#------------------------------------------------------------------------------ #$Date: 2019-10-09 10:50:07 +0300 (Wed, 09 Oct 2019) $ #$Revision: 219196 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/23/44/7234494.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_7234494 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 '-R 3' _space_group_name_H-M_alt 'R -3 :H' _symmetry_cell_setting rhombohedral _symmetry_Int_Tables_number 148 _symmetry_space_group_name_Hall '-R 3' _symmetry_space_group_name_H-M 'R -3 :H' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_formula_units_Z 3 _cell_length_a 16.9464(13) _cell_length_b 16.9464(13) _cell_length_c 14.0495(14) _cell_measurement_reflns_used 5847 _cell_measurement_temperature 25(2) _cell_measurement_theta_max 30.1912 _cell_measurement_theta_min 3.9493 _cell_volume 3494.2(5) _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2006)' _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2006)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2006)' _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 25(2) _diffrn_detector_area_resol_mean 14.7059 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device ; Mercury (2x2 bin mode) ; _diffrn_radiation_detector CCD _diffrn_radiation_monochromator Confocal _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71070 _diffrn_reflns_av_R_equivalents 0.0497 _diffrn_reflns_av_sigmaI/netI 0.0287 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 12352 _diffrn_reflns_theta_full 27.48 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_theta_min 3.95 _exptl_absorpt_coefficient_mu 11.823 _exptl_absorpt_correction_T_max 0.4853 _exptl_absorpt_correction_T_min 0.2585 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; Higashi, T. (2000). A numerical absorption correction program NUMABS Rigaku Corporation, Tokyo, Japan ; _exptl_crystal_colour black _exptl_crystal_density_diffrn 3.255 _exptl_crystal_density_method 'not measured' _exptl_crystal_description rhombohedral _exptl_crystal_F_000 3105 _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _refine_diff_density_max 0.811 _refine_diff_density_min -0.641 _refine_diff_density_rms 0.125 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 78 _refine_ls_number_reflns 1779 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.043 _refine_ls_R_factor_all 0.0168 _refine_ls_R_factor_gt 0.0151 _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^)+(0.0095P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0322 _refine_ls_wR_factor_ref 0.0325 _reflns_number_gt 1588 _reflns_number_total 1779 _reflns_threshold_expression >2sigma(I) _cod_data_source_file J-Mater-Chem-C-2015-3-11046.cif _cod_data_source_block TSF3_Mo6Cl14_Cl_25K _cod_depositor_comments ; The following automatic conversions were performed: data item '_exptl_absorpt_correction_type' value 'Numerical' was changed to 'numerical' 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. 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 7234494 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' 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 0.30196(15) 0.18153(15) 0.16686(15) 0.0071(5) Uani 1 1 d . . . C2 C 0.20668(15) 0.26745(15) 0.19962(16) 0.0086(5) Uani 1 1 d . . . H2 H 0.1866 0.3104 0.2229 0.010 Uiso 1 1 calc R . . C3 C 0.15089(15) 0.19570(15) 0.14654(16) 0.0091(5) Uani 1 1 d . . . H3 H 0.0885 0.1840 0.1303 0.011 Uiso 1 1 calc R . . Se1 Se 0.322704(15) 0.287263(15) 0.230230(16) 0.00665(6) Uani 1 1 d . . . Se2 Se 0.190676(15) 0.117197(15) 0.102880(16) 0.00666(6) Uani 1 1 d . . . Cl1 Cl 0.16908(4) 0.16845(4) 0.42836(4) 0.00651(12) Uani 1 1 d . . . Cl2 Cl 0.0000 0.0000 0.28442(6) 0.00578(19) Uani 1 3 d S . . Cl3 Cl 0.20607(4) -0.00203(4) 0.32587(4) 0.00777(12) Uani 1 1 d . . . Mo1 Mo 0.088685(13) -0.000443(12) 0.424219(13) 0.00424(6) Uani 1 1 d . . . Cl4 Cl 0.0000 0.0000 0.0000 0.0075(3) 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 0.0074(11) 0.0066(11) 0.0041(12) 0.0005(9) 0.0009(9) 0.0011(9) C2 0.0066(12) 0.0110(12) 0.0099(12) 0.0018(9) 0.0028(9) 0.0057(10) C3 0.0103(12) 0.0118(12) 0.0076(12) 0.0026(9) 0.0008(9) 0.0074(10) Se1 0.00612(12) 0.00650(12) 0.00700(13) -0.00130(9) -0.00030(9) 0.00291(10) Se2 0.00605(12) 0.00654(12) 0.00691(12) -0.00105(9) -0.00099(9) 0.00278(10) Cl1 0.0066(3) 0.0065(3) 0.0054(3) 0.0008(2) 0.0004(2) 0.0024(2) Cl2 0.0068(3) 0.0068(3) 0.0038(5) 0.000 0.000 0.00338(14) Cl3 0.0075(3) 0.0107(3) 0.0061(3) 0.0004(2) 0.0013(2) 0.0053(2) Mo1 0.00491(10) 0.00515(10) 0.00277(11) 0.00004(7) 0.00024(7) 0.00260(8) Cl4 0.0070(4) 0.0070(4) 0.0085(7) 0.000 0.000 0.0035(2) 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' Mo Mo -1.6832 0.6857 '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' 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 122.6(2) 13 . C1 C1 Se2 121.3(2) 13 . Se1 C1 Se2 116.05(12) . . C3 C2 Se1 119.62(17) . . C3 C2 H2 120.2 . . Se1 C2 H2 120.2 . . C2 C3 Se2 119.24(17) . . C2 C3 H3 120.4 . . Se2 C3 H3 120.4 . . C1 Se1 C2 92.37(10) . . C1 Se2 C3 92.57(10) . . Mo1 Cl1 Mo1 63.585(15) 12_556 2 Mo1 Cl1 Mo1 63.540(15) 12_556 . Mo1 Cl1 Mo1 63.527(15) 2 . Mo1 Cl2 Mo1 63.62(2) 3 2 Mo1 Cl2 Mo1 63.62(2) 3 . Mo1 Cl2 Mo1 63.62(2) 2 . Cl3 Mo1 Cl1 91.443(19) . 11_556 Cl3 Mo1 Cl2 92.89(2) . . Cl1 Mo1 Cl2 175.671(19) 11_556 . Cl3 Mo1 Cl1 91.830(19) . 3 Cl1 Mo1 Cl1 89.879(13) 11_556 3 Cl2 Mo1 Cl1 90.025(13) . 3 Cl3 Mo1 Cl1 92.616(19) . . Cl1 Mo1 Cl1 89.807(13) 11_556 . Cl2 Mo1 Cl1 89.953(13) . . Cl1 Mo1 Cl1 175.549(19) 3 . Cl3 Mo1 Mo1 134.290(15) . 11_556 Cl1 Mo1 Mo1 58.346(15) 11_556 11_556 Cl2 Mo1 Mo1 118.160(13) . 11_556 Cl1 Mo1 Mo1 58.154(13) 3 11_556 Cl1 Mo1 Mo1 118.126(14) . 11_556 Cl3 Mo1 Mo1 134.773(15) . 12_556 Cl1 Mo1 Mo1 58.266(15) 11_556 12_556 Cl2 Mo1 Mo1 118.160(13) . 12_556 Cl1 Mo1 Mo1 118.167(14) 3 12_556 Cl1 Mo1 Mo1 58.115(13) . 12_556 Mo1 Mo1 Mo1 60.027(11) 11_556 12_556 Cl3 Mo1 Mo1 135.218(15) . 3 Cl1 Mo1 Mo1 118.316(13) 11_556 3 Cl2 Mo1 Mo1 58.190(11) . 3 Cl1 Mo1 Mo1 58.297(14) 3 3 Cl1 Mo1 Mo1 118.159(14) . 3 Mo1 Mo1 Mo1 59.987(5) 11_556 3 Mo1 Mo1 Mo1 90.0 12_556 3 Cl3 Mo1 Mo1 135.709(15) . 2 Cl1 Mo1 Mo1 118.238(13) 11_556 2 Cl2 Mo1 Mo1 58.190(11) . 2 Cl1 Mo1 Mo1 118.278(14) 3 2 Cl1 Mo1 Mo1 58.178(14) . 2 Mo1 Mo1 Mo1 90.0 11_556 2 Mo1 Mo1 Mo1 59.986(5) 12_556 2 Mo1 Mo1 Mo1 60.0 3 2 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 C1 C1 1.386(4) 13 C1 Se1 1.870(2) . C1 Se2 1.870(2) . C2 C3 1.334(3) . C2 Se1 1.872(2) . C2 H2 1.0000 . C3 Se2 1.870(2) . C3 H3 1.0000 . Cl1 Mo1 2.4741(6) 12_556 Cl1 Mo1 2.4771(6) 2 Cl1 Mo1 2.4803(6) . Cl2 Mo1 2.4754(7) 3 Cl2 Mo1 2.4754(7) 2 Cl2 Mo1 2.4755(7) . Cl3 Mo1 2.4332(6) . Mo1 Cl1 2.4742(6) 11_556 Mo1 Cl1 2.4771(6) 3 Mo1 Mo1 2.6085(4) 11_556 Mo1 Mo1 2.6085(4) 12_556 Mo1 Mo1 2.6096(4) 3 Mo1 Mo1 2.6096(4) 2 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 -0.6(3) . . . . C1 C1 Se1 C2 -176.5(3) 13 . . . Se2 C1 Se1 C2 3.62(13) . . . . C3 C2 Se1 C1 -1.8(2) . . . . C1 C1 Se2 C3 176.3(3) 13 . . . Se1 C1 Se2 C3 -3.86(13) . . . . C2 C3 Se2 C1 2.7(2) . . . . Mo1 Cl2 Mo1 Cl3 143.614(17) 3 . . . Mo1 Cl2 Mo1 Cl3 -144.304(17) 2 . . . Mo1 Cl2 Mo1 Cl1 -36.95(19) 3 . . 11_556 Mo1 Cl2 Mo1 Cl1 35.13(19) 2 . . 11_556 Mo1 Cl2 Mo1 Cl1 51.781(15) 3 . . 3 Mo1 Cl2 Mo1 Cl1 123.863(14) 2 . . 3 Mo1 Cl2 Mo1 Cl1 -123.768(14) 3 . . . Mo1 Cl2 Mo1 Cl1 -51.686(15) 2 . . . Mo1 Cl2 Mo1 Mo1 -1.475(9) 3 . . 11_556 Mo1 Cl2 Mo1 Mo1 70.607(5) 2 . . 11_556 Mo1 Cl2 Mo1 Mo1 -70.608(5) 3 . . 12_556 Mo1 Cl2 Mo1 Mo1 1.475(9) 2 . . 12_556 Mo1 Cl2 Mo1 Mo1 72.082(10) 2 . . 3 Mo1 Cl2 Mo1 Mo1 -72.082(10) 3 . . 2 Mo1 Cl1 Mo1 Cl3 -143.312(16) 12_556 . . . Mo1 Cl1 Mo1 Cl3 144.583(15) 2 . . . Mo1 Cl1 Mo1 Cl1 -51.876(19) 12_556 . . 11_556 Mo1 Cl1 Mo1 Cl1 -123.982(17) 2 . . 11_556 Mo1 Cl1 Mo1 Cl2 123.801(16) 12_556 . . . Mo1 Cl1 Mo1 Cl2 51.696(16) 2 . . . Mo1 Cl1 Mo1 Cl1 34.1(3) 12_556 . . 3 Mo1 Cl1 Mo1 Cl1 -38.0(3) 2 . . 3 Mo1 Cl1 Mo1 Mo1 1.478(16) 12_556 . . 11_556 Mo1 Cl1 Mo1 Mo1 -70.627(14) 2 . . 11_556 Mo1 Cl1 Mo1 Mo1 -72.105(11) 2 . . 12_556 Mo1 Cl1 Mo1 Mo1 70.550(12) 12_556 . . 3 Mo1 Cl1 Mo1 Mo1 -1.555(14) 2 . . 3 Mo1 Cl1 Mo1 Mo1 72.105(11) 12_556 . . 2