Kinetic stabilization allows structural analysis of a benzoborirene
Sindlinger, Marvin; Ströbele, Markus; Maichle-Mössmer, Cäcilia; Bettinger, Holger F.; Chemical Communications  (2022) –; doi:10.1039/D1CC06588B

data_7129596
_publ_section_title
;
 Kinetic stabilization allows structural analysis of a benzoborirene
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D1CC06588B
_journal_year                    2022
_chemical_formula_moiety         'C42 H53 B'
_chemical_formula_sum            'C42 H53 B'
_chemical_formula_weight         568.65
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-05-02
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2020.11.27 svn.r5f609507 for Rigaku Oxford Diffraction, GUI svn.r6214)
;
_audit_update_record
;
2021-05-02 deposited with the CCDC.	2022-01-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.61817(14)
_cell_length_b                   25.11861(17)
_cell_length_c                   8.47933(6)
_cell_measurement_reflns_used    34701
_cell_measurement_temperature    99.99(11)
_cell_measurement_theta_max      79.4110
_cell_measurement_theta_min      3.4780
_cell_volume                     3539.49(5)
_computing_cell_refinement       'CrysAlisPro 1.171.41.108a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.108a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.108a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.99(11)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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     42.00 123.00   0.50    7.50    --   49.83  26.00  86.00  162
  2  \w    -80.00 -18.00   0.50   20.00    --  -90.00  99.00 -99.00  124
  3  \w    104.00 178.00   0.50   20.00    --  111.50  26.00  86.00  148
  4  \w     41.00 109.00   0.50   20.00    --  111.50-119.00  72.00  136
  5  \w    -26.00  24.00   0.50    7.50    --  -49.83  19.00-180.00  100
  6  \w   -122.00 -73.00   0.50    7.50    --  -49.83-125.00  30.00   98
  7  \w    -22.00  26.00   0.50    7.50    --   49.83 -19.00-180.00   96
  8  \w    -22.00  26.00   0.50    7.50    --   49.83 -19.00 150.00   96
  9  \w     41.00  71.00   0.50   20.00    --  111.50 -61.00 -60.00   60
 10  \w     41.00  71.00   0.50   20.00    --  111.50 -61.00  60.00   60
 11  \w     41.00  71.00   0.50   20.00    --  111.50 -61.00-180.00   60
 12  \w    102.00 178.00   0.50   20.00    --  111.50  45.00-180.00  152
 13  \w     41.00 106.00   0.50   20.00    --  111.50 -99.00 153.00  130
 14  \w     41.00  71.00   0.50   20.00    --  111.50 -61.00  30.00   60
 15  \w     41.00  71.00   0.50   20.00    --  111.50 -61.00 -90.00   60
 16  \w     41.00 106.00   0.50   20.00    --  111.50 -77.00 150.00  130
 17  \w     41.00 111.00   0.50   20.00    --  111.50-125.00 -30.00  140
 18  \w     41.00 105.00   0.50   20.00    --  111.50 -94.00 120.00  128
 19  \w     41.00  71.00   0.50   20.00    --  111.50 -61.00-150.00   60
 20  \w   -122.00 -29.00   0.50    7.50    --  -49.83 -77.00  30.00  186
 21  \w   -122.00 -29.00   0.50    7.50    --  -49.83 -77.00-150.00  186
 22  \w   -122.00 -29.00   0.50    7.50    --  -49.83 -77.00 -60.00  186
 23  \w     42.00 122.00   0.50    7.50    --   49.83  37.00 150.00  160
 24  \w   -161.00 -69.00   0.50   20.00    --  -90.00 -77.00 150.00  184
 25  \w   -161.00 -69.00   0.50   20.00    --  -90.00 -77.00  90.00  184
 26  \w   -161.00 -69.00   0.50   20.00    --  -90.00 -77.00  30.00  184
 27  \w   -161.00 -69.00   0.50   20.00    --  -90.00 -77.00-120.00  184
 28  \w   -161.00 -69.00   0.50   20.00    --  -90.00 -77.00 -90.00  184
 29  \w   -161.00 -69.00   0.50   20.00    --  -90.00 -77.00 -30.00  184
 30  \w   -161.00 -69.00   0.50   20.00    --  -90.00 -77.00-180.00  184
 31  \w    104.00 178.00   0.50   20.00    --  111.50  15.00 150.00  148
 32  \w    104.00 178.00   0.50   20.00    --  111.50  15.00  30.00  148
 33  \w     41.00 160.00   0.50   20.00    --  111.50   0.00   0.00  238
 34  \w     41.00  71.00   0.50   20.00    --  111.50 -61.00 -30.00   60
 35  \w     41.00 105.00   0.50   20.00    --  111.50 -94.00   0.00  128
 36  \w   -122.00 -29.00   0.50    7.50    --  -49.83 -77.00 -30.00  186
 37  \w   -122.00 -29.00   0.50    7.50    --  -49.83 -77.00 150.00  186
 38  \w   -122.00 -29.00   0.50    7.50    --  -49.83 -77.00  90.00  186
 39  \w     34.00  95.00   0.50    7.50    --   49.83-125.00  60.00  122
 40  \w   -161.00 -69.00   0.50   20.00    --  -90.00 -77.00-150.00  184
 41  \w   -161.00 -69.00   0.50   20.00    --  -90.00 -77.00 -60.00  184
 42  \w   -161.00 -69.00   0.50   20.00    --  -90.00 -77.00 120.00  184
 43  \w   -161.00 -69.00   0.50   20.00    --  -90.00 -77.00   0.00  184
 44  \w   -161.00 -69.00   0.50   20.00    --  -90.00 -77.00  60.00  184
 45  \w     41.00 111.00   0.50   20.00    --  111.50-125.00 -60.00  140
 46  \w     91.00 178.00   0.50   20.00    --  111.50  77.00 -90.00  174
 47  \w     41.00  71.00   0.50   20.00    --  111.50 -61.00 150.00   60
 48  \w     41.00 105.00   0.50   20.00    --  111.50 -94.00  60.00  128
 49  \w     97.00 178.00   0.50   20.00    --  111.50  61.00  30.00  162
 50  \w    102.00 178.00   0.50   20.00    --  111.50  45.00-150.00  152
 51  \w     97.00 178.00   0.50   20.00    --  111.50  61.00 150.00  162
 52  \w   -122.00 -29.00   0.50    7.50    --  -49.83 -77.00-120.00  186
 53  \w    -86.00 -13.00   0.50    7.50    --  -49.83 125.00  30.00  146
 54  \w     42.00 122.00   0.50    7.50    --   49.83  37.00 -60.00  160
 55  \w     42.00 122.00   0.50    7.50    --   49.83  37.00-150.00  160
 56  \w     41.00 111.00   0.50   20.00    --  111.50-125.00   0.00  140
 57  \w     97.00 178.00   0.50   20.00    --  111.50  61.00 -30.00  162
 58  \w     41.00 111.00   0.50   20.00    --  111.50-125.00 -90.00  140
 59  \w    102.00 127.00   0.50   20.00    --  111.50  45.00-120.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0311375000
_diffrn_orient_matrix_UB_12      -0.0255115000
_diffrn_orient_matrix_UB_13      0.1535100000
_diffrn_orient_matrix_UB_21      0.0030154000
_diffrn_orient_matrix_UB_22      0.0553020000
_diffrn_orient_matrix_UB_23      0.0783398000
_diffrn_orient_matrix_UB_31      -0.0872847000
_diffrn_orient_matrix_UB_32      -0.0072111000
_diffrn_orient_matrix_UB_33      0.0574249000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0625
_diffrn_reflns_av_unetI/netI     0.0190
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            80754
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        63.683
_diffrn_reflns_theta_max         63.683
_diffrn_reflns_theta_min         3.519
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.435
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.805
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.108a (Rigaku Oxford Diffraction, 2021)
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 orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.067
_exptl_crystal_description       block
_exptl_crystal_F_000             1240
_exptl_crystal_size_max          0.123
_exptl_crystal_size_mid          0.106
_exptl_crystal_size_min          0.065
_refine_diff_density_max         0.477
_refine_diff_density_min         -0.195
_refine_diff_density_rms         0.038
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     285
_refine_ls_number_reflns         2989
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0506
_refine_ls_R_factor_gt           0.0439
_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^)+(0.0566P)^2^+2.0304P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1118
_refine_ls_wR_factor_ref         0.1167
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2615
_reflns_number_total             2989
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc06588b2.cif
_cod_data_source_block           ms051v2
_cod_database_code               7129596
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C168  H212  B4  '
_reflns_odcompleteness_completeness 89.52
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(B1) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.02
3.a Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C)
;
_shelx_res_checksum              3677
_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
- Detector area scaling
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 3.271
_oxdiff_exptl_absorpt_empirical_full_min 0.351