C-H Bond Activation of the Methyl Group of the Supporting Ligand in an Osmium(III) Complex upon Reaction with H2O2: Formation of an Organometallic Osmium(IV) Complex
Hideki Sugimoto; Kenji Ashikari; Shinobu Itoh; Inorganic Chemistry 52 (2013) 543–545; doi:10.1021/ic302169k

data_4333604
_publ_contact_author_fax         +81-6-6879-7936
_publ_contact_author_name        'Hideki Sugimoto'
_publ_section_title
;
 C-H Bond Activation of the Methyl Group of the Supporting Ligand in an
 Osmium(III) Complex upon Reaction with H2O2: Formation of an
 Organometallic Osmium(IV) Complex
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              543
_journal_page_last               545
_journal_paper_doi               10.1021/ic302169k
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C30 H30 F6 N4 O2 Os P'
_chemical_formula_sum            'C30 H30 F6 N4 O2 Os P'
_chemical_formula_weight         813.76
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_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      62
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   11.9045(5)
_cell_length_b                   14.6137(8)
_cell_length_c                   20.9467(11)
_cell_measurement_reflns_used    22585
_cell_measurement_temperature    108
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      3.23
_cell_volume                     3644.1(3)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'CRYSTALS (Carruthers, et al., 1999)'
_computing_structure_solution    'Il Milione (Burla, et al., 2007)'
_diffrn_ambient_temperature      108
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_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
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_diffrn_reflns_limit_l_min       -27
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_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.601
_exptl_absorpt_correction_T_max  0.866
_exptl_absorpt_correction_T_min  0.435
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.483
_exptl_crystal_description       needle
_exptl_crystal_F_000             1596.00
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_refine_diff_density_min         -2.360
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_refine_ls_R_factor_gt           0.0543
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[0.0010Fo^2^ + 1.0000\s(Fo^2^)]/(4Fo^2^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1355
_reflns_number_gt                3337
_reflns_number_total             4258
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ic302169k_si_003_1.cif
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_cod_database_code               4333604