Tuning of the Properties of Transition-Metal Bispidine Complexes by Variation of the Basicity of the Aromatic Donor Groups
Peter Comba; Michael Morgen; Hubert Wadepohl; Inorganic Chemistry 52 (2013) 6481–6501; doi:10.1021/ic4004214

data_4335068
_publ_section_title
;
 Tuning of the Properties of Transition-Metal Bispidine Complexes by
 Variation of the Basicity of the Aromatic Donor Groups
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6481
_journal_page_last               6501
_journal_paper_doi               10.1021/ic4004214
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C25 H30 N4 O5'
_chemical_formula_weight         466.53
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_block_code                co_mimo55
_audit_creation_date
;
'Fri Jun 22 13:02:39 2012'
;
_audit_creation_method
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_audit_update_record             'Fri Jun 22 13:13:12 CEST 2012'
_cell_angle_alpha                90.00
_cell_angle_beta                 98.3614(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.13445(7)
_cell_length_b                   20.36668(11)
_cell_length_c                   12.66689(7)
_cell_measurement_reflns_used    48507
_cell_measurement_temperature    110.00(10)
_cell_measurement_theta_max      71.7817
_cell_measurement_theta_min      3.5238
_cell_volume                     2331.48(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SUPERFLIP (Palatinus, 2007-2009)'
_diffrn_ambient_temperature      110.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9621
_diffrn_detector_type            'Agilent EOS'
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_details
;
  1 omega   -6.00   21.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000    0.0000 27

  2 omega  -53.00  -17.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000    0.0000 36

  3 omega  -20.00   17.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000    0.0000 37

  4 omega   40.00   68.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000    0.0000 28

  5 omega  -14.00   38.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       14.0000   76.0000  -36.0000 52

  6 omega   -1.00   25.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       18.0000   80.0000   71.0000 26

  7 omega   11.00   38.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       38.0000   80.0000  -74.0000 27

  8 omega   10.00   37.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   80.0000 -127.0000 27

  9 omega   -6.00   20.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000   63.0000 -120.0000 26

 10 omega  -89.00  -63.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000  -90.0000 26

 11 omega  -50.00  -13.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000  -90.0000 37

 12 omega  -50.00   30.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000   38.0000  -30.0000 80

 13 omega  -48.00   29.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000   25.0000 -150.0000 77

 14 omega  -39.00  -12.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000   90.0000 27

 15 omega  -38.00  -12.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000  120.0000 26

 16 omega  -49.00  -23.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000   63.0000 -120.0000 26

 17 omega  -38.00  -12.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000  -30.0000 26

 18 omega  -61.00  -16.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000 -180.0000 45

 19 omega  -39.00  -12.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000   30.0000 27

 20 omega -107.00  -81.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000 -180.0000 26

 21 omega   18.00   44.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   77.0000   53.0000 26

 22 omega   14.00   39.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   80.0000   81.0000 25

 23 omega   15.00   40.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   80.0000 -163.0000 25

 24 omega   45.00   71.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   77.0000 -147.0000 26

 25 omega   19.00   44.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   78.0000  144.0000 25

 26 omega   19.00   45.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   80.0000  112.0000 26

 27 omega   19.00   44.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   79.0000  165.0000 25

 28 omega   65.00   95.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000   81.0000 30

 29 omega   24.00   49.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000   81.0000 25

 30 omega   23.00   48.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   78.0000  137.0000 25

 31 omega   23.00   48.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   78.0000  114.0000 25

 32 omega   24.00  113.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  -82.0000 89

 33 omega   23.00   48.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   78.0000  -10.0000 25

 34 omega   26.00  124.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  160.0000 98

 35 omega  -16.00   85.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       55.1171  -80.0000  105.0000 101

 36 omega   26.00   54.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       55.1171   77.0000  -90.0000 28

 37 omega   28.00   90.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       55.1171   71.0000  -24.0000 62

 38 omega   28.00   93.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000   98.0000 65

 39 omega   28.00   54.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000 -165.0000 26

 40 omega   41.00  125.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   73.0000 -147.0000 84

 41 omega   30.00  128.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   74.0000   18.0000 98

 42 omega    0.00   78.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000  -80.0000   22.0000 78

 43 omega   57.00   83.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000  -80.0000  -31.0000 26

 44 omega   11.00  110.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000  -79.0000 -150.0000 99

 45 omega   39.00   97.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -80.0000  166.0000 58

 46 omega   80.00  106.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000  -30.0000 26

 47 omega   70.00  141.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -80.0000   51.0000 71

 48 omega   39.00  141.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -80.0000  121.0000 102

 49 omega  125.00  167.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000 -120.0000 42

 50 omega   80.00  106.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000 -120.0000 26

 51 omega  113.00  177.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000  150.0000 64

 52 omega   80.00  106.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000  150.0000 26

 53 omega   40.00  140.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -80.0000  -62.0000 100

 54 omega   90.00  116.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   63.0000  -60.0000 26

 55 omega   88.00  114.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   63.0000 -120.0000 26

 56 omega  150.00  175.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000  120.0000 25

 57 omega   80.00  105.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000    0.0000 25

 58 omega   80.00  106.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000   90.0000 26

 59 omega   80.00  106.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000  120.0000 26

 60 omega  114.00  178.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000   30.0000 64

 61 omega   90.00  115.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   50.0000  150.0000 25

 62 omega   80.00  106.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000  -60.0000 26

 63 omega   80.00  106.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000   30.0000 26

 64 omega   91.00  149.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   50.0000  -90.0000 58

 65 omega   89.00  114.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   63.0000   60.0000 25

 66 omega  117.00  142.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -80.0000 -128.0000 25

 67 omega  125.00  168.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000 -180.0000 43

 68 omega   80.00  106.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000 -180.0000 26

 69 omega   70.00  103.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -80.0000 -128.0000 33

 70 omega  148.00  174.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000  -90.0000 26

 71 omega   91.00  177.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   50.0000  120.0000 86

 72 omega   91.00  160.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   50.0000 -150.0000 69

 73 omega   80.00  106.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000  -90.0000 26

 74 omega  130.00  167.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000   60.0000 37

 75 omega   86.00  112.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000   60.0000 26

 76 omega   80.00  105.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000   60.0000 25

 77 omega   93.00  155.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   50.0000   90.0000 62

 78 omega  111.00  177.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000 -150.0000 66

 79 omega   93.00  178.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   50.0000  -60.0000 85

 80 omega   92.00  119.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   50.0000 -120.0000 27

 81 omega   80.00  106.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000 -150.0000 26

 82 omega   85.00  120.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000  -60.0000 35

 83 omega   94.00  121.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   50.0000 -180.0000 27

 84 omega   86.00  127.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000    0.0000 41

 85 omega   93.00  156.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   50.0000    0.0000 63

 86 omega   89.00  115.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   63.0000  120.0000 26

 87 omega   85.00  114.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000  -30.0000 29

 88 omega   88.00  174.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   63.0000    0.0000 86

 89 omega   85.00  110.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000 -180.0000 25

 90 omega   85.00  116.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000   30.0000 31

 91 omega   85.00  126.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000  120.0000 41

 92 omega   89.00  114.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   63.0000 -180.0000 25

 93 omega   89.00  125.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   63.0000 -150.0000 36

 94 omega   91.00  118.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   63.0000  -30.0000 27

 95 omega   89.00  124.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   63.0000   30.0000 35

 96 omega   89.00  175.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   63.0000  -90.0000 86

 97 omega   89.00  178.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   63.0000   90.0000 89

 98 omega   86.00  111.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000  150.0000 25

 99 omega  151.00  178.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   50.0000  -30.0000 27

100 omega   85.00  112.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000 -120.0000 27

101 omega   89.00  114.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   50.0000  -30.0000 25

102 omega   88.00  116.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   63.0000  150.0000 28

103 omega   85.00  111.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000   90.0000 26

104 omega   81.00  108.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -80.0000 -160.0000 27

105 omega   99.00  125.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   50.0000   30.0000 26

106 omega   90.00  115.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   50.0000   60.0000 25

107 omega   85.00  111.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000  -90.0000 26

108 omega   39.00   64.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -80.0000 -160.0000 25

109 omega   85.00  112.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000 -150.0000 27

110 omega   77.00  105.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -80.0000   -4.0000 28

111 omega  -72.00   26.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -38.0000  120.0000 98

112 omega  -72.00   26.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -38.0000 -180.0000 98

113 omega  -72.00   26.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -38.0000   60.0000 98

114 omega  -15.00   84.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       14.0000   76.0000  -36.0000 99

115 omega -111.00  -21.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -57.0000    0.0000 90

116 omega -113.00  -12.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000  120.0000 101

117 omega -113.00  -12.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000 -120.0000 101

118 omega -116.00   29.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -12.0000  150.0000 145

119 omega  -63.00   26.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000   57.0000    0.0000 89

120 omega   14.00   46.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   80.0000   81.0000 32

121 omega   14.00   46.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   80.0000 -163.0000 32

122 omega   19.00   47.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   79.0000  165.0000 28

123 omega   20.00  120.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   77.0000 -147.0000 100

124 omega   19.00   47.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   79.0000    7.0000 28

125 omega   23.00   49.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   78.0000  -10.0000 26

126 omega   24.00  124.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  133.0000 100

127 omega   24.00  124.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  -82.0000 100

128 omega   24.00  124.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000   81.0000 100

129 omega   23.00   49.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   78.0000  137.0000 26

130 omega   23.00   49.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   78.0000  114.0000 26

131 omega  -18.00  128.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       55.1171    0.0000    0.0000 146

132 omega  -15.00   85.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       55.1171  -77.0000   90.0000 100

133 omega   28.00  124.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       55.1171   72.0000 -110.0000 96

134 omega  -15.00   85.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       55.1171  -77.0000 -180.0000 100

135 omega  -18.00  128.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       55.1171    0.0000  240.0000 146

136 omega   28.00  124.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       55.1171   71.0000  -24.0000 96

137 omega  -18.00  128.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       55.1171    0.0000  240.0000 146

138 omega  -18.00  128.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       55.1171    0.0000  120.0000 146

139 omega  -18.00  128.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       55.1171    0.0000  120.0000 146

140 omega  -18.00  128.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       55.1171    0.0000    0.0000 146

141 omega   30.00  127.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   73.0000 -147.0000 97

142 omega   28.00  128.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000 -165.0000 100

143 omega   28.00  128.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000   98.0000 100

144 omega   30.00  128.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   74.0000   18.0000 98

145 omega   -1.00  102.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000  -80.0000   22.0000 103

146 omega    7.00  110.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000  -80.0000  -31.0000 103

147 omega   37.00   68.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -25.0000 -120.0000 31

148 omega   37.00   94.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -25.0000  150.0000 57

149 omega   37.00   94.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -25.0000    0.0000 57

150 omega   37.00   94.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -25.0000   60.0000 57

;
_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      -0.0108417000
_diffrn_orient_matrix_UB_12      -0.0741855000
_diffrn_orient_matrix_UB_13      -0.0234571000
_diffrn_orient_matrix_UB_21      0.0672854000
_diffrn_orient_matrix_UB_22      -0.0146090000
_diffrn_orient_matrix_UB_23      0.1162799000
_diffrn_orient_matrix_UB_31      -0.1563311000
_diffrn_orient_matrix_UB_32      -0.0011670000
_diffrn_orient_matrix_UB_33      0.0321782000
_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  0.0529
_diffrn_reflns_av_sigmaI/netI    0.0957
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            80837
_diffrn_reflns_theta_full        66.97
_diffrn_reflns_theta_max         71.7817
_diffrn_reflns_theta_min         3.5238
_diffrn_source                   'Agilent SuperNova (Cu) x-ray Source'
_exptl_absorpt_coefficient_mu    0.768
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65950
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.329
_exptl_crystal_description       plate
_exptl_crystal_F_000             992
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.320
_refine_diff_density_min         -0.246
_refine_diff_density_rms         0.042
_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   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     355
_refine_ls_number_reflns         4492
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0366
_refine_ls_R_factor_gt           0.0356
_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^)+(0.0419P)^2^+1.1980P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0891
_refine_ls_wR_factor_ref         0.0898
_reflns_number_gt                4353
_reflns_number_total             4492
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic4004214_si_004_6.cif
_cod_data_source_block           co_mimo55
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4335068
_audit_block_refno               1529
_audit_block_usercomment         'Mimo456b, plate, colourless'
_cell_oxdiff_length_a            9.13041(18)
_cell_oxdiff_length_b            20.3726(3)
_cell_oxdiff_length_c            12.66878(18)
_cell_oxdiff_angle_alpha         90.0218(12)
_cell_oxdiff_angle_beta          98.3606(14)
_cell_oxdiff_angle_gamma         90.0134(14)
_cell_oxdiff_volume              2331.48(7)
_cell_oxdiff_measurement_reflns_used 48507
_reflns_odcompleteness_completeness 98.68
_reflns_odcompleteness_theta     66.97
_reflns_odcompleteness_iscentric 1