Completing the series of boron-nucleophilic cyanoborates: Boryl anions of type (NHC)−B(CN)2−
Böser, Richard; Haufe, Lisa Cathrin; Freytag, Matthias; Jones, P. G.; Hörner, Gerald; René, Frank; Chem. Sci.  (2017) –; doi:10.1039/C7SC02238G

data_1546452
_publ_section_title
;
 Completing the series of boron-nucleophilic cyanoborates: Boryl anions of
 type (NHC)&#x2212;B(CN)2&#x2212;
;
_journal_name_full               'Chem. Sci.'
_journal_paper_doi               10.1039/C7SC02238G
_journal_year                    2017
_chemical_formula_sum            'C243 H296 B9 K9 N36 O4'
_chemical_formula_weight         4234.35
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2017-05-17 deposited with the CCDC.
2017-07-03 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 106.881(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   33.0927(5)
_cell_length_b                   30.3266(4)
_cell_length_c                   25.1212(4)
_cell_measurement_reflns_used    137157
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      76.0780
_cell_measurement_theta_min      3.2040
_cell_volume                     24125.0(7)
_computing_cell_refinement
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) 
(compiled Aug 13 2014,18:06:01) 
;
_computing_data_collection
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) 
(compiled Aug 13 2014,18:06:01) 
;
_computing_data_reduction
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) 
(compiled Aug 13 2014,18:06:01) 
;
_computing_molecular_graphics    'Bruker XP'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.3543
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur, Atlas, Nova'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0662
_diffrn_reflns_av_sigmaI/netI    0.0284
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            563295
_diffrn_reflns_theta_full        75.00
_diffrn_reflns_theta_max         76.36
_diffrn_reflns_theta_min         3.21
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.898
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78658
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) 
(compiled Aug 13 2014,18:06:01) 
;
_exptl_crystal_colour            'intense red'
_exptl_crystal_density_diffrn    1.166
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'cut prism'
_exptl_crystal_F_000             9016
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
Several badly resolved regions of residual electron density were 
tentatively identified as four molecules of THF, another as four molecules 
of penane, but could not be refined satisfactorily. For this reason the 
program SQUEEZE (part of the PLATON suite; A. Spek, University of Utrecht, 
Netherlands, 2009) was used to remove mathematically the effects of the 
solvents.
Derived parameters such as the formular weight correspond to 16 molecules 
of THF and 16 molecules of pentane per cell.
;
_refine_diff_density_max         0.207
_refine_diff_density_min         -0.267
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     2404
_refine_ls_number_reflns         50397
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0474
_refine_ls_R_factor_gt           0.0390
_refine_ls_shift/su_max          0.073
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0550P)^2^+4.0894P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0968
_refine_ls_wR_factor_ref         0.1013
_reflns_number_gt                43480
_reflns_number_total             50397
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7sc02238g2.cif
_cod_data_source_block           rene07
_cod_original_cell_volume        24125.0(6)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1546452