Binuclear Oxidative Addition of Sb‒Cl Bonds: A Facile Synthetic Route to Main Group‒Transition Element Clusters and Rings
Li, Ying-Zhou; Ganguly, Rakesh; Leong, Weng Kee; Organometallics 33 (2014) 3867–; doi:10.1021/om500565d

data_4084017
_publ_section_title
;
 Binuclear Oxidative Addition of Sb--Cl Bonds: A Facile Synthetic Route to
 Main Group--Transition Element Clusters and Rings
;
_journal_issue                   14
_journal_name_full               Organometallics
_journal_page_first              3867
_journal_paper_doi               10.1021/om500565d
_journal_volume                  33
_journal_year                    2014
_chemical_formula_sum            'C38.7 H29.4 Cl3.4 O10 Os3 Sb2'
_chemical_formula_weight         1589.05
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
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_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                101.7337(17)
_cell_angle_beta                 105.3496(17)
_cell_angle_gamma                108.7234(17)
_cell_formula_units_Z            2
_cell_length_a                   12.7426(4)
_cell_length_b                   14.6320(4)
_cell_length_c                   15.3921(5)
_cell_measurement_reflns_used    9988
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      27.34
_cell_measurement_theta_min      2.26
_cell_volume                     2486.98(14)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      103(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0795
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_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            91054
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.26
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.937
_exptl_absorpt_correction_T_max  0.4685
_exptl_absorpt_correction_T_min  0.2680
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.122
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1459
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.854
_refine_diff_density_min         -1.816
_refine_diff_density_rms         0.259
_refine_ls_extinction_method     constr
_refine_ls_goodness_of_fit_ref   1.187
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     586
_refine_ls_number_reflns         10164
_refine_ls_number_restraints     372
_refine_ls_restrained_S_all      1.184
_refine_ls_R_factor_all          0.0535
_refine_ls_R_factor_gt           0.0418
_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^)+(0.0308P)^2^+36.8771P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0975
_refine_ls_wR_factor_ref         0.1078
_reflns_number_gt                8699
_reflns_number_total             10164
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om500565d_si_003.cif
_cod_data_source_block           lwk362
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 4084009--4084020.cif.
;
_cod_original_cell_volume        2486.97(13)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C38.70 H29.40 Cl3.40 O10 Os3 Sb2'
_cod_database_code               4084017