Nucleophilic Addition Reactions of the Osmium−Antimony Cluster (μ-H)Os3(CO)9(μ3-C6H4)(μ-SbPh2): Orthometalation of Triphenylphosphine at Ambient Temperature
Chen, Guizhu; Deng, Mingli; Lee, Chee Keong; Leong, Weng Kee; Organometallics 21 (2002) 1227–; doi:10.1021/om010959a

data_4076702
_publ_section_title
;
 Nucleophilic Addition Reactions of the Osmium&#x2212;Antimony Cluster
 (\m-H)Os3(CO)9(\m3-C6H4)(\m-SbPh2):&#x00A0; Orthometalation of
 Triphenylphosphine at Ambient Temperature
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              1227
_journal_paper_doi               10.1021/om010959a
_journal_volume                  21
_journal_year                    2002
_chemical_formula_sum            'C45 H30 O9 Os3 P Sb'
_chemical_formula_weight         1438.01
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 106.4270(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.1280(2)
_cell_length_b                   18.9541(2)
_cell_length_c                   18.533
_cell_measurement_reflns_used    7021
_cell_measurement_temperature    293(2)
_cell_volume                     4423.32(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.902
_diffrn_measured_fraction_theta_max 0.902
_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  0.0360
_diffrn_reflns_av_sigmaI/netI    0.0427
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            28891
_diffrn_reflns_theta_full        29.31
_diffrn_reflns_theta_max         29.31
_diffrn_reflns_theta_min         2.01
_exptl_absorpt_coefficient_mu    9.283
_exptl_absorpt_correction_T_max  0.189284
_exptl_absorpt_correction_T_min  0.100457
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    2.159
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             2664
_exptl_crystal_size_max          0.430
_exptl_crystal_size_mid          0.390
_exptl_crystal_size_min          0.160
_refine_diff_density_max         1.722
_refine_diff_density_min         -1.572
_refine_diff_density_rms         0.196
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.149
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     548
_refine_ls_number_reflns         10920
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.151
_refine_ls_R_factor_all          0.0716
_refine_ls_R_factor_gt           0.0457
_refine_ls_shift/su_max          0.020
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0381P)^2^+18.6500P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0986
_refine_ls_wR_factor_ref         0.1110
_reflns_number_gt                8323
_reflns_number_total             10920
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om010959a.cif
_cod_data_source_block           cz30
_cod_original_cell_volume        4423.41(8)
_cod_database_code               4076702