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_1572800
_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      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
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2024-08-26
_audit_creation_method           'CIF-fill 1.5e (K.Radacki, 2005-23)'
_audit_update_record
;
2024-09-10 deposited with the CCDC.	2024-10-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.8020(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.9904(2)
_cell_length_b                   17.1121(2)
_cell_length_c                   19.3321(2)
_cell_measurement_reflns_used    30429
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      72.8000
_cell_measurement_theta_min      3.4130
_cell_volume                     4354.53(10)
_computing_cell_refinement       'CrysAlisPro 1.171.43.89a (Rigaku OD, 2023)'
_computing_data_collection
;
 CrysAlisPro system (CCD 43.128a 64-bit (release 20-06-2024))
;
_computing_data_reduction        'CrysAlisPro 1.171.43.89a (Rigaku OD, 2023)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_computing_publication_material  'SHELXL-2019/1 (Sheldrick, 2019)'
_computing_structure_refinement  'SHELXL-2019/1 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 HPA
_diffrn_detector_area_resol_mean 10.0
_diffrn_detector_type            'HyPix Arc150'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_details
;
 List of Runs (angles in degrees, time in seconds):
 --------------------------------------------------------------------------
  1  \w   -104.00 -79.00   0.50    0.05    --  -58.00 -49.00 133.01   50
  2  \w   -121.00 -94.00   0.50    0.05    --  -78.50 -59.00  67.98   54
  3  \w   -117.00 -91.00   0.50    0.05    --  -74.00 -54.00   6.91   52
  4  \w   -124.00 -98.00   0.50    0.05    --  -78.50 -48.00  28.92   52
  5  \w   -122.00 -97.00   0.50    0.05    --  -78.50 -57.00 -12.85   50
  6  \w    -99.00 -71.00   0.50    0.05    --  -54.00 -50.00-116.94   56
  7  \w   -116.00 -88.00   0.50    0.05    --  -70.00 -44.00-149.68   56
  8  \w   -121.00 -92.00   0.50    0.05    --  -74.00 -42.00-131.45   58
  9  \w   -124.00 -98.00   0.50    0.05    --  -78.50 -48.00-166.52   52
 10  \w   -124.00 -97.00   0.50    0.05    --  -78.50 -49.00-102.88   54
 11  \w   -121.00 -96.00   0.50    0.05    --  -74.00 -42.00 -64.15   50
 12  \w   -120.00 -93.00   0.50    0.05    --  -74.00 -35.00 -40.75   54
 13  \w   -126.00-101.00   0.50    0.05    --  -78.50 -40.00 -41.14   50
 14  \w   -125.00 -97.00   0.50    0.05    --  -78.50 -41.00 161.66   56
 15  \w   -108.00 -83.00   0.50    0.05    --  -62.00 -47.00 113.54   50
 16  \w     -6.00  20.00   0.50    0.05    --  -14.00  78.00  88.12   52
 17  \w    -90.00 -26.00   0.50    0.05    --  -69.75 120.00 125.00  128
 18  \w    -80.00 -17.00   0.50    0.05    --  -60.27 120.00 125.00  126
 19  \w    -95.00 -32.00   0.50    0.05    --  -75.18 120.00 125.00  126
 20  \w    -86.00 -60.00   0.50    0.05    --  -78.50 114.00 110.96   52
 21  \w    -78.00 -52.00   0.50    0.05    --  -78.50 110.00  66.26   52
 22  \w    -61.00 -35.00   0.50    0.05    --  -78.50 121.00  60.43   52
 23  \w    -99.00 -70.00   0.50    0.05    --  -78.50 121.00  60.43   58
 24  \w    -72.00 -35.00   0.50    0.05    --  -78.50 128.00 -99.57   74
 25  \w    -83.00 -32.00   0.50    0.05    --  -74.00 109.00 -98.44  102
 26  \w     55.00  83.00   0.50    0.05    --   38.00  51.00 -61.53   56
 27  \w     45.00  98.00   0.50    0.05    --   80.80-119.00  58.09  106
 28  \w     28.00  91.00   0.50    0.05    --   71.40-120.00  41.00  126
 29  \w     34.00  97.00   0.50    0.05    --   76.88-120.00  41.00  126
 30  \w     65.00  98.00   0.50    0.05    --   80.80-115.00  92.32   66
 31  \w     16.00  79.00   0.50    0.05    --   58.63-120.00  41.00  126
 32  \w     41.00  98.00   0.50    0.05    --   80.80-118.00-169.50  114
 33  \w     40.00  79.00   0.50    0.05    --   80.80-105.00-129.89   78
 34  \w     20.00  46.00   0.50    0.05    --    6.00  63.00-138.32   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku XtaLAB Synergy-R'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
;
 CrysAlisPro convention (1999,Acta A55,543-557)
;
_diffrn_orient_matrix_UB_11      -0.0966419000
_diffrn_orient_matrix_UB_12      0.0102187000
_diffrn_orient_matrix_UB_13      0.0202112000
_diffrn_orient_matrix_UB_21      0.0029499000
_diffrn_orient_matrix_UB_22      0.0887540000
_diffrn_orient_matrix_UB_23      -0.0126833000
_diffrn_orient_matrix_UB_31      -0.0659843000
_diffrn_orient_matrix_UB_32      -0.0111736000
_diffrn_orient_matrix_UB_33      -0.0812817000
_diffrn_radiation_monochromator  'multi-layer mirror'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_xray_symbol    K-L~2,3~
_diffrn_reflns_av_R_equivalents  0.0204
_diffrn_reflns_av_unetI/netI     0.0168
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            42906
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.103
_diffrn_reflns_theta_min         3.413
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet-R X-ray Source'
_exptl_absorpt_coefficient_mu    0.720
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.498
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
 CrysAlisPro 1.171.43.89a (Rigaku Oxford Diffraction, 2023) Numerical 
 absorption correction based on gaussian integration over a multifaceted 
 crystal model Empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    1.130
_exptl_crystal_description       block
_exptl_crystal_F_000             1520
_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          0.300
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.342
_refine_diff_density_min         -0.289
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     532
_refine_ls_number_reflns         8374
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0401
_refine_ls_R_factor_gt           0.0381
_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^)+(0.0550P)^2^+2.0385P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1018
_refine_ls_wR_factor_ref         0.1032
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7819
_reflns_number_total             8374
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc06144f3.cif
_cod_data_source_block           4a
_cod_depositor_comments
'Adding full bibliography for 1572799--1572802.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1572800
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_min   0.813
_shelx_estimated_absorpt_t_max   0.919
_shelx_res_checksum              67989
_shelx_hkl_checksum              26015
_shelx_fab_checksum              3164