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_1572802
_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         'C26 H46 B31 O P'
_chemical_formula_sum            'C26 H46 B31 O P'
_chemical_formula_weight         740.71
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2024-02-20
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-05-15 deposited with the CCDC.	2024-10-03 downloaded from the CCDC.
;
_cell_angle_alpha                91.154(8)
_cell_angle_beta                 106.328(9)
_cell_angle_gamma                117.784(7)
_cell_formula_units_Z            2
_cell_length_a                   12.196(3)
_cell_length_b                   12.565(3)
_cell_length_c                   15.872(4)
_cell_measurement_reflns_used    9324
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.46
_cell_measurement_theta_min      2.49
_cell_volume                     2032.1(9)
_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 0.999
_diffrn_measured_fraction_theta_max 1.000
_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      0,0183336
_diffrn_orient_matrix_UB_12      0,0768884
_diffrn_orient_matrix_UB_13      -0,0246888
_diffrn_orient_matrix_UB_21      -0,0587488
_diffrn_orient_matrix_UB_22      0,0114845
_diffrn_orient_matrix_UB_23      0,0277748
_diffrn_orient_matrix_UB_31      0,0764193
_diffrn_orient_matrix_UB_32      0,0481028
_diffrn_orient_matrix_UB_33      0,0554132
_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  0.0623
_diffrn_reflns_av_unetI/netI     0.0340
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            68538
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.731
_diffrn_reflns_theta_min         1.862
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Incoatec ImS 2.0'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.096
_exptl_absorpt_correction_T_max  0.7412
_exptl_absorpt_correction_T_min  0.7112
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2016/2 (Bruker AXS)'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.211
_exptl_crystal_description       block
_exptl_crystal_F_000             760
_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          0.34
_exptl_crystal_size_mid          0.236
_exptl_crystal_size_min          0.116
_refine_diff_density_max         0.816
_refine_diff_density_min         -0.257
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     535
_refine_ls_number_reflns         8626
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0562
_refine_ls_R_factor_gt           0.0498
_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^)+(0.0592P)^2^+1.3660P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1258
_refine_ls_wR_factor_ref         0.1300
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7654
_reflns_number_total             8626
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc06144f3.cif
_cod_data_source_block           3a
_cod_depositor_comments
'Adding full bibliography for 1572799--1572802.cif.'
_cod_database_code               1572802
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.989
_shelx_estimated_absorpt_t_min   0.968
_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.a Aromatic/amide H refined with riding coordinates:
 C00B(H00B), C00D(H00D), C00E(H00E), C00F(H00F), C00G(H00G), C00H(H00H),
 C00I(H00I), C00J(H00J), C00K(H00K), C00L(H00L), C00M(H00M), C00N(H00N),
 C00P(H00P), C00Q(H00Q), C00R(H00R)
1.b Boron cage BH refined with riding coordinates:
 B00U(H00U), B00V(H00V), B00W(H00W), B00X(H00X), B00Y(H00Y), B00Z(H00Z),
 B010(H010), B011(H011), B012(H012), B013(H013), B014(H014), B015(H015),
 B016(H016), B017(H017), B018(H018), B019(H019), B01A(H01A), B01B(H01B),
 B01C(H01C), B01D(H01D), B01E(H01E), B01F(H01F), B01G(H01G), B01H(H01H),
 B01I(H01I), B01J(H01J), B01K(H01K), B01L(H01L), B01M(H01M), B01N(H01N)
;
_shelx_res_checksum              96941
_shelx_hkl_checksum              40260
_olex2_submission_special_instructions 'No special instructions were received'