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_4134171
_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         'C16 H13 N O2'
_chemical_formula_sum            'C16 H13 N O2'
_chemical_formula_weight         251.27
_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             2019-10-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                69.193(3)
_cell_angle_beta                 84.170(3)
_cell_angle_gamma                86.052(3)
_cell_formula_units_Z            6
_cell_length_a                   6.0297(2)
_cell_length_b                   17.3499(5)
_cell_length_c                   18.4258(7)
_cell_measurement_reflns_used    6307
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.8700
_cell_measurement_theta_min      3.8070
_cell_volume                     1791.46(11)
_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 0.996
_diffrn_measured_fraction_theta_max 0.878
_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     35.00  95.00   1.00   28.00    --   18.95 178.00  60.00   60
  2  \w    -50.00  39.00   1.00   28.00    --   18.95 -57.00-120.00   89
  3  \w    -45.00  53.00   1.00   28.00    --  -19.50  37.00-180.00   98
  4  \w    -25.00  22.00   1.00   28.00    --  -19.50 -99.00-180.00   47
  5  \w    -92.00   6.00   1.00   28.00    --  -19.50 -37.00   0.00   98
  6  \w    -25.00  22.00   1.00   28.00    --  -19.50 -99.00   0.00   47
  7  \w    -88.00   2.00   1.00   28.00    --  -19.50 -57.00 120.00   90
  8  \w    -67.00  16.00   1.00   28.00    --  -19.50 110.00  12.00   83
  9  \w    -25.00  22.00   1.00   28.00    --  -19.50 -99.00 -90.00   47
 10  \w    -88.00   0.00   1.00   28.00    --  -19.50 -57.00 -90.00   88
 11  \w    -92.00  25.00   1.00   28.00    --  -19.50 -19.00 150.00  117
;
_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      -0.0618592000
_diffrn_orient_matrix_UB_12      0.0188925000
_diffrn_orient_matrix_UB_13      -0.0329578000
_diffrn_orient_matrix_UB_21      -0.1002182000
_diffrn_orient_matrix_UB_22      -0.0140298000
_diffrn_orient_matrix_UB_23      0.0234032000
_diffrn_orient_matrix_UB_31      -0.0113786000
_diffrn_orient_matrix_UB_32      0.0368958000
_diffrn_orient_matrix_UB_33      0.0085787000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0477
_diffrn_reflns_av_unetI/netI     0.0685
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.878
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            31130
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.878
_diffrn_reflns_theta_full        27.000
_diffrn_reflns_theta_max         29.399
_diffrn_reflns_theta_min         3.334
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.093
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95466
_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            yellow
_exptl_crystal_density_diffrn    1.397
_exptl_crystal_description       block
_exptl_crystal_F_000             792
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.494
_refine_diff_density_min         -0.286
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     514
_refine_ls_number_reflns         8686
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.1000
_refine_ls_R_factor_gt           0.0576
_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^)+(0.0489P)^2^+0.2897P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1145
_refine_ls_wR_factor_ref         0.1306
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5647
_reflns_number_total             8686
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b12930_si_002.cif
_cod_data_source_block           hp350
_cod_depositor_comments
'Adding full bibliography for 4134168--4134181.cif.'
_cod_database_code               4134171
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C20H20N1O2
_chemical_oxdiff_usercomment     'yellow block (from rod) 0.30 x 0.26 x 0.14'
_shelx_estimated_absorpt_t_max   0.987
_shelx_estimated_absorpt_t_min   0.973
_reflns_odcompleteness_completeness 99.85
_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:
 C1A(H1A), C1B(H1B), C1C(H1C), C4A(H4A), C4B(H4B), C4C(H4C), C5A(H5A),
 C5B(H5B), C5C(H5C), C10A(H10A), C10B(H10B), C10C(H10C)
2.b Aromatic/amide H refined with riding coordinates:
 C3A(H3A), C3B(H3B), C3C(H3C), C6A(H6A), C6B(H6B), C6C(H6C), C7A(H7A),
 C7B(H7B), C7C(H7C), C8A(H8A), C8B(H8B), C8C(H8C), C9A(H9A), C9B(H9B), C9C(H9C),
  C12A(H12A), C12B(H12B), C12C(H12C), C13A(H13A), C13B(H13B), C13C(H13C),
 C15A(H15A), C15B(H15B), C15C(H15C), C16A(H16A), C16B(H16B), C16C(H16C)
;
_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 1.061
_oxdiff_exptl_absorpt_empirical_full_min 0.922