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_7717350
_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           41
_space_group_name_Hall           'A 2 -2ab'
_space_group_name_H-M_alt        'A e a 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-07-18
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2021.10.07 svn.r9718050b for OlexSys, GUI svn.r6410)
;
_audit_update_record
;
2024-07-18 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                   20.7855(3)
_cell_length_b                   19.9491(3)
_cell_length_c                   11.25789(16)
_cell_measurement_reflns_used    23408
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      79.5620
_cell_measurement_theta_min      4.2180
_cell_volume                     4668.11(12)
_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  (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 1.000
_diffrn_measured_fraction_theta_max 0.990
_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   -114.00 -89.00   0.50    3.50    --  -49.39-147.00 171.00   50
  2  \w    -85.00 -21.00   0.50    3.50    --  -49.39 123.00  56.00  128
  3  \w   -102.00 -25.00   0.50    3.50    --  -49.39 147.00-139.00  154
  4  \w     46.00  86.00   0.50    3.50    --   49.39-147.00 171.00   80
  5  \w     38.00  63.00   0.50    3.50    --   49.39-123.00 -23.00   50
  6  \w   -141.00-116.00   0.50   13.00    --  -90.00-123.00 -23.00   50
  7  \w    -77.00 -52.00   0.50   13.00    --  -90.00 123.00  56.00   50
  8  \w    -75.00 -49.00   0.50   13.00    --  -90.00 147.00-139.00   52
  9  \w   -115.00 -89.00   0.50   13.00    --  -90.00-147.00 171.00   52
 10  \w    115.00 177.00   0.50   13.00    --  111.50 123.00  56.00  124
 11  \w     57.00 127.00   0.50   13.00    --  111.50-147.00 171.00  140
 12  \w     52.00  77.00   0.50   13.00    --  111.50-123.00 -23.00   50
 13  \w    100.00 125.00   0.50   13.00    --  111.50 147.00-139.00   50
 14  \w   -119.00 -90.00   0.50    3.50    --  -49.39 -77.00 -30.00   58
 15  \w    -21.00  23.00   0.50    3.50    --  -49.39  19.00-180.00   88
 16  \w   -121.00 -46.00   0.50    3.50    --  -49.39 -37.00-150.00  150
 17  \w   -118.00 -90.00   0.50    3.50    --  -49.39 -77.00 -60.00   56
 18  \w   -122.00 -43.00   0.50    3.50    --  -49.39 -37.00 -90.00  158
 19  \w     92.00 121.00   0.50    3.50    --   49.39  77.00 150.00   58
 20  \w     41.00  68.00   0.50    3.50    --   49.39  57.00 -30.00   54
 21  \w   -104.00 -78.00   0.50   13.00    --  -90.00 -57.00 -89.64   52
 22  \w   -102.00 -76.00   0.50   13.00    --  -90.00 -61.00 -60.00   52
 23  \w   -101.00 -75.00   0.50   13.00    --  -90.00 -64.00 -86.90   52
 24  \w   -112.00 -74.00   0.50   13.00    --  -90.00 -66.00-102.63   76
 25  \w   -100.00 -75.00   0.50   13.00    --  -90.00 -63.00 -70.10   50
 26  \w   -101.00 -76.00   0.50   13.00    --  -90.00 -61.00 -30.00   50
 27  \w   -154.00-125.00   0.50   13.00    --  -90.00 -66.00-102.63   58
 28  \w   -160.00-130.00   0.50   13.00    --  -90.00 -64.00 -86.90   60
 29  \w   -162.00-108.00   0.50   13.00    --  -90.00 -30.00  30.00  108
 30  \w   -104.00 -78.00   0.50   13.00    --  -90.00 -62.00 -48.15   52
 31  \w   -158.00-132.00   0.50   13.00    --  -90.00 -62.00 -48.15   52
 32  \w     99.00 162.00   0.50   13.00    --  111.50  61.00-120.00  126
 33  \w     98.00 164.00   0.50   13.00    --  111.50  61.00 -60.00  132
 34  \w     64.00  90.00   0.50   13.00    --  111.50 -77.00 120.00   52
 35  \w     42.00  68.00   0.50   13.00    --  111.50 -61.00-120.00   52
 36  \w    133.00 176.00   0.50   13.00    --  111.50  77.00-120.00   86
 37  \w    131.00 176.00   0.50   13.00    --  111.50  77.00-150.00   90
 38  \w     49.00  75.00   0.50   13.00    --  111.50 -94.00   0.00   52
 39  \w     97.00 170.00   0.50   13.00    --  111.50  61.00 -30.00  146
 40  \w     41.00  83.00   0.50   13.00    --  111.50 -94.00  90.00   84
 41  \w     91.00 127.00   0.50   13.00    --  111.50  77.00-120.00   72
 42  \w     93.00 178.00   0.50   13.00    --  111.50  77.00 -90.00  170
 43  \w     52.00 110.00   0.50   13.00    --  111.50-125.00  60.00  116
 44  \w     77.00 111.00   0.50   13.00    --  111.50-125.00-120.00   68
 45  \w     43.00  69.00   0.50   13.00    --  111.50-125.00-120.00   52
 46  \w    102.00 128.00   0.50   13.00    --  111.50  61.00 150.00   52
 47  \w     95.00 138.00   0.50   13.00    --  111.50 125.00 150.00   86
 48  \w     98.00 126.00   0.50   13.00    --  111.50  77.00-150.00   56
 49  \w    143.00 170.00   0.50   13.00    --  111.50  77.00 -60.00   54
 50  \w     92.00 118.00   0.50   13.00    --  111.50  77.00 -60.00   52
 51  \w     97.00 145.00   0.50   13.00    --  111.50  61.00 -90.00   96
 52  \w     49.00 102.00   0.50   13.00    --  111.50 -94.00 150.00  106
 53  \w    143.00 177.00   0.50   13.00    --  111.50  61.00 150.00   68
 54  \w    135.00 170.00   0.50   13.00    --  111.50  45.00-150.00   70
 55  \w     44.00  72.00   0.50   13.00    --  111.50 -61.00  90.00   56
 56  \w    104.00 166.00   0.50   13.00    --  111.50  30.00  90.00  124
 57  \w    114.00 173.00   0.50   13.00    --  111.50  15.00  60.00  118
 58  \w     95.00 147.00   0.50   13.00    --  111.50  77.00 -30.00  104
 59  \w    136.00 161.00   0.50   13.00    --  111.50  30.00 120.00   50
 60  \w     45.00 111.00   0.50   13.00    --  111.50 -77.00 -60.00  132
 61  \w    128.00 177.00   0.50   13.00    --  111.50  45.00 150.00   98
 62  \w     44.00  70.00   0.50   13.00    --  111.50 -61.00 -60.00   52
 63  \w    106.00 132.00   0.50   13.00    --  111.50 -77.00 120.00   52
 64  \w     44.00  69.00   0.50   13.00    --  111.50 -61.00   0.00   50
 65  \w     45.00  70.00   0.50   13.00    --  111.50 -61.00-180.00   50
;
_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      0.0708791000
_diffrn_orient_matrix_UB_12      0.0182682000
_diffrn_orient_matrix_UB_13      0.0233295000
_diffrn_orient_matrix_UB_21      0.0205944000
_diffrn_orient_matrix_UB_22      -0.0432941000
_diffrn_orient_matrix_UB_23      -0.1067134000
_diffrn_orient_matrix_UB_31      -0.0066232000
_diffrn_orient_matrix_UB_32      0.0613617000
_diffrn_orient_matrix_UB_33      -0.0822724000
_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  0.0696
_diffrn_reflns_av_unetI/netI     0.0364
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            41813
_diffrn_reflns_point_group_measured_fraction_full 0.946
_diffrn_reflns_point_group_measured_fraction_max 0.926
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.624
_diffrn_reflns_theta_min         4.254
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.756
_exptl_absorpt_correction_T_max  0.962
_exptl_absorpt_correction_T_min  0.350
_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    1.275
_exptl_crystal_description       prism
_exptl_crystal_F_000             1840
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.068
_refine_diff_density_max         0.789
_refine_diff_density_min         -0.522
_refine_diff_density_rms         0.075
_refine_ls_abs_structure_details
;
 Flack x determined using 1838 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.013(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     309
_refine_ls_number_reflns         4759
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0493
_refine_ls_R_factor_gt           0.0473
_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^)+(0.0919P)^2^+4.6442P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1312
_refine_ls_wR_factor_ref         0.1344
_reflns_Friedel_coverage         0.775
_reflns_Friedel_fraction_full    0.886
_reflns_Friedel_fraction_max     0.853
_reflns_number_gt                4559
_reflns_number_total             4759
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02588a2.cif
_cod_data_source_block           gr-db-732-3-f2-gg
_cod_depositor_comments
'Adding full bibliography for 7717349--7717350.cif.'
_cod_original_cell_volume        4668.09(11)
_cod_original_sg_symbol_Hall     'A 2 -2ac'
_cod_database_code               7717350
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C10 H32 B18 Co N3'
_shelx_estimated_absorpt_t_max   0.696
_shelx_estimated_absorpt_t_min   0.286
_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. Uiso/Uaniso restraints and constraints
Uanis(C4B) = Uanis(C4A)
3. Others
 Sof(C4A)=Sof(H4AA)=Sof(H4AB)=Sof(H4AC)=1-FVAR(1)
 Sof(C4B)=Sof(H4BA)=Sof(H4BB)=Sof(H4BC)=FVAR(1)
 Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=1-FVAR(2)
 Sof(C1B)=Sof(H1BA)=Sof(H1BB)=Sof(H1BC)=FVAR(2)
4.a Idealised Me refined as rotating group:
 C2AB(H2AA,H2AB,H2AC), C3AB(H3AA,H3AB,H3AC), C1A(H1AA,H1AB,H1AC), C4A(H4AA,
 H4AB,H4AC), C4B(H4BA,H4BB,H4BC), C1B(H1BA,H1BB,H1BC)
4.b Boron cage BH refined with riding coordinates:
 C2(H2), C2'(H2'), B4(H4), B11'(H11'), B8'(H8'), B7(H7), B8(H8), B4'(H4'),
 B10'(H10'), B6'(H6'), B7'(H7'), B5(H5), B5'(H5'), B9'(H9'), B10(H10), B6(H6),
 B12'(H12'), B9(H9), B12(H12), B11(H11)
;
_shelx_res_checksum              55496
_shelx_hkl_checksum              40394
_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 2.602
_oxdiff_exptl_absorpt_empirical_full_min 0.536