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_4063953
_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         'C32 H48 Os P2 '
_chemical_formula_sum            'C32 H48 Os P2'
_chemical_formula_weight         684.88
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                72.2309(9)
_cell_angle_beta                 79.1741(10)
_cell_angle_gamma                75.0332(10)
_cell_formula_units_Z            1
_cell_length_a                   6.13650(10)
_cell_length_b                   9.8469(2)
_cell_length_c                   13.4415(3)
_cell_measurement_reflns_used    7945
_cell_measurement_temperature    298.1
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.1
_cell_volume                     741.96(3)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.032
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            7894
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_exptl_absorpt_coefficient_mu    4.421
_exptl_absorpt_correction_T_max  0.643
_exptl_absorpt_correction_T_min  0.345
_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    1.533
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             346.00
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.60
_refine_diff_density_min         -0.57
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     257
_refine_ls_number_reflns         3387
_refine_ls_R_factor_gt           0.0199
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0129P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0418
_reflns_number_gt                3386
_reflns_number_total             3387
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            om101060n_si_002.cif
_cod_data_source_block           '_complex9a_in_P-1'
_cod_original_formula_sum        'C32 H48 Os P2 '
_cod_database_code               4063953