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_7129763
_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 H43 B N2'
_chemical_formula_sum            'C28 H43 B N2'
_chemical_formula_weight         418.45
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2021-04-15
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-08-08 deposited with the CCDC.	2022-02-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   19.167(2)
_cell_length_b                   14.1542(17)
_cell_length_c                   39.176(5)
_cell_measurement_reflns_used    9061
_cell_measurement_temperature    100
_cell_measurement_theta_max      24.11
_cell_measurement_theta_min      2.34
_cell_volume                     10628(2)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 VENTURE Kappa Duo PHOTON II CPAD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1436
_diffrn_reflns_av_unetI/netI     0.0351
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            465420
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.419
_diffrn_reflns_theta_min         2.069
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.059
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6275
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1366 before and 0.0879 after correction. The Ratio of minimum to maximum transmission is 0.8418. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.046
_exptl_crystal_description       block
_exptl_crystal_F_000             3680
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.295
_refine_diff_density_min         -0.483
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.145
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     599
_refine_ls_number_reflns         10905
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.145
_refine_ls_R_factor_all          0.0902
_refine_ls_R_factor_gt           0.0644
_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^)+(0.0596P)^2^+7.8981P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1465
_refine_ls_wR_factor_ref         0.1612
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8657
_reflns_number_total             10905
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc06816d2.cif
_cod_data_source_block           mo_aj6siprbh3_0ma_a
_cod_database_code               7129763
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.996
_shelx_estimated_absorpt_t_min   0.993
_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:
 C7(H7), C34(H34), C10(H10), C50(H50), C53(H53), C25(H25), C37(H37), C22(H22)
2.b Secondary CH2 refined with riding coordinates:
 C40(H40A,H40B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C41(H41A,
 H41B), C42(H42A,H42B)
2.c Aromatic/amide H refined with riding coordinates:
 C18(H18), C3(H3), C5(H5), C20(H20), C48(H48), C4(H4), C32(H32), C19(H19),
 C47(H47), C46(H46), C31(H31), C30(H30)
2.d Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C8(H8A,H8B,H8C), C12(H12A,H12B,H12C), C11(H11A,H11B,H11C),
 C39(H39A,H39B,H39C), C36(H36A,H36B,H36C), C55(H55A,H55B,H55C), C35(H35A,H35B,
 H35C), C52(H52A,H52B,H52C), C38(H38A,H38B,H38C), C26(H26A,H26B,H26C), C51(H51A,
 H51B,H51C), C54(H54A,H54B,H54C), C27(H27A,H27B,H27C), C24(H24A,H24B,H24C),
 C23(H23A,H23B,H23C)
;
_shelx_res_checksum              5197
_shelx_hkl_checksum              38067
_olex2_submission_special_instructions 'No special instructions were received'