Substitution at sp3 boron of a six-membered NHC·BH3: convenient access to a dihydroxyborenium cation
Kundu, Gargi; Ajithkumar, V. S.; Raj, K. Vipin; Vanka, Kumar; Tothadi, Srinu; Sen, Sakya S.; Chemical Communications  (2022) –; doi:10.1039/D1CC06816D

data_7129767
_publ_section_title
;
 Substitution at sp3 boron of a six-membered NHC&#x00B7;BH3: convenient
 access to a dihydroxyborenium cation
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D1CC06816D
_journal_year                    2022
_chemical_formula_moiety         'C28 H42 B I N2, 2(C3.5 H3.5)'
_chemical_formula_sum            'C35 H49 B I N2'
_chemical_formula_weight         635.47
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-12-02
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-12-02 deposited with the CCDC.	2022-02-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 118.551(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   30.7004(15)
_cell_length_b                   13.6937(5)
_cell_length_c                   18.6768(8)
_cell_measurement_reflns_used    9187
_cell_measurement_temperature    100
_cell_measurement_theta_max      33.32
_cell_measurement_theta_min      2.43
_cell_volume                     6896.9(6)
_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      100.0
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.997
_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  0.0516
_diffrn_reflns_av_unetI/netI     0.0170
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       51
_diffrn_reflns_limit_h_min       -51
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            325196
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         36.365
_diffrn_reflns_theta_min         1.851
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.952
_exptl_absorpt_correction_T_max  0.7471
_exptl_absorpt_correction_T_min  0.6797
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0960 before and 0.0604 after correction. The Ratio of minimum to maximum transmission is 0.9098. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.224
_exptl_crystal_description       block
_exptl_crystal_F_000             2648
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         3.047
_refine_diff_density_min         -2.301
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         16717
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.0409
_refine_ls_R_factor_gt           0.0345
_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^)+(0.0432P)^2^+10.6544P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0929
_refine_ls_wR_factor_ref         0.1005
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14908
_reflns_number_total             16717
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc06816d2.cif
_cod_data_source_block           mo_gar_110_0ma_b
_cod_original_cell_volume        6896.9(5)
_cod_database_code               7129767
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.894
_shelx_estimated_absorpt_t_min   0.797
_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. Others
 Fixed Sof: C28(0.5) H28A(0.5) H28B(0.5) H28C(0.5) C35(0.5) H35A(0.5)
 H35B(0.5) H35C(0.5)
3.a Ternary CH refined with riding coordinates:
 C22(H22), C13(H13), C7(H7), C10(H10)
3.b Secondary CH2 refined with riding coordinates:
 C33(H33A,H33B), C32(H32A,H32B), C34(H34A,H34B)
3.c Aromatic/amide H refined with riding coordinates:
 C17(H17), C19(H19), C4(H4), C18(H18), C3(H3), C5(H5), C31(H31), C29(H29),
 C27(H27), C26(H26)
3.d Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C8(H8A,H8B,H8C), C24(H24A,H24B,H24C), C14(H14A,H14B,H14C),
 C15(H15A,H15B,H15C), C23(H23A,H23B,H23C), C11(H11A,H11B,H11C), C12(H12A,H12B,
 H12C), C28(H28A,H28B,H28C), C35(H35A,H35B,H35C)
;
_shelx_res_checksum              39484
_shelx_hkl_checksum              9001
_olex2_submission_special_instructions 'No special instructions were received'