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_4076708
_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            'C74.375 H54.75 Cl0.75 O8 Os3 P3 Sb'
_chemical_formula_weight         1888.28
_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                64.5220(10)
_cell_angle_beta                 82.5900(10)
_cell_angle_gamma                89.9100(10)
_cell_formula_units_Z            4
_cell_length_a                   13.40470(10)
_cell_length_b                   23.8087(3)
_cell_length_c                   26.25160(10)
_cell_measurement_reflns_used    7996
_cell_measurement_temperature    293(2)
_cell_volume                     7486.61(13)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_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  0.0616
_diffrn_reflns_av_sigmaI/netI    0.1539
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            55114
_diffrn_reflns_theta_full        24.71
_diffrn_reflns_theta_max         29.37
_diffrn_reflns_theta_min         2.04
_exptl_absorpt_coefficient_mu    5.573
_exptl_absorpt_correction_T_max  0.603987
_exptl_absorpt_correction_T_min  0.455841
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.675
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3607
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.318
_refine_diff_density_min         -2.334
_refine_diff_density_rms         0.238
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     522
_refine_ls_number_reflns         24945
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.1335
_refine_ls_R_factor_gt           0.0715
_refine_ls_shift/su_max          0.047
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0780P)^2^+83.2812P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1657
_refine_ls_wR_factor_ref         0.1996
_reflns_number_gt                17084
_reflns_number_total             34796
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om010959a.cif
_cod_data_source_block           cz26
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'TRICLINIC' changed to 'triclinic'
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 

2026-02-27
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_weight         3776.56
_cod_original_formula_units_Z            2
_cod_original_cell_volume        7486.61(11)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C148.75 H109.50 Cl1.50 O16 Os6 P6 Sb2'
_cod_database_code               4076708