Synthesis and Structure of Ta4S9Br8. An Emergent Family of Early Transition Metal Chalcogenide Clusters
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; Inorganic Chemistry 44 (2005) 8756–8761; doi:10.1021/ic051014e

data_4310078
_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