# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1784 # This file contains the CIF data for the five structures reported in the # paper: # # "Molybdenum and tungsten complexes of the N(CH2CH2S)3 3- ligand with..." # # by S.C. Davies, D.L. Hughes, R.L. Richards and J.R. Sanders. # data_ray19 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C12 H24 Mo2 N2 S7, 0.3(H2 O)' _chemical_formula_structural '[(Mo{N(CH2CH2S)3})2(mu-S)].0.3H2O' _chemical_formula_analytical ? _chemical_formula_sum 'C12 H24.6 Mo2 N2 O0.3 S7' _chemical_formula_weight 618.0 _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' 'Mo' 'Mo' -1.6832 0.6857 '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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Rhombohedral _symmetry_space_group_name_H-M 'R-3 (no. 148)' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'z, x, y' 'y, z, x' '-x, -y, -z' '-z, -x, -y' '-y, -z, -x' _cell_length_a 8.3292(5) _cell_length_b 8.3292(5) _cell_length_c 8.3292(5) _cell_angle_alpha 77.833(7) _cell_angle_beta 77.833(7) _cell_angle_gamma 77.833(7) _cell_volume 543.74(7) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 9.4 _cell_measurement_theta_max 11 _exptl_crystal_description rhombs _exptl_crystal_colour 'very dark red' _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.887 _exptl_crystal_density_method ? _exptl_crystal_F_000 309 _exptl_absorpt_coefficient_mu 1.83 _exptl_absorpt_correction_type 'semi-empirical psi-scans' _exptl_absorpt_correction_T_min 0.98 _exptl_absorpt_correction_T_max 1.00 _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 'Enraf-Nonius CAD4 diffractometer' _diffrn_measurement_method 'scintillation counter; \w/\q scans' _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time '10000 s' _diffrn_standards_decay_% 0 _diffrn_reflns_number 3814 _diffrn_reflns_av_R_equivalents 0.030 _diffrn_reflns_av_sigmaI/netI 0.0390 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.54 _diffrn_reflns_theta_max 24.97 _reflns_number_total 641 _reflns_number_observed 573 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'CAD4/EXPRESS (Enraf-Nonius, 1992) ' _computing_cell_refinement 'CAD4/EXPRESS (Enraf-Nonius, 1992) ' _computing_data_reduction 'CAD4 (Hursthouse, 1976) ' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'ORTEP (Johnson, 1971)' _computing_publication_material 'SHELXL-93 (Sheldrick, 1993)' _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^)+(0.0272P)^2^+0.3071P] 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, in idealised positions' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 641 _refine_ls_number_parameters 37 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0276 _refine_ls_R_factor_obs 0.0242 _refine_ls_wR_factor_all 0.0741 _refine_ls_wR_factor_obs 0.0723 _refine_ls_goodness_of_fit_all 1.147 _refine_ls_goodness_of_fit_obs 1.187 _refine_ls_restrained_S_all 1.147 _refine_ls_restrained_S_obs 1.187 _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 Mo Mo 0.12459(3) 0.12459(3) 0.12459(3) 0.0355(2) Uani 1 d S . S1 S 0.33014(13) 0.18520(13) -0.09923(12) 0.0476(3) Uani 1 d . . C14 C 0.4519(5) 0.2950(5) -0.0146(6) 0.0549(10) Uani 1 d . . H14A H 0.5686(5) 0.2691(5) -0.0641(6) 0.066 Uiso 1 calc R . H14B H 0.4154(5) 0.4143(5) -0.0440(6) 0.066 Uiso 1 calc R . C41 C 0.4335(4) 0.2469(5) 0.1733(5) 0.0482(9) Uani 1 d . . H41A H 0.4931(4) 0.1343(5) 0.2016(5) 0.058 Uiso 1 calc R . H41B H 0.4835(4) 0.3211(5) 0.2155(5) 0.058 Uiso 1 calc R . N4 N 0.2555(3) 0.2555(3) 0.2555(3) 0.0361(11) Uani 1 d S . S5 S 0.0000 0.0000 0.0000 0.0434(5) Uani 1 d S . O6 O 0.5000 0.5000 0.5000 0.178(22) Uiso 0.30 d SP . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo 0.0364(2) 0.0364(2) 0.0364(2) -0.00842(10) -0.00842(10) -0.00842(10) S1 0.0508(6) 0.0505(6) 0.0412(5) -0.0120(4) -0.0007(4) -0.0114(4) C14 0.052(2) 0.051(2) 0.062(3) -0.012(2) 0.005(2) -0.021(2) C41 0.038(2) 0.051(2) 0.059(2) -0.012(2) -0.007(2) -0.016(2) N4 0.0371(12) 0.0371(12) 0.0371(12) -0.0086(10) -0.0086(10) -0.0086(10) S5 0.0457(6) 0.0457(6) 0.0457(6) -0.0130(4) -0.0130(4) -0.0130(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 Mo S5 2.1429(5) . ? Mo N4 2.251(4) . ? Mo S1 2.2986(10) 3 ? Mo S1 2.2986(10) 2 ? Mo S1 2.2986(10) . ? S1 C14 1.824(4) . ? C14 C41 1.515(6) . ? C14 H14A 0.97 . ? C14 H14B 0.97 . ? C41 N4 1.490(4) . ? C41 H41A 0.97 . ? C41 H41B 0.97 . ? N4 C41 1.490(4) 3 ? N4 C41 1.490(4) 2 ? S5 Mo 2.1429(5) 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 S5 Mo N4 180.00(12) . . ? S5 Mo S1 96.07(3) . 3 ? N4 Mo S1 83.93(3) . 3 ? S5 Mo S1 96.07(3) . 2 ? N4 Mo S1 83.93(3) . 2 ? S1 Mo S1 118.898(10) 3 2 ? S5 Mo S1 96.07(3) . . ? N4 Mo S1 83.93(3) . . ? S1 Mo S1 118.897(10) 3 . ? S1 Mo S1 118.898(10) 2 . ? C14 S1 Mo 102.31(14) . . ? C41 C14 S1 111.7(3) . . ? C41 C14 H14A 109.3(2) . . ? S1 C14 H14A 109.29(13) . . ? C41 C14 H14B 109.3(2) . . ? S1 C14 H14B 109.29(15) . . ? H14A C14 H14B 107.9 . . ? N4 C41 C14 112.1(3) . . ? N4 C41 H41A 109.2(2) . . ? C14 C41 H41A 109.2(2) . . ? N4 C41 H41B 109.2(2) . . ? C14 C41 H41B 109.2(2) . . ? H41A C41 H41B 107.9 . . ? C41 N4 C41 109.3(2) 3 . ? C41 N4 C41 109.3(2) 3 2 ? C41 N4 C41 109.3(2) . 2 ? C41 N4 Mo 109.6(2) 3 . ? C41 N4 Mo 109.6(2) . . ? C41 N4 Mo 109.6(2) 2 . ? Mo S5 Mo 180.0 4 . ? _refine_diff_density_max 1.158 _refine_diff_density_min -0.605 _refine_diff_density_rms 0.076 #===end data_ray18 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C7 H15 Mo N3 S3' _chemical_formula_structural [Mo(NNMe){N(CH2CH2S)3}] _chemical_formula_analytical ? _chemical_formula_sum 'C7 H15 Mo N3 S3' _chemical_formula_weight 333.34 _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' 'Mo' 'Mo' -1.6832 0.6857 '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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'Pmcn (equiv. to no. 62) ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, z' 'x, -y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-x, -y, -z' 'x-1/2, -y, -z' '-x, y-1/2, -z-1/2' 'x-1/2, y-1/2, -z-1/2' _cell_length_a 8.4093(7) _cell_length_b 10.5438(10) _cell_length_c 14.0272(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1243.7(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10 _cell_measurement_theta_max 11 _exptl_crystal_description 'rectangular prisms' _exptl_crystal_colour 'Dark red' _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.780 _exptl_crystal_density_method ? _exptl_crystal_F_000 672 _exptl_absorpt_coefficient_mu 1.526 _exptl_absorpt_correction_type 'semi-empirical psi-scans' _exptl_absorpt_correction_T_min 0.94 _exptl_absorpt_correction_T_max 1.00 _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 'Enraf-Nonius CAD4 diffractometer' _diffrn_measurement_method 'scintillation counter; \w/\q scans' _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time '10000 s' _diffrn_standards_decay_% 0 _diffrn_reflns_number 1604 _diffrn_reflns_av_R_equivalents 0.009 _diffrn_reflns_av_sigmaI/netI 0.0292 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.42 _diffrn_reflns_theta_max 24.96 _reflns_number_total 1168 _reflns_number_observed 1064 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'CAD4/EXPRESS (Enraf-Nonius, 1992) ' _computing_cell_refinement 'CAD4/EXPRESS (Enraf-Nonius, 1992) ' _computing_data_reduction 'CAD4 (Hursthouse, 1976) ' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'ORTEP (Johnson, 1971)' _computing_publication_material 'SHELXL-93 (Sheldrick, 1993)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 1 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^)+(0.0152P)^2^+0.2556P] 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 in idealised positions' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1167 _refine_ls_number_parameters 89 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0212 _refine_ls_R_factor_obs 0.0182 _refine_ls_wR_factor_all 0.0497 _refine_ls_wR_factor_obs 0.0475 _refine_ls_goodness_of_fit_all 1.126 _refine_ls_goodness_of_fit_obs 1.133 _refine_ls_restrained_S_all 1.242 _refine_ls_restrained_S_obs 1.133 _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 Mo Mo 0.2500 0.66822(2) 0.19010(2) 0.03314(11) Uani 1 d S . S1 S 0.2500 0.69777(9) 0.35340(6) 0.0569(2) Uani 1 d S . C14 C 0.2500 0.8713(4) 0.3620(2) 0.0576(9) Uani 1 d S . H14A H 0.1420 0.9005(4) 0.3725(2) 0.069 Uiso 0.50 calc PR . H14B H 0.3133 0.8966(4) 0.4166(2) 0.069 Uiso 0.50 calc PR . C41 C 0.3146(6) 0.9333(4) 0.2749(3) 0.0464(10) Uani 0.50 d P . H41A H 0.2916(6) 1.0233(4) 0.2780(3) 0.056 Uiso 0.50 calc PR . H41B H 0.4293(6) 0.9235(4) 0.2745(3) 0.056 Uiso 0.50 calc PR . S2 S 0.01688(8) 0.68604(6) 0.10715(5) 0.0551(2) Uani 1 d . . C24 C -0.0055(3) 0.8572(2) 0.0964(2) 0.0554(6) Uani 1 d . . H24A H 0.0320(3) 0.8838(2) 0.0341(2) 0.066 Uiso 0.50 calc PR 1 H24B H -0.1174(3) 0.8788(2) 0.1009(2) 0.066 Uiso 0.50 calc PR 1 H34A H -0.0549(3) 0.8768(2) 0.0357(2) 0.066 Uiso 0.50 calc PR 2 H34B H -0.0754(3) 0.8874(2) 0.1465(2) 0.066 Uiso 0.50 calc PR 2 C42 C 0.0839(6) 0.9279(4) 0.1713(4) 0.0482(11) Uani 0.50 d P 1 H42A H 0.0865(6) 1.0171(4) 0.1544(4) 0.058 Uiso 0.50 calc PR 1 H42B H 0.0276(6) 0.9202(4) 0.2314(4) 0.058 Uiso 0.50 calc PR 1 C43 C 0.3498(5) 0.9256(4) 0.1031(3) 0.0454(10) Uani 0.50 d P 2 H43A H 0.3700(5) 1.0158(4) 0.1099(3) 0.055 Uiso 0.50 calc PR 2 H43B H 0.2913(5) 0.9132(4) 0.0442(3) 0.055 Uiso 0.50 calc PR 2 N4 N 0.2500 0.8820(2) 0.1844(2) 0.0344(5) Uani 1 d S . N5 N 0.2500 0.4966(2) 0.1914(2) 0.0420(6) Uani 1 d S . N51 N 0.2500 0.3818(3) 0.1961(2) 0.0612(8) Uani 1 d S . C52 C 0.2500 0.3083(4) 0.1126(4) 0.091(2) Uani 1 d S . H52A H 0.1886(39) 0.2327(19) 0.1228(10) 0.136 Uiso 0.50 calc PR . H52B H 0.3573(4) 0.2856(31) 0.0965(16) 0.136 Uiso 0.50 calc PR . H52C H 0.2041(43) 0.3563(14) 0.0614(8) 0.136 Uiso 0.50 calc PR . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo 0.0352(2) 0.0319(2) 0.0323(2) 0.00277(9) 0.000 0.000 S1 0.0831(6) 0.0560(5) 0.0314(4) 0.0097(4) 0.000 0.000 C14 0.077(2) 0.063(2) 0.033(2) -0.006(2) 0.000 0.000 C41 0.057(3) 0.043(2) 0.039(2) -0.008(2) -0.002(2) -0.005(2) S2 0.0471(3) 0.0530(3) 0.0652(4) 0.0031(3) -0.0195(3) -0.0085(3) C24 0.0480(13) 0.0631(15) 0.0551(14) 0.0045(12) -0.0154(12) 0.0102(12) C42 0.047(2) 0.044(2) 0.054(3) 0.001(2) 0.001(2) 0.013(2) C43 0.056(3) 0.041(2) 0.040(2) 0.005(2) 0.007(2) -0.003(2) N4 0.0375(13) 0.0345(12) 0.0312(12) 0.0016(10) 0.000 0.000 N5 0.0471(14) 0.0361(14) 0.0428(14) 0.0051(11) 0.000 0.000 N51 0.078(2) 0.040(2) 0.065(2) 0.0072(13) 0.000 0.000 C52 0.120(4) 0.055(2) 0.097(4) -0.027(2) 0.000 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo N5 1.809(3) . ? Mo N4 2.256(2) . ? Mo S2 2.2875(6) . ? Mo S2 2.2875(6) 2 ? Mo S1 2.3117(9) . ? S1 C14 1.833(4) . ? C14 C41 1.488(5) . ? C14 H14A 0.97 . ? C14 H14B 0.97 . ? C41 N4 1.483(4) . ? C41 H41A 0.97 . ? C41 H41B 0.97 . ? S2 C24 1.821(2) . ? C24 C42 1.491(5) . ? C24 C43 1.497(5) 2 ? C24 H24A 0.97 . ? C24 H24B 0.97 . ? C24 H34A 0.97 . ? C24 H34B 0.97 . ? C42 N4 1.489(5) . ? C42 H42A 0.97 . ? C42 H42B 0.97 . ? C43 N4 1.489(4) . ? C43 C24 1.497(5) 2 ? C43 H43A 0.97 . ? C43 H43B 0.97 . ? N4 C41 1.483(4) 2 ? N4 C43 1.489(4) 2 ? N4 C42 1.489(5) 2 ? N5 N51 1.213(4) . ? N51 C52 1.405(5) . ? C52 H52A 0.96 . ? C52 H52B 0.96 . ? C52 H52C 0.96 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N5 Mo N4 178.53(10) . . ? N5 Mo S2 95.00(4) . . ? N4 Mo S2 84.25(3) . . ? N5 Mo S2 95.00(4) . 2 ? N4 Mo S2 84.25(3) . 2 ? S2 Mo S2 117.97(4) . 2 ? N5 Mo S1 97.17(8) . . ? N4 Mo S1 84.30(6) . . ? S2 Mo S1 119.54(2) . . ? S2 Mo S1 119.54(2) 2 . ? C14 S1 Mo 101.51(11) . . ? C41 C14 S1 112.6(2) . . ? C41 C14 H14A 109.1(2) . . ? S1 C14 H14A 109.072(15) . . ? C41 C14 H14B 109.1(2) . . ? S1 C14 H14B 109.07(8) . . ? H14A C14 H14B 107.8 . . ? N4 C41 C14 114.1(3) . . ? N4 C41 H41A 108.7(2) . . ? C14 C41 H41A 108.7(2) . . ? N4 C41 H41B 108.7(2) . . ? C14 C41 H41B 108.7(2) . . ? H41A C41 H41B 107.6 . . ? C24 S2 Mo 102.23(8) . . ? C42 C24 S2 112.7(2) . . ? C43 C24 S2 112.5(2) 2 . ? C42 C24 H24A 109.1(2) . . ? S2 C24 H24A 109.06(9) . . ? C42 C24 H24B 109.1(2) . . ? S2 C24 H24B 109.06(9) . . ? H24A C24 H24B 107.8 . . ? C43 C24 H34A 109.1(2) 2 . ? S2 C24 H34A 109.11(8) . . ? C43 C24 H34B 109.1(2) 2 . ? S2 C24 H34B 109.11(9) . . ? H34A C24 H34B 107.8 . . ? N4 C42 C24 113.4(3) . . ? N4 C42 H42A 108.9(2) . . ? C24 C42 H42A 108.9(2) . . ? N4 C42 H42B 108.9(2) . . ? C24 C42 H42B 108.9(2) . . ? H42A C42 H42B 107.7 . . ? N4 C43 C24 113.1(3) . 2 ? N4 C43 H43A 109.0(2) . . ? C24 C43 H43A 109.0(2) 2 . ? N4 C43 H43B 109.0(2) . . ? C24 C43 H43B 109.0(2) 2 . ? H43A C43 H43B 107.8 . . ? C41 N4 C41 43.0(4) . 2 ? C41 N4 C43 138.6(3) . 2 ? C41 N4 C43 109.7(3) 2 2 ? C41 N4 C43 109.7(3) . . ? C41 N4 C43 138.6(3) 2 . ? C43 N4 C43 68.6(4) 2 . ? C41 N4 C42 69.1(3) . 2 ? C41 N4 C42 109.3(3) 2 2 ? C41 N4 C42 109.3(3) . . ? C41 N4 C42 69.1(3) 2 . ? C42 N4 C42 139.4(4) 2 . ? C41 N4 Mo 109.5(2) . . ? C41 N4 Mo 109.5(2) 2 . ? C43 N4 Mo 109.6(2) 2 . ? C43 N4 Mo 109.6(2) . . ? C42 N4 Mo 109.2(2) 2 . ? C42 N4 Mo 109.2(2) . . ? N51 N5 Mo 177.4(3) . . ? N5 N51 C52 120.3(3) . . ? N51 C52 H52A 109.5(2) . . ? N51 C52 H52B 109.47(2) . . ? H52A C52 H52B 109.5 . . ? N51 C52 H52C 109.5(2) . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? _refine_diff_density_max 0.471 _refine_diff_density_min -0.221 _refine_diff_density_rms 0.054 #===end data_ray20 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C12 H17 Mo N2 S3' _chemical_formula_structural [Mo{N(CH2CH2S)3)}(NNPh)] _chemical_formula_analytical ? _chemical_formula_sum 'C12 H17 Mo N3 S3' _chemical_formula_weight 395.41 _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' 'Mo' 'Mo' -1.6832 0.6857 '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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P c a b (equiv. to no. 61) ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y, -z+1/2' '-x, -y+1/2, z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z' '-x-1/2, y, z-1/2' 'x, y-1/2, -z-1/2' _cell_length_a 15.1833(14) _cell_length_b 12.2873(14) _cell_length_c 16.861(2) _cell_angle_alpha 90.000(9) _cell_angle_beta 90.000(8) _cell_angle_gamma 90.000(8) _cell_volume 3145.6(6) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10 _cell_measurement_theta_max 11 _exptl_crystal_description 'diamond prisms' _exptl_crystal_colour 'Very dark red' _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.670 _exptl_crystal_density_method ? _exptl_crystal_F_000 1600 _exptl_absorpt_coefficient_mu 1.222 _exptl_absorpt_correction_type 'semi-empirical psi-scans' _exptl_absorpt_correction_T_min 0.98 _exptl_absorpt_correction_T_max 1.00 _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 'Enraf-Nonius CAD4 diffractometer' _diffrn_measurement_method 'scintillation counter; \w/\q scans' _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time '10000 s' _diffrn_standards_decay_% 4.0 _diffrn_reflns_number 3168 _diffrn_reflns_av_R_equivalents 0.036 _diffrn_reflns_av_sigmaI/netI 0.0590 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.5 _diffrn_reflns_theta_max 25 _reflns_number_total 2759 _reflns_number_observed 1266 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'CAD4/EXPRESS (Enraf-Nonius, 1992) ' _computing_cell_refinement 'CAD4/EXPRESS (Enraf-Nonius, 1992) ' _computing_data_reduction 'CAD4 (Hursthouse, 1976) ' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'ORTEP (Johnson, 1971)' _computing_publication_material 'SHELXL-93 (Sheldrick, 1993)' _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^)+(0.0418P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'automated Patterson' _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ; Coordinates were of idealised positions and set to ride on the parent carbon atoms. They were not included in the disordered phenyl ring with site occupancy of 0.2. Isotropic thermal parameters were set to be 1.2 x Ueq of the parent carbons. ; _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2759 _refine_ls_number_parameters 181 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1030 _refine_ls_R_factor_obs 0.0383 _refine_ls_wR_factor_all 0.1137 _refine_ls_wR_factor_obs 0.0852 _refine_ls_goodness_of_fit_all 0.994 _refine_ls_goodness_of_fit_obs 1.142 _refine_ls_restrained_S_all 0.994 _refine_ls_restrained_S_obs 1.142 _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 Mo Mo 0.01347(3) 0.25010(6) 0.04064(3) 0.0417(2) Uani 1 d . . S1 S -0.04175(12) 0.0910(2) 0.09011(12) 0.0624(6) Uani 1 d . . C14 C -0.1415(4) 0.0720(6) 0.0309(4) 0.064(2) Uani 1 d . . H14A H -0.1287(4) 0.0234(6) -0.0129(4) 0.077 Uiso 0.50 calc PR 1 H14B H -0.1864(4) 0.0379(6) 0.0635(4) 0.077 Uiso 0.50 calc PR 1 H14C H -0.1494(4) -0.0048(6) 0.0196(4) 0.077 Uiso 0.50 calc PR 2 H14D H -0.1923(4) 0.0967(6) 0.0609(4) 0.077 Uiso 0.50 calc PR 2 S2 S -0.05003(13) 0.4115(2) 0.08170(12) 0.0625(6) Uani 1 d . . C24 C -0.1458(5) 0.4201(7) 0.0150(5) 0.076(3) Uani 1 d . . H24A H -0.1980(5) 0.3969(7) 0.0436(5) 0.091 Uiso 0.50 calc PR 1 H24B H -0.1544(5) 0.4954(7) -0.0004(5) 0.091 Uiso 0.50 calc PR 1 H24C H -0.1951(5) 0.4506(7) 0.0441(5) 0.091 Uiso 0.50 calc PR 2 H24D H -0.1320(5) 0.4695(7) -0.0281(5) 0.091 Uiso 0.50 calc PR 2 S3 S 0.09406(10) 0.2448(2) -0.07380(10) 0.0650(5) Uani 1 d . . C34 C 0.0090(4) 0.2359(8) -0.1488(4) 0.079(2) Uani 1 d . . H34A H -0.0027(4) 0.3080(8) -0.1698(4) 0.095 Uiso 0.50 calc PR 1 H34B H 0.0296(4) 0.1906(8) -0.1921(4) 0.095 Uiso 0.50 calc PR 1 H34C H 0.0294(4) 0.2724(8) -0.1964(4) 0.095 Uiso 0.50 calc PR 2 H34D H -0.0003(4) 0.1599(8) -0.1620(4) 0.095 Uiso 0.50 calc PR 2 C41A C -0.1750(9) 0.1726(12) 0.0002(8) 0.054(4) Uiso 0.50 d P 1 H41A H -0.2002(9) 0.2143(12) 0.0435(8) 0.065 Uiso 0.50 calc PR 1 H41B H -0.2219(9) 0.1570(12) -0.0371(8) 0.065 Uiso 0.50 calc PR 1 C42A C -0.1366(11) 0.3530(13) -0.0575(9) 0.063(4) Uiso 0.50 d P 1 H42A H -0.1937(11) 0.3474(13) -0.0831(9) 0.075 Uiso 0.50 calc PR 1 H42B H -0.0970(11) 0.3895(13) -0.0939(9) 0.075 Uiso 0.50 calc PR 1 C43A C -0.0775(9) 0.1874(12) -0.1148(8) 0.058(4) Uiso 0.50 d P 1 H43A H -0.1241(9) 0.1942(12) -0.1539(8) 0.070 Uiso 0.50 calc PR 1 H43B H -0.0691(9) 0.1106(12) -0.1039(8) 0.070 Uiso 0.50 calc PR 1 C41B C -0.1357(10) 0.1364(12) -0.0482(9) 0.059(4) Uiso 0.50 d P 2 H41C H -0.0982(10) 0.0962(12) -0.0844(9) 0.071 Uiso 0.50 calc PR 2 H41D H -0.1940(10) 0.1393(12) -0.0716(9) 0.071 Uiso 0.50 calc PR 2 C42B C -0.1709(10) 0.3202(13) -0.0166(10) 0.061(4) Uiso 0.50 d P 2 H42C H -0.2084(10) 0.3348(13) -0.0620(10) 0.074 Uiso 0.50 calc PR 2 H42D H -0.2070(10) 0.2837(13) 0.0227(10) 0.074 Uiso 0.50 calc PR 2 C43B C -0.0727(9) 0.2822(11) -0.1257(8) 0.061(4) Uiso 0.50 d P 2 H43C H -0.1172(9) 0.2629(11) -0.1645(8) 0.073 Uiso 0.50 calc PR 2 H43D H -0.0672(9) 0.3608(11) -0.1255(8) 0.073 Uiso 0.50 calc PR 2 N4 N -0.1032(3) 0.2433(6) -0.0421(3) 0.0504(12) Uani 1 d . . N5 N 0.1084(3) 0.2561(5) 0.1044(3) 0.0472(11) Uani 1 d . . N51 N 0.1770(3) 0.2534(6) 0.1435(3) 0.0593(13) Uani 1 d . . C511 C 0.1987(5) 0.3473(6) 0.1936(4) 0.038(2) Uani 0.80 d P 3 C512 C 0.1408(5) 0.4340(7) 0.2092(4) 0.047(2) Uani 0.80 d P 3 H512 H 0.0836(5) 0.4324(7) 0.1895(4) 0.057 Uiso 0.80 calc PR 3 C513 C 0.1689(9) 0.5220(10) 0.2541(8) 0.076(5) Uani 0.80 d P 3 H513 H 0.1321(9) 0.5816(10) 0.2621(8) 0.091 Uiso 0.80 calc PR 3 C514 C 0.2518(8) 0.5200(7) 0.2867(6) 0.073(3) Uani 0.80 d P 3 H514 H 0.2706(8) 0.5779(7) 0.3180(6) 0.088 Uiso 0.80 calc PR 3 C515 C 0.3058(7) 0.4361(9) 0.2741(5) 0.073(3) Uani 0.80 d P 3 H515 H 0.3617(7) 0.4372(9) 0.2966(5) 0.088 Uiso 0.80 calc PR 3 C516 C 0.2811(6) 0.3473(8) 0.2283(5) 0.061(3) Uani 0.80 d P 3 H516 H 0.3193(6) 0.2890(8) 0.2212(5) 0.073 Uiso 0.80 calc PR 3 C521 C 0.1965(25) 0.1584(26) 0.1859(18) 0.094(16) Uiso 0.20 d PG 4 C522 C 0.1354(18) 0.0775(33) 0.2030(23) 0.112(19) Uiso 0.20 d PG 4 C523 C 0.1587(24) -0.0091(27) 0.2517(27) 0.045(15) Uiso 0.20 d PG 4 C524 C 0.2431(28) -0.0148(27) 0.2833(24) 0.152(28) Uiso 0.20 d PG 4 C525 C 0.3042(19) 0.0661(33) 0.2663(21) 0.098(16) Uiso 0.20 d PG 4 C526 C 0.2809(22) 0.1527(26) 0.2176(20) 0.077(14) Uiso 0.20 d PG 4 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo 0.0306(3) 0.0417(3) 0.0529(3) -0.0028(4) -0.0017(2) 0.0007(3) S1 0.0505(11) 0.0574(13) 0.0792(14) 0.0095(11) 0.0039(10) -0.0030(10) C14 0.050(4) 0.055(5) 0.087(6) 0.004(4) 0.007(4) -0.008(4) S2 0.0575(12) 0.0516(13) 0.0785(13) -0.0165(11) -0.0082(11) 0.0173(11) C24 0.050(5) 0.086(7) 0.091(6) 0.000(5) -0.012(4) 0.036(5) S3 0.0396(8) 0.0913(13) 0.0640(9) -0.0007(15) 0.0064(7) -0.0031(13) C34 0.052(4) 0.121(7) 0.065(4) -0.002(6) 0.002(3) -0.001(5) N4 0.032(2) 0.055(3) 0.064(3) -0.004(4) -0.004(2) 0.002(3) N5 0.037(2) 0.047(3) 0.058(3) -0.009(4) -0.002(2) 0.004(3) N51 0.040(3) 0.064(3) 0.074(3) -0.002(4) -0.014(2) 0.005(4) C511 0.042(4) 0.046(4) 0.026(4) 0.005(3) -0.006(3) -0.003(4) C512 0.054(5) 0.051(5) 0.036(4) -0.008(4) -0.017(4) 0.016(4) C513 0.111(11) 0.045(8) 0.071(8) -0.011(8) -0.032(7) 0.009(6) C514 0.116(9) 0.039(5) 0.064(6) 0.004(4) -0.044(6) 0.012(6) C515 0.073(6) 0.078(7) 0.068(7) 0.001(6) -0.039(5) -0.029(6) C516 0.051(6) 0.064(6) 0.067(6) 0.001(5) -0.010(4) -0.003(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo N5 1.801(4) . ? Mo N4 2.257(4) . ? Mo S1 2.285(2) . ? Mo S3 2.286(2) . ? Mo S2 2.311(2) . ? S1 C14 1.829(7) . ? C14 C41A 1.434(14) . ? C14 C41B 1.554(15) . ? C14 H14A 0.97 . ? C14 H14B 0.97 . ? C14 H14C 0.97 . ? C14 H14D 0.97 . ? S2 C24 1.842(7) . ? C24 C42B 1.39(2) . ? C24 C42A 1.48(2) . ? C24 H24A 0.97 . ? C24 H24B 0.97 . ? C24 H24C 0.97 . ? C24 H24D 0.97 . ? S3 C34 1.811(7) . ? C34 C43B 1.418(15) . ? C34 C43A 1.552(15) . ? C34 H34A 0.97 . ? C34 H34B 0.97 . ? C34 H34C 0.97 . ? C34 H34D 0.97 . ? C41A N4 1.566(14) . ? C41A H41A 0.97 . ? C41A H41B 0.97 . ? C42A N4 1.462(15) . ? C42A H42A 0.97 . ? C42A H42B 0.97 . ? C43A N4 1.459(14) . ? C43A H43A 0.97 . ? C43A H43B 0.97 . ? C41B N4 1.407(14) . ? C41B H41C 0.97 . ? C41B H41D 0.97 . ? C42B N4 1.46(2) . ? C42B H42C 0.97 . ? C42B H42D 0.97 . ? C43B N4 1.559(14) . ? C43B H43C 0.97 . ? C43B H43D 0.97 . ? N5 N51 1.232(6) . ? N51 C521 1.40(3) . ? N51 C511 1.468(9) . ? C511 C516 1.382(10) . ? C511 C512 1.406(10) . ? C512 C513 1.39(2) . ? C512 H512 0.93 . ? C513 C514 1.374(15) . ? C513 H513 0.93 . ? C514 C515 1.334(13) . ? C514 H514 0.93 . ? C515 C516 1.388(11) . ? C515 H515 0.93 . ? C516 H516 0.93 . ? C521 C522 1.39 . ? C521 C526 1.39 . ? C522 C523 1.39 . ? C523 C524 1.39 . ? C524 C525 1.39 . ? C525 C526 1.39 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N5 Mo N4 178.5(2) . . ? N5 Mo S1 96.4(2) . . ? N4 Mo S1 84.6(2) . . ? N5 Mo S3 94.40(14) . . ? N4 Mo S3 84.11(12) . . ? S1 Mo S3 118.69(9) . . ? N5 Mo S2 96.9(2) . . ? N4 Mo S2 83.6(2) . . ? S1 Mo S2 118.15(7) . . ? S3 Mo S2 120.05(9) . . ? C14 S1 Mo 102.4(2) . . ? C41A C14 S1 112.4(7) . . ? C41B C14 S1 110.9(7) . . ? C41A C14 H14A 109.1(7) . . ? S1 C14 H14A 109.1(2) . . ? C41A C14 H14B 109.1(6) . . ? S1 C14 H14B 109.1(2) . . ? H14A C14 H14B 107.9 . . ? C41B C14 H14C 109.5(6) . . ? S1 C14 H14C 109.5(2) . . ? C41B C14 H14D 109.5(6) . . ? S1 C14 H14D 109.5(2) . . ? H14C C14 H14D 108.1 . . ? C24 S2 Mo 101.3(3) . . ? C42B C24 S2 113.5(8) . . ? C42A C24 S2 113.4(7) . . ? C42A C24 H24A 108.9(7) . . ? S2 C24 H24A 108.9(3) . . ? C42A C24 H24B 108.9(7) . . ? S2 C24 H24B 108.9(3) . . ? H24A C24 H24B 107.7 . . ? C42B C24 H24C 108.9(7) . . ? S2 C24 H24C 108.9(3) . . ? C42B C24 H24D 108.9(8) . . ? S2 C24 H24D 108.9(3) . . ? H24C C24 H24D 107.7 . . ? C34 S3 Mo 102.1(2) . . ? C43B C34 S3 114.0(7) . . ? C43A C34 S3 111.6(7) . . ? C43A C34 H34A 109.3(7) . . ? S3 C34 H34A 109.3(3) . . ? C43A C34 H34B 109.3(6) . . ? S3 C34 H34B 109.3(3) . . ? H34A C34 H34B 108.0 . . ? C43B C34 H34C 108.7(7) . . ? S3 C34 H34C 108.7(3) . . ? C43B C34 H34D 108.7(7) . . ? S3 C34 H34D 108.7(3) . . ? H34C C34 H34D 107.6 . . ? C14 C41A N4 113.3(10) . . ? C14 C41A H41A 108.9(7) . . ? N4 C41A H41A 108.9(6) . . ? C14 C41A H41B 108.9(6) . . ? N4 C41A H41B 108.9(5) . . ? H41A C41A H41B 107.7 . . ? N4 C42A C24 113.6(11) . . ? N4 C42A H42A 108.8(6) . . ? C24 C42A H42A 108.8(7) . . ? N4 C42A H42B 108.8(7) . . ? C24 C42A H42B 108.8(8) . . ? H42A C42A H42B 107.7 . . ? N4 C43A C34 110.8(10) . . ? N4 C43A H43A 109.5(6) . . ? C34 C43A H43A 109.5(6) . . ? N4 C43A H43B 109.5(7) . . ? C34 C43A H43B 109.5(7) . . ? H43A C43A H43B 108.1 . . ? N4 C41B C14 115.7(10) . . ? N4 C41B H41C 108.4(7) . . ? C14 C41B H41C 108.4(6) . . ? N4 C41B H41D 108.4(6) . . ? C14 C41B H41D 108.4(6) . . ? H41C C41B H41D 107.4 . . ? C24 C42B N4 119.4(12) . . ? C24 C42B H42C 107.5(7) . . ? N4 C42B H42C 107.5(6) . . ? C24 C42B H42D 107.5(8) . . ? N4 C42B H42D 107.5(7) . . ? H42C C42B H42D 107.0 . . ? C34 C43B N4 112.7(9) . . ? C34 C43B H43C 109.1(7) . . ? N4 C43B H43C 109.1(5) . . ? C34 C43B H43D 109.1(7) . . ? N4 C43B H43D 109.1(6) . . ? H43C C43B H43D 107.8 . . ? C41B N4 C42B 112.3(10) . . ? C43A N4 C42A 112.2(9) . . ? C41B N4 C43B 108.9(8) . . ? C42B N4 C43B 106.1(9) . . ? C43A N4 C41A 108.0(9) . . ? C42A N4 C41A 110.5(8) . . ? C41B N4 Mo 110.8(7) . . ? C43A N4 Mo 109.1(6) . . ? C42B N4 Mo 110.3(7) . . ? C42A N4 Mo 110.3(7) . . ? C43B N4 Mo 108.3(6) . . ? C41A N4 Mo 106.6(6) . . ? N51 N5 Mo 174.1(5) . . ? N5 N51 C521 118.4(17) . . ? N5 N51 C511 118.4(6) . . ? C516 C511 C512 119.1(7) . . ? C516 C511 N51 116.6(7) . . ? C512 C511 N51 124.3(7) . . ? C513 C512 C511 120.0(8) . . ? C513 C512 H512 120.0(6) . . ? C511 C512 H512 120.0(5) . . ? C514 C513 C512 119.1(9) . . ? C514 C513 H513 120.5(7) . . ? C512 C513 H513 120.5(6) . . ? C515 C514 C513 120.9(10) . . ? C515 C514 H514 119.6(6) . . ? C513 C514 H514 119.6(7) . . ? C514 C515 C516 122.0(9) . . ? C514 C515 H515 119.0(6) . . ? C516 C515 H515 119.0(6) . . ? C511 C516 C515 118.7(9) . . ? C511 C516 H516 120.7(5) . . ? C515 C516 H516 120.7(6) . . ? C522 C521 C526 120.0 . . ? C522 C521 N51 124.1(28) . . ? C526 C521 N51 115.7(28) . . ? C521 C522 C523 120.0 . . ? C522 C523 C524 120.0 . . ? C525 C524 C523 120.0 . . ? C526 C525 C524 120.0 . . ? C525 C526 C521 120.0 . . ? _refine_diff_density_max 0.866 _refine_diff_density_min -0.407 _refine_diff_density_rms 0.081 #===end data_ray22 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C6 H12 Mo N2 O S3' _chemical_formula_structural [Mo{N(CH2CH2S)3}(NO)] _chemical_formula_analytical ? _chemical_formula_sum 'C6 H12 Mo N2 O S3' _chemical_formula_weight 320.3 _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' 'Mo' 'Mo' -1.6832 0.6857 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P-1 (no. 2)' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.5200(13) _cell_length_b 13.435(2) _cell_length_c 7.9567(8) _cell_angle_alpha 90.410(9) _cell_angle_beta 101.230(10) _cell_angle_gamma 96.569(10) _cell_volume 1095.3(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10 _cell_measurement_theta_max 11 _exptl_crystal_description prisms _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.942 _exptl_crystal_density_method ? _exptl_crystal_F_000 640 _exptl_absorpt_coefficient_mu 1.733 _exptl_absorpt_correction_type 'semi-empirical psi-scans' _exptl_absorpt_correction_T_min 0.846 _exptl_absorpt_correction_T_max 0.998 _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 'Enraf-Nonius CAD4 diffractometer' _diffrn_measurement_method 'scintillation counter; \w/\q scans' _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time '10000 s' _diffrn_standards_decay_% 3.16 _diffrn_reflns_number 6811 _diffrn_reflns_av_R_equivalents 0.0222 _diffrn_reflns_av_sigmaI/netI 0.0415 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.5 _diffrn_reflns_theta_max 30 _reflns_number_total 6366 _reflns_number_observed 5078 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'CAD4/EXPRESS (Enraf-Nonius, 1992) ' _computing_cell_refinement 'CAD4/EXPRESS (Enraf-Nonius, 1992)' _computing_data_reduction 'CAD4 (Hursthouse, 1976)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'ORTEP (Johnson, 1971)' _computing_publication_material 'SHELXL-93 (Sheldrick, 1993)' _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^)+(0.0346P)^2^+0.1104P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'automated Patterson' _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ; Coordinates were located in idealised positions and subsequently allowed to refine freely. All isotropic thermal displacement parameters were allowed to refine freely. ; _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6366 _refine_ls_number_parameters 331 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0401 _refine_ls_R_factor_obs 0.0294 _refine_ls_wR_factor_all 0.0774 _refine_ls_wR_factor_obs 0.0708 _refine_ls_goodness_of_fit_all 1.060 _refine_ls_goodness_of_fit_obs 1.092 _refine_ls_restrained_S_all 1.060 _refine_ls_restrained_S_obs 1.092 _refine_ls_shift/esd_max -0.002 _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 0.20839(2) 0.205287(15) 0.08789(3) 0.02643(6) Uani 1 d . . S1 S -0.00611(6) 0.23360(5) 0.03807(10) 0.03606(14) Uani 1 d . . C14 C 0.0076(3) 0.3695(2) 0.0669(4) 0.0358(6) Uani 1 d . . H14A H 0.0004(28) 0.3962(22) -0.0477(40) 0.032(8) Uiso 1 d . . H14B H -0.0695(28) 0.3806(21) 0.1105(38) 0.029(7) Uiso 1 d . . C41 C 0.1309(3) 0.4094(2) 0.1922(4) 0.0319(5) Uani 1 d . . H41A H 0.1442(27) 0.4879(21) 0.2048(37) 0.031(7) Uiso 1 d . . H41B H 0.1262(32) 0.3879(26) 0.3093(48) 0.052(10) Uiso 1 d . . S2 S 0.33306(7) 0.24127(6) -0.11729(10) 0.0419(2) Uani 1 d . . C24 C 0.3831(3) 0.3752(3) -0.0772(4) 0.0438(7) Uani 1 d . . H24A H 0.4716(31) 0.3862(23) -0.0100(41) 0.035(8) Uiso 1 d . . H24B H 0.3939(33) 0.3970(27) -0.1783(49) 0.050(10) Uiso 1 d . . C42 C 0.2837(3) 0.4250(2) -0.0035(4) 0.0384(6) Uani 1 d . . H42A H 0.3132(30) 0.4957(25) 0.0346(42) 0.040(8) Uiso 1 d . . H42B H 0.2028(32) 0.4274(24) -0.0917(43) 0.042(9) Uiso 1 d . . S3 S 0.30797(7) 0.18944(5) 0.36980(9) 0.03692(15) Uani 1 d . . C34 C 0.3432(3) 0.3208(2) 0.4437(3) 0.0351(5) Uani 1 d . . H34A H 0.2674(28) 0.3321(22) 0.4987(38) 0.031(7) Uiso 1 d . . H34B H 0.4222(31) 0.3220(24) 0.5223(43) 0.041(9) Uiso 1 d . . C43 C 0.3603(3) 0.3900(2) 0.2985(4) 0.0357(6) Uani 1 d . . H43A H 0.3686(26) 0.4622(21) 0.3391(36) 0.026(7) Uiso 1 d . . H43B H 0.4448(30) 0.3787(23) 0.2625(41) 0.038(8) Uiso 1 d . . N4 N 0.2494(2) 0.37159(15) 0.1484(3) 0.0268(4) Uani 1 d . . N5 N 0.1761(2) 0.0751(2) 0.0305(3) 0.0370(5) Uani 1 d . . O5 O 0.1554(3) -0.0105(2) -0.0168(3) 0.0625(7) Uani 1 d . . Mo2 Mo 0.78802(2) 0.293524(15) 0.47728(3) 0.02717(6) Uani 1 d . . S6 S 1.00362(6) 0.26887(5) 0.54238(10) 0.03777(15) Uani 1 d . . C69 C 0.9931(3) 0.1337(2) 0.5647(4) 0.0371(6) Uani 1 d . . H69A H 1.0042(32) 0.1043(25) 0.4608(45) 0.047(9) Uiso 1 d . . H69B H 1.0763(29) 0.1226(23) 0.6532(41) 0.036(8) Uiso 1 d . . C96 C 0.8702(3) 0.0922(2) 0.6234(4) 0.0324(5) Uani 1 d . . H96A H 0.8569(28) 0.0134(23) 0.6182(39) 0.036(8) Uiso 1 d . . H96B H 0.8765(33) 0.1181(26) 0.7453(48) 0.053(10) Uiso 1 d . . S7 S 0.68420(7) 0.30945(5) 0.70485(9) 0.03682(15) Uani 1 d . . C79 C 0.6515(3) 0.1779(2) 0.7591(4) 0.0357(6) Uani 1 d . . H79A H 0.7257(32) 0.1672(25) 0.8530(44) 0.045(9) Uiso 1 d . . H79B H 0.5795(34) 0.1709(26) 0.7922(47) 0.051(10) Uiso 1 d . . C97 C 0.6394(3) 0.1074(2) 0.6062(4) 0.0338(5) Uani 1 d . . H97A H 0.6376(39) 0.0349(32) 0.6404(55) 0.075(13) Uiso 1 d . . H97B H 0.5557(28) 0.1139(21) 0.5248(38) 0.028(7) Uiso 1 d . . S8 S 0.66693(7) 0.25430(6) 0.20641(9) 0.0416(2) Uani 1 d . . C89 C 0.6208(3) 0.1196(2) 0.2176(4) 0.0420(6) Uani 1 d . . H89A H 0.5242(36) 0.1089(27) 0.2353(46) 0.054(10) Uiso 1 d . . H89B H 0.6144(38) 0.0899(30) 0.1069(54) 0.068(12) Uiso 1 d . . C98 C 0.7197(3) 0.0719(2) 0.3467(4) 0.0382(6) Uani 1 d . . H98A H 0.6860(35) 0.0030(29) 0.3635(49) 0.058(11) Uiso 1 d . . H98B H 0.8038(29) 0.0710(22) 0.3007(39) 0.034(8) Uiso 1 d . . N9 N 0.7509(2) 0.12728(15) 0.5164(3) 0.0263(4) Uani 1 d . . N10 N 0.8170(3) 0.4234(2) 0.4350(3) 0.0400(5) Uani 1 d . . O10 O 0.8363(3) 0.5083(2) 0.3970(3) 0.0681(8) 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 0.02945(11) 0.02376(10) 0.02668(11) 0.00070(7) 0.00582(8) 0.00522(7) S1 0.0285(3) 0.0322(3) 0.0440(4) -0.0047(3) -0.0001(3) 0.0014(2) C14 0.0314(12) 0.0321(13) 0.043(2) 0.0025(11) 0.0008(11) 0.0098(10) C41 0.0345(12) 0.0277(12) 0.0339(13) -0.0014(10) 0.0049(10) 0.0089(10) S2 0.0452(4) 0.0475(4) 0.0376(4) -0.0005(3) 0.0184(3) 0.0075(3) C24 0.044(2) 0.051(2) 0.039(2) 0.0108(13) 0.0172(13) 0.0016(13) C42 0.047(2) 0.0320(13) 0.0375(15) 0.0094(11) 0.0117(12) 0.0018(11) S3 0.0415(3) 0.0374(3) 0.0322(3) 0.0086(3) 0.0033(3) 0.0122(3) C34 0.0324(13) 0.0433(15) 0.0275(13) -0.0007(11) -0.0010(10) 0.0073(11) C43 0.0315(13) 0.0371(14) 0.0353(14) -0.0013(11) 0.0019(10) -0.0006(10) N4 0.0275(9) 0.0257(10) 0.0268(10) 0.0013(8) 0.0049(8) 0.0027(7) N5 0.0514(13) 0.0271(10) 0.0352(12) 0.0003(9) 0.0142(10) 0.0067(9) O5 0.106(2) 0.0256(10) 0.061(2) -0.0086(10) 0.0317(15) 0.0040(12) Mo2 0.03100(11) 0.02422(10) 0.02710(11) 0.00249(7) 0.00612(8) 0.00584(8) S6 0.0293(3) 0.0344(3) 0.0505(4) 0.0067(3) 0.0119(3) 0.0005(2) C69 0.0307(13) 0.0356(14) 0.048(2) 0.0031(12) 0.0122(11) 0.0098(10) C96 0.0330(12) 0.0269(12) 0.0382(14) 0.0047(10) 0.0064(10) 0.0078(9) S7 0.0416(3) 0.0368(3) 0.0353(3) -0.0048(3) 0.0119(3) 0.0109(3) C79 0.0321(13) 0.0432(15) 0.0349(14) 0.0019(11) 0.0142(11) 0.0043(11) C97 0.0315(12) 0.0356(13) 0.0348(14) 0.0008(11) 0.0105(10) -0.0008(10) S8 0.0470(4) 0.0472(4) 0.0293(3) 0.0041(3) 0.0013(3) 0.0105(3) C89 0.044(2) 0.047(2) 0.0312(14) -0.0075(12) 0.0024(12) 0.0021(13) C98 0.048(2) 0.0342(14) 0.0324(14) -0.0078(11) 0.0082(12) 0.0047(12) N9 0.0280(9) 0.0259(10) 0.0260(10) -0.0018(8) 0.0078(8) 0.0034(7) N10 0.0585(15) 0.0294(11) 0.0335(12) 0.0037(9) 0.0101(11) 0.0086(10) O10 0.121(2) 0.0275(11) 0.054(2) 0.0101(10) 0.014(2) 0.0076(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 N5 1.782(2) . ? Mo1 N4 2.257(2) . ? Mo1 S1 2.2900(7) . ? Mo1 S3 2.3058(8) . ? Mo1 S2 2.3063(8) . ? S1 C14 1.824(3) . ? C14 C41 1.514(4) . ? C14 H14A 0.97(3) . ? C14 H14B 0.97(3) . ? C41 N4 1.498(3) . ? C41 H41A 1.05(3) . ? C41 H41B 0.99(4) . ? S2 C24 1.824(3) . ? C24 C42 1.510(4) . ? C24 H24A 0.97(3) . ? C24 H24B 0.88(4) . ? C42 N4 1.493(3) . ? C42 H42A 0.99(3) . ? C42 H42B 1.00(3) . ? S3 C34 1.830(3) . ? C34 C43 1.514(4) . ? C34 H34A 1.01(3) . ? C34 H34B 0.94(3) . ? C43 N4 1.495(3) . ? C43 H43A 1.01(3) . ? C43 H43B 1.01(3) . ? N5 O5 1.191(3) . ? Mo2 N10 1.782(2) . ? Mo2 N9 2.257(2) . ? Mo2 S6 2.2890(8) . ? Mo2 S8 2.3036(8) . ? Mo2 S7 2.3099(7) . ? S6 C69 1.819(3) . ? C69 C96 1.509(4) . ? C69 H69A 0.95(4) . ? C69 H69B 1.04(3) . ? C96 N9 1.499(3) . ? C96 H96A 1.05(3) . ? C96 H96B 1.02(4) . ? S7 C79 1.832(3) . ? C79 C97 1.514(4) . ? C79 H79A 0.99(3) . ? C79 H79B 0.84(4) . ? C97 N9 1.489(3) . ? C97 H97A 1.01(4) . ? C97 H97B 1.00(3) . ? S8 C89 1.827(3) . ? C89 C98 1.515(4) . ? C89 H89A 1.05(4) . ? C89 H89B 0.95(4) . ? C98 N9 1.497(3) . ? C98 H98A 0.97(4) . ? C98 H98B 1.02(3) . ? N10 O10 1.188(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N5 Mo1 N4 177.46(9) . . ? N5 Mo1 S1 95.43(8) . . ? N4 Mo1 S1 84.52(5) . . ? N5 Mo1 S3 97.52(8) . . ? N4 Mo1 S3 84.75(6) . . ? S1 Mo1 S3 116.73(3) . . ? N5 Mo1 S2 93.81(8) . . ? N4 Mo1 S2 84.05(5) . . ? S1 Mo1 S2 120.38(3) . . ? S3 Mo1 S2 120.10(3) . . ? C14 S1 Mo1 101.88(9) . . ? C41 C14 S1 111.5(2) . . ? C41 C14 H14A 114.7(17) . . ? S1 C14 H14A 105.8(18) . . ? C41 C14 H14B 111.3(17) . . ? S1 C14 H14B 103.9(17) . . ? H14A C14 H14B 108.9(24) . . ? N4 C41 C14 111.9(2) . . ? N4 C41 H41A 110.5(15) . . ? C14 C41 H41A 113.0(15) . . ? N4 C41 H41B 106.9(20) . . ? C14 C41 H41B 110.7(20) . . ? H41A C41 H41B 103.3(25) . . ? C24 S2 Mo1 101.62(10) . . ? C42 C24 S2 111.5(2) . . ? C42 C24 H24A 114.8(19) . . ? S2 C24 H24A 109.9(18) . . ? C42 C24 H24B 114.1(23) . . ? S2 C24 H24B 103.5(24) . . ? H24A C24 H24B 102.2(28) . . ? N4 C42 C24 111.7(2) . . ? N4 C42 H42A 106.6(19) . . ? C24 C42 H42A 113.6(18) . . ? N4 C42 H42B 109.1(19) . . ? C24 C42 H42B 110.4(19) . . ? H42A C42 H42B 105.2(26) . . ? C34 S3 Mo1 101.21(9) . . ? C43 C34 S3 111.7(2) . . ? C43 C34 H34A 114.1(17) . . ? S3 C34 H34A 103.8(17) . . ? C43 C34 H34B 110.1(20) . . ? S3 C34 H34B 103.1(20) . . ? H34A C34 H34B 113.4(26) . . ? N4 C43 C34 112.2(2) . . ? N4 C43 H43A 109.1(16) . . ? C34 C43 H43A 110.3(16) . . ? N4 C43 H43B 109.8(18) . . ? C34 C43 H43B 107.8(18) . . ? H43A C43 H43B 107.6(23) . . ? C42 N4 C43 110.0(2) . . ? C42 N4 C41 109.3(2) . . ? C43 N4 C41 109.3(2) . . ? C42 N4 Mo1 109.7(2) . . ? C43 N4 Mo1 108.9(2) . . ? C41 N4 Mo1 109.66(15) . . ? O5 N5 Mo1 176.4(2) . . ? N10 Mo2 N9 177.05(9) . . ? N10 Mo2 S6 95.49(9) . . ? N9 Mo2 S6 84.54(5) . . ? N10 Mo2 S8 93.36(8) . . ? N9 Mo2 S8 84.10(6) . . ? S6 Mo2 S8 120.36(3) . . ? N10 Mo2 S7 97.81(8) . . ? N9 Mo2 S7 84.79(5) . . ? S6 Mo2 S7 116.91(3) . . ? S8 Mo2 S7 119.97(3) . . ? C69 S6 Mo2 101.78(9) . . ? C96 C69 S6 111.9(2) . . ? C96 C69 H69A 114.3(21) . . ? S6 C69 H69A 108.4(21) . . ? C96 C69 H69B 112.0(17) . . ? S6 C69 H69B 104.5(17) . . ? H69A C69 H69B 105.0(26) . . ? N9 C96 C69 112.0(2) . . ? N9 C96 H96A 107.5(16) . . ? C69 C96 H96A 111.9(16) . . ? N9 C96 H96B 107.3(19) . . ? C69 C96 H96B 107.8(20) . . ? H96A C96 H96B 110.3(26) . . ? C79 S7 Mo2 100.94(9) . . ? C97 C79 S7 112.2(2) . . ? C97 C79 H79A 112.8(19) . . ? S7 C79 H79A 104.4(19) . . ? C97 C79 H79B 107.8(25) . . ? S7 C79 H79B 107.7(24) . . ? H79A C79 H79B 111.9(31) . . ? N9 C97 C79 112.3(2) . . ? N9 C97 H97A 106.0(23) . . ? C79 C97 H97A 112.0(24) . . ? N9 C97 H97B 109.9(16) . . ? C79 C97 H97B 109.1(17) . . ? H97A C97 H97B 107.4(27) . . ? C89 S8 Mo2 102.04(10) . . ? C98 C89 S8 111.6(2) . . ? C98 C89 H89A 116.3(20) . . ? S8 C89 H89A 107.6(20) . . ? C98 C89 H89B 109.7(24) . . ? S8 C89 H89B 108.4(24) . . ? H89A C89 H89B 102.7(30) . . ? N9 C98 C89 112.0(2) . . ? N9 C98 H98A 108.7(23) . . ? C89 C98 H98A 109.7(22) . . ? N9 C98 H98B 108.9(17) . . ? C89 C98 H98B 109.4(17) . . ? H98A C98 H98B 108.1(27) . . ? C97 N9 C98 109.7(2) . . ? C97 N9 C96 109.3(2) . . ? C98 N9 C96 109.2(2) . . ? C97 N9 Mo2 109.1(2) . . ? C98 N9 Mo2 109.9(2) . . ? C96 N9 Mo2 109.56(15) . . ? O10 N10 Mo2 176.1(2) . . ? _refine_diff_density_max 0.464 _refine_diff_density_min -1.168 _refine_diff_density_rms 0.140 #===end data_ray17 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C24 H52 N4 S12 W2' _chemical_formula_structural [{W[N(CH2CH2S)3]}2{mu-SCH2CH2N(CH2CH2SH)2}2] _chemical_formula_analytical ? _chemical_formula_sum 'C24 H52 N4 S12 W2' _chemical_formula_weight 1149.1 _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' 'W' 'W' -0.8490 6.8722 '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/a (equiv. to no. 14)' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' _cell_length_a 12.2952(14) _cell_length_b 13.9137(15) _cell_length_c 11.6072(14) _cell_angle_alpha 90.00 _cell_angle_beta 107.072(10) _cell_angle_gamma 90.00 _cell_volume 1898.2(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 8 _cell_measurement_theta_max 10 _exptl_crystal_description 'thin, rectangular plates' _exptl_crystal_colour 'dark brown' _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.010 _exptl_crystal_density_method ? _exptl_crystal_F_000 1128 _exptl_absorpt_coefficient_mu 6.740 _exptl_absorpt_correction_type 'semi-empirical, psi-scans' _exptl_absorpt_correction_T_min 0.69 _exptl_absorpt_correction_T_max 0.73 _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 'Enraf-Nonius CAD4 diffractometer' _diffrn_measurement_method 'scintillation counter; \w/\q scans' _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time '10000 s' _diffrn_standards_decay_% 3.0 _diffrn_reflns_number 3076 _diffrn_reflns_av_R_equivalents 0.048 _diffrn_reflns_av_sigmaI/netI 0.0720 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 22.97 _reflns_number_total 2636 _reflns_number_observed 1853 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'CAD4/EXPRESS (Enraf-Nonius, 1992) _computing_cell_refinement 'CAD4/EXPRESS (Enraf-Nonius, 1992) _computing_data_reduction 'CAD4 (Hursthouse, 1976) _computing_structure_solution 'SHELX (Sheldrick, 1976)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'ORTEP (Johnson, 1971) _computing_publication_material 'SHELXL-93 (Sheldrick, 1993)' _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^)+(0.0767P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'heavy atom' _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 'riding in idealised positions' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2636 _refine_ls_number_parameters 189 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0714 _refine_ls_R_factor_obs 0.0478 _refine_ls_wR_factor_all 0.1304 _refine_ls_wR_factor_obs 0.1126 _refine_ls_goodness_of_fit_all 1.000 _refine_ls_goodness_of_fit_obs 1.043 _refine_ls_restrained_S_all 1.000 _refine_ls_restrained_S_obs 1.043 _refine_ls_shift/esd_max 0.007 _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 W W 0.04969(4) 0.58133(3) -0.02549(5) 0.0394(2) Uani 1 d . . S1 S -0.0033(3) 0.7067(3) -0.1731(4) 0.0671(11) Uani 1 d . . C11 C 0.1370(15) 0.7433(16) -0.1758(17) 0.110(8) Uani 1 d . . H11A H 0.1673(15) 0.6952(16) -0.2186(17) 0.132 Uiso 1 calc R . H11B H 0.1311(15) 0.8034(16) -0.2195(17) 0.132 Uiso 1 calc R . C12 C 0.2163(12) 0.7558(11) -0.0541(14) 0.068(4) Uani 1 d . . H12A H 0.1964(12) 0.8141(11) -0.0193(14) 0.081 Uiso 1 calc R . H12B H 0.2926(12) 0.7639(11) -0.0607(14) 0.081 Uiso 1 calc R . S2 S 0.1648(3) 0.4953(3) -0.1246(4) 0.0581(10) Uani 1 d . . C21 C 0.3018(13) 0.5569(12) -0.0791(17) 0.077(5) Uani 1 d . . H21A H 0.3624(13) 0.5100(12) -0.0675(17) 0.093 Uiso 1 calc R . H21B H 0.3067(13) 0.6003(12) -0.1428(17) 0.093 Uiso 1 calc R . C22 C 0.3171(11) 0.6108(11) 0.0314(18) 0.078(6) Uani 1 d . . H22A H 0.3831(11) 0.6521(11) 0.0438(18) 0.094 Uiso 1 calc R . H22B H 0.3323(11) 0.5662(11) 0.0984(18) 0.094 Uiso 1 calc R . S3 S 0.0145(3) 0.6717(2) 0.1308(3) 0.0507(9) Uani 1 d . . C31 C 0.1304(13) 0.7581(11) 0.1638(16) 0.073(5) Uani 1 d . . H31A H 0.1090(13) 0.8123(11) 0.1091(16) 0.087 Uiso 1 calc R . H31B H 0.1439(13) 0.7820(11) 0.2453(16) 0.087 Uiso 1 calc R . C32 C 0.2351(12) 0.7150(11) 0.1515(15) 0.068(4) Uani 1 d . . H32A H 0.2618(12) 0.6663(11) 0.2130(15) 0.082 Uiso 1 calc R . H32B H 0.2935(12) 0.7641(11) 0.1637(15) 0.082 Uiso 1 calc R . N4 N 0.2167(8) 0.6714(7) 0.0319(9) 0.046(3) Uani 1 d . . S5 S 0.1418(3) 0.4631(2) 0.1300(3) 0.0447(8) Uani 1 d . . C51 C 0.1469(12) 0.4890(10) 0.2900(12) 0.058(4) Uani 1 d . . H51A H 0.1658(12) 0.5561(10) 0.3082(12) 0.070 Uiso 1 calc R . H51B H 0.0728(12) 0.4770(10) 0.3009(12) 0.070 Uiso 1 calc R . C52 C 0.2333(14) 0.4272(12) 0.3727(16) 0.076(5) Uani 1 d . . H52A H 0.3077(14) 0.4452(12) 0.3669(16) 0.091 Uiso 1 calc R . H52B H 0.2195(14) 0.3611(12) 0.3454(16) 0.091 Uiso 1 calc R . S6 S 0.4719(5) 0.4934(6) 0.6922(7) 0.142(3) Uani 1 d . . C61 C 0.3625(24) 0.5568(19) 0.5915(33) 0.173(13) Uani 1 d . . H61A H 0.3596(24) 0.6198(19) 0.6263(33) 0.207 Uiso 1 calc R . H61B H 0.3850(24) 0.5666(19) 0.5190(33) 0.207 Uiso 1 calc R . C62 C 0.2517(22) 0.5211(23) 0.5557(20) 0.141(10) Uani 1 d . . H62A H 0.2239(22) 0.5199(23) 0.6257(20) 0.169 Uiso 1 calc R . H62B H 0.2045(22) 0.5661(23) 0.4986(20) 0.169 Uiso 1 calc R . S7 S -0.0257(7) 0.2635(6) 0.5422(7) 0.152(3) Uani 1 d . . C71A C 0.1081(53) 0.3072(41) 0.5285(47) 0.180(22) Uiso 0.68(5) d P 1 H71A H 0.1681(53) 0.2842(41) 0.5974(47) 0.216 Uiso 0.68(5) calc PR 1 H71B H 0.1202(53) 0.2784(41) 0.4571(47) 0.216 Uiso 0.68(5) calc PR 1 C72A C 0.1193(46) 0.4001(35) 0.5214(42) 0.143(18) Uiso 0.68(5) d P 1 H72A H 0.1115(46) 0.4295(35) 0.5944(42) 0.172 Uiso 0.68(5) calc PR 1 H72B H 0.0582(46) 0.4243(35) 0.4543(42) 0.172 Uiso 0.68(5) calc PR 1 C71B C 0.0327(53) 0.3679(44) 0.4867(49) 0.074(22) Uiso 0.32(5) d P 2 H71C H 0.0036(53) 0.3736(44) 0.3997(49) 0.089 Uiso 0.32(5) calc PR 2 H71D H 0.0179(53) 0.4268(44) 0.5240(49) 0.089 Uiso 0.32(5) calc PR 2 C72B C 0.1698(51) 0.3397(45) 0.5305(48) 0.068(19) Uiso 0.32(5) d P 2 H72C H 0.1944(51) 0.3242(45) 0.6157(48) 0.082 Uiso 0.32(5) calc PR 2 H72D H 0.1840(51) 0.2845(45) 0.4858(48) 0.082 Uiso 0.32(5) calc PR 2 N8 N 0.2362(16) 0.4314(13) 0.5042(14) 0.104(6) 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 W 0.0340(3) 0.0280(3) 0.0595(4) 0.0002(3) 0.0187(2) -0.0035(2) S1 0.063(2) 0.050(2) 0.082(3) 0.020(2) 0.012(2) -0.006(2) C11 0.084(13) 0.127(18) 0.094(14) 0.063(13) -0.013(11) -0.021(13) C12 0.054(9) 0.045(8) 0.101(12) 0.011(9) 0.016(9) -0.018(7) S2 0.058(2) 0.045(2) 0.083(3) -0.012(2) 0.041(2) -0.008(2) C21 0.055(10) 0.060(10) 0.125(15) -0.022(10) 0.041(10) -0.022(8) C22 0.030(8) 0.052(9) 0.159(18) 0.001(11) 0.037(10) -0.007(7) S3 0.045(2) 0.037(2) 0.075(2) -0.005(2) 0.025(2) 0.000(2) C31 0.072(11) 0.050(9) 0.105(13) -0.029(9) 0.041(10) -0.023(9) C32 0.048(9) 0.061(10) 0.095(12) -0.035(9) 0.021(8) -0.034(8) N4 0.031(6) 0.045(6) 0.058(7) -0.004(6) 0.008(5) -0.012(5) S5 0.038(2) 0.033(2) 0.064(2) -0.001(2) 0.015(2) 0.0013(14) C51 0.056(9) 0.050(9) 0.071(10) -0.008(8) 0.022(8) -0.006(8) C52 0.064(10) 0.073(11) 0.091(12) 0.008(10) 0.025(9) 0.008(9) S6 0.091(4) 0.179(8) 0.147(6) 0.026(5) 0.021(4) -0.009(5) C61 0.104(20) 0.122(22) 0.272(39) -0.002(23) 0.025(24) -0.013(18) C62 0.110(19) 0.200(29) 0.088(15) -0.048(18) -0.012(14) 0.036(20) S7 0.186(7) 0.147(7) 0.153(6) -0.002(5) 0.096(6) -0.033(6) N8 0.116(14) 0.114(14) 0.068(10) -0.028(10) 0.008(9) 0.000(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 W N4 2.329(9) . ? W S3 2.349(3) . ? W S2 2.391(3) . ? W S5 2.391(3) 3_565 ? W S1 2.397(4) . ? W S5 2.459(3) . ? W W 2.7185(9) 3_565 ? S1 C11 1.81(2) . ? C11 C12 1.47(2) . ? C11 H11A 0.97 . ? C11 H11B 0.97 . ? C12 N4 1.54(2) . ? C12 H12A 0.97 . ? C12 H12B 0.97 . ? S2 C21 1.824(14) . ? C21 C22 1.45(2) . ? C21 H21A 0.97 . ? C21 H21B 0.97 . ? C22 N4 1.50(2) . ? C22 H22A 0.97 . ? C22 H22B 0.97 . ? S3 C31 1.817(14) . ? C31 C32 1.47(2) . ? C31 H31A 0.97 . ? C31 H31B 0.97 . ? C32 N4 1.47(2) . ? C32 H32A 0.97 . ? C32 H32B 0.97 . ? S5 C51 1.875(14) . ? S5 W 2.391(3) 3_565 ? C51 C52 1.48(2) . ? C51 H51A 0.97 . ? C51 H51B 0.97 . ? C52 N8 1.52(2) . ? C52 H52A 0.97 . ? C52 H52B 0.97 . ? S6 C61 1.74(3) . ? C61 C62 1.39(3) . ? C61 H61A 0.97 . ? C61 H61B 0.97 . ? C62 N8 1.37(3) . ? C62 H62A 0.97 . ? C62 H62B 0.97 . ? S7 C71A 1.80(6) . ? S7 C71B 1.82(6) . ? C71A C72A 1.31(7) . ? C71A H71A 0.97 . ? C71A H71B 0.97 . ? C72A N8 1.57(5) . ? C72A H72A 0.97 . ? C72A H72B 0.97 . ? C71B C72B 1.66(10) . ? C71B H71C 0.97 . ? C71B H71D 0.97 . ? C72B N8 1.59(6) . ? C72B H72C 0.97 . ? C72B H72D 0.97 . ? 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 N4 W S3 80.7(3) . . ? N4 W S2 79.0(3) . . ? S3 W S2 155.32(13) . . ? N4 W S5 159.7(3) . 3_565 ? S3 W S5 98.79(12) . 3_565 ? S2 W S5 105.11(12) . 3_565 ? N4 W S1 81.1(3) . . ? S3 W S1 95.13(14) . . ? S2 W S1 95.47(14) . . ? S5 W S1 78.75(13) 3_565 . ? N4 W S5 88.4(3) . . ? S3 W S5 86.63(12) . . ? S2 W S5 78.93(13) . . ? S5 W S5 111.84(9) 3_565 . ? S1 W S5 168.92(12) . . ? N4 W W 143.2(3) . 3_565 ? S3 W W 94.65(9) . 3_565 ? S2 W W 93.19(9) . 3_565 ? S5 W W 57.10(8) 3_565 3_565 ? S1 W W 135.73(10) . 3_565 ? S5 W W 54.74(8) . 3_565 ? C11 S1 W 99.0(6) . . ? C12 C11 S1 112.6(13) . . ? C12 C11 H11A 109.1(12) . . ? S1 C11 H11A 109.1(8) . . ? C12 C11 H11B 109.1(10) . . ? S1 C11 H11B 109.1(6) . . ? H11A C11 H11B 107.8 . . ? C11 C12 N4 114.0(12) . . ? C11 C12 H12A 108.8(12) . . ? N4 C12 H12A 108.8(7) . . ? C11 C12 H12B 108.8(10) . . ? N4 C12 H12B 108.8(7) . . ? H12A C12 H12B 107.6 . . ? C21 S2 W 104.6(5) . . ? C22 C21 S2 111.6(11) . . ? C22 C21 H21A 109.3(9) . . ? S2 C21 H21A 109.3(5) . . ? C22 C21 H21B 109.3(10) . . ? S2 C21 H21B 109.3(6) . . ? H21A C21 H21B 108.0 . . ? C21 C22 N4 113.7(14) . . ? C21 C22 H22A 108.8(8) . . ? N4 C22 H22A 108.8(7) . . ? C21 C22 H22B 108.8(10) . . ? N4 C22 H22B 108.8(8) . . ? H22A C22 H22B 107.7 . . ? C31 S3 W 101.9(5) . . ? C32 C31 S3 111.4(10) . . ? C32 C31 H31A 109.3(10) . . ? S3 C31 H31A 109.3(6) . . ? C32 C31 H31B 109.3(9) . . ? S3 C31 H31B 109.3(5) . . ? H31A C31 H31B 108.0 . . ? C31 C32 N4 111.4(12) . . ? C31 C32 H32A 109.4(10) . . ? N4 C32 H32A 109.4(8) . . ? C31 C32 H32B 109.4(8) . . ? N4 C32 H32B 109.4(7) . . ? H32A C32 H32B 108.0 . . ? C32 N4 C22 109.7(12) . . ? C32 N4 C12 105.5(11) . . ? C22 N4 C12 105.8(11) . . ? C32 N4 W 111.8(8) . . ? C22 N4 W 110.8(8) . . ? C12 N4 W 113.0(7) . . ? C51 S5 W 107.1(5) . 3_565 ? C51 S5 W 118.2(5) . . ? W S5 W 68.16(9) 3_565 . ? C52 C51 S5 109.8(10) . . ? C52 C51 H51A 109.7(9) . . ? S5 C51 H51A 109.7(4) . . ? C52 C51 H51B 109.7(8) . . ? S5 C51 H51B 109.7(4) . . ? H51A C51 H51B 108.2 . . ? C51 C52 N8 115.5(14) . . ? C51 C52 H52A 108.4(8) . . ? N8 C52 H52A 108.4(10) . . ? C51 C52 H52B 108.4(9) . . ? N8 C52 H52B 108.4(9) . . ? H52A C52 H52B 107.5 . . ? C62 C61 S6 121.0(23) . . ? C62 C61 H61A 107.1(17) . . ? S6 C61 H61A 107.1(11) . . ? C62 C61 H61B 107.1(19) . . ? S6 C61 H61B 107.1(12) . . ? H61A C61 H61B 106.8 . . ? N8 C62 C61 116.9(24) . . ? N8 C62 H62A 108.1(15) . . ? C61 C62 H62A 108.1(19) . . ? N8 C62 H62B 108.1(12) . . ? C61 C62 H62B 108.1(18) . . ? H62A C62 H62B 107.3 . . ? C72A C71A S7 117.1(50) . . ? C72A C71A H71A 108.0(39) . . ? S7 C71A H71A 108.0(18) . . ? C72A C71A H71B 108.0(32) . . ? S7 C71A H71B 108.0(16) . . ? H71A C71A H71B 107.3 . . ? C71A C72A N8 113.6(50) . . ? C71A C72A H72A 108.9(32) . . ? N8 C72A H72A 108.8(18) . . ? C71A C72A H72B 108.9(40) . . ? N8 C72A H72B 108.8(19) . . ? H72A C72A H72B 107.7 . . ? C72B C71B S7 100.0(39) . . ? C72B C71B H71C 111.8(25) . . ? S7 C71B H71C 111.8(18) . . ? C72B C71B H71D 111.8(30) . . ? S7 C71B H71D 111.8(18) . . ? H71C C71B H71D 109.5 . . ? N8 C72B C71B 106.5(42) . . ? N8 C72B H72C 110.4(20) . . ? C71B C72B H72C 110.4(25) . . ? N8 C72B H72D 110.4(22) . . ? C71B C72B H72D 110.4(30) . . ? H72C C72B H72D 108.6 . . ? C62 N8 C52 115.6(19) . . ? C62 N8 C72A 102.2(25) . . ? C52 N8 C72A 111.4(21) . . ? C62 N8 C72B 131.3(28) . . ? C52 N8 C72B 107.4(23) . . ? _refine_diff_density_max 1.563 _refine_diff_density_min -1.738 _refine_diff_density_rms 0.207 #===end