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_4073534
_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            'C104 H122 Cl4 O18 Sb10'
_chemical_formula_weight         3019.42
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                62.465(5)
_cell_angle_beta                 63.750(5)
_cell_angle_gamma                82.683(5)
_cell_formula_units_Z            1
_cell_length_a                   15.066(3)
_cell_length_b                   15.160(3)
_cell_length_c                   15.218(3)
_cell_measurement_temperature    173
_cell_volume                     2751.2(10)
_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 0.983
_diffrn_measured_fraction_theta_max 0.983
_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  0.0269
_diffrn_reflns_av_sigmaI/netI    0.0410
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            27579
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         1.52
_exptl_absorpt_coefficient_mu    2.572
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.68
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.822
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1468
_exptl_crystal_size_max          .5
_exptl_crystal_size_mid          .25
_exptl_crystal_size_min          .1
_refine_diff_density_max         2.275
_refine_diff_density_min         -1.362
_refine_diff_density_rms         0.237
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     613
_refine_ls_number_reflns         12462
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0646
_refine_ls_R_factor_gt           0.0408
_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^)+(0.0581P)^2^+9.5323P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1057
_refine_ls_wR_factor_ref         0.1210
_reflns_number_gt                9353
_reflns_number_total             12462
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om700434m-file002.cif
_cod_data_source_block           publication_text
_cod_original_cell_volume        2751.2(9)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4073534