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_4067389
_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         'C82.5 H11 O10 Os3 P S'
_chemical_formula_sum            'C82.5 H11 O10 Os3 P S'
_chemical_formula_weight         1795.54
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           85
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4a'
_symmetry_space_group_name_H-M   'P 4/n :2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   29.0200(4)
_cell_length_b                   29.0200(4)
_cell_length_c                   14.4970(2)
_cell_measurement_reflns_used    80593
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      25.028
_cell_measurement_theta_min      2.037
_cell_volume                     12208.8(3)
_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      200(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.1048
_diffrn_reflns_av_sigmaI/netI    0.0768
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            71893
_diffrn_reflns_theta_full        25.04
_diffrn_reflns_theta_max         25.04
_diffrn_reflns_theta_min         2.11
_exptl_absorpt_coefficient_mu    6.358
_exptl_absorpt_correction_T_max  0.5887
_exptl_absorpt_correction_T_min  0.3376
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 ?
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.954
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             6760
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.894
_refine_diff_density_min         -2.574
_refine_diff_density_rms         0.402
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    fixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     874
_refine_ls_number_reflns         10808
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0970
_refine_ls_R_factor_gt           0.0614
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1142P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1724
_refine_ls_wR_factor_ref         0.1904
_reflns_number_gt                7703
_reflns_number_total             10808
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900914a_si_002.cif
_cod_data_source_block           9834a
_cod_depositor_comments
;

2021-08-27
Formula fixed to be consistent with given Z
                 miguel
;
_cod_original_formula_sum            'C165 H22 O20 Os6 P2 S2'
_cod_original_formula_weight         3591.09
_cod_original_formula_moiety         'C165 H22 O20 Os6 P2 S2'
_cod_original_sg_symbol_H-M      'P 4/n'
_cod_database_code               4067389