Modification of cobalt bis(dicarbollide) ions with nitrile groups on carbon atoms: a unique low-temperature skeletal rearrangement due to the specific electron-donor character of CN substitution.
Tüzün, Ece Zeynep; Hnyk, Drahomír; Bavol, Dmytro; Litecká, Miroslava; Fanfrlík, Jindřich; Grűner, Bohumír; Dalton transactions (Cambridge, England : 2003) 53 (2024) 18462–18466; doi:10.1039/d4dt02588a

data_7717349
_publ_section_title
;
 Modification of cobalt bis(dicarbollide) ions with nitrile groups on
 carbon atoms: a unique low-temperature skeletal rearrangement due to the
 specific electron-donor character of CN substitution.
;
_journal_issue                   46
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              18462
_journal_page_last               18466
_journal_paper_doi               10.1039/d4dt02588a
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C6 H20 B18 Co N2, C4 H12 N'
_chemical_formula_sum            'C10 H32 B18 Co N3'
_chemical_formula_weight         447.89
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-07-11
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2021.10.07 svn.r9718050b for OlexSys, GUI svn.r6410)
;
_audit_update_record
;
2024-07-12 deposited with the CCDC.	2024-10-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.3386(3)
_cell_length_b                   10.7908(2)
_cell_length_c                   20.2460(3)
_cell_measurement_reflns_used    19173
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      77.6070
_cell_measurement_theta_min      4.1210
_cell_volume                     4661.86(13)
_computing_cell_refinement       'CrysAlisPro 1.171.43.105a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.104a 64-bit (release 22-12-2023))'
_computing_data_reduction        'CrysAlisPro 1.171.43.105a (Rigaku OD, 2024)'
_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 0.951
_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   -117.00 -60.00   0.50   10.00    --  -49.64 -68.00-151.00  114
  2  \w    -12.00  19.00   0.50   10.00    --  -49.64  68.00 -19.00   62
  3  \w     65.00  91.00   0.50   10.00    --   49.64  68.00 -19.00   52
  4  \w     -3.00  26.00   0.50   10.00    --   49.64 -68.00-151.00   58
  5  \w    -45.00 -18.00   0.50   40.00    --  -90.00  68.00 -19.00   54
  6  \w   -145.00-115.00   0.50   40.00    --  -90.00 -68.00-151.00   60
  7  \w    100.00 178.00   0.50   40.00    --  107.54  68.00 -19.00  156
  8  \w     42.00  80.00   0.50   40.00    --  107.54 -68.00-151.00   76
  9  \w   -117.00 -81.00   0.50   10.00    --  -49.64-125.00 -90.00   72
 10  \w   -120.00 -95.00   0.50   10.00    --  -49.64 -77.00 -30.00   50
 11  \w   -120.00 -90.00   0.50   10.00    --  -49.64 -77.00  90.00   60
 12  \w   -119.00 -89.00   0.50   10.00    --  -49.64 -77.00 -90.00   60
 13  \w    -86.00 -34.00   0.50   40.00    --  -90.00 125.00  30.00  104
 14  \w    -66.00 -18.00   0.50   40.00    --  -90.00  57.00  30.00   96
 15  \w   -118.00 -93.00   0.50   40.00    --  -90.00 -99.00   0.00   50
 16  \w    -66.00 -18.00   0.50   40.00    --  -90.00  57.00-180.00   96
 17  \w   -132.00 -91.00   0.50   40.00    --  -90.00 -99.00 -90.00   82
 18  \w    -66.00 -26.00   0.50   40.00    --  -90.00  57.00 -60.00   80
 19  \w    -63.00 -27.00   0.50   40.00    --  -90.00  57.00 150.00   72
 20  \w    -62.00 -21.00   0.50   40.00    --  -90.00 125.00   0.00   82
 21  \w   -146.00-101.00   0.50   40.00    --  -90.00 -77.00 -90.00   90
 22  \w    113.00 139.00   0.50   40.00    --  107.54  37.00 -90.00   52
 23  \w    106.00 143.00   0.50   40.00    --  107.54 125.00 150.00   74
 24  \w     36.00  62.00   0.50   40.00    --  107.54 -57.00  60.00   52
 25  \w     36.00  62.00   0.50   40.00    --  107.54 -57.00  30.00   52
 26  \w     75.00 107.00   0.50   40.00    --  107.54 -99.00   0.00   64
 27  \w     36.00  61.00   0.50   40.00    --  107.54 -57.00 -90.00   50
 28  \w    145.00 176.00   0.50   40.00    --  107.54  37.00 -90.00   62
;
_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      0.0043317000
_diffrn_orient_matrix_UB_12      0.1145822000
_diffrn_orient_matrix_UB_13      -0.0451947000
_diffrn_orient_matrix_UB_21      -0.0561032000
_diffrn_orient_matrix_UB_22      -0.0479252000
_diffrn_orient_matrix_UB_23      -0.0404958000
_diffrn_orient_matrix_UB_31      -0.0452479000
_diffrn_orient_matrix_UB_32      0.0704022000
_diffrn_orient_matrix_UB_33      0.0458904000
_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  0.0302
_diffrn_reflns_av_unetI/netI     0.0193
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            34211
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.001
_diffrn_reflns_theta_min         4.144
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.764
_exptl_absorpt_correction_T_max  0.844
_exptl_absorpt_correction_T_min  0.706
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.105a (Rigaku Oxford Diffraction, 2024)
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    1.276
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1840
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.188
_refine_diff_density_min         -0.572
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     293
_refine_ls_number_reflns         4798
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0463
_refine_ls_R_factor_gt           0.0438
_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^)+(0.0725P)^2^+4.9509P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1264
_refine_ls_wR_factor_ref         0.1283
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4486
_reflns_number_total             4798
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02588a2.cif
_cod_data_source_block           gr732-10m-gg
_cod_depositor_comments
'Adding full bibliography for 7717349--7717350.cif.'
_cod_database_code               7717349
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C10 H32 N3 Co'
_shelx_estimated_absorpt_t_max   0.724
_shelx_estimated_absorpt_t_min   0.596
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C)
2.b Boron cage BH refined with riding coordinates:
 C1'(H1'), C2'(H2'), B3(H3), B7'(H7'), B11(H11), B6(H6), B7(H7), B4'(H4'),
 B8'(H8'), B4(H4), B10(H10), B5(H5), B12(H12), B5'(H5'), B9'(H9'), B9(H9),
 B6'(H6'), B12'(H12'), B10'(H10'), B11'(H11')
;
_shelx_res_checksum              8827
_shelx_hkl_checksum              9277
_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 1.482
_oxdiff_exptl_absorpt_empirical_full_min 0.801