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

data_4080994
_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            'C39 H53 N5 Ti'
_chemical_formula_weight         639.76
_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_psch14
_audit_creation_date
;
'Fri Nov 16 09:50:46 2012'
;
_audit_creation_method           SHELXL-2012
_audit_update_record             'Wed Feb 20 18:28:27 CET 2013'
_cell_angle_alpha                102.414(2)
_cell_angle_beta                 101.959(2)
_cell_angle_gamma                116.935(3)
_cell_formula_units_Z            2
_cell_length_a                   12.0332(3)
_cell_length_b                   13.2330(3)
_cell_length_c                   13.8121(3)
_cell_measurement_reflns_used    23838
_cell_measurement_temperature    115(1)
_cell_measurement_theta_max      71.8109
_cell_measurement_theta_min      3.4946
_cell_volume                     1793.94(10)
_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 0.986
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_details
;
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omega____ theta____ kappa____ phi______ frames
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  2 omega  -26.00   33.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
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  3 omega  -26.00   24.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
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  4 omega  -66.00   19.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
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  5 omega   31.00   69.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
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  6 omega   19.00   46.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       10.0000   79.0000  158.6611 27

  7 omega  -14.00   15.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
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  8 omega  -25.00    0.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
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  9 omega   10.00   35.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   80.0000   40.1272 25

 10 omega   10.00   35.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   80.0000 -107.3738 25

 11 omega   16.00   41.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   79.0000 -159.0823 25

 12 omega  -38.00  -12.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000   60.0000 26

 13 omega  -51.00  -22.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -64.0000  -30.0000 29

 14 omega  -47.00  -14.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000 -152.4230 33

 15 omega  -40.00   -6.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000   71.0000  -95.0000 34

 16 omega  -40.00  -13.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000 -180.0000 27

 17 omega   15.00   40.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   78.0000   86.4796 25

 18 omega   15.00   40.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   79.0000    8.1056 25

 19 omega   16.00   42.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   79.0000  158.9744 26

 20 omega   19.00   46.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   79.0000  -91.2281 27

 21 omega   18.00   43.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   80.0000  -46.8019 25

 22 omega   19.00   44.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   78.0000   29.3195 25

 23 omega   19.00   44.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   78.0000 -147.2885 25

 24 omega   19.00   44.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   78.0000   53.6351 25

 25 omega   33.00   60.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   74.0000  126.0250 27

 26 omega   24.00   51.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  -59.2631 27

 27 omega   89.00  116.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   76.0000  -26.8687 27

 28 omega   27.00   54.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
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 29 omega   25.00   52.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   76.0000  -26.8687 27

 30 omega  -15.00   83.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       55.1171  -77.0000  150.0000 98

 31 omega   31.00   57.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   73.0000   19.0115 26

 32 omega   28.00   54.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000  104.3963 26

 33 omega   37.00  103.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   76.0000  -90.4598 66

 34 omega   84.00  110.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000  104.3963 26

 35 omega   32.00   57.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   72.0000  179.2477 25

 36 omega   92.00  123.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   72.0000  179.2477 31

 37 omega   36.00   75.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   73.0000 -166.5994 39

 38 omega   30.00   57.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   73.0000   58.4406 27

 39 omega  102.00  127.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   76.0000 -155.8291 25

 40 omega   35.00   69.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   76.0000 -155.8291 34

 41 omega   34.00   61.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   75.0000   76.1698 27

 42 omega   41.00   77.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   49.0000  -14.1301 36

 43 omega   33.00   60.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   76.0000  -26.3437 27

 44 omega   32.00   73.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   77.0000 -105.9504 41

 45 omega   36.00   62.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   77.0000 -140.6063 26

 46 omega   41.00   68.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   69.0000  104.5272 27

 47 omega   39.00   65.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   74.0000   48.3455 26

 48 omega  100.00  127.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   77.0000 -140.6063 27

 49 omega   -5.00   97.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
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 50 omega   53.00  133.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   64.0000   25.6712 80

 51 omega   71.00   97.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   72.0000  134.9081 26

 52 omega   43.00   69.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   72.0000  134.9081 26

 53 omega   60.00  132.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   51.0000 -100.0306 72

 54 omega    0.00  101.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000  -80.0000   44.3038 101

 55 omega   59.00  122.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   60.0000 -166.1702 63

 56 omega   52.00   78.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   51.0000 -172.5205 26

 57 omega   47.00   73.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   72.0000  -45.1162 26

 58 omega   59.00   86.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   60.0000   -0.1728 27

 59 omega   58.00  102.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   55.0000  134.9747 44

 60 omega   61.00   92.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   60.0000 -174.3476 31

 61 omega   54.00  119.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   67.0000   93.1003 65

 62 omega   52.00   94.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   71.0000 -147.0215 42

 63 omega   54.00  123.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   40.0000  -67.2938 69

 64 omega   48.00   85.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   77.0000   48.1231 37

 65 omega   53.00  134.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   76.0000   -7.9651 81

 66 omega   62.00   94.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   60.0000  177.7279 32

 67 omega   58.00  148.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   68.0000  130.3115 90

 68 omega   61.00   95.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   38.0000 -179.0514 34

 69 omega   57.00   84.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   75.0000  -33.4693 27

 70 omega   70.00  101.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   54.0000  -41.4678 31

 71 omega   73.00  134.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       98.0000   69.0000  104.3064 61

 72 omega   76.00  108.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       98.0000   64.0000   33.6743 32

 73 omega   81.00  106.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000  -17.5836 25

 74 omega   67.00   94.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -80.0000  -63.1374 27

 75 omega   79.00  107.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -80.0000  102.9670 28

 76 omega   88.00  157.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000  -30.0000 69

 77 omega   90.00  117.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   50.0000  120.0000 27

 78 omega   51.00  105.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -80.0000  -46.3043 54

 79 omega   89.00  114.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   64.0000  -60.0000 25

 80 omega   46.00   99.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -80.0000 -158.8602 53

 81 omega   87.00  118.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   71.0000   84.0000 31

 82 omega   88.00  163.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   64.0000  150.0000 75

 83 omega   88.00  177.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   64.0000  120.0000 89

 84 omega   88.00  178.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   64.0000  -30.0000 90

 85 omega   88.00  177.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   64.0000 -180.0000 89

 86 omega   86.00  161.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   71.0000   46.0000 75

 87 omega   86.00  119.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000  -60.0000 33

 88 omega   41.00  130.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -79.0000    9.5214 89

 89 omega   89.00  177.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   64.0000 -150.0000 88

 90 omega   68.00  100.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -80.0000  145.7334 32

 91 omega   86.00  128.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000  -90.0000 42

 92 omega   80.00  177.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000    0.0000 97

 93 omega   88.00  178.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   64.0000   60.0000 90

 94 omega   80.00  107.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000  -30.0000 27

 95 omega   43.00  141.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -79.0000   54.8939 98

 96 omega   80.00  106.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000 -180.0000 26

 97 omega   85.00  160.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000  120.0000 75

 98 omega   81.00  106.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000   30.0000 25

 99 omega   81.00  108.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000 -150.0000 27

100 omega  123.00  176.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000 -120.0000 53

101 omega   80.00  110.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000 -120.0000 30

102 omega   80.00  106.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000  150.0000 26

103 omega  153.00  178.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   64.0000   30.0000 25

104 omega   91.00  136.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   64.0000   30.0000 45

105 omega  112.00  176.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000  -90.0000 64

106 omega  152.00  178.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   71.0000   84.0000 26

107 omega   81.00  107.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000  -90.0000 26

108 omega   40.00  140.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -80.0000  -95.3192 100

109 omega   90.00  116.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   64.0000    0.0000 26

110 omega   97.00  122.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   50.0000 -150.0000 25

111 omega   81.00  106.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000  120.0000 25

112 omega   86.00  119.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000 -150.0000 33

113 omega  135.00  164.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000  -60.0000 29

114 omega   82.00  109.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000  -60.0000 27

115 omega   80.00  107.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000   60.0000 27

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

117 omega  -70.00   30.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -77.0000  -90.0000 100

118 omega  -72.00   26.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
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119 omega  -21.00   69.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000 -120.0000 90

120 omega  -44.00   73.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   19.0000  150.0000 117

121 omega  -12.00   88.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0000   77.0000  -11.0714 100

122 omega   15.00   49.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
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123 omega   15.00   47.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
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124 omega   19.00   47.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
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125 omega   19.00   49.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
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126 omega   19.00   47.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   79.0000  -12.0941 28

127 omega   19.00   49.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   78.0000 -147.2885 30

128 omega   19.00   49.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   78.0000   29.3195 30

129 omega   29.00  124.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   75.0000    5.4516 95

130 omega   29.00  128.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   76.0000  -90.4598 99

131 omega   33.00  132.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   76.0000 -155.8291 99

132 omega   -9.00   94.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000  -80.0000  -61.6907 103

133 omega   -1.00  102.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000  -80.0000   82.9128 103

134 omega   43.00  139.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   72.0000  134.9081 96

135 omega   47.00  137.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   64.0000   25.6712 90

136 omega   47.00  143.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   72.0000  -45.1162 96

137 omega   54.00  146.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   67.0000   93.1003 92

138 omega   51.00  147.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   71.0000 -147.0215 96

139 omega   53.00  150.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   40.0000  -67.2938 97

140 omega   48.00  148.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   77.0000   48.1231 100

141 omega   61.00  150.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   60.0000  177.7279 89

142 omega   53.00  152.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   76.0000   -7.9651 99

143 omega   58.00  150.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   68.0000  130.3115 92

;
_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      0.0542787000
_diffrn_orient_matrix_UB_12      0.1183419000
_diffrn_orient_matrix_UB_13      0.0922605000
_diffrn_orient_matrix_UB_21      0.1237132000
_diffrn_orient_matrix_UB_22      0.0619665000
_diffrn_orient_matrix_UB_23      -0.0306928000
_diffrn_orient_matrix_UB_31      -0.0724323000
_diffrn_orient_matrix_UB_32      0.0406442000
_diffrn_orient_matrix_UB_33      -0.0735387000
_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  0.0418
_diffrn_reflns_av_unetI/netI     0.0203
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            55551
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.956
_diffrn_reflns_theta_min         3.498
_diffrn_source                   'microfocus X-Ray tube'
_diffrn_source_type              'Agilent SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.264
_exptl_absorpt_correction_T_max  0.822
_exptl_absorpt_correction_T_min  0.750
_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            green
_exptl_crystal_density_diffrn    1.184
_exptl_crystal_description       plate
_exptl_crystal_F_000             688
_exptl_crystal_size_max          0.2179
_exptl_crystal_size_mid          0.1330
_exptl_crystal_size_min          0.1077
_refine_diff_density_max         0.276
_refine_diff_density_min         -0.294
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     556
_refine_ls_number_reflns         6862
_refine_ls_number_restraints     101
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0453
_refine_ls_R_factor_gt           0.0430
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0356P)^2^+1.4666P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1059
_refine_ls_wR_factor_ref         0.1073
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6497
_reflns_number_total             6862
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om400323p_si_002.cif
_cod_data_source_block           complex_3a
_cod_original_cell_volume        1793.95(9)
_cod_database_code               4080994
_audit_block_refno               1637
_audit_block_usercomment         'PDLS13_2, plate, green'
_shelx_estimated_absorpt_t_min   0.560
_shelx_estimated_absorpt_t_max   0.673
_shelxl_version_number           2012-6
_shelx_res_checksum              294
_cell_oxdiff_length_a            12.0332(3)
_cell_oxdiff_length_b            13.2330(3)
_cell_oxdiff_length_c            13.8121(3)
_cell_oxdiff_angle_alpha         102.414(2)
_cell_oxdiff_angle_beta          101.959(2)
_cell_oxdiff_angle_gamma         116.935(2)
_cell_oxdiff_volume              1793.95(8)
_cell_oxdiff_measurement_reflns_used 23838
_reflns_odcompleteness_completeness 98.63
_reflns_odcompleteness_theta     66.97
_reflns_odcompleteness_iscentric 1