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_4334756
_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            'C23 H21 F6 N8 P Ru'
_chemical_formula_weight         655.52
_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                73.8770(10)
_cell_angle_beta                 89.4520(10)
_cell_angle_gamma                84.8560(10)
_cell_formula_units_Z            4
_cell_length_a                   13.4461(13)
_cell_length_b                   14.5506(14)
_cell_length_c                   16.7938(16)
_cell_measurement_temperature    120(2)
_cell_volume                     3143.3(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.930
_diffrn_measured_fraction_theta_max 0.930
_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  0.0228
_diffrn_reflns_av_sigmaI/netI    0.0611
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            17868
_diffrn_reflns_theta_full        27.60
_diffrn_reflns_theta_max         27.60
_diffrn_reflns_theta_min         1.26
_exptl_absorpt_coefficient_mu    0.610
_exptl_absorpt_correction_T_max  0.9585
_exptl_absorpt_correction_T_min  0.8724
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'
_exptl_crystal_density_diffrn    1.385
_exptl_crystal_F_000             1312
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.834
_refine_diff_density_min         -0.619
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     721
_refine_ls_number_reflns         13576
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0654
_refine_ls_R_factor_gt           0.0464
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0534P)^2^+1.2369P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1077
_refine_ls_wR_factor_ref         0.1147
_reflns_number_gt                10000
_reflns_number_total             13576
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400412f_N3.cif
_cod_data_source_block           makino17
_cod_database_code               4334756