Structure-constraint induced increase in Lewis acidity of tris(<i>ortho</i>-carboranyl)borane and selective complexation with Bestmann ylides.
Xiang, Libo; Wang, Junyi; Matler, Alexander; Ye, Qing; Chemical science 15 (2024) 17944–17949; doi:10.1039/d4sc06144f

data_1572799
_publ_section_title
;
 Structure-constraint induced increase in Lewis acidity of
 tris(<i>ortho</i>-carboranyl)borane and selective complexation with
 Bestmann ylides.
;
_journal_issue                   43
_journal_name_full               'Chemical science'
_journal_page_first              17944
_journal_page_last               17949
_journal_paper_doi               10.1039/d4sc06144f
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C6.04 H31 B30.96'
_chemical_formula_sum            'C6.04 H31 B30.96'
_chemical_formula_weight         438.46
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
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;
Olex2 1.5
(compiled 2024.01.12 svn.r2f8d729c for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-05-15 deposited with the CCDC.	2024-10-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.640(4)
_cell_length_b                   16.954(3)
_cell_length_c                   6.7999(12)
_cell_measurement_reflns_used    9876
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.58
_cell_measurement_theta_min      2.23
_cell_volume                     2494.8(8)
_computing_cell_refinement       'Saint+ ver. 8.40B (Bruker AXS)'
_computing_data_collection       'BIS 6.2.14 / APEX4 ver. 2021.10 (Bruker AXS)'
_computing_data_reduction        'Saint+ ver. 8.40B (Bruker AXS)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2019/1 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)''
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 CPA
_diffrn_detector_area_resol_mean 7.5
_diffrn_detector_type            'Photon II'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8-Quest'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_orient_matrix_type
;
 Sparks R.A., Computational Crystallography p1-18 (Clarendon Press, 1982)
;
_diffrn_orient_matrix_UB_11      0.0159889
_diffrn_orient_matrix_UB_12      -0.0026215
_diffrn_orient_matrix_UB_13      -0.0458919
_diffrn_orient_matrix_UB_21      -0.1313381
_diffrn_orient_matrix_UB_22      -0.0261338
_diffrn_orient_matrix_UB_23      -0.0036021
_diffrn_orient_matrix_UB_31      -0.0641972
_diffrn_orient_matrix_UB_32      0.0528131
_diffrn_orient_matrix_UB_33      -0.0040604
_diffrn_radiation_monochromator  'multi-layer mirror'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~2,3~
_diffrn_reflns_av_R_equivalents  0.0596
_diffrn_reflns_av_unetI/netI     0.0306
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            29339
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.646
_diffrn_reflns_theta_min         1.882
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Incoatec ImS 2.0'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.047
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6468
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2016/2 (Bruker AXS)'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.167
_exptl_crystal_description       block
_exptl_crystal_F_000             888
_exptl_crystal_preparation
;
 For data collection the crystal was immersed in a film of perfluoropolyether 
 oil, mounted on a polyimide loop and transferred to stream of cold nitrogen 
 (Oxford Cryostream 800).
;
_exptl_crystal_size_max          0.444
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.251
_refine_diff_density_max         0.368
_refine_diff_density_min         -0.234
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     189
_refine_ls_number_reflns         2984
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0601
_refine_ls_R_factor_gt           0.0504
_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^)+(0.0772P)^2^+1.0046P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1400
_refine_ls_wR_factor_ref         0.1494
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2537
_reflns_number_total             2984
_reflns_threshold_expression     'I > 2\s(I)'
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_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 1572799--1572802.cif.'
_cod_original_cell_volume        2494.7(8)
_cod_database_code               1572799
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.988
_shelx_estimated_absorpt_t_min   0.979
_exptl_absorpt_special_details
;
 Incident beam scaling, empirical absorption correction using spherical 
 harmonics, and outlier rejection was employed as implemented in SADABS. 
 Additional spherical absorption correction with mu*r value set to 0.2 was 
 applied.
;
_olex2_refinement_description
;
1. Others
 Sof(B4)=Sof(H4A)=1-FVAR(1)
 Sof(C4)=Sof(H4)=FVAR(1)
2.a Boron cage BH refined with riding coordinates:
 B1(H1), B2(H2), B3(H3), C4(H4), B4(H4A), B5(H5), B6(H6), B7(H7), B8(H8),
 B9(H9), B10(H10), B11(H11), B13(H13), B14(H14), B15(H15), B16(H16), B17(H17),
 B18(H18)
;
_shelx_res_checksum              49487
_shelx_hkl_checksum              32781
_olex2_submission_special_instructions 'No special instructions were received'