Tuneable reversible redox of cobalt(iii) carbazole complexes.
Bennington, Michael S.; Feltham, Humphrey L. C.; Buxton, Zoë J; White, Nicholas G.; Brooker, Sally; Dalton transactions (Cambridge, England : 2003) 46 (2017) 4696–4710; doi:10.1039/c7dt00295e

data_7042363
_publ_section_title
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 Tuneable reversible redox of cobalt(iii) carbazole complexes.
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_journal_issue                   14
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4696
_journal_page_last               4710
_journal_paper_doi               10.1039/c7dt00295e
_journal_volume                  46
_journal_year                    2017
_chemical_compound_source        synthesized
_chemical_formula_moiety         'C76 H76 Co1 N14, B F4'
_chemical_formula_sum            'C76 H76 B Co F4 N14'
_chemical_formula_weight         1331.27
_space_group_IT_number           85
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4a'
_symmetry_space_group_name_H-M   'P 4/n :2'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_update_record
;
2016-10-17 deposited with the CCDC.
2017-03-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.32274(18)
_cell_length_b                   16.32274(18)
_cell_length_c                   13.22212(18)
_cell_measurement_reflns_used    11029
_cell_measurement_temperature    100
_cell_measurement_theta_max      76.2
_cell_measurement_theta_min      5.08
_cell_volume                     3522.79(7)
_computing_cell_refinement       'CrysAlisPro, (Agilent, 2011)'
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_data_reduction        'CrysAlisPro, (Agilent, 2011)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.052
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            19255
_diffrn_reflns_theta_full        74.699
_diffrn_reflns_theta_max         76.224
_diffrn_reflns_theta_min         3.342
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.426
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.63
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlisPro, (Agilent, 2011)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.255
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1396
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.35
_refine_diff_density_max         1.44
_refine_diff_density_min         -1.09
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0276
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     237
_refine_ls_number_reflns         3664
_refine_ls_number_restraints     94
_refine_ls_R_factor_all          0.0673
_refine_ls_R_factor_gt           0.0619
_refine_ls_shift/su_max          0.0001658
_refine_ls_shift/su_mean         0.0000220
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 0.436E+04 0.730E+04 0.494E+04 0.235E+04 714. 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1809
_refine_ls_wR_factor_gt          0.1725
_refine_ls_wR_factor_ref         0.1809
_reflns_limit_h_max              14
_reflns_limit_h_min              -13
_reflns_limit_k_max              20
_reflns_limit_k_min              0
_reflns_limit_l_max              16
_reflns_limit_l_min              0
_reflns_number_gt                3191
_reflns_number_total             3681
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.14
_oxford_diffrn_Wilson_scale      0.06
_oxford_refine_ls_r_factor_ref   0.0673
_oxford_refine_ls_scale          4.52(15)
_oxford_reflns_number_all        3664
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_cod_data_source_file            c7dt00295e2.cif
_cod_data_source_block           NGW201317_compound1
_cod_depositor_comments
'Adding full bibliography for 7042363--7042366.cif.'
_cod_original_cell_volume        3522.79(5)
_cod_original_sg_symbol_H-M      'P 4/n '
_cod_original_formula_sum        'C76 H76 B1 Co1 F4 N14'
_cod_database_code               7042363
_iucr_refine_instructions_details_constraints
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BLOCK SCALE X'S  U'S 
SUMFIX ELEMENT SCALES 
RIDE C   (   1,X'S) H   (  11,X'S) 
RIDE C   (   2,X'S) H   (  21,X'S) 
RIDE C   (   3,X'S) H   (  31,X'S) 
RIDE C   (   4,X'S) H   (  41,X'S) 
RIDE C   (   5,X'S) H   (  51,X'S) 
RIDE C   (   7,X'S) H   (  72,X'S) H   (  71,X'S) 
RIDE C   (  11,X'S) H   ( 111,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) 
RIDE C   (  21,X'S) H   ( 213,X'S) H   ( 211,X'S) H   ( 212,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) H   ( 223,X'S) H   ( 222,X'S) 
RIDE C   (  23,X'S) H   ( 232,X'S) H   ( 231,X'S) H   ( 233,X'S) 
END    
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_iucr_refine_instructions_details_restraints
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DIST 1.40, 0.01 = B(1) TO F(11), B(1) TO F(12) 
CONT B(2) TO F(21), B(2) TO F(22) 
ANGL 109, 1 = F(11) TO B(1) TO F(12) 
CONT F(21) TO B(2) TO F(22) 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
REM   THERMSIM   START (DO NOT REMOVE THIS LINE) 
U(IJ) .0, 0.04000 = B(1) TO F(12,2) 
U(IJ) .0, 0.04000 = B(1) TO F(12,4) 
U(IJ) .0, 0.04000 = B(1) TO F(12,3) 
U(IJ) .0, 0.04000 = B(1) TO F(11) 
U(IJ) .0, 0.04000 = B(1) TO F(12) 
U(IJ) .0, 0.04000 = F(11) TO F(21,3,1,0,0,1) 
U(IJ) .0, 0.04000 = F(21) TO B(2) 
U(IJ) .0, 0.04000 = B(2) TO F(22,3) 
U(IJ) .0, 0.04000 = B(2) TO F(22,2) 
U(IJ) .0, 0.04000 = B(2) TO F(22,4) 
U(IJ) .0, 0.04000 = B(2) TO F(22) 
REM   THERMSIM   END (DO NOT REMOVE THIS LINE) 
REM   DELU   START (DO NOT REMOVE THIS LINE) 
VIBR .0, 0.00200 = B(1) TO F(12,2) 
VIBR .0, 0.00200 = B(1) TO F(12,4) 
VIBR .0, 0.00200 = B(1) TO F(12,3) 
VIBR .0, 0.00200 = B(1) TO F(11) 
VIBR .0, 0.00200 = B(1) TO F(12) 
VIBR .0, 0.00500 = F(12,4) TO F(12,2) 
VIBR .0, 0.00500 = F(12,3) TO F(12,2) 
VIBR .0, 0.00500 = F(12,3) TO F(12,4) 
VIBR .0, 0.00500 = F(11) TO F(12,2) 
VIBR .0, 0.00500 = F(11) TO F(12,4) 
VIBR .0, 0.00500 = F(11) TO F(12,3) 
VIBR .0, 0.00500 = F(12) TO F(12,2) 
VIBR .0, 0.00500 = F(12) TO F(12,4) 
VIBR .0, 0.00500 = F(12) TO F(12,3) 
VIBR .0, 0.00500 = F(12) TO F(11) 
VIBR .0, 0.00200 = F(11) TO F(21,3,1,0,0,1) 
VIBR .0, 0.00500 = B(1) TO F(21,3,1,0,0,1) 
VIBR .0, 0.00200 = F(21) TO B(2) 
VIBR .0, 0.00500 = B(2) TO F(11,1,1,0,0,-1) 
VIBR .0, 0.00200 = B(2) TO F(22,3) 
VIBR .0, 0.00200 = B(2) TO F(22,2) 
VIBR .0, 0.00200 = B(2) TO F(22,4) 
VIBR .0, 0.00200 = B(2) TO F(22) 
VIBR .0, 0.00500 = F(22,3) TO F(21) 
VIBR .0, 0.00500 = F(22,2) TO F(21) 
VIBR .0, 0.00500 = F(22,2) TO F(22,3) 
VIBR .0, 0.00500 = F(22,4) TO F(21) 
VIBR .0, 0.00500 = F(22,4) TO F(22,3) 
VIBR .0, 0.00500 = F(22,4) TO F(22,2) 
VIBR .0, 0.00500 = F(22) TO F(21) 
VIBR .0, 0.00500 = F(22) TO F(22,3) 
VIBR .0, 0.00500 = F(22) TO F(22,2) 
VIBR .0, 0.00500 = F(22) TO F(22,4) 
REM   DELU   END (DO NOT REMOVE THIS LINE) 
END                                                                             
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