Synthesis and Properties of Oxo-carboxylato- and Dioxo-Bridged Diosmium Complexes of Tris(2-pyridylmethyl)amine
Hideki Sugimoto; Kazuhiro Kitayama; Kenji Ashikari; Chikako Matsunami; Naomi Ueda; Keisuke Umakoshi; Yuko Hosokoshi; Yoichi Sasaki; Shinobu Itoh; Inorganic Chemistry 50 (2011) 9014–9023; doi:10.1021/ic201230k

data_4326253
_publ_contact_author_email       sugimoto@mls.eng.osaka-u.ac.jp
_publ_contact_author_name        'Hideki Sugimoto'
_publ_section_title
;
 Synthesis and Properties of Oxo-carboxylato- and Dioxo-Bridged Diosmium
 Complexes of Tris(2-pyridylmethyl)amine
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9014
_journal_page_last               9023
_journal_paper_doi               10.1021/ic201230k
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C40 H42 F18 N10 O2 Os2 P3'
_chemical_formula_sum            'C40 H42 F18 N10 O2 Os2 P3'
_chemical_formula_weight         1510.13
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 113.0153(8)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   21.7247(6)
_cell_length_b                   11.6280(3)
_cell_length_c                   20.8290(5)
_cell_measurement_reflns_used    20655
_cell_measurement_temperature    98
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.19
_cell_volume                     4842.9(2)
_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      98
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0298
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            22668
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.457
_exptl_absorpt_correction_T_max  0.721
_exptl_absorpt_correction_T_min  0.576
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.071
_exptl_crystal_description       block
_exptl_crystal_F_000             2908.00
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.060
_refine_diff_density_max         1.360
_refine_diff_density_min         -0.690
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     361
_refine_ls_number_reflns         5522
_refine_ls_R_factor_gt           0.0179
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[0.0002Fo^2^ + 1.0000\s(Fo^2^)]/(4Fo^2^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0454
_reflns_number_gt                5171
_reflns_number_total             5522
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ic201230k_si_002_1.cif
_cod_data_source_block           5
_cod_database_code               4326253