Oxidative Addition across Sb–H and Sb–Sb Bonds by an Osmium Carbonyl Cluster: Trapping the Intermediate
Li, Ying-Zhou; Ganguly, Rakesh; Leong, Weng Kee; Organometallics 33 (2014) 823–; doi:10.1021/om401206d

data_4082432
_publ_section_title
;
 Oxidative Addition across Sb--H and Sb--Sb Bonds by an Osmium Carbonyl
 Cluster: Trapping the Intermediate
;
_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              823
_journal_paper_doi               10.1021/om401206d
_journal_volume                  33
_journal_year                    2014
_chemical_formula_sum            'C49.2 H26.4 O22.8 Os6 Sb2'
_chemical_formula_weight         2367.00
_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                 91.3300(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.5936(8)
_cell_length_b                   11.7000(5)
_cell_length_c                   27.9621(10)
_cell_measurement_reflns_used    2756
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      30.96
_cell_measurement_theta_min      2.71
_cell_volume                     5754.3(4)
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1128
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            19532
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         31.03
_diffrn_reflns_theta_min         1.89
_exptl_absorpt_coefficient_mu    14.192
_exptl_absorpt_correction_T_max  0.3964
_exptl_absorpt_correction_T_min  0.1844
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.732
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4248
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.654
_refine_diff_density_min         -1.630
_refine_diff_density_rms         0.363
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     731
_refine_ls_number_reflns         12727
_refine_ls_number_restraints     300
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0712
_refine_ls_R_factor_gt           0.0485
_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^)+(0.0000P)^2^+130.4457P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0876
_refine_ls_wR_factor_ref         0.0961
_reflns_number_gt                13751
_reflns_number_total             19532
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om401206d_si_001.cif
_cod_data_source_block           lwk163s
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from
2011-04-26.

'_exptl_absorpt_correction_type' value 'MULTI-SCAN'
changed to 'multi-scan' according to
/usr/data/users/saulius/automatic-downloads/current/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 
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_original_formula_sum        'C49.20 H26.40 O22.80 Os6 Sb2'
_cod_database_code               4082432