Binuclear Ruthenium Complexes of a Neutral Radical Bridging Ligand. A New "Spin" on Mixed Valency
Stephen D. J. McKinnon; Brian O. Patrick; A. B. P. Lever; Robin G. Hicks; Inorganic Chemistry 52 (2013) 8053–8066; doi:10.1021/ic400704j

data_4335465
_publ_section_title
;
 Binuclear Ruthenium Complexes of a Neutral Radical Bridging Ligand. A New
 "Spin" on Mixed Valency
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8053
_journal_page_last               8066
_journal_paper_doi               10.1021/ic400704j
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C34 H25 F24.01 N6 O9 Ru2, C10 H10 Co'
_chemical_formula_sum            'C50 H49 Co F24 N6 O9 Ru2'
_chemical_formula_weight         1595.02
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2013-06-02
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:59:47, GUI svn.r4466)
;
_cell_angle_alpha                90
_cell_angle_beta                 102.025(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.2706(9)
_cell_length_b                   23.2010(17)
_cell_length_c                   17.8901(13)
_cell_measurement_reflns_used    3121
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      20.38
_cell_measurement_theta_min      2.28
_cell_volume                     5793.3(7)
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.728
_diffrn_measured_fraction_theta_max 0.995
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.1085
_diffrn_reflns_Laue_measured_fraction_full 0.728
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.728
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         22.598
_diffrn_reflns_theta_min         1.458
_exptl_absorpt_coefficient_mu    0.935
_exptl_absorpt_correction_T_max  0.954
_exptl_absorpt_correction_T_min  0.788
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2008)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.829
_exptl_crystal_description       plate
_exptl_crystal_F_000             3176
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.703
_refine_diff_density_min         -0.560
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.968
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     883
_refine_ls_number_reflns         7636
_refine_ls_number_restraints     1487
_refine_ls_restrained_S_all      0.894
_refine_ls_R_factor_all          0.1113
_refine_ls_R_factor_gt           0.0506
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0740P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1183
_refine_ls_wR_factor_ref         0.1384
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4415
_reflns_number_total             7636
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic400704j_si_002.cif
_cod_data_source_block           rh072_0m
_cod_database_code               4335465
_cod_database_fobs_code          4335465
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C21-F1 \\sim C21-F2 \\sim C21-F3
 with sigma of 0.01
 F1-F2 \\sim F2-F3 \\sim F3-F1 \\sim F4-F5 \\sim F5-F6 \\sim F6-F4
 with sigma of 0.01
 F7-F8 \\sim F8-F9 \\sim F9-F7 \\sim F10-F11 \\sim F11-F12 \\sim F12-F10
 with sigma of 0.01
 F13-F14 \\sim F14-F15 \\sim F15-F13 \\sim F16-F17 \\sim F17-F18 \\sim F18-F16
 with sigma of 0.01
 F19-F20 \\sim F20-F21 \\sim F21-F19 \\sim F22-F23 \\sim F23-F24 \\sim F24-F22
 with sigma of 0.01
 F19-F20 \\sim F19B-F20B \\sim F20B-F21B \\sim F21B-F19B \\sim F21C-F20C
 \\sim F20C-F20C \\sim F20C-F21C
 with sigma of 0.01
 C51-F19 \\sim C51-F19B \\sim C51-F20 \\sim C51-F20B \\sim C51-F21
 \\sim C51-F21B
 with sigma of 0.01
 C41-F13 \\sim C41-F13C \\sim C41-F14C \\sim C41-F15C
 with sigma of 0.01
 F13C-F14C \\sim F14C-F15C \\sim F15C-F13C
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08
All non-hydrogen atoms restrained to be isotropic: with sigma of 0.1 and sigma 
for terminal atoms of 0.2
Uanis(F19B) = Uanis(F21)
Uanis(F13C) = Uanis(F14B)
4. others
 1*[Sof(F19)+Sof(F20)+Sof(F21)]+1*[Sof(F19B)+Sof(F20B)+Sof(F21B)]+1*[Sof(F21C)+
 Sof(F20C)+Sof(F19C)]=1 with esd of 0.001
 1*[Sof(F13)+Sof(F14)+Sof(F15)]+1*[Sof(F13B)+Sof(F14B)+Sof(F15B)]+1*[Sof(F13C)+
 Sof(F14C)+Sof(F15C)]=1 with esd of 0.001
 Sof(F19)=Sof(F20)=Sof(F21)=FVAR(1)
 Sof(F19B)=Sof(F20B)=Sof(F21B)=FVAR(2)
 Sof(F21C)=Sof(F20C)=Sof(F19C)=FVAR(3)
 Sof(F13)=Sof(F14)=Sof(F15)=FVAR(4)
 Sof(F13B)=Sof(F14B)=Sof(F15B)=FVAR(5)
 Sof(F13C)=Sof(F14C)=Sof(F15C)=FVAR(6)
5.a Ternary CH refined with riding coordinates:
 C3(H3), C6(H6)
5.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C23(H23), C33(H33), C43(H43), C53(H53), C56(H56), C57(H57),
 C58(H58), C59(H59), C60(H60), C61(H61), C62(H62), C63(H63), C64(H64), C65(H65)
5.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C15(H15A,
 H15B,H15C), C16(H16A,H16B,H16C)
;
_shelxl_version_number           2012-9