Icosahedral carboranes as scaffolds for congested regioselective polyaryl compounds. The distinct distance tuning of C-C and its antipodal B-B.
Vinas, Clara; Kelemen, Zsolt; Pepiol, Ariadna; Lupu, Marius; Sillanpää, Reijo; Hänninen, Mikko; Teixidor, Francesc; Chemical Communications  (2019) –; doi:10.1039/C9CC04526K

data_7123721
_publ_section_title
;
 Icosahedral carboranes as scaffolds for congested regioselective polyaryl
 compounds. The distinct distance tuning of C-C and its antipodal B-B.
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC04526K
_journal_year                    2019
_chemical_formula_moiety         'C26 H28 B10'
_chemical_formula_sum            'C26 H28 B10'
_chemical_formula_weight         448.58
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-03-08
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_audit_update_record
;
2018-10-08 deposited with the CCDC.    2019-06-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.834(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.0809(3)
_cell_length_b                   9.02379(19)
_cell_length_c                   13.9208(3)
_cell_measurement_reflns_used    2477
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      75.7180
_cell_measurement_theta_min      4.4420
_cell_volume                     1243.77(5)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3953
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -64.00  11.00   1.00   15.00    --  -41.90  57.00-150.00   75
  2  \w   -113.00 -19.00   1.00   15.00    --  -41.90 -37.00  30.00   94
  3  \w   -100.00 -74.00   1.00   15.00    --  -41.90-136.00 144.00   26
  4  \w     45.00 138.00   1.00   50.00    --  112.00 -61.00   0.00   93
  5  \w     96.00 175.00   1.00   50.00    --  112.00  45.00  90.00   79
  6  \w    111.00 165.00   1.00   50.00    --  112.00 111.00  30.00   54
  7  \w    102.00 174.00   1.00   50.00    --  112.00 111.00  90.00   72
  8  \w     85.00 173.00   1.00   50.00    --  112.00  61.00 150.00   88
  9  \w     29.00  83.00   1.00   50.00    --  112.00 -94.00   0.00   54
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0236042000
_diffrn_orient_matrix_UB_12      0.0066893000
_diffrn_orient_matrix_UB_13      0.1124794000
_diffrn_orient_matrix_UB_21      -0.0860869000
_diffrn_orient_matrix_UB_22      0.1419589000
_diffrn_orient_matrix_UB_23      -0.0060479000
_diffrn_orient_matrix_UB_31      -0.1274548000
_diffrn_orient_matrix_UB_32      -0.0946975000
_diffrn_orient_matrix_UB_33      -0.0010352000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0260
_diffrn_reflns_av_unetI/netI     0.0383
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            4729
_diffrn_reflns_point_group_measured_fraction_full 0.685
_diffrn_reflns_point_group_measured_fraction_max 0.685
_diffrn_reflns_theta_full        70.952
_diffrn_reflns_theta_max         70.952
_diffrn_reflns_theta_min         4.466
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.446
_exptl_absorpt_correction_T_max  0.77387
_exptl_absorpt_correction_T_min  0.76211
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Spherical absorption correction
 using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.198
_exptl_crystal_description       plate
_exptl_crystal_F_000             468
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.326
_refine_diff_density_min         -0.208
_refine_diff_density_rms         0.037
_refine_ls_abs_structure_details
;
 Flack x determined using 655 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.5(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         3289
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0417
_refine_ls_R_factor_gt           0.0385
_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^)+(0.0524P)^2^+0.1795P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0959
_refine_ls_wR_factor_ref         0.0989
_reflns_Friedel_coverage         0.289
_reflns_Friedel_fraction_full    0.330
_reflns_Friedel_fraction_max     0.330
_reflns_number_gt                3104
_reflns_number_total             3289
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc04526k2.cif
_cod_data_source_block           zk-2
_cod_database_code               7123721
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C26 H28 B10'
_reflns_odcompleteness_completeness 98.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C14(H14), C33(H33), C30(H30), C18(H18), C36(H36), C16(H16), C28(H28),
 C32(H32), C34(H34), C24(H24), C20(H20), C23(H23), C17(H17), C27(H27), C22(H22),
  C29(H29), C21(H21), C26(H26), C15(H15), C35(H35)
2.b Boron cage BH refined with riding coordinates:
 B5(H5), C2(H2), C1(H1), B3(H3), B4(H4), B6(H6), B7(H7), B11(H11)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.076
_oxdiff_exptl_absorpt_empirical_full_min 0.926