Redox Activity and Two-Step Valence Tautomerism in a Family of Dinuclear Cobalt Complexes with a Spiroconjugated Bis(dioxolene) Ligand
Kerwyn G. Alley; Giordano Poneti; Peter S. D. Robinson; Ayman Nafady; Boujemaa Moubaraki; Jade B. Aitken; Simon C. Drew; Chris Ritchie; Brendan F. Abrahams; Rosalie K. Hocking; Keith S. Murray; Alan M. Bond; Hugh H. Harris; Lorenzo Sorace; Colette Boskovic; Journal of the American Chemical Society 135 (2013) 8304–8323; doi:10.1021/ja4021155

data_4119833
_publ_section_title
;
 Redox Activity and Two-Step Valence Tautomerism in a Family of Dinuclear
 Cobalt Complexes with a Spiroconjugated Bis(dioxolene) Ligand
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8304
_journal_page_last               8323
_journal_paper_doi               10.1021/ja4021155
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'C69 H80 Co2 F24 N8 O8 P4'
_chemical_formula_weight         1847.15
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   22.8044(9)
_cell_length_b                   41.7897(11)
_cell_length_c                   17.9753(9)
_cell_measurement_reflns_used    8078
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      75.4699
_cell_measurement_theta_min      3.1703
_cell_volume                     17130.3(12)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) x-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0999
_diffrn_reflns_av_sigmaI/netI    0.0958
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            36733
_diffrn_reflns_theta_full        59.99
_diffrn_reflns_theta_max         59.99
_diffrn_reflns_theta_min         3.30
_exptl_absorpt_coefficient_mu    4.686
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.39926
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.432
_exptl_crystal_description       'rectangular plate'
_exptl_crystal_F_000             7552
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.211
_exptl_crystal_size_min          0.023
_platon_squeeze_details
;
;
_refine_diff_density_max         0.816
_refine_diff_density_min         -0.644
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.986
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     851
_refine_ls_number_reflns         12700
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.986
_refine_ls_R_factor_all          0.1545
_refine_ls_R_factor_gt           0.1114
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1967P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3037
_refine_ls_wR_factor_ref         0.3312
_reflns_number_gt                6493
_reflns_number_total             12700
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja4021155_si_002_3.cif
_cod_data_source_block           compound6b
_cod_database_code               4119833