The First Mixed-Valent Antimony(III/V) Oxo Clusters (2,6-Mes2C6H3Sb)2(ClSb)4O8and (2,6-Mes2C6H3Sb)4(ClSb)4(HOSb)2O14†
Beckmann, Jens; Heek, Timm; Takahashi, Masashi; Organometallics 26 (2007) 3633–; doi:10.1021/om700434m

data_4073535
_publ_section_title
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 The First Mixed-Valent Antimony(III/V) Oxo Clusters
 (2,6-Mes2C6H3Sb)2(ClSb)4O8and (2,6-Mes2C6H3Sb)4(ClSb)4(HOSb)2O14&#x2020;
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_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              3633
_journal_paper_doi               10.1021/om700434m
_journal_volume                  26
_journal_year                    2007
_chemical_formula_sum            'C52 H60 Cl4 O Sb2'
_chemical_formula_weight         1086.36
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 93.371(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.657(2)
_cell_length_b                   17.087(3)
_cell_length_c                   13.974(3)
_cell_measurement_temperature    173
_cell_volume                     2540.2(9)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      173
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans with .3 deg in omega'
_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  0.0221
_diffrn_reflns_av_sigmaI/netI    0.0313
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            31220
_diffrn_reflns_theta_full        30.57
_diffrn_reflns_theta_max         30.57
_diffrn_reflns_theta_min         1.46
_exptl_absorpt_coefficient_mu    1.308
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.76
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.420
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1100
_exptl_crystal_size_max          .44
_exptl_crystal_size_mid          .40
_exptl_crystal_size_min          .09
_refine_diff_density_max         1.295
_refine_diff_density_min         -0.643
_refine_diff_density_rms         0.090
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.438(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     609
_refine_ls_number_reflns         15013
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0398
_refine_ls_R_factor_gt           0.0329
_refine_ls_shift/su_max          2.280
_refine_ls_shift/su_mean         0.049
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0487P)^2^+1.1184P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0822
_refine_ls_wR_factor_ref         0.0882
_reflns_number_gt                13553
_reflns_number_total             15013
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om700434m-file002.cif
_cod_data_source_block           publication_text
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        2540.3(9)
_cod_original_sg_symbol_H-M      'P2(1)   '
_cod_original_formula_sum        'C52 H60 Cl4 O1 Sb2'
_cod_database_code               4073535