Bis(1,4-diazoniabicyclo[2.2.2]octane) di-μ-chlorido-bis[tetrachloridoantimonate(III)] dihydrate
Ben Rhaiem, Tarek; Boughzala, Habib; Driss, Ahmed; Acta Crystallographica Section E 69 (2013) m330–; doi:10.1107/S160053681301307X

data_2238079
_publ_section_title
;
 Bis(1,4-diazoniabicyclo[2.2.2]octane)
 di-\m-chlorido-bis[tetrachloridoantimonate(III)] dihydrate
;
_journal_coeditor_code           WM2740
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m330
_journal_paper_doi               10.1107/S160053681301307X
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          '(C6 H14 N2)2 [Sb2 Cl10], 2H2 O'
_chemical_formula_moiety         '2(C6 H14 N2 2+), Sb2 Cl10 4-, 2(H2 O)'
_chemical_formula_sum            'C12 H32 Cl10 N4 O2 Sb2'
_chemical_formula_weight         862.46
_chemical_melting_point          571
_chemical_name_systematic
;
Bis(1,4-diazoniabicyclo[2.2.2]octane)
di-\m-chlorido-bis[tetrachloridoantimonate(III)]
dihydrate
;
_space_group_IT_number           58
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2 2n'
_symmetry_space_group_name_H-M   'P n n m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.1620(10)
_cell_length_b                   20.869(7)
_cell_length_c                   7.566(2)
_cell_measurement_reflns_used    1700
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.0
_cell_measurement_theta_min      2.4
_cell_volume                     1446.6(6)
_computing_cell_refinement       'CAD-4 EXPRESS (Duisenberg, 1992)'
_computing_data_collection       'CAD-4 EXPRESS (Duisenberg, 1992)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2006)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Enraf--Nonius CAD-4'
_diffrn_measurement_method       'non-profiled omega/2theta 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  0.0287
_diffrn_reflns_av_sigmaI/netI    0.0246
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       3
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            2797
_diffrn_reflns_theta_full        26.97
_diffrn_reflns_theta_max         26.97
_diffrn_reflns_theta_min         2.43
_diffrn_standards_decay_%        1
_diffrn_standards_interval_time  120
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    2.809
_exptl_absorpt_correction_T_max  0.4312
_exptl_absorpt_correction_T_min  0.3341
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
(North <i>et al.</i>, 1968)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.980
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          0.36
_refine_diff_density_max         0.591
_refine_diff_density_min         -0.365
_refine_ls_extinction_coef       0.0099(5)
_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   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     82
_refine_ls_number_reflns         1700
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0289
_refine_ls_R_factor_gt           0.0227
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0268P)^2^+1.1425P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0579
_refine_ls_wR_factor_ref         0.0608
_reflns_number_gt                1488
_reflns_number_total             1700
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            wm2740.cif
_cod_data_source_block           I
_cod_original_cell_volume        1446.8(7)
_cod_database_code               2238079
_cod_database_fobs_code          2238079