Complexation and C−H/C−P Bond Activation of the (PPh2)C60H Molecule on Triosmium Carbonyl Clusters
Yeh, Wen-Yann; Tsai, Kune-You; Organometallics 29 (2010) 604–; doi:10.1021/om900914a

data_4067390
_publ_section_title
;
 Complexation and C&#x2212;H/C&#x2212;P Bond Activation of the (PPh2)C60H
 Molecule on Triosmium Carbonyl Clusters
;
_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              604
_journal_paper_doi               10.1021/om900914a
_journal_volume                  29
_journal_year                    2010
_chemical_formula_moiety         'C84 H11 O11 Os3 P S2'
_chemical_formula_sum            'C84 H11 O11 Os3 P S2'
_chemical_formula_weight         1861.62
_chemical_name_systematic
;
 ?
;
_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                100.7800(10)
_cell_angle_beta                 99.9110(10)
_cell_angle_gamma                107.0880(10)
_cell_formula_units_Z            2
_cell_length_a                   13.5272(2)
_cell_length_b                   14.7670(3)
_cell_length_c                   15.3027(4)
_cell_measurement_reflns_used    15263
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.028
_cell_measurement_theta_min      2.037
_cell_volume                     2785.10(10)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'HKL Denzo and Scalepack'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_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  0.0881
_diffrn_reflns_av_sigmaI/netI    0.1366
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            24107
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.27
_exptl_absorpt_coefficient_mu    7.009
_exptl_absorpt_correction_T_max  0.5329
_exptl_absorpt_correction_T_min  0.3914
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 ?
;
_exptl_crystal_colour            brown-yellow(dark)
_exptl_crystal_density_diffrn    2.220
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1756
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.267
_refine_diff_density_min         -1.675
_refine_diff_density_rms         0.345
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    fixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     881
_refine_ls_number_reflns         9756
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.1355
_refine_ls_R_factor_gt           0.0689
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0826P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1545
_refine_ls_wR_factor_ref         0.1867
_reflns_number_gt                5791
_reflns_number_total             9756
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900914a_si_003.cif
_cod_data_source_block           9919
_cod_database_code               4067390