Synthesis of Disubstituted Carboxonium Derivatives of <i>Closo</i>-Decaborate Anion [2,6-B<sub>10</sub>H<sub>8</sub>O<sub>2</sub>CC<sub>6</sub>H<sub>5</sub>]<sup>-</sup>: Theoretical and Experimental Study.
Klyukin, Ilya N.; Kolbunova, Anastasia V.; Novikov, Alexander S.; Nelyubin, Alexey V.; Zhdanov, Andrey P.; Kubasov, Alexey S.; Selivanov, Nikita A.; Bykov, Alexander Yu; Zhizhin, Konstantin Yu; Kuznetsov, Nikolay T.; Molecules (Basel, Switzerland) 28 (2023) 1757–; doi:10.3390/molecules28041757

data_1568609
_publ_section_title
;
 Synthesis of Disubstituted Carboxonium Derivatives of
 <i>Closo</i>-Decaborate Anion
 [2,6-B<sub>10</sub>H<sub>8</sub>O<sub>2</sub>CC<sub>6</sub>H<sub>5</sub>]<sup>-</sup>:
 Theoretical and Experimental Study.
;
_journal_issue                   4
_journal_name_full               'Molecules (Basel, Switzerland)'
_journal_page_first              1757
_journal_paper_doi               10.3390/molecules28041757
_journal_volume                  28
_journal_year                    2023
_chemical_formula_moiety         'C7 H13 B10 O2, C16 H36 N'
_chemical_formula_sum            'C23 H49 B10 N O2'
_chemical_formula_weight         479.73
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-11-10
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_cell_angle_alpha                90
_cell_angle_beta                 90.4380(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.2162(2)
_cell_length_b                   15.0449(3)
_cell_length_c                   19.1173(3)
_cell_measurement_reflns_used    8096
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      66.676
_cell_measurement_theta_min      3.739
_cell_volume                     2938.28(9)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0770
_diffrn_reflns_av_unetI/netI     0.0586
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            26288
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        66.728
_diffrn_reflns_theta_max         66.728
_diffrn_reflns_theta_min         3.739
_diffrn_source_current           1.1
_diffrn_source_power             0.05500000000000001
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.449
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.5156
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1439 before and 0.0842 after correction.
The Ratio of minimum to maximum transmission is 0.6849.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.084
_exptl_crystal_description       block
_exptl_crystal_F_000             1040
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.672
_refine_diff_density_min         -0.308
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     329
_refine_ls_number_reflns         5172
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.1295
_refine_ls_R_factor_gt           0.0966
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0750P)^2^+6.0225P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2187
_refine_ls_wR_factor_ref         0.2385
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3708
_reflns_number_total             5172
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            B10H8O2CPh.cif
_cod_data_source_block           cu_22kub245_0m_a
_cod_database_code               1568609
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.978
_shelx_estimated_absorpt_t_min   0.936
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C12(H12A,H12B), C13(H13A,H13B),
 C14(H14A,H14B), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B), C20(H20A,H20B),
  C21(H21A,H21B), C22(H22A,H22B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C7(H7)
2.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C15(H15A,H15B,H15C), C19(H19A,H19B,H19C), C23(H23A,H23B,
 H23C)
2.d Boron cage BH refined with riding coordinates:
 B1(H1), B3(H3A), B4(H4A), B5(H5A), B7(H7A), B8(H8), B9(H9), B10(H10)
;
_shelx_res_checksum              685
_shelx_hkl_checksum              54592
_olex2_submission_special_instructions 'No special instructions were received'