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_7246898
_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         'C H9 B9 Cl, C6 H7 Cl N'
_chemical_formula_sum            'C7 H16 B9 Cl2 N'
_chemical_formula_weight         282.40
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2023-05-18 deposited with the CCDC.	2023-06-15 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 102.4150(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.9849(2)
_cell_length_b                   14.3250(3)
_cell_length_c                   10.8831(2)
_cell_measurement_reflns_used    9751
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      2.51
_cell_volume                     1520.25(5)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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_collimation    miracol
_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  0.0759
_diffrn_reflns_av_sigmaI/netI    0.0670
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            17724
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.51
_exptl_absorpt_coefficient_mu    0.401
_exptl_absorpt_correction_T_max  0.9490
_exptl_absorpt_correction_T_min  0.8240
_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    1.234
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             576
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.384
_refine_diff_density_min         -0.428
_refine_diff_density_rms         0.052
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.65(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     471
_refine_ls_number_reflns         6746
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0591
_refine_ls_R_factor_gt           0.0482
_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^)+(0.0762P)^2^+0.0181P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1184
_refine_ls_wR_factor_ref         0.1250
_reflns_number_gt                5817
_reflns_number_total             6746
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d3ce00357d2.cif
_cod_data_source_block           1i_af32a
_cod_depositor_comments
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The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Monoclinic' was changed to
'monoclinic' 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.
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_cod_original_sg_symbol_H-M      P21
_cod_database_code               7246898