Synthesis and Characterization of an Azido-Bridged Dinuclear Ruthenium(II) Polypyridylamine Complex Forming a Mixed-Valence State
Misaki Makino; Tomoya Ishizuka; Shingo Ohzu; Jiang Hua; Hiroaki Kotani; Takahiko Kojima; Inorganic Chemistry 52 (2013) 5507–5514; doi:10.1021/ic400412f

data_4334759
_publ_section_title
;
 Synthesis and Characterization of an Azido-Bridged Dinuclear
 Ruthenium(II) Polypyridylamine Complex Forming a Mixed-Valence State
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5507
_journal_page_last               5514
_journal_paper_doi               10.1021/ic400412f
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C46 H42 F18 N13 P3 Ru2'
_chemical_formula_weight         1413.98
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           24
_symmetry_space_group_name_Hall  'I 2b 2c'
_symmetry_space_group_name_H-M   'I 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.914(4)
_cell_length_b                   13.120(4)
_cell_length_c                   39.995(13)
_cell_measurement_temperature    120(2)
_cell_volume                     6776(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0689
_diffrn_reflns_av_sigmaI/netI    0.0944
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            17379
_diffrn_reflns_theta_full        26.33
_diffrn_reflns_theta_max         26.33
_diffrn_reflns_theta_min         1.63
_exptl_absorpt_coefficient_mu    0.605
_exptl_absorpt_correction_T_max  0.9762
_exptl_absorpt_correction_T_min  0.9094
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'
_exptl_crystal_density_diffrn    1.386
_exptl_crystal_F_000             2816
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.110
_refine_diff_density_min         -1.246
_refine_diff_density_rms         0.145
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.17(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     372
_refine_ls_number_reflns         6864
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.1180
_refine_ls_R_factor_gt           0.0988
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1307P)^2^+54.7420P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2474
_refine_ls_wR_factor_ref         0.2594
_reflns_number_gt                5222
_reflns_number_total             6864
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400412f_uN3.cif
_cod_data_source_block           makino13
_cod_database_code               4334759