Crystalline radical cations of bis-BN-based analogues of Thiele's hydrocarbon
Xie, Zhuofeng; Dai, Yuyang; Bao, Manling; Feng, Zhongtao; Wang, Wenjuan; Liu, Chunmeng; Wang, Xinping; Su, Yuanting; Chemical Communications  (2022) –; doi:10.1039/D2CC01254E

data_7129975
_publ_section_title
;
 Crystalline radical cations of bis-BN-based analogues of Thiele's
 hydrocarbon
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC01254E
_journal_year                    2022
_chemical_formula_moiety         '2(C28 H38 B N3), F6 Sb'
_chemical_formula_sum            'C56 H76 B2 F6 N6 Sb'
_chemical_formula_weight         1090.59
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-01-28
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-02-28 deposited with the CCDC.	2022-03-30 downloaded from the CCDC.
;
_cell_angle_alpha                97.006(2)
_cell_angle_beta                 103.374(2)
_cell_angle_gamma                109.486(2)
_cell_formula_units_Z            2
_cell_length_a                   10.4503(9)
_cell_length_b                   13.9363(12)
_cell_length_c                   22.1346(19)
_cell_measurement_reflns_used    9782
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      53.92
_cell_measurement_theta_min      4.06
_cell_volume                     2886.1(4)
_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      140.0
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0681
_diffrn_reflns_av_unetI/netI     0.0634
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            44616
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         53.952
_diffrn_reflns_theta_min         1.828
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.868
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'bluwise purple'
_exptl_crystal_density_diffrn    1.255
_exptl_crystal_description       block
_exptl_crystal_F_000             1138
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.298
_refine_diff_density_min         -0.946
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     675
_refine_ls_number_reflns         10281
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      1.115
_refine_ls_R_factor_all          0.0485
_refine_ls_R_factor_gt           0.0482
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0739P)^2^+2.5043P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1300
_refine_ls_wR_factor_ref         0.1304
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10127
_reflns_number_total             10281
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc01254e2.cif
_cod_data_source_block           1radicalcation
_cod_database_code               7129975
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.762
_shelx_estimated_absorpt_t_min   0.598
_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. Restrained distances
 C17-C19A \\sim C19-C17
 with sigma of 0.02
 C18-C17 \\sim C18A-C17
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C19 \\sim C19A: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
C18 \\sim C18A: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
4. Rigid body (RIGU) restrains
 C17, C19, C19A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C17, C18, C18A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
5. Others
 Sof(H17)=Sof(C18A)=Sof(H18D)=Sof(H18E)=Sof(H18F)=Sof(C19A)=Sof(H19D)=
 Sof(H19E)=Sof(H19F)=1-FVAR(1)
 Sof(H17A)=Sof(C18)=Sof(H18A)=Sof(H18B)=Sof(H18C)=Sof(C19)=Sof(H19A)=Sof(H19B)=
 Sof(H19C)=FVAR(1)
6.a Riding coordinates:
 C18A(H18D,H18E,H18F), C19A(H19D,H19E,H19F)
6.b Ternary CH refined with riding coordinates:
 C17(H17A), C17(H17), C20(H20), C23(H23), C26(H26), C45(H45), C48(H48),
 C51(H51), C54(H54)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C9(H9), C10(H10), C11(H11), C13(H13), C14(H14),
 C15(H15), C16(H16), C31(H31), C32(H32), C33(H33), C37(H37), C38(H38), C39(H39),
  C41(H41), C42(H42), C43(H43), C44(H44)
6.d Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C21(H21A,H21B,H21C), C22(H22A,H22B,
 H22C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C27(H27A,H27B,H27C), C28(H28A,
 H28B,H28C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C49(H49A,H49B,H49C),
 C50(H50A,H50B,H50C), C52(H52A,H52B,H52C), C53(H53A,H53B,H53C), C55(H55A,H55B,
 H55C), C56(H56A,H56B,H56C)
;
_shelx_res_checksum              38320
_shelx_hkl_checksum              22114
_olex2_submission_special_instructions 'No special instructions were received'