A Readily Accessible Chiral NNN Pincer Ligand with a Pyrrole Backbone and Its Ni(II) Chemistry: Syntheses, Structural Chemistry, and Bond Activations.
Wenz, Jan; Kochan, Alexander; Wadepohl, Hubert; Gade, Lutz H.; Inorganic chemistry 56 (2017) 3631–3643; doi:10.1021/acs.inorgchem.7b00077

data_4345589
_publ_section_title
;
 A Readily Accessible Chiral NNN Pincer Ligand with a Pyrrole Backbone and
 Its Ni(II) Chemistry: Syntheses, Structural Chemistry, and Bond
 Activations.
;
_journal_issue                   6
_journal_name_full               'Inorganic chemistry'
_journal_page_first              3631
_journal_page_last               3643
_journal_paper_doi               10.1021/acs.inorgchem.7b00077
_journal_volume                  56
_journal_year                    2017
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C18 H24 F N3 Ni O2, 0.5(H2 O)'
_chemical_formula_sum            'C18 H25 F N3 Ni O2.5'
_chemical_formula_weight         401.12
_space_group_crystal_system      trigonal
_space_group_IT_number           146
_space_group_name_Hall           'R 3'
_space_group_name_H-M_alt        'R 3'
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'R 3'
_symmetry_space_group_name_H-M   'R 3 :H'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_block_code                ga_jw16
_audit_creation_date
;
'Fri Sep 11 11:23:27 2015'
;
_audit_creation_method
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Olex2 1.2
(compiled Nov 22 2016 12:06:14 for OlexSys, GUI svn.r5269)
;
_audit_update_record
'13.12.2016 16:07:49 CET UTC+01:00  encif 1.59'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   40.6952(6)
_cell_length_b                   40.6952(6)
_cell_length_c                   6.06539(10)
_cell_measurement_reflns_used    30621
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      70.4610
_cell_measurement_theta_min      4.3300
_cell_volume                     8699.1(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material
'encif (Wadepohl, 2009-16); 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      120(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9621
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.9997
_diffrn_measured_fraction_theta_max 0.9923
_diffrn_measurement_details
;
  1 omega  -68.00  -43.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000  -30.0000 25

  2 omega  -18.00   14.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000  -30.0000 32

  3 omega  -72.00   42.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -19.0000   30.0000 114

  4 omega   -3.00   24.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000  -90.0000 27

  5 omega  -20.00   63.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000  150.0000 83

  6 omega   -8.00   48.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       10.0000   78.0000   32.3700 56

  7 omega   -6.00   19.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       26.0000   80.0000 -131.5788 25

  8 omega    2.00   27.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       34.0000   80.0000  131.8479 25

  9 omega    8.00   46.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       38.0000   78.0000  -69.9271 38

 10 omega    6.00   31.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       38.0000   80.0000  -30.7243 25

 11 omega   12.00   42.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   78.0000   92.4492 30

 12 omega   10.00   35.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   80.0000 -165.2235 25

 13 omega   15.00   40.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   79.0000  -46.5324 25

 14 omega   14.00   39.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   80.0000  -83.2309 25

 15 omega   15.00   40.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   78.0000    6.2451 25

 16 omega   18.00   46.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   79.0000  -24.5432 28

 17 omega   14.00   39.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   80.0000   63.3349 25

 18 omega   19.00   44.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   78.0000   60.6282 25

 19 omega   19.00   44.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   79.0000 -164.5674 25

 20 omega   26.00   52.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000   90.0000 26

 21 omega   31.00   57.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000   30.0000 26

 22 omega   98.00  124.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   75.0000   20.5210 26

 23 omega   24.00   50.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000 -120.0000 26

 24 omega   25.00   51.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   76.0000    8.6401 26

 25 omega   23.00   48.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   78.0000 -156.1063 25

 26 omega   25.00   52.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  -90.0000 27

 27 omega   26.00   51.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   75.0000   20.5210 25

 28 omega   25.00   51.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000    0.0000 26

 29 omega  -14.00   74.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -57.0000  150.0000 88

 30 omega   28.00   54.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  120.0000 26

 31 omega   28.00  125.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000  149.7778 97

 32 omega   30.00   56.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   75.0000   14.1823 26

 33 omega   29.00   55.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   76.0000  -45.0386 26

 34 omega   29.00   55.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   76.0000  -64.8749 26

 35 omega   81.00  118.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   76.0000  -64.8749 37

 36 omega   28.00   54.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000   50.1777 26

 37 omega   32.00   58.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   76.0000  128.6004 26

 38 omega   28.00   54.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000  100.8618 26

 39 omega   37.00   71.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   70.0000 -163.0735 34

 40 omega   33.00   70.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   75.0000  -89.1631 37

 41 omega   36.00   78.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   72.0000 -134.8045 42

 42 omega   81.00  130.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   72.0000 -134.8045 49

 43 omega   37.00   63.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   70.0000  -62.8412 26

 44 omega   33.00   59.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   76.0000 -165.0399 26

 45 omega   45.00   71.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   59.0000   47.7330 26

 46 omega   19.00   45.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000  -78.0000 -133.5883 26

 47 omega   -5.00   78.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000  -80.0000  -99.0855 83

 48 omega   49.00   76.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000  -78.0000 -133.5883 27

 49 omega   38.00   68.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   77.0000  -39.3859 30

 50 omega   37.00   64.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   75.0000   74.7833 27

 51 omega   45.00   71.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   69.0000   60.3874 26

 52 omega   43.00   72.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   76.0000  -15.8576 29

 53 omega   44.00   74.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   70.0000  178.0676 30

 54 omega    0.00   78.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000  -80.0000  -34.5229 78

 55 omega   42.00   67.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   73.0000  119.7296 25

 56 omega    3.00   87.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000  -79.0000   55.9323 84

 57 omega   50.00   75.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   68.0000  -23.9080 25

 58 omega   47.00   73.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   74.0000 -154.3120 26

 59 omega   45.00  125.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   77.0000  -79.0391 80

 60 omega   54.00  139.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   68.0000  177.9957 85

 61 omega   55.00  147.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   70.0000   66.1456 92

 62 omega   50.00   76.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   77.0000  -12.3400 26

 63 omega   49.00   78.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   76.0000   12.5823 29

 64 omega   64.00   90.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000  -80.0000  153.6053 26

 65 omega   71.00  111.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   55.0000  -90.7819 40

 66 omega   53.00   79.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   76.0000   95.7241 26

 67 omega   56.00   95.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   70.0000   46.4548 39

 68 omega   54.00   80.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   74.0000 -142.2654 26

 69 omega   53.00   85.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   76.0000  125.1141 32

 70 omega   56.00   82.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   70.0000  -16.2021 26

 71 omega   65.00   93.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   58.0000  -35.3811 28

 72 omega   64.00  119.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   64.0000  120.2771 55

 73 omega   63.00   89.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   65.0000 -153.8150 26

 74 omega   58.00   87.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   75.0000 -127.6866 29

 75 omega   58.00   84.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   74.0000  117.0554 26

 76 omega   61.00   93.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   76.0000   21.7752 32

 77 omega   62.00   88.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   74.0000   18.9996 26

 78 omega   60.00   91.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   77.0000  -30.7906 31

 79 omega   70.00   96.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       94.0000   67.0000 -171.8289 26

 80 omega   79.00  114.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       94.0000   61.0000  -86.2023 35

 81 omega   72.00  106.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       94.0000   64.0000   63.3929 34

 82 omega   80.00  119.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       98.0000   67.0000    9.3385 39

 83 omega   53.00  139.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000 -145.5147 86

 84 omega   82.00  108.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000  -30.0000 26

 85 omega   86.00  113.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  -90.0000 27

 86 omega   47.00  101.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000  156.6104 54

 87 omega   87.00  153.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000 -180.0000 66

 88 omega   86.00  174.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000    0.0000 88

 89 omega   88.00  175.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000   60.0000 87

 90 omega   85.00  174.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  120.0000 89

 91 omega   86.00  174.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  150.0000 88

 92 omega   79.00  106.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -60.0000 27

 93 omega   78.00  170.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   30.0000 92

 94 omega   73.00  104.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -79.0000  -73.9682 31

 95 omega   46.00   71.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -79.0000  -73.9682 25

 96 omega   78.00  177.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -150.0000 99

 97 omega  114.00  175.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -120.0000 61

 98 omega   83.00  109.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -120.0000 26

 99 omega   78.00  104.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   90.0000 26

100 omega   78.00  105.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000    0.0000 27

101 omega  114.00  178.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -90.0000 64

102 omega   85.00  174.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  -30.0000 89

103 omega   78.00  104.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -90.0000 26

104 omega  153.00  178.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  150.0000 25

105 omega   79.00  104.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  150.0000 25

106 omega  142.00  173.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -180.0000 31

107 omega   78.00  104.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -180.0000 26

108 omega   48.00  103.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000  -19.7937 55

109 omega   78.00  104.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   60.0000 26

110 omega   78.00  105.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  120.0000 27

111 omega   79.00  104.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -30.0000 25

112 omega   85.00  174.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  -60.0000 89

113 omega   85.00  112.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000   30.0000 27

114 omega   85.00  175.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000   90.0000 90

115 omega   47.00  140.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000   92.2348 93

116 omega   72.00  127.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -79.0000   20.0072 55

117 omega   87.00  112.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   63.0000  -90.8852 25

118 omega   70.00   97.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -79.0000 -106.7837 27

119 omega  -26.00   72.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   38.0000  -60.0000 98

120 omega  -72.00   26.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -38.0000   90.0000 98

121 omega  -73.00   44.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -19.0000 -120.0000 117

122 omega  -21.00   69.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000 -180.0000 90

123 omega   -8.00   92.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       22.0000   77.0000 -126.3048 100

124 omega   -2.00   95.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       26.0000   73.0000   52.8144 97

125 omega   -3.00   96.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       26.0000   76.0000  114.0990 99

126 omega   10.00   46.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   80.0000 -165.2235 36

127 omega   14.00   46.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   80.0000   63.3349 32

128 omega   15.00   47.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   79.0000  -46.5324 32

129 omega   14.00   46.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   80.0000  -83.2309 32

130 omega   19.00   49.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   78.0000  126.3454 30

131 omega   19.00   49.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   78.0000   60.6282 30

132 omega  -15.00   75.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -57.0000   30.0000 90

133 omega   23.00   49.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   78.0000 -156.1063 26

134 omega   29.00  128.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   76.0000  -64.8749 99

135 omega   34.00  131.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   73.0000  148.5480 97

136 omega   41.00  131.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   55.0000  -99.5004 90

137 omega   35.00  114.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   72.0000 -134.8045 79

138 omega   -4.00   97.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000  -78.0000 -133.5883 101

139 omega   -5.00   98.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000  -80.0000   15.4571 103

140 omega   45.00  138.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   69.0000   60.3874 93

141 omega   -1.00  102.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000  -80.0000  -34.5229 103

142 omega   44.00  144.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   77.0000  -79.0391 100

143 omega   46.00  144.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   74.0000 -154.3120 98

144 omega   50.00  142.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   68.0000  -23.9080 92

145 omega   49.00  148.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   76.0000   12.5823 99

146 omega   52.00  147.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   70.0000   66.1456 95

147 omega   56.00  146.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   63.0000  122.5549 90

148 omega   48.00  148.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   77.0000  -12.3400 100

149 omega   54.00  146.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   68.0000  177.9957 92

150 omega    7.00  110.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000  -80.0000  153.6053 103

;
_diffrn_measurement_device       'four-circle 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      0.0060254000
_diffrn_orient_matrix_UB_12      -0.0344776000
_diffrn_orient_matrix_UB_13      -0.0059428000
_diffrn_orient_matrix_UB_21      -0.0112779000
_diffrn_orient_matrix_UB_22      -0.0078679000
_diffrn_orient_matrix_UB_23      0.2449347000
_diffrn_orient_matrix_UB_31      -0.0417935000
_diffrn_orient_matrix_UB_32      -0.0256935000
_diffrn_orient_matrix_UB_33      -0.0669835000
_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  0.0581
_diffrn_reflns_av_unetI/netI     0.0241
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       49
_diffrn_reflns_limit_h_min       -49
_diffrn_reflns_limit_k_max       49
_diffrn_reflns_limit_k_min       -49
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            97877
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.132
_diffrn_reflns_theta_min         3.763
_diffrn_source                   'microfocus X-Ray tube'
_diffrn_source_type              'Agilent SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.691
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85861
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.378
_exptl_crystal_description       needle
_exptl_crystal_F_000             3798
_exptl_crystal_size_max          0.158
_exptl_crystal_size_mid          0.037
_exptl_crystal_size_min          0.029
_refine_diff_density_max         0.232
_refine_diff_density_min         -0.189
_refine_diff_density_rms         0.033
_refine_ls_abs_structure_details
;
 Flack x determined using 3306 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.032(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     474
_refine_ls_number_reflns         7438
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0281
_refine_ls_R_factor_gt           0.0265
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0266P)^2^+4.5506P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0571
_refine_ls_wR_factor_ref         0.0576
_reflns_Friedel_coverage         0.992
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.988
_reflns_number_gt                7184
_reflns_number_total             7438
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic7b00077_si_002.cif
_cod_data_source_block           ga_jw16_sq
_cod_original_cell_volume        8699.1(3)
_cod_original_formula_sum        'C18 H25 F N3 Ni O2.50'
_cod_database_code               4345589
_audit_block_refno               2522
_audit_block_usercomment         'jwig027, needle, red'
_chemical_oxdiff_formula         'C18 H25 F N3 Ni O2.5'
_chemical_oxdiff_usercomment     'jwig027, needle, red'
_shelx_estimated_absorpt_t_max   0.953
_shelx_estimated_absorpt_t_min   0.776
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_shelxl_version_number           2016/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.3 times of:
  All O(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C1(H1), C12(H12), C13(H13), C16(H16), C51(H51), C62(H62), C63(H63), C66(H66)
2.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C11(H11A,H11B), C52(H52A,H52B), C61(H61A,H61B)
2.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C7(H7), C9(H9), C54(H54), C56(H56), C57(H57), C59(H59)
2.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C17(H17A,H17B,H17C), C18(H18A,H18B,
 H18C), C64(H64A,H64B,H64C), C65(H65A,H65B,H65C), C67(H67A,H67B,H67C), C68(H68A,
 H68B,H68C)
;
_shelx_hkl_checksum              82748
_shelx_fab_checksum              69744
_olex2_submission_special_instructions 'No special instructions were received'
_shelx_res_checksum              3711
_cell_oxdiff_length_a            40.6959(8)
_cell_oxdiff_length_b            40.6907(7)
_cell_oxdiff_length_c            6.06507(10)
_cell_oxdiff_angle_alpha         89.9870(13)
_cell_oxdiff_angle_beta          90.0113(15)
_cell_oxdiff_angle_gamma         119.985(2)
_cell_oxdiff_volume              8699.1(3)
_cell_oxdiff_measurement_reflns_used 30625