Synthetic routes to carbon substituted cobalt bis(dicarbollide) alkyl halides and aromatic amines along with closely related irregular pathways.
Nekvinda, Jan; Bavol, Dmytro; Litecká, Miroslava; Tüzün, Ece Zeynep; Dušek, Michal; Grüner, Bohumír; Dalton transactions (Cambridge, England : 2003) 53 (2024) 5816–5826; doi:10.1039/d4dt00072b

data_7715212
_publ_section_title
;
 Synthetic routes to carbon substituted cobalt bis(dicarbollide) alkyl
 halides and aromatic amines along with closely related irregular
 pathways.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5816
_journal_page_last               5826
_journal_paper_doi               10.1039/d4dt00072b
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C8 H26 B18 Co, C4 H12 N'
_chemical_formula_sum            'C12 H38 B18 Co N'
_chemical_formula_weight         449.94
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-12-11
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2021.10.07 svn.r9718050b for OlexSys, GUI svn.r6410)
;
_audit_update_record
;
2023-12-11 deposited with the CCDC.	2024-02-19 downloaded from the CCDC.
;
_cell_angle_alpha                84.7500(17)
_cell_angle_beta                 87.7997(15)
_cell_angle_gamma                88.905(2)
_cell_formula_units_Z            2
_cell_length_a                   9.8900(2)
_cell_length_b                   10.5598(3)
_cell_length_c                   11.48866(18)
_cell_measurement_reflns_used    16276
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      78.1450
_cell_measurement_theta_min      3.8610
_cell_volume                     1193.77(5)
_computing_cell_refinement       'CrysAlisPro 1.171.42.73a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.73a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.73a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -115.00 -88.00   0.50    3.00    --  -49.14 -77.00 -84.00   54
  2  \w     96.00 121.00   0.50    3.00    --   49.14  77.00  40.00   50
  3  \w     29.00  56.00   0.50    3.00    --   49.14  77.00  40.00   54
  4  \w    -96.00 -70.00   0.50   12.00    --  -90.00 -77.00 -84.00   52
  5  \w    -65.00 -31.00   0.50   12.00    --  -90.00  77.00  40.00   68
  6  \w   -146.00-120.00   0.50   12.00    --  -90.00 -77.00 -84.00   52
  7  \w    141.00 177.00   0.50   12.00    --  111.50  77.00  40.00   72
  8  \w     91.00 134.00   0.50   12.00    --  111.50  77.00  40.00   86
  9  \w     -8.00  18.00   0.50    3.00    --   14.00  80.00 118.94   52
 10  \w     -1.00  24.00   0.50    3.00    --   18.00  73.00-110.44   50
 11  \w     -1.00  24.00   0.50    3.00    --   18.00  73.00  67.90   50
 12  \w      7.00  32.00   0.50    3.00    --   22.00  66.00  33.08   50
 13  \w     16.00  41.00   0.50    3.00    --   30.00  60.00  -9.17   50
 14  \w     17.00  42.00   0.50    3.00    --   30.00  59.00-104.04   50
 15  \w     21.00  46.00   0.50    3.00    --   34.00  57.00  71.08   50
 16  \w    -55.00 -28.00   0.50    3.00    --  -38.00 -54.00  89.54   54
 17  \w     26.00  51.00   0.50    3.00    --   38.00  55.00 166.82   50
 18  \w     26.00  51.00   0.50    3.00    --   38.00  55.00  13.77   50
 19  \w    -59.00 -33.00   0.50    3.00    --  -42.00 -52.00 135.05   52
 20  \w    -65.00 -29.00   0.50    3.00    --  -49.14 -77.00 -84.00   72
 21  \w    -84.00 -16.00   0.50    3.00    --  -49.14 125.00  30.00  136
 22  \w    -68.00 -14.00   0.50    3.00    --  -49.14  77.00  40.00  108
 23  \w     39.00  69.00   0.50    3.00    --   49.14  51.00-122.70   60
 24  \w    -20.00  68.00   0.50    3.00    --   49.14 -77.00 -84.00  176
 25  \w     42.00  69.00   0.50    3.00    --   50.00  52.00 -90.96   54
 26  \w   -114.00 -47.00   0.50    3.00    --  -58.00 -52.00  11.45  134
 27  \w    -74.00 -47.00   0.50    3.00    --  -58.00 -51.00  42.01   54
 28  \w    -74.00 -48.00   0.50    3.00    --  -58.00 -48.00 161.34   52
 29  \w    -72.00 -47.00   0.50    3.00    --  -58.00 -52.00 110.83   50
 30  \w    -78.00 -53.00   0.50    3.00    --  -62.00 -45.00 -31.03   50
 31  \w   -114.00 -88.00   0.50    3.00    --  -62.00 -45.00 -31.03   52
 32  \w    -96.00 -57.00   0.50    3.00    --  -66.00 -45.00-105.50   78
 33  \w   -137.00-111.00   0.50    3.00    --  -70.00 -51.00 -49.14   52
 34  \w    -86.00 -60.00   0.50    3.00    --  -70.00 -49.00  76.04   52
 35  \w    -87.00 -62.00   0.50    3.00    --  -70.00 -48.00  94.44   50
 36  \w    -85.00 -59.00   0.50    3.00    --  -70.00 -51.00 144.16   52
 37  \w    -87.00 -61.00   0.50    3.00    --  -70.00 -51.00 -49.14   52
 38  \w    -89.00 -63.00   0.50    3.00    --  -70.00 -50.00 162.37   52
 39  \w    -85.00 -59.00   0.50    3.00    --  -70.00 -50.00 -32.38   52
 40  \w    -91.00 -63.00   0.50    3.00    --  -74.00 -51.00-129.71   56
 41  \w    -98.00 -65.00   0.50    3.00    --  -74.00 -45.00-124.24   66
 42  \w    -95.00 -68.00   0.50    3.00    --  -78.00 -50.00-179.96   54
 43  \w    -93.00 -67.00   0.50    3.00    --  -78.00 -50.00 141.87   52
 44  \w    -96.00 -68.00   0.50    3.00    --  -78.00 -49.00 -57.47   56
 45  \w    -96.00 -71.00   0.50   12.00    --  -82.00 -51.00 125.21   50
 46  \w    -97.00 -71.00   0.50   12.00    --  -82.00 -50.00  83.31   52
 47  \w   -150.00-125.00   0.50   12.00    --  -82.00 -51.00 125.21   50
 48  \w   -101.00 -76.00   0.50   12.00    --  -86.00 -49.00  32.67   50
 49  \w   -101.00 -76.00   0.50   12.00    --  -86.00 -49.00  44.97   50
 50  \w   -154.00-128.00   0.50   12.00    --  -86.00 -49.00  32.67   52
 51  \w   -101.00 -75.00   0.50   12.00    --  -86.00 -51.00-135.60   52
 52  \w   -110.00 -82.00   0.50   12.00    --  -90.00 -52.00-146.34   56
 53  \w   -109.00 -83.00   0.50   12.00    --  -90.00 -52.00  79.07   52
 54  \w   -161.00-134.00   0.50   12.00    --  -90.00 -50.00 179.86   54
 55  \w   -108.00 -81.00   0.50   12.00    --  -90.00 -52.00  32.04   54
 56  \w   -107.00 -81.00   0.50   12.00    --  -90.00 -47.00 110.62   52
 57  \w   -115.00 -79.00   0.50   12.00    --  -90.00 -51.00   1.54   72
 58  \w   -105.00 -79.00   0.50   12.00    --  -90.00 -50.00 179.86   52
 59  \w   -153.00-125.00   0.50   12.00    --  -90.00 -51.00   1.54   56
 60  \w   -106.00 -80.00   0.50   12.00    --  -90.00 -52.00 -85.24   52
 61  \w   -161.00-135.00   0.50   12.00    --  -90.00 -51.00  63.24   52
 62  \w   -118.00 -84.00   0.50   12.00    --  -90.00 -51.00 -10.38   68
 63  \w   -107.00 -81.00   0.50   12.00    --  -90.00 -52.00 166.78   52
 64  \w   -115.00 -81.00   0.50   12.00    --  -90.00 -50.00 -30.84   68
 65  \w   -159.00-129.00   0.50   12.00    --  -90.00 -50.00 -30.84   60
 66  \w   -153.00-128.00   0.50   12.00    --  -90.00 -52.00 166.78   50
 67  \w   -108.00 -83.00   0.50   12.00    --  -90.00 -48.00 -68.58   50
 68  \w   -104.00 -79.00   0.50   12.00    --  -90.00 -51.00  20.45   50
 69  \w   -118.00 -87.00   0.50   12.00    --  -90.00 -52.00  98.14   62
 70  \w   -104.00 -79.00   0.50   12.00    --  -90.00 -51.00  63.24   50
 71  \w    144.00 170.00   0.50   12.00    --  111.50  45.00 -90.00   52
 72  \w    108.00 142.00   0.50   12.00    --  111.50  45.00 -90.00   68
 73  \w     43.00  74.00   0.50   12.00    --  111.50-125.00-120.00   62
 74  \w     44.00 105.00   0.50   12.00    --  111.50 -94.00 -90.00  122
 75  \w    137.00 163.00   0.50   12.00    --  111.50  45.00 120.00   52
 76  \w    105.00 130.00   0.50   12.00    --  111.50  45.00 -30.00   50
 77  \w     41.00 105.00   0.50   12.00    --  111.50 -94.00  30.00  128
 78  \w    102.00 132.00   0.50   12.00    --  111.50  45.00 120.00   60
 79  \w    148.00 174.00   0.50   12.00    --  111.50  61.00 150.00   52
 80  \w    144.00 170.00   0.50   12.00    --  111.50  45.00   0.00   52
 81  \w    107.00 139.00   0.50   12.00    --  111.50  45.00   0.00   64
 82  \w    109.00 172.00   0.50   12.00    --  111.50  61.00  30.00  126
 83  \w    107.00 160.00   0.50   12.00    --  111.50  77.00 120.00  106
 84  \w    109.00 137.00   0.50   12.00    --  111.50  45.00  30.00   56
 85  \w     76.00 101.00   0.50   12.00    --  111.50 -94.00   0.00   50
 86  \w     99.00 126.00   0.50   12.00    --  111.50  61.00 150.00   54
 87  \w    105.00 136.00   0.50   12.00    --  111.50  77.00-180.00   62
 88  \w     49.00 103.00   0.50   12.00    --  111.50 -94.00 -30.00  108
 89  \w     43.00  74.00   0.50   12.00    --  111.50 -94.00   0.00   62
 90  \w    153.00 178.00   0.50   12.00    --  111.50  61.00 -60.00   50
 91  \w     43.00 111.00   0.50   12.00    --  111.50-125.00 150.00  136
 92  \w     56.00 102.00   0.50   12.00    --  111.50 -94.00 150.00   92
 93  \w     61.00  87.00   0.50   12.00    --  111.50 -77.00 -84.00   52
 94  \w     78.00 103.00   0.50   12.00    --  111.50-125.00-180.00   50
 95  \w     45.00  70.00   0.50   12.00    --  111.50-125.00-180.00   50
 96  \w    101.00 134.00   0.50   12.00    --  111.50  61.00 -60.00   66
 97  \w    105.00 164.00   0.50   12.00    --  111.50  45.00-120.00  118
 98  \w    105.00 178.00   0.50   12.00    --  111.50  77.00  60.00  146
 99  \w    146.00 173.00   0.50   12.00    --  111.50  77.00 -90.00   54
100  \w     78.00 103.00   0.50   12.00    --  111.50-125.00   0.00   50
101  \w    106.00 133.00   0.50   12.00    --  111.50  77.00 -90.00   54
102  \w     44.00  69.00   0.50   12.00    --  111.50-125.00   0.00   50
103  \w     47.00  72.00   0.50   12.00    --  111.50 -61.00-180.00   50
104  \w     43.00 100.00   0.50   12.00    --  111.50-125.00 -90.00  114
105  \w     99.00 132.00   0.50   12.00    --  111.50  61.00 120.00   66
106  \w     41.00  72.00   0.50   12.00    --  111.50 -61.00  30.00   62
107  \w     41.00  72.00   0.50   12.00    --  111.50 -61.00  60.00   62
108  \w     74.00 101.00   0.50   12.00    --  111.50 -94.00  90.00   54
109  \w    104.00 131.00   0.50   12.00    --  111.50  45.00-180.00   54
110  \w    146.00 178.00   0.50   12.00    --  111.50  77.00-180.00   64
111  \w    133.00 175.00   0.50   12.00    --  111.50  61.00 -30.00   84
112  \w     99.00 125.00   0.50   12.00    --  111.50  61.00   0.00   52
113  \w    151.00 178.00   0.50   12.00    --  111.50  61.00-120.00   54
114  \w    101.00 126.00   0.50   12.00    --  111.50  61.00 -30.00   50
115  \w     99.00 126.00   0.50   12.00    --  111.50  61.00-120.00   54
116  \w    142.00 172.00   0.50   12.00    --  111.50  61.00-150.00   60
117  \w    105.00 142.00   0.50   12.00    --  111.50 125.00 120.00   74
118  \w     43.00  70.00   0.50   12.00    --  111.50 -61.00 150.00   54
119  \w     68.00 103.00   0.50   12.00    --  111.50 -94.00-120.00   70
120  \w    104.00 131.00   0.50   12.00    --  111.50  61.00-150.00   54
121  \w    148.00 175.00   0.50   12.00    --  111.50  45.00 -60.00   54
122  \w    104.00 130.00   0.50   12.00    --  111.50  45.00 -60.00   52
123  \w    147.00 174.00   0.50   12.00    --  111.50  61.00-180.00   54
124  \w    153.00 178.00   0.50   12.00    --  111.50  45.00  90.00   50
125  \w     73.00  98.00   0.50   12.00    --  111.50 -94.00-180.00   50
126  \w     42.00  67.00   0.50   12.00    --  111.50 -94.00-180.00   50
127  \w    100.00 141.00   0.50   12.00    --  111.50  61.00-180.00   82
128  \w     86.00 111.00   0.50   12.00    --  111.50-125.00-120.00   50
129  \w    102.00 148.00   0.50   12.00    --  111.50  45.00  90.00   92
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0988906000
_diffrn_orient_matrix_UB_12      -0.0168446000
_diffrn_orient_matrix_UB_13      -0.1045566000
_diffrn_orient_matrix_UB_21      0.0940629000
_diffrn_orient_matrix_UB_22      0.0992182000
_diffrn_orient_matrix_UB_23      0.0429206000
_diffrn_orient_matrix_UB_31      0.0753593000
_diffrn_orient_matrix_UB_32      -0.1064921000
_diffrn_orient_matrix_UB_33      0.0733715000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0689
_diffrn_reflns_av_unetI/netI     0.0349
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            32591
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        66.581
_diffrn_reflns_theta_max         66.581
_diffrn_reflns_theta_min         3.866
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.600
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.547
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.73a (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.252
_exptl_crystal_description       irregular
_exptl_crystal_F_000             468
_exptl_crystal_size_max          0.157
_exptl_crystal_size_mid          0.088
_exptl_crystal_size_min          0.054
_refine_diff_density_max         0.975
_refine_diff_density_min         -0.310
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     293
_refine_ls_number_reflns         4211
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0541
_refine_ls_R_factor_gt           0.0513
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1101P)^2^+0.3439P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1443
_refine_ls_wR_factor_ref         0.1471
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3931
_reflns_number_total             4211
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00072b2.cif
_cod_data_source_block           gr756-1-3-gg
_cod_depositor_comments
'Adding full bibliography for 7715207--7715212.cif.'
_cod_database_code               7715212
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C12 H38 B18 Co N'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C6(H6A,H6B), C5(H5A,H5B), C3(H3A,H3B)
2.b Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C29(H29A,H29B,H29C), C31(H31A,H31B,H31C), C32(H32A,H32B,
 H32C)
2.c Boron cage BH refined with riding coordinates:
 C2(H2), C2'(H2'), B7(H7), B4(H4), B4'(H4'), B7'(H7'), B12(H12), B6'(H6'),
 B12'(H12'), B6(H6), B11'(H11'), B9'(H9'), B9(H9), B10(H10), B5'(H5'),
 B10'(H10'), B11(H11), B5(H5)
;
_shelx_res_checksum              62678
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 4.159
_oxdiff_exptl_absorpt_empirical_full_min 0.479