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_4106662
_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            'C99 H115 B2 Cl3 N10 O11 Ru2'
_chemical_formula_weight         1951.12
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_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                 94.241(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.9465(16)
_cell_length_b                   28.851(5)
_cell_length_c                   32.054(5)
_cell_measurement_reflns_used    8035
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      21.98
_cell_measurement_theta_min      2.29
_cell_volume                     10095(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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     0.71069
_diffrn_reflns_av_R_equivalents  0.0730
_diffrn_reflns_av_sigmaI/netI    0.0758
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            11639
_diffrn_reflns_theta_full        22.37
_diffrn_reflns_theta_max         22.37
_diffrn_reflns_theta_min         1.55
_exptl_absorpt_coefficient_mu    0.439
_exptl_absorpt_correction_T_max  0.987
_exptl_absorpt_correction_T_min  0.834
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.284
_exptl_crystal_description       plate
_exptl_crystal_F_000             4064
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.03
_platon_squeeze_details
;
;
_refine_diff_density_max         0.382
_refine_diff_density_min         -1.034
_refine_diff_density_rms         0.064
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.47(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1102
_refine_ls_number_reflns         11639
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0644
_refine_ls_R_factor_gt           0.0460
_refine_ls_shift/su_max          0.140
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0493P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0894
_refine_ls_wR_factor_ref         0.0948
_reflns_number_gt                9489
_reflns_number_total             11639
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja204575u_si_001.cif
_cod_data_source_block           rh063
_cod_database_code               4106662