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_4106664
_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            'C33 H30 Co F12 N5 O5 Ru'
_chemical_formula_weight         964.62
_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                80.4750(10)
_cell_angle_beta                 87.4290(10)
_cell_angle_gamma                83.0430(10)
_cell_formula_units_Z            2
_cell_length_a                   10.6135(3)
_cell_length_b                   12.8879(4)
_cell_length_c                   14.7751(4)
_cell_measurement_reflns_used    9992
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.82
_cell_measurement_theta_min      2.36
_cell_volume                     1977.85(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_method       'area detector'
_diffrn_radiation_monochromator  'Bruker X8 APEX II'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0204
_diffrn_reflns_av_sigmaI/netI    0.0213
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            31694
_diffrn_reflns_theta_full        27.90
_diffrn_reflns_theta_max         27.90
_diffrn_reflns_theta_min         2.30
_exptl_absorpt_coefficient_mu    0.903
_exptl_absorpt_correction_T_max  0.835
_exptl_absorpt_correction_T_min  0.758
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.620
_exptl_crystal_description       prism
_exptl_crystal_F_000             964
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.642
_refine_diff_density_min         -0.368
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     622
_refine_ls_number_reflns         9385
_refine_ls_number_restraints     121
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.0456
_refine_ls_R_factor_gt           0.0330
_refine_ls_shift/su_max          0.075
_refine_ls_shift/su_mean         0.024
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0590P)^2^+0.4827P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0935
_refine_ls_wR_factor_ref         0.1056
_reflns_number_gt                7724
_reflns_number_total             9385
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja204575u_si_003.cif
_cod_data_source_block           ael102
_cod_database_code               4106664