Insertion reactions of the C-B-N-substituted borinium cation [MesBN<sup>i</sup>Pr<sub>2</sub>]<sup/>.
Bamford, Karlee L.; Stephan, Douglas W.; Dalton transactions (Cambridge, England : 2003) 49 (2020) 17571–17577; doi:10.1039/d0dt03665j

data_7705789
_publ_section_title
;
 Insertion reactions of the C-B-N-substituted borinium cation
 [MesBN<sup>i</sup>Pr<sub>2</sub>]<sup/>.
;
_journal_issue                   48
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17571
_journal_page_last               17577
_journal_paper_doi               10.1039/d0dt03665j
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'B C24 F20, C17 H18 N, 1.5(C6 H4 Cl2)'
_chemical_formula_sum            'C50 H24 B Cl3 F20 N'
_chemical_formula_weight         1135.86
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-10-21
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2020-10-21 deposited with the CCDC.	2020-11-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 117.460(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.669(2)
_cell_length_b                   17.8450(18)
_cell_length_c                   17.410(2)
_cell_measurement_reflns_used    1204
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      19.06
_cell_measurement_theta_min      2.58
_cell_volume                     4595.3(9)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150.15
_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  0.1126
_diffrn_reflns_av_unetI/netI     0.0943
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            62751
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.806
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.320
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6847
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1055 before and 0.0574 after correction.
The Ratio of minimum to maximum transmission is 0.9184.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.642
_exptl_crystal_description       needle
_exptl_crystal_F_000             2268
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.740
_refine_diff_density_min         -0.632
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     723
_refine_ls_number_reflns         8079
_refine_ls_number_restraints     181
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.1557
_refine_ls_R_factor_gt           0.0621
_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^)+(0.0591P)^2^+8.1102P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1278
_refine_ls_wR_factor_ref         0.1732
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4103
_reflns_number_total             8079
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03665j2.cif
_cod_data_source_block           mono_a
_cod_depositor_comments
'Adding full bibliography for 7705788--7705792.cif.'
_cod_original_cell_volume        4595.3(10)
_cod_database_code               7705789
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.997
_shelx_estimated_absorpt_t_min   0.930
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Cl0B-C91B \\sim Cl0B-C95B
 with sigma of 0.005
 Cl5B-C94B \\sim Cl5B-C90B
 with sigma of 0.005
 Cl0A-C91A \\sim Cl0A-C95A
 with sigma of 0.005
 Cl5A-C94A \\sim Cl5A-C90A
 with sigma of 0.005
3. Restrained planarity
 Cl0B, Cl5B, C90B, C91B, C92B, C93B, C94B, C95B
 with sigma of 0.1
 Cl0A, Cl5A, C90A, C91A, C92A, C93A, C94A, C95A
 with sigma of 0.1
 Cl8, Cl13, C8, C9, C10, C11, C12, C13
 with sigma of 0.1
4. Rigid bond restraints
 Cl0A, Cl5A, C90A, C91A, C92A, C93A, C94A, C95A
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
5. Uiso/Uaniso restraints and constraints
C90B \\sim C91B \\sim C92B \\sim C93B \\sim C94B \\sim C95B: within 2A with
sigma of 0.005 and sigma for terminal atoms of 0.01 within 2A
Cl0A \\sim Cl5A \\sim C90A \\sim C91A \\sim C92A \\sim C93A \\sim C94A \\sim
C95A: within 2A with sigma of 0.005 and sigma for terminal atoms of 0.01 within
2A
Cl8 \\sim Cl13 \\sim C8 \\sim C9 \\sim C10 \\sim C11 \\sim C12 \\sim C13:
within 2A with sigma of 0.005 and sigma for terminal atoms of 0.01 within 2A
Uanis(Cl0B) \\sim Ueq, Uanis(Cl5B) \\sim Ueq: with sigma of 0.003 and sigma for
terminal atoms of 0.006
Uanis(C90A) = Uanis(C90B)
Uanis(C91A) = Uanis(C91B)
Uanis(C92A) = Uanis(C92A)
Uanis(C93A) = Uanis(C93B)
Uanis(C94A) = Uanis(C94B)
Uanis(C95A) = Uanis(C94B)
6. Others
 Sof(Cl0B)=Sof(Cl5B)=Sof(C90B)=Sof(C91B)=Sof(H91B)=Sof(C92B)=Sof(H92B)=
 Sof(C93B)=Sof(H93B)=Sof(C94B)=Sof(H94B)=Sof(C95B)=1-FVAR(1)
 Sof(Cl0A)=Sof(Cl5A)=Sof(C90A)=Sof(C91A)=Sof(H91A)=Sof(C92A)=Sof(H92A)=
 Sof(C93A)=Sof(H93A)=Sof(C94A)=Sof(H94A)=Sof(C95A)=FVAR(1)
 Fixed Sof: Cl8(0.5) Cl13(0.5) C8(0.5) C9(0.5) H9(0.5) C10(0.5) H10(0.5)
 C11(0.5) H11(0.5) C12(0.5) H12(0.5) C13(0.5)
7.a Aromatic/amide H refined with riding coordinates:
 C102(H102), C104(H104), C201(H201), C202(H202), C204(H204), C205(H205),
 C9(H9), C10(H10), C11(H11), C12(H12), C91A(H91A), C92A(H92A), C93A(H93A),
 C94A(H94A), C91B(H91B), C92B(H92B), C93B(H93B), C94B(H94B)
7.b Fitted hexagon refined as free rotating group:
 C8(C9,C10,C11,C12,C13), C90A(C91A,C92A,C93A,C94A,C95A), C90B(C91B,C92B,C93B,
 C94B,C95B)
7.c Idealised Me refined as rotating group:
 C01(H01A,H01B,H01C), C02(H02A,H02B,H02C), C03(H03A,H03B,H03C), C04(H04A,H04B,
 H04C)
;
_shelx_res_checksum              61187
_olex2_submission_special_instructions 'No special instructions were received'