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

data_4080996
_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            'C20 H24 N4'
_chemical_formula_weight         320.43
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_block_code                ga_psch10
_audit_creation_date
;
'Wed Sep 12 15:10:01 2012'
;
_audit_creation_method
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_audit_update_record             'Wed Sep 12 15:36:01 CEST 2012'
_cell_angle_alpha                90
_cell_angle_beta                 100.4209(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.04507(12)
_cell_length_b                   7.06049(8)
_cell_length_c                   20.7577(3)
_cell_measurement_reflns_used    19071
_cell_measurement_temperature    115.01(10)
_cell_measurement_theta_max      71.8791
_cell_measurement_theta_min      3.7281
_cell_volume                     1736.20(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_publication_material  'encifer 1.4 (CCDC, 2011)'
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'
_computing_structure_solution    'SUPERFLIP (Palatinus, 2007-2009)'
_diffrn_ambient_temperature      115.01(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 0.978
_diffrn_measurement_details
;
  1 omega  -70.00  -29.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -38.0000   60.0000 41

  2 omega  -19.00   13.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000  -60.0000 32

  3 omega   44.00   69.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000  -60.0000 25

  4 omega  -65.00  -24.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -38.0000  150.0000 41

  5 omega  -24.00   25.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -38.0000   60.0000 49

  6 omega   -7.00   26.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -38.0000  150.0000 33

  7 omega   -6.00   31.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       10.0000   78.0000  113.3067 37

  8 omega   -8.00   21.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0000   78.0000   70.1921 29

  9 omega -107.00   -9.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.0000  -76.0000   19.4585 98

 10 omega    6.00   31.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       38.0000   80.0000   54.6625 25

 11 omega    8.00   38.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       38.0000   80.0000 -153.6275 30

 12 omega   -4.00   30.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000   38.0000   90.0000 34

 13 omega  -45.00  -12.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000 -150.0000 33

 14 omega   15.00   40.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   78.0000   45.7401 25

 15 omega   14.00   39.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   80.0000  -86.2509 25

 16 omega   15.00   40.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   79.0000 -135.0363 25

 17 omega   16.00   44.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   78.0000  171.8512 28

 18 omega   15.00   40.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   79.0000  131.7086 25

 19 omega   18.00   43.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   80.0000  -67.6498 25

 20 omega   18.00   43.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   80.0000   74.7163 25

 21 omega   19.00   44.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   78.0000  -23.3681 25

 22 omega   96.00  121.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   76.0000 -112.3304 25

 23 omega   23.00   49.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   78.0000   87.1252 26

 24 omega   23.00   48.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   78.0000   -7.3715 25

 25 omega   25.00   50.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   76.0000 -112.3304 25

 26 omega   23.00   48.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   78.0000 -144.2658 25

 27 omega   23.00   49.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   78.0000  162.2012 26

 28 omega   23.00   48.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   78.0000   37.8171 25

 29 omega   28.00   54.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       55.1171   77.0000 -180.0000 26

 30 omega  -16.00   86.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       55.1171  -80.0000  -64.7764 102

 31 omega   76.00  127.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   73.0000   29.8090 51

 32 omega   30.00   59.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   73.0000  -60.6576 29

 33 omega   35.00   61.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   73.0000   29.8090 26

 34 omega   30.00   64.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   74.0000 -150.2303 34

 35 omega   34.00   60.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000  -40.3674 26

 36 omega   30.00   56.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   75.0000  132.5982 26

 37 omega  105.00  131.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   72.0000 -107.4648 26

 38 omega   49.00   75.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   72.0000 -107.4648 26

 39 omega   32.00  127.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   77.0000  -60.5766 95

 40 omega   33.00   59.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   77.0000   52.7165 26

 41 omega   86.00  112.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   77.0000   52.7165 26

 42 omega   40.00   66.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   71.0000 -118.1820 26

 43 omega   45.00   71.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   66.0000   30.1260 26

 44 omega   43.00   69.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   67.0000  143.4892 26

 45 omega   42.00   67.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   68.0000 -168.7699 25

 46 omega  113.00  138.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   65.0000   94.4522 25

 47 omega   47.00   95.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   65.0000   94.4522 48

 48 omega   50.00   83.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   60.0000  -26.7153 33

 49 omega   48.00   73.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   51.0000   87.0514 25

 50 omega   50.00   76.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   54.0000  154.9760 26

 51 omega   54.00   93.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   68.0000 -172.4603 39

 52 omega   48.00  136.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   64.0000 -146.9641 88

 53 omega   -1.00   94.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000  -80.0000  156.6783 95

 54 omega   49.00   75.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   60.0000    4.3046 26

 55 omega   46.00   85.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   76.0000   14.8908 39

 56 omega   54.00   91.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   66.0000 -116.4213 37

 57 omega  121.00  147.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   74.0000  -20.4574 26

 58 omega   50.00   83.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   74.0000  -20.4574 33

 59 omega   52.00   97.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   71.0000  147.6345 45

 60 omega   29.00  108.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000  -78.0000  -50.2409 79

 61 omega   58.00   84.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   46.0000  134.6152 26

 62 omega   73.00   98.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000  -79.0000 -112.7357 25

 63 omega  117.00  152.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   68.0000  -31.8876 35

 64 omega   62.00  108.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   68.0000  -31.8876 46

 65 omega   67.00  133.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   63.0000  135.1751 66

 66 omega   66.00  139.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   57.0000  169.1748 73

 67 omega   58.00   92.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   74.0000  -51.9919 34

 68 omega   65.00  119.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000  -79.0000    8.7924 54

 69 omega   70.00   96.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       98.0000   75.0000   86.2182 26

 70 omega   78.00  114.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       98.0000   60.0000   64.5506 36

 71 omega   69.00  138.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       98.0000   76.0000 -109.3261 69

 72 omega   74.00  100.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      102.0000   73.0000   95.6679 26

 73 omega   85.00  149.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000   60.0000 64

 74 omega   87.00  113.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000   30.0000 26

 75 omega   86.00  111.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000    0.0000 25

 76 omega   86.00  111.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000  -90.0000 25

 77 omega   87.00  114.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000 -180.0000 27

 78 omega   98.00  155.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   50.0000    0.0000 57

 79 omega   89.00  115.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   50.0000 -180.0000 26

 80 omega   89.00  177.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   64.0000  -60.0000 88

 81 omega   91.00  118.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   50.0000  -90.0000 27

 82 omega   89.00  114.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   64.0000  -30.0000 25

 83 omega   88.00  115.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   64.0000 -150.0000 27

 84 omega   85.00  112.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000 -150.0000 27

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

 86 omega   88.00  177.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   64.0000   60.0000 89

 87 omega   80.00  107.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000    0.0000 27

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

 89 omega  149.00  175.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   64.0000   30.0000 26

 90 omega   88.00  115.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   64.0000   30.0000 27

 91 omega   80.00  106.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000  -90.0000 26

 92 omega  119.00  177.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000  150.0000 58

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

 94 omega  139.00  177.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000 -120.0000 38

 95 omega   86.00  111.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000 -120.0000 25

 96 omega   82.00  108.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000  -60.0000 26

 97 omega   80.00  106.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000   30.0000 26

 98 omega   88.00  178.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   64.0000    0.0000 90

 99 omega  129.00  155.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   64.0000 -180.0000 26

100 omega   88.00  114.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   64.0000 -180.0000 26

101 omega   81.00  106.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000   60.0000 25

102 omega   81.00  108.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000  120.0000 27

103 omega   80.00  178.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000 -150.0000 98

104 omega  129.00  168.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000  -30.0000 39

105 omega   81.00  107.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000  -30.0000 26

106 omega   93.00  165.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000   90.0000 72

107 omega   88.00  177.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   64.0000  -90.0000 89

108 omega   41.00  141.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -79.0000   96.2065 100

109 omega   86.00  112.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000  -30.0000 26

110 omega   95.00  167.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   50.0000 -150.0000 72

111 omega   74.00  104.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -80.0000   35.7665 30

112 omega   44.00   95.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -80.0000 -114.2996 51

113 omega   65.00  137.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -80.0000 -151.4211 72

114 omega   40.00   67.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -80.0000   35.7665 27

115 omega   80.00  140.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -79.0000  148.1350 60

116 omega   41.00   71.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -79.0000  148.1350 30

117 omega   59.00  108.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -80.0000  -85.1626 49

118 omega   41.00  107.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -79.0000  -12.4659 66

;
_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      -0.1299616000
_diffrn_orient_matrix_UB_12      -0.0040803000
_diffrn_orient_matrix_UB_13      -0.0131236000
_diffrn_orient_matrix_UB_21      -0.0024150000
_diffrn_orient_matrix_UB_22      0.2182074000
_diffrn_orient_matrix_UB_23      -0.0013189000
_diffrn_orient_matrix_UB_31      -0.0009657000
_diffrn_orient_matrix_UB_32      -0.0031330000
_diffrn_orient_matrix_UB_33      -0.0743160000
_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  0.0339
_diffrn_reflns_av_sigmaI/netI    0.0390
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            37772
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.025
_diffrn_reflns_theta_min         3.731
_diffrn_source                   'Agilent SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.577
_exptl_absorpt_correction_T_max  0.961
_exptl_absorpt_correction_T_min  0.908
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
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            yellow
_exptl_crystal_density_diffrn    1.226
_exptl_crystal_description       block
_exptl_crystal_F_000             688
_exptl_crystal_size_max          0.2139
_exptl_crystal_size_mid          0.1244
_exptl_crystal_size_min          0.0732
_refine_diff_density_max         0.180
_refine_diff_density_min         -0.227
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         3333
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0348
_refine_ls_R_factor_gt           0.0323
_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^)+(0.0417P)^2^+0.5119P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0824
_refine_ls_wR_factor_ref         0.0847
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3082
_reflns_number_total             3333
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om400323p_si_002.cif
_cod_data_source_block           tBuNHC(NNfluoren)NHEt
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4080996
_audit_block_refno               1581
_audit_block_usercomment         'PDK103, block, yellow'
_shelx_estimated_absorpt_t_min   0.945
_shelx_estimated_absorpt_t_max   0.945
_diffrn_reflns_sigmai/neti       0.0136
_shelxl_version_number           2012-4
_shelx_res_checksum              56536
_cell_oxdiff_length_a            12.0517(3)
_cell_oxdiff_length_b            7.0581(2)
_cell_oxdiff_length_c            20.7556(6)
_cell_oxdiff_angle_alpha         89.993(2)
_cell_oxdiff_angle_beta          100.456(2)
_cell_oxdiff_angle_gamma         90.014(2)
_cell_oxdiff_volume              1736.20(9)
_cell_oxdiff_measurement_reflns_used 19071
_reflns_odcompleteness_completeness 98.11
_reflns_odcompleteness_theta     66.97
_reflns_odcompleteness_iscentric 1