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_7715207
_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         'C5 H23 B18 Co I, C4 H12 N'
_chemical_formula_sum            'C9 H35 B18 Co I N'
_chemical_formula_weight         537.79
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yc'
_space_group_name_H-M_alt        'P 1 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                 95.816(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.0665(2)
_cell_length_b                   10.5685(3)
_cell_length_c                   10.2132(2)
_cell_measurement_reflns_used    13649
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      78.4510
_cell_measurement_theta_min      3.9850
_cell_volume                     1188.35(5)
_computing_cell_refinement       'CrysAlisPro 1.171.42.66a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.66a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.66a (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 0.999
_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    -90.00 -16.00   0.50    5.00    --  -50.65 131.00  30.00  148
  2  \w   -120.00 -70.00   0.50    5.00    --  -50.65-131.00 -40.00  100
  3  \w    -95.00 -19.00   0.50    5.00    --  -50.65 137.00-153.00  152
  4  \w   -121.00 -66.00   0.50    5.00    --  -50.65-137.00 143.00  110
  5  \w     38.00  97.00   0.50    5.00    --   50.65-131.00 -40.00  118
  6  \w     41.00 102.00   0.50    5.00    --   50.65-137.00 143.00  122
  7  \w   -160.00 -70.00   0.50   20.00    --  -90.00-131.00 -40.00  180
  8  \w    -91.00 -20.00   0.50   20.00    --  -90.00 131.00  30.00  142
  9  \w   -159.00 -66.00   0.50   20.00    --  -90.00-137.00 143.00  186
 10  \w     38.00 116.00   0.50   20.00    --  107.79-131.00 -40.00  156
 11  \w     91.00 178.00   0.50   20.00    --  107.79 131.00  30.00  174
 12  \w     87.00 178.00   0.50   20.00    --  107.79 137.00-153.00  182
 13  \w     41.00 120.00   0.50   20.00    --  107.79-137.00 143.00  158
 14  \w    -23.00  21.00   0.50    5.00    --  -50.65  19.00 120.00   88
 15  \w   -121.00 -89.00   0.50    5.00    --  -50.65 -77.00-150.00   64
 16  \w    -23.00  21.00   0.50    5.00    --  -50.65  19.00 -60.00   88
 17  \w     89.00 121.00   0.50    5.00    --   50.65  77.00   0.00   64
 18  \w     89.00 121.00   0.50    5.00    --   50.65  77.00 -60.00   64
 19  \w   -159.00 -80.00   0.50   20.00    --  -90.00-125.00-180.00  158
 20  \w   -138.00 -83.00   0.50   20.00    --  -90.00   0.00   0.00  110
 21  \w   -138.00 -83.00   0.50   20.00    --  -90.00   0.00-180.00  110
 22  \w   -138.00 -83.00   0.50   20.00    --  -90.00   0.00 120.00  110
 23  \w     36.00  66.00   0.50   20.00    --  107.79 -57.00 -90.00   60
 24  \w     36.00  66.00   0.50   20.00    --  107.79 -57.00  30.00   60
 25  \w     38.00 106.00   0.50   20.00    --  107.79 -99.00-180.00  136
 26  \w     36.00  66.00   0.50   20.00    --  107.79 -57.00   0.00   60
 27  \w     36.00  66.00   0.50   20.00    --  107.79 -57.00 -60.00   60
 28  \w     38.00 106.00   0.50   20.00    --  107.79 -99.00   0.00  136
 29  \w     38.00 106.00   0.50   20.00    --  107.79 -99.00-150.00  136
 30  \w     36.00  66.00   0.50   20.00    --  107.79 -57.00-180.00   60
 31  \w     95.00 177.00   0.50   20.00    --  107.79 125.00 -60.00  164
 32  \w     89.00 178.00   0.50   20.00    --  107.79  77.00 -90.00  178
 33  \w     38.00 106.00   0.50   20.00    --  107.79 -99.00 120.00  136
 34  \w     38.00 106.00   0.50   20.00    --  107.79 -99.00  30.00  136
 35  \w     36.00  66.00   0.50   20.00    --  107.79 -57.00 -30.00   60
 36  \w   -121.00 -39.00   0.50    5.00    --  -50.65 -57.00  90.00  164
 37  \w   -121.00 -39.00   0.50    5.00    --  -50.65 -57.00   0.00  164
 38  \w   -121.00 -39.00   0.50    5.00    --  -50.65 -57.00-180.00  164
 39  \w   -121.00 -39.00   0.50    5.00    --  -50.65 -57.00 -90.00  164
 40  \w   -121.00 -81.00   0.50    5.00    --  -50.65 -57.00 120.00   80
 41  \w     39.00 121.00   0.50    5.00    --   50.65  57.00 -90.00  164
;
_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      0.0132049000
_diffrn_orient_matrix_UB_12      -0.1451720000
_diffrn_orient_matrix_UB_13      0.0050349000
_diffrn_orient_matrix_UB_21      0.1392570000
_diffrn_orient_matrix_UB_22      0.0136282000
_diffrn_orient_matrix_UB_23      0.0156098000
_diffrn_orient_matrix_UB_31      -0.0006142000
_diffrn_orient_matrix_UB_32      0.0035514000
_diffrn_orient_matrix_UB_33      0.1506934000
_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  0.0580
_diffrn_reflns_av_unetI/netI     0.0358
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            20291
_diffrn_reflns_point_group_measured_fraction_full 0.850
_diffrn_reflns_point_group_measured_fraction_max 0.850
_diffrn_reflns_theta_full        66.597
_diffrn_reflns_theta_max         66.597
_diffrn_reflns_theta_min         4.015
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    15.795
_exptl_absorpt_correction_T_max  0.804
_exptl_absorpt_correction_T_min  0.597
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.66a (Rigaku Oxford Diffraction, 2022)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
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    1.503
_exptl_crystal_description       needle
_exptl_crystal_F_000             532
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.001
_refine_diff_density_min         -0.605
_refine_diff_density_rms         0.131
_refine_ls_abs_structure_details
;
 Flack x determined using 1264 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.030(12)
_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     279
_refine_ls_number_reflns         3565
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0518
_refine_ls_R_factor_gt           0.0485
_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^)+(0.1092P)^2^+0.2550P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1328
_refine_ls_wR_factor_ref         0.1374
_reflns_Friedel_coverage         0.697
_reflns_Friedel_fraction_full    0.700
_reflns_Friedel_fraction_max     0.700
_reflns_number_gt                3297
_reflns_number_total             3565
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00072b2.cif
_cod_data_source_block           jn-q2-17_02_cu_100-aa-fm
_cod_depositor_comments
'Adding full bibliography for 7715207--7715212.cif.'
_cod_database_code               7715207
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C9 H35 N Co B18 I'
_shelx_estimated_absorpt_t_max   0.743
_shelx_estimated_absorpt_t_min   0.571
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 I2-C3
 2.13 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
I1 \\sim I2: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 2A
Uanis(I1) = Uanis(I2)
4. Others
 Sof(H3AA)=Sof(H3AB)=Sof(I1)=1-FVAR(1)
 Sof(H3BC)=Sof(H3BD)=Sof(I2)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C3(H3AA,H3AB), C3(H3BC,H3BD)
5.b Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C4(H4A,H4B,H4C)
5.c Boron cage BH refined with riding coordinates:
 B4(H4), B7(H7), C1'(H1'), B8(H8), B10'(H10'), C2(H2), B6'(H6'), B5'(H5'),
 B12(H12), B8'(H8'), B7'(H7'), C2'(H2'), B6(H6), B11'(H11'), B9(H9), B12'(H12'),
  B4'(H4'), B11(H11), B5(H5), B10(H10), B9'(H9')
;
_shelx_res_checksum              70801
_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 2.005
_oxdiff_exptl_absorpt_empirical_full_min 0.637