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_4334757
_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            'C25 H24 F12 N6 P2 Ru'
_chemical_formula_weight         799.51
_space_group_IT_number           2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                89.976(2)
_cell_angle_beta                 89.898(3)
_cell_angle_gamma                89.418(2)
_cell_formula_units_Z            4
_cell_length_a                   12.529(2)
_cell_length_b                   12.734(2)
_cell_length_c                   18.789(3)
_cell_measurement_temperature    120(2)
_cell_volume                     2997.5(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_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  0.0555
_diffrn_reflns_av_sigmaI/netI    0.1840
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            16155
_diffrn_reflns_theta_full        26.55
_diffrn_reflns_theta_max         26.55
_diffrn_reflns_theta_min         1.08
_exptl_absorpt_coefficient_mu    0.734
_exptl_absorpt_correction_T_max  0.9302
_exptl_absorpt_correction_T_min  0.8378
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'
_exptl_crystal_density_diffrn    1.772
_exptl_crystal_F_000             1592
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.852
_refine_diff_density_min         -0.738
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.949
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     831
_refine_ls_number_reflns         12077
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.949
_refine_ls_R_factor_all          0.1648
_refine_ls_R_factor_gt           0.0669
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0449P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1161
_refine_ls_wR_factor_ref         0.1489
_reflns_number_gt                6076
_reflns_number_total             12077
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400412f_NCCH3.cif
_cod_data_source_block           oz2
_cod_original_cell_volume        2997.4(8)
_cod_database_code               4334757