Tris(<i>N</i>,<i>N</i>-dimethylanilinium) tri-μ-bromido-bis[tribromidoantimonate(III)]
Kharrat, Houda; Kamoun, Slaheddine; Michaud, François; Acta Crystallographica Section E 69 (2013) m353–; doi:10.1107/S1600536813014335

data_2238274
_publ_section_title
;
 Tris(<i>N</i>,<i>N</i>-dimethylanilinium)
 tri-\m-bromido-bis[tribromidoantimonate(III)]
;
_journal_coeditor_code           VN2071
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m353
_journal_paper_doi               10.1107/S1600536813014335
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          '(C8 H12 N)3[Sb2 Br9]'
_chemical_formula_moiety         '3(C8 H12 N +), (Sb2 Br9 3-)'
_chemical_formula_sum            'C24 H36 Br9 N3 Sb2'
_chemical_formula_weight         1329.25
_chemical_name_systematic
;
Tris(<i>N</i>,<i>N</i>-dimethylanilinium)
tri-\m-bromido-bis[tribromidoantimonate(III)]
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                66.581(4)
_cell_angle_beta                 78.689(3)
_cell_angle_gamma                72.601(3)
_cell_formula_units_Z            2
_cell_length_a                   9.7857(3)
_cell_length_b                   13.7658(5)
_cell_length_c                   17.0297(6)
_cell_measurement_reflns_used    8586
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      44.7157
_cell_measurement_theta_min      3.0518
_cell_volume                     2000.90(14)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, 2009)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2009)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2009)'
_computing_molecular_graphics
;
<i>DIAMOND</i> (Brandenburg & Berndt, 1999) and
<i>Mercury</i> (Macrae <i>et al.</i>, 2008)
;
_computing_publication_material
;
<i>WinGX</i> (Farrugia, 2012) and <i>publCIF</i> (Westrip, 2010)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare <i>et al.</i>, 1993)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 8.3622
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device       'Kappa-geometry diffractometer'
_diffrn_measurement_device_type
'Oxford Diffraction Xcalibur (Sapphire2, large Be window)'
_diffrn_measurement_method       '\w and \p scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0546
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            29905
_diffrn_reflns_theta_full        30.51
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         3.06
_exptl_absorpt_coefficient_mu    10.355
_exptl_absorpt_correction_T_max  0.126
_exptl_absorpt_correction_T_min  0.038
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrysAlis RED; Oxford Diffraction, 2009)'
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    2.206
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'truncated prism, axis [1 0 0]'
_exptl_crystal_F_000             1236
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.326
_refine_diff_density_min         -0.89
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.875
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     398
_refine_ls_number_reflns         12050
_refine_ls_number_restraints     88
_refine_ls_restrained_S_all      0.873
_refine_ls_R_factor_all          0.1036
_refine_ls_R_factor_gt           0.0422
_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^)+(0.0451P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0843
_refine_ls_wR_factor_ref         0.0956
_reflns_number_gt                6232
_reflns_number_total             12050
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            vn2071.cif
_cod_data_source_block           I
_cod_original_cell_volume        2000.91(14)
_cod_database_code               2238274
_cod_database_fobs_code          2238274