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_4333882
_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_formula_sum            'C50 H54 Cl N O P2 Pd'
_chemical_formula_weight         888.73
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_block_code                ga_ng23a
_audit_creation_date
;
'Tue Jun 19 11:36:04 2012'
;
_audit_creation_method
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_audit_update_record             'Tue Jun 19 11:38:13 CEST 2012'
_cell_angle_alpha                63.244(3)
_cell_angle_beta                 75.697(3)
_cell_angle_gamma                68.328(3)
_cell_formula_units_Z            2
_cell_length_a                   12.7237(4)
_cell_length_b                   13.9205(5)
_cell_length_c                   14.7922(4)
_cell_measurement_reflns_used    18751
_cell_measurement_temperature    110.00(10)
_cell_measurement_theta_max      71.7495
_cell_measurement_theta_min      3.7225
_cell_volume                     2163.78(14)
_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  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SUPERFLIP (Palatinus, 2007-2009)'
_diffrn_ambient_temperature      110.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9241
_diffrn_detector_type            'Agilent EOS'
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_details
;
  1 omega  -20.00    7.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   38.0000   60.0000 27

  2 omega  -19.00   64.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000  -90.0000 83

  3 omega  -67.00  -42.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000    0.0000 25

  4 omega   24.00   61.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   38.0000   60.0000 37

  5 omega  -88.00  -40.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.0000  -76.0000  -62.0000 48

  6 omega  -24.00    1.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.0000  -76.0000  -62.0000 25

  7 omega  -24.00    2.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      -30.0000  -80.0000   75.0000 26

  8 omega  -39.00  -12.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000   60.0000 27

  9 omega  -40.00  -13.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000   30.0000 27

 10 omega  -47.00  -12.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000 -150.0000 35

 11 omega  -45.00   29.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000   38.0000 -120.0000 74

 12 omega  -49.00   27.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000   25.0000   30.0000 76

 13 omega  -42.00  -15.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000  120.0000 27

 14 omega  -44.00  -17.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000   90.0000 27

 15 omega  -48.00  -13.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000  -60.0000 35

 16 omega -111.00  -82.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -57.0000 -180.0000 29

 17 omega  -46.00   25.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000   63.0000  120.0000 71

 18 omega  -40.00  -13.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000 -120.0000 27

 19 omega   14.00   39.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   80.0000   68.0000 25

 20 omega   15.00   41.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   78.0000  -18.0000 26

 21 omega   18.00   43.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   80.0000 -112.0000 25

 22 omega   19.00   44.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   79.0000   -6.0000 25

 23 omega   19.00   44.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   79.0000 -175.0000 25

 24 omega   18.00   43.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   80.0000  133.0000 25

 25 omega   19.00   44.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   79.0000 -146.0000 25

 26 omega   59.00   86.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   77.0000   28.0000 27

 27 omega   21.00   50.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   77.0000   28.0000 29

 28 omega   55.00  107.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  103.0000 52

 29 omega   23.00   48.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   78.0000  -18.0000 25

 30 omega   23.00   48.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   78.0000   80.0000 25

 31 omega   71.00  123.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   76.0000 -127.0000 52

 32 omega   27.00   60.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   76.0000 -127.0000 33

 33 omega   23.00   48.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   78.0000  165.0000 25

 34 omega   26.00   60.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   75.0000  -75.0000 34

 35 omega   23.00   48.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   78.0000  100.0000 25

 36 omega    7.00   83.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       55.1171  -77.0000   30.0000 76

 37 omega   26.00   55.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       55.1171   77.0000  -60.0000 29

 38 omega   58.00  103.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       55.1171   77.0000  -60.0000 45

 39 omega   -1.00   84.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       55.1171  -77.0000  -60.0000 85

 40 omega   30.00  112.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   76.0000  -35.0000 82

 41 omega   29.00  128.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   76.0000   54.0000 99

 42 omega   34.00  128.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   74.0000   91.0000 94

 43 omega   30.00  127.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   73.0000 -159.0000 97

 44 omega   51.00   78.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000  -80.0000 -104.0000 27

 45 omega    4.00  105.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000  -80.0000  159.0000 101

 46 omega   54.00   81.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000  -79.0000 -118.0000 27

 47 omega  115.00  142.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -80.0000  138.0000 27

 48 omega   70.00  110.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -80.0000  138.0000 40

 49 omega   40.00  142.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -80.0000 -143.0000 102

 50 omega   40.00   66.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -77.0000 -180.0000 26

 51 omega  146.00  172.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000  -60.0000 26

 52 omega   40.00  141.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -80.0000   35.0000 101

 53 omega   80.00  107.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000  -60.0000 27

 54 omega   86.00  111.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000  120.0000 25

 55 omega   91.00  118.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -77.0000 -180.0000 27

 56 omega   89.00  177.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   50.0000   60.0000 88

 57 omega   91.00  157.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   50.0000  150.0000 66

 58 omega   80.00  106.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000  -90.0000 26

 59 omega  141.00  168.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000 -180.0000 27

 60 omega   85.00  120.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000   30.0000 35

 61 omega   81.00  106.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000   60.0000 25

 62 omega  153.00  178.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000   60.0000 25

 63 omega   81.00  106.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000 -180.0000 25

 64 omega  148.00  175.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000   90.0000 27

 65 omega   80.00  106.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000   90.0000 26

 66 omega   40.00  116.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -80.0000  -78.0000 76

 67 omega   88.00  115.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   63.0000 -120.0000 27

 68 omega   81.00  106.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000    0.0000 25

 69 omega   91.00  177.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   63.0000 -150.0000 86

 70 omega  123.00  171.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000 -120.0000 48

 71 omega  117.00  142.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -80.0000   96.0000 25

 72 omega   80.00  106.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000 -120.0000 26

 73 omega   92.00  177.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   50.0000  -60.0000 85

 74 omega   44.00   99.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -80.0000   96.0000 55

 75 omega  144.00  171.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000  -30.0000 27

 76 omega   80.00  106.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000   30.0000 26

 77 omega   80.00  106.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000  -30.0000 26

 78 omega   91.00  118.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   50.0000  120.0000 27

 79 omega   92.00  145.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   50.0000    0.0000 53

 80 omega  132.00  172.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   63.0000  120.0000 40

 81 omega   90.00  117.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   50.0000   90.0000 27

 82 omega   89.00  116.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   50.0000 -180.0000 27

 83 omega   89.00  114.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   63.0000  120.0000 25

 84 omega   88.00  177.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   50.0000   30.0000 89

 85 omega   88.00  117.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   50.0000 -120.0000 29

 86 omega   86.00  115.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000   60.0000 29

 87 omega  117.00  149.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   50.0000 -150.0000 32

 88 omega  150.00  177.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   63.0000   30.0000 27

 89 omega   89.00  114.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   63.0000  -30.0000 25

 90 omega   92.00  119.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   50.0000  -90.0000 27

 91 omega   39.00   88.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -80.0000   87.0000 49

 92 omega   94.00  121.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   50.0000  -30.0000 27

 93 omega   89.00  116.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   50.0000 -150.0000 27

 94 omega   89.00  116.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   63.0000   30.0000 27

 95 omega   85.00  111.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000  150.0000 26

 96 omega   81.00  106.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000 -150.0000 25

 97 omega   85.00  111.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000  -30.0000 26

 98 omega   88.00  176.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   63.0000  -90.0000 88

 99 omega   88.00  115.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   63.0000  -60.0000 27

100 omega  152.00  177.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   63.0000  -60.0000 25

101 omega   89.00  116.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   63.0000   60.0000 27

102 omega   89.00  114.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   63.0000  150.0000 25

103 omega   85.00  111.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000  -60.0000 26

104 omega   85.00  178.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000   90.0000 93

105 omega   85.00  115.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000 -120.0000 30

106 omega   86.00  111.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000 -150.0000 25

107 omega   89.00  176.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   63.0000    0.0000 87

108 omega  149.00  176.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000 -180.0000 27

109 omega   80.00  106.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000  120.0000 26

110 omega   89.00  114.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   63.0000   90.0000 25

111 omega   85.00  111.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000 -180.0000 26

112 omega   85.00  154.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000    0.0000 69

113 omega   85.00  157.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000  -90.0000 72

114 omega   67.00   94.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -78.0000  -17.0000 27

115 omega   88.00  115.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   63.0000 -180.0000 27

116 omega   41.00   66.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -78.0000  -17.0000 25

117 omega   81.00  174.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000  150.0000 93

118 omega   77.00  108.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   25.0000  -90.0000 31

119 omega   74.00   99.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -79.0000   -4.0000 25

120 omega  -26.00   72.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   38.0000 -180.0000 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  -26.00   72.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   38.0000    0.0000 98

123 omega  -63.00   26.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000   57.0000  -90.0000 89

124 omega   20.00  120.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   77.0000  -97.0000 100

125 omega   18.00   46.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   80.0000  115.0000 28

126 omega   23.00   49.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   78.0000  165.0000 26

127 omega  -15.00   85.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       55.1171  -77.0000   60.0000 100

128 omega  -13.00   90.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000  -80.0000  148.0000 103

129 omega   30.00  128.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   74.0000   91.0000 98

130 omega   29.00  128.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   76.0000  -35.0000 99

131 omega   30.00  127.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   73.0000 -159.0000 97

132 omega   29.00  128.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   76.0000   54.0000 99

133 omega   -1.00  102.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000  -80.0000 -104.0000 103

;
_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      -0.0084695000
_diffrn_orient_matrix_UB_12      -0.0538873000
_diffrn_orient_matrix_UB_13      0.1171261000
_diffrn_orient_matrix_UB_21      -0.0757007000
_diffrn_orient_matrix_UB_22      0.1144118000
_diffrn_orient_matrix_UB_23      0.0028415000
_diffrn_orient_matrix_UB_31      -0.1064664000
_diffrn_orient_matrix_UB_32      -0.0294419000
_diffrn_orient_matrix_UB_33      0.0026928000
_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  0.0668
_diffrn_reflns_av_sigmaI/netI    0.1311
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            56830
_diffrn_reflns_theta_full        66.97
_diffrn_reflns_theta_max         71.7495
_diffrn_reflns_theta_min         3.7225
_diffrn_source                   'Agilent SuperNova (Cu) x-ray Source'
_exptl_absorpt_coefficient_mu    5.010
_exptl_absorpt_correction_T_max  0.886
_exptl_absorpt_correction_T_min  0.539
_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            red
_exptl_crystal_density_diffrn    1.364
_exptl_crystal_description       plate
_exptl_crystal_F_000             924
_exptl_crystal_size_max          0.1636
_exptl_crystal_size_mid          0.0631
_exptl_crystal_size_min          0.0248
_refine_diff_density_max         0.698
_refine_diff_density_min         -0.680
_refine_diff_density_rms         0.070
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     511
_refine_ls_number_reflns         8291
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0366
_refine_ls_R_factor_gt           0.0309
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0357P)^2^+1.7061P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0742
_refine_ls_wR_factor_ref         0.0770
_reflns_number_gt                7423
_reflns_number_total             8291
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302454n_si_002_2.cif
_cod_data_source_block           complex_8
_cod_original_cell_volume        2163.78(12)
_cod_database_code               4333882
_audit_block_refno               1524
_audit_block_usercomment         'NG-265-1, red,plate'
_cell_oxdiff_length_a            12.7237(4)
_cell_oxdiff_length_b            13.9205(5)
_cell_oxdiff_length_c            14.7922(4)
_cell_oxdiff_angle_alpha         63.244(3)
_cell_oxdiff_angle_beta          75.697(3)
_cell_oxdiff_angle_gamma         68.328(3)
_cell_oxdiff_volume              2163.78(12)
_cell_oxdiff_measurement_reflns_used 18751
_reflns_odcompleteness_completeness 98.49
_reflns_odcompleteness_theta     66.97
_reflns_odcompleteness_iscentric 1