Fusing 10-vertex closo-Carborane Anions with N-Heterocyclic Carbenes
Tej, Varun; McArthur, Sarah; Banda, Isaac; Gregory, Aaron; Fisher, Steven P.; McArthur, Scott; Lavallo, Vince; Chemical Communications  (2022) –; doi:10.1039/D2CC02596E

data_7130537
_publ_section_title
;
 Fusing 10-vertex closo-Carborane Anions with N-Heterocyclic Carbenes
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC02596E
_journal_year                    2022
_chemical_formula_sum            'C33 H76 B18 K2 N2 O7'
_chemical_formula_weight         885.73
_space_group_crystal_system      orthorhombic
_space_group_IT_number           40
_space_group_name_Hall           'A 2 -2a'
_space_group_name_H-M_alt        'A m a 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2018-06-11 deposited with the CCDC.	2022-08-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   60.951(6)
_cell_length_b                   17.6644(17)
_cell_length_c                   9.8809(10)
_cell_measurement_reflns_used    9992
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      26.67
_cell_measurement_theta_min      2.36
_cell_volume                     10638.4(18)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0275
_diffrn_reflns_av_unetI/netI     0.0132
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       75
_diffrn_reflns_limit_h_min       -75
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            129683
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.022
_diffrn_reflns_theta_min         2.005
_exptl_absorpt_coefficient_mu    0.219
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.106
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'prism frag'
_exptl_crystal_F_000             3776
_exptl_crystal_size_max          0.589
_exptl_crystal_size_mid          0.559
_exptl_crystal_size_min          0.478
_exptl_transmission_factor_max   0.942
_exptl_transmission_factor_min   0.859
_refine_diff_density_max         0.589
_refine_diff_density_min         -0.311
_refine_diff_density_rms         0.048
_refine_ls_abs_structure_details
; 
 Flack x determined using 4263 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons and Flack (2004), Acta Cryst. A60, s61). 
;
_refine_ls_abs_structure_Flack   0.038(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     775
_refine_ls_number_reflns         10591
_refine_ls_number_restraints     971
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.0630
_refine_ls_R_factor_gt           0.0590
_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^)+(0.1116P)^2^+3.5383P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1698
_refine_ls_wR_factor_ref         0.1747
_reflns_Friedel_coverage         0.886
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                9804
_reflns_number_total             10591
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc02596e1.cif
_cod_data_source_block           vL157SL_70A_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_cell_volume        10638.3(18)
_cod_database_code               7130537
_shelx_estimated_absorpt_t_min   0.882
_shelx_estimated_absorpt_t_max   0.903
_shelxl_version_number           2013-4
_shelx_res_checksum              50229
_shelx_hkl_checksum              61388