Crystal structure of [Me3Sb–SbMe2]2[(MeSbBr3)2], a trimethylstibine adduct of the dimethylstibenium ion or a stibinostibonium salt?
Althaus, Henrik; Breunig, Hans J.; Lork, Enno; Chemical Communications  (1999) 1971–; doi:10.1039/a905837k

data_7110657
_publ_section_title
;
 Crystal structure of [Me3Sb--SbMe2]2[(MeSbBr3)2], a trimethylstibine
 adduct of the dimethylstibenium ion or a stibinostibonium salt?
;
_journal_issue                   19
_journal_name_full               'Chemical Communications'
_journal_page_first              1971
_journal_paper_doi               10.1039/a905837k
_journal_year                    1999
_chemical_formula_sum            'C12 H36 Br6 Sb6'
_chemical_formula_weight         1390.35
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 107.06(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.894(2)
_cell_length_b                   7.711(2)
_cell_length_c                   19.067(5)
_cell_measurement_reflns_used    45
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      12.5165
_cell_measurement_theta_min      3.479
_cell_volume                     1671.8(7)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens XSCANS'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.890
_diffrn_measured_fraction_theta_max 0.890
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_measurement_method       '2\q/\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0354
_diffrn_reflns_av_sigmaI/netI    0.0602
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            4409
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         2.87
_diffrn_standards_decay_%        'random variation +/-2.0'
_diffrn_standards_interval_count 197
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    11.949
_exptl_absorpt_correction_T_max  0.0868
_exptl_absorpt_correction_T_min  0.0657
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
'North, Phillips, Mathews, Acta. Crystallogr. 1968'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.762
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.40
_refine_diff_density_max         1.786
_refine_diff_density_min         -1.716
_refine_diff_density_rms         0.258
_refine_ls_extinction_coef       0.0044(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     117
_refine_ls_number_reflns         3408
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0704
_refine_ls_R_factor_gt           0.0522
_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^)+(0.0836P)^2^+0.8334P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1287
_refine_ls_wR_factor_ref         0.1391
_reflns_number_gt                2635
_reflns_number_total             3408
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            905837ksup1.cif
_cod_data_source_block           '[(CH3)5Sb2]2[(CH3)2Sb2Br6]'
_cod_depositor_comments
;
The following automatic conversions were performed:
'_atom_site_symetry_multiplicity' tag replaced with
'_atom_site_symmetry_multiplicity'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7110657