N,O-Benzamide difluoroboron complexes as near-infrared probes for the detection of β-amyloid and tau fibrils.
Chen, Yimin; Yuan, Chang; Xie, Tianxin; Li, Yuying; Dai, Bin; Zhou, Kaixiang; Liang, Yi; Dai, Jiapei; Tan, Hongwei; Cui, Mengchao; Chemical communications (Cambridge, England) 56 (2020) 7269–7272; doi:10.1039/d0cc02820g

data_7126594
_publ_section_title
;
 N,O-Benzamide difluoroboron complexes as near-infrared probes for the
 detection of \b-amyloid and tau fibrils.
;
_journal_issue                   53
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              7269
_journal_page_last               7272
_journal_paper_doi               10.1039/d0cc02820g
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C22 H20 B F2 N3 O'
_chemical_formula_sum            'C22 H20 B F2 N3 O'
_chemical_formula_weight         391.22
_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     dual
_audit_creation_date             2019-04-09
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                74.878(6)
_cell_angle_beta                 76.982(6)
_cell_angle_gamma                83.501(6)
_cell_formula_units_Z            2
_cell_length_a                   7.9478(6)
_cell_length_b                   8.3539(5)
_cell_length_c                   14.6488(10)
_cell_measurement_reflns_used    2094
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      75.4040
_cell_measurement_theta_min      5.4810
_cell_volume                     913.27(11)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2137
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.962
_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    -65.00  -4.00   1.00    2.67    --  -40.81 125.00 -30.00   61
  2  \w    -64.00  33.00   1.00    2.67    --  -40.81  38.00 -90.00   97
  3  \w   -113.00 -20.00   1.00    2.67    --  -40.81 -44.00 101.00   93
  4  \w      5.00  55.00   1.00    2.67    --   40.81 -99.00 -30.00   50
  5  \w     55.00  97.00   1.00    2.67    --   40.81-125.00-180.00   42
  6  \w    120.00 167.00   1.00   10.67    --  110.27 125.00-150.00   47
  7  \w     54.00 135.00   1.00   10.67    --  110.27 -45.00 120.00   81
  8  \w     56.00  81.00   1.00   10.67    --  110.27 -30.00-180.00   25
  9  \w     60.00 105.00   1.00   10.67    --  110.27 -95.00 -30.00   45
 10  \w    102.00 137.00   1.00   10.67    --  110.27 -30.00  30.00   35
 11  \w     68.00  94.00   1.00   10.67    --  110.27 -30.00  30.00   26
 12  \w     74.00 178.00   1.00   10.67    --  110.27  15.00 120.00  104
 13  \w     59.00 108.00   1.00   10.67    --  110.27 -95.00-120.00   49
 14  \w     29.00 108.00   1.00   10.67    --  110.27 -95.00  30.00   79
 15  \w     94.00 126.00   1.00   10.67    --  110.27 125.00 120.00   32
 16  \w     60.00 132.00   1.00   10.67    --  110.27 -45.00-150.00   72
 17  \w     98.00 178.00   1.00   10.67    --  110.27  77.00-180.00   80
 18  \w     36.00 106.00   1.00   10.67    --  110.27 -95.00 150.00   70
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1384417000
_diffrn_orient_matrix_UB_12      0.0214511000
_diffrn_orient_matrix_UB_13      -0.0615379000
_diffrn_orient_matrix_UB_21      -0.0323925000
_diffrn_orient_matrix_UB_22      0.1839474000
_diffrn_orient_matrix_UB_23      0.0032770000
_diffrn_orient_matrix_UB_31      0.1396374000
_diffrn_orient_matrix_UB_32      0.0481364000
_diffrn_orient_matrix_UB_33      -0.0926595000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0264
_diffrn_reflns_av_unetI/netI     0.0456
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            6123
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.965
_diffrn_reflns_theta_min         5.495
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.843
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87793
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_density_diffrn    1.423
_exptl_crystal_description       needle
_exptl_crystal_F_000             408
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.325
_refine_diff_density_min         -0.260
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     264
_refine_ls_number_reflns         3674
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0623
_refine_ls_R_factor_gt           0.0467
_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^)+(0.0675P)^2^+0.0497P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1206
_refine_ls_wR_factor_ref         0.1332
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2860
_reflns_number_total             3674
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc02820g4.cif
_cod_data_source_block           20190408chenyimin-1-3
_cod_depositor_comments          'Adding full bibliography for 7126594.cif.'
_cod_database_code               7126594
_shelx_shelxl_version_number     2014/7
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     67.79
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C00A(H00A), C00B(H00B), C00D(H00D), C00E(H00E), C00F(H00F), C00G(H00G),
 C00J(H00J), C00K(H00K), C00L(H00L), C00M(H00M), C00N(H00N), C00O(H00O),
 C00P(H00P), C00Q(H00Q)
2.b Idealised Me refined as rotating group:
 C00R(H00C,H00H,H00I), C00S(H00R,H00S,H00T)
;
_shelx_res_checksum              48590
_shelx_hkl_checksum              77224
_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 1.403
_oxdiff_exptl_absorpt_empirical_full_min 0.751