#------------------------------------------------------------------------------ #$Date: 2019-10-09 10:50:07 +0300 (Wed, 09 Oct 2019) $ #$Revision: 219196 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/23/44/7234495.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_7234495 loop_ _publ_author_name 'Takaaki Hiramatsu' 'Yukihiro Yoshida' 'Gunzi Saito' 'Akihiro Otsuka' 'Hideki Yamochi' 'Yasuhiro Shimizu' 'Yuma Hattori' 'Yuto Nakamura' 'Hideo Kishida' 'Hiroshi Ito' 'Kaplan Kirakci' 'Stephane Cordier' 'Christiane Perrin' _publ_section_title ; Spin frustration in antiperovskite systems: (TTF.+ or TSF.+)3[(Mo6X14)2-Y-] ; _journal_name_full 'Journal of Materials Chemistry C' _journal_page_first 11046 _journal_page_last 11054 _journal_paper_doi 10.1039/C5TC02075A _journal_volume 3 _journal_year 2015 _chemical_formula_moiety '(C6 Se4 H4 +)3, Mo6 Cl14 2-, Cl -' _chemical_formula_sum 'C18 H12 Cl15 Mo6 Se12' _chemical_formula_weight 2283.19 _chemical_name_common ; (TSF)3[(Mo6Cl14)Cl] ; _space_group_IT_number 148 _space_group_name_Hall '-P 3*' _space_group_name_H-M_alt 'R -3 :R' _symmetry_cell_setting rhombohedral _symmetry_Int_Tables_number 148 _symmetry_space_group_name_Hall '-P 3*' _symmetry_space_group_name_H-M 'R -3 :R' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 102.6318(2) _cell_angle_beta 102.6318(2) _cell_angle_gamma 102.6318(2) _cell_formula_units_Z 1 _cell_length_a 10.8505(5) _cell_length_b 10.8505(5) _cell_length_c 10.8505(5) _cell_measurement_reflns_used 5073 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 28.10 _cell_measurement_theta_min 2.40 _cell_volume 1167.76(9) _computing_cell_refinement 'APEX2 (Bruker AXS, 2006)' _computing_data_collection 'APEX2 ' _computing_data_reduction 'SAINT (Bruker AXS, 2004)' _computing_publication_material 'Yadokari-XG 2009 (Wakita, Nemoto et al., 2009)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 100(2) _diffrn_detector_area_resol_mean 8.333 _diffrn_measured_fraction_theta_full 0.982 _diffrn_measured_fraction_theta_max 0.982 _diffrn_measurement_device_type 'Bruker APEXII CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0143 _diffrn_reflns_av_sigmaI/netI 0.0122 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 6491 _diffrn_reflns_theta_full 27.50 _diffrn_reflns_theta_max 27.50 _diffrn_reflns_theta_min 2.00 _exptl_absorpt_coefficient_mu 11.792 _exptl_absorpt_correction_T_max 0.4677 _exptl_absorpt_correction_T_min 0.3354 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; APEX2 Software ; _exptl_crystal_colour black _exptl_crystal_density_diffrn 3.247 _exptl_crystal_density_method 'not measured' _exptl_crystal_description rhombohedral _exptl_crystal_F_000 1035 _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.08 _refine_diff_density_max 0.563 _refine_diff_density_min -0.419 _refine_diff_density_rms 0.073 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 78 _refine_ls_number_reflns 1762 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.086 _refine_ls_R_factor_all 0.0145 _refine_ls_R_factor_gt 0.0132 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0133P)^2^+0.9427P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0295 _refine_ls_wR_factor_ref 0.0299 _reflns_number_gt 1688 _reflns_number_total 1762 _reflns_threshold_expression >2sigma(I) _cod_data_source_file J-Mater-Chem-C-2015-3-11046.cif _cod_data_source_block TSF3_Mo6Cl14_Cl_100K _cod_depositor_comments ; The following automatic conversions were performed: data item '_symmetry_cell_setting' value 'Rhombohedral' was changed to 'rhombohedral' in accordance with the built-in table derived from the CIF Core dictionary named 'cif_core.dic' version 2.4.5 last updated on 2014-11-21. Automatic conversion script Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas ; _cod_original_sg_symbol_H-M 'R-3 ' _cod_database_code 7234495 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'z, x, y' 'y, z, x' '-x, -y, -z' '-z, -x, -y' '-y, -z, -x' 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 C1 C 0.51494(18) 0.45407(18) 0.03132(18) 0.0128(4) Uani 1 1 d . . . C2 C 0.5498(2) 0.3088(2) 0.2022(2) 0.0175(4) Uani 1 1 d . . . H2 H 0.5552 0.2747 0.2811 0.021 Uiso 1 1 calc R . . C3 C 0.5679(2) 0.2397(2) 0.0937(2) 0.0169(4) Uani 1 1 d . . . H3 H 0.5873 0.1533 0.0903 0.020 Uiso 1 1 calc R . . Se1 Se 0.51429(2) 0.470351(19) 0.206033(19) 0.01454(5) Uani 1 1 d . . . Se2 Se 0.55679(2) 0.305461(19) -0.052754(19) 0.01443(5) Uani 1 1 d . . . Cl1 Cl 0.90257(4) 0.23985(4) 0.07152(4) 0.01274(9) Uani 1 1 d . . . Cl2 Cl 1.21463(5) 0.21463(5) 0.21463(5) 0.01152(14) Uani 1 3 d S . . Cl3 Cl 0.96744(5) 0.17223(5) 0.38114(4) 0.01492(9) Uani 1 1 d . . . Mo1 Mo 0.986702(15) 0.075277(15) 0.164405(15) 0.00923(5) Uani 1 1 d . . . Cl4 Cl 0.5000 0.5000 0.5000 0.0139(2) Uani 1 6 d S . . 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 C1 0.0119(9) 0.0140(9) 0.0123(9) 0.0024(7) 0.0054(7) 0.0025(7) C2 0.0180(10) 0.0172(10) 0.0182(10) 0.0084(8) 0.0042(8) 0.0042(8) C3 0.0179(10) 0.0151(10) 0.0198(10) 0.0088(8) 0.0053(8) 0.0047(8) Se1 0.01767(10) 0.01593(10) 0.01182(10) 0.00448(7) 0.00582(7) 0.00601(7) Se2 0.01805(10) 0.01290(10) 0.01437(10) 0.00411(7) 0.00716(7) 0.00550(7) Cl1 0.0127(2) 0.0102(2) 0.0140(2) 0.00138(16) 0.00258(16) 0.00377(16) Cl2 0.01052(16) 0.01052(16) 0.01052(16) 0.00093(19) 0.00093(19) 0.00093(19) Cl3 0.0154(2) 0.0150(2) 0.0121(2) 0.00000(17) 0.00553(17) 0.00189(17) Mo1 0.00895(8) 0.00904(8) 0.00828(8) 0.00113(6) 0.00188(6) 0.00148(6) Cl4 0.0150(3) 0.0150(3) 0.0150(3) 0.0065(3) 0.0065(3) 0.0065(3) 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' Cl Cl 0.1484 0.1585 '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' 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 C1 C1 Se1 121.62(19) 4_665 . C1 C1 Se2 122.50(19) 4_665 . Se1 C1 Se2 115.88(10) . . C3 C2 Se1 119.43(16) . . C3 C2 H2 120.3 . . Se1 C2 H2 120.3 . . C2 C3 Se2 119.45(16) . . C2 C3 H3 120.3 . . Se2 C3 H3 120.3 . . C1 Se1 C2 92.61(9) . . C3 Se2 C1 92.51(9) . . Mo1 Cl1 Mo1 63.592(12) 5_665 3_654 Mo1 Cl1 Mo1 63.560(12) 5_665 . Mo1 Cl1 Mo1 63.534(13) 3_654 . Mo1 Cl2 Mo1 63.627(17) 3_654 . Mo1 Cl2 Mo1 63.627(17) 3_654 2_645 Mo1 Cl2 Mo1 63.628(17) . 2_645 Cl3 Mo1 Cl1 91.534(15) . 6_656 Cl3 Mo1 Cl2 92.809(15) . . Cl1 Mo1 Cl2 175.657(16) 6_656 . Cl3 Mo1 Cl1 91.871(16) . 2_645 Cl1 Mo1 Cl1 89.863(11) 6_656 2_645 Cl2 Mo1 Cl1 90.018(11) . 2_645 Cl3 Mo1 Cl1 92.592(16) . . Cl1 Mo1 Cl1 89.813(11) 6_656 . Cl2 Mo1 Cl1 89.967(11) . . Cl1 Mo1 Cl1 175.532(16) 2_645 . Cl3 Mo1 Mo1 134.819(13) . 5_665 Cl1 Mo1 Mo1 58.267(12) 6_656 5_665 Cl2 Mo1 Mo1 118.159(10) . 5_665 Cl1 Mo1 Mo1 118.148(12) 2_645 5_665 Cl1 Mo1 Mo1 58.116(10) . 5_665 Cl3 Mo1 Mo1 134.360(13) . 6_656 Cl1 Mo1 Mo1 58.323(12) 6_656 6_656 Cl2 Mo1 Mo1 118.159(10) . 6_656 Cl1 Mo1 Mo1 58.140(10) 2_645 6_656 Cl1 Mo1 Mo1 118.122(12) . 6_656 Mo1 Mo1 Mo1 60.022(8) 5_665 6_656 Cl3 Mo1 Mo1 135.639(13) . 3_654 Cl1 Mo1 Mo1 118.243(11) 6_656 3_654 Cl2 Mo1 Mo1 58.186(9) . 3_654 Cl1 Mo1 Mo1 118.255(12) 2_645 3_654 Cl1 Mo1 Mo1 58.192(12) . 3_654 Mo1 Mo1 Mo1 59.990(4) 5_665 3_654 Mo1 Mo1 Mo1 90.0 6_656 3_654 Cl3 Mo1 Mo1 135.174(13) . 2_645 Cl1 Mo1 Mo1 118.297(11) 6_656 2_645 Cl2 Mo1 Mo1 58.187(9) . 2_645 Cl1 Mo1 Mo1 58.274(12) 2_645 2_645 Cl1 Mo1 Mo1 118.173(12) . 2_645 Mo1 Mo1 Mo1 90.0 5_665 2_645 Mo1 Mo1 Mo1 59.989(4) 6_656 2_645 Mo1 Mo1 Mo1 60.0 3_654 2_645 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 C1 C1 1.379(4) 4_665 C1 Se1 1.8668(19) . C1 Se2 1.8699(19) . C2 C3 1.329(3) . C2 Se1 1.869(2) . C2 H2 1.0000 . C3 Se2 1.870(2) . C3 H3 1.0000 . Cl1 Mo1 2.4714(5) 5_665 Cl1 Mo1 2.4748(5) 3_654 Cl1 Mo1 2.4770(5) . Cl2 Mo1 2.4726(6) 3_654 Cl2 Mo1 2.4727(6) . Cl2 Mo1 2.4727(6) 2_645 Cl3 Mo1 2.4310(5) . Mo1 Cl1 2.4714(5) 6_656 Mo1 Cl1 2.4748(5) 2_645 Mo1 Mo1 2.6061(3) 5_665 Mo1 Mo1 2.6061(3) 6_656 Mo1 Mo1 2.6070(3) 3_654 Mo1 Mo1 2.6070(3) 2_645 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 Se1 C2 C3 Se2 -0.2(2) . . . . C1 C1 Se1 C2 176.0(2) 4_665 . . . Se2 C1 Se1 C2 -3.38(11) . . . . C3 C2 Se1 C1 2.20(18) . . . . C2 C3 Se2 C1 -1.87(18) . . . . C1 C1 Se2 C3 -176.1(2) 4_665 . . . Se1 C1 Se2 C3 3.29(11) . . . . Mo1 Cl2 Mo1 Cl3 -144.284(15) 3_654 . . . Mo1 Cl2 Mo1 Cl3 143.630(15) 2_645 . . . Mo1 Cl2 Mo1 Cl1 35.41(16) 3_654 . . 6_656 Mo1 Cl2 Mo1 Cl1 -36.68(16) 2_645 . . 6_656 Mo1 Cl2 Mo1 Cl1 123.841(12) 3_654 . . 2_645 Mo1 Cl2 Mo1 Cl1 51.755(13) 2_645 . . 2_645 Mo1 Cl2 Mo1 Cl1 -51.691(13) 3_654 . . . Mo1 Cl2 Mo1 Cl1 -123.777(12) 2_645 . . . Mo1 Cl2 Mo1 Mo1 1.480(8) 3_654 . . 5_665 Mo1 Cl2 Mo1 Mo1 -70.606(3) 2_645 . . 5_665 Mo1 Cl2 Mo1 Mo1 70.607(3) 3_654 . . 6_656 Mo1 Cl2 Mo1 Mo1 -1.479(8) 2_645 . . 6_656 Mo1 Cl2 Mo1 Mo1 -72.086(8) 2_645 . . 3_654 Mo1 Cl2 Mo1 Mo1 72.086(8) 3_654 . . 2_645 Mo1 Cl1 Mo1 Cl3 -143.400(14) 5_665 . . . Mo1 Cl1 Mo1 Cl3 144.496(12) 3_654 . . . Mo1 Cl1 Mo1 Cl1 -51.873(16) 5_665 . . 6_656 Mo1 Cl1 Mo1 Cl1 -123.977(15) 3_654 . . 6_656 Mo1 Cl1 Mo1 Cl2 123.789(13) 5_665 . . . Mo1 Cl1 Mo1 Cl2 51.686(13) 3_654 . . . Mo1 Cl1 Mo1 Cl1 34.0(2) 5_665 . . 2_645 Mo1 Cl1 Mo1 Cl1 -38.1(2) 3_654 . . 2_645 Mo1 Cl1 Mo1 Mo1 -72.104(9) 3_654 . . 5_665 Mo1 Cl1 Mo1 Mo1 1.460(14) 5_665 . . 6_656 Mo1 Cl1 Mo1 Mo1 -70.644(12) 3_654 . . 6_656 Mo1 Cl1 Mo1 Mo1 72.104(9) 5_665 . . 3_654 Mo1 Cl1 Mo1 Mo1 70.539(10) 5_665 . . 2_645 Mo1 Cl1 Mo1 Mo1 -1.565(12) 3_654 . . 2_645