#------------------------------------------------------------------------------ #$Date: 2016-03-21 05:35:49 +0200 (Mon, 21 Mar 2016) $ #$Revision: 178486 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/03/07/4030722.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_4030722 loop_ _publ_author_name 'Xiqu Wang' _publ_section_title ; Synthesis and crystal structure of a new microporous thioantimonate(III) [H3N(CH2)3NH3]Sb10S16 ; _journal_name_full 'European Journal of Solid State and Inorganic Chemistry' _journal_page_first 303 _journal_page_last 312 _journal_volume 32 _journal_year 1995 _chemical_formula_sum 'C3 H12 N2 S16 Sb10' _chemical_formula_weight 1806.78 _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _cell_angle_alpha 90 _cell_angle_beta 111.44(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 18.359(4) _cell_length_b 10.927(2) _cell_length_c 17.389(3) _cell_volume 3247.0(12) _diffrn_ambient_temperature 293 _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 9.213 _exptl_crystal_density_diffrn 3.696 _refine_ls_number_parameters 256 _refine_ls_number_reflns 3210 _refine_ls_R_factor_gt 0.071 _refine_ls_wR_factor_gt 0.162 _cod_data_source_file EJSSIC-1995-32-303-312.cif _cod_data_source_block Sb10S16 _cod_original_cell_volume 3247(1) _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 4030722 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 1/2-x,1/2+y,1/2-z 3 -x,-y,-z 4 1/2+x,1/2-y,1/2+z 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 Sb1 0.0190(10) 0.0100(10) 0.0220(10) 0.0020(10) 0.0040(10) 0.0010(10) SbS 0.0170(10) 0.0120(10) 0.0230(10) 0.0000(10) 0.0050(10) 0.0020(10) Sb2 0.0160(10) 0.0080(10) 0.0230(10) 0.0010(10) 0.0040(10) 0.0000(10) Sb3 0.0210(10) 0.0090(10) 0.0220(10) 0.0020(10) 0.0040(10) 0.0010(10) Sb4 0.0190(10) 0.0130(10) 0.0190(10) 0.0020(10) 0.0050(10) -0.0010(10) Sb6 0.0190(10) 0.0090(10) 0.0190(10) 0.0010(10) 0.0060(10) 0.0010(10) Sb7 0.0160(10) 0.0120(10) 0.0220(10) -0.0010(10) 0.0010(10) 0.0000(10) Sb8 0.0200(10) 0.0120(10) 0.0220(10) -0.0010(10) 0.0060(10) 0.0000(10) Sb9 0.0260(10) 0.0200(10) 0.0260(10) 0.0010(10) 0.0100(10) 0.0000(10) Sb10 0.0290(10) 0.0170(10) 0.0270(10) -0.0010(10) 0.0120(10) -0.0020(10) S1 0.027(5) 0.013(4) 0.021(4) -0.002(4) 0.006(4) -0.004(4) S2 0.020(4) 0.008(4) 0.030(5) 0.006(4) 0.006(4) 0.002(3) S3 0.021(4) 0.009(3) 0.021(4) -0.004(4) 0.007(3) -0.001(4) S4 0.021(4) 0.012(4) 0.015(4) -0.002(3) 0.005(3) -0.001(4) S5 0.022(4) 0.012(4) 0.041(5) 0.002(4) 0.008(4) -0.001(4) S6 0.012(4) 0.011(4) 0.021(4) -0.004(4) 0.000(3) 0.002(3) S7 0.010(4) 0.018(4) 0.025(4) 0.002(4) 0.002(3) 0.000(3) S8 0.010(4) 0.014(4) 0.035(5) -0.003(4) 0.007(4) 0.000(3) S9 0.011(4) 0.032(5) 0.013(4) 0.005(4) 0.006(3) -0.001(4) S10 0.020(4) 0.020(4) 0.012(4) -0.001(3) 0.002(3) 0.002(3) S11 0.022(5) 0.019(4) 0.028(5) 0.003(4) 0.012(4) -0.003(4) S12 0.039(5) 0.014(4) 0.030(5) 0.000(4) 0.019(4) 0.002(4) S13 0.030(5) 0.019(4) 0.025(4) 0.004(4) 0.008(4) 0.000(4) S14 0.034(5) 0.037(5) 0.023(4) -0.011(4) 0.012(4) -0.008(5) S15 0.024(5) 0.032(5) 0.023(5) 0.006(4) 0.009(4) -0.002(4) S16 0.020(4) 0.023(4) 0.018(4) 0.000(4) 0.003(4) -0.001(3) loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv Sb1 Sb Uani 0.10900(10) 0.8761(2) 0.08640(10) 1.000 0.0180(6) SbS Sb Uani 0.23080(10) 0.1313(2) 0.02530(10) 1.000 0.0180(6) Sb2 Sb Uani 0.05140(10) 0.3630(2) 0.95440(10) 1.000 0.0166(6) Sb3 Sb Uani 0.19970(10) 0.3776(2) 0.19950(10) 1.000 0.0184(6) Sb4 Sb Uani 0.19720(10) 0.1552(2) 0.36820(10) 1.000 0.0176(6) Sb6 Sb Uani 0.11320(10) 0.6454(2) 0.25310(10) 1.000 0.0159(6) Sb7 Sb Uani 0.03780(10) 0.1466(2) 0.15850(10) 1.000 0.0183(6) Sb8 Sb Uani 0.15080(10) 0.6493(2) 0.91430(10) 1.000 0.0185(6) Sb9 Sb Uani 0.04400(10) 0.5553(2) 0.6881(2) 1.000 0.0239(6) Sb10 Sb Uani 0.12280(10) 0.4819(2) 0.53450(10) 1.000 0.0238(6) S1 S Uani 0.1222(5) 0.6579(8) 0.0800(5) 1.000 0.021(3) S2 S Uani 0.0400(5) 0.1410(7) 0.9704(5) 1.000 0.020(3) S3 S Uani 0.2103(5) 0.1583(7) 0.1964(5) 1.000 0.017(2) S4 S Uani 0.2105(5) 0.3763(7) 0.3490(5) 1.000 0.016(2) S5 S Uani 0.2002(5) 0.3496(8) 0.0032(6) 1.000 0.026(3) S6 S Uani 0.1238(4) 0.8674(7) 0.2390(5) 1.000 0.016(2) S7 S Uani 0.0498(5) 0.3661(8) 0.1386(5) 1.000 0.019(2) S8 S Uani 0.1086(5) 0.8617(7) 0.9034(5) 1.000 0.020(3) S9 S Uani 0.0358(5) 0.3412(8) 0.8043(5) 1.000 0.018(3) S10 S Uani 0.1272(5) 0.6776(8) 0.4018(5) 1.000 0.018(2) S11 S Uani 0.0489(5) 0.1693(8) 0.3073(5) 1.000 0.022(3) S12 S Uani 0.1128(6) 0.3776(8) 0.6573(5) 1.000 0.026(3) S13 S Uani 0.0454(5) 0.6513(8) 0.5591(5) 1.000 0.025(3) S14 S Uani 0.1680(6) 0.6482(9) 0.7784(5) 1.000 0.031(3) S15 S Uani 0.2484(5) 0.5904(8) 0.6066(5) 1.000 0.026(3) S16 S Uani 0.2903(5) 0.7018(8) 0.9848(5) 1.000 0.021(2) N1 N Uiso 0.485(2) 0.611(4) 0.827(2) 1.000 0.067(12) N2 N Uiso 0.268(2) 0.365(4) 0.834(2) 1.000 0.055(10) C1 C Uiso 0.447(3) 0.559(5) 0.882(3) 1.000 0.057(13) C2 C Uiso 0.378(3) 0.499(4) 0.823(3) 1.000 0.054(12) C3 C Uiso 0.340(3) 0.429(4) 0.881(3) 1.000 0.054(12) 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' 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' Sb Sb -0.5866 1.5461 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 S1 Sb1 S6 92.1(3) . . yes S1 Sb1 S2 91.2(3) . 3_566 yes S2 Sb1 S6 95.2(3) 3_566 . yes S5 SbS S10 91.1(3) . 2_545 yes S5 SbS S15 97.7(3) . 2_545 yes S10 SbS S15 91.2(3) 2_545 2_545 yes S2 Sb2 S9 92.4(3) . . yes S2 Sb2 S5 91.8(3) . 1_556 yes S5 Sb2 S9 92.4(3) 1_556 . yes S3 Sb3 S4 92.3(3) . . yes S3 Sb3 S7 91.5(3) . . yes S4 Sb3 S7 95.3(3) . . yes S4 Sb4 S11 91.6(3) . . yes S4 Sb4 S16 87.9(3) . 2_546 yes S11 Sb4 S16 95.5(3) . 2_546 yes S6 Sb6 S10 89.0(3) . . yes S6 Sb6 S9 91.0(3) . 3_566 yes S9 Sb6 S10 94.9(3) 3_566 . yes S7 Sb7 S11 94.1(3) . . yes S7 Sb7 S8 96.5(3) . 3_566 yes S8 Sb7 S11 96.6(3) 3_566 . yes S8 Sb8 S14 94.5(3) . . yes S8 Sb8 S16 93.4(3) . . yes S14 Sb8 S16 90.2(3) . . yes S12 Sb9 S13 87.8(3) . . yes S12 Sb9 S14 92.0(3) . . yes S13 Sb9 S14 95.1(3) . . yes S12 Sb10 S13 88.1(3) . . yes S12 Sb10 S15 97.6(3) . . yes S13 Sb10 S15 92.4(3) . . yes Sb1 S2 Sb2 98.7(3) 3_566 . yes Sb3 S4 Sb4 99.8(3) . . yes SbS S5 Sb2 105.3(3) . 1_554 yes Sb1 S6 Sb6 99.1(3) . . yes Sb3 S7 Sb7 97.4(3) . . yes Sb7 S8 Sb8 105.1(3) 3_566 . yes Sb2 S9 Sb6 95.7(3) . 3_566 yes SbS S10 Sb6 100.8(3) 2_555 . yes Sb4 S11 Sb7 95.4(3) . . yes Sb9 S12 Sb10 91.7(3) . . yes Sb9 S13 Sb10 92.1(3) . . yes Sb8 S14 Sb9 101.4(4) . . yes SbS S15 Sb10 92.7(3) 2_555 . yes Sb4 S16 Sb8 98.6(3) 2_556 . yes N1 C1 C2 102(4) . . yes C1 C2 C3 104(4) . . no N2 C3 C2 113(4) . . yes 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 Sb1 S1 2.403(9) . yes Sb1 S6 2.569(8) . yes Sb1 S2 2.553(10) 3_566 yes SbS S5 2.449(9) . yes SbS S10 2.499(10) 2_545 yes SbS S15 2.499(9) 2_545 yes Sb2 S2 2.459(8) . yes Sb2 S9 2.531(8) . yes Sb2 S5 2.551(10) 1_556 yes Sb3 S3 2.406(8) . yes Sb3 S4 2.534(8) . yes Sb3 S7 2.565(10) . yes Sb4 S4 2.463(8) . yes Sb4 S11 2.540(10) . yes Sb4 S16 2.533(8) 2_546 yes Sb6 S6 2.453(8) . yes Sb6 S10 2.528(8) . yes Sb6 S9 2.550(10) 3_566 yes Sb7 S7 2.445(9) . yes Sb7 S11 2.532(8) . yes Sb7 S8 2.505(10) 3_566 yes Sb8 S8 2.432(8) . yes Sb8 S14 2.496(9) . yes Sb8 S16 2.469(10) . yes Sb9 S12 2.479(10) . yes Sb9 S13 2.485(9) . yes Sb9 S14 2.463(10) . yes Sb10 S12 2.486(9) . yes Sb10 S13 2.464(9) . yes Sb10 S15 2.486(9) . yes N1 C1 1.49(7) . yes N2 C3 1.45(7) . yes C1 C2 1.46(7) . no C2 C3 1.61(7) . no 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_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag S1 Sb1 S6 Sb6 -10.8(3) . . . no S2 Sb1 S6 Sb6 80.6(3) 3_566 . . no S1 Sb1 S2 Sb2 13.1(3) . 3_566 3_566 no S6 Sb1 S2 Sb2 -79.1(3) . 3_566 3_566 no S10 SbS S5 Sb2 -168.2(3) 2_545 . 1_554 no S15 SbS S5 Sb2 100.5(4) 2_545 . 1_554 no S5 SbS S10 Sb6 103.2(3) . 2_545 2_545 no S5 SbS S15 Sb10 131.4(3) . 2_545 2_545 no S9 Sb2 S2 Sb1 -83.4(3) . . 3_566 no S5 Sb2 S2 Sb1 -175.9(3) 1_556 . 3_566 no S2 Sb2 S9 Sb6 88.5(3) . . 3_566 no S5 Sb2 S9 Sb6 -179.7(3) 1_556 . 3_566 no S2 Sb2 S5 SbS 2.9(4) . 1_556 1_556 no S9 Sb2 S5 SbS -89.5(4) . 1_556 1_556 no S3 Sb3 S4 Sb4 -10.6(4) . . . no S7 Sb3 S4 Sb4 81.1(3) . . . no S3 Sb3 S7 Sb7 13.3(3) . . . no S4 Sb3 S7 Sb7 -79.2(3) . . . no S11 Sb4 S4 Sb3 -84.0(3) . . . no S16 Sb4 S4 Sb3 -179.5(3) 2_546 . . no S4 Sb4 S11 Sb7 86.0(3) . . . no S16 Sb4 S11 Sb7 174.0(3) 2_546 . . no S4 Sb4 S16 Sb8 -99.6(3) . 2_546 2_546 no S11 Sb4 S16 Sb8 169.0(3) . 2_546 2_546 no S10 Sb6 S6 Sb1 -179.0(3) . . . no S9 Sb6 S6 Sb1 -84.1(3) 3_566 . . no S6 Sb6 S10 SbS -98.7(3) . . 2_555 no S9 Sb6 S10 SbS 170.4(3) 3_566 . 2_555 no S6 Sb6 S9 Sb2 88.4(3) . 3_566 3_566 no S10 Sb6 S9 Sb2 177.4(3) . 3_566 3_566 no S11 Sb7 S7 Sb3 83.7(3) . . . no S8 Sb7 S7 Sb3 -179.2(3) 3_566 . . no S7 Sb7 S11 Sb4 -88.5(3) . . . no S8 Sb7 S11 Sb4 174.5(3) 3_566 . . no S7 Sb7 S8 Sb8 -13.2(3) . 3_566 3_566 no S11 Sb7 S8 Sb8 81.6(3) . 3_566 3_566 no S14 Sb8 S8 Sb7 93.6(4) . . 3_566 no S16 Sb8 S8 Sb7 -175.9(3) . . 3_566 no S8 Sb8 S14 Sb9 -97.9(4) . . . no S16 Sb8 S14 Sb9 168.6(4) . . . no S8 Sb8 S16 Sb4 99.9(3) . . 2_556 no S14 Sb8 S16 Sb4 -165.6(3) . . 2_556 no S13 Sb9 S12 Sb10 4.1(3) . . . no S14 Sb9 S12 Sb10 -90.9(3) . . . no S12 Sb9 S13 Sb10 -4.2(3) . . . no S14 Sb9 S13 Sb10 87.7(3) . . . no S12 Sb9 S14 Sb8 -117.5(4) . . . no S13 Sb9 S14 Sb8 154.6(3) . . . no S13 Sb10 S12 Sb9 -4.2(3) . . . no S15 Sb10 S12 Sb9 88.0(3) . . . no S12 Sb10 S13 Sb9 4.1(3) . . . no S15 Sb10 S13 Sb9 -93.4(3) . . . no S12 Sb10 S15 SbS 163.2(3) . . 2_555 no S13 Sb10 S15 SbS -108.4(3) . . 2_555 no N1 C1 C2 C3 174(4) . . . no C1 C2 C3 N2 178(4) . . . no