Tetrakis(tetramethylammonium) dodeca-μ-chloro-hexachloro-<i>octahedro</i>-hexatantalate chloride
Vojnović, Marija; Jozić, Dražan; Bašic, Ivan; Rončević, Sanda; Planinić, Pavica; Acta Crystallographica Section C 60 (2004) m33–m34; doi:10.1107/S0108270103025071

data_2013876
_publ_section_title
;
 Tetrakis(tetramethylammonium)
 dodeca-\m-chloro-hexachloro-<i>octahedro</i>-hexatantalate chloride
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m33
_journal_page_last               m34
_journal_paper_doi               10.1107/S0108270103025071
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          '(C4 H12 N)4 [Ta6 Cl18] Cl'
_chemical_formula_moiety         'C16 H48 Cl19 N4 Ta6'
_chemical_formula_structural     '((C H3)4 N)4 ((Ta6 Cl12) Cl6) Cl'
_chemical_formula_sum            'C16 H48 Cl19 N4 Ta6'
_chemical_formula_weight         2055.83
_chemical_name_systematic
;
Tetrakis(tetramethylammonium)dodeca-\m-chloro-hexachloro-octahedro-
hexatantalate chloride
;
_space_group_IT_number           225
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  '-F 4 2 3'
_symmetry_space_group_name_H-M   'F m -3 m'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.1781(4)
_cell_length_b                   18.1781(4)
_cell_length_c                   18.1781(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.2114
_cell_measurement_theta_min      20.4262
_cell_volume                     6006.8(2)
_computing_cell_refinement       'CAD-4 Software'
_computing_data_collection       'CAD-4 Software (Enraf--Nonius, 1998)'
_computing_data_reduction        'HELENA (Spek, 1997)'
_computing_molecular_graphics    'WinGX (Farrugia, 1999)'
_computing_publication_material  'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean '?   # Not in version 2.0.1'
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Enraf--Nonius CAD4'
_diffrn_measurement_method       \w/2\q
_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  0.0633
_diffrn_reflns_av_sigmaI/netI    0.0388
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            1958
_diffrn_reflns_theta_full        27.85
_diffrn_reflns_theta_max         27.85
_diffrn_reflns_theta_min         2.24
_diffrn_standards_decay_%        54
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    11.745
_exptl_absorpt_correction_T_max  0.244
_exptl_absorpt_correction_T_min  0.201
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(North et al., 1968)'
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    2.273
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       octahedra-like
_exptl_crystal_F_000             3732
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.91
_refine_diff_density_min         -1.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.137
_refine_ls_goodness_of_fit_ref   1.148
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     24
_refine_ls_number_reflns         412
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.137
_refine_ls_restrained_S_obs      1.148
_refine_ls_R_factor_all          0.0374
_refine_ls_R_factor_gt           0.0272
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0331P)^2^+58.2675P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0622
_refine_ls_wR_factor_ref         0.068
_reflns_number_gt                351
_reflns_number_total             412
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sq1032.cif
_cod_data_source_block           I
_cod_database_code               2013876
_cod_database_fobs_code          2013876