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_4326256
_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         'C43 H49 F24 N8 O4 Os2 P4'
_chemical_formula_sum            'C43 H49 F24 N8 O4 Os2 P4'
_chemical_formula_weight         1702.17
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 91.838(4)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   19.587(7)
_cell_length_b                   12.304(5)
_cell_length_c                   23.333(8)
_cell_measurement_reflns_used    14720
_cell_measurement_temperature    113
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.10
_cell_volume                     5620(4)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2002 (Burla, et al., 2003)'
_diffrn_ambient_temperature      113
_diffrn_detector_area_resol_mean 7.314
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Rigaku Mercury70'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.1198
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            39301
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.56
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.758
_exptl_absorpt_correction_T_max  0.867
_exptl_absorpt_correction_T_min  0.457
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.012
_exptl_crystal_description       prism
_exptl_crystal_F_000             3292.00
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.030
_refine_diff_density_max         4.130
_refine_diff_density_min         -2.270
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.787
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     766
_refine_ls_number_reflns         12703
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0648
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0774P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1611
_reflns_number_gt                8408
_reflns_number_total             12703
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ic201230k_si_002_4.cif
_cod_data_source_block           '_4'
_cod_database_code               4326256