C6 C 0.9554(3) 0.2853(8) 0.5635(4) 0.0307(15) Uani 1 1 d . . . H6 H 0.9502 0.3781 0.5761 0.037 Uiso 1 1 calc R . . C7 C 0.9828(3) 0.1971(9) 0.6200(5) 0.0351(17) Uani 1 1 d . . . H7 H 0.9966 0.2290 0.6713 0.042 Uiso 1 1 calc R . . C8 C 0.9893(3) 0.0590(8) 0.5976(4) 0.0271(13) Uani 1 1 d . . . H8 H 1.0069 -0.0030 0.6346 0.033 Uiso 1 1 calc R . . C9 C 0.9698(3) 0.0142(7) 0.5212(5) 0.0269(14) Uani 1 1 d . . . C10 C 0.9768(3) -0.1273(7) 0.4911(4) 0.0257(13) Uani 1 1 d . . . C11 C 1.0021(3) -0.2317(8) 0.5384(5) 0.0330(16) Uani 1 1 d . . . H11 H 1.0146 -0.2137 0.5926 0.040 Uiso 1 1 calc R . . C12 C 1.0090(4) -0.3626(8) 0.5057(6) 0.0414(18) Uani 1 1 d . . . H12 H 1.0261 -0.4335 0.5371 0.050 Uiso 1 1 calc R . . C13 C 0.9893(4) -0.3853(8) 0.4229(6) 0.0406(17) Uani 1 1 d . . . H13 H 0.9929 -0.4720 0.3987 0.049 Uiso 1 1 calc R . . C14 C 0.9646(3) -0.2759(7) 0.3784(5) 0.0300(14) Uani 1 1 d . . . H14 H 0.9510 -0.2923 0.3244 0.036 Uiso 1 1 calc R . . C15 C 0.7893(3) -0.1337(7) 0.1508(5) 0.0312(15) Uani 1 1 d . . . H15A H 0.8063 -0.0737 0.1932 0.037 Uiso 1 1 calc R . . H15B H 0.8151 -0.2150 0.1478 0.037 Uiso 1 1 calc R . . C16 C 0.7924(3) -0.0600(8) 0.0683(5) 0.0322(15) Uani 1 1 d . . . H16A H 0.7693 0.0252 0.0718 0.039 Uiso 1 1 calc R . . H16B H 0.7738 -0.1171 0.0258 0.039 Uiso 1 1 calc R . . C17 C 0.8578(4) -0.0278(9) 0.0439(6) 0.0413(19) Uani 1 1 d . . . H17A H 0.8759 0.0317 0.0857 0.050 Uiso 1 1 calc R . . H17B H 0.8812 -0.1128 0.0425 0.050 Uiso 1 1 calc R . . C18 C 0.8621(4) 0.0408(11) -0.0388(6) 0.050(2) Uani 1 1 d . . . H18A H 0.9042 0.0598 -0.0513 0.076 Uiso 1 1 calc R . . H18B H 0.8394 0.1256 -0.0376 0.076 Uiso 1 1 calc R . . H18C H 0.8454 -0.0188 -0.0807 0.076 Uiso 1 1 calc R . . C19 C 0.6821(3) -0.0528(8) 0.1812(5) 0.0299(14) Uani 1 1 d . . . H19A H 0.6759 -0.0198 0.1249 0.036 Uiso 1 1 calc R . . H19B H 0.6427 -0.0820 0.2027 0.036 Uiso 1 1 calc R . . C20 C 0.7054(3) 0.0664(7) 0.2343(5) 0.0334(15) Uani 1 1 d . . . H20A H 0.7156 0.0334 0.2896 0.040 Uiso 1 1 calc R . . H20B H 0.7422 0.1048 0.2096 0.040 Uiso 1 1 calc R . . C21 C 0.6562(3) 0.1772(8) 0.2401(6) 0.0373(17) Uani 1 1 d . . . H21A H 0.6204 0.1391 0.2672 0.045 Uiso 1 1 calc R . . H21B H 0.6445 0.2052 0.1844 0.045 Uiso 1 1 calc R . . C22 C 0.6783(4) 0.3046(8) 0.2890(7) 0.049(2) Uani 1 1 d . . . H22A H 0.6462 0.3721 0.2907 0.073 Uiso 1 1 calc R . . H22B H 0.7136 0.3432 0.2621 0.073 Uiso 1 1 calc R . . H22C H 0.6888 0.2778 0.3447 0.073 Uiso 1 1 calc R . . C23 C 0.7331(3) -0.2431(7) 0.2635(5) 0.0308(14) Uani 1 1 d . . . H23A H 0.7523 -0.1757 0.2997 0.037 Uiso 1 1 calc R . . H23B H 0.7613 -0.3200 0.2580 0.037 Uiso 1 1 calc R . . C24 C 0.6752(3) -0.2949(8) 0.3056(5) 0.0329(15) Uani 1 1 d . . . H24A H 0.6462 -0.2197 0.3111 0.040 Uiso 1 1 calc R . . H24B H 0.6564 -0.3661 0.2717 0.040 Uiso 1 1 calc R . . C25 C 0.6901(3) -0.3528(8) 0.3912(5) 0.0360(16) Uani 1 1 d . . . H25A H 0.7108 -0.2829 0.4240 0.043 Uiso 1 1 calc R . . H25B H 0.7176 -0.4307 0.3853 0.043 Uiso 1 1 calc R . . C26 C 0.6315(4) -0.3991(10) 0.4366(6) 0.046(2) Uani 1 1 d . . . H26A H 0.6420 -0.4358 0.4902 0.070 Uiso 1 1 calc R . . H26B H 0.6112 -0.4689 0.4044 0.070 Uiso 1 1 calc R . . H26C H 0.6046 -0.3216 0.4435 0.070 Uiso 1 1 calc R . . C27 C 0.6960(3) -0.2795(7) 0.1176(5) 0.0294(14) Uani 1 1 d . . . H27A H 0.6550 -0.3006 0.1370 0.035 Uiso 1 1 calc R . . H27B H 0.6921 -0.2342 0.0641 0.035 Uiso 1 1 calc R . . C28 C 0.7301(3) -0.4142(7) 0.1049(5) 0.0343(15) Uani 1 1 d . . . H28A H 0.7350 -0.4604 0.1581 0.041 Uiso 1 1 calc R . . H28B H 0.7705 -0.3953 0.0828 0.041 Uiso 1 1 calc R . . C29 C 0.6957(4) -0.5082(8) 0.0453(6) 0.042(2) Uani 1 1 d . . . H29A H 0.6903 -0.4611 -0.0075 0.051 Uiso 1 1 calc R . . H29B H 0.6553 -0.5273 0.0678 0.051 Uiso 1 1 calc R . . C30 C 0.7291(4) -0.6445(9) 0.0302(7) 0.051(2) Uani 1 1 d . . . H30A H 0.7059 -0.7001 -0.0078 0.077 Uiso 1 1 calc R . . H30B H 0.7337 -0.6927 0.0821 0.077 Uiso 1 1 calc R . . H30C H 0.7688 -0.6262 0.0070 0.077 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 0.0199(2) 0.0262(3) 0.0200(3) -0.0006(3) -0.0012(2) -0.00193(16) S1 0.0219(7) 0.0378(9) 0.0270(9) -0.0001(7) 0.0018(6) -0.0079(6) S2 0.0211(7) 0.0331(8) 0.0322(9) -0.0004(7) -0.0033(6) 0.0003(6) S3 0.0206(6) 0.0231(7) 0.0263(7) 0.0033(6) -0.0028(6) 0.0006(5) O1 0.030(2) 0.028(3) 0.029(3) 0.001(2) -0.0017(18) -0.0025(17) N1 0.020(2) 0.033(3) 0.022(3) 0.002(2) -0.0035(19) -0.004(2) N2 0.030(3) 0.025(3) 0.027(3) 0.002(2) 0.005(2) 0.004(2) N3 0.049(4) 0.034(4) 0.060(5) 0.008(3) -0.016(4) 0.006(3) N4 0.030(3) 0.037(3) 0.044(4) 0.022(3) -0.004(3) -0.004(2) N5 0.024(3) 0.025(3) 0.032(3) 0.000(2) -0.008(2) 0.000(2) C1 0.030(3) 0.034(4) 0.024(3) -0.003(3) 0.002(2) 0.000(2) C2 0.029(3) 0.025(3) 0.026(3) -0.004(3) -0.005(3) 0.005(2) C3 0.032(4) 0.029(4) 0.041(4) 0.004(3) -0.003(3) 0.004(3) C4 0.027(3) 0.029(3) 0.031(4) 0.004(3) -0.003(3) 0.007(2) C5 0.028(3) 0.031(3) 0.024(3) -0.003(3) 0.003(3) 0.004(3) C6 0.029(3) 0.034(4) 0.030(4) -0.009(3) -0.003(3) -0.001(3) C7 0.027(3) 0.048(4) 0.030(4) -0.016(3) 0.003(3) -0.001(3) C8 0.026(3) 0.042(4) 0.014(3) 0.001(3) -0.006(2) -0.001(3) C9 0.015(3) 0.032(3) 0.033(4) 0.001(3) 0.003(3) -0.002(2) C10 0.025(3) 0.037(4) 0.015(3) 0.003(3) -0.008(2) -0.005(2) C11 0.038(4) 0.034(4) 0.027(4) 0.011(3) -0.005(3) -0.005(3) C12 0.043(4) 0.037(4) 0.044(5) 0.010(4) 0.001(3) 0.003(3) C13 0.049(4) 0.032(4) 0.041(4) -0.001(3) 0.001(4) 0.002(3) C14 0.029(3) 0.028(3) 0.032(4) -0.005(3) -0.010(3) -0.002(2) C15 0.028(3) 0.029(3) 0.036(4) 0.000(3) 0.002(3) -0.004(2) C16 0.019(3) 0.041(4) 0.037(4) 0.002(3) -0.007(3) -0.002(3) C17 0.028(4) 0.052(5) 0.044(5) 0.001(4) -0.011(3) -0.009(3) C18 0.033(4) 0.077(7) 0.041(5) 0.007(5) 0.005(4) -0.014(4) C19 0.022(3) 0.031(3) 0.037(4) 0.000(3) -0.005(3) 0.001(3) C20 0.031(4) 0.030(3) 0.039(4) 0.000(3) -0.002(3) 0.006(3) C21 0.034(4) 0.030(4) 0.048(5) -0.003(3) 0.001(3) 0.006(3) C22 0.058(5) 0.028(4) 0.061(6) -0.005(4) -0.004(5) 0.010(3) C23 0.032(3) 0.024(3) 0.036(4) 0.002(3) -0.003(3) 0.005(2) C24 0.030(3) 0.032(3) 0.037(4) 0.002(3) -0.005(3) -0.001(3) C25 0.032(4) 0.034(4) 0.042(5) 0.006(3) 0.000(3) -0.004(3) C26 0.039(4) 0.055(5) 0.045(5) 0.008(4) 0.001(3) -0.004(4) C27 0.026(3) 0.032(3) 0.030(4) 0.001(3) -0.005(3) -0.006(2) C28 0.037(4) 0.030(3) 0.036(4) -0.004(3) -0.004(3) -0.005(3) C29 0.037(4) 0.042(4) 0.049(5) -0.020(4) -0.002(4) -0.013(3) C30 0.053(5) 0.041(4) 0.059(6) -0.021(4) 0.012(4) -0.010(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 O1 1.681(5) . ? Mo1 N2 2.196(6) . ? Mo1 N1 2.313(6) . ? Mo1 S2 2.3959(19) . ? Mo1 S3 2.4149(16) . ? Mo1 S1 2.4578(18) . ? S2 C1 1.750(7) . ? S3 C2 1.767(7) . ? N1 C5 1.336(9) . ? N1 C9 1.358(9) . ? N2 C14 1.355(8) . ? N2 C10 1.381(9) . ? N3 C3 1.152(10) . ? N4 C4 1.168(10) . ? N5 C23 1.514(9) . ? N5 C27 1.523(9) . ? N5 C19 1.535(9) . ? N5 C15 1.537(9) . ? C1 C2 1.363(9) . ? C1 C3 1.447(10) . ? C2 C4 1.414(10) . ? C5 C6 1.357(10) . ? C6 C7 1.383(11) . ? C7 C8 1.395(11) . ? C8 C9 1.369(10) . ? C9 C10 1.464(9) . ? C10 C11 1.381(9) . ? C11 C12 1.382(11) . ? C12 C13 1.415(13) . ? C13 C14 1.389(11) . ? C15 C16 1.507(11) . ? C16 C17 1.515(10) . ? C17 C18 1.488(13) . ? C19 C20 1.524(10) . ? C20 C21 1.523(10) . ? C21 C22 1.542(12) . ? C23 C24 1.521(10) . ? C24 C25 1.520(11) . ? C25 C26 1.541(11) . ? C27 C28 1.518(10) . ? C28 C29 1.522(10) . ? C29 C30 1.530(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 O1 Mo1 N2 87.0(2) . . ? O1 Mo1 N1 157.0(2) . . ? N2 Mo1 N1 70.6(2) . . ? O1 Mo1 S2 105.96(18) . . ? N2 Mo1 S2 165.94(16) . . ? N1 Mo1 S2 96.86(15) . . ? O1 Mo1 S3 99.26(17) . . ? N2 Mo1 S3 98.21(15) . . ? N1 Mo1 S3 79.57(14) . . ? S2 Mo1 S3 85.35(6) . . ? O1 Mo1 S1 103.78(16) . . ? N2 Mo1 S1 85.91(15) . . ? N1 Mo1 S1 80.33(14) . . ? S2 Mo1 S1 85.65(6) . . ? S3 Mo1 S1 156.79(7) . . ? C1 S2 Mo1 104.5(2) . . ? C2 S3 Mo1 104.5(2) . . ? C5 N1 C9 118.2(6) . . ? C5 N1 Mo1 123.6(4) . . ? C9 N1 Mo1 118.1(5) . . ? C14 N2 C10 116.7(6) . . ? C14 N2 Mo1 121.3(5) . . ? C10 N2 Mo1 121.7(4) . . ? C23 N5 C27 111.1(5) . . ? C23 N5 C19 112.0(5) . . ? C27 N5 C19 106.1(5) . . ? C23 N5 C15 105.6(5) . . ? C27 N5 C15 112.0(5) . . ? C19 N5 C15 110.0(5) . . ? C2 C1 C3 119.0(7) . . ? C2 C1 S2 123.8(6) . . ? C3 C1 S2 117.1(5) . . ? C1 C2 C4 121.0(6) . . ? C1 C2 S3 121.5(6) . . ? C4 C2 S3 117.4(5) . . ? N3 C3 C1 178.2(9) . . ? N4 C4 C2 177.0(7) . . ? N1 C5 C6 123.8(7) . . ? C5 C6 C7 118.9(7) . . ? C6 C7 C8 117.9(7) . . ? C9 C8 C7 120.3(7) . . ? N1 C9 C8 120.9(6) . . ? N1 C9 C10 115.0(6) . . ? C8 C9 C10 124.2(7) . . ? C11 C10 N2 122.4(6) . . ? C11 C10 C9 123.2(6) . . ? N2 C10 C9 114.3(6) . . ? C10 C11 C12 120.6(7) . . ? C11 C12 C13 117.8(7) . . ? C14 C13 C12 118.9(7) . . ? N2 C14 C13 123.5(7) . . ? C16 C15 N5 115.4(6) . . ? C15 C16 C17 111.6(6) . . ? C18 C17 C16 112.5(7) . . ? C20 C19 N5 114.5(5) . . ? C21 C20 C19 109.5(6) . . ? C20 C21 C22 112.1(7) . . ? N5 C23 C24 116.1(6) . . ? C25 C24 C23 110.2(6) . . ? C24 C25 C26 111.0(6) . . ? C28 C27 N5 116.0(5) . . ? C27 C28 C29 111.0(6) . . ? C28 C29 C30 112.4(8) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 28.35 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.803 _refine_diff_density_min -1.563 _refine_diff_density_rms 0.198 data_21maya _database_code_depnum_ccdc_archive 'CCDC 781140' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H36 N, C16 H9 Mo N4 O S3' _chemical_formula_sum 'C32 H45 Mo N5 O S3' _chemical_formula_weight 707.88 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 P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.381(5) _cell_length_b 8.671(5) _cell_length_c 25.304(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 106.757(5) _cell_angle_gamma 90.000(5) _cell_volume 3442(2) _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 'rectangular block' _exptl_crystal_colour blue _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.366 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1480 _exptl_absorpt_coefficient_mu 0.595 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.986 _exptl_absorpt_correction_T_max 0.988 _exptl_absorpt_process_details 'SADABS (Bruker, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD Area Detector' _diffrn_measurement_method /w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20195 _diffrn_reflns_av_R_equivalents 0.0949 _diffrn_reflns_av_sigmaI/netI 0.1255 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.40 _diffrn_reflns_theta_max 27.75 _reflns_number_total 8065 _reflns_number_gt 4507 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART 5.628 (Bruker, 2003)' _computing_cell_refinement 'SAINT 6.45 ( Bruker, 2003)' _computing_data_reduction 'SAINT 6.45 ( Bruker, 2003)' _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 3.1e, Ortep' _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^)+(0.1532P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8065 _refine_ls_number_parameters 388 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1411 _refine_ls_R_factor_gt 0.0719 _refine_ls_wR_factor_ref 0.2667 _refine_ls_wR_factor_gt 0.1852 _refine_ls_goodness_of_fit_ref 0.998 _refine_ls_restrained_S_all 1.000 _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 0.71865(4) 0.33821(7) 0.97834(2) 0.0311(2) Uani 1 1 d . . . S1 S 0.68163(11) 0.3959(2) 1.06100(7) 0.0333(4) Uani 1 1 d . . . S2 S 0.86238(11) 0.3396(2) 1.03692(8) 0.0415(5) Uani 1 1 d . . . S3 S 0.77351(12) 0.1904(2) 0.91307(8) 0.0377(4) Uani 1 1 d . . . H3 H 0.8375 0.2499 0.9089 0.057 Uiso 1 1 calc R . . O1 O 0.7024(3) 0.5102(5) 0.94704(19) 0.0369(11) Uani 1 1 d . . . N1 N 0.7664(4) 0.6046(9) 1.1925(3) 0.0541(18) Uani 1 1 d . . . N2 N 0.9953(4) 0.5299(9) 1.1655(3) 0.0517(17) Uani 1 1 d . . . N3 N 0.6878(4) 0.0879(7) 0.9976(2) 0.0364(13) Uani 1 1 d . . . N4 N 0.5865(3) 0.2831(7) 0.9303(2) 0.0304(12) Uani 1 1 d . . . N5 N 0.8109(3) 0.7506(6) 0.8480(2) 0.0302(12) Uani 1 1 d . . . C1 C 0.7784(4) 0.4570(8) 1.1067(3) 0.0345(16) Uani 1 1 d . . . C2 C 0.8547(4) 0.4302(9) 1.0971(3) 0.0383(16) Uani 1 1 d . . . C3 C 0.7742(4) 0.5371(9) 1.1554(3) 0.0377(16) Uani 1 1 d . . . C4 C 0.9323(5) 0.4851(10) 1.1355(3) 0.0451(19) Uani 1 1 d . . . C5 C 0.7415(5) -0.0077(9) 1.0322(3) 0.0454(19) Uani 1 1 d . . . H5 H 0.7944 0.0289 1.0529 0.055 Uiso 1 1 calc R . . C6 C 0.7198(6) -0.1626(9) 1.0381(4) 0.058(2) Uani 1 1 d . . . H6 H 0.7586 -0.2266 1.0624 0.069 Uiso 1 1 calc R . . C7 C 0.6437(6) -0.2191(9) 1.0088(4) 0.052(2) Uani 1 1 d . . . H7 H 0.6298 -0.3219 1.0122 0.063 Uiso 1 1 calc R . . C8 C 0.5863(5) -0.1210(8) 0.9735(3) 0.045(2) Uani 1 1 d . . . C9 C 0.6110(5) 0.0323(8) 0.9685(3) 0.0364(17) Uani 1 1 d . . . C10 C 0.5018(6) -0.1661(9) 0.9419(4) 0.054(2) Uani 1 1 d . . . H10 H 0.4841 -0.2671 0.9441 0.065 Uiso 1 1 calc R . . C11 C 0.4484(6) -0.0660(10) 0.9095(4) 0.054(2) Uani 1 1 d . . . H11 H 0.3935 -0.0984 0.8908 0.065 Uiso 1 1 calc R . . C12 C 0.4727(5) 0.0909(9) 0.9024(3) 0.0430(18) Uani 1 1 d . . . C13 C 0.5552(4) 0.1375(8) 0.9329(3) 0.0353(16) Uani 1 1 d . . . C14 C 0.4203(5) 0.2035(11) 0.8696(3) 0.049(2) Uani 1 1 d . . . H14 H 0.3648 0.1786 0.8493 0.059 Uiso 1 1 calc R . . C15 C 0.4501(5) 0.3483(10) 0.8672(3) 0.0471(19) Uani 1 1 d . . . H15 H 0.4155 0.4231 0.8454 0.057 Uiso 1 1 calc R . . C16 C 0.5337(4) 0.3839(9) 0.8980(3) 0.0368(16) Uani 1 1 d . . . H16 H 0.5535 0.4835 0.8958 0.044 Uiso 1 1 calc R . . C17 C 0.8646(4) 0.6858(8) 0.9026(3) 0.0367(16) Uani 1 1 d . . . H17A H 0.8329 0.6030 0.9133 0.044 Uiso 1 1 calc R . . H17B H 0.9157 0.6410 0.8970 0.044 Uiso 1 1 calc R . . C18 C 0.8910(5) 0.7985(10) 0.9499(3) 0.051(2) Uani 1 1 d . . . H18A H 0.9306 0.8724 0.9423 0.061 Uiso 1 1 calc R . . H18B H 0.8412 0.8547 0.9526 0.061 Uiso 1 1 calc R . . C19 C 0.9315(5) 0.7221(11) 1.0032(3) 0.053(2) Uani 1 1 d . . . H19A H 0.9745 0.6517 0.9979 0.064 Uiso 1 1 calc R . . H19B H 0.8885 0.6604 1.0128 0.064 Uiso 1 1 calc R . . C20 C 0.9723(7) 0.8232(10) 1.0509(4) 0.064(3) Uani 1 1 d . . . H20A H 0.9962 0.7608 1.0830 0.095 Uiso 1 1 calc R . . H20B H 0.9304 0.8915 1.0577 0.095 Uiso 1 1 calc R . . H20C H 1.0167 0.8826 1.0428 0.095 Uiso 1 1 calc R . . C21 C 0.8546(4) 0.8960(9) 0.8321(3) 0.0374(16) Uani 1 1 d . . . H21A H 0.8194 0.9331 0.7967 0.045 Uiso 1 1 calc R . . H21B H 0.8554 0.9760 0.8591 0.045 Uiso 1 1 calc R . . C22 C 0.9449(5) 0.8757(9) 0.8284(3) 0.0426(18) Uani 1 1 d . . . H22A H 0.9829 0.8519 0.8646 0.051 Uiso 1 1 calc R . . H22B H 0.9467 0.7905 0.8039 0.051 Uiso 1 1 calc R . . C23 C 0.9738(5) 1.0204(10) 0.8070(3) 0.0453(19) Uani 1 1 d . . . H23A H 0.9639 1.1071 0.8286 0.054 Uiso 1 1 calc R . . H23B H 0.9397 1.0363 0.7691 0.054 Uiso 1 1 calc R . . C24 C 1.0667(5) 1.0177(13) 0.8090(4) 0.068(3) Uani 1 1 d . . . H24A H 1.0814 1.1132 0.7950 0.102 Uiso 1 1 calc R . . H24B H 1.0767 0.9338 0.7869 0.102 Uiso 1 1 calc R . . H24C H 1.1010 1.0042 0.8465 0.102 Uiso 1 1 calc R . . C25 C 0.7248(4) 0.7993(8) 0.8529(3) 0.0374(16) Uani 1 1 d . . . H25A H 0.7005 0.7126 0.8674 0.045 Uiso 1 1 calc R . . H25B H 0.7338 0.8813 0.8801 0.045 Uiso 1 1 calc R . . C26 C 0.6599(5) 0.8540(10) 0.8015(3) 0.0456(19) Uani 1 1 d . . . H26A H 0.6843 0.9357 0.7847 0.055 Uiso 1 1 calc R . . H26B H 0.6446 0.7696 0.7753 0.055 Uiso 1 1 calc R . . C27 C 0.5813(5) 0.9127(12) 0.8140(3) 0.056(2) Uani 1 1 d . . . H27A H 0.5979 0.9913 0.8423 0.067 Uiso 1 1 calc R . . H27B H 0.5557 0.8285 0.8288 0.067 Uiso 1 1 calc R . . C28 C 0.5154(5) 0.9793(13) 0.7651(4) 0.068(3) Uani 1 1 d . . . H28A H 0.4675 1.0148 0.7764 0.102 Uiso 1 1 calc R . . H28B H 0.4970 0.9015 0.7372 0.102 Uiso 1 1 calc R . . H28C H 0.5396 1.0643 0.7505 0.102 Uiso 1 1 calc R . . C29 C 0.8021(5) 0.6312(8) 0.8027(3) 0.0384(17) Uani 1 1 d . . . H29A H 0.7770 0.6808 0.7674 0.046 Uiso 1 1 calc R . . H29B H 0.8586 0.5966 0.8033 0.046 Uiso 1 1 calc R . . C30 C 0.7498(5) 0.4935(9) 0.8065(4) 0.051(2) Uani 1 1 d . B . H30A H 0.6904 0.5236 0.7987 0.061 Uiso 1 1 calc R . . H30B H 0.7682 0.4525 0.8437 0.061 Uiso 1 1 calc R . . C31 C 0.7580(6) 0.3693(12) 0.7659(5) 0.086(4) Uani 1 1 d D . . H31A H 0.7584 0.4205 0.7319 0.103 Uiso 1 1 calc R A 1 H31B H 0.8134 0.3215 0.7807 0.103 Uiso 1 1 calc R A 1 C32A C 0.6977(10) 0.2510(17) 0.7521(7) 0.071(5) Uani 0.60 1 d P B 1 H32A H 0.7114 0.1832 0.7259 0.107 Uiso 0.60 1 calc PR B 1 H32B H 0.6421 0.2945 0.7362 0.107 Uiso 0.60 1 calc PR B 1 H32C H 0.6981 0.1940 0.7847 0.107 Uiso 0.60 1 calc PR B 1 C32B C 0.7187(14) 0.373(3) 0.7094(7) 0.073(8) Uani 0.40 1 d PD B 2 H32D H 0.7340 0.2821 0.6927 0.109 Uiso 0.40 1 calc PR B 2 H32E H 0.7370 0.4628 0.6939 0.109 Uiso 0.40 1 calc PR B 2 H32F H 0.6580 0.3760 0.7026 0.109 Uiso 0.40 1 calc PR B 2 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 0.0370(4) 0.0234(3) 0.0366(4) 0.0011(2) 0.0164(3) 0.0016(2) S1 0.0342(9) 0.0305(9) 0.0376(9) 0.0013(7) 0.0140(7) 0.0026(7) S2 0.0370(10) 0.0465(12) 0.0448(11) -0.0032(9) 0.0176(8) 0.0032(8) S3 0.0494(11) 0.0297(10) 0.0421(10) -0.0029(7) 0.0261(8) 0.0056(8) O1 0.049(3) 0.028(3) 0.038(3) -0.005(2) 0.019(2) 0.002(2) N1 0.048(4) 0.073(5) 0.039(4) -0.010(3) 0.010(3) 0.005(4) N2 0.040(4) 0.064(5) 0.049(4) -0.007(3) 0.010(3) 0.006(3) N3 0.045(3) 0.024(3) 0.047(3) 0.002(3) 0.023(3) 0.002(3) N4 0.035(3) 0.026(3) 0.036(3) -0.002(2) 0.020(2) 0.002(2) N5 0.030(3) 0.028(3) 0.034(3) -0.004(2) 0.011(2) -0.001(2) C1 0.044(4) 0.034(4) 0.029(3) 0.004(3) 0.015(3) 0.007(3) C2 0.033(4) 0.035(4) 0.043(4) 0.007(3) 0.007(3) 0.004(3) C3 0.035(4) 0.043(5) 0.034(4) 0.003(3) 0.010(3) 0.001(3) C4 0.044(5) 0.046(5) 0.050(5) 0.004(4) 0.021(4) 0.015(4) C5 0.052(5) 0.048(5) 0.046(4) 0.010(4) 0.030(4) 0.019(4) C6 0.092(7) 0.027(4) 0.072(6) 0.021(4) 0.052(5) 0.025(5) C7 0.076(6) 0.024(4) 0.074(6) 0.005(4) 0.049(5) -0.002(4) C8 0.069(5) 0.025(4) 0.060(5) -0.007(4) 0.048(4) -0.010(4) C9 0.056(4) 0.024(4) 0.046(4) -0.001(3) 0.040(4) -0.003(3) C10 0.080(6) 0.028(4) 0.075(6) -0.015(4) 0.053(5) -0.008(4) C11 0.057(5) 0.052(5) 0.073(6) -0.024(5) 0.048(5) -0.018(4) C12 0.046(4) 0.041(5) 0.052(5) -0.012(4) 0.030(4) -0.003(4) C13 0.044(4) 0.025(4) 0.047(4) -0.008(3) 0.029(3) -0.006(3) C14 0.042(4) 0.070(6) 0.042(4) -0.011(4) 0.023(4) -0.002(4) C15 0.055(5) 0.050(5) 0.044(4) 0.000(4) 0.027(4) 0.007(4) C16 0.038(4) 0.033(4) 0.043(4) -0.003(3) 0.019(3) 0.002(3) C17 0.040(4) 0.029(4) 0.042(4) 0.001(3) 0.015(3) -0.002(3) C18 0.059(5) 0.049(5) 0.038(4) 0.003(4) 0.003(4) -0.002(4) C19 0.055(5) 0.063(6) 0.041(4) 0.001(4) 0.012(4) 0.019(4) C20 0.088(7) 0.052(6) 0.047(5) -0.003(4) 0.013(5) -0.005(5) C21 0.039(4) 0.039(4) 0.036(4) 0.002(3) 0.013(3) 0.002(3) C22 0.041(4) 0.048(5) 0.041(4) -0.005(3) 0.016(3) -0.003(3) C23 0.047(4) 0.054(5) 0.038(4) 0.001(4) 0.017(3) -0.016(4) C24 0.051(5) 0.112(9) 0.045(5) 0.000(5) 0.019(4) -0.027(5) C25 0.041(4) 0.028(4) 0.047(4) -0.002(3) 0.019(3) 0.002(3) C26 0.037(4) 0.055(5) 0.045(4) -0.007(4) 0.013(3) 0.001(4) C27 0.039(4) 0.082(7) 0.048(5) -0.005(4) 0.016(4) 0.012(4) C28 0.052(5) 0.095(8) 0.062(6) 0.003(5) 0.023(5) 0.024(5) C29 0.042(4) 0.039(4) 0.037(4) -0.006(3) 0.016(3) 0.005(3) C30 0.050(5) 0.037(5) 0.071(6) -0.014(4) 0.026(4) -0.007(4) C31 0.067(6) 0.073(7) 0.130(11) -0.060(7) 0.047(7) -0.018(5) C32A 0.084(11) 0.038(9) 0.101(13) -0.020(9) 0.041(10) -0.020(8) C32B 0.054(13) 0.13(2) 0.030(11) 0.000(12) -0.001(10) 0.012(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 O1 1.673(5) . ? Mo1 N4 2.208(5) . ? Mo1 N3 2.312(6) . ? Mo1 S1 2.3924(18) . ? Mo1 S2 2.393(2) . ? Mo1 S3 2.4564(18) . ? S1 C1 1.753(7) . ? S2 C2 1.751(8) . ? N1 C3 1.142(9) . ? N2 C4 1.157(9) . ? N3 C5 1.336(9) . ? N3 C9 1.350(9) . ? N4 C16 1.331(9) . ? N4 C13 1.371(8) . ? N5 C25 1.513(8) . ? N5 C17 1.517(8) . ? N5 C29 1.520(8) . ? N5 C21 1.559(9) . ? C1 C2 1.359(9) . ? C1 C3 1.435(10) . ? C2 C4 1.440(11) . ? C5 C6 1.408(11) . ? C6 C7 1.346(12) . ? C7 C8 1.385(12) . ? C8 C9 1.405(10) . ? C8 C10 1.440(12) . ? C9 C13 1.417(10) . ? C10 C11 1.333(12) . ? C11 C12 1.443(11) . ? C12 C14 1.404(12) . ? C12 C13 1.408(10) . ? C14 C15 1.355(11) . ? C15 C16 1.402(11) . ? C17 C18 1.507(10) . ? C18 C19 1.477(10) . ? C19 C20 1.486(11) . ? C21 C22 1.519(9) . ? C22 C23 1.496(10) . ? C23 C24 1.507(10) . ? C25 C26 1.501(10) . ? C26 C27 1.501(10) . ? C27 C28 1.503(11) . ? C29 C30 1.489(11) . ? C30 C31 1.520(12) . ? C31 C32B 1.389(15) . ? C31 C32A 1.397(16) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Mo1 N4 86.3(2) . . ? O1 Mo1 N3 157.2(2) . . ? N4 Mo1 N3 70.9(2) . . ? O1 Mo1 S1 100.48(16) . . ? N4 Mo1 S1 94.04(14) . . ? N3 Mo1 S1 83.49(15) . . ? O1 Mo1 S2 106.40(17) . . ? N4 Mo1 S2 167.23(16) . . ? N3 Mo1 S2 96.30(16) . . ? S1 Mo1 S2 84.81(6) . . ? O1 Mo1 S3 100.70(16) . . ? N4 Mo1 S3 90.46(14) . . ? N3 Mo1 S3 78.22(15) . . ? S1 Mo1 S3 158.58(7) . . ? S2 Mo1 S3 86.20(7) . . ? C1 S1 Mo1 103.3(2) . . ? C2 S2 Mo1 103.7(2) . . ? C5 N3 C9 118.0(7) . . ? C5 N3 Mo1 125.3(5) . . ? C9 N3 Mo1 116.5(4) . . ? C16 N4 C13 116.6(6) . . ? C16 N4 Mo1 123.8(5) . . ? C13 N4 Mo1 119.6(5) . . ? C25 N5 C17 109.7(5) . . ? C25 N5 C29 111.4(5) . . ? C17 N5 C29 109.9(5) . . ? C25 N5 C21 107.7(5) . . ? C17 N5 C21 110.2(5) . . ? C29 N5 C21 108.0(5) . . ? C2 C1 C3 120.7(7) . . ? C2 C1 S1 122.3(5) . . ? C3 C1 S1 117.0(5) . . ? C1 C2 C4 120.2(7) . . ? C1 C2 S2 122.1(5) . . ? C4 C2 S2 117.6(5) . . ? N1 C3 C1 176.0(8) . . ? N2 C4 C2 178.7(8) . . ? N3 C5 C6 121.5(8) . . ? C7 C6 C5 120.7(8) . . ? C6 C7 C8 118.7(8) . . ? C7 C8 C9 118.7(8) . . ? C7 C8 C10 123.8(7) . . ? C9 C8 C10 117.5(8) . . ? N3 C9 C8 122.4(7) . . ? N3 C9 C13 116.5(6) . . ? C8 C9 C13 121.1(7) . . ? C11 C10 C8 121.4(8) . . ? C10 C11 C12 122.3(8) . . ? C14 C12 C13 116.8(7) . . ? C14 C12 C11 125.9(8) . . ? C13 C12 C11 117.3(8) . . ? N4 C13 C12 123.5(7) . . ? N4 C13 C9 116.2(6) . . ? C12 C13 C9 120.3(7) . . ? C15 C14 C12 120.3(8) . . ? C14 C15 C16 119.1(8) . . ? N4 C16 C15 123.7(7) . . ? C18 C17 N5 116.2(6) . . ? C19 C18 C17 112.6(7) . . ? C18 C19 C20 117.1(8) . . ? C22 C21 N5 116.7(6) . . ? C23 C22 C21 109.9(6) . . ? C22 C23 C24 113.3(7) . . ? C26 C25 N5 117.4(6) . . ? C27 C26 C25 111.1(6) . . ? C26 C27 C28 114.4(7) . . ? C30 C29 N5 115.4(6) . . ? C29 C30 C31 111.1(7) . . ? C32B C31 C32A 71.0(14) . . ? C32B C31 C30 125.1(15) . . ? C32A C31 C30 119.7(10) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.75 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.006 _refine_diff_density_min -2.262 _refine_diff_density_rms 0.235 data_bp4Me _database_code_depnum_ccdc_archive 'CCDC 890843' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H36 N, C21 H15 Mo N4 O S3' _chemical_formula_sum 'C37 H51 Mo N5 O S3 ' _chemical_formula_weight 773.96 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Tricilinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.436(5) _cell_length_b 11.629(5) _cell_length_c 19.400(5) _cell_angle_alpha 79.233(5) _cell_angle_beta 75.964(5) _cell_angle_gamma 83.538(5) _cell_volume 2023.8(15) _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 blue _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.270 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 812 _exptl_absorpt_coefficient_mu 0.508 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method /w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12103 _diffrn_reflns_av_R_equivalents 0.0316 _diffrn_reflns_av_sigmaI/netI 0.0752 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.23 _diffrn_reflns_theta_max 27.00 _reflns_number_total 8826 _reflns_number_gt 5748 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART 5.628 (Bruker, 2003)' _computing_cell_refinement 'SAINT 6.45 ( Bruker, 2003)' _computing_data_reduction 'SAINT 6.45 ( Bruker, 2003)' _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 3.1e, Ortep' _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^)+(0.1367P)^2^+4.6288P] 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 8523 _refine_ls_number_parameters 473 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1054 _refine_ls_R_factor_gt 0.0686 _refine_ls_wR_factor_ref 0.2308 _refine_ls_wR_factor_gt 0.1808 _refine_ls_goodness_of_fit_ref 0.960 _refine_ls_restrained_S_all 0.960 _refine_ls_shift/su_max 0.005 _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 0.03367(5) 0.98857(4) 0.28492(3) 0.03798(19) Uani 1 1 d . . . S1 S 0.12357(16) 0.92095(13) 0.17218(8) 0.0409(4) Uani 1 1 d . . . S2 S 0.14749(15) 0.80362(12) 0.33420(8) 0.0374(3) Uani 1 1 d . . . S3 S -0.13155(17) 1.11672(14) 0.22134(10) 0.0532(4) Uani 1 1 d . . . O1 O 0.1573(4) 1.0800(3) 0.2891(2) 0.0453(10) Uani 1 1 d . . . N1 N -0.0879(5) 1.0283(4) 0.3911(3) 0.0403(11) Uani 1 1 d . . . N2 N -0.1722(5) 0.8836(4) 0.3254(3) 0.0430(12) Uani 1 1 d . . . N3 N 0.3795(6) 0.6931(5) 0.0844(3) 0.0497(13) Uani 1 1 d . . . N4 N 0.4228(6) 0.5634(5) 0.2838(3) 0.0501(13) Uani 1 1 d . . . N5 N 0.3468(5) 0.2916(4) 0.1169(2) 0.0316(9) Uani 1 1 d . . . C1 C 0.2392(6) 0.7936(5) 0.1910(3) 0.0383(13) Uani 1 1 d . . . C2 C 0.2496(6) 0.7472(5) 0.2587(3) 0.0353(12) Uani 1 1 d . . . C3 C 0.3458(6) 0.6453(5) 0.2723(3) 0.0363(12) Uani 1 1 d . . . C4 C 0.3169(6) 0.7396(5) 0.1327(3) 0.0403(13) Uani 1 1 d . . . C5 C -0.2892(7) 1.1620(6) 0.2841(4) 0.059(2) Uani 1 1 d . . . C6 C -0.2880(7) 1.2535(6) 0.3204(5) 0.066(2) Uani 1 1 d . . . H6 H -0.1996 1.2850 0.3167 0.079 Uiso 1 1 calc R . . C7 C -0.4140(7) 1.2994(7) 0.3618(5) 0.077(3) Uani 1 1 d . . . H7 H -0.4114 1.3621 0.3849 0.093 Uiso 1 1 calc R . . C8 C -0.5466(8) 1.2495(8) 0.3684(6) 0.086(3) Uani 1 1 d . . . C9 C -0.5492(8) 1.1556(8) 0.3364(5) 0.071(3) Uani 1 1 d . . . H9 H -0.6362 1.1203 0.3427 0.086 Uiso 1 1 calc R . . C10 C -0.4202(7) 1.1128(7) 0.2940(4) 0.065(2) Uani 1 1 d . . . H10 H -0.4225 1.0490 0.2718 0.079 Uiso 1 1 calc R . . C11 C -0.6859(9) 1.3077(9) 0.4107(6) 0.111(4) Uani 1 1 d . . . H11A H -0.6612 1.3730 0.4282 0.167 Uiso 1 1 calc R . . H11B H -0.7315 1.2517 0.4506 0.167 Uiso 1 1 calc R . . H11C H -0.7524 1.3348 0.3797 0.167 Uiso 1 1 calc R . . C12 C -0.0435(6) 1.1082(5) 0.4224(3) 0.0400(13) Uani 1 1 d . . . H12 H 0.0398 1.1467 0.3977 0.048 Uiso 1 1 calc R . . C13 C -0.1130(6) 1.1352(5) 0.4877(4) 0.0437(14) Uani 1 1 d . . . H13 H -0.0787 1.1915 0.5067 0.052 Uiso 1 1 calc R . . C14 C -0.2357(7) 1.0779(6) 0.5256(4) 0.0513(16) Uani 1 1 d . . . H14 H -0.2842 1.0932 0.5711 0.062 Uiso 1 1 calc R . . C15 C -0.2847(6) 0.9977(6) 0.4947(4) 0.0484(16) Uani 1 1 d . . . H15 H -0.3674 0.9583 0.5193 0.058 Uiso 1 1 calc R . . C16 C -0.2127(6) 0.9754(5) 0.4279(3) 0.0430(14) Uani 1 1 d . . . C17 C -0.2599(6) 0.8934(5) 0.3898(4) 0.0442(14) Uani 1 1 d . . . C18 C -0.3856(7) 0.8321(6) 0.4173(4) 0.0573(19) Uani 1 1 d . . . H18 H -0.4429 0.8390 0.4628 0.069 Uiso 1 1 calc R . . C19 C -0.4237(7) 0.7617(6) 0.3765(4) 0.0597(19) Uani 1 1 d . . . H19 H -0.5074 0.7203 0.3936 0.072 Uiso 1 1 calc R . . C20 C -0.3341(7) 0.7535(6) 0.3088(5) 0.062(2) Uani 1 1 d . . . H20 H -0.3580 0.7066 0.2799 0.074 Uiso 1 1 calc R . . C21 C -0.2104(7) 0.8148(6) 0.2848(4) 0.0545(17) Uani 1 1 d . . . H21 H -0.1514 0.8089 0.2394 0.065 Uiso 1 1 calc R . . C22 C 0.4043(6) 0.1642(4) 0.1349(3) 0.0318(11) Uani 1 1 d . . . H22A H 0.4346 0.1544 0.1801 0.038 Uiso 1 1 calc R . . H22B H 0.3242 0.1145 0.1424 0.038 Uiso 1 1 calc R . . C23 C 0.5302(7) 0.1215(5) 0.0794(5) 0.064(2) Uani 1 1 d . B . H23A H 0.6192 0.1546 0.0805 0.076 Uiso 1 1 calc R . . H23B H 0.5111 0.1464 0.0317 0.076 Uiso 1 1 calc R . . C24 C 0.5490(9) -0.0125(6) 0.0956(7) 0.099(4) Uani 1 1 d . . . H24A H 0.4933 -0.0436 0.0682 0.118 Uiso 1 1 calc R A 1 H24B H 0.5056 -0.0373 0.1462 0.118 Uiso 1 1 calc R A 1 C25A C 0.7056(15) -0.0689(11) 0.0795(8) 0.054(3) Uani 0.50 1 d P B 1 H25A H 0.7036 -0.1526 0.0917 0.080 Uiso 0.50 1 calc PR B 1 H25B H 0.7619 -0.0416 0.1076 0.080 Uiso 0.50 1 calc PR B 1 H25C H 0.7496 -0.0477 0.0292 0.080 Uiso 0.50 1 calc PR B 1 C25B C 0.5847(14) -0.0672(11) 0.1492(7) 0.043(3) Uani 0.50 1 d P B 2 H25D H 0.5892 -0.1497 0.1482 0.065 Uiso 0.50 1 calc PR B 2 H25E H 0.5140 -0.0492 0.1913 0.065 Uiso 0.50 1 calc PR B 2 H25F H 0.6792 -0.0458 0.1506 0.065 Uiso 0.50 1 calc PR B 2 C26 C 0.4698(5) 0.3744(4) 0.0967(3) 0.0282(10) Uani 1 1 d . . . H26A H 0.5392 0.3538 0.0542 0.034 Uiso 1 1 calc R . . H26B H 0.4287 0.4536 0.0837 0.034 Uiso 1 1 calc R . . C27 C 0.5518(7) 0.3744(5) 0.1542(3) 0.0472(15) Uani 1 1 d . D . H27A H 0.5947 0.2961 0.1676 0.057 Uiso 1 1 calc R . . H27B H 0.4850 0.3976 0.1966 0.057 Uiso 1 1 calc R . . C28 C 0.6733(7) 0.4610(5) 0.1252(4) 0.0481(15) Uani 1 1 d . . . H28A H 0.7255 0.4440 0.0782 0.058 Uiso 1 1 calc R C 1 H28B H 0.6250 0.5389 0.1173 0.058 Uiso 1 1 calc R C 1 C29A C 0.7821(14) 0.4679(11) 0.1648(7) 0.048(3) Uani 0.50 1 d P D 1 H29A H 0.8477 0.5267 0.1386 0.073 Uiso 0.50 1 calc PR D 1 H29B H 0.8364 0.3933 0.1713 0.073 Uiso 0.50 1 calc PR D 1 H29C H 0.7348 0.4884 0.2111 0.073 Uiso 0.50 1 calc PR D 1 C29B C 0.7974(11) 0.4083(10) 0.0838(6) 0.038(2) Uani 0.50 1 d P D 2 H29D H 0.8712 0.4637 0.0657 0.057 Uiso 0.50 1 calc PR D 2 H29E H 0.7716 0.3837 0.0441 0.057 Uiso 0.50 1 calc PR D 2 H29F H 0.8344 0.3414 0.1131 0.057 Uiso 0.50 1 calc PR D 2 C30 C 0.2798(8) 0.3087(6) 0.0527(4) 0.0563(19) Uani 1 1 d . F . H30A H 0.3559 0.2939 0.0111 0.068 Uiso 1 1 calc R . . H30B H 0.2432 0.3902 0.0434 0.068 Uiso 1 1 calc R . . C31 C 0.1550(9) 0.2310(7) 0.0602(5) 0.079(3) Uani 1 1 d . . . H31A H 0.1031 0.2137 0.1102 0.094 Uiso 1 1 calc R E 1 H31B H 0.1933 0.1575 0.0436 0.094 Uiso 1 1 calc R E 1 C32A C 0.0495(12) 0.2991(10) 0.0135(6) 0.036(2) Uani 0.50 1 d P F 1 H32A H 0.0080 0.3705 0.0319 0.043 Uiso 0.50 1 calc PR F 1 H32B H 0.1037 0.3207 -0.0358 0.043 Uiso 0.50 1 calc PR F 1 C33A C -0.0732(14) 0.2229(12) 0.0151(7) 0.051(3) Uani 0.50 1 d P F 1 H33A H -0.1372 0.2655 -0.0139 0.076 Uiso 0.50 1 calc PR F 1 H33B H -0.1277 0.2027 0.0639 0.076 Uiso 0.50 1 calc PR F 1 H33C H -0.0319 0.1526 -0.0035 0.076 Uiso 0.50 1 calc PR F 1 C32B C 0.1168(11) 0.2465(10) -0.0205(6) 0.034(2) Uani 0.50 1 d P F 2 H32C H 0.0763 0.3258 -0.0333 0.041 Uiso 0.50 1 calc PR F 2 H32D H 0.2063 0.2339 -0.0562 0.041 Uiso 0.50 1 calc PR F 2 C33B C 0.0085(15) 0.1602(12) -0.0211(8) 0.053(3) Uani 0.50 1 d P F 2 H33D H -0.0127 0.1717 -0.0680 0.079 Uiso 0.50 1 calc PR F 2 H33E H -0.0802 0.1727 0.0141 0.079 Uiso 0.50 1 calc PR F 2 H33F H 0.0497 0.0816 -0.0099 0.079 Uiso 0.50 1 calc PR F 2 C34 C 0.2370(8) 0.3154(5) 0.1843(4) 0.062(2) Uani 1 1 d . H . H34A H 0.2871 0.3014 0.2235 0.074 Uiso 1 1 calc R . . H34B H 0.1636 0.2586 0.1956 0.074 Uiso 1 1 calc R . . C35 C 0.1592(12) 0.4359(9) 0.1826(6) 0.097(3) Uiso 1 1 d . . . H35A H 0.2249 0.4849 0.1935 0.116 Uiso 1 1 calc R G 1 H35B H 0.1553 0.4637 0.1327 0.116 Uiso 1 1 calc R G 1 C36A C 0.0242(17) 0.4639(13) 0.2220(9) 0.070(5) Uani 0.50 1 d P H 1 H36A H 0.0308 0.4440 0.2720 0.084 Uiso 0.50 1 calc PR H 1 H36B H -0.0399 0.4096 0.2151 0.084 Uiso 0.50 1 calc PR H 1 C37A C -0.0539(16) 0.5775(13) 0.2152(9) 0.064(4) Uani 0.50 1 d P H 1 H37A H -0.1476 0.5742 0.2485 0.096 Uiso 0.50 1 calc PR H 1 H37B H -0.0676 0.6002 0.1669 0.096 Uiso 0.50 1 calc PR H 1 H37C H 0.0013 0.6340 0.2256 0.096 Uiso 0.50 1 calc PR H 1 C36B C 0.0865(14) 0.4266(11) 0.2792(7) 0.046(3) Uani 0.50 1 d P H 2 H36C H 0.0341 0.3561 0.2980 0.055 Uiso 0.50 1 calc PR H 2 H36D H 0.1662 0.4226 0.3033 0.055 Uiso 0.50 1 calc PR H 2 C37B C -0.0151(15) 0.5327(12) 0.2935(7) 0.054(3) Uani 0.50 1 d P H 2 H37D H -0.0536 0.5279 0.3445 0.081 Uiso 0.50 1 calc PR H 2 H37E H -0.0942 0.5359 0.2699 0.081 Uiso 0.50 1 calc PR H 2 H37F H 0.0375 0.6021 0.2753 0.081 Uiso 0.50 1 calc PR H 2 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 0.0288(3) 0.0294(3) 0.0552(4) 0.0018(2) -0.0135(2) -0.00585(18) S1 0.0367(7) 0.0365(7) 0.0491(9) 0.0074(6) -0.0171(6) -0.0089(6) S2 0.0385(7) 0.0323(7) 0.0433(8) -0.0039(6) -0.0158(6) -0.0002(5) S3 0.0359(8) 0.0434(9) 0.0745(12) 0.0148(8) -0.0188(8) -0.0059(6) O1 0.031(2) 0.034(2) 0.071(3) -0.0093(19) -0.0100(19) -0.0028(16) N1 0.026(2) 0.031(2) 0.059(3) 0.007(2) -0.015(2) 0.0019(18) N2 0.038(3) 0.037(3) 0.056(3) 0.005(2) -0.022(2) -0.007(2) N3 0.057(3) 0.051(3) 0.041(3) -0.003(2) -0.007(3) -0.020(3) N4 0.054(3) 0.042(3) 0.055(3) -0.011(2) -0.015(3) 0.003(2) N5 0.027(2) 0.028(2) 0.036(2) -0.0032(18) -0.0014(18) -0.0054(17) C1 0.035(3) 0.032(3) 0.049(3) -0.002(2) -0.013(3) -0.012(2) C2 0.034(3) 0.031(3) 0.044(3) -0.004(2) -0.015(2) -0.009(2) C3 0.041(3) 0.031(3) 0.040(3) -0.005(2) -0.013(2) -0.009(2) C4 0.040(3) 0.037(3) 0.043(3) 0.005(3) -0.012(3) -0.014(2) C5 0.039(3) 0.044(4) 0.086(5) 0.028(4) -0.025(3) -0.011(3) C6 0.035(3) 0.050(4) 0.099(6) 0.025(4) -0.015(4) -0.006(3) C7 0.036(4) 0.048(4) 0.126(8) 0.014(4) 0.001(4) 0.003(3) C8 0.034(4) 0.074(6) 0.118(8) 0.056(5) -0.012(4) 0.000(4) C9 0.038(4) 0.084(6) 0.083(6) 0.044(5) -0.030(4) -0.026(4) C10 0.043(4) 0.072(5) 0.072(5) 0.040(4) -0.030(4) -0.017(3) C11 0.044(4) 0.104(7) 0.142(10) 0.058(7) -0.003(5) 0.003(5) C12 0.027(3) 0.034(3) 0.058(4) -0.001(3) -0.012(3) -0.003(2) C13 0.030(3) 0.043(3) 0.057(4) 0.001(3) -0.015(3) -0.003(2) C14 0.032(3) 0.067(4) 0.051(4) 0.000(3) -0.012(3) 0.004(3) C15 0.026(3) 0.053(4) 0.064(4) 0.012(3) -0.018(3) -0.010(2) C16 0.029(3) 0.042(3) 0.053(4) 0.010(3) -0.012(3) -0.007(2) C17 0.032(3) 0.039(3) 0.060(4) 0.008(3) -0.018(3) -0.005(2) C18 0.031(3) 0.047(4) 0.089(5) 0.010(3) -0.014(3) -0.016(3) C19 0.031(3) 0.057(4) 0.089(6) 0.011(4) -0.017(3) -0.021(3) C20 0.045(4) 0.053(4) 0.096(6) -0.003(4) -0.031(4) -0.019(3) C21 0.049(4) 0.046(4) 0.072(5) 0.001(3) -0.027(3) -0.008(3) C22 0.033(3) 0.029(3) 0.031(3) -0.002(2) -0.007(2) -0.003(2) C23 0.043(4) 0.034(3) 0.102(6) -0.024(4) 0.023(4) -0.014(3) C24 0.060(5) 0.029(4) 0.180(11) -0.027(5) 0.034(6) -0.012(3) C25A 0.057(8) 0.040(7) 0.063(9) -0.023(6) -0.009(7) 0.013(6) C25B 0.048(7) 0.028(6) 0.054(8) -0.010(5) -0.015(6) 0.010(5) C26 0.024(2) 0.027(2) 0.031(3) 0.003(2) -0.006(2) -0.0054(18) C27 0.063(4) 0.040(3) 0.045(3) 0.001(3) -0.025(3) -0.016(3) C28 0.047(3) 0.031(3) 0.072(4) -0.007(3) -0.022(3) -0.009(2) C29A 0.056(8) 0.038(6) 0.055(8) 0.002(5) -0.027(6) -0.004(5) C29B 0.027(5) 0.043(6) 0.044(7) 0.001(5) -0.015(5) -0.001(4) C30 0.059(4) 0.047(4) 0.068(4) 0.024(3) -0.039(4) -0.028(3) C31 0.083(5) 0.070(5) 0.095(6) 0.046(4) -0.069(5) -0.052(4) C32A 0.029(6) 0.045(6) 0.036(6) -0.004(5) -0.009(5) -0.008(5) C33A 0.041(7) 0.061(8) 0.054(8) -0.017(7) -0.012(6) -0.005(6) C32B 0.023(5) 0.046(6) 0.031(6) -0.002(5) -0.005(4) -0.007(5) C33B 0.055(8) 0.054(8) 0.059(8) -0.017(7) -0.022(7) -0.009(6) C34 0.053(4) 0.040(3) 0.077(5) -0.022(3) 0.031(4) -0.022(3) C36A 0.064(9) 0.055(8) 0.072(10) -0.027(8) 0.037(8) -0.010(7) C37A 0.053(8) 0.058(9) 0.074(10) -0.018(7) -0.001(7) 0.010(7) C36B 0.043(7) 0.045(7) 0.047(7) -0.007(6) -0.004(6) -0.012(5) C37B 0.059(8) 0.066(9) 0.042(7) -0.022(6) -0.006(6) -0.017(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 O1 1.689(4) . ? Mo1 N1 2.205(5) . ? Mo1 N2 2.305(5) . ? Mo1 S1 2.3905(18) . ? Mo1 S3 2.4282(18) . ? Mo1 S2 2.4296(16) . ? S1 C1 1.773(6) . ? S2 C2 1.743(6) . ? S3 C5 1.777(8) . ? N1 C12 1.352(8) . ? N1 C16 1.366(7) . ? N2 C17 1.337(8) . ? N2 C21 1.353(8) . ? N3 C4 1.170(8) . ? N4 C3 1.153(7) . ? N5 C30 1.502(8) . ? N5 C34 1.507(7) . ? N5 C26 1.523(6) . ? N5 C22 1.526(6) . ? C1 C2 1.346(8) . ? C1 C4 1.402(9) . ? C2 C3 1.434(8) . ? C5 C10 1.377(9) . ? C5 C6 1.383(11) . ? C6 C7 1.378(10) . ? C7 C8 1.406(11) . ? C8 C9 1.358(13) . ? C8 C11 1.531(13) . ? C9 C10 1.392(12) . ? C12 C13 1.354(9) . ? C13 C14 1.379(8) . ? C14 C15 1.372(9) . ? C15 C16 1.366(9) . ? C16 C17 1.475(9) . ? C17 C18 1.393(8) . ? C18 C19 1.368(10) . ? C19 C20 1.392(11) . ? C20 C21 1.374(9) . ? C22 C23 1.505(8) . ? C23 C24 1.529(9) . ? C24 C25B 1.215(16) . ? C24 C25A 1.532(14) . ? C26 C27 1.504(8) . ? C27 C28 1.543(8) . ? C28 C29B 1.399(12) . ? C28 C29A 1.442(13) . ? C30 C31 1.527(8) . ? C31 C32A 1.559(13) . ? C31 C32B 1.663(13) . ? C32A C33A 1.526(16) . ? C32B C33B 1.514(16) . ? C34 C35 1.506(12) . ? C35 C36A 1.357(16) . ? C35 C36B 1.821(16) . ? C36A C37A 1.44(2) . ? C36B C37B 1.500(19) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Mo1 N1 86.63(19) . . ? O1 Mo1 N2 156.5(2) . . ? N1 Mo1 N2 69.90(18) . . ? O1 Mo1 S1 105.40(15) . . ? N1 Mo1 S1 167.96(13) . . ? N2 Mo1 S1 98.08(14) . . ? O1 Mo1 S3 103.04(15) . . ? N1 Mo1 S3 93.27(12) . . ? N2 Mo1 S3 80.61(13) . . ? S1 Mo1 S3 83.77(6) . . ? O1 Mo1 S2 99.29(14) . . ? N1 Mo1 S2 94.27(12) . . ? N2 Mo1 S2 81.45(12) . . ? S1 Mo1 S2 84.31(5) . . ? S3 Mo1 S2 156.80(6) . . ? C1 S1 Mo1 105.1(2) . . ? C2 S2 Mo1 104.28(19) . . ? C5 S3 Mo1 109.8(2) . . ? C12 N1 C16 116.7(5) . . ? C12 N1 Mo1 121.4(4) . . ? C16 N1 Mo1 121.9(4) . . ? C17 N2 C21 118.4(5) . . ? C17 N2 Mo1 119.6(4) . . ? C21 N2 Mo1 121.9(5) . . ? C30 N5 C34 112.4(5) . . ? C30 N5 C26 105.8(4) . . ? C34 N5 C26 111.6(4) . . ? C30 N5 C22 110.9(4) . . ? C34 N5 C22 104.7(4) . . ? C26 N5 C22 111.5(4) . . ? C2 C1 C4 120.5(5) . . ? C2 C1 S1 121.8(5) . . ? C4 C1 S1 117.7(4) . . ? C1 C2 C3 120.7(5) . . ? C1 C2 S2 123.2(4) . . ? C3 C2 S2 116.1(4) . . ? N4 C3 C2 179.6(7) . . ? N3 C4 C1 178.6(6) . . ? C10 C5 C6 117.7(8) . . ? C10 C5 S3 120.6(7) . . ? C6 C5 S3 121.5(5) . . ? C7 C6 C5 121.9(7) . . ? C6 C7 C8 118.6(9) . . ? C9 C8 C7 120.5(8) . . ? C9 C8 C11 122.2(8) . . ? C7 C8 C11 117.2(10) . . ? C8 C9 C10 119.2(7) . . ? C5 C10 C9 121.9(9) . . ? C13 C12 N1 123.9(5) . . ? C12 C13 C14 118.8(6) . . ? C15 C14 C13 118.6(6) . . ? C14 C15 C16 120.4(6) . . ? N1 C16 C15 121.6(6) . . ? N1 C16 C17 114.4(6) . . ? C15 C16 C17 124.0(5) . . ? N2 C17 C18 122.4(6) . . ? N2 C17 C16 114.1(5) . . ? C18 C17 C16 123.5(6) . . ? C19 C18 C17 119.3(7) . . ? C18 C19 C20 118.4(6) . . ? C21 C20 C19 119.9(7) . . ? N2 C21 C20 121.7(7) . . ? C23 C22 N5 115.8(5) . . ? C22 C23 C24 109.2(6) . . ? C25B C24 C23 123.9(11) . . ? C25B C24 C25A 67.3(9) . . ? C23 C24 C25A 117.1(7) . . ? C27 C26 N5 115.4(4) . . ? C26 C27 C28 109.1(5) . . ? C29B C28 C29A 78.8(8) . . ? C29B C28 C27 110.6(7) . . ? C29A C28 C27 121.5(7) . . ? N5 C30 C31 115.0(5) . . ? C30 C31 C32A 107.6(6) . . ? C30 C31 C32B 107.2(6) . . ? C32A C31 C32B 37.3(6) . . ? C33A C32A C31 110.1(9) . . ? C33B C32B C31 111.1(8) . . ? N5 C34 C35 117.2(7) . . ? C36A C35 C34 126.4(10) . . ? C36A C35 C36B 47.9(10) . . ? C34 C35 C36B 97.4(8) . . ? C35 C36A C37A 125.6(13) . . ? C37B C36B C35 109.3(10) . . ? _diffrn_measured_fraction_theta_max 0.966 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.966 _refine_diff_density_max 1.922 _refine_diff_density_min -0.795 _refine_diff_density_rms 0.139 data_op4Me _database_code_depnum_ccdc_archive 'CCDC 890844' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C16 H36 N), C45 H30 Mo2 N8 O2 S6, H2 O' _chemical_formula_sum 'C77 H104 Mo2 N10 O3 S6' _chemical_formula_weight 1602.00 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 34.781(5) _cell_length_b 13.822(5) _cell_length_c 17.232(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 103.548(5) _cell_angle_gamma 90.000(5) _cell_volume 8054(4) _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 blue _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.321 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3360 _exptl_absorpt_coefficient_mu 0.518 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.968 _exptl_absorpt_correction_T_max 0.976 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method /w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25577 _diffrn_reflns_av_R_equivalents 0.0716 _diffrn_reflns_av_sigmaI/netI 0.0868 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 45 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 28.00 _reflns_number_total 9671 _reflns_number_gt 6026 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART 5.628 (Bruker, 2003)' _computing_cell_refinement 'SAINT 6.45 ( Bruker, 2003)' _computing_data_reduction 'SAINT 6.45 ( Bruker, 2003)' _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 3.1e, Ortep' _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^)+(0.1167P)^2^+52.7231P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9671 _refine_ls_number_parameters 444 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1368 _refine_ls_R_factor_gt 0.0867 _refine_ls_wR_factor_ref 0.2609 _refine_ls_wR_factor_gt 0.2131 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _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 0.398274(16) 0.38236(4) 0.09064(3) 0.03890(19) Uani 1 1 d . . . S1 S 0.39658(5) 0.55705(11) 0.10889(10) 0.0379(4) Uani 1 1 d . . . S2 S 0.32879(5) 0.39217(12) 0.08858(11) 0.0445(4) Uani 1 1 d . . . S3 S 0.37786(6) 0.23037(12) 0.02376(12) 0.0515(5) Uani 1 1 d . . . O1 O 0.42221(15) 0.3500(4) 0.1842(3) 0.0523(12) Uani 1 1 d . . . O2 O 0.5000 0.1362(7) 0.2500 0.092(3) Uani 1 2 d S . . H1W H 0.5102 0.0946 0.2274 1.5(9) Uiso 1 1 calc R . . N1 N 0.33888(19) 0.7487(4) 0.1801(4) 0.0544(15) Uani 1 1 d . . . N2 N 0.25237(19) 0.5499(5) 0.1423(5) 0.0658(19) Uani 1 1 d . . . N3 N 0.39273(15) 0.4352(4) -0.0384(3) 0.0402(12) Uani 1 1 d . . . N4 N 0.45672(15) 0.3726(4) 0.0600(4) 0.0433(13) Uani 1 1 d . . . N5 N 0.29805(17) 0.0451(4) 0.1387(3) 0.0462(13) Uani 1 1 d . . . C1 C 0.35041(19) 0.5794(4) 0.1278(4) 0.0373(13) Uani 1 1 d . . . C2 C 0.32100(18) 0.5107(5) 0.1184(4) 0.0384(13) Uani 1 1 d . . . C3 C 0.34366(19) 0.6734(5) 0.1554(4) 0.0418(14) Uani 1 1 d . . . C4 C 0.2832(2) 0.5337(5) 0.1333(4) 0.0473(16) Uani 1 1 d . . . C5 C 0.3598(2) 0.4733(5) -0.0863(4) 0.0476(16) Uani 1 1 d . . . H5 H 0.3370 0.4762 -0.0673 0.057 Uiso 1 1 calc R . . C6 C 0.3584(2) 0.5083(5) -0.1619(4) 0.0513(17) Uani 1 1 d . . . H6 H 0.3352 0.5358 -0.1920 0.062 Uiso 1 1 calc R . . C7 C 0.3914(2) 0.5019(6) -0.1920(4) 0.0548(18) Uani 1 1 d . . . H7 H 0.3910 0.5257 -0.2427 0.066 Uiso 1 1 calc R . . C8 C 0.4256(2) 0.4595(5) -0.1460(4) 0.0494(17) Uani 1 1 d . . . C9 C 0.42488(19) 0.4289(4) -0.0684(4) 0.0396(14) Uani 1 1 d . . . C10 C 0.4599(2) 0.3932(4) -0.0155(4) 0.0443(16) Uani 1 1 d . . . C11 C 0.4944(2) 0.3833(5) -0.0435(5) 0.056(2) Uani 1 1 d . . . C12 C 0.4940(3) 0.4106(6) -0.1232(6) 0.063(2) Uani 1 1 d . . . H12 H 0.5167 0.4018 -0.1423 0.075 Uiso 1 1 calc R . . C13 C 0.4618(3) 0.4486(6) -0.1713(5) 0.066(2) Uani 1 1 d . . . H13 H 0.4629 0.4684 -0.2223 0.079 Uiso 1 1 calc R . . C14 C 0.5282(3) 0.3491(6) 0.0108(7) 0.070(2) Uani 1 1 d . . . H14 H 0.5519 0.3406 -0.0045 0.084 Uiso 1 1 calc R . . C15 C 0.5254(2) 0.3284(5) 0.0870(6) 0.068(3) Uani 1 1 d . . . H15 H 0.5475 0.3056 0.1237 0.081 Uiso 1 1 calc R . . C16 C 0.4899(2) 0.3408(5) 0.1108(5) 0.059(2) Uani 1 1 d . . . H16 H 0.4892 0.3266 0.1632 0.071 Uiso 1 1 calc R . . C17 C 0.4114(2) 0.1929(5) -0.0336(5) 0.0527(18) Uani 1 1 d . . . C18 C 0.4474(2) 0.1488(5) 0.0035(6) 0.066(2) Uani 1 1 d . . . H18 H 0.4537 0.1375 0.0583 0.079 Uiso 1 1 calc R . . C19 C 0.4734(3) 0.1224(7) -0.0424(10) 0.096(4) Uani 1 1 d . . . H19 H 0.4974 0.0942 -0.0174 0.115 Uiso 1 1 calc R . . C20 C 0.4654(3) 0.1359(9) -0.1213(10) 0.105(5) Uani 1 1 d . . . C21 C 0.4297(3) 0.1800(7) -0.1586(7) 0.085(3) Uani 1 1 d . . . H21 H 0.4239 0.1913 -0.2133 0.102 Uiso 1 1 calc R . . C22 C 0.4034(2) 0.2065(6) -0.1149(5) 0.059(2) Uani 1 1 d . . . H22 H 0.3795 0.2344 -0.1407 0.070 Uiso 1 1 calc R . . C23 C 0.4915(9) 0.111(2) -0.1737(18) 0.147(12) Uiso 0.50 1 d P . . H23A H 0.4771 0.0740 -0.2180 0.220 Uiso 1 1 calc R . . H23B H 0.5136 0.0746 -0.1444 0.220 Uiso 1 1 calc R . . H23C H 0.5009 0.1699 -0.1931 0.220 Uiso 1 1 calc R . . C24 C 0.3192(2) 0.0311(6) 0.0710(5) 0.0563(19) Uani 1 1 d . . . H24A H 0.2998 0.0116 0.0234 0.068 Uiso 1 1 calc R . . H24B H 0.3299 0.0929 0.0598 0.068 Uiso 1 1 calc R . . C25 C 0.3519(3) -0.0418(8) 0.0869(6) 0.079(3) Uani 1 1 d . . . H25A H 0.3419 -0.1039 0.0993 0.095 Uiso 1 1 calc R . . H25B H 0.3725 -0.0215 0.1324 0.095 Uiso 1 1 calc R . . C26 C 0.3690(3) -0.0511(7) 0.0131(6) 0.077(3) Uani 1 1 d . . . H26A H 0.3483 -0.0708 -0.0322 0.093 Uiso 1 1 calc R . . H26B H 0.3788 0.0114 0.0008 0.093 Uiso 1 1 calc R . . C27 C 0.4027(4) -0.1250(11) 0.0263(8) 0.122(5) Uani 1 1 d . . . H27A H 0.4128 -0.1292 -0.0208 0.183 Uiso 1 1 calc R . . H27B H 0.3929 -0.1871 0.0376 0.183 Uiso 1 1 calc R . . H27C H 0.4234 -0.1049 0.0706 0.183 Uiso 1 1 calc R . . C28 C 0.2784(2) -0.0469(5) 0.1552(4) 0.0475(16) Uani 1 1 d . . . H28A H 0.2988 -0.0951 0.1731 0.057 Uiso 1 1 calc R . . H28B H 0.2659 -0.0349 0.1991 0.057 Uiso 1 1 calc R . . C29 C 0.2481(2) -0.0892(5) 0.0882(5) 0.0489(17) Uani 1 1 d . . . H29A H 0.2603 -0.1059 0.0447 0.059 Uiso 1 1 calc R . . H29B H 0.2275 -0.0420 0.0687 0.059 Uiso 1 1 calc R . . C30 C 0.2303(2) -0.1791(6) 0.1165(5) 0.0591(19) Uani 1 1 d . . . H30A H 0.2511 -0.2263 0.1350 0.071 Uiso 1 1 calc R . . H30B H 0.2191 -0.1622 0.1612 0.071 Uiso 1 1 calc R . . C31 C 0.1988(3) -0.2236(6) 0.0522(6) 0.075(3) Uani 1 1 d . . . H31A H 0.1885 -0.2800 0.0728 0.112 Uiso 1 1 calc R . . H31B H 0.2098 -0.2417 0.0082 0.112 Uiso 1 1 calc R . . H31C H 0.1779 -0.1777 0.0345 0.112 Uiso 1 1 calc R . . C32 C 0.2674(3) 0.1251(5) 0.1126(5) 0.065(2) Uani 1 1 d . . . H32A H 0.2809 0.1830 0.1014 0.078 Uiso 1 1 calc R . . H32B H 0.2494 0.1054 0.0633 0.078 Uiso 1 1 calc R . . C33 C 0.2433(3) 0.1502(8) 0.1730(7) 0.095(4) Uani 1 1 d . . . H33A H 0.2611 0.1757 0.2206 0.114 Uiso 1 1 calc R . . H33B H 0.2319 0.0912 0.1880 0.114 Uiso 1 1 calc R . . C34 C 0.2099(3) 0.2240(8) 0.1443(8) 0.115(5) Uani 1 1 d D . . H34A H 0.1947 0.2036 0.0923 0.138 Uiso 1 1 calc R . . H34B H 0.1924 0.2216 0.1806 0.138 Uiso 1 1 calc R . . C35 C 0.2212(4) 0.3179(7) 0.1386(7) 0.107(4) Uani 1 1 d D . . H35A H 0.1982 0.3574 0.1199 0.161 Uiso 1 1 calc R . . H35B H 0.2380 0.3220 0.1017 0.161 Uiso 1 1 calc R . . H35C H 0.2353 0.3403 0.1901 0.161 Uiso 1 1 calc R . . C36 C 0.3272(2) 0.0735(6) 0.2173(4) 0.0516(17) Uani 1 1 d . . . H36A H 0.3126 0.0768 0.2588 0.062 Uiso 1 1 calc R . . H36B H 0.3466 0.0222 0.2316 0.062 Uiso 1 1 calc R . . C37 C 0.3488(3) 0.1667(6) 0.2171(5) 0.071(2) Uani 1 1 d . . . H37A H 0.3301 0.2198 0.2104 0.085 Uiso 1 1 calc R . . H37B H 0.3612 0.1674 0.1722 0.085 Uiso 1 1 calc R . . C38 C 0.3807(3) 0.1816(7) 0.2948(5) 0.080(3) Uani 1 1 d . . . H38A H 0.3699 0.1658 0.3403 0.095 Uiso 1 1 calc R . . H38B H 0.3889 0.2489 0.2993 0.095 Uiso 1 1 calc R . . C39 C 0.4181(4) 0.1136(10) 0.2944(10) 0.142(6) Uani 1 1 d . . . H39A H 0.4379 0.1228 0.3431 0.213 Uiso 1 1 calc R . . H39B H 0.4290 0.1303 0.2498 0.213 Uiso 1 1 calc R . . H39C H 0.4099 0.0471 0.2900 0.213 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 0.0394(3) 0.0335(3) 0.0460(3) 0.0005(2) 0.0145(2) 0.0000(2) S1 0.0376(8) 0.0331(8) 0.0452(8) -0.0005(6) 0.0140(7) -0.0021(6) S2 0.0441(9) 0.0381(8) 0.0587(10) -0.0033(7) 0.0271(8) -0.0052(7) S3 0.0542(10) 0.0358(9) 0.0728(12) -0.0066(8) 0.0315(9) -0.0090(7) O1 0.058(3) 0.040(3) 0.057(3) 0.004(2) 0.008(2) 0.004(2) O2 0.062(5) 0.061(6) 0.144(9) 0.000 0.006(6) 0.000 N1 0.056(4) 0.041(3) 0.067(4) 0.002(3) 0.016(3) 0.008(3) N2 0.044(3) 0.060(4) 0.104(6) -0.006(4) 0.038(4) 0.000(3) N3 0.040(3) 0.038(3) 0.046(3) -0.008(2) 0.015(2) -0.006(2) N4 0.035(3) 0.028(3) 0.068(4) -0.006(2) 0.013(3) -0.001(2) N5 0.050(3) 0.034(3) 0.055(3) 0.009(2) 0.014(3) 0.005(2) C1 0.043(3) 0.034(3) 0.038(3) 0.002(2) 0.016(3) 0.003(3) C2 0.033(3) 0.041(3) 0.045(3) 0.000(3) 0.018(3) -0.001(3) C3 0.039(3) 0.041(4) 0.048(4) 0.005(3) 0.014(3) 0.004(3) C4 0.047(4) 0.039(4) 0.058(4) -0.004(3) 0.018(3) -0.001(3) C5 0.053(4) 0.043(4) 0.049(4) -0.006(3) 0.017(3) -0.007(3) C6 0.056(4) 0.053(4) 0.044(4) -0.003(3) 0.010(3) -0.008(3) C7 0.069(5) 0.054(4) 0.043(4) -0.013(3) 0.017(4) -0.015(4) C8 0.057(4) 0.044(4) 0.058(4) -0.012(3) 0.034(4) -0.012(3) C9 0.045(4) 0.030(3) 0.050(4) -0.009(3) 0.024(3) -0.011(3) C10 0.043(4) 0.031(3) 0.065(4) -0.011(3) 0.026(3) -0.008(3) C11 0.047(4) 0.033(3) 0.096(6) -0.013(4) 0.032(4) -0.008(3) C12 0.056(5) 0.063(5) 0.085(6) -0.013(4) 0.048(5) -0.011(4) C13 0.085(6) 0.055(5) 0.073(5) -0.019(4) 0.053(5) -0.020(4) C14 0.053(5) 0.041(4) 0.122(8) -0.007(5) 0.035(5) -0.003(4) C15 0.030(4) 0.041(4) 0.122(8) -0.006(4) -0.001(4) 0.001(3) C16 0.052(4) 0.040(4) 0.080(5) 0.003(4) 0.003(4) 0.005(3) C17 0.046(4) 0.028(3) 0.089(6) -0.011(3) 0.026(4) -0.007(3) C18 0.056(5) 0.034(4) 0.107(7) -0.011(4) 0.015(5) -0.003(3) C19 0.047(5) 0.053(5) 0.187(13) -0.043(7) 0.026(7) 0.009(4) C20 0.067(7) 0.105(9) 0.155(12) -0.072(9) 0.049(8) -0.014(6) C21 0.082(7) 0.084(7) 0.101(7) -0.037(6) 0.043(6) -0.009(5) C22 0.058(5) 0.051(4) 0.075(5) -0.018(4) 0.031(4) -0.011(3) C24 0.062(5) 0.055(5) 0.056(4) -0.001(3) 0.022(4) -0.023(4) C25 0.068(6) 0.086(7) 0.097(7) -0.001(5) 0.049(5) -0.003(5) C26 0.084(6) 0.073(6) 0.090(6) -0.035(5) 0.051(5) -0.040(5) C27 0.089(8) 0.163(14) 0.132(11) -0.038(9) 0.058(8) -0.009(8) C28 0.048(4) 0.036(3) 0.063(4) 0.009(3) 0.022(3) 0.008(3) C29 0.038(3) 0.037(3) 0.075(5) 0.005(3) 0.021(3) 0.003(3) C30 0.047(4) 0.052(4) 0.077(5) 0.006(4) 0.011(4) -0.003(3) C31 0.065(5) 0.039(4) 0.109(7) 0.004(4) -0.003(5) -0.010(4) C32 0.070(5) 0.038(4) 0.074(5) 0.003(4) -0.009(4) 0.011(4) C33 0.089(7) 0.076(7) 0.106(8) -0.027(6) -0.008(6) 0.045(6) C34 0.100(8) 0.080(8) 0.138(10) -0.025(7) -0.027(8) 0.044(7) C35 0.125(9) 0.055(6) 0.105(8) 0.015(6) -0.047(7) 0.000(6) C36 0.049(4) 0.060(5) 0.043(4) 0.007(3) 0.007(3) 0.009(3) C37 0.094(7) 0.048(5) 0.056(5) 0.010(4) -0.011(4) -0.011(4) C38 0.098(7) 0.055(5) 0.067(5) 0.005(4) -0.019(5) -0.005(5) C39 0.098(9) 0.111(11) 0.177(15) -0.031(10) -0.051(10) 0.008(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 O1 1.692(5) . ? Mo1 N4 2.221(5) . ? Mo1 N3 2.305(5) . ? Mo1 S2 2.4123(18) . ? Mo1 S3 2.4212(19) . ? Mo1 S1 2.4374(18) . ? S1 C1 1.739(6) . ? S2 C2 1.757(7) . ? S3 C17 1.776(7) . ? O2 H1W 0.8200 . ? N1 C3 1.152(8) . ? N2 C4 1.142(8) . ? N3 C9 1.341(7) . ? N3 C5 1.351(9) . ? N4 C16 1.350(9) . ? N4 C10 1.361(9) . ? N5 C28 1.503(8) . ? N5 C32 1.528(9) . ? N5 C24 1.529(9) . ? N5 C36 1.540(9) . ? C1 C2 1.377(9) . ? C1 C3 1.421(9) . ? C2 C4 1.433(9) . ? C5 C6 1.379(10) . ? C5 H5 0.9300 . ? C6 C7 1.369(10) . ? C6 H6 0.9300 . ? C7 C8 1.394(11) . ? C7 H7 0.9300 . ? C8 C9 1.407(9) . ? C8 C13 1.435(10) . ? C9 C10 1.428(10) . ? C10 C11 1.401(9) . ? C11 C14 1.402(12) . ? C11 C12 1.421(12) . ? C12 C13 1.334(13) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 C15 1.368(13) . ? C14 H14 0.9300 . ? C15 C16 1.398(11) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 C22 1.375(11) . ? C17 C18 1.405(11) . ? C18 C19 1.382(14) . ? C18 H18 0.9300 . ? C19 C20 1.336(18) . ? C19 H19 0.9300 . ? C20 C21 1.396(17) . ? C20 C23 1.46(3) . ? C21 C22 1.366(11) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 C25 1.497(12) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C26 1.531(11) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 C27 1.530(16) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 C29 1.487(10) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 C30 1.520(10) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 C31 1.495(11) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 C33 1.521(13) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 C34 1.537(12) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 C35 1.367(12) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 C37 1.491(11) . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 C38 1.539(11) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 C39 1.609(16) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Mo1 N4 86.4(2) . . ? O1 Mo1 N3 156.1(2) . . ? N4 Mo1 N3 70.4(2) . . ? O1 Mo1 S2 107.25(18) . . ? N4 Mo1 S2 165.80(16) . . ? N3 Mo1 S2 96.37(14) . . ? O1 Mo1 S3 104.37(18) . . ? N4 Mo1 S3 90.96(14) . . ? N3 Mo1 S3 82.34(14) . . ? S2 Mo1 S3 81.99(6) . . ? O1 Mo1 S1 99.22(17) . . ? N4 Mo1 S1 98.16(13) . . ? N3 Mo1 S1 79.14(14) . . ? S2 Mo1 S1 83.79(6) . . ? S3 Mo1 S1 155.18(7) . . ? C1 S1 Mo1 104.6(2) . . ? C2 S2 Mo1 105.7(2) . . ? C17 S3 Mo1 111.1(2) . . ? C9 N3 C5 116.9(6) . . ? C9 N3 Mo1 117.6(4) . . ? C5 N3 Mo1 125.5(4) . . ? C16 N4 C10 116.1(6) . . ? C16 N4 Mo1 123.9(5) . . ? C10 N4 Mo1 119.9(4) . . ? C28 N5 C32 110.5(6) . . ? C28 N5 C24 111.0(5) . . ? C32 N5 C24 107.1(6) . . ? C28 N5 C36 106.5(5) . . ? C32 N5 C36 110.1(6) . . ? C24 N5 C36 111.6(5) . . ? C2 C1 C3 119.5(6) . . ? C2 C1 S1 123.2(5) . . ? C3 C1 S1 117.2(5) . . ? C1 C2 C4 120.9(6) . . ? C1 C2 S2 121.1(5) . . ? C4 C2 S2 118.1(5) . . ? N1 C3 C1 177.8(8) . . ? N2 C4 C2 177.1(8) . . ? N3 C5 C6 123.6(7) . . ? N3 C5 H5 118.2 . . ? C6 C5 H5 118.2 . . ? C7 C6 C5 119.1(7) . . ? C7 C6 H6 120.5 . . ? C5 C6 H6 120.5 . . ? C6 C7 C8 119.4(7) . . ? C6 C7 H7 120.3 . . ? C8 C7 H7 120.3 . . ? C7 C8 C9 117.7(6) . . ? C7 C8 C13 124.4(7) . . ? C9 C8 C13 117.9(8) . . ? N3 C9 C8 123.3(7) . . ? N3 C9 C10 116.1(6) . . ? C8 C9 C10 120.6(6) . . ? N4 C10 C11 125.2(7) . . ? N4 C10 C9 115.8(5) . . ? C11 C10 C9 119.0(7) . . ? C10 C11 C14 117.0(8) . . ? C10 C11 C12 119.5(8) . . ? C14 C11 C12 123.5(7) . . ? C13 C12 C11 121.3(7) . . ? C13 C12 H12 119.3 . . ? C11 C12 H12 119.3 . . ? C12 C13 C8 121.5(8) . . ? C12 C13 H13 119.2 . . ? C8 C13 H13 119.2 . . ? C15 C14 C11 118.4(8) . . ? C15 C14 H14 120.8 . . ? C11 C14 H14 120.8 . . ? C14 C15 C16 121.4(8) . . ? C14 C15 H15 119.3 . . ? C16 C15 H15 119.3 . . ? N4 C16 C15 121.9(8) . . ? N4 C16 H16 119.0 . . ? C15 C16 H16 119.0 . . ? C22 C17 C18 118.1(7) . . ? C22 C17 S3 121.6(6) . . ? C18 C17 S3 120.3(7) . . ? C19 C18 C17 119.0(10) . . ? C19 C18 H18 120.5 . . ? C17 C18 H18 120.5 . . ? C20 C19 C18 122.5(10) . . ? C20 C19 H19 118.7 . . ? C18 C19 H19 118.7 . . ? C19 C20 C21 118.8(10) . . ? C19 C20 C23 125.8(17) . . ? C21 C20 C23 115.4(18) . . ? C22 C21 C20 120.1(11) . . ? C22 C21 H21 120.0 . . ? C20 C21 H21 120.0 . . ? C21 C22 C17 121.5(9) . . ? C21 C22 H22 119.3 . . ? C17 C22 H22 119.3 . . ? C20 C23 H23A 109.5 . . ? C20 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C20 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 C24 N5 115.3(6) . . ? C25 C24 H24A 108.5 . . ? N5 C24 H24A 108.5 . . ? C25 C24 H24B 108.5 . . ? N5 C24 H24B 108.5 . . ? H24A C24 H24B 107.5 . . ? C24 C25 C26 109.3(8) . . ? C24 C25 H25A 109.8 . . ? C26 C25 H25A 109.8 . . ? C24 C25 H25B 109.8 . . ? C26 C25 H25B 109.8 . . ? H25A C25 H25B 108.3 . . ? C27 C26 C25 111.4(10) . . ? C27 C26 H26A 109.4 . . ? C25 C26 H26A 109.4 . . ? C27 C26 H26B 109.4 . . ? C25 C26 H26B 109.4 . . ? H26A C26 H26B 108.0 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C29 C28 N5 117.1(6) . . ? C29 C28 H28A 108.0 . . ? N5 C28 H28A 108.0 . . ? C29 C28 H28B 108.0 . . ? N5 C28 H28B 108.0 . . ? H28A C28 H28B 107.3 . . ? C28 C29 C30 109.9(6) . . ? C28 C29 H29A 109.7 . . ? C30 C29 H29A 109.7 . . ? C28 C29 H29B 109.7 . . ? C30 C29 H29B 109.7 . . ? H29A C29 H29B 108.2 . . ? C31 C30 C29 112.5(7) . . ? C31 C30 H30A 109.1 . . ? C29 C30 H30A 109.1 . . ? C31 C30 H30B 109.1 . . ? C29 C30 H30B 109.1 . . ? H30A C30 H30B 107.8 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C33 C32 N5 115.0(7) . . ? C33 C32 H32A 108.5 . . ? N5 C32 H32A 108.5 . . ? C33 C32 H32B 108.5 . . ? N5 C32 H32B 108.5 . . ? H32A C32 H32B 107.5 . . ? C32 C33 C34 115.3(10) . . ? C32 C33 H33A 108.5 . . ? C34 C33 H33A 108.5 . . ? C32 C33 H33B 108.5 . . ? C34 C33 H33B 108.5 . . ? H33A C33 H33B 107.5 . . ? C35 C34 C33 116.4(11) . . ? C35 C34 H34A 108.2 . . ? C33 C34 H34A 108.2 . . ? C35 C34 H34B 108.2 . . ? C33 C34 H34B 108.2 . . ? H34A C34 H34B 107.3 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C37 C36 N5 116.5(6) . . ? C37 C36 H36A 108.2 . . ? N5 C36 H36A 108.2 . . ? C37 C36 H36B 108.2 . . ? N5 C36 H36B 108.2 . . ? H36A C36 H36B 107.3 . . ? C36 C37 C38 112.0(7) . . ? C36 C37 H37A 109.2 . . ? C38 C37 H37A 109.2 . . ? C36 C37 H37B 109.2 . . ? C38 C37 H37B 109.2 . . ? H37A C37 H37B 107.9 . . ? C37 C38 C39 109.7(9) . . ? C37 C38 H38A 109.7 . . ? C39 C38 H38A 109.7 . . ? C37 C38 H38B 109.7 . . ? C39 C38 H38B 109.7 . . ? H38A C38 H38B 108.2 . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? 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 O1 Mo1 S1 C1 -95.9(3) . . . . ? N4 Mo1 S1 C1 176.4(3) . . . . ? N3 Mo1 S1 C1 108.3(3) . . . . ? S2 Mo1 S1 C1 10.6(2) . . . . ? S3 Mo1 S1 C1 65.9(3) . . . . ? O1 Mo1 S2 C2 87.7(3) . . . . ? N4 Mo1 S2 C2 -108.9(6) . . . . ? N3 Mo1 S2 C2 -88.4(3) . . . . ? S3 Mo1 S2 C2 -169.7(2) . . . . ? S1 Mo1 S2 C2 -10.1(2) . . . . ? O1 Mo1 S3 C17 -97.8(4) . . . . ? N4 Mo1 S3 C17 -11.3(3) . . . . ? N3 Mo1 S3 C17 58.8(3) . . . . ? S2 Mo1 S3 C17 156.3(3) . . . . ? S1 Mo1 S3 C17 100.7(3) . . . . ? O1 Mo1 N3 C9 18.3(8) . . . . ? N4 Mo1 N3 C9 3.8(4) . . . . ? S2 Mo1 N3 C9 -171.0(4) . . . . ? S3 Mo1 N3 C9 -90.0(4) . . . . ? S1 Mo1 N3 C9 106.6(4) . . . . ? O1 Mo1 N3 C5 -160.7(6) . . . . ? N4 Mo1 N3 C5 -175.3(5) . . . . ? S2 Mo1 N3 C5 9.9(5) . . . . ? S3 Mo1 N3 C5 90.9(5) . . . . ? S1 Mo1 N3 C5 -72.5(5) . . . . ? O1 Mo1 N4 C16 5.5(5) . . . . ? N3 Mo1 N4 C16 179.6(6) . . . . ? S2 Mo1 N4 C16 -158.7(5) . . . . ? S3 Mo1 N4 C16 -98.9(5) . . . . ? S1 Mo1 N4 C16 104.3(5) . . . . ? O1 Mo1 N4 C10 -179.1(5) . . . . ? N3 Mo1 N4 C10 -5.0(4) . . . . ? S2 Mo1 N4 C10 16.7(9) . . . . ? S3 Mo1 N4 C10 76.5(4) . . . . ? S1 Mo1 N4 C10 -80.3(4) . . . . ? Mo1 S1 C1 C2 -10.2(6) . . . . ? Mo1 S1 C1 C3 168.7(4) . . . . ? C3 C1 C2 C4 2.4(10) . . . . ? S1 C1 C2 C4 -178.7(5) . . . . ? C3 C1 C2 S2 -177.3(5) . . . . ? S1 C1 C2 S2 1.7(8) . . . . ? Mo1 S2 C2 C1 8.0(6) . . . . ? Mo1 S2 C2 C4 -171.6(5) . . . . ? C2 C1 C3 N1 102(20) . . . . ? S1 C1 C3 N1 -77(20) . . . . ? C1 C2 C4 N2 139(16) . . . . ? S2 C2 C4 N2 -42(17) . . . . ? C9 N3 C5 C6 -2.2(9) . . . . ? Mo1 N3 C5 C6 176.8(5) . . . . ? N3 C5 C6 C7 2.0(11) . . . . ? C5 C6 C7 C8 0.6(10) . . . . ? C6 C7 C8 C9 -2.8(10) . . . . ? C6 C7 C8 C13 179.8(7) . . . . ? C5 N3 C9 C8 -0.2(9) . . . . ? Mo1 N3 C9 C8 -179.3(5) . . . . ? C5 N3 C9 C10 176.8(5) . . . . ? Mo1 N3 C9 C10 -2.3(7) . . . . ? C7 C8 C9 N3 2.7(10) . . . . ? C13 C8 C9 N3 -179.7(6) . . . . ? C7 C8 C9 C10 -174.2(6) . . . . ? C13 C8 C9 C10 3.4(9) . . . . ? C16 N4 C10 C11 0.4(9) . . . . ? Mo1 N4 C10 C11 -175.4(5) . . . . ? C16 N4 C10 C9 -178.6(6) . . . . ? Mo1 N4 C10 C9 5.6(7) . . . . ? N3 C9 C10 N4 -2.0(8) . . . . ? C8 C9 C10 N4 175.1(5) . . . . ? N3 C9 C10 C11 179.0(6) . . . . ? C8 C9 C10 C11 -3.9(9) . . . . ? N4 C10 C11 C14 0.3(10) . . . . ? C9 C10 C11 C14 179.2(6) . . . . ? N4 C10 C11 C12 -177.8(6) . . . . ? C9 C10 C11 C12 1.1(9) . . . . ? C10 C11 C12 C13 2.3(11) . . . . ? C14 C11 C12 C13 -175.7(8) . . . . ? C11 C12 C13 C8 -2.9(12) . . . . ? C7 C8 C13 C12 177.4(8) . . . . ? C9 C8 C13 C12 0.1(11) . . . . ? C10 C11 C14 C15 -0.4(11) . . . . ? C12 C11 C14 C15 177.6(7) . . . . ? C11 C14 C15 C16 0.0(12) . . . . ? C10 N4 C16 C15 -0.8(10) . . . . ? Mo1 N4 C16 C15 174.7(5) . . . . ? C14 C15 C16 N4 0.7(12) . . . . ? Mo1 S3 C17 C22 -100.5(6) . . . . ? Mo1 S3 C17 C18 79.0(6) . . . . ? C22 C17 C18 C19 1.0(11) . . . . ? S3 C17 C18 C19 -178.5(6) . . . . ? C17 C18 C19 C20 -1.0(14) . . . . ? C18 C19 C20 C21 1.2(17) . . . . ? C18 C19 C20 C23 179.0(17) . . . . ? C19 C20 C21 C22 -1.4(16) . . . . ? C23 C20 C21 C22 -179.4(16) . . . . ? C20 C21 C22 C17 1.5(14) . . . . ? C18 C17 C22 C21 -1.3(11) . . . . ? S3 C17 C22 C21 178.2(7) . . . . ? C28 N5 C24 C25 -62.0(8) . . . . ? C32 N5 C24 C25 177.3(7) . . . . ? C36 N5 C24 C25 56.7(8) . . . . ? N5 C24 C25 C26 177.6(6) . . . . ? C24 C25 C26 C27 -179.9(9) . . . . ? C32 N5 C28 C29 59.6(8) . . . . ? C24 N5 C28 C29 -59.1(8) . . . . ? C36 N5 C28 C29 179.2(6) . . . . ? N5 C28 C29 C30 -177.7(6) . . . . ? C28 C29 C30 C31 178.4(7) . . . . ? C28 N5 C32 C33 59.4(9) . . . . ? C24 N5 C32 C33 -179.5(7) . . . . ? C36 N5 C32 C33 -58.0(9) . . . . ? N5 C32 C33 C34 -174.7(8) . . . . ? C32 C33 C34 C35 -73.1(14) . . . . ? C28 N5 C36 C37 -176.6(7) . . . . ? C32 N5 C36 C37 -56.7(9) . . . . ? C24 N5 C36 C37 62.1(8) . . . . ? N5 C36 C37 C38 -172.9(7) . . . . ? C36 C37 C38 C39 75.3(12) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 2.830 _refine_diff_density_min -0.843 _refine_diff_density_rms 0.149