# Copyright The Royal Society of Chemistry, 1998 data_1 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ; cis-Dioxo-(S-benzyl-3-(2-mercapto-phenyl)-methylendithiocarbazate) (4-methyl-pyridine)molybdenum(VI) ; _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C22 H21 Mo N3 O2 S3' _chemical_formula_weight 551.54 _chemical_melting_point ? _chemical_compound_source ? 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 P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.779(2) _cell_length_b 12.678(2) _cell_length_c 17.567(3) _cell_angle_alpha 90.00 _cell_angle_beta 100.89(2) _cell_angle_gamma 90.00 _cell_volume 2357.4(7) _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 needles _exptl_crystal_colour orange _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.554 _exptl_crystal_density_method ? _exptl_crystal_F_000 1120 _exptl_absorpt_coefficient_mu 0.846 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5446 _diffrn_reflns_av_R_equivalents 0.0518 _diffrn_reflns_av_sigmaI/netI 0.0556 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.36 _diffrn_reflns_theta_max 27.06 _reflns_number_total 5160 _reflns_number_observed 3544 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0488P)^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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5160 _refine_ls_number_parameters 280 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0625 _refine_ls_R_factor_obs 0.0375 _refine_ls_wR_factor_all 0.0902 _refine_ls_wR_factor_obs 0.0839 _refine_ls_goodness_of_fit_all 0.887 _refine_ls_goodness_of_fit_obs 1.007 _refine_ls_restrained_S_all 0.887 _refine_ls_restrained_S_obs 1.007 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Mo1 Mo 0.02184(3) 0.14935(2) 0.71801(2) 0.03958(9) Uani 1 d . . S1 S -0.13831(8) 0.02061(8) 0.72676(5) 0.0475(2) Uani 1 d . . S2 S 0.24639(10) 0.19700(8) 0.73525(6) 0.0569(3) Uani 1 d . . S3 S 0.46903(10) 0.06285(11) 0.77254(8) 0.0819(4) Uani 1 d . . O1 O -0.0154(3) 0.2523(2) 0.77149(13) 0.0595(7) Uani 1 d . . O2 O -0.0314(2) 0.1827(2) 0.62409(13) 0.0530(6) Uani 1 d . . N1 N 0.1168(2) 0.0024(2) 0.67947(14) 0.0355(6) Uani 1 d . . N2 N 0.2466(3) -0.0151(2) 0.7091(2) 0.0453(7) Uani 1 d . . N3 N 0.1026(2) 0.0690(2) 0.84288(14) 0.0371(6) Uani 1 d . . C1 C -0.1654(3) -0.0324(2) 0.6327(2) 0.0408(7) Uani 1 d . . C2 C -0.2918(4) -0.0450(3) 0.5972(2) 0.0573(10) Uani 1 d . . H2 H -0.3552(4) -0.0262(3) 0.6239(2) 0.069 Uiso 1 calc R . C3 C -0.3235(4) -0.0851(3) 0.5229(2) 0.0644(11) Uani 1 d . . H3 H -0.4081(4) -0.0936(3) 0.5001(2) 0.077 Uiso 1 calc R . C4 C -0.2314(4) -0.1123(3) 0.4829(2) 0.0584(10) Uani 1 d . . H4 H -0.2531(4) -0.1363(3) 0.4321(2) 0.070 Uiso 1 calc R . C5 C -0.1065(4) -0.1043(3) 0.5179(2) 0.0453(8) Uani 1 d . . H5 H -0.0447(4) -0.1255(3) 0.4908(2) 0.054 Uiso 1 calc R . C6 C -0.0695(3) -0.0649(2) 0.5937(2) 0.0376(7) Uani 1 d . . C7 C 0.0672(3) -0.0663(2) 0.6282(2) 0.0365(7) Uani 1 d . . C8 C 0.1472(4) -0.1502(3) 0.6005(2) 0.0574(9) Uani 1 d . . H8A H 0.2332(4) -0.1427(3) 0.6270(2) 0.069 Uiso 1 calc R . H8B H 0.1432(4) -0.1427(3) 0.5457(2) 0.069 Uiso 1 calc R . H8C H 0.1163(4) -0.2186(3) 0.6111(2) 0.069 Uiso 1 calc R . C9 C 0.3056(3) 0.0698(3) 0.7349(2) 0.0502(9) Uani 1 d . . C10 C 0.4993(4) -0.0783(4) 0.7762(3) 0.086(2) Uani 1 d . . H10A H 0.4535(4) -0.1100(4) 0.7289(3) 0.103 Uiso 1 calc R . H10B H 0.5886(4) -0.0898(4) 0.7776(3) 0.103 Uiso 1 calc R . C11 C 0.4628(4) -0.1337(4) 0.8438(3) 0.0680(12) Uani 1 d . . C12 C 0.3786(5) -0.2158(4) 0.8338(4) 0.094(2) Uani 1 d . . H12 H 0.3406(5) -0.2362(4) 0.7841(4) 0.112 Uiso 1 calc R . C13 C 0.3500(5) -0.2679(4) 0.8964(5) 0.110(2) Uani 1 d . . H13 H 0.2920(5) -0.3230(4) 0.8883(5) 0.132 Uiso 1 calc R . C14 C 0.4040(4) -0.2413(4) 0.9703(4) 0.092(2) Uani 1 d . . H14 H 0.3846(4) -0.2785(4) 1.0122(4) 0.110 Uiso 1 calc R . C15 C 0.4866(5) -0.1596(4) 0.9817(3) 0.0896(15) Uani 1 d . . H15 H 0.5250(5) -0.1403(4) 1.0317(3) 0.108 Uiso 1 calc R . C16 C 0.5136(4) -0.1052(4) 0.9187(3) 0.0869(15) Uani 1 d . . H16 H 0.5678(4) -0.0475(4) 0.9272(3) 0.104 Uiso 1 calc R . C17 C 0.1368(3) 0.1339(2) 0.9037(2) 0.0429(8) Uani 1 d . . H17 H 0.1402(3) 0.2060(2) 0.8943(2) 0.051 Uiso 1 calc R . C18 C 0.1667(3) 0.0995(3) 0.9787(2) 0.0459(8) Uani 1 d . . H18 H 0.1894(3) 0.1479(3) 1.0187(2) 0.055 Uiso 1 calc R . C19 C 0.1634(3) -0.0079(3) 0.9956(2) 0.0388(7) Uani 1 d . . C20 C 0.1320(3) -0.0743(3) 0.9330(2) 0.0436(8) Uani 1 d . . H20 H 0.1306(3) -0.1468(3) 0.9408(2) 0.052 Uiso 1 calc R . C21 C 0.1027(3) -0.0344(2) 0.8592(2) 0.0410(7) Uani 1 d . . H21 H 0.0819(3) -0.0816(2) 0.8182(2) 0.049 Uiso 1 calc R . C22 C 0.1918(3) -0.0480(3) 1.0771(2) 0.0526(9) Uani 1 d . . H22A H 0.2115(3) 0.0102(3) 1.1122(2) 0.063 Uiso 1 calc R . H22B H 0.2626(3) -0.0952(3) 1.0832(2) 0.063 Uiso 1 calc R . H22C H 0.1195(3) -0.0849(3) 1.0882(2) 0.063 Uiso 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 0.0545(2) 0.03091(13) 0.03257(14) -0.00099(12) 0.00641(11) 0.00812(14) S1 0.0448(5) 0.0651(6) 0.0338(4) -0.0043(4) 0.0107(4) 0.0000(4) S2 0.0664(6) 0.0467(5) 0.0573(5) 0.0006(4) 0.0111(5) -0.0176(5) S3 0.0464(6) 0.1012(9) 0.0931(9) 0.0136(7) 0.0003(6) -0.0147(6) O1 0.091(2) 0.0403(13) 0.0456(14) -0.0050(11) 0.0086(13) 0.0197(13) O2 0.068(2) 0.0484(14) 0.0403(12) 0.0032(10) 0.0053(11) 0.0152(12) N1 0.0406(14) 0.0335(13) 0.0333(13) 0.0017(10) 0.0091(11) 0.0022(11) N2 0.039(2) 0.050(2) 0.048(2) 0.0021(13) 0.0097(12) 0.0055(13) N3 0.0435(15) 0.0335(13) 0.0333(13) -0.0006(10) 0.0050(11) -0.0002(11) C1 0.048(2) 0.041(2) 0.033(2) 0.0013(13) 0.0047(14) -0.0045(15) C2 0.051(2) 0.066(2) 0.054(2) -0.001(2) 0.006(2) -0.007(2) C3 0.062(3) 0.065(3) 0.057(2) 0.001(2) -0.014(2) -0.018(2) C4 0.085(3) 0.048(2) 0.036(2) 0.000(2) -0.004(2) -0.016(2) C5 0.067(2) 0.035(2) 0.033(2) 0.0013(14) 0.010(2) -0.008(2) C6 0.052(2) 0.0305(15) 0.0299(15) 0.0037(12) 0.0060(14) -0.0058(14) C7 0.051(2) 0.0301(15) 0.0324(15) 0.0041(12) 0.0174(14) 0.0034(14) C8 0.073(3) 0.042(2) 0.062(2) -0.010(2) 0.024(2) 0.006(2) C9 0.044(2) 0.063(2) 0.044(2) 0.006(2) 0.011(2) -0.006(2) C10 0.044(3) 0.120(4) 0.090(4) -0.006(3) 0.005(2) 0.023(3) C11 0.034(2) 0.073(3) 0.093(3) -0.010(3) 0.002(2) 0.012(2) C12 0.080(4) 0.058(3) 0.126(5) -0.012(3) -0.022(3) 0.003(3) C13 0.070(3) 0.051(3) 0.193(7) 0.016(4) -0.020(4) -0.013(2) C14 0.050(3) 0.074(3) 0.150(5) 0.038(3) 0.014(3) 0.009(2) C15 0.073(3) 0.102(4) 0.092(4) 0.001(3) 0.012(3) -0.017(3) C16 0.058(3) 0.099(4) 0.099(4) 0.005(3) 0.003(3) -0.029(3) C17 0.052(2) 0.032(2) 0.042(2) -0.0035(13) 0.0036(15) -0.0001(14) C18 0.052(2) 0.045(2) 0.037(2) -0.0071(15) -0.0016(15) -0.004(2) C19 0.031(2) 0.048(2) 0.037(2) 0.0038(14) 0.0038(13) -0.0034(14) C20 0.048(2) 0.034(2) 0.048(2) 0.0008(14) 0.008(2) -0.0016(15) C21 0.051(2) 0.034(2) 0.037(2) -0.0062(13) 0.0046(14) 0.0008(14) C22 0.053(2) 0.063(2) 0.040(2) 0.009(2) 0.003(2) -0.008(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 O2 1.695(2) . ? Mo1 O1 1.700(2) . ? Mo1 N1 2.288(2) . ? Mo1 S1 2.4017(10) . ? Mo1 N3 2.426(2) . ? Mo1 S2 2.4572(11) . ? S1 C1 1.756(3) . ? S2 C9 1.735(4) . ? S3 C9 1.763(4) . ? S3 C10 1.818(6) . ? N1 C7 1.294(4) . ? N1 N2 1.415(4) . ? N2 C9 1.288(4) . ? N3 C21 1.342(4) . ? N3 C17 1.343(4) . ? C1 C2 1.396(5) . ? C1 C6 1.406(5) . ? C2 C3 1.382(5) . ? C3 C4 1.365(6) . ? C4 C5 1.374(5) . ? C5 C6 1.407(4) . ? C6 C7 1.483(4) . ? C7 C8 1.507(4) . ? C10 C11 1.494(7) . ? C11 C12 1.370(6) . ? C11 C16 1.375(6) . ? C12 C13 1.367(8) . ? C13 C14 1.360(8) . ? C14 C15 1.356(7) . ? C15 C16 1.381(7) . ? C17 C18 1.368(4) . ? C18 C19 1.395(5) . ? C19 C20 1.376(4) . ? C19 C22 1.496(4) . ? C20 C21 1.372(4) . ? 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 O2 Mo1 O1 105.97(11) . . ? O2 Mo1 N1 90.16(10) . . ? O1 Mo1 N1 162.53(10) . . ? O2 Mo1 S1 96.69(9) . . ? O1 Mo1 S1 103.82(10) . . ? N1 Mo1 S1 80.37(7) . . ? O2 Mo1 N3 169.29(10) . . ? O1 Mo1 N3 84.51(10) . . ? N1 Mo1 N3 79.73(8) . . ? S1 Mo1 N3 78.26(7) . . ? O2 Mo1 S2 101.72(9) . . ? O1 Mo1 S2 94.18(10) . . ? N1 Mo1 S2 75.62(7) . . ? S1 Mo1 S2 149.58(3) . . ? N3 Mo1 S2 79.32(7) . . ? C1 S1 Mo1 101.18(11) . . ? C9 S2 Mo1 97.21(12) . . ? C9 S3 C10 102.8(2) . . ? C7 N1 N2 113.6(3) . . ? C7 N1 Mo1 127.2(2) . . ? N2 N1 Mo1 119.0(2) . . ? C9 N2 N1 112.8(3) . . ? C21 N3 C17 116.1(3) . . ? C21 N3 Mo1 126.0(2) . . ? C17 N3 Mo1 117.4(2) . . ? C2 C1 C6 119.6(3) . . ? C2 C1 S1 116.1(3) . . ? C6 C1 S1 124.3(2) . . ? C3 C2 C1 120.7(4) . . ? C4 C3 C2 120.3(4) . . ? C3 C4 C5 119.8(3) . . ? C4 C5 C6 121.9(3) . . ? C1 C6 C5 117.5(3) . . ? C1 C6 C7 124.7(3) . . ? C5 C6 C7 117.7(3) . . ? N1 C7 C6 121.6(3) . . ? N1 C7 C8 120.9(3) . . ? C6 C7 C8 117.5(3) . . ? N2 C9 S2 128.3(3) . . ? N2 C9 S3 118.9(3) . . ? S2 C9 S3 112.8(2) . . ? C11 C10 S3 114.7(3) . . ? C12 C11 C16 117.1(5) . . ? C12 C11 C10 121.5(5) . . ? C16 C11 C10 121.4(4) . . ? C13 C12 C11 120.6(5) . . ? C14 C13 C12 121.8(5) . . ? C15 C14 C13 118.8(6) . . ? C14 C15 C16 119.6(5) . . ? C11 C16 C15 122.0(5) . . ? N3 C17 C18 123.4(3) . . ? C17 C18 C19 120.4(3) . . ? C20 C19 C18 116.1(3) . . ? C20 C19 C22 122.1(3) . . ? C18 C19 C22 121.8(3) . . ? C21 C20 C19 120.5(3) . . ? N3 C21 C20 123.5(3) . . ? _refine_diff_density_max 0.355 _refine_diff_density_min -1.182 _refine_diff_density_rms 0.074 # = END data_2 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ; cis-Dioxo-1(1-(2-mercapto-acetophenone)-4-triphenylmethylthiosemicarbazone -S,S,N))(methanol)molybdenum(VI) ; _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C31 H33 Mo N3 O5 S2' _chemical_formula_weight 687.66 _chemical_melting_point ? _chemical_compound_source ? 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.715(2) _cell_length_b 10.256(2) _cell_length_c 18.122(3) _cell_angle_alpha 75.660(10) _cell_angle_beta 83.290(10) _cell_angle_gamma 64.600(10) _cell_volume 1580.1(5) _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 needles _exptl_crystal_colour orange _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.445 _exptl_crystal_density_method ? _exptl_crystal_F_000 708 _exptl_absorpt_coefficient_mu 0.590 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5347 _diffrn_reflns_av_R_equivalents 0.0313 _diffrn_reflns_av_sigmaI/netI 0.0697 _diffrn_reflns_limit_h_min -2 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 24.06 _reflns_number_total 4997 _reflns_number_observed 3730 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0881P)^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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4997 _refine_ls_number_parameters 415 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0713 _refine_ls_R_factor_obs 0.0507 _refine_ls_wR_factor_all 0.1339 _refine_ls_wR_factor_obs 0.1253 _refine_ls_goodness_of_fit_all 0.958 _refine_ls_goodness_of_fit_obs 1.051 _refine_ls_restrained_S_all 0.959 _refine_ls_restrained_S_obs 1.053 _refine_ls_shift/esd_max 0.133 _refine_ls_shift/esd_mean 0.003 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Mo1 Mo 0.19294(5) 0.19640(5) 0.18314(3) 0.0210(2) Uani 1 d . . S1 S 0.09963(15) 0.21138(15) 0.06367(7) 0.0251(3) Uani 1 d . . S2 S 0.24721(15) 0.07736(14) 0.31739(7) 0.0234(3) Uani 1 d . . O1 O 0.3707(4) 0.1924(4) 0.1623(2) 0.0340(9) Uani 1 d . . O2 O 0.0779(4) 0.3732(4) 0.1896(2) 0.0290(9) Uani 1 d . . O3 O 0.3086(4) -0.0480(4) 0.1710(2) 0.0290(9) Uani 1 d . . O4 O 0.2181(6) -0.1867(6) 0.0995(3) 0.0619(14) Uani 1 d . . H4 H 0.1478(68) -0.2124(99) 0.1102(3) 0.093 Uiso 1 calc R . N1 N 0.0056(5) 0.1134(4) 0.2256(2) 0.0187(9) Uani 1 d . . N2 N 0.0367(5) -0.0113(4) 0.2866(2) 0.0217(9) Uani 1 d . . N3 N 0.1797(5) -0.1395(5) 0.3949(2) 0.0199(9) Uani 1 d . . H3N H 0.2563(71) -0.1555(66) 0.4168(34) 0.036(18) Uiso 1 d . . C1 C -0.0943(6) 0.3293(6) 0.0738(3) 0.0236(11) Uani 1 d . . C2 C -0.1610(6) 0.4497(6) 0.0155(3) 0.0302(13) Uani 1 d . . H2 H -0.1017(6) 0.4668(6) -0.0267(3) 0.036 Uiso 1 calc R . C3 C -0.3141(7) 0.5472(6) 0.0172(3) 0.0378(15) Uani 1 d . . H3 H -0.3555(7) 0.6303(6) -0.0220(3) 0.045 Uiso 1 calc R . C4 C -0.4031(6) 0.5170(6) 0.0788(3) 0.0352(14) Uani 1 d . . H4A H -0.5061(6) 0.5793(6) 0.0807(3) 0.042 Uiso 1 calc R . C5 C -0.3400(6) 0.3959(6) 0.1370(3) 0.0301(13) Uani 1 d . . H5A H -0.4012(6) 0.3784(6) 0.1782(3) 0.036 Uiso 1 calc R . C6 C -0.1848(6) 0.2968(6) 0.1361(3) 0.0231(11) Uani 1 d . . C7 C -0.1296(6) 0.1648(5) 0.1997(3) 0.0206(11) Uani 1 d . . C8 C -0.2399(7) 0.0981(7) 0.2340(3) 0.040(2) Uani 1 d . . H8A H -0.3113(29) 0.1169(40) 0.1960(7) 0.060 Uiso 1 calc R . H8B H -0.2938(33) 0.1417(32) 0.2758(15) 0.060 Uiso 1 calc R . H8C H -0.1851(8) -0.0067(9) 0.2519(21) 0.060 Uiso 1 calc R . C9 C 0.1414(5) -0.0304(5) 0.3308(3) 0.0183(11) Uani 1 d . . C10 C 0.1210(5) -0.2539(5) 0.4246(3) 0.0179(10) Uani 1 d . . C11 C -0.0544(5) -0.1856(5) 0.4174(3) 0.0179(10) Uani 1 d . . C12 C -0.1294(6) -0.2556(6) 0.3938(3) 0.0237(11) Uani 1 d . . H12 H -0.0736(6) -0.3440(6) 0.3781(3) 0.028 Uiso 1 calc R . C13 C -0.2879(6) -0.1951(6) 0.3931(3) 0.0286(13) Uani 1 d . . H13 H -0.3372(6) -0.2434(6) 0.3770(3) 0.034 Uiso 1 calc R . C14 C -0.3720(6) -0.0650(6) 0.4159(3) 0.0278(12) Uani 1 d . . H14 H -0.4778(6) -0.0260(6) 0.4161(3) 0.033 Uiso 1 calc R . C15 C -0.2990(6) 0.0082(6) 0.4386(3) 0.0267(12) Uani 1 d . . H15 H -0.3557(6) 0.0971(6) 0.4535(3) 0.032 Uiso 1 calc R . C16 C -0.1406(6) -0.0515(6) 0.4391(3) 0.0245(12) Uani 1 d . . H16 H -0.0917(6) -0.0016(6) 0.4539(3) 0.029 Uiso 1 calc R . C17 C 0.1984(5) -0.3839(5) 0.3835(3) 0.0190(11) Uani 1 d . . C18 C 0.2273(6) -0.5290(6) 0.4223(3) 0.0239(12) Uani 1 d . . H18 H 0.1976(6) -0.5472(6) 0.4732(3) 0.029 Uiso 1 calc R . C19 C 0.2991(6) -0.6452(6) 0.3863(3) 0.0265(12) Uani 1 d . . H19 H 0.3185(6) -0.7408(6) 0.4136(3) 0.032 Uiso 1 calc R . C20 C 0.3421(6) -0.6230(6) 0.3119(3) 0.0312(13) Uani 1 d . . H20 H 0.3924(6) -0.7025(6) 0.2885(3) 0.037 Uiso 1 calc R . C21 C 0.3094(6) -0.4790(6) 0.2713(3) 0.0310(13) Uani 1 d . . H21 H 0.3356(6) -0.4622(6) 0.2199(3) 0.037 Uiso 1 calc R . C22 C 0.2386(6) -0.3606(6) 0.3063(3) 0.0275(12) Uani 1 d . . H22 H 0.2176(6) -0.2651(6) 0.2784(3) 0.033 Uiso 1 calc R . C23 C 0.1659(5) -0.3122(5) 0.5092(3) 0.0181(11) Uani 1 d . . C24 C 0.3195(5) -0.3668(6) 0.5281(3) 0.0228(11) Uani 1 d . . H24 H 0.3911(5) -0.3634(6) 0.4896(3) 0.027 Uiso 1 calc R . C25 C 0.3658(6) -0.4250(6) 0.6020(3) 0.0252(12) Uani 1 d . . H25 H 0.4681(6) -0.4601(6) 0.6134(3) 0.030 Uiso 1 calc R . C26 C 0.2608(7) -0.4320(6) 0.6605(3) 0.0302(13) Uani 1 d . . H26 H 0.2923(7) -0.4708(6) 0.7108(3) 0.036 Uiso 1 calc R . C27 C 0.1105(6) -0.3810(6) 0.6427(3) 0.0297(13) Uani 1 d . . H27 H 0.0397(6) -0.3864(6) 0.6813(3) 0.036 Uiso 1 calc R . C28 C 0.0634(6) -0.3213(6) 0.5677(3) 0.0248(12) Uani 1 d . . H28 H -0.0390(6) -0.2868(6) 0.5566(3) 0.030 Uiso 1 calc R . C29 C 0.4610(7) -0.1488(7) 0.1925(4) 0.051(2) Uani 1 d . . H29A H 0.5012(20) -0.2182(33) 0.1600(18) 0.077 Uiso 1 calc R . H29B H 0.4616(9) -0.2010(38) 0.2445(10) 0.077 Uiso 1 calc R . H29C H 0.5229(14) -0.0949(9) 0.1876(26) 0.077 Uiso 1 calc R . C30 C 0.2339(11) -0.1477(9) 0.0182(5) 0.086(3) Uani 1 d . . H30A H 0.1352(13) -0.0870(65) -0.0039(6) 0.130 Uiso 1 calc R . H30B H 0.2802(74) -0.2360(10) -0.0014(7) 0.130 Uiso 1 calc R . H30C H 0.2967(66) -0.0940(68) 0.0056(5) 0.130 Uiso 1 calc R . C31 C -0.1367(11) 0.7344(11) 0.1576(6) 0.090(3) Uani 1 d D . O5 O 0.0182(7) 0.6796(7) 0.1495(4) 0.068(2) Uani 0.816(12) d PD . O6 O -0.0833(28) 0.8514(24) 0.1226(13) 0.051(9) Uani 0.184(12) d PD . C32 C 0.3784(30) -0.0427(39) -0.0736(17) 0.068(11) Uani 0.25 d P . O7 O 0.4611(39) -0.0202(44) -0.0207(31) 0.158(18) Uani 0.25 d P . 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 0.0211(3) 0.0232(3) 0.0212(3) -0.0050(2) -0.0003(2) -0.0115(2) S1 0.0243(7) 0.0293(7) 0.0195(7) -0.0064(5) -0.0001(5) -0.0085(6) S2 0.0275(7) 0.0256(7) 0.0232(7) -0.0028(5) -0.0054(5) -0.0170(6) O1 0.031(2) 0.044(2) 0.037(2) -0.007(2) 0.000(2) -0.026(2) O2 0.035(2) 0.022(2) 0.027(2) -0.004(2) -0.002(2) -0.009(2) O3 0.018(2) 0.032(2) 0.032(2) -0.013(2) -0.004(2) -0.001(2) O4 0.061(4) 0.051(3) 0.085(4) -0.020(3) -0.024(3) -0.026(3) N1 0.021(2) 0.020(2) 0.018(2) -0.005(2) -0.001(2) -0.010(2) N2 0.022(2) 0.021(2) 0.022(2) 0.001(2) -0.004(2) -0.011(2) N3 0.020(2) 0.023(2) 0.020(2) -0.003(2) -0.007(2) -0.011(2) C1 0.026(3) 0.023(3) 0.022(3) -0.006(2) -0.006(2) -0.009(2) C2 0.027(3) 0.033(3) 0.028(3) 0.000(2) -0.002(2) -0.013(3) C3 0.035(3) 0.029(3) 0.037(3) 0.005(3) -0.011(3) -0.006(3) C4 0.024(3) 0.035(3) 0.038(3) -0.001(3) -0.006(3) -0.005(3) C5 0.021(3) 0.037(3) 0.031(3) -0.007(3) -0.001(2) -0.010(3) C6 0.027(3) 0.025(3) 0.019(3) -0.006(2) -0.002(2) -0.011(2) C7 0.018(3) 0.019(3) 0.023(3) -0.005(2) 0.001(2) -0.007(2) C8 0.030(3) 0.054(4) 0.036(3) 0.013(3) -0.013(3) -0.027(3) C9 0.017(3) 0.018(3) 0.022(3) -0.008(2) 0.002(2) -0.008(2) C10 0.015(3) 0.020(3) 0.018(3) -0.004(2) -0.002(2) -0.007(2) C11 0.013(2) 0.019(3) 0.017(2) -0.001(2) -0.003(2) -0.003(2) C12 0.023(3) 0.028(3) 0.022(3) -0.004(2) -0.003(2) -0.012(2) C13 0.021(3) 0.039(3) 0.030(3) -0.005(2) -0.006(2) -0.016(3) C14 0.014(3) 0.034(3) 0.031(3) -0.004(2) -0.001(2) -0.007(2) C15 0.020(3) 0.021(3) 0.033(3) -0.007(2) -0.003(2) -0.001(2) C16 0.024(3) 0.028(3) 0.024(3) -0.012(2) -0.001(2) -0.009(2) C17 0.010(2) 0.024(3) 0.024(3) -0.011(2) 0.000(2) -0.005(2) C18 0.026(3) 0.026(3) 0.027(3) -0.008(2) 0.005(2) -0.017(2) C19 0.021(3) 0.024(3) 0.039(3) -0.010(2) 0.004(2) -0.013(2) C20 0.021(3) 0.038(3) 0.044(4) -0.029(3) 0.005(3) -0.012(3) C21 0.026(3) 0.041(3) 0.023(3) -0.015(3) -0.003(2) -0.006(3) C22 0.026(3) 0.028(3) 0.024(3) -0.005(2) -0.001(2) -0.006(2) C23 0.018(3) 0.019(2) 0.018(3) -0.005(2) 0.000(2) -0.007(2) C24 0.015(3) 0.028(3) 0.028(3) -0.008(2) 0.001(2) -0.011(2) C25 0.023(3) 0.028(3) 0.024(3) -0.006(2) -0.006(2) -0.009(2) C26 0.041(3) 0.029(3) 0.020(3) -0.008(2) -0.005(2) -0.011(3) C27 0.032(3) 0.028(3) 0.023(3) -0.004(2) 0.004(2) -0.008(3) C28 0.019(3) 0.029(3) 0.025(3) -0.006(2) -0.002(2) -0.009(2) C29 0.022(3) 0.047(4) 0.081(5) -0.030(4) -0.009(3) 0.000(3) C30 0.104(8) 0.059(5) 0.092(7) -0.035(5) -0.050(6) -0.007(5) C31 0.070(6) 0.075(6) 0.083(7) -0.012(5) 0.016(5) 0.001(5) O5 0.053(4) 0.045(4) 0.110(6) -0.016(4) -0.021(4) -0.018(3) O6 0.061(18) 0.041(15) 0.043(15) -0.007(12) -0.019(12) -0.012(13) C32 0.028(14) 0.112(27) 0.066(20) -0.082(20) -0.009(13) 0.004(16) O7 0.081(28) 0.112(28) 0.266(57) -0.025(30) 0.005(29) -0.037(21) _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 O2 1.699(3) . ? Mo1 O1 1.709(4) . ? Mo1 N1 2.304(4) . ? Mo1 O3 2.322(4) . ? Mo1 S1 2.3890(14) . ? Mo1 S2 2.4420(14) . ? S1 C1 1.767(5) . ? S2 C9 1.767(5) . ? O3 C29 1.427(7) . ? O4 C30 1.437(10) . ? N1 C7 1.285(6) . ? N1 N2 1.412(5) . ? N2 C9 1.287(6) . ? N3 C9 1.355(6) . ? N3 C10 1.477(6) . ? C1 C2 1.374(7) . ? C1 C6 1.411(7) . ? C2 C3 1.393(8) . ? C3 C4 1.387(8) . ? C4 C5 1.371(8) . ? C5 C6 1.412(7) . ? C6 C7 1.482(7) . ? C7 C8 1.505(7) . ? C10 C23 1.542(7) . ? C10 C11 1.547(6) . ? C10 C17 1.549(7) . ? C11 C12 1.381(7) . ? C11 C16 1.396(7) . ? C12 C13 1.392(7) . ? C13 C14 1.370(8) . ? C14 C15 1.383(8) . ? C15 C16 1.391(7) . ? C17 C22 1.396(7) . ? C17 C18 1.399(7) . ? C18 C19 1.378(7) . ? C19 C20 1.358(8) . ? C20 C21 1.392(8) . ? C21 C22 1.384(7) . ? C23 C28 1.381(7) . ? C23 C24 1.402(7) . ? C24 C25 1.367(7) . ? C25 C26 1.393(8) . ? C26 C27 1.371(8) . ? C27 C28 1.388(7) . ? C31 O5 1.366(11) . ? C31 O6 1.48(2) . ? O5 O6 1.58(2) . ? C32 O7 1.44(4) . ? O7 O7 1.36(8) 2_655 ? 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 O2 Mo1 O1 105.7(2) . . ? O2 Mo1 N1 93.4(2) . . ? O1 Mo1 N1 159.6(2) . . ? O2 Mo1 O3 169.4(2) . . ? O1 Mo1 O3 84.3(2) . . ? N1 Mo1 O3 77.23(14) . . ? O2 Mo1 S1 96.17(13) . . ? O1 Mo1 S1 104.38(13) . . ? N1 Mo1 S1 80.28(10) . . ? O3 Mo1 S1 77.54(9) . . ? O2 Mo1 S2 100.81(12) . . ? O1 Mo1 S2 94.31(13) . . ? N1 Mo1 S2 74.57(10) . . ? O3 Mo1 S2 81.65(10) . . ? S1 Mo1 S2 150.29(5) . . ? C1 S1 Mo1 99.8(2) . . ? C9 S2 Mo1 99.0(2) . . ? C29 O3 Mo1 125.1(4) . . ? C7 N1 N2 112.5(4) . . ? C7 N1 Mo1 128.2(3) . . ? N2 N1 Mo1 119.3(3) . . ? C9 N2 N1 113.1(4) . . ? C9 N3 C10 129.4(4) . . ? C2 C1 C6 119.4(5) . . ? C2 C1 S1 118.1(4) . . ? C6 C1 S1 122.2(4) . . ? C1 C2 C3 122.5(5) . . ? C4 C3 C2 118.2(5) . . ? C5 C4 C3 120.3(5) . . ? C4 C5 C6 121.9(5) . . ? C1 C6 C5 117.4(5) . . ? C1 C6 C7 124.8(5) . . ? C5 C6 C7 117.8(5) . . ? N1 C7 C6 120.7(5) . . ? N1 C7 C8 121.9(4) . . ? C6 C7 C8 117.3(4) . . ? N2 C9 N3 121.2(4) . . ? N2 C9 S2 125.7(4) . . ? N3 C9 S2 113.1(4) . . ? N3 C10 C23 105.4(4) . . ? N3 C10 C11 110.4(4) . . ? C23 C10 C11 110.1(4) . . ? N3 C10 C17 110.9(4) . . ? C23 C10 C17 108.6(4) . . ? C11 C10 C17 111.2(4) . . ? C12 C11 C16 118.7(5) . . ? C12 C11 C10 122.4(4) . . ? C16 C11 C10 118.8(4) . . ? C11 C12 C13 120.6(5) . . ? C14 C13 C12 120.5(5) . . ? C13 C14 C15 119.9(5) . . ? C14 C15 C16 119.9(5) . . ? C15 C16 C11 120.5(5) . . ? C22 C17 C18 117.7(5) . . ? C22 C17 C10 121.6(4) . . ? C18 C17 C10 120.7(4) . . ? C19 C18 C17 120.8(5) . . ? C20 C19 C18 121.4(5) . . ? C19 C20 C21 118.8(5) . . ? C22 C21 C20 120.9(5) . . ? C21 C22 C17 120.3(5) . . ? C28 C23 C24 117.8(5) . . ? C28 C23 C10 123.2(4) . . ? C24 C23 C10 118.9(4) . . ? C25 C24 C23 121.0(5) . . ? C24 C25 C26 120.5(5) . . ? C27 C26 C25 119.1(5) . . ? C26 C27 C28 120.4(5) . . ? C23 C28 C27 121.1(5) . . ? O5 C31 O6 67.5(11) . . ? C31 O5 O6 59.7(9) . . ? C31 O6 O5 52.8(7) . . ? O7 O7 C32 170.9(60) 2_655 . ? _refine_diff_density_max 0.867 _refine_diff_density_min -1.077 _refine_diff_density_rms 0.114 # = END data_3 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ; (2-oxo)Bis(1-mercaptobenzaldehyde) -4-triphenylmethylthiosemicarbazone-S,S,N)-oxo-molybdenum(V) ; _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C57 H48 Cl6 Mo2 N6 O3 S4' _chemical_formula_weight 1397.83 _chemical_melting_point ? _chemical_compound_source ? 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' 'Cl' 'Cl' 0.1484 0.1585 '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 19.449(4) _cell_length_b 19.763(4) _cell_length_c 18.450(4) _cell_angle_alpha 90.00 _cell_angle_beta 121.59(3) _cell_angle_gamma 90.00 _cell_volume 6040.8(22) _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 ? _exptl_crystal_colour 'deep red to violet' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.537 _exptl_crystal_density_method ? _exptl_crystal_F_000 2824 _exptl_absorpt_coefficient_mu 0.867 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24807 _diffrn_reflns_av_R_equivalents 0.0892 _diffrn_reflns_av_sigmaI/netI 0.0549 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 5.30 _diffrn_reflns_theta_max 28.03 _reflns_number_total 6700 _reflns_number_observed 4575 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 14 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0889P)^2^+19.4345P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0039(5) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 6686 _refine_ls_number_parameters 355 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1017 _refine_ls_R_factor_obs 0.0672 _refine_ls_wR_factor_all 0.2131 _refine_ls_wR_factor_obs 0.1657 _refine_ls_goodness_of_fit_all 1.080 _refine_ls_goodness_of_fit_obs 1.036 _refine_ls_restrained_S_all 1.093 _refine_ls_restrained_S_obs 1.036 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Mo1 Mo 0.05650(3) 0.07819(2) 0.05525(3) 0.0600(2) Uani 1 d . . S1 S -0.04466(9) 0.13978(7) -0.06361(9) 0.0665(4) Uani 1 d . . S2 S 0.07307(11) 0.02404(7) 0.17726(11) 0.0749(5) Uani 1 d . . O1 O 0.0000 0.0000 0.0000 0.078(2) Uani 1 d S . O2 O 0.1419(3) 0.0797(3) 0.0558(4) 0.0920(15) Uani 1 d . . N1 N 0.0568(3) 0.1735(2) 0.1124(3) 0.0594(11) Uani 1 d . . N2 N 0.0386(3) 0.2321(2) 0.0610(3) 0.0651(12) Uani 1 d . . N3 N -0.0325(3) 0.2713(2) -0.0760(3) 0.0603(11) Uani 1 d . . H3N H -0.0603(3) 0.2604(2) -0.1316(3) 0.080 Uiso 1 d R . C1 C 0.1038(4) 0.0769(3) 0.2648(4) 0.0661(14) Uani 1 d . . C2 C 0.1291(4) 0.0455(4) 0.3418(4) 0.083(2) Uani 1 d . . H2A H 0.1341(4) -0.0029(4) 0.3446(4) 0.080 Uiso 1 d R . C3 C 0.1461(5) 0.0810(4) 0.4129(5) 0.089(2) Uani 1 d . . H3A H 0.1624(5) 0.0577(4) 0.4652(5) 0.080 Uiso 1 d R . C4 C 0.1410(4) 0.1504(4) 0.4097(4) 0.087(2) Uani 1 d . . H4A H 0.1516(4) 0.1757(4) 0.4589(4) 0.080 Uiso 1 d R . C5 C 0.1188(4) 0.1835(4) 0.3359(4) 0.083(2) Uani 1 d . . H5A H 0.1172(4) 0.2320(4) 0.3340(4) 0.080 Uiso 1 d R . C6 C 0.1000(4) 0.1478(3) 0.2611(4) 0.0665(14) Uani 1 d . . C7 C 0.0755(4) 0.1893(3) 0.1882(4) 0.0685(14) Uani 1 d . . H7A H 0.0712(4) 0.2366(3) 0.1970(4) 0.080 Uiso 1 d R . C8 C -0.0083(3) 0.2201(3) -0.0196(4) 0.0606(13) Uani 1 d . . C9 C -0.0177(3) 0.3443(2) -0.0541(3) 0.0527(11) Uani 1 d . . C10 C -0.0391(3) 0.3603(2) 0.0135(3) 0.0562(12) Uani 1 d . . C11 C -0.1114(4) 0.3351(3) 0.0010(4) 0.0672(14) Uani 1 d . . H11A H -0.1452(4) 0.3079(3) -0.0483(4) 0.080 Uiso 1 d R . C12 C -0.1352(4) 0.3495(4) 0.0582(4) 0.080(2) Uani 1 d . . H12A H -0.1851(4) 0.3318(4) 0.0491(4) 0.080 Uiso 1 d R . C13 C -0.0874(5) 0.3887(4) 0.1281(5) 0.088(2) Uani 1 d . . H13A H -0.1032(5) 0.3987(4) 0.1683(5) 0.080 Uiso 1 d R . C14 C -0.0162(5) 0.4133(3) 0.1406(4) 0.078(2) Uani 1 d . . H14A H 0.0170(5) 0.4417(3) 0.1888(4) 0.080 Uiso 1 d R . C15 C 0.0087(4) 0.3989(3) 0.0852(3) 0.0612(13) Uani 1 d . . H15A H 0.0599(4) 0.4150(3) 0.0963(3) 0.080 Uiso 1 d R . C16 C -0.0746(3) 0.3824(2) -0.1380(3) 0.0546(11) Uani 1 d . . C17 C -0.0661(4) 0.3707(3) -0.2066(4) 0.0697(15) Uani 1 d . . H17A H -0.0276(4) 0.3380(3) -0.2022(4) 0.080 Uiso 1 d R . C18 C -0.1149(5) 0.4055(4) -0.2824(4) 0.083(2) Uani 1 d . . H18A H -0.1086(5) 0.3982(4) -0.3300(4) 0.080 Uiso 1 d R . C19 C -0.1715(4) 0.4514(4) -0.2901(4) 0.079(2) Uani 1 d . . H19A H -0.2046(4) 0.4751(4) -0.3428(4) 0.080 Uiso 1 d R . C20 C -0.1796(4) 0.4626(3) -0.2226(5) 0.083(2) Uani 1 d . . H20A H -0.2193(4) 0.4944(3) -0.2280(5) 0.080 Uiso 1 d R . C21 C -0.1315(4) 0.4287(3) -0.1460(4) 0.0674(14) Uani 1 d . . H21A H -0.1373(4) 0.4369(3) -0.0982(4) 0.080 Uiso 1 d R . C22 C 0.0694(3) 0.3641(2) -0.0265(3) 0.0548(11) Uani 1 d . . C23 C 0.0904(4) 0.4315(3) -0.0186(4) 0.0622(13) Uani 1 d . . H23A H 0.0504(4) 0.4651(3) -0.0294(4) 0.080 Uiso 1 d R . C24 C 0.1672(4) 0.4523(3) 0.0033(4) 0.0687(14) Uani 1 d . . H24A H 0.1800(4) 0.4997(3) 0.0088(4) 0.080 Uiso 1 d R . C25 C 0.2246(4) 0.4049(3) 0.0170(4) 0.073(2) Uani 1 d . . H25A H 0.2779(4) 0.4191(3) 0.0328(4) 0.080 Uiso 1 d R . C26 C 0.2050(4) 0.3379(4) 0.0086(5) 0.081(2) Uani 1 d . . H26A H 0.2448(4) 0.3047(4) 0.0178(5) 0.080 Uiso 1 d R . C27 C 0.1285(4) 0.3170(3) -0.0133(4) 0.0690(15) Uani 1 d . . H27A H 0.1157(4) 0.2696(3) -0.0194(4) 0.080 Uiso 1 d R . C1L C 0.0000 -0.1319(6) 0.2500 0.100(3) Uani 1 d S . H1LA H -0.0078 -0.1034(6) 0.2873 0.080 Uiso 1 d R . Cl1 Cl -0.0832(2) -0.1800(2) 0.1915(2) 0.1760(14) Uani 1 d . . C2L C 0.2321(7) 0.3178(6) 0.2156(7) 0.134(4) Uani 1 d . . H2LA H 0.1802(7) 0.3212(6) 0.1641(7) 0.080 Uiso 1 d R . H2LB H 0.2680(7) 0.3483(6) 0.2108(7) 0.080 Uiso 1 d R . Cl3 Cl 0.2658(2) 0.23785(15) 0.2224(2) 0.1439(10) Uani 1 d . . Cl4 Cl 0.2221(2) 0.3434(2) 0.2984(2) 0.1571(12) Uani 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.0671(3) 0.0458(3) 0.0667(3) 0.0011(2) 0.0347(3) 0.0027(2) S1 0.0764(10) 0.0442(7) 0.0622(8) -0.0022(5) 0.0248(7) -0.0036(6) S2 0.0954(12) 0.0523(8) 0.0729(10) 0.0061(6) 0.0412(9) -0.0016(7) O1 0.112(5) 0.049(3) 0.066(3) 0.008(2) 0.042(3) 0.012(3) O2 0.083(3) 0.103(4) 0.105(4) 0.015(3) 0.059(3) 0.017(3) N1 0.065(3) 0.043(2) 0.062(3) -0.002(2) 0.028(2) -0.001(2) N2 0.080(3) 0.042(2) 0.058(3) 0.004(2) 0.025(2) -0.002(2) N3 0.073(3) 0.047(2) 0.049(2) 0.000(2) 0.024(2) 0.000(2) C1 0.064(3) 0.063(3) 0.068(3) 0.009(3) 0.032(3) 0.000(3) C2 0.088(5) 0.083(4) 0.069(4) 0.013(3) 0.034(3) 0.006(4) C3 0.088(5) 0.106(6) 0.069(4) 0.017(4) 0.037(4) 0.005(4) C4 0.088(5) 0.102(6) 0.060(4) 0.002(3) 0.033(3) 0.011(4) C5 0.093(5) 0.077(4) 0.067(4) -0.001(3) 0.035(3) 0.007(3) C6 0.066(3) 0.067(3) 0.062(3) -0.002(3) 0.031(3) 0.000(3) C7 0.079(4) 0.057(3) 0.061(3) 0.000(2) 0.031(3) 0.002(3) C8 0.067(3) 0.047(3) 0.060(3) 0.002(2) 0.028(3) -0.001(2) C9 0.063(3) 0.040(2) 0.049(3) 0.001(2) 0.026(2) 0.002(2) C10 0.069(3) 0.046(2) 0.054(3) 0.004(2) 0.032(2) 0.002(2) C11 0.078(4) 0.063(3) 0.064(3) 0.003(2) 0.039(3) -0.004(3) C12 0.082(4) 0.088(4) 0.076(4) 0.012(3) 0.046(4) -0.005(3) C13 0.105(6) 0.103(5) 0.074(4) -0.001(4) 0.060(4) -0.002(4) C14 0.094(5) 0.082(4) 0.054(3) -0.006(3) 0.037(3) -0.005(3) C15 0.070(3) 0.060(3) 0.051(3) 0.004(2) 0.030(3) 0.003(3) C16 0.062(3) 0.047(3) 0.051(3) 0.001(2) 0.027(2) -0.002(2) C17 0.076(4) 0.074(4) 0.058(3) 0.001(3) 0.033(3) 0.003(3) C18 0.092(5) 0.096(5) 0.056(3) 0.008(3) 0.036(3) 0.004(4) C19 0.076(4) 0.084(4) 0.057(3) 0.016(3) 0.022(3) 0.004(3) C20 0.077(4) 0.076(4) 0.081(5) 0.016(3) 0.032(3) 0.021(3) C21 0.078(4) 0.063(3) 0.060(3) 0.006(2) 0.035(3) 0.010(3) C22 0.065(3) 0.048(3) 0.049(3) -0.001(2) 0.027(2) 0.004(2) C23 0.071(3) 0.052(3) 0.063(3) -0.002(2) 0.034(3) 0.002(2) C24 0.074(4) 0.066(3) 0.071(4) -0.009(3) 0.041(3) -0.011(3) C25 0.070(4) 0.079(4) 0.069(4) -0.010(3) 0.036(3) -0.005(3) C26 0.069(4) 0.074(4) 0.099(5) -0.004(3) 0.043(4) 0.014(3) C27 0.073(4) 0.050(3) 0.084(4) -0.002(3) 0.041(3) 0.008(3) C1L 0.116(9) 0.080(7) 0.120(9) 0.000 0.073(8) 0.000 Cl1 0.095(2) 0.241(4) 0.157(3) -0.044(3) 0.042(2) -0.033(2) C2L 0.141(9) 0.144(8) 0.149(9) 0.053(7) 0.098(8) 0.058(7) Cl3 0.104(2) 0.127(2) 0.188(3) 0.020(2) 0.068(2) 0.030(2) Cl4 0.132(2) 0.210(3) 0.142(2) -0.028(2) 0.081(2) -0.004(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 O2 1.656(5) . ? Mo1 O1 1.8604(6) . ? Mo1 N1 2.158(4) . ? Mo1 S2 2.357(2) . ? Mo1 S1 2.375(2) . ? S1 C8 1.754(5) . ? S2 C1 1.745(7) . ? O1 Mo1 1.8603(6) 5 ? N1 C7 1.286(7) . ? N1 N2 1.417(6) . ? N2 C8 1.296(7) . ? N3 C8 1.348(6) . ? N3 C9 1.485(6) . ? C1 C2 1.384(9) . ? C1 C6 1.402(8) . ? C2 C3 1.368(10) . ? C3 C4 1.374(10) . ? C4 C5 1.360(9) . ? C5 C6 1.416(9) . ? C6 C7 1.427(8) . ? C9 C10 1.541(7) . ? C9 C22 1.542(8) . ? C9 C16 1.546(7) . ? C10 C15 1.382(7) . ? C10 C11 1.393(8) . ? C11 C12 1.385(9) . ? C12 C13 1.368(10) . ? C13 C14 1.369(10) . ? C14 C15 1.370(9) . ? C16 C17 1.379(8) . ? C16 C21 1.383(8) . ? C17 C18 1.393(9) . ? C18 C19 1.374(10) . ? C19 C20 1.353(10) . ? C20 C21 1.391(8) . ? C22 C23 1.379(7) . ? C22 C27 1.398(7) . ? C23 C24 1.390(8) . ? C24 C25 1.377(9) . ? C25 C26 1.364(9) . ? C26 C27 1.385(9) . ? C1L Cl1 1.690(7) 2 ? C1L Cl1 1.690(7) . ? C2L Cl3 1.690(10) . ? C2L Cl4 1.716(10) . ? 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 O2 Mo1 O1 108.7(2) . . ? O2 Mo1 N1 103.6(2) . . ? O1 Mo1 N1 147.42(13) . . ? O2 Mo1 S2 111.5(2) . . ? O1 Mo1 S2 83.81(5) . . ? N1 Mo1 S2 88.05(13) . . ? O2 Mo1 S1 109.9(2) . . ? O1 Mo1 S1 87.36(5) . . ? N1 Mo1 S1 78.01(13) . . ? S2 Mo1 S1 138.34(7) . . ? C8 S1 Mo1 95.6(2) . . ? C1 S2 Mo1 114.9(2) . . ? Mo1 O1 Mo1 180.0 5 . ? C7 N1 N2 111.1(4) . . ? C7 N1 Mo1 132.0(4) . . ? N2 N1 Mo1 116.8(3) . . ? C8 N2 N1 113.4(4) . . ? C8 N3 C9 125.5(4) . . ? C2 C1 C6 118.7(6) . . ? C2 C1 S2 116.5(5) . . ? C6 C1 S2 124.8(5) . . ? C3 C2 C1 122.1(7) . . ? C2 C3 C4 119.7(7) . . ? C5 C4 C3 120.1(7) . . ? C4 C5 C6 121.3(7) . . ? C1 C6 C5 118.0(6) . . ? C1 C6 C7 127.0(5) . . ? C5 C6 C7 114.9(6) . . ? N1 C7 C6 130.6(6) . . ? N2 C8 N3 120.0(5) . . ? N2 C8 S1 124.6(4) . . ? N3 C8 S1 115.4(4) . . ? N3 C9 C10 108.9(4) . . ? N3 C9 C22 111.0(4) . . ? C10 C9 C22 113.3(4) . . ? N3 C9 C16 105.4(4) . . ? C10 C9 C16 110.8(4) . . ? C22 C9 C16 107.0(4) . . ? C15 C10 C11 118.1(5) . . ? C15 C10 C9 123.9(5) . . ? C11 C10 C9 118.1(5) . . ? C12 C11 C10 120.8(6) . . ? C13 C12 C11 120.1(7) . . ? C14 C13 C12 119.2(6) . . ? C13 C14 C15 121.4(6) . . ? C14 C15 C10 120.4(6) . . ? C17 C16 C21 119.1(5) . . ? C17 C16 C9 118.0(5) . . ? C21 C16 C9 122.8(5) . . ? C16 C17 C18 119.5(6) . . ? C19 C18 C17 121.2(7) . . ? C20 C19 C18 119.0(6) . . ? C19 C20 C21 121.0(6) . . ? C16 C21 C20 120.1(6) . . ? C23 C22 C27 117.0(5) . . ? C23 C22 C9 119.6(5) . . ? C27 C22 C9 123.3(5) . . ? C22 C23 C24 122.0(6) . . ? C25 C24 C23 119.9(6) . . ? C26 C25 C24 119.1(6) . . ? C25 C26 C27 121.2(6) . . ? C26 C27 C22 120.7(5) . . ? Cl1 C1L Cl1 111.6(7) 2 . ? Cl3 C2L Cl4 115.4(6) . . ? _refine_diff_density_max 0.686 _refine_diff_density_min -1.078 _refine_diff_density_rms 0.097 # = END