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_7715211
_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, C H2 Cl2, C4 H12 N'
_chemical_formula_sum            'C13 H40 B18 Cl2 Co N'
_chemical_formula_weight         534.87
_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
_audit_creation_date             2023-12-07
_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                90
_cell_angle_beta                 109.088(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.3274(4)
_cell_length_b                   12.8952(3)
_cell_length_c                   14.3700(3)
_cell_measurement_reflns_used    19431
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      79.7810
_cell_measurement_theta_min      3.0300
_cell_volume                     2684.07(12)
_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)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.99(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    -64.00  18.00   0.50    6.00    --  -49.39  71.00 130.00  164
  2  \w   -111.00 -44.00   0.50    6.00    --  -49.39 -71.00   0.00  134
  3  \w    -12.00  67.00   0.50    6.00    --   49.39 -71.00   0.00  158
  4  \w     36.00 117.00   0.50    6.00    --   49.39  71.00 130.00  162
  5  \w   -141.00-116.00   0.50   24.00    --  -90.00 -71.00   0.00   50
  6  \w    -57.00 -31.00   0.50   24.00    --  -90.00  71.00 130.00   52
  7  \w     97.00 176.00   0.50   24.00    --  111.50  71.00 130.00  158
  8  \w     41.00  67.00   0.50   24.00    --  111.50 -71.00   0.00   52
  9  \w   -118.00 -93.00   0.50    6.00    --  -49.39-125.00 -60.00   50
 10  \w   -121.00 -96.00   0.50    6.00    --  -49.39 -57.00  60.00   50
 11  \w   -118.00 -93.00   0.50    6.00    --  -49.39-125.00 120.00   50
 12  \w   -118.00 -93.00   0.50    6.00    --  -49.39-125.00 -90.00   50
 13  \w   -121.00 -96.00   0.50    6.00    --  -49.39 -57.00 -60.00   50
 14  \w   -117.00 -92.00   0.50    6.00    --  -49.39-125.00-180.00   50
 15  \w   -121.00 -96.00   0.50    6.00    --  -49.39 -57.00-150.00   50
 16  \w     94.00 119.00   0.50    6.00    --   49.39  57.00  60.00   50
 17  \w    -18.00  22.00   0.50    6.00    --   49.39 -19.00  60.00   80
 18  \w     40.00  83.00   0.50    6.00    --   49.39-125.00  30.00   86
 19  \w   -151.00-126.00   0.50   24.00    --  -90.00 -77.00  60.00   50
 20  \w    -50.00 -20.00   0.50   24.00    --  -90.00  45.00 -90.00   60
 21  \w    -50.00 -19.00   0.50   24.00    --  -90.00  45.00 -60.00   62
 22  \w     82.00 110.00   0.50   24.00    --  111.50-125.00-150.00   56
 23  \w     43.00  69.00   0.50   24.00    --  111.50-125.00-150.00   52
 24  \w     77.00 106.00   0.50   24.00    --  111.50-106.00 -36.67   58
 25  \w     42.00  67.00   0.50   24.00    --  111.50 -61.00-120.00   50
 26  \w     46.00  75.00   0.50   24.00    --  111.50 -94.00   0.00   58
 27  \w     41.00  72.00   0.50   24.00    --  111.50 -61.00-180.00   62
 28  \w     44.00  71.00   0.50   24.00    --  111.50-106.00 -36.67   54
 29  \w     46.00  72.00   0.50   24.00    --  111.50 -61.00  60.00   52
 30  \w     66.00 111.00   0.50   24.00    --  111.50-125.00 -60.00   90
 31  \w     46.00  72.00   0.50   24.00    --  111.50 -94.00-180.00   52
 32  \w     79.00 104.00   0.50   24.00    --  111.50 -94.00   0.00   50
 33  \w     80.00 105.00   0.50   24.00    --  111.50 -94.00 -30.00   50
 34  \w     44.00 106.00   0.50   24.00    --  111.50-125.00-120.00  124
 35  \w    107.00 137.00   0.50   24.00    --  111.50  45.00-120.00   60
 36  \w     41.00  72.00   0.50   24.00    --  111.50 -61.00 -60.00   62
 37  \w     44.00  82.00   0.50   24.00    --  111.50-125.00-180.00   76
 38  \w    106.00 154.00   0.50   24.00    --  111.50  30.00 120.00   96
 39  \w    133.00 160.00   0.50   24.00    --  111.50   0.00  30.00   54
 40  \w    109.00 177.00   0.50   24.00    --  111.50  15.00  60.00  136
 41  \w     47.00 120.00   0.50   24.00    --  111.50   0.00  30.00  146
 42  \w    132.00 178.00   0.50   24.00    --  111.50  61.00  30.00   92
 43  \w     48.00 104.00   0.50   24.00    --  111.50 -94.00 120.00  112
 44  \w    102.00 174.00   0.50   24.00    --  111.50  45.00 -30.00  144
 45  \w     44.00  69.00   0.50   24.00    --  111.50 -94.00  90.00   50
 46  \w     72.00 102.00   0.50   24.00    --  111.50 -94.00  90.00   60
 47  \w     80.00 105.00   0.50   24.00    --  111.50 -94.00  60.00   50
 48  \w     75.00 105.00   0.50   24.00    --  111.50 -94.00  30.00   60
 49  \w     45.00 109.00   0.50   24.00    --  111.50-125.00 -30.00  128
 50  \w     43.00  68.00   0.50   24.00    --  111.50 -61.00   0.00   50
 51  \w     62.00  96.00   0.50   24.00    --  111.50 -94.00-120.00   68
 52  \w     41.00  72.00   0.50   24.00    --  111.50 -94.00  60.00   62
 53  \w    104.00 172.00   0.50   24.00    --  111.50  30.00  90.00  136
 54  \w    109.00 145.00   0.50   24.00    --  111.50  77.00-180.00   72
 55  \w     44.00 111.00   0.50   24.00    --  111.50-125.00 -90.00  134
 56  \w     79.00 104.00   0.50   24.00    --  111.50 -94.00-180.00   50
 57  \w     79.00 104.00   0.50   24.00    --  111.50 -94.00 -60.00   50
 58  \w    122.00 148.00   0.50   24.00    --  111.50  77.00-120.00   52
 59  \w     41.00  68.00   0.50   24.00    --  111.50 -61.00 150.00   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      -0.0347723000
_diffrn_orient_matrix_UB_12      0.1111639000
_diffrn_orient_matrix_UB_13      0.0053640000
_diffrn_orient_matrix_UB_21      -0.0776185000
_diffrn_orient_matrix_UB_22      -0.0429305000
_diffrn_orient_matrix_UB_23      0.0352774000
_diffrn_orient_matrix_UB_31      0.0638816000
_diffrn_orient_matrix_UB_32      0.0084663000
_diffrn_orient_matrix_UB_33      0.1077073000
_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  0.0542
_diffrn_reflns_av_unetI/netI     0.0268
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            39000
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        66.586
_diffrn_reflns_theta_max         66.586
_diffrn_reflns_theta_min         3.051
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.855
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.534
_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    1.324
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.128
_exptl_crystal_size_min          0.057
_refine_diff_density_max         0.320
_refine_diff_density_min         -0.351
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     353
_refine_ls_number_reflns         4743
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0381
_refine_ls_R_factor_gt           0.0352
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0506P)^2^+1.4523P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0933
_refine_ls_wR_factor_ref         0.0950
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4390
_reflns_number_total             4743
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00072b2.cif
_cod_data_source_block           gr752_100-gg
_cod_depositor_comments
'Adding full bibliography for 7715207--7715212.cif.'
_cod_original_cell_volume        2684.07(11)
_cod_database_code               7715211
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N O B Co'
_shelx_estimated_absorpt_t_max   0.696
_shelx_estimated_absorpt_t_min   0.302
_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. Rigid body (RIGU) restrains
 C31B, N28, C32A, C30A, C30B, C29, C31A, C32B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Sof(C32B)=Sof(H32D)=Sof(H32E)=Sof(H32F)=1-FVAR(1)
 Sof(C32A)=Sof(H32A)=Sof(H32B)=Sof(H32C)=FVAR(1)
 Sof(C31B)=Sof(H31D)=Sof(H31E)=Sof(H31F)=1-FVAR(2)
 Sof(C31A)=Sof(H31A)=Sof(H31B)=Sof(H31C)=FVAR(2)
 Sof(C30A)=Sof(H30A)=Sof(H30B)=Sof(H30C)=1-FVAR(3)
 Sof(C30B)=Sof(H30D)=Sof(H30E)=Sof(H30F)=FVAR(3)
4.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C6(H6A,H6B), C5(H5A,H5B), C3(H3A,H3B), C11(H11A,H11B)
4.b Idealised Me refined as rotating group:
 C31A(H31A,H31B,H31C), C30A(H30A,H30B,H30C), C32A(H32A,H32B,H32C), C31B(H31D,
 H31E,H31F), C30B(H30D,H30E,H30F), C32B(H32D,H32E,H32F), C29(H29A,H29B,H29C)
4.c Boron cage BH refined with riding coordinates:
 C2'(H2'), C2(H2), B6'(H6'), B5(H5), B4'(H4'), B10'(H10'), B5'(H5'),
 B11'(H11'), B4(H4), B12'(H12'), B8'(H8'), B9'(H9'), B11(H11), B6(H6), B9(H9),
 B12(H12), B10(H10), B8(H8)
;
_shelx_res_checksum              69923
_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 1.849
_oxdiff_exptl_absorpt_empirical_full_min 0.571