An air-stable N-heterocyclic carbene iminoxyl borate radical zwitterion.
Kim, Youngsuk; Lee, Eunsung; Chemical communications (Cambridge, England) 54 (2018) 6824–6827; doi:10.1039/c8cc01399c

data_7121447
_publ_section_title
;
 An air-stable N-heterocyclic carbene iminoxyl borate radical zwitterion.
;
_journal_issue                   50
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              6824
_journal_page_last               6827
_journal_paper_doi               10.1039/c8cc01399c
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         'C45 H36 B F15 N3 O, C5 H12'
_chemical_formula_sum            'C50 H48 B F15 N3 O'
_chemical_formula_weight         1002.72
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-06-22
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2018-02-10 deposited with the CCDC.
2018-03-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.18(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.812(3)
_cell_length_b                   20.438(4)
_cell_length_c                   15.737(3)
_cell_measurement_reflns_used    53024
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.092
_cell_measurement_theta_min      1.611
_cell_volume                     4751.4(16)
_computing_cell_refinement       HKL3000
_computing_data_collection       'PAL ADSC Quantum-210 ADX Program'
_computing_data_reduction        HKL3000
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.933
_diffrn_measured_fraction_theta_max 0.942
_diffrn_measurement_device_type  PAL-2D
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_monochromator  'Si(111) double crystal monochromator'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.700
_diffrn_reflns_av_R_equivalents  0.0351
_diffrn_reflns_av_unetI/netI     0.0372
_diffrn_reflns_Laue_measured_fraction_full 0.933
_diffrn_reflns_Laue_measured_fraction_max 0.942
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            34273
_diffrn_reflns_point_group_measured_fraction_full 0.933
_diffrn_reflns_point_group_measured_fraction_max 0.942
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.092
_diffrn_reflns_theta_min         1.611
_diffrn_source                   'PLSII 2D bending magnet'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.120
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'dark brown'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.402
_exptl_crystal_description       block
_exptl_crystal_F_000             2068
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.343
_refine_diff_density_min         -0.466
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     641
_refine_ls_number_reflns         12560
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0671
_refine_ls_R_factor_gt           0.0558
_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^)+(0.1071P)^2^+1.6145P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1699
_refine_ls_wR_factor_ref         0.1788
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10155
_reflns_number_total             12560
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc01399c2.cif
_cod_data_source_block           p21n
_cod_depositor_comments
'Adding full bibliography for 7121447--7121448.cif.'
_cod_original_cell_volume        4751.4(17)
_cod_database_code               7121447
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C012(H012), C017(H017), C01A(H01A), C01G(H01I)
2.b Secondary CH2 refined with riding coordinates:
 C01Q(H0AA,H), C01S(H1AA,HA), C01T(H2AA,HB)
2.c Aromatic/amide H refined with riding coordinates:
 C00O(H00O), C00R(H00R), C00U(H00U), C014(H014), C01E(H01E), C01H(H01J),
 C01M(H01N), C01X(H01)
2.d Idealised Me refined as rotating group:
 C01D(H01B,H01C,H01D), C01F(H01F,H01G,H01H), C01L(H01K,H01L,H01M), C01N(H01O,
 H01P,H01Q), C01O(H01R,H01S,H01T), C01R(H01U,H01V,H01W), C01U(H01X,H01Y,HC),
 C01V(H01Z,HD,HE), C01W(H3AA,HF,HG), C01Y(H4AA,HH,HI)
;
_olex2_submission_special_instructions 'No special instructions were received'