Preparation of Osmium η5-Phospholide Complexes and Their Reactions with Acyl Electrophiles: C═O Bond Cleavage and C−C Bond Formation within the Metal Coordination Sphere
Ogasawara, Masamichi; Shintani, Minoru; Watanabe, Susumu; Sakamoto, Takeshi; Nakajima, Kiyohiko; Takahashi, Tamotsu; Organometallics 30 (2011) 1487–; doi:10.1021/om101060n

data_4063955
_publ_section_title
;
 Preparation of Osmium \h5-Phospholide Complexes and Their Reactions with
 Acyl Electrophiles: C&#x2550;O Bond Cleavage and C&#x2212;C Bond
 Formation within the Metal Coordination Sphere
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              1487
_journal_paper_doi               10.1021/om101060n
_journal_volume                  30
_journal_year                    2011
_chemical_formula_moiety         'C36 H52 O2 Os P2 '
_chemical_formula_sum            'C36 H52 O2 Os P2'
_chemical_formula_weight         768.95
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_cell_angle_alpha                90.0000
_cell_angle_beta                 102.9210(7)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   10.7091(2)
_cell_length_b                   25.2803(5)
_cell_length_c                   12.6928(2)
_cell_measurement_reflns_used    29714
_cell_measurement_temperature    298.1
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.1
_cell_volume                     3349.30(11)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.8'
_computing_structure_refinement  SHELXL
_computing_structure_solution    SIR2004
_diffrn_ambient_temperature      298
_diffrn_detector_area_resol_mean 6.85
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku SCXmini'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.082
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            33784
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_exptl_absorpt_coefficient_mu    3.931
_exptl_absorpt_correction_T_max  0.675
_exptl_absorpt_correction_T_min  0.346
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
    Higashi, T. (1999). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.525
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1560.00
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.77
_refine_diff_density_min         -1.01
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_parameters     391
_refine_ls_number_reflns         7676
_refine_ls_R_factor_gt           0.0457
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0353P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0962
_reflns_number_gt                5778
_reflns_number_total             7676
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            om101060n_si_002.cif
_cod_data_source_block           '_complex12_in_P21/c'
_cod_original_formula_sum        'C36 H52 O2 Os P2 '
_cod_database_code               4063955