Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2001 data_global # *** Added by check_cif _journal_coden_Cambridge 182 _publ_contact_author 'Prof Minghuey Shieh' _publ_contact_author_address ; Prof Minghuey Shieh Department of Chemistry National Taiwan Normal University Taipei 116 TAIWAN ; _publ_requested_journal Chemical Communication _publ_requested_coeditor_name ? _publ_contact_letter ; ? #Insert text if wanted ; #=================================================================== # 2. PROCESSING SUMMARY (IUCr Office Use Only) #=================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; ? #Insert chemical title here ; loop_ _publ_author_name 'Ho, Li-Fang' 'Jang, Li-Fing' 'Liu, Yi-Huang' 'Peng, Shie-ming' 'Shieh, Minghuey' 'Ueng, Chuen-Her' #=================================================================== # 4. TEXT _publ_section_abstract ; ? #Insert appropriate text here if wanted. ; _publ_section_comment ; ? #Insert appropriate text here if wanted. ; _publ_section_experimental ; ? #Insert appropriate text here if wanted. ; _publ_section_references ; Gabe, E.J., Le Page, Y., Charland,.J.-P., Lee, F.L. and White, P.S. (1989) J. Appl. Cryst., 22, 384-387. Flack, H., (1983) Acta Cryst., A39, 876-881. International Tables for X-ray Crystallography, Vol. IV, (1974) Kynoch Press, Birmingham, England. Johnson, C.K., (1976) ORTEP - A Fortran Thermal Ellipsoid Plot Program, Technical Report ORNL-5138, Oak Ridge National Lab., U.S.A. Larson, A.C., (1970) p.293, Crystallographic Computing, Munksgaard, Copenhagen. Le Page, Y., (1988) J. Appl. Cryst., 21, 983-984. Le Page, Y. and Gabe, E.J., (1979) J. Appl. Cryst., 12, 464-466. Rogers, D., (1981) Acta Cryst., A37, 734-741. ? #Insert any other references here ; _publ_section_figure_captions ; ? #Insert figure captions here if wanted ; _publ_section_acknowledgements ; ? #Insert any acknowledgements here. ; #=================================================================== data_Complex_1 _database_code_CSD 159098 #=================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ? #Insert the chemical name here. ; _chemical_name_common ? _chemical_formula_moiety 'C10 Cr3 N2 O10 Se2 . 2 C8 H20 N ' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C26 H40 Cr3 N2 O10 Se2 ' _chemical_formula_weight 854.51 _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 ? 0.003 0.002 'International Tables Vol. IV Table 2.2B' H ? 0.000 0.000 'International Tables Vol. IV Table 2.2B' Cr ? 0.321 0.624 'International Tables Vol. IV Table 2.2B' N ? 0.006 0.003 'International Tables Vol. IV Table 2.2B' O ? 0.011 0.006 'International Tables Vol. IV Table 2.2B' Se ? -0.093 2.226 'International Tables Vol. IV Table 2.2B' #=================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'C mcm' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z 1/2+x,1/2+y,z 1/2-x,1/2-y,-z -x,y,z x,-y,-z 1/2-x,1/2+y,z 1/2+x,1/2-y,-z x,-y,1/2+z -x,y,1/2-z 1/2+x,1/2-y,1/2+z 1/2-x,1/2+y,1/2-z -x,-y,1/2+z x,y,1/2-z 1/2-x,1/2-y,1/2+z 1/2+x,1/2+y,1/2-z _cell_length_a 8.607(3) _cell_length_b 24.591(8) _cell_length_c 15.941(4) _cell_angle_alpha 90.0 _cell_angle_beta 90.0 _cell_angle_gamma 90.0 _cell_volume 3374.0(18) _cell_formula_units_Z 4 _cell_measurement_temperature 293 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10.20 _cell_measurement_theta_max 14.10 _cell_special_details ; ? #Insert any comments here. ; _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.15 _exptl_crystal_size_rad ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.682 _exptl_crystal_density_method ? _exptl_crystal_F_000 1720 _exptl_absorpt_coefficient_mu 3.16 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4244 _exptl_absorpt_correction_T_max 0.4937 #=================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; ? #Insert any special details here. ; _diffrn_ambient_temperature 293 _diffrn_radiation_wavelength 0.70930 _diffrn_radiation_type 'Molybdenum K\a' _diffrn_radiation_source 'xray tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Nonius CAD-4 ' _diffrn_measurement_method 'Theta/2theta scan b/P/b ' _diffrn_standards_number 3 _diffrn_standards_interval_count 300 _diffrn_standards_interval_time 7200 _diffrn_standards_decay_% ? loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -5 3 0 0 -12 5 0 2 11 _diffrn_reflns_number 1656 _diffrn_reflns_av_R_equivalents 0.000 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 0.00 _diffrn_reflns_theta_max 24.94 _diffrn_reflns_reduction_process ? _reflns_number_total 1656 _reflns_number_observed 904 _reflns_observed_criterion 'Inet > 2.5\s(Inet)' _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction 'NRCVAX DATRD2' _computing_structure_solution 'NRCVAX SOLVER' _computing_structure_refinement 'NRCVAX LSTSQ' _computing_molecular_graphics 'NRCVAX' _computing_publication_material 'NRCVAX TABLES Jan 94 Version' #=================================================================== # 8. REFINEMENT DATA _refine_special_details ; ? #Insert any special details here. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 1/\s^2^(F) _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method ? _refine_ls_extinction_coef ? _refine_ls_number_reflns 903 _refine_ls_number_parameters 139 _refine_ls_number_restraints ? _refine_ls_number_constraints ? _refine_ls_R_factor_all 0.132 _refine_ls_R_factor_obs 0.059 _refine_ls_wR_factor_all 0.049 _refine_ls_wR_factor_obs 0.047 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 2.33 _refine_ls_restrained_S_all ? _refine_ls_restrained_S_obs ? _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_mean ? _refine_diff_density_max 0.76 _refine_diff_density_min -0.72 #=================================================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _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_calc_flag _atom_site_refinement_flags _atom_site_type_symbol Se 0.29225(22) 0.34900(7) 0.25000 0.0420(11) Uij ? S Se Cr1 0.50000 0.42434(15) 0.25000 0.0359(25) Uij ? S Cr Cr2 0.50000 0.32470(12) 0.15892(18) 0.0454(19) Uij ? S Cr O1 0.50000 0.4506(5) 0.0670(8) 0.074(11) Uij ? S O O2 0.2509(15) 0.5081(5) 0.25000 0.056(8) Uij ? S O O3 0.2661(12) 0.3320(4) 0.0199(5) 0.089(8) Uij ? . O O4 0.50000 0.2047(5) 0.1506(10) 0.096(13) Uij ? S O N1 0.50000 0.00000 0.00000 0.049(14) Uij ? S N N2 0.00000 0.1743(8) 0.25000 0.035(12) Uij ? S N C1 0.50000 0.4337(8) 0.1344(11) 0.053(13) Uij ? S C C2 0.3461(20) 0.4749(6) 0.25000 0.038(11) Uij ? S C C3 0.3563(15) 0.3287(6) 0.0763(8) 0.073(11) Uij ? . C C4 0.50000 0.2520(7) 0.1545(14) 0.063(15) Uij ? S C C5 0.621(3) 0.0362(9) 0.0597(15) 0.055(16) Uij ? . C C5' 0.590(3) 0.0335(9) -0.0612(15) 0.047(15) Uij ? . C C6 0.50000 0.0724(8) -0.1161(11) 0.069(16) Uij ? S C C7 0.50000 0.0766(8) 0.1116(11) 0.13(3) Uij ? S C C8 0.116(3) 0.1394(8) 0.2045(12) 0.049(14) Uij ? . C C8' 0.102(3) 0.2112(9) 0.2003(14) 0.056(16) Uij ? . C C9 0.00000 0.2503(8) 0.1425(12) 0.078(17) Uij ? S C C10 0.00000 0.0995(7) 0.1417(10) 0.121(24) Uij ? S C H5 0.693 0.060 0.016 0.0565 Uiso ? . H H5' 0.690 0.009 0.095 0.0565 Uiso ? . H Ha5 0.618 0.017 0.000 0.0485 Uiso ? . H Ha5' 0.650 0.052 -0.006 0.0485 Uiso ? . H H6 0.558 0.073 -0.179 0.0662 Uiso ? . H H6' 0.500 0.112 -0.089 0.0662 Uiso ? S H H7 0.453 0.076 0.177 0.0835 Uiso ? . H H7' 0.500 0.120 0.102 0.0835 Uiso ? S H H8 0.169 0.176 0.177 0.0606 Uiso ? . H H8' 0.198 0.119 0.248 0.0604 Uiso ? . H Ha8 0.174 0.236 0.238 0.0606 Uiso ? . H Ha8' 0.184 0.187 0.162 0.0606 Uiso ? . H H9 0.081 0.264 0.092 0.0666 Uiso ? . H H9' 0.000 0.214 0.095 0.0666 Uiso ? S H H10 0.021 0.112 0.076 0.0796 Uiso ? . H H10' 0.000 0.055 0.142 0.0796 Uiso ? S H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol Se 0.0370(11) 0.0392(10) 0.0498(10) -0.0024(11) 0.00000 0.00000 Se Cr1 0.043(3) 0.0336(24) 0.0311(23) 0.00000 0.00000 0.00000 Cr Cr2 0.0502(21) 0.0457(19) 0.0403(18) 0.00000 0.00000 -0.0071(16) Cr O1 0.120(14) 0.062(10) 0.042(9) 0.00000 0.00000 0.002(8) O O2 0.058(10) 0.064(9) 0.047(7) 0.014(8) 0.00000 0.00000 O O3 0.079(8) 0.122(9) 0.068(6) -0.005(8) -0.011(7) -0.007(7) O O4 0.120(14) 0.056(9) 0.112(14) 0.00000 0.00000 -0.018(11) O N1 0.039(14) 0.049(14) 0.059(16) 0.00000 0.00000 -0.009(13) N N2 0.033(12) 0.030(12) 0.042(13) 0.00000 0.00000 0.00000 N C1 0.060(14) 0.071(15) 0.029(11) 0.00000 0.00000 -0.002(11) C C2 0.050(13) 0.043(11) 0.021(9) 0.010(10) 0.00000 0.00000 C C3 0.043(9) 0.102(13) 0.073(11) -0.003(10) -0.005(9) -0.017(10) C C4 0.072(16) 0.028(11) 0.088(16) 0.00000 0.00000 0.001(13) C C5 0.053(18) 0.055(17) 0.058(18) -0.026(15) -0.029(16) 0.000(14) C C5' 0.037(17) 0.048(16) 0.057(18) -0.016(13) -0.004(14) 0.031(14) C C6 0.114(20) 0.069(15) 0.025(11) 0.00000 0.00000 0.012(11) C C7 0.32(4) 0.048(14) 0.023(12) 0.00000 0.00000 -0.026(11) C C8 0.036(15) 0.058(18) 0.053(15) 0.004(14) 0.015(13) -0.010(13) C C8' 0.058(19) 0.048(17) 0.061(19) -0.004(15) 0.015(15) -0.009(13) C C9 0.113(21) 0.074(16) 0.046(14) 0.00000 0.00000 0.033(13) C C10 0.31(4) 0.041(13) 0.013(10) 0.00000 0.00000 0.003(11) C #=================================================================== # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Se Cr1 2.575(3) ? ? ? Se Cr2 2.3797(24) ? ? ? Se Cr2a 2.3797(24) ? ? ? Cr1 Sea 2.575(3) ? ? ? Cr1 Cr2 2.848(4) ? ? ? Cr1 Cr2a 2.848(4) ? ? ? Cr1 C1 1.857(18) ? ? ? Cr1 C1a 1.857(18) ? ? ? Cr1 C2 1.816(17) ? ? ? Cr1 C2a 1.816(17) ? ? ? Cr2 Sea 2.3797(24) ? ? ? Cr2 Cr2a 2.904(6) ? ? ? Cr2 C3 1.809(13) ? ? ? Cr2 C3a 1.809(13) ? ? ? Cr2 C4 1.789(18) ? ? ? O1 C1 1.151(22) ? ? ? O2 C2 1.158(21) ? ? ? O3 C3 1.191(16) ? ? ? O4 C4 1.166(22) ? ? ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cr1 Se Cr2 70.06(9) ? ? ? ? Cr1 Se Cr2a 70.06(9) ? ? ? ? Cr2 Se Cr2a 75.20(10) ? ? ? ? Se Cr1 Sea 87.97(13) ? ? ? ? Se Cr1 Cr2 51.75(8) ? ? ? ? Se Cr1 Cr2a 51.75(8) ? ? ? ? Se Cr1 C1 95.1(4) ? ? ? ? Se Cr1 C1a 95.1(4) ? ? ? ? Se Cr1 C2 89.2(5) ? ? ? ? Se Cr1 C2a 177.2(5) ? ? ? ? Sea Cr1 Cr2 51.75(8) ? ? ? ? Sea Cr1 Cr2a 51.75(8) ? ? ? ? Sea Cr1 C1 95.1(4) ? ? ? ? Sea Cr1 C1a 95.1(4) ? ? ? ? Sea Cr1 C2 177.2(5) ? ? ? ? Sea Cr1 C2a 89.2(5) ? ? ? ? Cr2 Cr1 Cr2a 61.30(12) ? ? ? ? Cr2 Cr1 C1 66.5(6) ? ? ? ? Cr2 Cr1 C1a 127.8(6) ? ? ? ? Cr2 Cr1 C2 126.1(4) ? ? ? ? Cr2 Cr1 C2a 126.1(4) ? ? ? ? Cr2a Cr1 C1 127.8(6) ? ? ? ? Cr2a Cr1 C1a 66.5(6) ? ? ? ? Cr2a Cr1 C2 126.1(4) ? ? ? ? Cr2a Cr1 C2a 126.1(4) ? ? ? ? C1 Cr1 C1a 165.7(9) ? ? ? ? C1 Cr1 C2 85.1(4) ? ? ? ? C1 Cr1 C2a 85.1(4) ? ? ? ? C1a Cr1 C2 85.1(4) ? ? ? ? C1a Cr1 C2a 85.1(4) ? ? ? ? C2 Cr1 C2a 93.7(8) ? ? ? ? Se Cr2 Sea 97.43(11) ? ? ? ? Se Cr2 Cr1 58.19(7) ? ? ? ? Se Cr2 Cr2a 52.40(6) ? ? ? ? Se Cr2 C3 85.2(4) ? ? ? ? Se Cr2 C3a 160.8(5) ? ? ? ? Se Cr2 C4 105.9(4) ? ? ? ? Sea Cr2 Cr1 58.19(7) ? ? ? ? Sea Cr2 Cr2a 52.40(6) ? ? ? ? Sea Cr2 C3 160.8(5) ? ? ? ? Sea Cr2 C3a 85.2(4) ? ? ? ? Sea Cr2 C4 105.9(4) ? ? ? ? Cr1 Cr2 Cr2a 59.35(9) ? ? ? ? Cr1 Cr2 C3 108.9(5) ? ? ? ? Cr1 Cr2 C3a 108.9(5) ? ? ? ? Cr1 Cr2 C4 151.6(7) ? ? ? ? Cr2a Cr2 C3 136.7(4) ? ? ? ? Cr2a Cr2 C3a 136.7(4) ? ? ? ? Cr2a Cr2 C4 92.2(7) ? ? ? ? C3 Cr2 C3a 86.3(6) ? ? ? ? C3 Cr2 C4 91.5(7) ? ? ? ? C3a Cr2 C4 91.5(7) ? ? ? ? Cr1 C1 O1 166.1(16) ? ? ? ? Cr1 C2 O2 178.2(15) ? ? ? ? Cr2 C3 O3 177.4(12) ? ? ? ? Cr2 C4 O4 179.2(19) ? ? ? ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag ? ? ? ? ? ? ? ? ? ? #==========================END data_Complex_2 _database_code_CSD 159099 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C26 H40 Cr2 Mo N2 O10 Se2' _chemical_formula_weight 898.46 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cr' 'Cr' 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Se' 'Se' -0.0929 2.2259 '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 Pnna loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z' '-x+1/2, y+1/2, -z+1/2' 'x, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' 'x-1/2, -y-1/2, z-1/2' '-x, y-1/2, z-1/2' _cell_length_a 24.8153(3) _cell_length_b 16.0695(3) _cell_length_c 8.6204(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3437.55(11) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 7630 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.736 _exptl_crystal_density_method ? _exptl_crystal_F_000 1792 _exptl_absorpt_coefficient_mu 3.150 _exptl_absorpt_correction_type 'used sadabs' _exptl_absorpt_correction_T_min 0.569 _exptl_absorpt_correction_T_max 0.634 _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'Siemens SMART CCD' _diffrn_measurement_method '\w scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22975 _diffrn_reflns_av_R_equivalents 0.0406 _diffrn_reflns_av_sigmaI/netI 0.0269 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 27.50 _reflns_number_total 3957 _reflns_number_observed 2780 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SAINT' _computing_data_reduction 'Siemens SAINT' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 331 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^)+(0.0736P)^2^+10.4733P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00016(14) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3626 _refine_ls_number_parameters 197 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0774 _refine_ls_R_factor_obs 0.0495 _refine_ls_wR_factor_all 0.1697 _refine_ls_wR_factor_obs 0.1442 _refine_ls_goodness_of_fit_all 1.098 _refine_ls_goodness_of_fit_obs 1.167 _refine_ls_restrained_S_all 1.142 _refine_ls_restrained_S_obs 1.167 _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 Se1 Se 0.40169(2) 0.24451(3) 0.96075(6) 0.0346(2) Uani 1 d . . Mo1 Mo 0.32268(3) 0.2500 0.7500 0.0394(2) Uani 1 d S . Cr1 Cr 0.42571(3) 0.15841(5) 0.74119(9) 0.0303(2) Uani 1 d . . O1 O 0.2371(2) 0.2473(2) 0.4951(6) 0.0548(11) Uani 1 d . . O2 O 0.2983(2) 0.0594(3) 0.7537(6) 0.0669(14) Uani 1 d . . O3 O 0.4157(3) 0.0234(3) 0.4986(6) 0.075(2) Uani 1 d . . O4 O 0.4200(3) 0.0146(3) 0.9670(6) 0.075(2) Uani 1 d . . O5 O 0.5454(2) 0.1457(4) 0.7318(7) 0.086(2) Uani 1 d . . C1 C 0.2698(2) 0.2483(3) 0.5870(7) 0.0366(11) Uani 1 d . . C2 C 0.3135(2) 0.1259(4) 0.7516(7) 0.0441(13) Uani 1 d . . C3 C 0.4197(3) 0.0773(4) 0.5907(7) 0.0484(14) Uani 1 d . . C4 C 0.4224(3) 0.0713(4) 0.8813(7) 0.0483(14) Uani 1 d . . C5 C 0.4986(3) 0.1504(4) 0.7354(7) 0.052(2) Uani 1 d . . N1 N 0.5740(3) 0.2500 1.2500 0.0375(14) Uani 1 d S . C6 C 0.5387(2) 0.1923(4) 1.1546(7) 0.0477(14) Uani 1 d . . H6A H 0.5163(2) 0.2260(4) 1.0870(7) 0.057 Uiso 1 calc R . H6B H 0.5618(2) 0.1586(4) 1.0890(7) 0.057 Uiso 1 calc R . C7 C 0.5029(3) 0.1353(5) 1.2458(8) 0.063(2) Uani 1 d . . H7A H 0.4823(3) 0.1014(5) 1.1759(8) 0.095 Uiso 1 calc R . H7B H 0.4789(3) 0.1677(5) 1.3090(8) 0.095 Uiso 1 calc R . H7C H 0.5245(3) 0.1003(5) 1.3110(8) 0.095 Uiso 1 calc R . C8 C 0.6087(3) 0.2015(4) 1.3620(7) 0.0500(15) Uani 1 d . . H8A H 0.6298(3) 0.2407(4) 1.4223(7) 0.060 Uiso 1 calc R . H8B H 0.5853(3) 0.1721(4) 1.4334(7) 0.060 Uiso 1 calc R . C9 C 0.6468(3) 0.1392(4) 1.2901(9) 0.063(2) Uani 1 d . . H9A H 0.6670(3) 0.1118(4) 1.3704(9) 0.094 Uiso 1 calc R . H9B H 0.6712(3) 0.1675(4) 1.2215(9) 0.094 Uiso 1 calc R . H9C H 0.6266(3) 0.0987(4) 1.2326(9) 0.094 Uiso 1 calc R . N2 N 0.2500 0.0000 1.2332(7) 0.0351(14) Uani 1 d S . C10 C 0.2132(2) 0.0509(4) 1.1277(7) 0.0442(13) Uani 1 d . . H10A H 0.2354(2) 0.0870(4) 1.0641(7) 0.053 Uiso 1 calc R . H10B H 0.1944(2) 0.0131(4) 1.0587(7) 0.053 Uiso 1 calc R . C11 C 0.1718(3) 0.1038(5) 1.2100(9) 0.063(2) Uani 1 d . . H11A H 0.1507(3) 0.1334(5) 1.1348(9) 0.095 Uiso 1 calc R . H11B H 0.1898(3) 0.1429(5) 1.2765(9) 0.095 Uiso 1 calc R . H11C H 0.1487(3) 0.0689(5) 1.2710(9) 0.095 Uiso 1 calc R . C12 C 0.2828(3) 0.0570(4) 1.3374(7) 0.0481(15) Uani 1 d . . H12A H 0.2581(3) 0.0896(4) 1.4000(7) 0.058 Uiso 1 calc R . H12B H 0.3039(3) 0.0229(4) 1.4075(7) 0.058 Uiso 1 calc R . C13 C 0.3203(3) 0.1159(5) 1.2537(8) 0.067(2) Uani 1 d . . H13A H 0.3393(3) 0.1494(5) 1.3282(8) 0.100 Uiso 1 calc R . H13B H 0.2998(3) 0.1513(5) 1.1862(8) 0.100 Uiso 1 calc R . H13C H 0.3458(3) 0.0845(5) 1.1936(8) 0.100 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Se1 0.0311(3) 0.0389(3) 0.0340(3) -0.0015(2) -0.0014(2) 0.0010(2) Mo1 0.0321(3) 0.0393(4) 0.0468(4) -0.0001(3) 0.000 0.000 Cr1 0.0285(4) 0.0275(4) 0.0348(4) -0.0032(3) -0.0010(4) 0.0060(3) O1 0.047(2) 0.057(3) 0.060(3) 0.004(2) -0.010(2) -0.003(2) O2 0.050(3) 0.046(3) 0.105(4) 0.004(2) 0.005(3) -0.010(2) O3 0.106(4) 0.053(3) 0.066(3) -0.018(3) -0.004(3) -0.001(3) O4 0.112(5) 0.045(3) 0.069(3) 0.008(3) -0.010(3) 0.002(3) O5 0.037(3) 0.111(5) 0.110(5) -0.006(3) 0.002(3) 0.021(3) C1 0.036(3) 0.031(3) 0.043(3) 0.002(2) 0.004(2) 0.001(2) C2 0.035(3) 0.044(3) 0.054(3) 0.001(3) -0.002(3) 0.005(2) C3 0.053(4) 0.040(3) 0.052(4) -0.001(3) -0.001(3) 0.003(3) C4 0.054(4) 0.041(3) 0.050(4) -0.005(3) -0.005(3) 0.005(3) C5 0.049(4) 0.055(4) 0.050(4) -0.001(3) 0.001(3) 0.008(3) N1 0.032(3) 0.046(4) 0.034(3) -0.004(3) 0.000 0.000 C6 0.043(3) 0.054(4) 0.046(3) -0.014(3) -0.007(3) -0.001(3) C7 0.049(4) 0.061(4) 0.081(5) -0.011(4) -0.004(4) -0.016(3) C8 0.050(4) 0.052(4) 0.049(3) 0.007(3) -0.011(3) -0.007(3) C9 0.047(4) 0.051(4) 0.090(5) 0.001(4) -0.012(4) 0.004(3) N2 0.033(3) 0.036(3) 0.037(3) 0.000 0.000 -0.003(3) C10 0.042(3) 0.048(3) 0.043(3) 0.005(3) -0.005(3) 0.000(3) C11 0.048(4) 0.061(4) 0.080(5) 0.011(4) 0.001(4) 0.016(3) C12 0.054(4) 0.045(3) 0.045(3) -0.009(3) -0.013(3) -0.002(3) C13 0.055(4) 0.058(4) 0.086(6) 0.001(4) -0.016(4) -0.025(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Se1 Cr1 2.4123(9) 4_556 ? Se1 Cr1 2.4190(9) . ? Se1 Mo1 2.6745(7) . ? Mo1 C1 1.923(6) 4_556 ? Mo1 C1 1.923(6) . ? Mo1 C2 2.007(6) . ? Mo1 C2 2.007(6) 4_556 ? Mo1 Se1 2.6743(7) 4_556 ? Mo1 Cr1 2.9511(9) . ? Mo1 Cr1 2.9513(9) 4_556 ? Cr1 C5 1.815(7) . ? Cr1 C3 1.845(6) . ? Cr1 C4 1.850(6) . ? Cr1 Se1 2.4123(9) 4_556 ? Cr1 Cr1 2.947(2) 4_556 ? O1 C1 1.134(7) . ? O2 C2 1.134(8) . ? O3 C3 1.179(7) . ? O4 C4 1.175(8) . ? O5 C5 1.162(8) . ? N1 C8 1.511(7) . ? N1 C8 1.511(7) 4_557 ? N1 C6 1.517(6) . ? N1 C6 1.518(6) 4_557 ? C6 C7 1.500(9) . ? C8 C9 1.510(9) . ? N2 C12 1.519(6) . ? N2 C12 1.519(6) 2 ? N2 C10 1.527(6) . ? N2 C10 1.527(6) 2 ? C10 C11 1.509(9) . ? C12 C13 1.512(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cr1 Se1 Cr1 75.19(3) 4_556 . ? Cr1 Se1 Mo1 70.71(2) 4_556 . ? Cr1 Se1 Mo1 70.61(2) . . ? C1 Mo1 C1 93.9(3) 4_556 . ? C1 Mo1 C2 86.1(2) 4_556 . ? C1 Mo1 C2 85.0(2) . . ? C1 Mo1 C2 85.0(2) 4_556 4_556 ? C1 Mo1 C2 86.1(2) . 4_556 ? C2 Mo1 C2 167.0(3) . 4_556 ? C1 Mo1 Se1 175.1(2) 4_556 4_556 ? C1 Mo1 Se1 90.3(2) . 4_556 ? C2 Mo1 Se1 96.9(2) . 4_556 ? C2 Mo1 Se1 92.6(2) 4_556 4_556 ? C1 Mo1 Se1 90.3(2) 4_556 . ? C1 Mo1 Se1 175.1(2) . . ? C2 Mo1 Se1 92.6(2) . . ? C2 Mo1 Se1 96.9(2) 4_556 . ? Se1 Mo1 Se1 85.70(3) 4_556 . ? C1 Mo1 Cr1 128.1(2) 4_556 . ? C1 Mo1 Cr1 124.4(2) . . ? C2 Mo1 Cr1 66.6(2) . . ? C2 Mo1 Cr1 126.4(2) 4_556 . ? Se1 Mo1 Cr1 50.49(2) 4_556 . ? Se1 Mo1 Cr1 50.64(2) . . ? C1 Mo1 Cr1 124.4(2) 4_556 4_556 ? C1 Mo1 Cr1 128.1(2) . 4_556 ? C2 Mo1 Cr1 126.4(2) . 4_556 ? C2 Mo1 Cr1 66.6(2) 4_556 4_556 ? Se1 Mo1 Cr1 50.64(2) 4_556 4_556 ? Se1 Mo1 Cr1 50.49(2) . 4_556 ? Cr1 Mo1 Cr1 59.92(3) . 4_556 ? C5 Cr1 C3 90.7(3) . . ? C5 Cr1 C4 90.5(3) . . ? C3 Cr1 C4 85.5(3) . . ? C5 Cr1 Se1 105.8(2) . 4_556 ? C3 Cr1 Se1 86.0(2) . 4_556 ? C4 Cr1 Se1 161.6(2) . 4_556 ? C5 Cr1 Se1 107.9(2) . . ? C3 Cr1 Se1 159.1(2) . . ? C4 Cr1 Se1 84.9(2) . . ? Se1 Cr1 Se1 97.69(3) 4_556 . ? C5 Cr1 Cr1 94.1(2) . 4_556 ? C3 Cr1 Cr1 137.9(2) . 4_556 ? C4 Cr1 Cr1 136.2(2) . 4_556 ? Se1 Cr1 Cr1 52.51(3) 4_556 4_556 ? Se1 Cr1 Cr1 52.30(3) . 4_556 ? C5 Cr1 Mo1 154.1(2) . . ? C3 Cr1 Mo1 107.5(2) . . ? C4 Cr1 Mo1 108.8(2) . . ? Se1 Cr1 Mo1 58.80(2) 4_556 . ? Se1 Cr1 Mo1 58.74(2) . . ? Cr1 Cr1 Mo1 60.04(2) 4_556 . ? O1 C1 Mo1 177.4(5) . . ? O2 C2 Mo1 167.0(5) . . ? O3 C3 Cr1 177.7(6) . . ? O4 C4 Cr1 178.2(6) . . ? O5 C5 Cr1 179.7(5) . . ? C8 N1 C8 110.4(6) . 4_557 ? C8 N1 C6 111.1(3) . . ? C8 N1 C6 107.3(4) 4_557 . ? C8 N1 C6 107.3(4) . 4_557 ? C8 N1 C6 111.1(3) 4_557 4_557 ? C6 N1 C6 109.5(6) . 4_557 ? C7 C6 N1 115.5(5) . . ? C9 C8 N1 115.9(5) . . ? C12 N2 C12 107.5(6) . 2 ? C12 N2 C10 110.4(3) . . ? C12 N2 C10 110.8(3) 2 . ? C12 N2 C10 110.8(3) . 2 ? C12 N2 C10 110.4(3) 2 2 ? C10 N2 C10 106.9(6) . 2 ? C11 C10 N2 115.4(5) . . ? C13 C12 N2 115.2(5) . . ? _refine_diff_density_max 0.819 _refine_diff_density_min -2.142 _refine_diff_density_rms 0.123 #==========================END