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_7042365
_publ_section_title
;
 Tuneable reversible redox of cobalt(iii) carbazole complexes.
;
_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
'C60 H44 Co N14, B F4, 0.5(C3 H7 N O), 0.5(H2 O) '
_chemical_formula_sum            'C61.5 H48.5 B Co F4 N14.5 O'
_chemical_formula_weight         1152.40
_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   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                 107.976(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.3437(3)
_cell_length_b                   24.7996(4)
_cell_length_c                   26.5881(5)
_cell_measurement_reflns_used    51951
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.5
_cell_measurement_theta_min      3.21
_cell_volume                     10877.8(4)
_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    'SHELXS 97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.912
_diffrn_measurement_device       Serial
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.029
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            175733
_diffrn_reflns_theta_full        25.286
_diffrn_reflns_theta_max         29.748
_diffrn_reflns_theta_min         2.867
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.388
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALE3 ABSPACK'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.407
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4760
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.02
_refine_diff_density_min         -0.67
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9564
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1501
_refine_ls_number_reflns         27139
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0696
_refine_ls_R_factor_gt           0.0582
_refine_ls_shift/su_max          0.0024461
_refine_ls_shift/su_mean         0.0000470
_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: 
 0.143E+04 0.235E+04 0.141E+04 556. 116. 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1517
_refine_ls_wR_factor_gt          0.1409
_refine_ls_wR_factor_ref         0.1516
_reflns_limit_h_max              22
_reflns_limit_h_min              -24
_reflns_limit_k_max              34
_reflns_limit_k_min              0
_reflns_limit_l_max              36
_reflns_limit_l_min              0
_reflns_number_gt                23001
_reflns_number_total             28282
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.54
_oxford_diffrn_Wilson_scale      0.74
_oxford_refine_ls_r_factor_ref   0.0695
_oxford_refine_ls_scale          1.210(3)
_oxford_reflns_number_all        27154
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_iucr_refine_instructions_details_constraints
;
BLOCK 
CONT SCALE 
CONT C    (  101 ,X'S,U'S)  UNTIL F    (   23 ) 
CONT H    ( 2112 ,X'S)  UNTIL H    ( 2111 ) 
RIDE C   ( 101,X'S) H   (1011,X'S) 
RIDE C   ( 102,X'S) H   (1021,X'S) 
RIDE C   ( 103,X'S) H   (1031,X'S) 
RIDE C   ( 104,X'S) H   (1041,X'S) 
RIDE C   ( 105,X'S) H   (1051,X'S) 
RIDE C   ( 107,X'S) H   (1071,X'S) H   (1072,X'S) 
RIDE C   ( 111,X'S) H   (1111,X'S) 
RIDE C   ( 114,X'S) H   (1141,X'S) 
RIDE C   ( 115,X'S) H   (1151,X'S) 
RIDE C   ( 116,X'S) H   (1161,X'S) 
RIDE C   ( 122,X'S) H   (1221,X'S) 
RIDE C   ( 123,X'S) H   (1231,X'S) 
RIDE C   ( 124,X'S) H   (1241,X'S) 
RIDE C   ( 127,X'S) H   (1271,X'S) 
RIDE C   ( 131,X'S) H   (1311,X'S) H   (1312,X'S) 
RIDE C   ( 133,X'S) H   (1331,X'S) 
RIDE C   ( 134,X'S) H   (1341,X'S) 
RIDE C   ( 135,X'S) H   (1351,X'S) 
RIDE C   ( 136,X'S) H   (1361,X'S) 
RIDE C   ( 137,X'S) H   (1371,X'S) 
RIDE C   ( 151,X'S) H   (1511,X'S) 
RIDE C   ( 152,X'S) H   (1521,X'S) 
RIDE C   ( 153,X'S) H   (1531,X'S) 
RIDE C   ( 154,X'S) H   (1541,X'S) 
RIDE C   ( 155,X'S) H   (1551,X'S) 
RIDE C   ( 157,X'S) H   (1571,X'S) H   (1572,X'S) 
RIDE C   ( 161,X'S) H   (1611,X'S) 
RIDE C   ( 164,X'S) H   (1641,X'S) 
RIDE C   ( 165,X'S) H   (1651,X'S) 
RIDE C   ( 166,X'S) H   (1661,X'S) 
RIDE C   ( 172,X'S) H   (1721,X'S) 
RIDE C   ( 173,X'S) H   (1731,X'S) 
RIDE C   ( 174,X'S) H   (1741,X'S) 
RIDE C   ( 177,X'S) H   (1771,X'S) 
RIDE C   ( 181,X'S) H   (1812,X'S) H   (1811,X'S) 
RIDE C   ( 183,X'S) H   (1831,X'S) 
RIDE C   ( 184,X'S) H   (1841,X'S) 
RIDE C   ( 185,X'S) H   (1851,X'S) 
RIDE C   ( 186,X'S) H   (1861,X'S) 
RIDE C   ( 187,X'S) H   (1871,X'S) 
RIDE C   ( 202,X'S) H   (2021,X'S) 
RIDE C   ( 204,X'S) H   (2041,X'S) H   (2043,X'S) H   (2042,X'S) 
RIDE C   ( 205,X'S) H   (2051,X'S) H   (2053,X'S) H   (2052,X'S) 
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   (  71,X'S) H   (  72,X'S) 
RIDE C   (  11,X'S) H   ( 111,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) 
RIDE C   (  27,X'S) H   ( 271,X'S) 
RIDE C   (  31,X'S) H   ( 312,X'S) H   ( 311,X'S) 
RIDE C   (  33,X'S) H   ( 331,X'S) 
RIDE C   (  34,X'S) H   ( 341,X'S) 
RIDE C   (  35,X'S) H   ( 351,X'S) 
RIDE C   (  36,X'S) H   ( 361,X'S) 
RIDE C   (  37,X'S) H   ( 371,X'S) 
RIDE C   (  51,X'S) H   ( 511,X'S) 
RIDE C   (  52,X'S) H   ( 521,X'S) 
RIDE C   (  53,X'S) H   ( 531,X'S) 
RIDE C   (  54,X'S) H   ( 541,X'S) 
RIDE C   (  55,X'S) H   ( 551,X'S) 
RIDE C   (  57,X'S) H   ( 572,X'S) H   ( 571,X'S) 
RIDE C   (  61,X'S) H   ( 611,X'S) 
RIDE C   (  64,X'S) H   ( 641,X'S) 
RIDE C   (  65,X'S) H   ( 651,X'S) 
RIDE C   (  66,X'S) H   ( 661,X'S) 
RIDE C   (  72,X'S) H   ( 721,X'S) 
RIDE C   (  73,X'S) H   ( 731,X'S) 
RIDE C   (  74,X'S) H   ( 741,X'S) 
RIDE C   (  77,X'S) H   ( 771,X'S) 
RIDE C   (  81,X'S) H   ( 811,X'S) H   ( 812,X'S) 
RIDE C   (  83,X'S) H   ( 831,X'S) 
RIDE C   (  84,X'S) H   ( 841,X'S) 
RIDE C   (  85,X'S) H   ( 851,X'S) 
RIDE C   (  86,X'S) H   ( 861,X'S) 
RIDE C   (  87,X'S) H   ( 871,X'S) 
END     
;
_iucr_refine_instructions_details_restraints
;
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM NO H   NO #H U MULT DIST 
REM C-H 
REM >4           1.5    .96 DISORDER 
REM 1      1     1.2    .93 C C-H (ACETYLENE) 
REM 1      2     1.2    .93 C-C(H)-C 
REM 1      3     1.2    .98 (C)3-C-H 
REM 2      1     1.2    .93 C=C-H(2) 
REM 2      2     1.2    .97 (C)2-C-(H)2 
REM 3      1     1.5    .96 C-C-(H)3 
REM N-H 
REM >4           1.5    .89 DISORDER 
REM 1      1     1.2    .86 N-N/H 
REM 1      2     1.2    .86 (C)2-N-H 
REM 1      3     1.2    .89 (C)3-N-H 
REM 2      1     1.2    .86 C-N-(H)2 
REM 2      2     1.2    .89 (C)2-N-(H)2 
REM 3      1     1.2    .89 C-H-(H)3 
REM O-H 
REM 1      1     1.5    .82 O-H 
REM 
REM DIST      ESD = 0.02 
REM VIB       ESD = 0.002 
REM ANGLE     ESD = 2.0 
REM       H ON O-HETRO ATOM 
DIST 0.82, 0.02 = 
CONT O ( 211) TO H(2112) 
CONT O ( 211) TO H(2111) 
REST 0.062, 0.002 = H(2112,U[ISO]) 
REST 0.062, 0.002 = H(2111,U[ISO]) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
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_cod_data_source_file            c7dt00295e2.cif
_cod_data_source_block           ZJB054_compound3
_cod_depositor_comments
;
Adding full bibliography for 7042363--7042366.cif.

2017-11-11
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_cell_volume        10877.7(2)
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_original_formula_moiety     '2(C60 H44 Co N14), 2(B F4), C3 H7 N O, H2 O '
_cod_original_formula_sum        'C123 H97 B2 Co2 F8 N29 O2'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     2304.80
_cod_database_code               7042365