Isolation and structural characterization of a titanacyclopropane as key intermediate in the double aryl Grignard addition to 2-(arylethynyl)pyridine derivatives.
Foschi, Francesco; Roth, Torsten; Enders, Markus; Wadepohl, Hubert; Clot, Eric; Gade, Lutz H.; Chemical communications (Cambridge, England) 54 (2018) 2228–2231; doi:10.1039/c8cc00478a

data_7121238
_publ_section_title
;
 Isolation and structural characterization of a titanacyclopropane as key
 intermediate in the double aryl Grignard addition to
 2-(arylethynyl)pyridine derivatives.
;
_journal_issue                   18
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              2228
_journal_page_last               2231
_journal_paper_doi               10.1039/c8cc00478a
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         'C24 H15 F3 N2'
_chemical_formula_sum            'C24 H15 F3 N2'
_chemical_formula_weight         388.38
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_block_code                ga_tro55
_audit_creation_date
;
'Thu Jan 23 17:11:22 2014'
;
_audit_creation_method
;
Olex2 1.2
(compiled Aug 10 2017 17:44:14 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-01-17 deposited with the CCDC.
2018-02-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.012(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.06788(17)
_cell_length_b                   5.50360(16)
_cell_length_c                   37.4304(11)
_cell_measurement_reflns_used    16733
_cell_measurement_temperature    110(1)
_cell_measurement_theta_max      70.3550
_cell_measurement_theta_min      4.7350
_cell_volume                     1857.73(8)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material
'encif (Wadepohl, 2009-17); encifer 1.5.2 (CCDC, 2016)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SUPERFLIP (Palatinus, 2007-2009)'
_diffrn_ambient_environment      'perfluoro polyether oil / N~2~'
_diffrn_ambient_temperature      110(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9621
_diffrn_detector_type            'Agilent EOS'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
;
  1 omega   43.00   68.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000 -180.0000 25

  2 omega   11.00   65.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   38.0000  -90.0000 54

  3 omega  -21.00   33.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000 -180.0000 54

  4 omega  -25.00    4.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   38.0000  -90.0000 29

  5 omega   15.00   43.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -19.0000  -60.0000 28

  6 omega  -38.00  -10.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -19.0000  -60.0000 28

  7 omega  -70.00    8.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -19.0000   90.0000 78

  8 omega  -18.00    9.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       10.0000   78.0000  -36.7725 27

  9 omega   33.00   84.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       14.0000   74.0000   45.8711 51

 10 omega  -14.00   30.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       14.0000   74.0000   45.8711 44

 11 omega    6.00   35.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       38.0000   80.0000   -4.7506 29

 12 omega    6.00   31.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       38.0000   80.0000 -143.4453 25

 13 omega   10.00   35.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   80.0000  -96.7895 25

 14 omega   10.00   35.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   80.0000   69.3420 25

 15 omega   15.00   40.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   79.0000  107.8577 25

 16 omega   14.00   39.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   80.0000 -158.1460 25

 17 omega   15.00   40.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   78.0000  155.1236 25

 18 omega   15.00   40.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   79.0000   18.9777 25

 19 omega   20.00   46.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   77.0000  -17.9530 26

 20 omega   93.00  120.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   77.0000   18.9330 27

 21 omega   20.00   46.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   79.0000  151.7550 26

 22 omega   21.00   47.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   77.0000   18.9330 26

 23 omega   19.00   44.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   78.0000 -121.7016 25

 24 omega   19.00   44.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   79.0000  -57.0658 25

 25 omega   19.00   44.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   79.0000  -89.5757 25

 26 omega   23.00   48.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   78.0000  179.9186 25

 27 omega   24.00   50.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  120.0000 26

 28 omega   89.00  124.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000 -150.0000 35

 29 omega   29.00   55.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000   30.0000 26

 30 omega   23.00   48.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   78.0000   80.3497 25

 31 omega  -16.00   84.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -77.0000  -90.0000 100

 32 omega   23.00   48.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   78.0000   52.5445 25

 33 omega   24.00   50.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000 -150.0000 26

 34 omega   25.00   51.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  -90.0000 26

 35 omega   25.00   50.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  -30.0000 25

 36 omega   23.00   48.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   78.0000   20.5820 25

 37 omega   29.00   55.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  -60.0000 26

 38 omega   33.00   59.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   71.0000   60.6661 26

 39 omega   28.00   53.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000  -23.8749 25

 40 omega   29.00   55.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000   23.4717 26

 41 omega   28.00   57.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000  146.0684 29

 42 omega   36.00   61.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   68.0000  112.1175 25

 43 omega   31.00   57.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   74.0000  -74.7545 26

 44 omega   35.00   61.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   71.0000 -125.2225 26

 45 omega   40.00   66.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   68.0000   49.3742 26

 46 omega   33.00   59.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   76.0000  126.4113 26

 47 omega   -9.00   94.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000  -80.0000  104.0746 103

 48 omega  109.00  134.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   68.0000   80.4749 25

 49 omega   43.00   93.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   68.0000   80.4749 50

 50 omega  105.00  131.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   68.0000 -141.4815 26

 51 omega   48.00   74.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   68.0000 -141.4815 26

 52 omega   37.00   63.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   76.0000 -177.1426 26

 53 omega   52.00   78.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000  -80.0000 -153.7299 26

 54 omega   37.00   83.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   75.0000   47.1184 46

 55 omega  110.00  136.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   74.0000 -166.5222 26

 56 omega   38.00   64.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   74.0000 -166.5222 26

 57 omega   70.00   95.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000  -80.0000  132.3742 25

 58 omega   50.00   76.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   67.0000 -151.2040 26

 59 omega   51.00  119.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   67.0000  -44.3505 68

 60 omega   41.00   71.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   75.0000 -113.5183 30

 61 omega   42.00   68.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   76.0000  106.9193 26

 62 omega   49.00   85.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   60.0000   29.7574 36

 63 omega   44.00   93.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   73.0000  127.2491 49

 64 omega   42.00   68.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   73.0000  101.0961 26

 65 omega   41.00   81.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   75.0000  -69.6152 40

 66 omega   41.00   90.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   76.0000  -14.5020 49

 67 omega   50.00  106.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   59.0000 -177.9111 56

 68 omega   46.00   72.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   72.0000  -93.2224 26

 69 omega   47.00   72.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   71.0000 -171.2837 25

 70 omega   51.00   77.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   64.0000 -105.8325 26

 71 omega   50.00   89.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   68.0000   86.0036 39

 72 omega   57.00   83.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   74.0000  -23.1273 26

 73 omega   52.00   90.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   62.0000  -72.5554 38

 74 omega   49.00   76.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   75.0000   30.7817 27

 75 omega   84.00  109.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   70.0000   48.7141 25

 76 omega   52.00   78.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   70.0000   48.7141 26

 77 omega   57.00  103.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   53.0000  -85.0892 46

 78 omega   49.00  147.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   76.0000  176.9435 98

 79 omega   51.00   81.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   72.0000   94.2292 30

 80 omega   49.00   75.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   75.0000  -31.2709 26

 81 omega   63.00   89.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   72.0000   60.7497 26

 82 omega   56.00   82.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   70.0000  -92.4924 26

 83 omega   62.00  149.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   63.0000  -10.1707 87

 84 omega   54.00   80.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   74.0000  -77.7744 26

 85 omega   57.00   86.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   75.0000  -75.3469 29

 86 omega   58.00   83.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   73.0000   50.8238 25

 87 omega   60.00   86.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   70.0000    6.2915 26

 88 omega   63.00   95.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   68.0000  150.1476 32

 89 omega   63.00   93.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   66.0000  -26.3335 30

 90 omega   64.00   91.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   35.0000  130.0871 27

 91 omega   60.00   86.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   70.0000   99.5368 26

 92 omega   58.00  144.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   75.0000  116.1103 86

 93 omega   64.00   90.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   45.0000  -98.2342 26

 94 omega   18.00   87.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000  -80.0000  -27.3800 69

 95 omega   61.00   87.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   76.0000   95.1330 26

 96 omega   70.00   96.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   48.0000 -154.1602 26

 97 omega   79.00  106.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       94.0000   63.0000   59.1814 27

 98 omega   66.00   97.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       94.0000   73.0000  133.3236 31

 99 omega   70.00   97.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       94.0000   67.0000   21.9161 27

100 omega   65.00  156.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       94.0000   75.0000  -64.4721 91

101 omega   71.00   97.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       94.0000   65.0000 -172.4761 26

102 omega   70.00   95.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       98.0000   74.0000  -86.9515 25

103 omega   71.00  103.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       98.0000   71.0000  149.5549 32

104 omega   81.00  108.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      102.0000   52.0000  -10.5839 27

105 omega   74.00  114.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      102.0000   73.0000   29.7923 40

106 omega   78.00  177.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -90.0000 99

107 omega  151.00  176.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   90.0000 25

108 omega   78.00  104.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   90.0000 26

109 omega  110.00  166.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  150.0000 56

110 omega   78.00  104.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  150.0000 26

111 omega  150.00  176.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -120.0000 26

112 omega   78.00  103.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -120.0000 25

113 omega   78.00  177.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -30.0000 99

114 omega  108.00  177.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   60.0000 69

115 omega   79.00  105.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   60.0000 26

116 omega  130.00  175.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000    0.0000 45

117 omega   86.00  127.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000    0.0000 41

118 omega   78.00  177.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  120.0000 99

119 omega  135.00  166.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -60.0000 31

120 omega   78.00  115.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -60.0000 37

121 omega  126.00  174.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000   90.0000 48

122 omega   85.00  122.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000   90.0000 37

123 omega   83.00  109.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   72.0000 -100.2567 26

124 omega   77.00  103.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -79.0000  114.1098 26

125 omega   78.00  178.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  167.3419 100

126 omega   78.00  104.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -150.0000 26

127 omega   80.00  106.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   76.0000 -141.8702 26

128 omega   83.00  139.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000  -27.5363 56

129 omega   70.00  123.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000   23.9275 53

130 omega   78.00  103.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000  103.1698 25

131 omega   48.00  134.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -79.0000  -90.7929 86

132 omega   46.00  107.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -79.0000  152.2262 61

133 omega   70.00  104.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -79.0000   73.3462 34

134 omega  132.00  176.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   61.0000 -157.2657 44

135 omega   86.00  112.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   61.0000 -157.2657 26

136 omega   85.00  162.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000 -120.0000 77

137 omega   87.00  156.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  120.0000 69

138 omega   85.00  111.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  150.0000 26

139 omega   85.00  111.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000 -150.0000 26

140 omega   86.00  115.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000   60.0000 29

141 omega   85.00  111.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  -60.0000 26

142 omega   85.00  174.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000 -120.0000 89

143 omega   83.00  127.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -79.0000 -130.4789 44

144 omega   78.00  177.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   30.0000 99

145 omega   78.00  104.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000    0.0000 26

146 omega   44.00   70.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -79.0000 -130.4789 26

147 omega   79.00  105.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -180.0000 26

148 omega  123.00  173.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -150.0000 50

149 omega   56.00  108.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -79.0000 -161.7266 52

150 omega  -69.00   21.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000    0.0000 90

151 omega  -72.00   26.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -38.0000   30.0000 98

152 omega  -73.00   44.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -19.0000   30.0000 117

153 omega  -19.00   80.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       10.0000   76.0000  148.4008 99

154 omega  -11.00   88.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0000   76.0000  -36.3579 99

155 omega   -7.00   92.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       22.0000   76.0000   76.1932 99

156 omega   -8.00   92.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       22.0000   77.0000    7.1442 100

157 omega   -4.00   96.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       26.0000   77.0000 -175.4551 100

158 omega    2.00   97.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       26.0000   44.0000  -70.1503 95

159 omega  -18.00   80.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -38.0000   90.0000 98

160 omega  -15.00   75.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -57.0000  -30.0000 90

161 omega    0.00  101.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000  -78.0000  -61.1795 101

162 omega   55.00  138.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   66.0000  132.6372 83

163 omega   57.00  148.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   53.0000  -85.0892 91

164 omega   49.00  148.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   75.0000   30.7817 99

;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Agilent SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'polyimid foil'
_diffrn_orient_matrix_UB_11      0.1659480000
_diffrn_orient_matrix_UB_12      -0.0049345000
_diffrn_orient_matrix_UB_13      -0.0055029000
_diffrn_orient_matrix_UB_21      -0.0135777000
_diffrn_orient_matrix_UB_22      -0.2698338000
_diffrn_orient_matrix_UB_23      -0.0107817000
_diffrn_orient_matrix_UB_31      -0.0381943000
_diffrn_orient_matrix_UB_32      0.0741857000
_diffrn_orient_matrix_UB_33      -0.0395844000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.1176
_diffrn_reflns_av_unetI/netI     0.0348
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            53581
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.874
_diffrn_reflns_theta_min         4.752
_diffrn_source                   'microfocus X-Ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.863
_exptl_absorpt_correction_T_max  0.964
_exptl_absorpt_correction_T_min  0.833
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Numerical absorption correction based on gaussian integration over
 a multifaceted crystal model (Busing & Levy, 1957).
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.389
_exptl_crystal_description       needle
_exptl_crystal_F_000             800
_exptl_crystal_size_max          0.274
_exptl_crystal_size_mid          0.098
_exptl_crystal_size_min          0.043
_refine_diff_density_max         0.228
_refine_diff_density_min         -0.275
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         3543
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0472
_refine_ls_R_factor_gt           0.0398
_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^)+(0.0522P)^2^+0.6680P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1029
_refine_ls_wR_factor_ref         0.1090
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3027
_reflns_number_total             3543
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc00478a2.cif
_cod_data_source_block           ga_tro55
_cod_depositor_comments
'Adding full bibliography for 7121234--7121240.cif.'
_cod_database_code               7121238
_audit_block_refno               1947
_audit_block_usercomment         'tr1186, needle, colourless'
_chemical_oxdiff_formula         'C24 H15 F3 N2'
_chemical_oxdiff_usercomment     'tr1186, needle, colourless'
_shelx_estimated_absorpt_t_max   0.919
_shelx_estimated_absorpt_t_min   0.919
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_shelxl_version_number           2018/1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
;
_olex2_submission_special_instructions 'No special instructions were received'
_shelx_res_checksum              39887
_cell_oxdiff_length_a            9.0687(2)
_cell_oxdiff_length_b            5.50418(15)
_cell_oxdiff_length_c            37.4255(9)
_cell_oxdiff_angle_alpha         89.998(2)
_cell_oxdiff_angle_beta          96.049(2)
_cell_oxdiff_angle_gamma         90.014(2)
_cell_oxdiff_volume              1857.73(8)
_cell_oxdiff_measurement_reflns_used 16733