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_7042364
_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         'C92 H108 Co N14, 1.5(C4 H10 O), B F4'
_chemical_formula_sum            'C98 H123 B Co F4 N14 O1.5'
_chemical_formula_weight         1666.90
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_update_record
;
2016-10-17 deposited with the CCDC.
2017-03-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.014(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.6488(4)
_cell_length_b                   20.3208(6)
_cell_length_c                   28.7288(11)
_cell_measurement_reflns_used    24866
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.2
_cell_measurement_theta_min      3.33
_cell_volume                     9695.6(5)
_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 0.955
_diffrn_measured_fraction_theta_max 0.862
_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  0.061
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            98773
_diffrn_reflns_theta_full        25.285
_diffrn_reflns_theta_max         29.747
_diffrn_reflns_theta_min         2.927
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.237
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.59
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALE3 ABSPACK'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.142
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3556
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.13
_platon_squeeze_details
;
;
_refine_diff_density_max         1.74
_refine_diff_density_min         -0.79
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9664
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1114
_refine_ls_number_reflns         17264
_refine_ls_number_restraints     190
_refine_ls_R_factor_all          0.1029
_refine_ls_R_factor_gt           0.0870
_refine_ls_shift/su_max          0.0010201
_refine_ls_shift/su_mean         0.0000213
_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: 
 0.109E+04 0.174E+04 0.107E+04 434. 100. 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2234
_refine_ls_wR_factor_gt          0.2103
_refine_ls_wR_factor_ref         0.2233
_reflns_limit_h_max              22
_reflns_limit_h_min              -22
_reflns_limit_k_max              27
_reflns_limit_k_min              0
_reflns_limit_l_max              39
_reflns_limit_l_min              0
_reflns_number_gt                14146
_reflns_number_total             23829
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.77
_oxford_diffrn_Wilson_scale      0.91
_oxford_refine_ls_r_factor_ref   0.1028
_oxford_refine_ls_scale          1.232(5)
_oxford_reflns_number_all        17270
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_cod_data_source_file            c7dt00295e2.cif
_cod_data_source_block           MSB113_compound2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Other' changed to 'other'
according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 7042363--7042366.cif.
;
_cod_original_cell_volume        9695.6(4)
_cod_original_sg_symbol_H-M      'P 21/c '
_cod_database_code               7042364
_iucr_refine_instructions_details_constraints
;
BLOCK SCALE X'S  U'S 
RIDE C   (   1,X'S) H   (  11,X'S) 
RIDE C   (   2,X'S) H   (  21,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   (  16,X'S) H   ( 161,X'S) 
RIDE C   (  22,X'S) H   ( 221,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   ( 311,X'S) H   ( 312,X'S) 
RIDE C   (  33,X'S) H   ( 331,X'S) 
RIDE C   (  34,X'S) H   ( 341,X'S) 
RIDE C   (  36,X'S) H   ( 361,X'S) 
RIDE C   (  37,X'S) H   ( 371,X'S) 
RIDE C   (  39,X'S) H   ( 392,X'S) H   ( 393,X'S) H   ( 391,X'S) 
RIDE C   (  40,X'S) H   ( 403,X'S) H   ( 401,X'S) H   ( 402,X'S) 
RIDE C   (  41,X'S) H   ( 411,X'S) H   ( 413,X'S) H   ( 412,X'S) 
RIDE C   (  43,X'S) H   ( 432,X'S) H   ( 431,X'S) H   ( 433,X'S) 
RIDE C   (  44,X'S) H   ( 442,X'S) H   ( 443,X'S) H   ( 441,X'S) 
RIDE C   (  45,X'S) H   ( 453,X'S) H   ( 451,X'S) H   ( 452,X'S) 
RIDE C   (  47,X'S) H   ( 471,X'S) H   ( 473,X'S) H   ( 472,X'S) 
RIDE C   (  48,X'S) H   ( 482,X'S) H   ( 481,X'S) H   ( 483,X'S) 
RIDE C   (  49,X'S) H   ( 492,X'S) H   ( 493,X'S) H   ( 491,X'S) 
RIDE C   (  51,X'S) H   ( 513,X'S) H   ( 511,X'S) H   ( 512,X'S) 
RIDE C   (  52,X'S) H   ( 521,X'S) H   ( 523,X'S) H   ( 522,X'S) 
RIDE C   (  53,X'S) H   ( 532,X'S) H   ( 531,X'S) H   ( 533,X'S) 
RIDE C   ( 101,X'S) H   (1011,X'S) 
RIDE C   ( 102,X'S) H   (1021,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   ( 116,X'S) H   (1161,X'S) 
RIDE C   ( 122,X'S) H   (1221,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   (1312,X'S) H   (1311,X'S) 
RIDE C   ( 133,X'S) H   (1331,X'S) 
RIDE C   ( 134,X'S) H   (1341,X'S) 
RIDE C   ( 136,X'S) H   (1361,X'S) 
RIDE C   ( 137,X'S) H   (1371,X'S) 
RIDE C   ( 139,X'S) H   (1391,X'S) H   (1392,X'S) H   (1393,X'S) 
RIDE C   ( 140,X'S) H   (1401,X'S) H   (1402,X'S) H   (1403,X'S) 
RIDE C   ( 141,X'S) H   (1411,X'S) H   (1412,X'S) H   (1413,X'S) 
RIDE C   ( 143,X'S) H   (1431,X'S) H   (1433,X'S) H   (1432,X'S) 
RIDE C   ( 144,X'S) H   (1442,X'S) H   (1441,X'S) H   (1443,X'S) 
RIDE C   ( 145,X'S) H   (1452,X'S) H   (1453,X'S) H   (1451,X'S) 
RIDE C   ( 147,X'S) H   (1473,X'S) H   (1471,X'S) H   (1472,X'S) 
RIDE C   ( 148,X'S) H   (1481,X'S) H   (1483,X'S) H   (1482,X'S) 
RIDE C   ( 149,X'S) H   (1492,X'S) H   (1491,X'S) H   (1493,X'S) 
RIDE C   ( 151,X'S) H   (1512,X'S) H   (1513,X'S) H   (1511,X'S) 
RIDE C   ( 152,X'S) H   (1523,X'S) H   (1521,X'S) H   (1522,X'S) 
RIDE C   ( 153,X'S) H   (1531,X'S) H   (1533,X'S) H   (1532,X'S) 
RIDE C   ( 201,X'S) H   (2012,X'S) H   (2011,X'S) H   (2013,X'S) 
RIDE C   ( 202,X'S) H   (2021,X'S) H   (2022,X'S) 
RIDE C   ( 204,X'S) H   (2041,X'S) H   (2042,X'S) 
RIDE C   ( 205,X'S) H   (2052,X'S) H   (2053,X'S) H   (2051,X'S) 
RIDE C   ( 211,X'S) H   (2111,X'S) H   (2112,X'S) H   (2113,X'S) 
RIDE C   ( 212,X'S) H   (2122,X'S) H   (2121,X'S) 
RIDE C   ( 214,X'S) H   (2142,X'S) H   (2141,X'S) 
RIDE C   ( 240,X'S) H   (2401,X'S) H   (2402,X'S) H   (2403,X'S) 
RIDE C   ( 241,X'S) H   (2411,X'S) H   (2412,X'S) H   (2413,X'S) 
RIDE C   ( 239,X'S) H   (2391,X'S) H   (2392,X'S) H   (2393,X'S) 
END                               
;
_iucr_refine_instructions_details_restraints
;                                              
REM 
REM ET2OS 
REM 
DIST 1.50, 0.01 = C(201) TO C(202), C(204) TO C(205) 
CONT C(211) TO C(212), C(211) TO C(214) 
DIST 1.43, 0.01 = C(202) TO O(203), O(203) TO C(204) 
CONT C(212) TO O(213), C(214) TO O(213) 
ANGL 109, 1 = C(201) TO C(202) TO O(203) 
CONT C(202) TO O(203) TO C(204) 
CONT O(203) TO C(204) TO C(205) 
CONT C(211) TO C(212) TO O(213) 
CONT C(211) TO C(214) TO O(213) 
REM 
REM TBUS 
REM 
DIST 1.52, 0.01 = C(138) TO C(139) 
CONT C(138) TO C(140) 
CONT C(138) TO C(141) 
CONT C(138) TO C(239) 
CONT C(138) TO C(240) 
CONT C(138) TO C(241) 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
REM   DELU   START (DO NOT REMOVE THIS LINE) 
VIBR .0, 0.00100 = C(46) TO C(47) 
VIBR .0, 0.00100 = C(46) TO C(48) 
VIBR .0, 0.00100 = C(46) TO C(49) 
VIBR .0, 0.00200 = C(47) TO C(15) 
VIBR .0, 0.00200 = C(48) TO C(15) 
VIBR .0, 0.00200 = C(48) TO C(47) 
VIBR .0, 0.00200 = C(49) TO C(15) 
VIBR .0, 0.00200 = C(49) TO C(47) 
VIBR .0, 0.00200 = C(49) TO C(48) 
VIBR .0, 0.00100 = C(38) TO C(39) 
VIBR .0, 0.00100 = C(38) TO C(40) 
VIBR .0, 0.00100 = C(38) TO C(41) 
VIBR .0, 0.00200 = C(39) TO C(3) 
VIBR .0, 0.00200 = C(40) TO C(3) 
VIBR .0, 0.00200 = C(40) TO C(39) 
VIBR .0, 0.00200 = C(41) TO C(3) 
VIBR .0, 0.00200 = C(41) TO C(39) 
VIBR .0, 0.00200 = C(41) TO C(40) 
VIBR .0, 0.00100 = C(138) TO C(139) 
VIBR .0, 0.00100 = C(138) TO C(140) 
VIBR .0, 0.00100 = C(138) TO C(141) 
VIBR .0, 0.00200 = C(139) TO C(103) 
VIBR .0, 0.00200 = C(140) TO C(103) 
VIBR .0, 0.00200 = C(140) TO C(139) 
VIBR .0, 0.00200 = C(141) TO C(103) 
VIBR .0, 0.00200 = C(141) TO C(139) 
VIBR .0, 0.00200 = C(141) TO C(140) 
VIBR .0, 0.00100 = C(138) TO C(239) 
VIBR .0, 0.00100 = C(138) TO C(240) 
VIBR .0, 0.00100 = C(138) TO C(241) 
VIBR .0, 0.00200 = C(139) TO C(103) 
VIBR .0, 0.00200 = C(240) TO C(103) 
VIBR .0, 0.00200 = C(240) TO C(239) 
VIBR .0, 0.00200 = C(241) TO C(103) 
VIBR .0, 0.00200 = C(241) TO C(239) 
VIBR .0, 0.00200 = C(241) TO C(240) 
VIBR .0, 0.00100 = C(201) TO C(202) 
VIBR .0, 0.00100 = C(202) TO O(203) 
VIBR .0, 0.00200 = O(203) TO C(201) 
VIBR .0, 0.00100 = O(203) TO C(204) 
VIBR .0, 0.00200 = C(204) TO C(202) 
VIBR .0, 0.00100 = C(204) TO C(205) 
VIBR .0, 0.00200 = C(205) TO O(203) 
VIBR .0, 0.00100 = C(211) TO C(212) 
VIBR .0, 0.00100 = C(212) TO O(213) 
VIBR .0, 0.00200 = O(213) TO C(211) 
VIBR .0, 0.00200 = C(212,-1,1,1,0,1) TO C(212) 
VIBR .0, 0.00100 = F(11) TO B(1) 
VIBR .0, 0.00100 = F(14) TO B(1) 
VIBR .0, 0.00100 = F(13) TO B(1) 
VIBR .0, 0.00100 = B(1) TO F(12) 
VIBR .0, 0.00200 = F(11) TO F(14) 
VIBR .0, 0.00200 = F(13) TO F(14) 
VIBR .0, 0.00200 = F(13) TO F(11) 
VIBR .0, 0.00200 = F(12) TO F(14) 
VIBR .0, 0.00200 = F(12) TO F(11) 
VIBR .0, 0.00200 = F(12) TO F(13) 
VIBR .0, 0.00200 = O(213) TO C(211) 
REM   DELU   END (DO NOT REMOVE THIS LINE) 
REM   THERMSIM   START (DO NOT REMOVE THIS LINE) 
U(IJ) .0, 0.02000 = C(46) TO C(47) 
U(IJ) .0, 0.02000 = C(46) TO C(48) 
U(IJ) .0, 0.02000 = C(46) TO C(49) 
U(IJ) .0, 0.02000 = C(138) TO C(139) 
U(IJ) .0, 0.02000 = C(138) TO C(140) 
U(IJ) .0, 0.02000 = C(138) TO C(141) 
U(IJ) .0, 0.02000 = C(138) TO C(239) 
U(IJ) .0, 0.02000 = C(138) TO C(240) 
U(IJ) .0, 0.02000 = C(138) TO C(241) 
U(IJ) .0, 0.02000 = C(201) TO C(202) 
U(IJ) .0, 0.01000 = C(202) TO O(203) 
U(IJ) .0, 0.01000 = O(203) TO C(204) 
U(IJ) .0, 0.02000 = C(204) TO C(205) 
U(IJ) .0, 0.01000 = C(211) TO C(212) 
U(IJ) .0, 0.01000 = C(212) TO O(213) 
U(IJ) .0, 0.02000 = F(11) TO B(1) 
U(IJ) .0, 0.02000 = F(14) TO B(1) 
U(IJ) .0, 0.02000 = F(13) TO B(1) 
U(IJ) .0, 0.02000 = B(1) TO F(12) 
REM   THERMSIM   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;