Titanium-Catalyzed Hydrohydrazination of Carbodiimides
Schweizer, Peter D.; Wadepohl, Hubert; Gade, Lutz H.; Organometallics 32 (2013) 3697–; doi:10.1021/om400323p

data_4080995
_publ_section_title
;
 Titanium-Catalyzed Hydrohydrazination of Carbodiimides
;
_journal_issue                   13
_journal_name_full               Organometallics
_journal_page_first              3697
_journal_paper_doi               10.1021/om400323p
_journal_volume                  32
_journal_year                    2013
_chemical_formula_sum            'C41 H54 N6 Ti'
_chemical_formula_weight         678.80
_chemical_properties_physical    air-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_block_code                ga_psch13
_audit_creation_date
;
'Thu Nov 15 09:39:17 2012'
;
_audit_creation_method           SHELXL-2012
_audit_update_record             'Thu Nov 15 09:49:42 CET 2012'
_cell_angle_alpha                82.3061(11)
_cell_angle_beta                 78.5139(13)
_cell_angle_gamma                82.9484(11)
_cell_formula_units_Z            2
_cell_length_a                   11.63073(17)
_cell_length_b                   12.68153(15)
_cell_length_c                   13.1652(2)
_cell_measurement_reflns_used    55196
_cell_measurement_temperature    115.01(10)
_cell_measurement_theta_max      71.8765
_cell_measurement_theta_min      3.4448
_cell_volume                     1876.53(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_publication_material
'encif (Wadepohl, 2012); encifer 1.4 (CCDC, 2011)'
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'
_computing_structure_solution    'SUPERFLIP (Palatinus, 2007-2009)'
_diffrn_ambient_temperature      115(1)
_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 0.977
_diffrn_measurement_details
;
  1 omega   38.00   65.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   38.0000 -150.0000 27

  2 omega   -5.00   69.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000   90.0000 74

  3 omega  -15.00   30.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   38.0000 -150.0000 45

  4 omega  -20.00   56.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000    0.0000 76

  5 omega   -7.00   25.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -38.0000   90.0000 32

  6 omega   61.00   86.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0000   75.0000 -139.8478 25

  7 omega  -11.00   31.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0000   75.0000 -139.8478 42

  8 omega -107.00  -43.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.0000  -77.0000   79.9168 64

  9 omega  -38.00   -8.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.0000  -77.0000   79.9168 30

 10 omega  -50.00  -12.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000  -30.0000 38

 11 omega  -38.00  -12.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000   30.0000 26

 12 omega  -38.00  -12.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000  -90.0000 26

 13 omega   -6.00   21.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000   38.0000  -90.0000 27

 14 omega   15.00   43.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   78.0000 -124.6396 28

 15 omega   14.00   39.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   80.0000 -166.7245 25

 16 omega   14.00   39.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   80.0000  -54.1945 25

 17 omega   19.00   44.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   79.0000   79.6405 25

 18 omega   19.00   44.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   78.0000  138.0407 25

 19 omega   18.00   43.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   80.0000   91.7078 25

 20 omega   19.00   44.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   78.0000  -46.4053 25

 21 omega   20.00   47.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   77.0000 -102.7660 27

 22 omega   99.00  124.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   76.0000  166.8869 25

 23 omega   85.00  111.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000 -137.9275 26

 24 omega   23.00   48.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   78.0000 -174.8757 25

 25 omega   26.00   52.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000 -137.9275 26

 26 omega   24.00   50.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  -20.2467 26

 27 omega   27.00   53.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   76.0000  166.8869 26

 28 omega   23.00   48.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   78.0000  -49.2394 25

 29 omega   95.00  123.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  -20.2467 28

 30 omega   23.00   48.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   78.0000   27.5364 25

 31 omega  -16.00   87.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       55.1171  -80.0000   13.4208 103

 32 omega   29.00   55.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   76.0000  173.7357 26

 33 omega   65.00   90.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000    0.5590 25

 34 omega   29.00   54.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000    0.5590 25

 35 omega   29.00   54.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000 -111.4751 25

 36 omega   95.00  122.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000   64.8835 27

 37 omega   32.00   58.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000   64.8835 26

 38 omega   30.00   56.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   75.0000   40.4440 26

 39 omega   29.00   55.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   75.0000 -123.2849 26

 40 omega   51.00  103.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   56.0000  171.8962 52

 41 omega   39.00  109.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   68.0000  135.9710 70

 42 omega   82.00  129.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   67.0000  -72.9412 47

 43 omega   38.00   66.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   67.0000   -6.2149 28

 44 omega   40.00   83.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   61.0000  -89.2118 43

 45 omega   34.00   59.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   76.0000 -179.6666 25

 46 omega   39.00   75.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   67.0000  -72.9412 36

 47 omega   42.00   69.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   73.0000   89.7629 27

 48 omega   38.00   64.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   73.0000  -36.0793 26

 49 omega   37.00   63.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   77.0000   76.2639 26

 50 omega   47.00  114.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   53.0000    1.4331 67

 51 omega   40.00   72.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   75.0000   22.9664 32

 52 omega   -4.00   97.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000  -80.0000 -153.0409 101

 53 omega   47.00   73.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   72.0000  -89.5044 26

 54 omega   45.00   71.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   69.0000 -101.3910 26

 55 omega   42.00   75.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   74.0000  -66.3956 33

 56 omega   46.00   98.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   71.0000  109.1221 52

 57 omega   50.00   76.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   67.0000 -158.9106 26

 58 omega   34.00  104.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000  -79.0000   69.8000 70

 59 omega   67.00   93.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   40.0000 -172.5683 26

 60 omega   47.00   72.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   74.0000 -105.2521 25

 61 omega   47.00   74.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   73.0000 -156.3184 27

 62 omega   44.00   73.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   77.0000   37.6419 29

 63 omega   51.00   83.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   66.0000  121.2384 32

 64 omega   51.00   77.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   74.0000   86.4221 26

 65 omega   60.00   88.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000  -80.0000 -106.7421 28

 66 omega   57.00   83.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   58.0000   77.9026 26

 67 omega   51.00  146.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   71.0000  -64.8613 95

 68 omega   62.00  103.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   64.0000   19.4225 41

 69 omega   59.00   84.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   66.0000   37.6763 25

 70 omega   55.00   81.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   69.0000  114.2589 26

 71 omega   54.00  102.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   76.0000  -23.5687 48

 72 omega   62.00   94.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   59.0000 -177.7941 32

 73 omega   60.00  120.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   64.0000  118.9690 60

 74 omega   62.00  118.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   53.0000 -117.7823 56

 75 omega   58.00  129.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   74.0000  121.3783 71

 76 omega   65.00  145.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   58.0000 -103.4530 80

 77 omega   68.00   95.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   64.0000 -164.1866 27

 78 omega  110.00  158.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       94.0000   53.0000   63.3809 48

 79 omega   73.00  105.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       94.0000   53.0000   63.3809 32

 80 omega   69.00  141.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       98.0000   75.0000 -154.8496 72

 81 omega   82.00  137.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      102.0000   57.0000   16.3924 55

 82 omega   77.00  119.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -80.0000   25.6143 42

 83 omega   42.00   69.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -80.0000   25.6143 27

 84 omega   86.00  118.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000  150.0000 32

 85 omega   86.00  118.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000   30.0000 32

 86 omega   71.00  126.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -80.0000  177.4335 55

 87 omega   40.00   68.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -80.0000  177.4335 28

 88 omega   40.00  101.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -77.0000   60.0000 61

 89 omega   71.00   98.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -77.0000  -90.0000 27

 90 omega   86.00  111.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000  120.0000 25

 91 omega  141.00  171.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000 -120.0000 30

 92 omega   81.00  108.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000 -120.0000 27

 93 omega   86.00  111.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000   60.0000 25

 94 omega   88.00  178.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   64.0000  -30.0000 90

 95 omega   88.00  177.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   64.0000  -90.0000 89

 96 omega   84.00  115.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -80.0000 -138.6380 31

 97 omega   81.00  107.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000    0.0000 26

 98 omega   80.00  107.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000 -180.0000 27

 99 omega   51.00  109.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -80.0000  -31.3138 58

100 omega   82.00  108.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   73.0000 -121.0000 26

101 omega   89.00  177.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   64.0000  150.0000 88

102 omega  144.00  171.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000    0.0000 27

103 omega   80.00  175.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000   90.0000 95

104 omega   80.00  106.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000  -60.0000 26

105 omega   80.00  177.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000   60.0000 97

106 omega   84.00  111.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000  150.0000 27

107 omega   80.00  107.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000  -30.0000 27

108 omega   80.00  175.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000   30.0000 95

109 omega   81.00  106.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000  -90.0000 25

110 omega   89.00  116.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   64.0000  120.0000 27

111 omega  119.00  177.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000  120.0000 58

112 omega   80.00  106.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000  120.0000 26

113 omega   80.00  177.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000 -150.0000 97

114 omega   88.00  115.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   64.0000   60.0000 27

115 omega  134.00  175.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   64.0000  -60.0000 41

116 omega   88.00  114.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   64.0000  -60.0000 26

117 omega   85.00  165.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000  -30.0000 80

118 omega   85.00  177.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000    0.0000 92

119 omega   89.00  177.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   64.0000 -180.0000 88

120 omega   87.00  148.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000  -90.0000 61

121 omega   81.00  108.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   76.0000 -112.2246 27

122 omega   40.00  129.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -80.0000  132.9108 89

123 omega  -30.00   70.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   77.0000  -60.0000 100

124 omega  -21.00   69.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000   60.0000 90

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

126 omega  -21.00   69.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000  150.0000 90

127 omega  -21.00   69.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000  120.0000 90

128 omega  -21.00   69.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000  -90.0000 90

129 omega  -17.00   47.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       14.0000   79.0000   37.7591 64

130 omega -108.00   -8.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.0000  -77.0000   79.9168 100

131 omega -115.00   30.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000    0.0000    0.0000 145

132 omega -115.00   30.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000    0.0000  120.0000 145

133 omega -115.00   30.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000    0.0000  120.0000 145

134 omega -115.00   30.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000    0.0000  240.0000 145

135 omega -115.00   30.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000    0.0000    0.0000 145

136 omega -113.00  -12.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000  -90.0000 101

137 omega -113.00  -12.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000   30.0000 101

138 omega   15.00   49.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   78.0000   66.0657 34

139 omega   14.00   46.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   80.0000  -54.1945 32

140 omega   14.00   46.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   80.0000    6.3465 32

141 omega   18.00   46.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   80.0000   91.7078 28

142 omega   19.00   49.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   78.0000  138.0407 30

143 omega   19.00   49.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   78.0000  -46.4053 30

144 omega   25.00  124.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   76.0000  -94.1877 99

145 omega   23.00   49.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   78.0000  -49.2394 26

146 omega  -14.00   83.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       55.1171  -73.0000  -58.0000 97

147 omega  -18.00  128.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       55.1171    0.0000  240.0000 146

148 omega  -18.00  128.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       55.1171    0.0000    0.0000 146

149 omega  -18.00  128.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       55.1171    0.0000    0.0000 146

150 omega  -18.00  128.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       55.1171    0.0000  120.0000 146

151 omega  -18.00  128.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       55.1171    0.0000  240.0000 146

152 omega  -18.00  128.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       55.1171    0.0000  120.0000 146

153 omega   28.00  128.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000    0.5590 100

154 omega   29.00  128.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   75.0000 -123.2849 99

155 omega   33.00  132.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   76.0000 -179.6666 99

156 omega   40.00  130.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   61.0000  -89.2118 90

157 omega   38.00  130.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   68.0000  135.9710 92

158 omega   34.00  131.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   73.0000  -36.0793 97

159 omega   38.00  130.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   67.0000  -72.9412 92

160 omega   37.00  136.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   75.0000   22.9664 99

161 omega   -5.00   98.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000  -80.0000  112.6968 103

162 omega   -5.00   98.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000  -80.0000 -153.0409 103

163 omega   43.00  139.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   72.0000  -89.5044 96

164 omega   49.00  139.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   56.0000  160.5618 90

165 omega   42.00  140.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   74.0000  -66.3956 98

166 omega   46.00  144.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   74.0000 -105.2521 98

167 omega   44.00  144.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   77.0000   37.6419 100

168 omega   46.00  143.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   73.0000 -156.3184 97

169 omega    3.00  105.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000  -79.0000   69.8000 102

170 omega   57.00  147.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   58.0000   77.9026 90

171 omega    7.00  110.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000  -80.0000 -106.7421 103

172 omega   55.00  145.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   64.0000   19.4225 90

173 omega   50.00  148.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   74.0000   86.4221 98

174 omega   55.00  146.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   66.0000   37.6763 91

175 omega   53.00  152.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   76.0000  -23.5687 99

176 omega   62.00  150.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   59.0000 -177.7941 88

177 omega   61.00  152.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   53.0000 -117.7823 91

178 omega   59.00  149.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   64.0000  118.9690 90

179 omega   65.00  155.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   58.0000 -103.4530 90

180 omega   58.00  156.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   74.0000  121.3783 98

181 omega   67.00  157.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   64.0000 -164.1866 90

182 omega   73.00  164.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       94.0000   53.0000   63.3809 91

183 omega   81.00  171.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      102.0000   57.0000   16.3924 90

184 phi      0.00  120.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
  40.0000  110.2342    0.0000     -     120

185 omega   40.00  104.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -50.0000 -150.0000 64

186 omega   40.00  140.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -77.0000  -30.0000 100

187 omega   40.00  104.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -50.0000   90.0000 64

188 omega   37.00   94.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -25.0000  150.0000 57

189 omega   37.00   94.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -25.0000  -30.0000 57

190 omega   37.00   94.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -25.0000 -120.0000 57

191 omega   37.00  178.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342    0.0000  120.0000 141

192 omega   37.00  178.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342    0.0000    0.0000 141

193 omega   37.00  178.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342    0.0000  120.0000 141

194 omega   37.00  178.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342    0.0000    0.0000 141

195 omega   37.00  178.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342    0.0000  240.0000 141

196 omega   37.00  178.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342    0.0000  120.0000 141

197 omega   37.00  178.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342    0.0000    0.0000 141

198 omega   40.00  140.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -77.0000  -90.0000 100

199 omega   85.00  178.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000  150.0000 93

200 omega   85.00  178.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000   30.0000 93

201 omega   88.00  178.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   64.0000   60.0000 90

202 omega   88.00  178.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   64.0000  -30.0000 90

203 omega   88.00  178.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   64.0000  -90.0000 90

204 omega   88.00  178.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   64.0000 -120.0000 90

205 omega   88.00  178.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   64.0000 -180.0000 90

206 omega   39.00  142.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -80.0000  177.4335 103

207 omega   39.00  142.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -80.0000  -31.3138 103

208 omega   80.00  178.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000    0.0000 98

209 omega   82.00  178.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   73.0000 -109.0000 96

210 omega   85.00  178.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000    0.0000 93

211 omega   88.00  178.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   50.0000  120.0000 90

212 omega   88.00  178.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   64.0000  -60.0000 90

213 omega   80.00  178.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000  150.0000 98

214 omega   80.00  178.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000  -60.0000 98

215 omega   39.00  142.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -80.0000   25.6143 103

216 omega   39.00  142.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -80.0000 -138.6380 103

217 omega   80.00  178.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000   60.0000 98

218 omega   80.00  178.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000  -90.0000 98

219 omega   80.00  178.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000   30.0000 98

220 omega   80.00  178.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000  -30.0000 98

221 omega   80.00  178.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000 -150.0000 98

222 omega   80.00  178.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000  120.0000 98

223 omega   38.00   93.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -38.0000   30.0000 55

224 omega   37.00  178.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342    0.0000  240.0000 141

225 omega   88.00  178.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   50.0000 -180.0000 90

226 omega   85.00  178.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000   90.0000 93

227 omega   39.00  142.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -80.0000  132.9108 103

228 omega  -73.00   73.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000    0.0000  240.0000 146

229 omega  -73.00   73.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000    0.0000  120.0000 146

230 omega  -73.00   73.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000    0.0000    0.0000 146

231 phi      0.00  120.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
 -40.0000    0.0000    0.0000     -     120

232 phi      0.00  120.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
   0.0000    0.0000  -20.0000     -     120

233 phi      0.00  120.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
   0.0000    0.0000   20.0000     -     120

234 omega  -11.00   88.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0000   75.0000 -139.8478 99

235 omega -115.00  -45.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000    0.0000    0.0000 70

236 omega -115.00   30.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000    0.0000  240.0000 145

;
_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      -0.0586373000
_diffrn_orient_matrix_UB_12      0.0203808000
_diffrn_orient_matrix_UB_13      -0.0968740000
_diffrn_orient_matrix_UB_21      -0.0173845000
_diffrn_orient_matrix_UB_22      -0.1196710000
_diffrn_orient_matrix_UB_23      0.0097544000
_diffrn_orient_matrix_UB_31      -0.1212814000
_diffrn_orient_matrix_UB_32      0.0209528000
_diffrn_orient_matrix_UB_33      0.0704396000
_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  0.0575
_diffrn_reflns_av_unetI/netI     0.0174
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            137282
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.022
_diffrn_reflns_theta_min         3.448
_diffrn_source                   'microfocus X-Ray tube'
_diffrn_source_type              'Agilent SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.202
_exptl_absorpt_correction_T_max  0.884
_exptl_absorpt_correction_T_min  0.686
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.201
_exptl_crystal_description       plate
_exptl_crystal_F_000             728
_exptl_crystal_size_max          0.2515
_exptl_crystal_size_mid          0.2138
_exptl_crystal_size_min          0.0740
_refine_diff_density_max         0.273
_refine_diff_density_min         -0.329
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     512
_refine_ls_number_reflns         7221
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0331
_refine_ls_R_factor_gt           0.0313
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0444P)^2^+0.7258P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0844
_refine_ls_wR_factor_ref         0.0857
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6879
_reflns_number_total             7221
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om400323p_si_002.cif
_cod_data_source_block           complex_4a
_cod_database_code               4080995
_audit_block_refno               1636
_audit_block_usercomment         'PD406, plate, black'
_shelx_estimated_absorpt_t_min   0.810
_shelx_estimated_absorpt_t_max   0.810
_shelxl_version_number           2012-6
_shelx_res_checksum              77580
_cell_oxdiff_length_a            11.63073(17)
_cell_oxdiff_length_b            12.68152(15)
_cell_oxdiff_length_c            13.1652(2)
_cell_oxdiff_angle_alpha         82.3061(11)
_cell_oxdiff_angle_beta          78.5139(13)
_cell_oxdiff_angle_gamma         82.9484(11)
_cell_oxdiff_volume              1876.53(5)
_cell_oxdiff_measurement_reflns_used 55196
_reflns_odcompleteness_completeness 98.63
_reflns_odcompleteness_theta     66.97
_reflns_odcompleteness_iscentric 1