Tris(4-methylanilinium) pentachloridoantimonate(III) chloride monohydrate
Xu, Qian; Acta Crystallographica Section E 68 (2012) m438–; doi:10.1107/S1600536812009427

data_2234478
_publ_section_title
;
 Tris(4-methylanilinium) pentachloridoantimonate(III) chloride monohydrate
;
_journal_coeditor_code           YK2046
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m438
_journal_paper_doi               10.1107/S1600536812009427
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '(C7 H10 N)3 [Sb Cl5] Cl, H2 O'
_chemical_formula_moiety         '3(C7 H10 N +), Cl5 Sb 2-, Cl -, H2 O'
_chemical_formula_sum            'C21 H32 Cl6 N3 O Sb'
_chemical_formula_weight         676.95
_chemical_name_systematic
;
Tris(4-methylanilinium) pentachloridoantimonate(III)
chloride monohydrate
;
_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                63.35(3)
_cell_angle_beta                 83.08(3)
_cell_angle_gamma                82.51(3)
_cell_formula_units_Z            2
_cell_length_a                   9.4109(19)
_cell_length_b                   12.867(3)
_cell_length_c                   13.501(3)
_cell_measurement_reflns_used    6609
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.4839
_cell_measurement_theta_min      2.2882
_cell_volume                     1445.1(7)
_computing_cell_refinement       'CrystalClear (Rigaku, 2005)'
_computing_data_collection       'CrystalClear (Rigaku, 2005)'
_computing_data_reduction        'CrystalClear (Rigaku, 2005)'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Putz, 2005)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku SCXmini'
_diffrn_measurement_method       '\w 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  0.0294
_diffrn_reflns_av_sigmaI/netI    0.0350
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            15103
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.05
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.528
_exptl_absorpt_correction_T_max  0.7298
_exptl_absorpt_correction_T_min  0.6488
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrystalClear; Rigaku, 2005)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.556
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             680
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.454
_refine_diff_density_min         -0.626
_refine_ls_extinction_coef       0.0277(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     304
_refine_ls_number_reflns         6609
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0322
_refine_ls_R_factor_gt           0.0275
_refine_ls_shift/su_max          0.041
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0383P)^2^+0.2569P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0680
_refine_ls_wR_factor_ref         0.0748
_reflns_number_gt                6031
_reflns_number_total             6609
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            yk2046.cif
_cod_data_source_block           I
_cod_original_cell_volume        1445.1(5)
_cod_database_code               2234478
_cod_database_fobs_code          2234478