Boronate Ester Bullvalenes.
Patel, Harshal D.; Tran, Thanh-Huyen; Sumby, Christopher J.; Pašteka, Lukáš F; Fallon, Thomas; Journal of the American Chemical Society 142 (2020) 3680–3685; doi:10.1021/jacs.9b12930

data_4134176
_publ_section_title
;
 Boronate Ester Bullvalenes.
;
_journal_issue                   8
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3680
_journal_page_last               3685
_journal_paper_doi               10.1021/jacs.9b12930
_journal_volume                  142
_journal_year                    2020
_chemical_formula_moiety         'C18 H14 N4'
_chemical_formula_sum            'C18 H14 N4'
_chemical_formula_weight         286.33
_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   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2019-10-09
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                109.120(5)
_cell_angle_beta                 92.769(4)
_cell_angle_gamma                96.001(4)
_cell_formula_units_Z            2
_cell_length_a                   5.9688(3)
_cell_length_b                   9.4191(5)
_cell_length_c                   12.8890(6)
_cell_measurement_reflns_used    3134
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.8420
_cell_measurement_theta_min      3.9420
_cell_volume                     678.27(6)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (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)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1695
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.896
_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    -88.00   2.00   1.00   30.00    --  -19.50 -57.00 -90.00   90
  2  \w    -95.00 -35.00   1.00   30.00    --  -19.50-178.00  30.00   60
  3  \w    -88.00   2.00   1.00   30.00    --  -19.50 -57.00-180.00   90
  4  \w    -50.00  51.00   1.00   30.00    --  -19.50  77.00 150.00  101
  5  \w    -25.00  22.00   1.00   30.00    --  -19.50 -99.00  30.00   47
  6  \w    -50.00  51.00   1.00   30.00    --  -19.50  77.00  30.00  101
  7  \w    -54.00  45.00   1.00   30.00    --   18.95 -37.00-120.00   99
  8  \w     -7.00  91.00   1.00   30.00    --   18.95  37.00-180.00   98
  9  \w    -25.00  22.00   1.00   30.00    --  -19.50 -99.00  90.00   47
 10  \w    -67.00  16.00   1.00   30.00    --  -19.50 109.00-121.00   83
 11  \w    -88.00   2.00   1.00   30.00    --  -19.50 -57.00   0.00   90
 12  \w    -16.00  58.00   1.00   30.00    --   18.95-109.00 143.00   74
 13  \w    -25.00  22.00   1.00   30.00    --  -19.50 -99.00-180.00   47
 14  \w    -95.00 -35.00   1.00   30.00    --  -19.50-178.00-120.00   60
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0359058000
_diffrn_orient_matrix_UB_12      0.0412432000
_diffrn_orient_matrix_UB_13      0.0560879000
_diffrn_orient_matrix_UB_21      -0.1137151000
_diffrn_orient_matrix_UB_22      0.0099978000
_diffrn_orient_matrix_UB_23      0.0108726000
_diffrn_orient_matrix_UB_31      -0.0129744000
_diffrn_orient_matrix_UB_32      -0.0682373000
_diffrn_orient_matrix_UB_33      0.0124391000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0446
_diffrn_reflns_av_unetI/netI     0.0440
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.896
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            15131
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.896
_diffrn_reflns_theta_full        27.000
_diffrn_reflns_theta_max         29.410
_diffrn_reflns_theta_min         3.359
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.087
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97366
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
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    1.402
_exptl_crystal_description       rod
_exptl_crystal_F_000             300
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.298
_refine_diff_density_min         -0.211
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         3346
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0741
_refine_ls_R_factor_gt           0.0473
_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^)+(0.0321P)^2^+0.2880P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0912
_refine_ls_wR_factor_ref         0.1007
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2495
_reflns_number_total             3346
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b12930_si_002.cif
_cod_data_source_block           HPbpyrimB
_cod_depositor_comments
'Adding full bibliography for 4134168--4134181.cif.'
_cod_database_code               4134176
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         C18H14N4
_chemical_oxdiff_usercomment     'colourless rod, 0.50 x 0.18 x 0.07'
_shelx_estimated_absorpt_t_max   0.994
_shelx_estimated_absorpt_t_min   0.958
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Ternary CH refined with riding coordinates:
 C1(H1), C4(H4), C5(H5), C10(H10)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C8(H8), C9(H9), C12(H12), C14(H14), C16(H16), C22(H22),
 C24(H24), C26(H26)
;
_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 1.068
_oxdiff_exptl_absorpt_empirical_full_min 0.952