Substituent effects on the [1-closo-CB9H10]− anion geometry: experimental and DFT studies
Pietrzak, Anna; Carr, Michael J.; Kaszyński, Piotr; CrystEngComm 25 (2023) 3790–3798; doi:10.1039/D3CE00357D

data_7246900
_publ_section_title
;
 Substituent effects on the [1-closo-CB9H10]&#x2212; anion geometry:
 experimental and DFT studies
;
_journal_issue                   26
_journal_name_full               CrystEngComm
_journal_page_first              3790
_journal_page_last               3798
_journal_paper_doi               10.1039/D3CE00357D
_journal_volume                  25
_journal_year                    2023
_chemical_formula_moiety         '2(C7 H15 B9 N3), 4(C8 H20 N), 2Br'
_chemical_formula_sum            'C46 H110 B18 Br2 N10'
_chemical_formula_weight         1157.84
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2022-11-21 deposited with the CCDC.	2023-06-15 downloaded from the CCDC.
;
_cell_angle_alpha                104.577(5)
_cell_angle_beta                 92.623(4)
_cell_angle_gamma                90.179(5)
_cell_formula_units_Z            2
_cell_length_a                   9.06020(10)
_cell_length_b                   16.88030(10)
_cell_length_c                   22.9672(2)
_cell_measurement_reflns_used    12321
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.00
_cell_measurement_theta_min      2.89
_cell_volume                     3395.56(9)
_computing_cell_refinement
;
  DENZO-SMN and COLLECT (Otwinowski & Minor, 1996)
;
_computing_data_collection
;
  DENZO-SMN and COLLECT (Otwinowski & Minor, 1996)
;
_computing_data_reduction
;
  DENZO-SMN and COLLECT (Otwinowski & Minor, 1996)
;
_computing_molecular_graphics
;
  ORTEP3 for Windows (Farrugia, 1997)
  XSeed (Barbour, 2001)
;
_computing_publication_material
;
 'enCIFer (CCDC, 2002)'
;
_computing_structure_refinement
;
  SHELXS-97 (Sheldrick, 1986)
;
_computing_structure_solution
;
  SHELXS-97 (Sheldrick, 1986)
;
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method
;
   Detector set at 30mm from sample with different 2theta offsets 
   1 degree phi exposures for chi=0 degree settings
   1 degree omega exposures for chi=90 degree settings
;
_diffrn_radiation_detector       'CCD plate'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1058
_diffrn_reflns_av_sigmaI/netI    0.0794
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            42246
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.89
_exptl_absorpt_coefficient_mu    1.232
_exptl_absorpt_correction_T_max  0.9187
_exptl_absorpt_correction_T_min  0.4969
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 Using multiple and symmetry-related data measurements via the program SORTAV
 See R.H. Blessing, Acta Cryst (1995), A51, 33-38 
;
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.132
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1232
_exptl_crystal_size_max          0.66
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.734
_refine_diff_density_min         -0.713
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     853
_refine_ls_number_reflns         13239
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0754
_refine_ls_R_factor_gt           0.0579
_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^)+(0.0654P)^2^+2.9989P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1417
_refine_ls_wR_factor_ref         0.1563
_reflns_number_gt                10459
_reflns_number_total             13239
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d3ce00357d2.cif
_cod_data_source_block           1j_AF79Ai
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Triclinic' was changed to
'triclinic' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 7246896--7246900.cif.
;
_cod_original_cell_volume        3395.56(5)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7246900