Electronic Structure Investigations of Neutral and Charged Ruthenium Bis(β-diketonate) Complexes of Redox-Active Verdazyl Radicals
Stephen D. J. McKinnon; Brian O. Patrick; A. B. P. Lever; Robin G. Hicks; Journal of the American Chemical Society 133 (2011) 13587–13603; doi:10.1021/ja204575u

data_4106663
_publ_section_title
;
 Electronic Structure Investigations of Neutral and Charged Ruthenium
 Bis(\b-diketonate) Complexes of Redox-Active Verdazyl Radicals
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13587
_journal_page_last               13603
_journal_paper_doi               10.1021/ja204575u
_journal_volume                  133
_journal_year                    2011
_chemical_formula_sum            'C23 H20 B F16 N5 O5 Ru'
_chemical_formula_weight         862.32
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                96.479(8)
_cell_angle_beta                 103.164(7)
_cell_angle_gamma                90.168(7)
_cell_formula_units_Z            4
_cell_length_a                   9.8754(14)
_cell_length_b                   18.263(3)
_cell_length_c                   18.489(3)
_cell_measurement_reflns_used    9655
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.81
_cell_measurement_theta_min      2.25
_cell_volume                     3224.8(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker X8 APEX II'
_diffrn_measurement_method       'area detector'
_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  0.0430
_diffrn_reflns_av_sigmaI/netI    0.0467
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            28136
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.12
_exptl_absorpt_coefficient_mu    0.621
_exptl_absorpt_correction_T_max  0.872
_exptl_absorpt_correction_T_min  0.756
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.776
_exptl_crystal_description       rod
_exptl_crystal_F_000             1704
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.991
_refine_diff_density_min         -0.594
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1007
_refine_ls_number_reflns         28136
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0617
_refine_ls_R_factor_gt           0.0435
_refine_ls_shift/su_max          0.035
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0587P)^2^+2.9392P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1104
_refine_ls_wR_factor_ref         0.1248
_reflns_number_gt                22635
_reflns_number_total             28136
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja204575u_si_002.cif
_cod_data_source_block           rh058
_cod_original_cell_volume        3224.8(8)
_cod_database_code               4106663