Tetra-μ~2~-oxido-di-μ~4~-peroxido-tetrakis[diphenylantimony(V)] chloroform disolvate
Betz, Richard; Lindner, Christoph; Klüfers, Peter; Mayer, Peter; Acta Crystallographica Section E 65 (2009) m253–m254; doi:10.1107/S160053680804419X

data_2221065
_publ_section_title
;
 Tetra-\m~2~-oxido-di-\m~4~-peroxido-tetrakis[diphenylantimony(V)]
 chloroform disolvate
;
_journal_coeditor_code           GK2183
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m253
_journal_page_last               m254
_journal_paper_doi               10.1107/S160053680804419X
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          '[Sb4 (C6 H5)8 O4 (O2)2], 2C H Cl3'
_chemical_formula_moiety         'C48 H40 O8 Sb4, 2(C H Cl3)'
_chemical_formula_sum            'C50 H42 Cl6 O8 Sb4'
_chemical_formula_weight         1470.54
_chemical_name_systematic
;
Tetra-\m~2~-oxido-di-\m~4~-peroxido-tetrakis[diphenylantimony(V)]
chloroform disolvate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 105.3795(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   23.0764(3)
_cell_length_b                   13.7353(2)
_cell_length_c                   34.6597(4)
_cell_measurement_reflns_used    79731
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      3.134
_cell_volume                     10592.4(2)
_computing_cell_refinement       'SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2004)'
_computing_data_reduction
'DENZO and SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics
'ORTEP-3 (Farrugia, 1997) and Mercury (Macrae <i>et al.</i>,  2006)'
_computing_publication_material
'SHELXL97 (Sheldrick, 2008) and PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Altomare <i>et al.</i>,  1999)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  'MONTEL, graded multilayered X-ray optics'
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0587
_diffrn_reflns_av_sigmaI/netI    0.0505
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            71535
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         3.19
_exptl_absorpt_coefficient_mu    2.372
_exptl_absorpt_correction_T_max  0.684
_exptl_absorpt_correction_T_min  0.599
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2001)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.844
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5696
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.983
_refine_diff_density_min         -0.889
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     614
_refine_ls_number_reflns         12127
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0700
_refine_ls_R_factor_gt           0.0366
_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^)+(0.0299P)^2^+28.2696P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0714
_refine_ls_wR_factor_ref         0.0817
_reflns_number_gt                8489
_reflns_number_total             12127
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            gk2183.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2221065
_cod_database_fobs_code          2221065