Data_C8N6H26MnHg3Sb4S10 #=================================================== # SUBMISSION DETAILS _publ_contact_author_name ; Xiao-Wu Lei ; _publ_contact_author_address ; Key Laboratory of Inorganic Chemistry in Universities of Shandong, Department of Chemistry and Chemical Engineering, Jining University, Qufu, Shandong, 273155, China ; _publ_contact_author_email xwlei_jnu@163.com #================================================ _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H26 Hg3 Mn N6 S10 Sb4' _chemical_formula_weight 1670.66 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' 'Mn' 'Mn' 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Sb' 'Sb' -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Hg' 'Hg' -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.7218(18) _cell_length_b 9.9484(15) _cell_length_c 14.020(2) _cell_angle_alpha 90.00 _cell_angle_beta 109.557(2) _cell_angle_gamma 90.00 _cell_volume 1540.6(4) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.602 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1490 _exptl_absorpt_coefficient_mu 19.428 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2468 _exptl_absorpt_correction_T_max 0.3433 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'Bruker SMART CCD area detector' _diffrn_measurement_method omega-scan _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 17426 _diffrn_reflns_av_R_equivalents 0.0312 _diffrn_reflns_av_sigmaI/netI 0.0233 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.84 _diffrn_reflns_theta_max 27.66 _reflns_number_total 3560 _reflns_number_gt 3290 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 Software Suite (Bruker,2005)' _computing_cell_refinement 'APEX2 Software Suite (Bruker,2005)' _computing_data_reduction 'APEX2 Software Suite (Bruker,2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0416P)^2^+1.6060P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00080(7) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3560 _refine_ls_number_parameters 149 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0253 _refine_ls_R_factor_gt 0.0220 _refine_ls_wR_factor_ref 0.0650 _refine_ls_wR_factor_gt 0.0633 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _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 Mn1 Mn 0.0000 -0.5000 0.0000 0.0143(2) Uani 1 2 d S . . Hg1 Hg 0.5000 0.5000 0.0000 0.02476(9) Uani 1 2 d S . . Hg2 Hg 0.60561(2) 0.20693(2) 0.166127(16) 0.02827(8) Uani 1 1 d . . . Sb1 Sb 0.42827(3) 0.15088(3) -0.12025(2) 0.01901(9) Uani 1 1 d . . . Sb2 Sb 0.32206(3) 0.05392(3) 0.19211(2) 0.02136(9) Uani 1 1 d . . . S1 S 0.40292(11) 0.29580(11) 0.01798(9) 0.0195(2) Uani 1 1 d . . . S2 S 0.53287(11) 0.08024(13) 0.29030(10) 0.0233(3) Uani 1 1 d . . . S3 S 0.73238(11) 0.41173(13) 0.18884(10) 0.0244(3) Uani 1 1 d . . . S4 S 0.68692(14) 0.02625(13) 0.07974(12) 0.0309(3) Uani 1 1 d . . . S5 S 0.24812(11) 0.23551(14) -0.25799(10) 0.0254(3) Uani 1 1 d . . . N1 N -0.0263(4) -0.2877(5) 0.0013(4) 0.0318(11) Uani 1 1 d . . . H1C H -0.0930 -0.2659 -0.0522 0.038 Uiso 1 1 calc R . . N2 N 0.1870(4) -0.4381(5) 0.0331(4) 0.0302(10) Uani 1 1 d . . . H2C H 0.2340 -0.4789 0.0900 0.036 Uiso 1 1 calc R . . H2D H 0.2128 -0.4630 -0.0179 0.036 Uiso 1 1 calc R . . N3 N 0.0146(4) -0.4767(5) 0.1592(3) 0.0320(11) Uani 1 1 d . . . H3C H -0.0502 -0.5142 0.1695 0.038 Uiso 1 1 calc R . . H3D H 0.0814 -0.5191 0.1990 0.038 Uiso 1 1 calc R . . C1 C 0.0806(6) -0.2217(6) -0.0128(5) 0.0432(16) Uani 1 1 d . . . H1A H 0.0845 -0.1289 0.0093 0.052 Uiso 1 1 calc R . . H1B H 0.0714 -0.2218 -0.0842 0.052 Uiso 1 1 calc R . . C2 C -0.0488(6) -0.2504(7) 0.0952(6) 0.0484(17) Uani 1 1 d . . . H2A H -0.1346 -0.2592 0.0843 0.058 Uiso 1 1 calc R . . H2B H -0.0270 -0.1568 0.1102 0.058 Uiso 1 1 calc R . . C3 C 0.1973(5) -0.2925(6) 0.0461(5) 0.0362(14) Uani 1 1 d . . . H3A H 0.2620 -0.2600 0.0235 0.043 Uiso 1 1 calc R . . H3B H 0.2182 -0.2709 0.1174 0.043 Uiso 1 1 calc R . . C4 C 0.0210(6) -0.3350(7) 0.1857(5) 0.0416(15) Uani 1 1 d . . . H4A H 0.1050 -0.3066 0.2100 0.050 Uiso 1 1 calc R . . H4B H -0.0121 -0.3215 0.2398 0.050 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 Mn1 0.0117(4) 0.0181(5) 0.0124(4) -0.0026(4) 0.0029(4) -0.0026(4) Hg1 0.03133(16) 0.01553(14) 0.02809(16) -0.00013(10) 0.01083(12) -0.00150(10) Hg2 0.03585(14) 0.02129(12) 0.02879(13) 0.00149(8) 0.01230(10) -0.00216(8) Sb1 0.02366(17) 0.01500(17) 0.01926(17) -0.00055(11) 0.00838(13) -0.00136(12) Sb2 0.02460(18) 0.02291(18) 0.01533(16) -0.00267(12) 0.00503(13) -0.00095(13) S1 0.0243(6) 0.0168(6) 0.0167(6) -0.0006(4) 0.0059(5) -0.0005(4) S2 0.0211(6) 0.0281(6) 0.0220(6) 0.0047(5) 0.0090(5) 0.0023(5) S3 0.0244(6) 0.0214(6) 0.0305(7) -0.0010(5) 0.0134(5) 0.0001(5) S4 0.0449(8) 0.0183(6) 0.0411(8) -0.0017(6) 0.0299(7) -0.0057(6) S5 0.0230(6) 0.0257(6) 0.0231(6) -0.0012(5) 0.0017(5) -0.0076(5) N1 0.027(2) 0.030(3) 0.030(2) 0.001(2) -0.002(2) 0.0037(19) N2 0.018(2) 0.041(3) 0.030(2) -0.004(2) 0.0064(19) -0.0027(19) N3 0.027(2) 0.050(3) 0.019(2) 0.001(2) 0.0075(19) -0.004(2) C1 0.052(4) 0.033(3) 0.040(4) 0.009(3) 0.009(3) -0.008(3) C2 0.044(4) 0.046(4) 0.051(4) -0.015(3) 0.011(3) 0.013(3) C3 0.030(3) 0.038(3) 0.038(3) 0.000(3) 0.009(3) -0.015(2) C4 0.036(3) 0.057(4) 0.030(3) -0.016(3) 0.010(3) -0.007(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 Mn1 N1 2.135(5) 3_545 ? Mn1 N1 2.135(5) . ? Mn1 N2 2.172(4) 3_545 ? Mn1 N2 2.172(4) . ? Mn1 N3 2.194(5) . ? Mn1 N3 2.194(5) 3_545 ? Hg1 S1 2.3827(12) 3_665 ? Hg1 S1 2.3827(12) . ? Hg2 S3 2.4787(13) . ? Hg2 S2 2.5179(13) . ? Hg2 S4 2.5256(14) . ? Hg2 S1 2.7270(13) . ? Sb1 S4 2.4010(13) 3_655 ? Sb1 S5 2.4834(13) . ? Sb1 S1 2.5116(12) . ? Sb2 S2 2.4067(13) . ? Sb2 S3 2.4304(13) 2_645 ? Sb2 S5 2.4565(14) 4_566 ? S3 Sb2 2.4304(13) 2_655 ? S4 Sb1 2.4010(13) 3_655 ? S5 Sb2 2.4565(14) 4_565 ? N1 C2 1.474(8) . ? N1 C1 1.485(8) . ? N1 H1C 0.9100 . ? N2 C3 1.461(7) . ? N2 H2C 0.9000 . ? N2 H2D 0.9000 . ? N3 C4 1.453(8) . ? N3 H3C 0.9000 . ? N3 H3D 0.9000 . ? C1 C3 1.514(9) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C4 1.513(10) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? 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 N1 Mn1 N1 180.0 3_545 . ? N1 Mn1 N2 81.72(18) 3_545 3_545 ? N1 Mn1 N2 98.28(18) . 3_545 ? N1 Mn1 N2 98.28(18) 3_545 . ? N1 Mn1 N2 81.72(18) . . ? N2 Mn1 N2 180.0 3_545 . ? N1 Mn1 N3 98.69(19) 3_545 . ? N1 Mn1 N3 81.30(19) . . ? N2 Mn1 N3 88.67(18) 3_545 . ? N2 Mn1 N3 91.33(18) . . ? N1 Mn1 N3 81.30(19) 3_545 3_545 ? N1 Mn1 N3 98.70(19) . 3_545 ? N2 Mn1 N3 91.33(18) 3_545 3_545 ? N2 Mn1 N3 88.67(18) . 3_545 ? N3 Mn1 N3 180.0 . 3_545 ? S1 Hg1 S1 180.0 3_665 . ? S3 Hg2 S2 130.53(4) . . ? S3 Hg2 S4 109.90(4) . . ? S2 Hg2 S4 104.17(4) . . ? S3 Hg2 S1 99.40(4) . . ? S2 Hg2 S1 106.17(4) . . ? S4 Hg2 S1 103.77(5) . . ? S4 Sb1 S5 91.93(5) 3_655 . ? S4 Sb1 S1 91.01(4) 3_655 . ? S5 Sb1 S1 96.66(4) . . ? S2 Sb2 S3 97.23(4) . 2_645 ? S2 Sb2 S5 97.87(4) . 4_566 ? S3 Sb2 S5 95.85(5) 2_645 4_566 ? Hg1 S1 Sb1 102.93(5) . . ? Hg1 S1 Hg2 91.82(4) . . ? Sb1 S1 Hg2 95.95(4) . . ? Sb2 S2 Hg2 100.34(5) . . ? Sb2 S3 Hg2 106.42(5) 2_655 . ? Sb1 S4 Hg2 94.39(5) 3_655 . ? Sb2 S5 Sb1 102.79(5) 4_565 . ? C2 N1 C1 114.8(5) . . ? C2 N1 Mn1 109.0(4) . . ? C1 N1 Mn1 107.8(4) . . ? C2 N1 H1C 108.4 . . ? C1 N1 H1C 108.4 . . ? Mn1 N1 H1C 108.4 . . ? C3 N2 Mn1 110.1(3) . . ? C3 N2 H2C 109.6 . . ? Mn1 N2 H2C 109.6 . . ? C3 N2 H2D 109.6 . . ? Mn1 N2 H2D 109.6 . . ? H2C N2 H2D 108.2 . . ? C4 N3 Mn1 110.0(4) . . ? C4 N3 H3C 109.7 . . ? Mn1 N3 H3C 109.7 . . ? C4 N3 H3D 109.7 . . ? Mn1 N3 H3D 109.7 . . ? H3C N3 H3D 108.2 . . ? N1 C1 C3 111.7(5) . . ? N1 C1 H1A 109.3 . . ? C3 C1 H1A 109.3 . . ? N1 C1 H1B 109.3 . . ? C3 C1 H1B 109.3 . . ? H1A C1 H1B 107.9 . . ? N1 C2 C4 113.6(5) . . ? N1 C2 H2A 108.8 . . ? C4 C2 H2A 108.8 . . ? N1 C2 H2B 108.8 . . ? C4 C2 H2B 108.8 . . ? H2A C2 H2B 107.7 . . ? N2 C3 C1 111.8(5) . . ? N2 C3 H3A 109.3 . . ? C1 C3 H3A 109.3 . . ? N2 C3 H3B 109.3 . . ? C1 C3 H3B 109.3 . . ? H3A C3 H3B 107.9 . . ? N3 C4 C2 111.0(5) . . ? N3 C4 H4A 109.4 . . ? C2 C4 H4A 109.4 . . ? N3 C4 H4B 109.4 . . ? C2 C4 H4B 109.4 . . ? H4A C4 H4B 108.0 . . ? 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 S1 Hg1 S1 Sb1 28(4) 3_665 . . . ? S1 Hg1 S1 Hg2 125(4) 3_665 . . . ? S4 Sb1 S1 Hg1 -177.00(5) 3_655 . . . ? S5 Sb1 S1 Hg1 -84.94(5) . . . . ? S4 Sb1 S1 Hg2 89.75(5) 3_655 . . . ? S5 Sb1 S1 Hg2 -178.20(4) . . . . ? S3 Hg2 S1 Hg1 6.66(4) . . . . ? S2 Hg2 S1 Hg1 143.87(4) . . . . ? S4 Hg2 S1 Hg1 -106.65(4) . . . . ? S3 Hg2 S1 Sb1 109.86(4) . . . . ? S2 Hg2 S1 Sb1 -112.93(4) . . . . ? S4 Hg2 S1 Sb1 -3.45(5) . . . . ? S3 Sb2 S2 Hg2 174.27(4) 2_645 . . . ? S5 Sb2 S2 Hg2 -88.76(5) 4_566 . . . ? S3 Hg2 S2 Sb2 132.26(5) . . . . ? S4 Hg2 S2 Sb2 -95.08(5) . . . . ? S1 Hg2 S2 Sb2 14.12(5) . . . . ? S2 Hg2 S3 Sb2 -35.34(8) . . . 2_655 ? S4 Hg2 S3 Sb2 -166.03(5) . . . 2_655 ? S1 Hg2 S3 Sb2 85.52(5) . . . 2_655 ? S3 Hg2 S4 Sb1 165.41(5) . . . 3_655 ? S2 Hg2 S4 Sb1 21.88(6) . . . 3_655 ? S1 Hg2 S4 Sb1 -89.07(5) . . . 3_655 ? S4 Sb1 S5 Sb2 172.26(5) 3_655 . . 4_565 ? S1 Sb1 S5 Sb2 81.02(5) . . . 4_565 ? N1 Mn1 N1 C2 -76.1(4) 3_545 . . . ? N2 Mn1 N1 C2 74.2(4) 3_545 . . . ? N2 Mn1 N1 C2 -105.8(4) . . . . ? N3 Mn1 N1 C2 -13.1(4) . . . . ? N3 Mn1 N1 C2 166.9(4) 3_545 . . . ? N1 Mn1 N1 C1 49(100) 3_545 . . . ? N2 Mn1 N1 C1 -160.6(4) 3_545 . . . ? N2 Mn1 N1 C1 19.4(4) . . . . ? N3 Mn1 N1 C1 112.1(4) . . . . ? N3 Mn1 N1 C1 -67.9(4) 3_545 . . . ? N1 Mn1 N2 C3 -175.7(4) 3_545 . . . ? N1 Mn1 N2 C3 4.2(4) . . . . ? N2 Mn1 N2 C3 139.5(15) 3_545 . . . ? N3 Mn1 N2 C3 -76.8(4) . . . . ? N3 Mn1 N2 C3 103.2(4) 3_545 . . . ? N1 Mn1 N3 C4 170.0(4) 3_545 . . . ? N1 Mn1 N3 C4 -10.0(4) . . . . ? N2 Mn1 N3 C4 -108.6(4) 3_545 . . . ? N2 Mn1 N3 C4 71.4(4) . . . . ? N3 Mn1 N3 C4 -164(5) 3_545 . . . ? C2 N1 C1 C3 81.4(7) . . . . ? Mn1 N1 C1 C3 -40.3(6) . . . . ? C1 N1 C2 C4 -86.3(7) . . . . ? Mn1 N1 C2 C4 34.7(7) . . . . ? Mn1 N2 C3 C1 -27.3(6) . . . . ? N1 C1 C3 N2 46.2(7) . . . . ? Mn1 N3 C4 C2 31.0(6) . . . . ? N1 C2 C4 N3 -44.9(8) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1C S5 0.91 2.67 3.538(5) 158.8 2_544 N2 H2C S2 0.90 2.75 3.391(5) 129.2 2_645 N2 H2D S3 0.90 2.73 3.552(5) 152.6 3_655 N3 H3C S3 0.90 2.75 3.642(5) 170.3 1_445 N3 H3D S5 0.90 2.83 3.653(5) 152.0 4_556 _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.66 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.560 _refine_diff_density_min -1.284 _refine_diff_density_rms 0.161