Synthesis and transition metal coordination chemistry of a novel hexadentate bispidine ligand.
Comba, Peter; Rudolf, Henning; Wadepohl, Hubert; Dalton transactions (Cambridge, England : 2003) 44 (2015) 2724–2736; doi:10.1039/c4dt03262d

data_7033230
_publ_section_title
;
 Synthesis and transition metal coordination chemistry of a novel
 hexadentate bispidine ligand.
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2724
_journal_page_last               2736
_journal_paper_doi               10.1039/c4dt03262d
_journal_volume                  44
_journal_year                    2015
_chemical_formula_sum            'C33.57 H34.13 B2 Cu F8 N6 O6'
_chemical_formula_weight         854.75
_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   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_block_code                co_hr21
_audit_creation_date
;
'Tue Jun 04 16:23:47 2013'
;
_audit_creation_method           encif
_audit_update_record             'Thu Jun  6 11:55:24 CEST 2013'
_cell_angle_alpha                90
_cell_angle_beta                 102.4417(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.74985(19)
_cell_length_b                   10.42825(8)
_cell_length_c                   17.69608(16)
_cell_measurement_reflns_used    40943
_cell_measurement_temperature    110(1)
_cell_measurement_theta_max      70.7230
_cell_measurement_theta_min      4.7640
_cell_volume                     3739.23(6)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_publication_material
'encif (Wadepohl, 2009-13); encifer 1.4 (CCDC, 2011)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SUPERFLIP (Palatinus, 2007-2009)'
_diffrn_ambient_temperature      110(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9621
_diffrn_detector_type            'Agilent EOS'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
  1 omega   42.00   67.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   77.0000    0.0000 25

  2 omega  -67.00   -1.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000 -120.0000 66

  3 omega  -29.00   18.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   77.0000    0.0000 47

  4 omega   22.00   64.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000 -180.0000 42

  5 omega  -68.00  -24.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000  120.0000 44

  6 omega  -20.00   17.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000  120.0000 37

  7 omega  -16.00   14.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000 -180.0000 30

  8 omega  -24.00   62.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       -3.5000   57.0000  -90.0000 86

  9 omega  -13.00   36.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0000   79.0000   67.4739 49

 10 omega    7.00   32.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       38.0000   79.0000  -58.6791 25

 11 omega    7.00   36.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       38.0000   80.0000  174.5541 29

 12 omega   11.00   36.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   79.0000 -139.2413 25

 13 omega   11.00   40.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   79.0000   81.3484 29

 14 omega   15.00   40.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   79.0000  -72.5386 25

 15 omega   15.00   40.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   78.0000  146.8481 25

 16 omega   15.00   40.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   79.0000   93.3014 25

 17 omega   14.00   39.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   80.0000    5.9825 25

 18 omega   79.00  105.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   77.0000  -31.4005 26

 19 omega   18.00   47.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   77.0000  -31.4005 29

 20 omega   15.00   40.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   78.0000 -161.7342 25

 21 omega   20.00   46.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   77.0000   -5.4129 26

 22 omega   18.00   43.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   80.0000 -150.3325 25

 23 omega   20.00   46.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   77.0000 -111.0801 26

 24 omega   19.00   44.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   78.0000   54.7903 25

 25 omega   19.00   44.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   79.0000   17.1455 25

 26 omega   33.00   84.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -77.0000   60.0000 51

 27 omega   98.00  124.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   76.0000    1.5390 26

 28 omega   29.00   54.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   76.0000 -149.0217 25

 29 omega   83.00  110.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   76.0000 -149.0217 27

 30 omega   30.00   56.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   75.0000  -70.2151 26

 31 omega   34.00   61.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   68.0000  172.9999 27

 32 omega  103.00  128.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   75.0000  120.6129 25

 33 omega   29.00   55.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   76.0000    1.5390 26

 34 omega   29.00   55.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000  130.3306 26

 35 omega   29.00   55.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   76.0000   65.3602 26

 36 omega   31.00   57.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   75.0000  109.6391 26

 37 omega   30.00   56.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000   94.6885 26

 38 omega   31.00   57.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   75.0000  120.6129 26

 39 omega   43.00   69.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   64.0000 -118.0862 26

 40 omega   43.00   70.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   61.0000 -145.1213 27

 41 omega   38.00   66.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   74.0000   21.3042 28

 42 omega   87.00  123.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   77.0000   50.1156 36

 43 omega   44.00   70.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   77.0000   50.1156 26

 44 omega   34.00   60.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   75.0000  -20.6154 26

 45 omega   -9.00   94.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000  -80.0000   11.6701 103

 46 omega   42.00   82.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   68.0000  -39.7633 40

 47 omega   36.00   62.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   77.0000  165.8160 26

 48 omega   38.00   69.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   76.0000 -116.3346 31

 49 omega   36.00   61.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   77.0000    0.1320 25

 50 omega   36.00   62.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   77.0000   42.3959 26

 51 omega   40.00  133.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   70.0000   94.1874 93

 52 omega   38.00   81.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   76.0000  126.5370 43

 53 omega   42.00   67.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   73.0000 -106.0257 25

 54 omega   47.00   79.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   66.0000   41.4072 32

 55 omega   46.00   78.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   67.0000  151.9422 32

 56 omega   50.00   81.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   60.0000 -133.1119 31

 57 omega   48.00  136.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   64.0000  -17.7021 88

 58 omega   46.00   85.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   74.0000 -104.7434 39

 59 omega   56.00   81.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   58.0000 -167.9922 25

 60 omega   56.00   85.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   70.0000   59.8720 29

 61 omega   46.00   85.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   75.0000  -96.2881 39

 62 omega    3.00  104.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000  -79.0000 -136.5691 101

 63 omega   57.00   83.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   65.0000   -9.0113 26

 64 omega   48.00   78.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   77.0000  -71.9036 30

 65 omega   69.00  136.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   56.0000   13.0914 67

 66 omega   52.00  115.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   70.0000  149.4492 63

 67 omega   75.00  101.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000  -80.0000  158.4276 26

 68 omega   52.00   77.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   70.0000 -171.4234 25

 69 omega   56.00   94.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   49.0000 -103.5196 38

 70 omega   57.00  143.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   68.0000  -99.0021 86

 71 omega   58.00   84.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000  -79.0000 -150.7973 26

 72 omega   57.00  112.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   67.0000  -35.2014 55

 73 omega   67.00   93.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000  -80.0000  -70.6220 26

 74 omega   54.00  123.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   74.0000   76.0723 69

 75 omega   59.00   93.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   65.0000   -6.0987 34

 76 omega   53.00   79.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   77.0000  -67.3400 26

 77 omega   11.00   77.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000  -79.0000  138.0169 66

 78 omega   57.00   83.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   75.0000   31.3550 26

 79 omega   57.00   84.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   75.0000  108.5713 27

 80 omega   65.00   98.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   58.0000  -19.3170 33

 81 omega   64.00  132.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   50.0000 -104.0639 68

 82 omega   78.00  129.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   61.0000   40.0189 51

 83 omega   70.00  158.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   56.0000   93.0822 88

 84 omega   61.00   89.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   75.0000  -75.7778 28

 85 omega   68.00  158.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   61.0000  -94.8840 90

 86 omega   61.00   92.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   75.0000  171.6989 31

 87 omega  107.00  140.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   58.0000 -144.8652 33

 88 omega   69.00  102.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   58.0000 -144.8652 33

 89 omega   69.00  104.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       94.0000   41.0000   12.4950 35

 90 omega   73.00   98.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       94.0000   40.0000 -175.0169 25

 91 omega   72.00  101.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       94.0000   62.0000   19.5152 29

 92 omega   81.00  107.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      102.0000   60.0000  105.1742 26

 93 omega   74.00  100.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      102.0000   76.0000  118.9630 26

 94 omega   39.00   65.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000  178.8725 26

 95 omega   85.00  175.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000   30.0000 90

 96 omega   85.00  121.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  -30.0000 36

 97 omega   85.00  111.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000 -180.0000 26

 98 omega   80.00  178.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  150.0000 98

 99 omega   80.00  175.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  120.0000 95

100 omega   85.00  111.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000   90.0000 26

101 omega   87.00  175.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000   60.0000 88

102 omega   78.00  103.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -150.0000 25

103 omega  114.00  178.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -30.0000 64

104 omega   78.00  103.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -30.0000 25

105 omega   78.00  104.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -90.0000 26

106 omega   78.00  104.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   30.0000 26

107 omega   87.00  113.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   60.0000 26

108 omega   78.00  176.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -180.0000 98

109 omega   78.00  104.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -120.0000 26

110 omega  134.00  161.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000    0.0000 27

111 omega   79.00  105.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000    0.0000 26

112 omega   85.00  111.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  150.0000 26

113 omega   85.00  175.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000 -150.0000 90

114 omega  141.00  167.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  -90.0000 26

115 omega   87.00  121.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  -90.0000 34

116 omega   38.00  140.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000  -42.1134 102

117 omega   85.00  175.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  -60.0000 90

118 omega  138.00  164.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   76.0000   89.4477 26

119 omega   79.00  105.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   76.0000   89.4477 26

120 omega   70.00  140.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000    5.6794 70

121 omega   78.00  104.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000   52.9990 26

122 omega   80.00  106.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -60.0000 26

123 omega   45.00  102.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000   77.6850 57

124 omega   37.00  103.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000  132.8233 66

125 omega   78.00  110.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000 -105.7235 32

126 omega   85.00  175.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000 -120.0000 90

127 omega   41.00   67.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000 -105.7235 26

128 omega   81.00  107.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   90.0000 26

129 omega   85.00  158.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000  120.0000 73

130 omega   86.00  155.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000   30.0000 69

131 omega   86.00  156.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000  -60.0000 70

132 omega   85.00  111.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000    0.0000 26

133 omega   40.00   95.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -77.0000 -150.0000 55

134 omega   68.00  140.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000  178.8725 72

;
_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      -0.0759211000
_diffrn_orient_matrix_UB_12      0.0043940000
_diffrn_orient_matrix_UB_13      -0.0216479000
_diffrn_orient_matrix_UB_21      -0.0001831000
_diffrn_orient_matrix_UB_22      -0.1125442000
_diffrn_orient_matrix_UB_23      -0.0564460000
_diffrn_orient_matrix_UB_31      -0.0031748000
_diffrn_orient_matrix_UB_32      -0.0956671000
_diffrn_orient_matrix_UB_33      0.0654979000
_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  0.0403
_diffrn_reflns_av_unetI/netI     0.0150
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            92804
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.813
_diffrn_reflns_theta_min         4.769
_diffrn_source                   'microfocus X-Ray tube'
_diffrn_source_type              'Agilent SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.652
_exptl_absorpt_correction_T_max  0.957
_exptl_absorpt_correction_T_min  0.785
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.518
_exptl_crystal_description       plate
_exptl_crystal_F_000             1746
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.137
_refine_diff_density_min         -1.166
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     528
_refine_ls_number_reflns         7169
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0830
_refine_ls_R_factor_gt           0.0803
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1388P)^2^+12.6248P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2317
_refine_ls_wR_factor_ref         0.2343
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6735
_reflns_number_total             7169
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt03262d2.cif
_cod_data_source_block           co_hr21
_cod_depositor_comments
'Adding full bibliography for 7033230--7033235.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7033230
_audit_block_refno               1769
_audit_block_usercomment         'HR209, plate, blue'
_shelx_estimated_absorpt_t_min   0.852
_shelx_estimated_absorpt_t_max   0.852
_shelxl_version_number           2013-3
_shelx_res_checksum              65400
_cell_oxdiff_length_a            20.7523(4)
_cell_oxdiff_length_b            10.42497(16)
_cell_oxdiff_length_c            17.6917(3)
_cell_oxdiff_angle_alpha         89.9729(12)
_cell_oxdiff_angle_beta          102.3259(14)
_cell_oxdiff_angle_gamma         89.9580(14)
_cell_oxdiff_volume              3739.23(11)
_cell_oxdiff_measurement_reflns_used 40945
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_theta     66.97
_reflns_odcompleteness_iscentric 1