MANUSCRIPT # OM040112P _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H9 Mo N O2 S' _chemical_formula_weight 327.20 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)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 6.3568(12) _cell_length_b 12.5627(16) _cell_length_c 14.658(2) _cell_angle_alpha 90.00 _cell_angle_beta 94.750(14) _cell_angle_gamma 90.00 _cell_volume 1166.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.863 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 648 _exptl_absorpt_coefficient_mu 1.289 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.6266 _exptl_absorpt_correction_T_max 0.9383 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2298 _diffrn_reflns_av_R_equivalents 0.0132 _diffrn_reflns_av_sigmaI/netI 0.0284 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 25.30 _reflns_number_total 2065 _reflns_number_gt 1729 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0479P)^2^+0.0614P] 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 SHELXL _refine_ls_extinction_coef 0.0178(9) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2065 _refine_ls_number_parameters 155 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0349 _refine_ls_R_factor_gt 0.0261 _refine_ls_wR_factor_ref 0.0736 _refine_ls_wR_factor_gt 0.0707 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.13163(3) 0.004015(14) 0.298537(14) 0.01643(13) Uani 1 1 d . . . S2 S 0.40544(12) -0.00235(5) 0.18352(6) 0.02710(19) Uani 1 1 d . . . O1 O -0.0453(3) 0.21506(14) 0.37411(13) 0.0324(5) Uani 1 1 d . . . O2 O 0.4998(3) 0.10154(16) 0.42503(15) 0.0415(6) Uani 1 1 d . . . N1 N 0.0416(3) 0.07966(14) 0.16699(13) 0.0173(4) Uani 1 1 d . . . C1 C 0.0171(4) 0.1367(2) 0.34519(17) 0.0214(6) Uani 1 1 d . . . C2 C 0.3658(5) 0.0661(2) 0.37656(19) 0.0278(6) Uani 1 1 d . . . C3 C -0.1298(4) 0.13094(19) 0.12928(18) 0.0221(6) Uani 1 1 d . . . H3 H -0.2463 0.1421 0.1647 0.027 Uiso 1 1 calc R . . C4 C -0.1404(5) 0.1676(2) 0.04073(19) 0.0282(7) Uani 1 1 d . . . H4 H -0.2625 0.2038 0.0151 0.034 Uiso 1 1 calc R . . C5 C 0.0302(5) 0.1507(2) -0.01063(17) 0.0304(7) Uani 1 1 d . . . H5 H 0.0246 0.1751 -0.0721 0.037 Uiso 1 1 calc R . . C6 C 0.2072(5) 0.0990(2) 0.02678(18) 0.0273(6) Uani 1 1 d . . . H6 H 0.3250 0.0876 -0.0079 0.033 Uiso 1 1 calc R . . C7 C 0.2090(4) 0.06362(17) 0.11724(17) 0.0202(5) Uani 1 1 d . . . C8 C -0.1494(5) -0.0923(2) 0.3473(2) 0.0334(7) Uani 1 1 d . . . H8 H -0.2757 -0.0565 0.3595 0.040 Uiso 1 1 calc R . . C9 C 0.0301(6) -0.1067(2) 0.4097(2) 0.0375(8) Uani 1 1 d . . . H9 H 0.0449 -0.0836 0.4716 0.045 Uiso 1 1 calc R . . C10 C 0.1833(5) -0.1615(2) 0.3635(2) 0.0335(7) Uani 1 1 d . . . H10 H 0.3210 -0.1805 0.3883 0.040 Uiso 1 1 calc R . . C11 C 0.0950(4) -0.1830(2) 0.2740(2) 0.0265(6) Uani 1 1 d . . . H11 H 0.1626 -0.2203 0.2282 0.032 Uiso 1 1 calc R . . C12 C -0.1082(4) -0.14025(19) 0.26379(19) 0.0259(6) Uani 1 1 d . . . H12 H -0.2022 -0.1431 0.2100 0.031 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 0.01878(17) 0.01380(17) 0.01672(18) 0.00152(7) 0.00146(11) 0.00140(8) S2 0.0198(4) 0.0306(4) 0.0318(4) 0.0034(3) 0.0077(3) 0.0044(2) O1 0.0412(13) 0.0237(11) 0.0328(11) -0.0021(8) 0.0048(10) 0.0084(9) O2 0.0370(12) 0.0357(12) 0.0486(14) -0.0138(10) -0.0161(11) -0.0008(9) N1 0.0198(11) 0.0136(10) 0.0184(11) 0.0012(8) 0.0017(9) -0.0007(8) C1 0.0242(14) 0.0215(14) 0.0185(13) 0.0042(10) 0.0015(11) -0.0007(11) C2 0.0311(16) 0.0214(14) 0.0309(15) -0.0018(11) 0.0017(13) 0.0068(11) C3 0.0209(14) 0.0158(12) 0.0293(15) 0.0006(10) 0.0007(11) -0.0016(10) C4 0.0379(18) 0.0175(13) 0.0269(14) -0.0010(11) -0.0112(13) -0.0006(11) C5 0.055(2) 0.0193(14) 0.0165(14) -0.0007(10) -0.0008(14) -0.0036(13) C6 0.0419(17) 0.0201(13) 0.0215(14) -0.0022(11) 0.0122(13) -0.0061(12) C7 0.0241(14) 0.0143(12) 0.0229(13) -0.0017(10) 0.0060(11) -0.0032(10) C8 0.0367(17) 0.0184(13) 0.0485(19) 0.0042(12) 0.0231(15) -0.0029(12) C9 0.066(2) 0.0239(14) 0.0232(15) 0.0044(12) 0.0076(15) -0.0120(14) C10 0.0425(19) 0.0168(13) 0.0394(17) 0.0093(12) -0.0083(14) 0.0021(12) C11 0.0285(15) 0.0152(13) 0.0365(16) -0.0025(11) 0.0065(13) -0.0003(10) C12 0.0281(15) 0.0191(13) 0.0297(15) 0.0034(11) -0.0018(12) -0.0072(11) _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 C2 1.962(3) . ? Mo1 C1 1.965(3) . ? Mo1 N1 2.1830(19) . ? Mo1 C9 2.276(3) . ? Mo1 C10 2.299(2) . ? Mo1 C8 2.319(3) . ? Mo1 C11 2.385(2) . ? Mo1 C12 2.396(3) . ? Mo1 S2 2.5227(9) . ? S2 C7 1.729(3) . ? O1 C1 1.155(3) . ? O2 C2 1.153(3) . ? N1 C3 1.345(3) . ? N1 C7 1.354(3) . ? C3 C4 1.374(4) . ? C4 C5 1.387(4) . ? C5 C6 1.374(4) . ? C6 C7 1.398(4) . ? C8 C12 1.408(4) . ? C8 C9 1.414(5) . ? C9 C10 1.410(4) . ? C10 C11 1.410(4) . ? C11 C12 1.395(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 C2 Mo1 C1 75.21(11) . . ? C2 Mo1 N1 118.19(10) . . ? C1 Mo1 N1 81.98(9) . . ? C2 Mo1 C9 94.13(12) . . ? C1 Mo1 C9 97.70(10) . . ? N1 Mo1 C9 146.03(10) . . ? C2 Mo1 C10 92.45(10) . . ? C1 Mo1 C10 131.87(11) . . ? N1 Mo1 C10 141.04(9) . . ? C9 Mo1 C10 35.90(11) . . ? C2 Mo1 C8 126.47(12) . . ? C1 Mo1 C8 91.03(10) . . ? N1 Mo1 C8 110.30(10) . . ? C9 Mo1 C8 35.84(11) . . ? C10 Mo1 C8 59.19(11) . . ? C2 Mo1 C11 122.65(10) . . ? C1 Mo1 C11 148.64(10) . . ? N1 Mo1 C11 106.28(9) . . ? C9 Mo1 C11 58.41(10) . . ? C10 Mo1 C11 34.97(9) . . ? C8 Mo1 C11 57.63(10) . . ? C2 Mo1 C12 149.70(10) . . ? C1 Mo1 C12 117.92(11) . . ? N1 Mo1 C12 91.48(8) . . ? C9 Mo1 C12 58.46(10) . . ? C10 Mo1 C12 58.03(10) . . ? C8 Mo1 C12 34.72(9) . . ? C11 Mo1 C12 33.94(9) . . ? C2 Mo1 S2 82.54(8) . . ? C1 Mo1 S2 123.76(8) . . ? N1 Mo1 S2 64.43(6) . . ? C9 Mo1 S2 135.34(9) . . ? C10 Mo1 S2 99.53(8) . . ? C8 Mo1 S2 141.38(7) . . ? C11 Mo1 S2 86.11(7) . . ? C12 Mo1 S2 107.22(7) . . ? C7 S2 Mo1 81.62(9) . . ? C3 N1 C7 119.7(2) . . ? C3 N1 Mo1 135.72(18) . . ? C7 N1 Mo1 104.52(16) . . ? O1 C1 Mo1 178.2(2) . . ? O2 C2 Mo1 177.6(3) . . ? N1 C3 C4 121.6(3) . . ? C3 C4 C5 118.8(3) . . ? C6 C5 C4 120.5(3) . . ? C5 C6 C7 118.1(3) . . ? N1 C7 C6 121.2(2) . . ? N1 C7 S2 109.38(18) . . ? C6 C7 S2 129.4(2) . . ? C12 C8 C9 108.0(3) . . ? C12 C8 Mo1 75.63(16) . . ? C9 C8 Mo1 70.44(16) . . ? C10 C9 C8 107.7(3) . . ? C10 C9 Mo1 72.95(16) . . ? C8 C9 Mo1 73.73(15) . . ? C11 C10 C9 107.6(3) . . ? C11 C10 Mo1 75.83(15) . . ? C9 C10 Mo1 71.15(15) . . ? C12 C11 C10 108.7(3) . . ? C12 C11 Mo1 73.46(15) . . ? C10 C11 Mo1 69.20(14) . . ? C11 C12 C8 108.0(3) . . ? C11 C12 Mo1 72.60(15) . . ? C8 C12 Mo1 69.65(15) . . ? _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 25.30 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 0.554 _refine_diff_density_min -0.900 _refine_diff_density_rms 0.098 #===END _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H13 Mn Mo N2 O4 S2' _chemical_formula_weight 548.31 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' 'Mn' 'Mn' 0.3368 0.7283 '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 P212121 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 10.680(2) _cell_length_b 12.0922(18) _cell_length_c 15.335(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1980.5(6) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.839 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1088 _exptl_absorpt_coefficient_mu 1.511 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.5833 _exptl_absorpt_correction_T_max 0.8636 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3558 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0381 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 25.34 _reflns_number_total 3558 _reflns_number_gt 3280 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0357P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.02(2) _refine_ls_number_reflns 3558 _refine_ls_number_parameters 262 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0318 _refine_ls_R_factor_gt 0.0255 _refine_ls_wR_factor_ref 0.0632 _refine_ls_wR_factor_gt 0.0615 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _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 0.19738(3) 0.04635(2) 0.368357(19) 0.01800(9) Uani 1 1 d . . . Mn1 Mn 0.28967(5) 0.21539(4) 0.26920(3) 0.01890(13) Uani 1 1 d . . . S1 S 0.09946(8) 0.23468(7) 0.34937(5) 0.01947(19) Uani 1 1 d . . . S2 S 0.18690(8) 0.06185(7) 0.21036(5) 0.02022(18) Uani 1 1 d . . . O1 O 0.5223(3) 0.1691(3) 0.1729(2) 0.0453(8) Uani 1 1 d . . . O2 O 0.2464(2) 0.3956(2) 0.14399(19) 0.0336(7) Uani 1 1 d . . . O3 O 0.4349(3) 0.3602(3) 0.3877(2) 0.0419(8) Uani 1 1 d . . . O4 O 0.4806(2) 0.0097(2) 0.3424(2) 0.0358(7) Uani 1 1 d . . . N1 N 0.2266(3) 0.1611(2) 0.47696(18) 0.0177(6) Uani 1 1 d . . . N2 N 0.0313(3) 0.1153(3) 0.0846(2) 0.0252(7) Uani 1 1 d . . . C1 C 0.4312(4) 0.1847(3) 0.2107(3) 0.0283(9) Uani 1 1 d . . . C2 C 0.2603(3) 0.3249(3) 0.1928(2) 0.0239(8) Uani 1 1 d . . . C3 C 0.3775(3) 0.3031(3) 0.3424(2) 0.0266(9) Uani 1 1 d . . . C4 C 0.3760(4) 0.0378(3) 0.3475(2) 0.0256(8) Uani 1 1 d . . . C5 C 0.2286(4) -0.1056(3) 0.4531(3) 0.0333(10) Uani 1 1 d . . . H5 H 0.3057 -0.1138 0.4834 0.040 Uiso 1 1 calc R . . C6 C 0.1186(4) -0.0570(3) 0.4868(3) 0.0325(9) Uani 1 1 d . . . H6 H 0.1093 -0.0266 0.5435 0.039 Uiso 1 1 calc R . . C7 C 0.0242(4) -0.0608(3) 0.4219(3) 0.0310(9) Uani 1 1 d . . . H7 H -0.0590 -0.0339 0.4272 0.037 Uiso 1 1 calc R . . C8 C 0.0775(4) -0.1124(3) 0.3474(3) 0.0300(9) Uani 1 1 d . . . H8 H 0.0352 -0.1261 0.2940 0.036 Uiso 1 1 calc R . . C9 C 0.2039(4) -0.1404(3) 0.3657(3) 0.0308(8) Uani 1 1 d . . . H9 H 0.2611 -0.1755 0.3272 0.037 Uiso 1 1 calc R . . C10 C 0.1584(3) 0.2508(3) 0.4564(2) 0.0187(8) Uani 1 1 d . . . C11 C 0.1397(3) 0.3380(3) 0.5134(2) 0.0245(8) Uani 1 1 d . . . H11 H 0.0891 0.3995 0.4980 0.029 Uiso 1 1 calc R . . C12 C 0.1980(4) 0.3316(3) 0.5941(2) 0.0281(8) Uani 1 1 d . . . H12 H 0.1881 0.3898 0.6351 0.034 Uiso 1 1 calc R . . C13 C 0.2709(3) 0.2404(3) 0.6149(2) 0.0277(9) Uani 1 1 d . . . H13 H 0.3120 0.2359 0.6697 0.033 Uiso 1 1 calc R . . C14 C 0.2827(4) 0.1566(3) 0.5549(2) 0.0237(8) Uani 1 1 d . . . H14 H 0.3321 0.0937 0.5692 0.028 Uiso 1 1 calc R . . C15 C 0.0310(3) 0.0864(3) 0.1689(2) 0.0186(7) Uani 1 1 d . . . C16 C -0.0777(3) 0.0675(3) 0.2154(2) 0.0231(8) Uani 1 1 d . . . H16 H -0.0743 0.0497 0.2757 0.028 Uiso 1 1 calc R . . C17 C -0.1916(4) 0.0749(3) 0.1727(2) 0.0241(8) Uani 1 1 d . . . H17 H -0.2676 0.0610 0.2030 0.029 Uiso 1 1 calc R . . C18 C -0.1929(4) 0.1029(3) 0.0852(2) 0.0276(8) Uani 1 1 d . . . H18 H -0.2693 0.1070 0.0537 0.033 Uiso 1 1 calc R . . C19 C -0.0805(4) 0.1245(3) 0.0451(2) 0.0277(9) Uani 1 1 d . . . H19 H -0.0819 0.1474 -0.0141 0.033 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.01620(14) 0.01716(14) 0.02064(15) -0.00003(13) -0.00484(14) 0.00049(14) Mn1 0.0128(2) 0.0221(3) 0.0217(3) 0.0004(2) -0.0005(2) 0.0009(2) S1 0.0158(4) 0.0233(4) 0.0193(5) 0.0007(3) -0.0011(3) 0.0040(3) S2 0.0147(4) 0.0246(4) 0.0213(4) -0.0036(4) -0.0020(4) 0.0020(4) O1 0.0207(15) 0.063(2) 0.0520(19) -0.0036(17) 0.0096(14) 0.0093(15) O2 0.0260(14) 0.0406(16) 0.0342(17) 0.0163(14) -0.0013(12) 0.0015(12) O3 0.0349(17) 0.0442(17) 0.0465(18) -0.0106(15) -0.0159(15) -0.0097(14) O4 0.0143(13) 0.0410(17) 0.0520(18) -0.0012(14) -0.0068(12) 0.0095(12) N1 0.0187(16) 0.0198(15) 0.0146(14) -0.0001(12) -0.0022(12) -0.0011(12) N2 0.0220(17) 0.0350(19) 0.0185(16) -0.0024(14) -0.0019(13) 0.0038(14) C1 0.023(2) 0.031(2) 0.031(2) -0.0007(18) -0.0069(18) 0.0034(16) C2 0.0123(17) 0.032(2) 0.027(2) -0.0018(17) 0.0054(14) -0.0013(15) C3 0.0202(19) 0.028(2) 0.031(2) 0.0068(17) -0.0001(17) 0.0041(16) C4 0.031(2) 0.0234(19) 0.0220(19) 0.0000(16) -0.0117(15) -0.0010(17) C5 0.037(3) 0.026(2) 0.037(2) 0.0087(18) -0.0164(19) -0.0055(18) C6 0.038(2) 0.028(2) 0.031(2) 0.0069(19) -0.0066(18) -0.0100(19) C7 0.026(2) 0.032(2) 0.034(2) 0.0091(19) -0.0049(17) -0.0104(18) C8 0.036(2) 0.025(2) 0.029(2) 0.0028(16) -0.0148(18) -0.0119(18) C9 0.031(2) 0.0175(16) 0.044(2) -0.0026(16) -0.014(2) -0.0012(17) C10 0.0136(16) 0.0218(19) 0.0208(18) 0.0006(14) 0.0028(13) -0.0020(14) C11 0.0193(18) 0.0252(19) 0.029(2) -0.0033(16) 0.0016(16) -0.0029(15) C12 0.0270(19) 0.032(2) 0.0248(18) -0.0101(15) 0.0032(18) -0.004(2) C13 0.024(2) 0.038(2) 0.0216(19) -0.0006(17) -0.0043(15) -0.0063(16) C14 0.021(2) 0.0238(19) 0.0261(19) 0.0016(15) -0.0020(16) -0.0017(16) C15 0.0168(18) 0.0182(17) 0.0208(18) -0.0041(15) -0.0012(14) 0.0007(14) C16 0.0211(18) 0.027(2) 0.0210(17) 0.0014(16) -0.0015(15) 0.0023(15) C17 0.0172(18) 0.0237(18) 0.0315(19) -0.0037(15) -0.0014(17) 0.0032(16) C18 0.0217(19) 0.0253(19) 0.036(2) -0.0058(16) -0.0106(19) 0.0059(18) C19 0.026(2) 0.038(2) 0.0195(19) -0.0030(16) -0.0012(16) 0.0040(18) _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 C4 1.937(4) . ? Mo1 N1 2.190(3) . ? Mo1 C9 2.259(3) . ? Mo1 C5 2.276(4) . ? Mo1 C8 2.330(4) . ? Mo1 C6 2.359(4) . ? Mo1 C7 2.403(4) . ? Mo1 S2 2.4328(9) . ? Mo1 S1 2.5228(9) . ? Mo1 Mn1 2.7316(7) . ? Mn1 C2 1.795(4) . ? Mn1 C1 1.797(4) . ? Mn1 C3 1.807(4) . ? Mn1 S2 2.3380(10) . ? Mn1 S1 2.3859(11) . ? Mn1 C4 2.628(4) . ? S1 C10 1.768(4) . ? S2 C15 1.807(4) . ? O1 C1 1.149(5) . ? O2 C2 1.147(5) . ? O3 C3 1.155(5) . ? O4 C4 1.170(5) . ? N1 C14 1.338(5) . ? N1 C10 1.344(5) . ? N2 C15 1.340(5) . ? N2 C19 1.342(5) . ? C5 C6 1.412(6) . ? C5 C9 1.430(6) . ? C6 C7 1.417(6) . ? C7 C8 1.420(6) . ? C8 C9 1.420(6) . ? C10 C11 1.384(5) . ? C11 C12 1.387(5) . ? C12 C13 1.387(6) . ? C13 C14 1.374(5) . ? C15 C16 1.381(5) . ? C16 C17 1.384(5) . ? C17 C18 1.385(5) . ? C18 C19 1.374(6) . ? 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 C4 Mo1 N1 91.08(13) . . ? C4 Mo1 C9 85.02(16) . . ? N1 Mo1 C9 129.98(13) . . ? C4 Mo1 C5 84.63(16) . . ? N1 Mo1 C5 93.23(13) . . ? C9 Mo1 C5 36.75(14) . . ? C4 Mo1 C8 118.32(16) . . ? N1 Mo1 C8 134.84(13) . . ? C9 Mo1 C8 36.00(15) . . ? C5 Mo1 C8 59.59(14) . . ? C4 Mo1 C6 116.73(15) . . ? N1 Mo1 C6 78.53(13) . . ? C9 Mo1 C6 59.71(16) . . ? C5 Mo1 C6 35.41(15) . . ? C8 Mo1 C6 58.24(14) . . ? C4 Mo1 C7 141.75(16) . . ? N1 Mo1 C7 101.05(13) . . ? C9 Mo1 C7 59.38(16) . . ? C5 Mo1 C7 58.81(15) . . ? C8 Mo1 C7 34.87(15) . . ? C6 Mo1 C7 34.60(13) . . ? C4 Mo1 S2 83.42(10) . . ? N1 Mo1 S2 135.65(8) . . ? C9 Mo1 S2 93.47(11) . . ? C5 Mo1 S2 129.64(11) . . ? C8 Mo1 S2 84.32(10) . . ? C6 Mo1 S2 142.27(10) . . ? C7 Mo1 S2 110.27(10) . . ? C4 Mo1 S1 115.96(12) . . ? N1 Mo1 S1 64.85(8) . . ? C9 Mo1 S1 155.89(11) . . ? C5 Mo1 S1 148.83(12) . . ? C8 Mo1 S1 120.00(10) . . ? C6 Mo1 S1 114.76(11) . . ? C7 Mo1 S1 101.96(11) . . ? S2 Mo1 S1 78.25(3) . . ? C4 Mo1 Mn1 65.99(11) . . ? N1 Mo1 Mn1 84.13(8) . . ? C9 Mo1 Mn1 136.62(12) . . ? C5 Mo1 Mn1 150.39(11) . . ? C8 Mo1 Mn1 137.59(10) . . ? C6 Mo1 Mn1 162.43(10) . . ? C7 Mo1 Mn1 150.63(10) . . ? S2 Mo1 Mn1 53.46(2) . . ? S1 Mo1 Mn1 53.83(3) . . ? C2 Mn1 C1 88.48(17) . . ? C2 Mn1 C3 93.61(17) . . ? C1 Mn1 C3 89.74(17) . . ? C2 Mn1 S2 104.59(13) . . ? C1 Mn1 S2 92.17(13) . . ? C3 Mn1 S2 161.74(12) . . ? C2 Mn1 S1 96.61(11) . . ? C1 Mn1 S1 173.67(13) . . ? C3 Mn1 S1 93.68(12) . . ? S2 Mn1 S1 82.92(4) . . ? C2 Mn1 C4 164.21(14) . . ? C1 Mn1 C4 76.37(15) . . ? C3 Mn1 C4 90.79(14) . . ? S2 Mn1 C4 72.07(8) . . ? S1 Mn1 C4 98.23(9) . . ? C2 Mn1 Mo1 148.42(11) . . ? C1 Mn1 Mo1 115.28(13) . . ? C3 Mn1 Mo1 106.30(12) . . ? S2 Mn1 Mo1 56.72(3) . . ? S1 Mn1 Mo1 58.61(3) . . ? C4 Mn1 Mo1 42.32(9) . . ? C10 S1 Mn1 100.72(11) . . ? C10 S1 Mo1 81.08(12) . . ? Mn1 S1 Mo1 67.56(3) . . ? C15 S2 Mn1 115.97(12) . . ? C15 S2 Mo1 113.93(12) . . ? Mn1 S2 Mo1 69.83(3) . . ? C14 N1 C10 119.1(3) . . ? C14 N1 Mo1 135.8(2) . . ? C10 N1 Mo1 104.8(2) . . ? C15 N2 C19 117.0(3) . . ? O1 C1 Mn1 177.5(4) . . ? O2 C2 Mn1 177.3(3) . . ? O3 C3 Mn1 178.5(4) . . ? O4 C4 Mo1 165.2(3) . . ? O4 C4 Mn1 122.8(3) . . ? Mo1 C4 Mn1 71.69(12) . . ? C6 C5 C9 108.1(4) . . ? C6 C5 Mo1 75.5(2) . . ? C9 C5 Mo1 71.0(2) . . ? C5 C6 C7 108.8(4) . . ? C5 C6 Mo1 69.1(2) . . ? C7 C6 Mo1 74.4(2) . . ? C6 C7 C8 107.1(4) . . ? C6 C7 Mo1 71.0(2) . . ? C8 C7 Mo1 69.8(2) . . ? C9 C8 C7 109.1(4) . . ? C9 C8 Mo1 69.3(2) . . ? C7 C8 Mo1 75.4(2) . . ? C8 C9 C5 106.9(4) . . ? C8 C9 Mo1 74.7(2) . . ? C5 C9 Mo1 72.2(2) . . ? N1 C10 C11 122.9(3) . . ? N1 C10 S1 108.8(3) . . ? C11 C10 S1 128.3(3) . . ? C10 C11 C12 117.2(4) . . ? C11 C12 C13 120.1(3) . . ? C14 C13 C12 119.0(3) . . ? N1 C14 C13 121.7(3) . . ? N2 C15 C16 122.9(3) . . ? N2 C15 S2 112.4(3) . . ? C16 C15 S2 124.4(3) . . ? C15 C16 C17 118.9(3) . . ? C16 C17 C18 118.9(4) . . ? C19 C18 C17 118.1(4) . . ? N2 C19 C18 124.0(3) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.34 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.316 _refine_diff_density_min -0.489 _refine_diff_density_rms 0.067 #===END _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H19 Mo3 N O2 S2' _chemical_formula_weight 681.32 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 ? _symmetry_space_group_name_H-M ? 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 13.2230(5) _cell_length_b 16.7951(5) _cell_length_c 9.5772(3) _cell_angle_alpha 90.00 _cell_angle_beta 95.2087(11) _cell_angle_gamma 90.00 _cell_volume 2118.14(12) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.137 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1328 _exptl_absorpt_coefficient_mu 1.967 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.6945 _exptl_absorpt_correction_T_max 0.9617 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16841 _diffrn_reflns_av_R_equivalents 0.0792 _diffrn_reflns_av_sigmaI/netI 0.0847 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 27.50 _reflns_number_total 4819 _reflns_number_gt 3484 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0156P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4819 _refine_ls_number_parameters 271 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0677 _refine_ls_R_factor_gt 0.0366 _refine_ls_wR_factor_ref 0.0727 _refine_ls_wR_factor_gt 0.0649 _refine_ls_goodness_of_fit_ref 0.968 _refine_ls_restrained_S_all 0.968 _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 0.28004(3) -0.05124(2) 0.38357(3) 0.01166(10) Uani 1 1 d . . . Mo2 Mo 0.22155(3) 0.00939(2) 0.09552(3) 0.01128(10) Uani 1 1 d . . . Mo3 Mo 0.15778(3) 0.09700(2) 0.31381(3) 0.01184(10) Uani 1 1 d . . . S1 S 0.10108(8) 0.10844(6) 0.08002(10) 0.0143(2) Uani 1 1 d . . . S2 S 0.11475(8) -0.03858(6) 0.26416(10) 0.0132(2) Uani 1 1 d . . . O1 O 0.3558(2) 0.09438(18) 0.5620(3) 0.0218(7) Uani 1 1 d . . . O2 O 0.4607(2) -0.03823(17) 0.2021(3) 0.0210(7) Uani 1 1 d . . . C1 C 0.3177(3) 0.0478(3) 0.4815(4) 0.0164(10) Uani 1 1 d . . . C2 C 0.3834(3) -0.0346(2) 0.2541(4) 0.0148(9) Uani 1 1 d . . . C3 C 0.3161(3) -0.1878(2) 0.3945(4) 0.0179(10) Uani 1 1 d . . . H3 H 0.3204 -0.2178 0.3111 0.022 Uiso 1 1 calc R . . C4 C 0.3976(3) -0.1463(2) 0.4718(4) 0.0177(10) Uani 1 1 d . . . H4 H 0.4660 -0.1441 0.4490 0.021 Uiso 1 1 calc R . . C5 C 0.3589(3) -0.1096(3) 0.5869(4) 0.0184(10) Uani 1 1 d . . . H5 H 0.3969 -0.0781 0.6554 0.022 Uiso 1 1 calc R . . C6 C 0.2533(3) -0.1270(3) 0.5848(4) 0.0180(10) Uani 1 1 d . . . H6 H 0.2084 -0.1095 0.6504 0.022 Uiso 1 1 calc R . . C7 C 0.2283(4) -0.1757(2) 0.4654(4) 0.0193(10) Uani 1 1 d . . . H7 H 0.1629 -0.1968 0.4376 0.023 Uiso 1 1 calc R . . C8 C 0.2768(3) -0.1074(3) -0.0149(4) 0.0178(10) Uani 1 1 d . . . H8 H 0.3114 -0.1491 0.0367 0.021 Uiso 1 1 calc R . . C9 C 0.1700(3) -0.1011(3) -0.0468(4) 0.0185(10) Uani 1 1 d . . . H9 H 0.1205 -0.1376 -0.0197 0.022 Uiso 1 1 calc R . . C10 C 0.1507(3) -0.0313(3) -0.1254(4) 0.0175(10) Uani 1 1 d . . . H10 H 0.0858 -0.0126 -0.1617 0.021 Uiso 1 1 calc R . . C11 C 0.2448(3) 0.0067(3) -0.1413(4) 0.0186(10) Uani 1 1 d . . . H11 H 0.2540 0.0553 -0.1891 0.022 Uiso 1 1 calc R . . C12 C 0.3224(3) -0.0411(3) -0.0730(4) 0.0165(10) Uani 1 1 d . . . H12 H 0.3931 -0.0302 -0.0674 0.020 Uiso 1 1 calc R . . C13 C 0.0177(3) 0.1094(3) 0.4509(4) 0.0177(10) Uani 1 1 d . . . H13 H -0.0310 0.0681 0.4540 0.021 Uiso 1 1 calc R . . C14 C 0.0139(3) 0.1729(3) 0.3546(4) 0.0216(11) Uani 1 1 d . . . H14 H -0.0383 0.1820 0.2815 0.026 Uiso 1 1 calc R . . C15 C 0.1010(3) 0.2208(3) 0.3852(4) 0.0194(10) Uani 1 1 d . . . H15 H 0.1178 0.2676 0.3367 0.023 Uiso 1 1 calc R . . C16 C 0.1586(4) 0.1862(3) 0.5016(4) 0.0206(10) Uani 1 1 d . . . H16 H 0.2213 0.2056 0.5446 0.025 Uiso 1 1 calc R . . C17 C 0.1071(3) 0.1184(3) 0.5422(4) 0.0206(10) Uani 1 1 d . . . H17 H 0.1287 0.0842 0.6182 0.025 Uiso 1 1 calc R . . N1 N 0.3232(3) 0.1082(2) 0.1358(3) 0.0115(8) Uani 0.50 1 d P . . C18' C 0.3232(3) 0.1082(2) 0.1358(3) 0.0115(8) Uani 0.50 1 d P . . C18 C 0.2924(3) 0.1510(2) 0.2462(3) 0.0140(8) Uani 0.50 1 d P . . N1' N 0.2924(3) 0.1510(2) 0.2462(3) 0.0140(8) Uani 0.50 1 d P . . C19 C 0.3489(3) 0.2161(3) 0.2936(4) 0.0179(10) Uani 1 1 d . . . H19 H 0.3284 0.2449 0.3710 0.022 Uiso 1 1 d . . . C20 C 0.4333(3) 0.2403(3) 0.2321(4) 0.0215(11) Uani 1 1 d . . . H20 H 0.4701 0.2862 0.2648 0.026 Uiso 1 1 calc R . . C21 C 0.4638(3) 0.1958(3) 0.1202(4) 0.0204(10) Uani 1 1 d . . . H21 H 0.5224 0.2109 0.0759 0.024 Uiso 1 1 calc R . . C22 C 0.4088(3) 0.1305(3) 0.0748(4) 0.0166(9) Uani 1 1 d . . . H22 H 0.4305 0.0998 -0.0006 0.020 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.0096(2) 0.0140(2) 0.01153(19) 0.00120(14) 0.00171(14) 0.00140(16) Mo2 0.0092(2) 0.0145(2) 0.01023(18) -0.00037(14) 0.00172(13) -0.00084(16) Mo3 0.0099(2) 0.0140(2) 0.01185(19) -0.00005(14) 0.00251(14) 0.00087(16) S1 0.0112(6) 0.0171(6) 0.0145(5) 0.0022(4) 0.0010(4) 0.0008(5) S2 0.0102(6) 0.0158(6) 0.0139(5) 0.0010(4) 0.0019(4) -0.0012(5) O1 0.0176(19) 0.0248(19) 0.0217(16) -0.0032(13) -0.0062(13) -0.0018(15) O2 0.0116(18) 0.032(2) 0.0202(16) 0.0032(13) 0.0050(13) 0.0032(15) C1 0.014(2) 0.024(3) 0.012(2) 0.0058(18) 0.0016(17) 0.004(2) C2 0.016(3) 0.017(2) 0.011(2) -0.0031(17) -0.0019(18) 0.000(2) C3 0.025(3) 0.009(2) 0.020(2) 0.0027(17) 0.0056(19) 0.003(2) C4 0.011(2) 0.020(3) 0.023(2) 0.0098(19) 0.0037(18) 0.008(2) C5 0.022(3) 0.023(3) 0.010(2) 0.0024(17) -0.0022(18) 0.004(2) C6 0.022(3) 0.019(3) 0.013(2) 0.0059(17) 0.0017(18) 0.005(2) C7 0.019(3) 0.008(2) 0.030(3) 0.0093(18) 0.002(2) -0.0005(19) C8 0.017(3) 0.020(3) 0.016(2) -0.0055(17) 0.0019(18) 0.008(2) C9 0.018(3) 0.021(3) 0.017(2) -0.0105(18) 0.0051(18) -0.008(2) C10 0.012(2) 0.029(3) 0.011(2) -0.0081(18) -0.0028(17) -0.001(2) C11 0.023(3) 0.026(3) 0.008(2) 0.0001(17) 0.0020(17) 0.003(2) C12 0.009(2) 0.028(3) 0.013(2) -0.0054(18) 0.0036(17) -0.001(2) C13 0.014(2) 0.025(3) 0.016(2) -0.0017(18) 0.0124(18) 0.004(2) C14 0.018(3) 0.029(3) 0.018(2) -0.0037(19) 0.0013(19) 0.010(2) C15 0.022(3) 0.010(2) 0.027(2) -0.0070(18) 0.010(2) 0.003(2) C16 0.021(3) 0.021(3) 0.021(2) -0.0101(18) 0.0044(19) 0.000(2) C17 0.023(3) 0.028(3) 0.011(2) -0.0029(18) 0.0053(18) 0.005(2) N1 0.009(2) 0.015(2) 0.0110(19) 0.0037(14) 0.0017(15) 0.0002(16) C18' 0.009(2) 0.015(2) 0.0110(19) 0.0037(14) 0.0017(15) 0.0002(16) C18 0.014(2) 0.013(2) 0.0141(19) 0.0030(15) -0.0012(15) 0.0032(17) N1' 0.014(2) 0.013(2) 0.0141(19) 0.0030(15) -0.0012(15) 0.0032(17) C19 0.018(3) 0.018(3) 0.017(2) 0.0022(18) -0.0003(18) 0.000(2) C20 0.023(3) 0.017(3) 0.024(3) 0.0040(18) -0.003(2) -0.005(2) C21 0.013(3) 0.021(3) 0.027(2) 0.0036(19) 0.0027(19) -0.006(2) C22 0.017(3) 0.018(2) 0.015(2) 0.0047(18) 0.0039(17) 0.001(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 C2 1.947(4) . ? Mo1 C1 1.952(5) . ? Mo1 C4 2.333(4) . ? Mo1 C5 2.339(4) . ? Mo1 C3 2.343(4) . ? Mo1 C7 2.356(4) . ? Mo1 C6 2.363(4) . ? Mo1 S2 2.3824(11) . ? Mo1 Mo2 2.9762(5) . ? Mo1 Mo3 3.0104(5) . ? Mo2 N1 2.149(4) . ? Mo2 S1 2.2987(11) . ? Mo2 C11 2.317(4) . ? Mo2 C10 2.337(4) . ? Mo2 C12 2.343(4) . ? Mo2 C9 2.365(4) . ? Mo2 C8 2.374(4) . ? Mo2 S2 2.3803(10) . ? Mo2 C2 2.616(4) . ? Mo2 Mo3 2.7508(5) . ? Mo3 C18 2.150(4) . ? Mo3 S1 2.3038(10) . ? Mo3 C15 2.334(4) . ? Mo3 C16 2.339(4) . ? Mo3 C14 2.353(4) . ? Mo3 C17 2.373(4) . ? Mo3 C13 2.375(4) . ? Mo3 S2 2.3844(11) . ? O1 C1 1.179(5) . ? O2 C2 1.178(5) . ? C3 C7 1.413(6) . ? C3 C4 1.432(6) . ? C3 H3 0.9500 . ? C4 C5 1.400(6) . ? C4 H4 0.9500 . ? C5 C6 1.425(6) . ? C5 H5 0.9500 . ? C6 C7 1.420(6) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 C12 1.404(6) . ? C8 C9 1.421(6) . ? C8 H8 0.9500 . ? C9 C10 1.405(6) . ? C9 H9 0.9500 . ? C10 C11 1.417(6) . ? C10 H10 0.9500 . ? C11 C12 1.415(6) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.408(6) . ? C13 C17 1.413(6) . ? C13 H13 0.9500 . ? C14 C15 1.413(6) . ? C14 H14 0.9500 . ? C15 C16 1.417(6) . ? C15 H15 0.9500 . ? C16 C17 1.399(6) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? N1 C18 1.371(5) . ? N1 C22 1.372(5) . ? C18 C19 1.377(5) . ? C19 C20 1.370(6) . ? C19 H19 0.9451 . ? C20 C21 1.395(6) . ? C20 H20 0.9500 . ? C21 C22 1.365(6) . ? C21 H21 0.9500 . ? C22 H22 0.9530 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Mo1 C1 91.19(17) . . ? C2 Mo1 C4 81.11(16) . . ? C1 Mo1 C4 106.06(16) . . ? C2 Mo1 C5 107.74(16) . . ? C1 Mo1 C5 83.22(16) . . ? C4 Mo1 C5 34.88(14) . . ? C2 Mo1 C3 90.96(16) . . ? C1 Mo1 C3 140.41(16) . . ? C4 Mo1 C3 35.66(15) . . ? C5 Mo1 C3 58.61(15) . . ? C2 Mo1 C7 125.51(16) . . ? C1 Mo1 C7 131.73(15) . . ? C4 Mo1 C7 58.42(15) . . ? C5 Mo1 C7 58.15(15) . . ? C3 Mo1 C7 34.99(14) . . ? C2 Mo1 C6 139.67(16) . . ? C1 Mo1 C6 96.76(15) . . ? C4 Mo1 C6 58.67(15) . . ? C5 Mo1 C6 35.27(14) . . ? C3 Mo1 C6 58.75(14) . . ? C7 Mo1 C6 35.04(14) . . ? C2 Mo1 S2 110.35(12) . . ? C1 Mo1 S2 109.73(13) . . ? C4 Mo1 S2 141.92(11) . . ? C5 Mo1 S2 139.22(11) . . ? C3 Mo1 S2 106.45(11) . . ? C7 Mo1 S2 87.55(11) . . ? C6 Mo1 S2 103.94(11) . . ? C2 Mo1 Mo2 59.93(12) . . ? C1 Mo1 Mo2 100.80(11) . . ? C4 Mo1 Mo2 132.72(10) . . ? C5 Mo1 Mo2 166.84(10) . . ? C3 Mo1 Mo2 114.26(10) . . ? C7 Mo1 Mo2 123.57(11) . . ? C6 Mo1 Mo2 153.48(11) . . ? S2 Mo1 Mo2 51.29(2) . . ? C2 Mo1 Mo3 97.70(12) . . ? C1 Mo1 Mo3 60.68(12) . . ? C4 Mo1 Mo3 166.72(11) . . ? C5 Mo1 Mo3 136.14(10) . . ? C3 Mo1 Mo3 157.31(11) . . ? C7 Mo1 Mo3 129.89(11) . . ? C6 Mo1 Mo3 120.63(11) . . ? S2 Mo1 Mo3 50.87(3) . . ? Mo2 Mo1 Mo3 54.705(11) . . ? N1 Mo2 S1 82.59(10) . . ? N1 Mo2 C11 93.13(15) . . ? S1 Mo2 C11 95.95(11) . . ? N1 Mo2 C10 125.52(14) . . ? S1 Mo2 C10 86.25(11) . . ? C11 Mo2 C10 35.46(15) . . ? N1 Mo2 C12 91.00(14) . . ? S1 Mo2 C12 130.66(11) . . ? C11 Mo2 C12 35.34(14) . . ? C10 Mo2 C12 58.45(15) . . ? N1 Mo2 C9 148.45(14) . . ? S1 Mo2 C9 111.64(11) . . ? C11 Mo2 C9 58.49(15) . . ? C10 Mo2 C9 34.76(14) . . ? C12 Mo2 C9 58.10(15) . . ? N1 Mo2 C8 120.34(14) . . ? S1 Mo2 C8 143.94(11) . . ? C11 Mo2 C8 58.28(15) . . ? C10 Mo2 C8 57.97(15) . . ? C12 Mo2 C8 34.63(14) . . ? C9 Mo2 C8 34.90(14) . . ? N1 Mo2 S2 122.66(9) . . ? S1 Mo2 S2 80.70(4) . . ? C11 Mo2 S2 142.85(12) . . ? C10 Mo2 S2 107.57(11) . . ? C12 Mo2 S2 138.98(11) . . ? C9 Mo2 S2 88.15(11) . . ? C8 Mo2 S2 104.37(11) . . ? N1 Mo2 C2 69.43(13) . . ? S1 Mo2 C2 140.14(9) . . ? C11 Mo2 C2 112.88(14) . . ? C10 Mo2 C2 133.05(14) . . ? C12 Mo2 C2 79.12(14) . . ? C9 Mo2 C2 106.88(14) . . ? C8 Mo2 C2 75.91(13) . . ? S2 Mo2 C2 90.85(10) . . ? N1 Mo2 Mo3 71.35(9) . . ? S1 Mo2 Mo3 53.38(3) . . ? C11 Mo2 Mo3 146.27(11) . . ? C10 Mo2 Mo3 135.99(11) . . ? C12 Mo2 Mo3 161.77(11) . . ? C9 Mo2 Mo3 139.93(11) . . ? C8 Mo2 Mo3 155.26(10) . . ? S2 Mo2 Mo3 54.81(3) . . ? C2 Mo2 Mo3 90.06(9) . . ? N1 Mo2 Mo1 89.56(9) . . ? S1 Mo2 Mo1 115.32(3) . . ? C11 Mo2 Mo1 148.69(11) . . ? C10 Mo2 Mo1 142.04(11) . . ? C12 Mo2 Mo1 113.48(10) . . ? C9 Mo2 Mo1 107.61(11) . . ? C8 Mo2 Mo1 93.76(10) . . ? S2 Mo2 Mo1 51.36(3) . . ? C2 Mo2 Mo1 40.10(9) . . ? Mo3 Mo2 Mo1 63.278(12) . . ? C18 Mo3 S1 82.95(9) . . ? C18 Mo3 C15 90.54(15) . . ? S1 Mo3 C15 97.20(11) . . ? C18 Mo3 C16 90.88(15) . . ? S1 Mo3 C16 132.22(11) . . ? C15 Mo3 C16 35.29(15) . . ? C18 Mo3 C14 121.69(15) . . ? S1 Mo3 C14 85.37(10) . . ? C15 Mo3 C14 35.09(15) . . ? C16 Mo3 C14 58.17(15) . . ? C18 Mo3 C17 121.65(14) . . ? S1 Mo3 C17 142.12(11) . . ? C15 Mo3 C17 57.99(15) . . ? C16 Mo3 C17 34.54(14) . . ? C14 Mo3 C17 57.64(14) . . ? C18 Mo3 C13 146.94(14) . . ? S1 Mo3 C13 109.20(11) . . ? C15 Mo3 C13 58.11(15) . . ? C16 Mo3 C13 57.85(16) . . ? C14 Mo3 C13 34.66(14) . . ? C17 Mo3 C13 34.64(14) . . ? C18 Mo3 S2 122.15(10) . . ? S1 Mo3 S2 80.51(4) . . ? C15 Mo3 S2 146.28(11) . . ? C16 Mo3 S2 138.50(11) . . ? C14 Mo3 S2 111.65(12) . . ? C17 Mo3 S2 104.25(11) . . ? C13 Mo3 S2 90.60(11) . . ? C18 Mo3 Mo2 71.18(9) . . ? S1 Mo3 Mo2 53.21(3) . . ? C15 Mo3 Mo2 145.90(10) . . ? C16 Mo3 Mo2 161.14(12) . . ? C14 Mo3 Mo2 136.43(10) . . ? C17 Mo3 Mo2 155.97(11) . . ? C13 Mo3 Mo2 140.86(11) . . ? S2 Mo3 Mo2 54.67(3) . . ? C18 Mo3 Mo1 88.48(10) . . ? S1 Mo3 Mo1 113.92(3) . . ? C15 Mo3 Mo1 148.47(11) . . ? C16 Mo3 Mo1 113.20(11) . . ? C14 Mo3 Mo1 146.90(11) . . ? C17 Mo3 Mo1 96.39(11) . . ? C13 Mo3 Mo1 112.34(10) . . ? S2 Mo3 Mo1 50.81(3) . . ? Mo2 Mo3 Mo1 62.016(12) . . ? Mo2 S1 Mo3 73.41(3) . . ? Mo2 S2 Mo1 77.35(3) . . ? Mo2 S2 Mo3 70.52(3) . . ? Mo1 S2 Mo3 78.32(3) . . ? O1 C1 Mo1 162.8(4) . . ? O2 C2 Mo1 161.4(3) . . ? O2 C2 Mo2 117.7(3) . . ? Mo1 C2 Mo2 79.97(15) . . ? C7 C3 C4 107.1(4) . . ? C7 C3 Mo1 73.0(2) . . ? C4 C3 Mo1 71.8(2) . . ? C7 C3 H3 126.4 . . ? C4 C3 H3 126.4 . . ? Mo1 C3 H3 120.6 . . ? C5 C4 C3 108.0(4) . . ? C5 C4 Mo1 72.8(2) . . ? C3 C4 Mo1 72.6(2) . . ? C5 C4 H4 126.0 . . ? C3 C4 H4 126.0 . . ? Mo1 C4 H4 120.5 . . ? C4 C5 C6 109.0(4) . . ? C4 C5 Mo1 72.3(2) . . ? C6 C5 Mo1 73.3(2) . . ? C4 C5 H5 125.5 . . ? C6 C5 H5 125.5 . . ? Mo1 C5 H5 120.6 . . ? C7 C6 C5 106.6(4) . . ? C7 C6 Mo1 72.2(2) . . ? C5 C6 Mo1 71.5(2) . . ? C7 C6 H6 126.7 . . ? C5 C6 H6 126.7 . . ? Mo1 C6 H6 121.5 . . ? C3 C7 C6 109.1(4) . . ? C3 C7 Mo1 72.0(2) . . ? C6 C7 Mo1 72.7(2) . . ? C3 C7 H7 125.4 . . ? C6 C7 H7 125.4 . . ? Mo1 C7 H7 121.5 . . ? C12 C8 C9 108.0(4) . . ? C12 C8 Mo2 71.5(2) . . ? C9 C8 Mo2 72.2(2) . . ? C12 C8 H8 126.0 . . ? C9 C8 H8 126.0 . . ? Mo2 C8 H8 122.0 . . ? C10 C9 C8 107.8(4) . . ? C10 C9 Mo2 71.5(2) . . ? C8 C9 Mo2 72.9(2) . . ? C10 C9 H9 126.1 . . ? C8 C9 H9 126.1 . . ? Mo2 C9 H9 121.3 . . ? C9 C10 C11 108.3(4) . . ? C9 C10 Mo2 73.7(2) . . ? C11 C10 Mo2 71.5(2) . . ? C9 C10 H10 125.8 . . ? C11 C10 H10 125.8 . . ? Mo2 C10 H10 120.7 . . ? C12 C11 C10 107.6(4) . . ? C12 C11 Mo2 73.4(2) . . ? C10 C11 Mo2 73.0(2) . . ? C12 C11 H11 126.2 . . ? C10 C11 H11 126.2 . . ? Mo2 C11 H11 119.3 . . ? C8 C12 C11 108.3(4) . . ? C8 C12 Mo2 73.9(2) . . ? C11 C12 Mo2 71.3(2) . . ? C8 C12 H12 125.9 . . ? C11 C12 H12 125.9 . . ? Mo2 C12 H12 120.7 . . ? C14 C13 C17 107.7(4) . . ? C14 C13 Mo3 71.8(2) . . ? C17 C13 Mo3 72.6(2) . . ? C14 C13 H13 126.2 . . ? C17 C13 H13 126.2 . . ? Mo3 C13 H13 121.2 . . ? C13 C14 C15 108.3(4) . . ? C13 C14 Mo3 73.5(2) . . ? C15 C14 Mo3 71.7(2) . . ? C13 C14 H14 125.8 . . ? C15 C14 H14 125.8 . . ? Mo3 C14 H14 120.6 . . ? C14 C15 C16 107.4(4) . . ? C14 C15 Mo3 73.2(2) . . ? C16 C15 Mo3 72.5(2) . . ? C14 C15 H15 126.3 . . ? C16 C15 H15 126.3 . . ? Mo3 C15 H15 119.9 . . ? C17 C16 C15 108.2(4) . . ? C17 C16 Mo3 74.0(2) . . ? C15 C16 Mo3 72.2(2) . . ? C17 C16 H16 125.9 . . ? C15 C16 H16 125.9 . . ? Mo3 C16 H16 119.7 . . ? C16 C17 C13 108.3(4) . . ? C16 C17 Mo3 71.4(2) . . ? C13 C17 Mo3 72.8(2) . . ? C16 C17 H17 125.8 . . ? C13 C17 H17 125.8 . . ? Mo3 C17 H17 121.7 . . ? C18 N1 C22 120.0(4) . . ? C18 N1 Mo2 108.6(3) . . ? C22 N1 Mo2 131.4(3) . . ? N1 C18 C19 118.7(4) . . ? N1 C18 Mo3 108.9(3) . . ? C19 C18 Mo3 132.4(3) . . ? C20 C19 C18 122.1(4) . . ? C20 C19 H19 119.2 . . ? C18 C19 H19 118.7 . . ? C19 C20 C21 118.4(4) . . ? C19 C20 H20 120.8 . . ? C21 C20 H20 120.8 . . ? C22 C21 C20 119.4(4) . . ? C22 C21 H21 120.3 . . ? C20 C21 H21 120.3 . . ? C21 C22 N1 121.3(4) . . ? C21 C22 H22 119.2 . . ? N1 C22 H22 119.5 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.886 _refine_diff_density_min -0.990 _refine_diff_density_rms 0.180 #===END