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_7715210
_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         'C10 H36 B18 Co N'
_chemical_formula_sum            'C10 H36 B18 Co N'
_chemical_formula_weight         423.91
_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                 94.582(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.7657(3)
_cell_length_b                   11.6644(2)
_cell_length_c                   14.2364(3)
_cell_measurement_reflns_used    10536
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      73.4000
_cell_measurement_theta_min      3.2150
_cell_volume                     2278.61(8)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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    -71.00  19.00   0.50   25.00    --  -49.54  81.00  -7.00  180
  2  \w    -18.00  37.00   0.50   25.00    --   49.54 -81.00-129.00  110
  3  \w   -111.00 -85.00   0.50  100.00    --  -90.00  81.00  -7.00   52
  4  \w    -59.00 -27.00   0.50  100.00    --  -90.00  81.00  -7.00   64
  5  \w   -153.00-127.00   0.50  100.00    --  -90.00 -81.00-129.00   52
  6  \w     37.00  98.00   0.50  100.00    --  107.40 -81.00-129.00  122
  7  \w    -41.00  23.00   0.50   25.00    --  -49.54  37.00 120.00  128
  8  \w    -22.00  24.00   0.50   25.00    --  -49.54  19.00 -30.00   92
  9  \w   -118.00 -91.00   0.50   25.00    --  -49.54 -77.00-120.00   54
 10  \w   -110.00 -80.00   0.50   25.00    --  -49.54-125.00  30.00   60
 11  \w    -22.00  23.00   0.50   25.00    --   49.54 -19.00 -60.00   90
 12  \w   -160.00 -83.00   0.50  100.00    --  -90.00 -37.00 120.00  154
 13  \w    -60.00 -21.00   0.50  100.00    --  -90.00  57.00 -60.00   78
 14  \w   -160.00 -91.00   0.50  100.00    --  -90.00 -99.00 -90.00  138
 15  \w    -66.00 -24.00   0.50  100.00    --  -90.00  57.00-180.00   84
 16  \w   -160.00 -83.00   0.50  100.00    --  -90.00 -37.00 150.00  154
 17  \w   -157.00 -82.00   0.50  100.00    --  -90.00 -19.00-120.00  150
 18  \w   -161.00 -89.00   0.50  100.00    --  -90.00 -77.00 120.00  144
 19  \w    101.00 176.00   0.50  100.00    --  107.40  37.00   0.00  150
 20  \w     39.00 111.00   0.50  100.00    --  107.40-125.00   0.00  144
 21  \w     38.00 105.00   0.50  100.00    --  107.40 -99.00-120.00  134
 22  \w     40.00 112.00   0.50  100.00    --  107.40-125.00  30.00  144
 23  \w     96.00 178.00   0.50  100.00    --  107.40  57.00  30.00  164
 24  \w     38.00  64.00   0.50  100.00    --  107.40 -57.00  90.00   52
 25  \w     36.00  66.00   0.50  100.00    --  107.40 -57.00  60.00   60
 26  \w    104.00 177.00   0.50  100.00    --  107.40  19.00 -60.00  146
 27  \w    136.00 162.00   0.50  100.00    --  107.40  81.00  -7.00   52
;
_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      -0.0647224000
_diffrn_orient_matrix_UB_12      0.0411995000
_diffrn_orient_matrix_UB_13      -0.0866603000
_diffrn_orient_matrix_UB_21      0.0292212000
_diffrn_orient_matrix_UB_22      -0.1065049000
_diffrn_orient_matrix_UB_23      -0.0552842000
_diffrn_orient_matrix_UB_31      -0.0869943000
_diffrn_orient_matrix_UB_32      -0.0664227000
_diffrn_orient_matrix_UB_33      0.0347383000
_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  0.0476
_diffrn_reflns_av_unetI/netI     0.0350
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            20741
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        66.599
_diffrn_reflns_theta_max         66.599
_diffrn_reflns_theta_min         3.221
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.836
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.887
_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    1.236
_exptl_crystal_description       prism
_exptl_crystal_F_000             880
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.824
_refine_diff_density_min         -0.580
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         4007
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0527
_refine_ls_R_factor_gt           0.0466
_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^)+(0.0733P)^2^+1.4047P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1225
_refine_ls_wR_factor_ref         0.1257
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3554
_reflns_number_total             4007
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00072b2.cif
_cod_data_source_block           q2-39-3_10_cu_100-gg
_cod_depositor_comments
'Adding full bibliography for 7715207--7715212.cif.'
_cod_database_code               7715210
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C10 H36 N B18'
_shelx_estimated_absorpt_t_max   0.844
_shelx_estimated_absorpt_t_min   0.622
_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:
 C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B)
2.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C6(H6A,H6B,H6C)
2.c Boron cage BH refined with riding coordinates:
 C1'(H1'), C2'(H2'), B4(H4), C2(H2), B7'(H7'), B6(H6), B8'(H8'), B4'(H4'),
 B7(H7), B8(H8), B5(H5), B11(H11), B5'(H5'), B12'(H12'), B6'(H6'), B12(H12),
 B10(H10), B11'(H11'), B9'(H9'), B9(H9), B10'(H10')
;
_shelx_res_checksum              39836
_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 1.368
_oxdiff_exptl_absorpt_empirical_full_min 0.767