Bis(tetramethylammonium) hexaaquadodeca-μ-bromo-<i>octahedro</i>-hexatantalum tetrabromide dihydrate
Vojnović, Marija; Jozić, Dražan; Giester, Gerald; Perić, Berislav; Planinić, Pavica; Brničević, Nevenka; Acta Crystallographica Section C 58 (2002) m219–m220; doi:10.1107/S0108270102001841

data_2012652
_publ_section_title
;
 Bis(tetramethylammonium)
 hexaaquadodeca-\m-bromo-<i>octahedro</i>-hexatantalum tetrabromide
 dihydrate
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m219
_journal_page_last               m220
_journal_paper_doi               10.1107/S0108270102001841
_journal_volume                  58
_journal_year                    2002
_chemical_formula_iupac          '(C4 H12 N)2 [Ta6 Br12 (H2 O)6] Br4 , 2H2O'
_chemical_formula_moiety
'2C4 H12 N + , Br12 H12 O6 Ta6 2+ , 4Br - , 2H2 O'
_chemical_formula_structural     '(C4 H12 N)2 [Ta6 Br12 (H2 O)6] Br4 , 2H2O'
_chemical_formula_sum            'C8 H40 Br16 N2 O8 Ta6'
_chemical_formula_weight         2656.52
_chemical_name_systematic
;
Hexaaquadodecabromohexatantalum(I,II) bis(tetramethylammonium) tetrabromide
dihydrate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 127.74(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.388(5)
_cell_length_b                   12.470(2)
_cell_length_c                   18.425(4)
_cell_measurement_reflns_used    12960
_cell_measurement_temperature    200
_cell_measurement_theta_max      30.52
_cell_measurement_theta_min      2.11
_cell_volume                     4431(2)
_computing_cell_refinement       'DENZO-SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction        DENZO-SCALEPACK
_computing_molecular_graphics
'ATOMS (Dowty, 2001) and ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'PLATON (Spek, 1990)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      200
_diffrn_detector_area_resol_mean 18.4
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Nonius KappaCCD area-detector'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.033
_diffrn_reflns_av_sigmaI/netI    0.037
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            12960
_diffrn_reflns_reduction_process
;
 ?
;
_diffrn_reflns_theta_full        30.52
_diffrn_reflns_theta_max         30.52
_diffrn_reflns_theta_min         2.11
_exptl_absorpt_coefficient_mu    29.214
_exptl_absorpt_correction_T_max  0.232
_exptl_absorpt_correction_T_min  0.054
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO-SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    3.982
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4656
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.50
_refine_diff_density_min         -2.94
_refine_ls_extinction_coef       0.000407(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 1997)'
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     219
_refine_ls_number_reflns         6770
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.036
_refine_ls_R_factor_gt           0.028
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0172P)^2^+7.5089P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.066
_refine_ls_wR_factor_ref         0.069
_reflns_number_gt                5864
_reflns_number_total             6770
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sk1533.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' 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_sg_symbol_H-M      'C 2/c'
_cod_database_code               2012652
_cod_database_fobs_code          2012652