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_4326255
_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         'C47 H47 F18 N10 O3 Os2 P3 '
_chemical_formula_sum            'C47 H47 F18 N10 O3 Os2 P3'
_chemical_formula_weight         1615.25
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_cell_angle_alpha                90.0000
_cell_angle_beta                 100.4270(10)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   12.0808(12)
_cell_length_b                   19.3190(18)
_cell_length_c                   23.521(2)
_cell_measurement_reflns_used    16369
_cell_measurement_temperature    113.1
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.1
_cell_volume                     5398.9(9)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.8'
_computing_structure_refinement  SHELXL
_computing_structure_solution    SIR2002
_diffrn_ambient_temperature      113
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.045
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            39226
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_exptl_absorpt_coefficient_mu    4.903
_exptl_absorpt_correction_T_max  0.394
_exptl_absorpt_correction_T_min  0.263
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.987
_exptl_crystal_description       prism
_exptl_crystal_F_000             3128.00
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.19
_refine_diff_density_max         4.39
_refine_diff_density_min         -1.61
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.656
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     749
_refine_ls_number_reflns         12192
_refine_ls_R_factor_gt           0.0365
_refine_ls_shift/su_max          0.0030
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1568
_reflns_number_gt                10587
_reflns_number_total             12192
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ic201230k_si_002_3.cif
_cod_data_source_block           '__3'
_cod_original_formula_sum        'C47 H47 F18 N10 O3 Os2 P3 '
_cod_database_code               4326255