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_4076703
_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            'C48 H36 O9 Os3 P Sb'
_chemical_formula_weight         1480.09
_chemical_name_systematic
; 
 ? 
;
_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                 102.5070(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.7183(2)
_cell_length_b                   17.4565(3)
_cell_length_c                   20.1485(2)
_cell_measurement_reflns_used    6881
_cell_measurement_temperature    293(2)
_cell_volume                     4710.53(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.898
_diffrn_measured_fraction_theta_max 0.898
_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  0.0380
_diffrn_reflns_av_sigmaI/netI    0.0465
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            30987
_diffrn_reflns_theta_full        29.39
_diffrn_reflns_theta_max         29.39
_diffrn_reflns_theta_min         2.02
_exptl_absorpt_coefficient_mu    8.721
_exptl_absorpt_correction_T_max  0.297276
_exptl_absorpt_correction_T_min  0.195012
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    2.087
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             2760
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.180
_refine_diff_density_max         1.374
_refine_diff_density_min         -1.422
_refine_diff_density_rms         0.159
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     563
_refine_ls_number_reflns         11660
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0689
_refine_ls_R_factor_gt           0.0394
_refine_ls_shift/su_max          0.031
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0227P)^2^+14.0188P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0698
_refine_ls_wR_factor_ref         0.0810
_reflns_number_gt                8619
_reflns_number_total             11660
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om010959a.cif
_cod_data_source_block           cz32
_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_sg_symbol_H-M      P2(1)/n
_cod_database_code               4076703