#------------------------------------------------------------------------------ #$Date: 2016-03-23 01:24:16 +0200 (Wed, 23 Mar 2016) $ #$Revision: 179139 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/31/00/4310078.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_4310078 loop_ _publ_author_name 'Maxim N. Sokolov' 'Artem L. Gushchin' 'Pavel A. Abramov' 'Alexandr V. Virovets' 'Eugenia V. Peresypkina' 'Svetlana G. Kozlova' 'Boris A. Kolesov' 'Cristian Vicent' 'Vladimir P. Fedin' _publ_contact_author_address ; Nikolaev Institute of Inorganic Chemistry SD RAS Ak.Lavrentiev prosp. 3 Novosibirsk 630090 Russia ; _publ_contact_author_email peresyp@che.nsk.su _publ_contact_author_fax '007 3832 309489' _publ_contact_author_name 'Dr Eugenia V Peresypkina' _publ_contact_author_phone '007 3832 309466' _publ_section_title ; Synthesis and Structure of Ta4S9Br8. An Emergent Family of Early Transition Metal Chalcogenide Clusters ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 8756 _journal_page_last 8761 _journal_paper_doi 10.1021/ic051014e _journal_volume 44 _journal_year 2005 _chemical_formula_moiety 'Br8 S9 Ta4' _chemical_formula_sum 'Br8 S9 Ta4' _chemical_formula_weight 1651.62 _chemical_name_systematic ; mu4-sulfo-tetrakis(mu2,hapta2-disulfo)-octabromo-tetratantalum(IV,V) ; _space_group_IT_number 107 _symmetry_cell_setting tetragonal _symmetry_space_group_name_Hall 'I 4 -2' _symmetry_space_group_name_H-M 'I 4 m m' _atom_sites_solution_hydrogens none _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 12.765(5) _cell_length_b 12.765(5) _cell_length_c 6.966(4) _cell_measurement_reflns_used 459 _cell_measurement_temperature 295(2) _cell_measurement_theta_max 24.09 _cell_measurement_theta_min 2.26 _cell_volume 1135.1(9) _computing_cell_refinement 'APEX2 v.1.0-8 (Bruker, 2003)' _computing_data_collection 'APEX2 v.1.0-8 (Bruker, 2003)' _computing_data_reduction 'APEX2 v.1.0-8 (Bruker, 2003)' _computing_molecular_graphics 'SHELXTL v.6.22 (Bruker, 1990-2003)' _computing_publication_material 'local programs' _computing_structure_refinement 'SHELXTL v.6.22 (Bruker, 1990-2003)' _computing_structure_solution 'SHELXTL v.6.22 (Bruker, 1990-2003)' _diffrn_ambient_temperature 295(2) _diffrn_detector_area_resol_mean 25.6 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Bruker X8APEX CCD diffractometer' _diffrn_measurement_method 'phi 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 0.0677 _diffrn_reflns_av_sigmaI/netI 0.0675 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 5 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_number 2459 _diffrn_reflns_theta_full 25.00 _diffrn_reflns_theta_max 27.44 _diffrn_reflns_theta_min 2.26 _diffrn_standards_decay_% 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 34.112 _exptl_absorpt_correction_T_max 0.51 _exptl_absorpt_correction_T_min 0.22 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'based on intensities, SADABS (Bruker)' _exptl_crystal_colour black _exptl_crystal_density_diffrn 4.833 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description 'tetragonal prism' _exptl_crystal_F_000 1432 _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _refine_diff_density_max 1.586 _refine_diff_density_min -1.107 _refine_diff_density_rms 0.266 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881, 246 Friedel pairs' _refine_ls_abs_structure_Flack 0.03(4) _refine_ls_extinction_coef 0 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_hydrogen_treatment none _refine_ls_matrix_type full _refine_ls_number_parameters 34 _refine_ls_number_reflns 656 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.015 _refine_ls_R_factor_all 0.0488 _refine_ls_R_factor_gt 0.0335 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0183P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0649 _refine_ls_wR_factor_ref 0.0695 _reflns_number_gt 546 _reflns_number_total 656 _reflns_threshold_expression >2sigma(I) _cod_data_source_file ic051014esi20050622_121326.cif _cod_data_source_block compound1 _cod_depositor_comments ; The following automatic conversions were performed: '_exptl_crystal_density_meas' value 'none' was changed to '?' - the value is perceived as not measured. Automatic conversion script Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas ; _cod_original_cell_volume 1135.0(9) _cod_database_code 4310078 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y, x, z' 'y, -x, z' 'x, -y, z' '-x, y, z' '-y, -x, z' 'y, x, z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-y+1/2, x+1/2, z+1/2' 'y+1/2, -x+1/2, z+1/2' 'x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, z+1/2' '-y+1/2, -x+1/2, z+1/2' 'y+1/2, x+1/2, z+1/2' 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 Ta1 Ta 0.0000 0.18290(5) 0.93341(12) 0.0269(2) Uani 1 2 d S . . S1 S 0.0000 0.0000 0.8216(14) 0.029(2) Uani 1 8 d S . . S2 S 0.1970(2) 0.1970(2) 0.9301(12) 0.0369(10) Uani 1 2 d S . . S3 S 0.1348(3) 0.1348(3) 1.1784(8) 0.0342(12) Uani 1 2 d S . . Br1 Br 0.0000 0.23194(17) 0.5885(3) 0.0419(5) Uani 1 2 d S . . Br2 Br 0.0000 0.36009(16) 1.0762(5) 0.0471(6) Uani 1 2 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 Ta1 0.0249(4) 0.0195(4) 0.0363(4) 0.0009(5) 0.000 0.000 S1 0.024(3) 0.024(3) 0.040(6) 0.000 0.000 0.000 S2 0.0269(14) 0.0269(14) 0.057(3) -0.002(3) -0.002(3) -0.0037(19) S3 0.0324(19) 0.0324(19) 0.038(3) -0.0046(19) -0.0046(19) -0.001(3) Br1 0.0493(13) 0.0355(12) 0.0410(13) 0.0078(11) 0.000 0.000 Br2 0.0473(14) 0.0212(10) 0.0728(15) -0.0097(13) 0.000 0.000 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ta Ta -0.7052 6.5227 '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 Ta1 Ta1 Ta1 90.0 3 4 yes S1 Ta1 Ta1 47.88(7) . 3 ? S1 Ta1 Ta1 47.88(7) . 4 ? S1 Ta1 S2 93.71(8) . 3 ? S1 Ta1 S2 93.71(8) . . yes S1 Ta1 S3 89.04(19) . 3 ? S1 Ta1 S3 89.04(19) . . yes S1 Ta1 Br1 86.1(2) . . yes S1 Ta1 Br2 174.7(2) . . yes S2 Ta1 Ta1 49.08(7) 3 3 ? S2 Ta1 Ta1 139.08(7) . 3 yes S2 Ta1 Ta1 139.08(7) 3 4 yes S2 Ta1 Ta1 49.08(7) . 4 ? S2 Ta1 S2 171.77(14) 3 . yes S3 Ta1 Ta1 48.68(8) 3 3 ? S3 Ta1 Ta1 108.25(12) . 3 yes S3 Ta1 Ta1 108.25(12) 3 4 yes S3 Ta1 Ta1 48.68(8) . 4 ? S3 Ta1 S2 48.47(19) 3 3 ? S3 Ta1 S2 135.3(2) . 3 yes S3 Ta1 S2 135.3(2) 3 . yes S3 Ta1 S2 48.47(19) . . yes S3 Ta1 S3 87.0(2) 3 . yes Br1 Ta1 Ta1 100.27(4) . 3 yes Br1 Ta1 Ta1 100.27(4) . 4 yes Br1 Ta1 S2 88.47(18) . 3 yes Br1 Ta1 S2 88.47(18) . . yes Br1 Ta1 S3 136.25(12) . 3 yes Br1 Ta1 S3 136.25(12) . . yes Br2 Ta1 Ta1 130.34(3) . 3 yes Br2 Ta1 Ta1 130.34(3) . 4 yes Br2 Ta1 S2 86.47(9) . 3 ? Br2 Ta1 S2 86.47(9) . . yes Br2 Ta1 S3 87.12(10) . 3 ? Br2 Ta1 S3 87.12(10) . . yes Br2 Ta1 Br1 99.14(10) . . yes Ta1 S1 Ta1 143.1(4) 4 3 yes Ta1 S1 Ta1 84.25(13) 4 2 ? Ta1 S1 Ta1 84.25(13) 3 2 ? Ta1 S1 Ta1 84.25(13) 4 . yes Ta1 S1 Ta1 84.25(13) 3 . yes Ta1 S1 Ta1 143.1(4) 2 . yes Ta1 S2 Ta1 81.83(13) . 4 yes S3 S2 Ta1 65.25(17) . . yes S3 S2 Ta1 65.25(17) . 4 ? Ta1 S3 Ta1 82.64(16) . 4 ? S2 S3 Ta1 66.28(16) . . yes S2 S3 Ta1 66.28(16) . 4 ? 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 Ta1 Ta1 3.3017(15) 3 yes Ta1 Ta1 3.3017(15) 4 yes Ta1 S1 2.461(3) . yes Ta1 S2 2.521(3) 3 yes Ta1 S2 2.521(3) . yes Ta1 S3 2.500(4) 3 yes Ta1 S3 2.500(4) . yes Ta1 Br1 2.483(3) . yes Ta1 Br2 2.471(2) . yes S1 Ta1 2.461(3) 4 yes S1 Ta1 2.461(3) 3 yes S1 Ta1 2.461(3) 2 yes S2 Ta1 2.521(3) 4 yes S2 S3 2.061(8) . yes S3 Ta1 2.500(4) 4 yes