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_4063954
_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         'C34 H50 O Os P2 '
_chemical_formula_sum            'C34 H50 O Os P2'
_chemical_formula_weight         726.92
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_cell_angle_alpha                90.0000
_cell_angle_beta                 109.9417(16)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   12.1843(9)
_cell_length_b                   20.2214(15)
_cell_length_c                   13.8982(10)
_cell_measurement_reflns_used    27285
_cell_measurement_temperature    298.1
_cell_measurement_theta_max      28.2
_cell_measurement_theta_min      3.0
_cell_volume                     3219.0(4)
_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  0.081
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            32372
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_exptl_absorpt_coefficient_mu    4.083
_exptl_absorpt_correction_T_max  0.665
_exptl_absorpt_correction_T_min  0.248
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.500
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1472.00
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.00
_refine_diff_density_min         -1.21
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_parameters     368
_refine_ls_number_reflns         7371
_refine_ls_R_factor_gt           0.0472
_refine_ls_shift/su_max          0.0030
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0338P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0967
_reflns_number_gt                5623
_reflns_number_total             7371
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            om101060n_si_002.cif
_cod_data_source_block           '_complex10_in_P21/a'
_cod_original_formula_sum        'C34 H50 O Os P2 '
_cod_database_code               4063954