Octahedral distortion caused by hydrogen bonding in tris(diethylammonium) hexachloridoantimonate(III)
Bujak, Maciej; Acta Crystallographica Section C 66 (2010) m101–m103; doi:10.1107/S0108270110006074

data_2017596
_publ_section_title
;
 Octahedral distortion caused by hydrogen bonding in
 tris(diethylammonium) hexachloridoantimonate(III)
;
_journal_coeditor_code           EM3030
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m101
_journal_page_last               m103
_journal_paper_doi               10.1107/S0108270110006074
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '(C4 H12 N)3 [Sb Cl6]'
_chemical_formula_moiety         '3(C4 H12 N +), Sb Cl6 3-'
_chemical_formula_sum            'C12 H36 Cl6 N3 Sb'
_chemical_formula_weight         556.90
_chemical_name_systematic
;
Tris(diethylammonium) hexachloridoantimonate(III)
;
_space_group_crystal_system      trigonal
_space_group_IT_number           161
_symmetry_space_group_name_Hall  'R 3 -2"c'
_symmetry_space_group_name_H-M   'R 3 c :H'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   14.71917(18)
_cell_length_b                   14.71917(18)
_cell_length_c                   18.9694(3)
_cell_measurement_reflns_used    8381
_cell_measurement_temperature    85.00(10)
_cell_measurement_theta_max      29.71
_cell_measurement_theta_min      2.76
_cell_volume                     3559.19(8)
_computing_cell_refinement       'CrysAlisPro (Oxford Diffraction, 2009)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2009)'
_computing_data_reduction        'CrysAlisPro (Oxford Diffraction, 2009)'
_computing_molecular_graphics    'Mercury (Macrae <i>et al.</i>,  2008)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      85.00(10)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur'
_diffrn_measurement_method       \w--scan
_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  0.0120
_diffrn_reflns_av_sigmaI/netI    0.0089
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            9101
_diffrn_reflns_theta_full        29.00
_diffrn_reflns_theta_max         29.48
_diffrn_reflns_theta_min         2.68
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.839
_exptl_absorpt_correction_T_max  0.760
_exptl_absorpt_correction_T_min  0.713
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlis RED (Oxford Diffraction, 2009); analytical numeric absorption
correction using a multifaceted crystal
model based on expressions derived by Clark & Reid (1995)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.559
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tabular
_exptl_crystal_F_000             1692
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.528
_refine_diff_density_min         -0.542
_refine_ls_abs_structure_details 'Flack (1983), 973 Friedel pairs'
_refine_ls_abs_structure_Flack   0.001(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.478
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     78
_refine_ls_number_reflns         2056
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.477
_refine_ls_R_factor_all          0.0095
_refine_ls_R_factor_gt           0.0082
_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^)+(0.0038P)^2^+4.6787P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0180
_refine_ls_wR_factor_ref         0.0296
_reflns_number_gt                2018
_reflns_number_total             2056
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            em3030.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'R 3 c'
_cod_database_code               2017596
_cod_database_fobs_code          2017596