Observation of Redox-Induced Electron Transfer and Spin Crossover for Dinuclear Cobalt and Iron Complexes with the 2,5-Di-tert-butyl-3,6-dihydroxy-1,4-benzoquinonate Bridging Ligand
Kil Sik Min; Antonio G. DiPasquale; Arnold L. Rheingold; Henry S. White; Joel S. Miller; Journal of the American Chemical Society 131 (2009) 6229–6236; doi:10.1021/ja900909u

data_4104312
_publ_section_title
;
 Observation of Redox-Induced Electron Transfer and Spin Crossover for
 Dinuclear Cobalt and Iron Complexes with the
 2,5-Di-tert-butyl-3,6-dihydroxy-1,4-benzoquinonate Bridging Ligand
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6229
_journal_page_last               6236
_journal_paper_doi               10.1021/ja900909u
_journal_volume                  131
_journal_year                    2009
_chemical_formula_sum            'C56 H63 B4 Co2 F16 N14 O4'
_chemical_formula_weight         1461.30
_chemical_name_common            KS-127-03A
_chemical_name_systematic
;
 ?
;
_space_group.centring_type       P
_space_group_IT_number           14
_space_group.IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 109.888(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.953(3)
_cell_length_b                   19.739(3)
_cell_length_c                   19.190(3)
_cell_measurement_reflns_used    8015
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.09
_cell_measurement_theta_min      2.26
_cell_volume                     6394.9(18)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    ORTEP-32
_computing_publication_material  WinGX
_computing_structure_refinement  SHELXL-97
_computing_structure_solution    SIR-2004
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0585
_diffrn_reflns_av_sigmaI/netI    0.0622
_diffrn_refln_scan_rate          30
_diffrn_refln_scan_width         0.5
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            44852
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.06
_exptl_absorpt_coefficient_mu    0.623
_exptl_absorpt_correction_T_max  0.9577
_exptl_absorpt_correction_T_min  0.9124
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.518
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2988
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.07
_platon_squeeze_details
;
 SQUEEZE (PLATON, A.Spek) was used to treat diffuse solvent
 and anion contributions.  Total electron count found = 942/unit cell.
 Calculated for 12 acetonitrile (the re'xtal solvent) and 16 BF4- anions
 = 912/unit cell.  The intensive properties (density, F(000), etc.)
 reflect these contributions.
;
_refine_diff_density_max         1.241
_refine_diff_density_min         -0.581
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     583
_refine_ls_number_reflns         11307
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.1047
_refine_ls_R_factor_gt           0.0778
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1089P)^2^+3.9926P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1916
_refine_ls_wR_factor_ref         0.2041
_reflns_number_gt                7796
_reflns_number_total             11307
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja900909u_si_003.cif
_cod_data_source_block           jsm130
_cod_depositor_comments
;
The following automatic conversions were performed:

'_space_group.centring_type' value 'primitive' was replaced with the
value 'P' as specified in the replacement file
'/home/antanas/src/cod-tools/trunk/data/replacement-values/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 5642 2017-10-24 12:04:52Z antanas 
;
_cod_original_cell_volume        6394.9(16)
_cod_database_code               4104312