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_7715209
_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         'C12 H32 B18 Co N'
_chemical_formula_sum            'C12 H32 B18 Co N'
_chemical_formula_weight         443.89
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-03-01
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2021.10.07 svn.r9718050b for OlexSys, GUI svn.r6410)
;
_audit_update_record
;
2023-03-03 deposited with the CCDC.	2024-02-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.1000(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.2945(2)
_cell_length_b                   12.39900(10)
_cell_length_c                   13.30760(10)
_cell_measurement_reflns_used    19290
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      78.1490
_cell_measurement_theta_min      3.2010
_cell_volume                     2266.10(4)
_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 2018/2 (Sheldrick, 2018)'
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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    -67.00 -42.00   0.50   20.00    --  -49.54 -38.00 -37.00   50
  2  \w    -41.00  18.00   0.50   20.00    --  -49.54  38.00 118.00  118
  3  \w   -105.00 -79.00   0.50   20.00    --  -49.54 -38.00 -37.00   52
  4  \w    -17.00  33.00   0.50   20.00    --   49.54 -38.00 -37.00  100
  5  \w   -122.00 -82.00   0.50   80.00    --  -90.00 -38.00 -37.00   80
  6  \w    107.00 162.00   0.50   80.00    --  111.50  38.00 118.00  110
  7  \w    -73.00 -37.00   0.50   20.00    --  -49.54 -57.00-150.00   72
  8  \w   -118.00 -81.00   0.50   20.00    --  -49.54-125.00  90.00   74
  9  \w   -121.00 -89.00   0.50   20.00    --  -49.54 -77.00-180.00   64
 10  \w    -21.00  24.00   0.50   20.00    --  -49.54  19.00 -90.00   90
 11  \w   -115.00 -42.00   0.50   20.00    --  -49.54 -19.00-120.00  146
 12  \w    -89.00 -39.00   0.50   20.00    --  -49.54 -57.00-180.00  100
 13  \w     38.00 100.00   0.50   20.00    --   49.54  57.00-180.00  124
 14  \w     50.00 106.00   0.50   20.00    --   49.54  38.00 118.00  112
 15  \w   -101.00 -75.00   0.50   80.00    --  -90.00 -64.00-109.09   52
 16  \w   -159.00-129.00   0.50   80.00    --  -90.00 -62.00-136.68   60
 17  \w    -56.00 -30.00   0.50   80.00    --  -90.00  57.00-150.00   52
 18  \w    -66.00 -23.00   0.50   80.00    --  -90.00  57.00 -60.00   86
 19  \w   -160.00 -74.00   0.50   80.00    --  -90.00 -64.00-102.99  172
 20  \w   -106.00 -78.00   0.50   80.00    --  -90.00 -59.00 173.70   56
 21  \w   -106.00 -76.00   0.50   80.00    --  -90.00 -61.00-155.97   60
 22  \w   -161.00 -80.00   0.50   80.00    --  -90.00 -68.00 166.18  162
 23  \w   -160.00-127.00   0.50   80.00    --  -90.00 -57.00 -90.00   66
 24  \w   -160.00-102.00   0.50   80.00    --  -90.00 -37.00 -90.00  116
 25  \w   -105.00 -80.00   0.50   80.00    --  -90.00 -61.00-149.51   50
 26  \w   -104.00 -78.00   0.50   80.00    --  -90.00 -57.00 -90.00   52
 27  \w   -109.00 -78.00   0.50   80.00    --  -90.00 -53.00-139.21   62
 28  \w   -150.00-124.00   0.50   80.00    --  -90.00 -62.00-119.95   52
 29  \w   -106.00 -81.00   0.50   80.00    --  -90.00 -62.00-119.95   50
 30  \w   -160.00-104.00   0.50   80.00    --  -90.00 -65.00-160.11  112
 31  \w    -99.00 -74.00   0.50   80.00    --  -90.00 -65.00-160.11   50
 32  \w   -100.00 -75.00   0.50   80.00    --  -90.00 -62.00-136.68   50
 33  \w   -100.00 -75.00   0.50   80.00    --  -90.00 -63.00-129.57   50
 34  \w    -99.00 -74.00   0.50   80.00    --  -90.00 -64.00-174.90   50
 35  \w   -114.00 -76.00   0.50   80.00    --  -90.00 -67.00-108.07   76
 36  \w   -107.00 -75.00   0.50   80.00    --  -90.00 -63.00 169.05   64
 37  \w    -52.00 -23.00   0.50   80.00    --  -90.00  57.00 -90.00   58
 38  \w    -61.00 -22.00   0.50   80.00    --  -90.00  57.00  60.00   78
 39  \w    -65.00 -19.00   0.50   80.00    --  -90.00  57.00-120.00   92
 40  \w   -153.00-127.00   0.50   80.00    --  -90.00 -64.00-174.90   52
 41  \w   -161.00-110.00   0.50   80.00    --  -90.00 -19.00  30.00  102
 42  \w   -141.00-115.00   0.50   80.00    --  -90.00 -63.00-129.57   52
 43  \w   -103.00 -77.00   0.50   80.00    --  -90.00 -57.00-180.00   52
 44  \w   -101.00 -76.00   0.50   80.00    --  -90.00 -61.00-144.58   50
 45  \w   -150.00-124.00   0.50   80.00    --  -90.00 -61.00-155.97   52
 46  \w    112.00 169.00   0.50   80.00    --  111.50  37.00  60.00  114
 47  \w     80.00 109.00   0.50   80.00    --  111.50 -99.00 -30.00   58
 48  \w     45.00  76.00   0.50   80.00    --  111.50 -99.00 -30.00   62
 49  \w    120.00 146.00   0.50   80.00    --  111.50 125.00   0.00   52
 50  \w    150.00 175.00   0.50   80.00    --  111.50 125.00 -60.00   50
 51  \w     96.00 121.00   0.50   80.00    --  111.50 125.00 -60.00   50
 52  \w    109.00 178.00   0.50   80.00    --  111.50  37.00  90.00  138
 53  \w    113.00 172.00   0.50   80.00    --  111.50  19.00  30.00  118
 54  \w     90.00 115.00   0.50   80.00    --  111.50-125.00-150.00   50
 55  \w     48.00  75.00   0.50   80.00    --  111.50-125.00-150.00   54
;
_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      -0.0586073000
_diffrn_orient_matrix_UB_12      0.0450730000
_diffrn_orient_matrix_UB_13      -0.1067807000
_diffrn_orient_matrix_UB_21      0.0951684000
_diffrn_orient_matrix_UB_22      0.0385403000
_diffrn_orient_matrix_UB_23      -0.0212535000
_diffrn_orient_matrix_UB_31      0.0094161000
_diffrn_orient_matrix_UB_32      -0.1091915000
_diffrn_orient_matrix_UB_33      -0.0516328000
_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  0.0404
_diffrn_reflns_av_unetI/netI     0.0219
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            34472
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        66.585
_diffrn_reflns_theta_max         66.585
_diffrn_reflns_theta_min         3.218
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.899
_exptl_absorpt_correction_T_max  0.992
_exptl_absorpt_correction_T_min  0.708
_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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.301
_exptl_crystal_description       irregular
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.561
_refine_diff_density_min         -0.279
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         4003
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0331
_refine_ls_R_factor_gt           0.0306
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0562P)^2^+0.5265P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0838
_refine_ls_wR_factor_ref         0.0852
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3751
_reflns_number_total             4003
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00072b2.cif
_cod_data_source_block           q2-mz364_10_cu_100-gg
_cod_depositor_comments
'Adding full bibliography for 7715207--7715212.cif.'
_cod_database_code               7715209
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C12 H32 B18 Co N'
_shelx_estimated_absorpt_t_max   0.843
_shelx_estimated_absorpt_t_min   0.619
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B)
2.b Aromatic/amide H refined with riding coordinates:
 C10(H10A), C6(H6A), C7(H7A), C8(H8A), C9(H9A)
2.c Boron cage BH refined with riding coordinates:
 C1'(H1'), C2'(H2'), C2(H2), B4'(H4'), B8'(H8'), B4(H4), B12'(H12'), B7'(H7'),
 B9(H9), B1(H1), B10(H10), B12(H12), B6(H6), B7(H7), B5(H5), B9'(H9'), B11(H11),
  B11'(H11'), B6'(H6'), B5'(H5'), B10'(H10')
;
_shelx_res_checksum              2761
_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 1.955
_oxdiff_exptl_absorpt_empirical_full_min 0.708