Achiral and Chiral PNP-Pincer Ligands with a Carbazole Backbone: Coordination Chemistry with d8 Transition Metals
Nora Grüger; Lara-Isabel Rodríguez; Hubert Wadepohl; Lutz H. Gade; Inorganic Chemistry 52 (2013) 2050–2059; doi:10.1021/ic302454n

data_4333887
_publ_section_title
;
 Achiral and Chiral PNP-Pincer Ligands with a Carbazole Backbone:
 Coordination Chemistry with d8 Transition Metals
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2050
_journal_page_last               2059
_journal_paper_doi               10.1021/ic302454n
_journal_volume                  52
_journal_year                    2013
_chemical_absolute_configuration ad
_chemical_formula_sum            'C59 H70 Br N Ni P2'
_chemical_formula_weight         993.72
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_block_code                ga_ng24b
_audit_creation_date
;
'Tue Jul 31 00:22:06 2012'
;
_audit_creation_method           SHELXL-97
_audit_update_record             'Mon Oct 29 17:37:06 CET 2012'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.0831(7)
_cell_length_b                   20.0090(11)
_cell_length_c                   25.1315(11)
_cell_measurement_reflns_used    21126
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      73.3544
_cell_measurement_theta_min      3.5144
_cell_volume                     5070.3(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_publication_material
'encif (Wadepohl, 2012); encifer 1.4 (CCDC, 2011)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SUPERFLIP (Palatinus, 2007-2009)'
_diffrn_ambient_temperature      120.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9621
_diffrn_detector_type            'Agilent EOS'
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_details
;
  1 omega  -68.00   21.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000   30.0000 89

  2 omega  -68.00  -42.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000   86.0000 26

  3 omega    1.00   34.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000  -90.0000 33

  4 omega  -52.00   -6.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000  150.0000 46

  5 omega   -6.00   69.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000 -180.0000 75

  6 omega  -17.00   44.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       10.0000   80.0000  -32.0000 61

  7 omega   -6.00   19.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       26.0000   80.0000  112.0000 25

  8 omega    3.00   28.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       34.0000   78.0000  176.0000 25

  9 omega    7.00   32.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       38.0000   79.0000  103.0000 25

 10 omega   11.00   36.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   78.0000  -69.0000 25

 11 omega   12.00   37.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   80.0000  105.0000 25

 12 omega   11.00   37.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   80.0000  134.0000 26

 13 omega  -72.00   24.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000   77.0000 -180.0000 96

 14 omega  -51.00   30.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000   25.0000  150.0000 81

 15 omega  -44.00  -17.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000  120.0000 27

 16 omega  -39.00  -12.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000   90.0000 27

 17 omega   14.00   42.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   80.0000 -126.0000 28

 18 omega   15.00   40.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   79.0000  -52.0000 25

 19 omega   14.00   39.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   80.0000   35.0000 25

 20 omega   14.00   39.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   80.0000 -157.0000 25

 21 omega   15.00   40.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   79.0000   10.0000 25

 22 omega   15.00   40.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   78.0000   75.0000 25

 23 omega   18.00   43.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   80.0000  -64.0000 25

 24 omega   19.00   44.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   78.0000   66.0000 25

 25 omega   19.00   44.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   79.0000  124.0000 25

 26 omega   18.00   43.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   80.0000  -36.0000 25

 27 omega   19.00   44.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   79.0000   75.0000 25

 28 omega   19.00   46.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   78.0000  -87.0000 27

 29 omega   18.00   43.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   80.0000 -132.0000 25

 30 omega   19.00   45.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   78.0000   35.0000 26

 31 omega   20.00   45.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   78.0000  -13.0000 25

 32 omega   27.00   54.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   76.0000  -35.0000 27

 33 omega   80.00  107.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   76.0000  -35.0000 27

 34 omega   23.00   48.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   78.0000   62.0000 25

 35 omega   24.00   51.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  121.0000 27

 36 omega   24.00   51.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000 -177.0000 27

 37 omega   25.00   52.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   76.0000  139.0000 27

 38 omega   23.00   48.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   78.0000  -57.0000 25

 39 omega   99.00  124.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000 -177.0000 25

 40 omega   25.00   52.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000 -146.0000 27

 41 omega   23.00   48.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   78.0000   91.0000 25

 42 omega   23.00   48.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   78.0000   -2.0000 25

 43 omega   30.00   65.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   73.0000  -95.0000 35

 44 omega   28.00   55.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000  -90.0000 27

 45 omega   29.00   54.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000   84.0000 25

 46 omega   28.00   54.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000 -123.0000 26

 47 omega   29.00   54.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000   94.0000 25

 48 omega   28.00  104.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000 -150.0000 76

 49 omega   28.00   55.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000 -169.0000 27

 50 omega  103.00  128.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   75.0000  156.0000 25

 51 omega   85.00  112.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   75.0000   52.0000 27

 52 omega   30.00   57.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   75.0000  156.0000 27

 53 omega   29.00   55.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   75.0000   52.0000 26

 54 omega   31.00   59.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   73.0000  -23.0000 28

 55 omega   35.00  114.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   71.0000  -30.0000 79

 56 omega   33.00  131.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   75.0000  105.0000 98

 57 omega   34.00  107.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   73.0000 -125.0000 73

 58 omega   91.00  118.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   73.0000  -75.0000 27

 59 omega   36.00  131.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   70.0000   30.0000 95

 60 omega   34.00   83.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   73.0000  -75.0000 49

 61 omega   34.00  131.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   75.0000  142.0000 97

 62 omega   34.00  131.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   74.0000  128.0000 97

 63 omega   -4.00   82.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000  -80.0000   45.0000 86

 64 omega   -5.00   97.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000  -80.0000  -89.0000 102

 65 omega   69.00   94.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000  -79.0000  -55.0000 25

 66 omega   53.00   80.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000  -79.0000   -7.0000 27

 67 omega   53.00   80.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000  -79.0000   72.0000 27

 68 omega   12.00   87.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000  -80.0000  165.0000 75

 69 omega  125.00  159.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000  150.0000 34

 70 omega   93.00  120.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   50.0000  -90.0000 27

 71 omega   85.00  123.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000  150.0000 38

 72 omega   41.00  140.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -79.0000   41.0000 99

 73 omega   88.00  115.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   64.0000 -150.0000 27

 74 omega   85.00  111.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000 -150.0000 26

 75 omega   77.00  142.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -80.0000   79.0000 65

 76 omega   78.00  107.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -80.0000  -39.0000 29

 77 omega  117.00  142.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -80.0000  136.0000 25

 78 omega   82.00  108.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -80.0000  136.0000 26

 79 omega   88.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   64.0000   90.0000 90

 80 omega  153.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000   30.0000 25

 81 omega   86.00  113.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -80.0000  167.0000 27

 82 omega   48.00   75.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -80.0000  167.0000 27

 83 omega  122.00  177.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   64.0000   60.0000 55

 84 omega   40.00  141.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -80.0000  -84.0000 101

 85 omega   93.00  120.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   50.0000   60.0000 27

 86 omega   64.00   91.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -80.0000   93.0000 27

 87 omega   80.00  129.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -80.0000   -8.0000 49

 88 omega   39.00  141.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -80.0000 -137.0000 102

 89 omega   90.00  157.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   50.0000  -60.0000 67

 90 omega  152.00  177.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   64.0000    0.0000 25

 91 omega   88.00  115.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   64.0000    0.0000 27

 92 omega   89.00  114.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   64.0000 -120.0000 25

 93 omega   85.00  111.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000    0.0000 26

 94 omega   80.00  106.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000  -60.0000 26

 95 omega   88.00  177.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   64.0000 -180.0000 89

 96 omega   85.00  111.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000  120.0000 26

 97 omega   80.00  106.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000  150.0000 26

 98 omega   85.00  111.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000   60.0000 26

 99 omega   85.00  146.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000   90.0000 61

100 omega   85.00  128.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000 -120.0000 43

101 omega   89.00  116.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   57.0000  -86.0000 27

102 omega   85.00  141.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000 -180.0000 56

103 omega  132.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000  120.0000 46

104 omega   80.00  106.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000  120.0000 26

105 omega   80.00  106.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000 -180.0000 26

106 omega   88.00  117.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   64.0000   60.0000 29

107 omega  143.00  170.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000  -30.0000 27

108 omega   89.00  116.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   50.0000   30.0000 27

109 omega   80.00  106.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000  -30.0000 26

110 omega   86.00  113.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000   30.0000 27

111 omega  153.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   64.0000  150.0000 25

112 omega   88.00  115.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   64.0000  150.0000 27

113 omega   93.00  175.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   50.0000 -120.0000 82

114 omega   92.00  119.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   50.0000   90.0000 27

115 omega   80.00  106.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000    0.0000 26

116 omega   88.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   64.0000  -60.0000 90

117 omega   89.00  114.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   64.0000  120.0000 25

118 omega   96.00  176.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   50.0000  150.0000 80

119 omega   80.00  106.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000   30.0000 26

120 omega   80.00  177.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000 -120.0000 97

121 omega   88.00  114.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   64.0000  -30.0000 26

122 omega   89.00  114.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   50.0000 -150.0000 25

123 omega  136.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000 -150.0000 42

124 omega   91.00  177.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   50.0000    0.0000 86

125 omega   96.00  123.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   50.0000  120.0000 27

126 omega   85.00  118.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000  -30.0000 33

127 omega   80.00  106.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000 -150.0000 26

128 omega   80.00  111.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   25.0000  150.0000 31

129 omega   80.00  106.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000   60.0000 26

130 omega   80.00  117.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   25.0000   90.0000 37

131 omega   86.00  112.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000  -60.0000 26

132 omega  128.00  171.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000  -90.0000 43

133 omega   80.00  106.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000  -90.0000 26

134 omega   86.00  111.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000  -90.0000 25

135 omega  142.00  169.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   64.0000   30.0000 27

136 omega   80.00  106.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000   90.0000 26

137 omega   89.00  114.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   64.0000   30.0000 25

138 omega   88.00  115.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   64.0000  -90.0000 27

139 omega   94.00  119.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   50.0000 -180.0000 25

140 omega   92.00  177.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   50.0000  -30.0000 85

;
_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      0.0013910000
_diffrn_orient_matrix_UB_12      0.0598372000
_diffrn_orient_matrix_UB_13      0.0386118000
_diffrn_orient_matrix_UB_21      0.1439934000
_diffrn_orient_matrix_UB_22      0.0156670000
_diffrn_orient_matrix_UB_23      -0.0162178000
_diffrn_orient_matrix_UB_31      -0.0509901000
_diffrn_orient_matrix_UB_32      0.0458380000
_diffrn_orient_matrix_UB_33      -0.0447887000
_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  0.1064
_diffrn_reflns_av_sigmaI/netI    0.0392
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            122909
_diffrn_reflns_theta_full        73.51
_diffrn_reflns_theta_max         73.51
_diffrn_reflns_theta_min         3.52
_diffrn_source                   'microfocus X-Ray tube'
_diffrn_source_type              'Agilent SuperNova (Cu) x-ray Source'
_exptl_absorpt_coefficient_mu    2.354
_exptl_absorpt_correction_T_max  0.981
_exptl_absorpt_correction_T_min  0.890
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.302
_exptl_crystal_description       needle
_exptl_crystal_F_000             2096
_exptl_crystal_size_max          0.3288
_exptl_crystal_size_mid          0.0720
_exptl_crystal_size_min          0.0333
_refine_diff_density_max         0.860
_refine_diff_density_min         -0.603
_refine_diff_density_rms         0.077
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.027(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     585
_refine_ls_number_reflns         9958
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0463
_refine_ls_R_factor_gt           0.0426
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0752P)^2^+1.4243P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1108
_refine_ls_wR_factor_ref         0.1153
_reflns_number_gt                9344
_reflns_number_total             9958
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302454n_si_002_7.cif
_cod_data_source_block           complex_13b
_cod_original_cell_volume        5070.4(5)
_cod_database_code               4333887
_audit_block_refno               1552
_audit_block_usercomment         'NGBP-004, needle, green'
_cell_oxdiff_length_a            10.0851(6)
_cell_oxdiff_length_b            20.0112(7)
_cell_oxdiff_length_c            25.1240(8)
_cell_oxdiff_angle_alpha         90.042(3)
_cell_oxdiff_angle_beta          90.017(4)
_cell_oxdiff_angle_gamma         90.022(4)
_cell_oxdiff_volume              5070.4(4)
_cell_oxdiff_measurement_reflns_used 21103
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_theta     66.97
_reflns_odcompleteness_iscentric 1