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_4333885
_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            'C53 H60 N Ni O P2'
_chemical_formula_weight         847.67
_chemical_properties_physical    air-sensitive
_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     dual
_atom_sites_solution_secondary   difmap
_audit_block_code                ga_ng15
_audit_creation_date
;
'Tue Nov 15 13:47:51 2011'
;
_audit_creation_method
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_audit_update_record             'Wed Nov 16 12:06:35 CET 2011'
_cell_angle_alpha                116.303(8)
_cell_angle_beta                 106.596(6)
_cell_angle_gamma                96.028(6)
_cell_formula_units_Z            2
_cell_length_a                   13.3657(8)
_cell_length_b                   14.1839(12)
_cell_length_c                   14.3602(11)
_cell_measurement_reflns_used    23414
_cell_measurement_temperature    120.0(2)
_cell_measurement_theta_max      72.4293
_cell_measurement_theta_min      3.5769
_cell_volume                     2252.3(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SUPERFLIP (Palatinus, 2007-2009)'
_diffrn_ambient_temperature      120.0(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9241
_diffrn_detector_type            'Agilent EOS'
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_details
;
  1 omega  -14.00   72.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   38.0000  120.0000 86

  2 omega  -16.00   26.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       14.0000   77.0000 -123.0000 42

  3 omega   37.00   82.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       14.0000   77.0000 -123.0000 45

  4 omega  -25.00    1.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -30.0000  -78.0000   -8.0000 26

  5 omega  -65.00   10.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000   77.0000  120.0000 75

  6 omega  -38.00  -12.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000  150.0000 26

  7 omega -112.00  -67.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000 -150.0000 45

  8 omega  -50.00   29.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000   38.0000 -120.0000 79

  9 omega  -41.00  -12.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000 -150.0000 29

 10 omega -111.00  -86.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000  150.0000 25

 11 omega  -69.00  -42.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000  150.0000 27

 12 omega   14.00   39.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   80.0000  -92.0000 25

 13 omega   14.00   39.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   80.0000   67.0000 25

 14 omega   19.00   44.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   79.0000  -66.0000 25

 15 omega   18.00   43.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   80.0000    7.0000 25

 16 omega   19.00   44.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   79.0000   87.0000 25

 17 omega   20.00   47.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   79.0000  158.0000 27

 18 omega   18.00   44.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   80.0000 -135.0000 26

 19 omega   19.00   44.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   78.0000  -16.0000 25

 20 omega   75.00  122.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   76.0000   87.0000 47

 21 omega   89.00  124.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   75.0000 -161.0000 35

 22 omega   24.00   86.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  120.0000 62

 23 omega   24.00  121.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  -53.0000 97

 24 omega   25.00   52.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   76.0000   87.0000 27

 25 omega   25.00   51.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   75.0000 -161.0000 26

 26 omega   23.00   48.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   78.0000   44.0000 25

 27 omega   99.00  124.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  120.0000 25

 28 omega   -9.00   75.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       55.1171  -77.0000    0.0000 84

 29 omega   30.00   87.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   75.0000  103.0000 57

 30 omega   95.00  126.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   75.0000 -131.0000 31

 31 omega   96.00  127.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   75.0000  103.0000 31

 32 omega   29.00   57.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   75.0000 -131.0000 28

 33 omega   34.00  127.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   73.0000   33.0000 93

 34 omega   75.00  102.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   75.0000   -7.0000 27

 35 omega   94.00  127.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   70.0000 -113.0000 33

 36 omega   43.00   90.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   70.0000 -113.0000 47

 37 omega   30.00   66.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   75.0000   -7.0000 36

 38 omega    2.00   79.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000  -80.0000  -99.0000 77

 39 omega   44.00   94.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000  -79.0000  117.0000 50

 40 omega   74.00  136.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -79.0000  154.0000 62

 41 omega   80.00  107.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000  -60.0000 27

 42 omega   39.00  100.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -80.0000  -42.0000 61

 43 omega   39.00  141.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -80.0000   13.0000 102

 44 omega  125.00  177.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   63.0000   30.0000 52

 45 omega   88.00  118.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   63.0000   30.0000 30

 46 omega   48.00  138.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -79.0000   64.0000 90

 47 omega   85.00  111.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000   90.0000 26

 48 omega   88.00  170.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   63.0000  150.0000 82

 49 omega   85.00  112.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000 -150.0000 27

 50 omega   80.00  178.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000  -30.0000 98

 51 omega  137.00  176.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000  -90.0000 39

 52 omega   80.00  106.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000  -90.0000 26

 53 omega   88.00  175.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   63.0000  -60.0000 87

 54 omega   88.00  178.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   63.0000 -150.0000 90

 55 omega   80.00  106.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000  150.0000 26

 56 omega  121.00  177.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000    0.0000 56

 57 omega   80.00  107.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000    0.0000 27

 58 omega   85.00  111.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000   30.0000 26

 59 omega   80.00  106.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000  120.0000 26

 60 omega   81.00  106.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000 -120.0000 25

 61 omega   88.00  116.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   63.0000  -30.0000 28

 62 omega   80.00  107.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000   30.0000 27

 63 omega  115.00  177.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000   60.0000 62

 64 omega   91.00  118.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   50.0000   90.0000 27

 65 omega   80.00  106.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000   60.0000 26

 66 omega   89.00  114.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   50.0000 -180.0000 25

 67 omega   81.00  106.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000 -150.0000 25

 68 omega   85.00  148.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000  -60.0000 63

 69 omega   88.00  117.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   50.0000  150.0000 29

 70 omega   80.00  178.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000 -180.0000 98

 71 omega   94.00  156.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   50.0000   60.0000 62

 72 omega   88.00  172.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   63.0000   90.0000 84

 73 omega   80.00  106.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000   90.0000 26

 74 omega   88.00  114.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   63.0000  -90.0000 26

 75 omega   93.00  120.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   50.0000   30.0000 27

 76 omega   88.00  177.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   63.0000 -120.0000 89

 77 omega   89.00  114.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   50.0000 -150.0000 25

 78 omega   88.00  178.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   63.0000  120.0000 90

 79 omega   72.00  142.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -80.0000 -134.0000 70

 80 omega  -26.00   72.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   38.0000  -30.0000 98

 81 phi    120.00  240.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
 -40.0000    0.0000    0.0000     -     120

 82 omega  -30.00   70.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   77.0000    0.0000 100

 83 omega  -28.00    1.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -30.0000  -78.0000   -8.0000 29

 84 omega  -51.00   30.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000   25.0000   60.0000 81

 85 omega   14.00   46.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   80.0000  164.0000 32

 86 omega   14.00   46.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   80.0000   67.0000 32

 87 omega   15.00   49.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   78.0000 -108.0000 34

 88 omega   14.00   46.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   80.0000  108.0000 32

 89 omega   14.00   46.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   80.0000  -43.0000 32

 90 omega   19.00   49.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   78.0000  -16.0000 30

 91 omega   19.00   47.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   79.0000   87.0000 28

 92 omega   19.00   47.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   79.0000  158.0000 28

 93 omega   18.00   46.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   80.0000 -135.0000 28

 94 omega   18.00   46.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   80.0000  135.0000 28

 95 omega   25.00  124.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   76.0000   87.0000 99

 96 omega   24.00  124.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  120.0000 100

 97 omega   24.00  124.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  -53.0000 100

 98 omega   23.00   49.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   78.0000   44.0000 26

 99 omega   25.00  124.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   75.0000 -161.0000 99

100 omega  -15.00   85.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       55.1171  -77.0000 -150.0000 100

101 omega   30.00  128.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       55.1171   38.0000   60.0000 98

102 omega  -15.00   85.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       55.1171  -77.0000  -30.0000 100

103 omega   29.00  128.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   75.0000  103.0000 99

104 omega   30.00  127.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   73.0000   33.0000 97

105 omega   32.00  127.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   70.0000 -113.0000 95

106 omega   29.00  128.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   75.0000   -7.0000 99

107 omega   -1.00  102.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000  -80.0000  -99.0000 103

108 omega    7.00  109.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000  -79.0000  117.0000 102

109 omega   11.00  114.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000  -80.0000   91.0000 103

110 omega   37.00   94.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -25.0000 -120.0000 57

111 omega   85.00  178.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000  -90.0000 93

112 omega   88.00  178.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   50.0000  120.0000 90

113 omega   39.00  142.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -80.0000 -171.0000 103

114 omega   37.00   94.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -25.0000  150.0000 57

115 omega   37.00   94.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -25.0000   90.0000 57

116 omega   37.00   94.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -25.0000  -30.0000 57

117 omega   85.00  110.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000   60.0000 25

118 omega   37.00   94.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -25.0000   30.0000 57

;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Agilent SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w and \p scans'
_diffrn_measurement_specimen_support 'polyimid foil'
_diffrn_orient_matrix_UB_11      0.0101242000
_diffrn_orient_matrix_UB_12      0.0827145000
_diffrn_orient_matrix_UB_13      -0.0411941000
_diffrn_orient_matrix_UB_21      -0.0141380000
_diffrn_orient_matrix_UB_22      -0.0930746000
_diffrn_orient_matrix_UB_23      -0.1159640000
_diffrn_orient_matrix_UB_31      -0.1235581000
_diffrn_orient_matrix_UB_32      -0.0171733000
_diffrn_orient_matrix_UB_33      -0.0386396000
_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  0.0716
_diffrn_reflns_av_sigmaI/netI    0.0914
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            60163
_diffrn_reflns_theta_full        66.97
_diffrn_reflns_theta_max         72.4293
_diffrn_reflns_theta_min         3.5769
_diffrn_source                   'Agilent SuperNova (Cu) x-ray Source'
_exptl_absorpt_coefficient_mu    1.581
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.47332
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.250
_exptl_crystal_description       neddle
_exptl_crystal_F_000             902
_exptl_crystal_size_max          0.2950
_exptl_crystal_size_mid          0.1021
_exptl_crystal_size_min          0.1016
_platon_squeeze_details
;
;
_refine_diff_density_max         0.978
_refine_diff_density_min         -0.768
_refine_diff_density_rms         0.079
_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   1.079
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     461
_refine_ls_number_reflns         8624
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0554
_refine_ls_R_factor_gt           0.0525
_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^)+(0.1028P)^2^+0.8214P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1506
_refine_ls_wR_factor_ref         0.1540
_reflns_number_gt                7836
_reflns_number_total             8624
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302454n_si_002_5.cif
_cod_data_source_block           complex_10
_cod_original_cell_volume        2252.3(3)
_cod_database_code               4333885
_audit_block_refno               1370
_cell_oxdiff_length_a            13.3840(6)
_cell_oxdiff_length_b            14.2036(8)
_cell_oxdiff_length_c            14.3503(7)
_cell_oxdiff_angle_alpha         116.251(5)
_cell_oxdiff_angle_beta          106.504(4)
_cell_oxdiff_angle_gamma         96.243(4)
_cell_oxdiff_volume              2257.02(18)
_cell_oxdiff_measurement_reflns_used 23414
_reflns_odcompleteness_completeness 98.32
_reflns_odcompleteness_theta     66.97
_reflns_odcompleteness_iscentric 1