Coronene-Containing N-Heteroarenes: 13 Rings in a Row.
Endres, Alexander H.; Schaffroth, Manuel; Paulus, Fabian; Reiss, Hilmar; Wadepohl, Hubert; Rominger, Frank; Krämer, Roland; Bunz, Uwe H. F.; Journal of the American Chemical Society 138 (2016) 1792–1795; doi:10.1021/jacs.5b12642

data_4130011
_publ_section_title
;
 Coronene-Containing N-Heteroarenes: 13 Rings in a Row.
;
_journal_issue                   6
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1792
_journal_page_last               1795
_journal_paper_doi               10.1021/jacs.5b12642
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety         'C112 H126 N10 O4 Si4, 7(C4 H8 O2)'
_chemical_formula_sum            'C140 H182 N10 O18 Si4'
_chemical_formula_weight         2405.31
_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_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
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_audit_creation_date
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'Thu Sep 17 16:50:29 2015'
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Olex2 1.2
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_audit_update_record             '01.12.2015 17:58:46 CET UTC+01:00  encif 1.36'
_cell_angle_alpha                79.0943(15)
_cell_angle_beta                 89.6706(14)
_cell_angle_gamma                77.4838(15)
_cell_formula_units_Z            1
_cell_length_a                   8.16795(14)
_cell_length_b                   17.8145(3)
_cell_length_c                   23.4233(4)
_cell_measurement_reflns_used    27385
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      70.7980
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;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
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_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
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'encif (Wadepohl, 2009-15); encifer 1.5 (CCDC, 2014)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SUPERFLIP (Palatinus, 2007-2009)'
_diffrn_ambient_environment      'perfluoro polyether oil / N~2~'
_diffrn_ambient_temperature      120(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9621
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_diffrn_measured_fraction_theta_max 0.975
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;
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omega____ theta____ kappa____ phi______ frames
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  2 omega  -20.00   69.00   1.0000    2.0000
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  3 omega  -71.00   25.00   1.0000    2.0000
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  4 omega  -72.00   41.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
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  5 omega    5.00   47.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
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  6 omega   10.00   37.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
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  7 omega    3.00   28.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
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  8 omega    3.00   28.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
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  9 omega    6.00   31.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
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 10 omega   12.00   40.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   78.0000   52.8593 28

 11 omega   15.00   40.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   78.0000  135.0044 25

 12 omega   15.00   40.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   78.0000   66.2702 25

 13 omega   19.00   44.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
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 14 omega   18.00   43.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
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 15 omega   18.00   43.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
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 16 omega   20.00   46.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
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 17 omega   18.00   43.00   1.0000    8.0000
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 18 omega   18.00   43.00   1.0000    8.0000
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 19 omega   19.00   44.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   79.0000  143.4726 25

 20 omega   98.00  124.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000   60.0000 26

 21 omega   26.00   52.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  -30.0000 26

 22 omega   23.00   48.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   78.0000  -94.8617 25

 23 omega   28.00   61.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000   60.0000 33

 24 omega   25.00   51.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000   30.0000 26

 25 omega   14.00   86.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -80.0000 -167.4394 72

 26 omega   24.00   50.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  120.0000 26

 27 omega   27.00   52.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000   90.0000 25

 28 omega   25.00   51.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000 -180.0000 26

 29 omega   24.00   50.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  150.0000 26

 30 omega   28.00   54.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000  111.8546 26

 31 omega  100.00  126.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   76.0000  -66.7654 26

 32 omega   29.00   55.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   76.0000  -66.7654 26

 33 omega   30.00   55.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   76.0000  177.2524 25

 34 omega   34.00   67.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   74.0000  -84.2797 33

 35 omega   29.00   55.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   75.0000   74.5378 26

 36 omega   28.00   54.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000  -18.1846 26

 37 omega   28.00   54.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000   33.7471 26

 38 omega   31.00   70.00   1.0000    8.0000
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 39 omega   49.00   75.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
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 40 omega   42.00   75.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   64.0000   13.4372 33

 41 omega   37.00   63.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
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 42 omega   -9.00   94.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
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 43 omega   38.00   64.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   68.0000  147.7897 26

 44 omega   44.00   69.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   64.0000 -176.9911 25

 45 omega   34.00  129.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   73.0000 -111.3018 95

 46 omega   39.00   65.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   72.0000  153.1548 26

 47 omega   42.00   68.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   68.0000  -66.4676 26

 48 omega   -5.00   98.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
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 49 omega   38.00   63.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   74.0000   85.9408 25

 50 omega   51.00   80.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   62.0000  161.0798 29

 51 omega   51.00  121.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   58.0000  -44.3380 70

 52 omega   49.00   75.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   68.0000   99.2974 26

 53 omega   41.00   66.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   76.0000   -0.6814 25

 54 omega   48.00   73.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   64.0000  131.6699 25

 55 omega   43.00   75.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   72.0000 -128.0846 32

 56 omega   42.00  125.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   74.0000  -35.9140 83

 57 omega   62.00   90.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   42.0000 -169.4231 28

 58 omega   44.00   70.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   77.0000   20.9702 26

 59 omega   52.00  121.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   74.0000   28.9575 69

 60 omega   46.00   72.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   73.0000   98.9732 26

 61 omega   54.00   79.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   67.0000  -96.6515 25

 62 omega   57.00  105.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
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 63 omega   54.00   80.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
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 64 omega   56.00   82.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000  -80.0000  -35.8504 26

 65 omega   51.00   77.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   76.0000   67.9378 26

 66 omega   50.00   76.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   73.0000 -141.0294 26

 67 omega   57.00  146.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   62.0000 -177.0239 89

 68 omega   48.00   74.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   77.0000 -163.9640 26

 69 omega   56.00  110.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   61.0000  -86.8963 54

 70 omega   54.00  136.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   74.0000   47.1114 82

 71 omega   57.00   83.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   74.0000   10.7921 26

 72 omega   52.00   78.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   77.0000  177.5499 26

 73 omega   53.00  151.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   75.0000   93.4208 98

 74 omega   58.00   84.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   74.0000  -17.0337 26

 75 omega   62.00  154.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   68.0000  -45.1168 92

 76 omega   61.00   89.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   69.0000  124.2372 28

 77 omega   68.00   94.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   60.0000 -165.3857 26

 78 omega   64.00   94.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   44.0000 -101.3003 30

 79 omega   57.00   84.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   76.0000   68.5931 27

 80 omega   67.00   96.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   66.0000   15.8183 29

 81 omega   65.00   91.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   75.0000  -15.6907 26

 82 omega   67.00  148.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   66.0000 -166.0854 81

 83 omega   63.00  102.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   71.0000   26.7443 39

 84 omega   61.00   87.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   75.0000 -104.4732 26

 85 omega   53.00   79.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       94.0000  -80.0000  171.3581 26

 86 omega   72.00   98.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       94.0000   50.0000  145.4590 26

 87 omega   70.00  104.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       94.0000   68.0000   81.6716 34

 88 omega   66.00   92.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       94.0000   73.0000  -40.3582 26

 89 omega   73.00  128.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
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 90 omega   69.00   95.00   1.0000   16.0000
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 91 omega   77.00  103.00   1.0000   16.0000
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 92 omega   89.00  123.00   1.0000   16.0000
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 94 omega   85.00  146.00   1.0000   16.0000
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 95 omega  138.00  178.00   1.0000   16.0000
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    -      108.0000   77.0000 -120.0000 40

 96 omega   79.00  105.00   1.0000   16.0000
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    -      108.0000   77.0000 -120.0000 26

 97 omega   85.00  174.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
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 98 omega   56.00   98.00   1.0000   16.0000
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    -      108.0000  -80.0000 -161.0528 42

 99 omega   53.00  121.00   1.0000   16.0000
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    -      108.0000  -80.0000  151.7684 68

100 omega  142.00  173.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000   60.0000 31

101 omega   65.00  140.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000 -120.7819 75

102 omega   85.00  138.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000   60.0000 53

103 omega   78.00  104.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  150.0000 26

104 omega  120.00  177.00   1.0000   16.0000
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    -      108.0000   77.0000   30.0000 57

105 omega   78.00  104.00   1.0000   16.0000
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    -      108.0000   77.0000   30.0000 26

106 omega   81.00  175.00   1.0000   16.0000
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107 omega   78.00  176.00   1.0000   16.0000
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    -      108.0000   77.0000  -90.0000 98

108 omega   78.00  104.00   1.0000   16.0000
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    -      108.0000   77.0000   90.0000 26

109 omega  150.00  176.00   1.0000   16.0000
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    -      108.0000   77.0000   90.0000 26

110 omega   78.00  178.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -30.0000 100

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

112 omega  153.00  178.00   1.0000   16.0000
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113 omega   78.00  103.00   1.0000   16.0000
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    -      108.0000   77.0000   60.0000 25

114 omega  142.00  168.00   1.0000   16.0000
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115 omega   78.00  104.00   1.0000   16.0000
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    -      108.0000   77.0000  120.0000 26

116 omega   85.00  175.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000   90.0000 90

117 omega  132.00  177.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -180.0000 45

118 omega   80.00  106.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000  -39.9336 26

119 omega   80.00  106.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -180.0000 26

120 omega   85.00  157.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000 -120.0000 72

121 omega   85.00  143.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000   30.0000 58

122 omega   82.00  109.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -60.0000 27

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

124 omega   82.00  108.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   73.0000 -100.3688 26

125 omega   80.00  175.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   74.0000  159.8580 95

126 omega   44.00  140.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000   78.0858 96

127 omega   39.00  132.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000  -15.1681 93

128 omega  -26.00   72.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
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129 omega  -72.00   26.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
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130 omega  -26.00   72.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
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131 omega   -8.00   84.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
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132 omega  -13.00   47.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
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133 omega   -3.00   96.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       26.0000   76.0000   12.7575 99

134 omega   -5.00   47.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       26.0000   79.0000  110.6060 52

135 omega  -16.00   84.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -77.0000   30.0000 100

136 omega   42.00  136.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   74.0000  -35.9140 94

137 omega    0.00  100.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000  -77.0000 -151.7296 100

138 omega    7.00  110.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000  -80.0000  -35.8504 103

139 omega   48.00  148.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   77.0000 -163.9640 100

140 omega   57.00  147.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   57.0000   56.5325 90

141 omega   57.00  147.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   54.0000  -97.0997 90

;
_diffrn_measurement_device       'four-circle 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      -0.0691244000
_diffrn_orient_matrix_UB_12      0.0442151000
_diffrn_orient_matrix_UB_13      0.0485850000
_diffrn_orient_matrix_UB_21      0.1135963000
_diffrn_orient_matrix_UB_22      0.0583775000
_diffrn_orient_matrix_UB_23      -0.0185029000
_diffrn_orient_matrix_UB_31      -0.1403399000
_diffrn_orient_matrix_UB_32      0.0527839000
_diffrn_orient_matrix_UB_33      -0.0423030000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0475
_diffrn_reflns_av_unetI/netI     0.0254
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            98708
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.034
_diffrn_reflns_theta_min         3.510
_diffrn_source                   'microfocus X-Ray tube'
_diffrn_source_type              'Agilent SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.974
_exptl_absorpt_correction_T_max  0.955
_exptl_absorpt_correction_T_min  0.896
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.223
_exptl_crystal_description       needle
_exptl_crystal_F_000             1292
_exptl_crystal_size_max          0.208
_exptl_crystal_size_mid          0.092
_exptl_crystal_size_min          0.080
_refine_diff_density_max         1.248
_refine_diff_density_min         -0.750
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     798
_refine_ls_number_reflns         12276
_refine_ls_number_restraints     160
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0824
_refine_ls_R_factor_gt           0.0677
_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^)+(0.0956P)^2^+4.0689P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1802
_refine_ls_wR_factor_ref         0.1929
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9927
_reflns_number_total             12276
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b12642_si_002.cif
_cod_data_source_block           kr_ae5
_cod_database_code               4130011
_audit_block_refno               2530
_audit_block_usercomment         'KR_AE428, needle, red'
_chemical_oxdiff_formula         'C140 H172 N10 O18 Si4'
_chemical_oxdiff_usercomment     'KR_AE428, needle, red'
_shelx_estimated_absorpt_t_max   0.926
_shelx_estimated_absorpt_t_min   0.823
_reflns_odcompleteness_completeness 98.54
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_shelxl_version_number           2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.13 times of:
  {H49A,H49B,H49C} of C49
 At 1.5 times of:
  {H52A,H52B,H52C} of C52, {H56A,H56B,H56C} of C56, {H50A,H50B,H50C} of C50,
  {H34A,H34B,H34C} of C34A, {H47A,H47B,H47C} of C47, {H43A,H43B,H43C} of C43,
  {H35D,H35E,H35F} of C35B, {H40A,H40B,H40C} of C40, {H46A,H46B,H46C} of C46,
  {H53A,H53B,H53C} of C53, {H34D,H34E,H34F} of C34B, {H41A,H41B,H41C} of C41,
  {H55A,H55B,H55C} of C55, {H38A,H38B,H38C} of C38, {H35A,H35B,H35C} of C35A,
  {H44A,H44B,H44C} of C44, {H37A,H37B,H37C} of C37
2. Restrained distances
 C33-C34A \\sim C33-C34B \\sim C33-C35A \\sim C33-C35B
 with sigma of 0.005
 C34A-C35A \\sim C34B-C35B
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 C33, C34A, C34B, C35A, C35B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C36, C37, C38
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C39, C40, C41
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C42, C43, C44
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C45, C46, C47
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C48, C49, C50
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O91, C92, C93, O94, C95, C96
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O81, C82, C83, O84, C85, C86
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O101, C102, C106
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Same fragment restrains
{C42, C43, C44} sigma for 1-2: 0.02, 1-3: 0.04
as
{C45, C46, C47}
{C42, C43, C44} sigma for 1-2: 0.02, 1-3: 0.04
as
{C48, C49, C50}
5. Others
 Sof(H33A)=Sof(C34B)=Sof(H34D)=Sof(H34E)=Sof(H34F)=Sof(C35B)=Sof(H35D)=
 Sof(H35E)=Sof(H35F)=1-FVAR(1)
 Sof(H33)=Sof(C34A)=Sof(H34A)=Sof(H34B)=Sof(H34C)=Sof(C35A)=Sof(H35A)=
 Sof(H35B)=Sof(H35C)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C33(H33), C33(H33A), C36(H36), C39(H39), C42(H42), C45(H45), C48(H48),
 C51(H51), C54(H54)
6.b Secondary CH2 refined with riding coordinates:
 C92(H92A,H92B), C93(H93A,H93B), C95(H95A,H95B), C96(H96A,H96B), C72(H72A,
 H72B), C73(H73A,H73B), C75(H75A,H75B), C76(H76A,H76B), C82(H82A,H82B),
 C83(H83A,H83B), C85(H85A,H85B), C86(H86A,H86B), C102(H10A,H10B), C106(H10C,
 H10D)
6.c Me refined with riding coordinates:
 C34A(H34A,H34B,H34C), C35A(H35A,H35B,H35C), C34B(H34D,H34E,H34F), C35B(H35D,
 H35E,H35F), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C40(H40A,H40B,H40C),
 C41(H41A,H41B,H41C), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C46(H46A,H46B,
 H46C), C47(H47A,H47B,H47C), C49(H49A,H49B,H49C), C50(H50A,H50B,H50C)
6.d Aromatic/amide H refined with riding coordinates:
 C5(H5), C10(H10), C11(H11), C12(H12), C16(H16), C23(H23), C28(H28)
6.e Idealised Me refined as rotating group:
 C52(H52A,H52B,H52C), C53(H53A,H53B,H53C), C55(H55A,H55B,H55C), C56(H56A,H56B,
 H56C)
;
_shelx_res_checksum              75531
_shelx_hkl_checksum              8757
_olex2_submission_special_instructions 'No special instructions were received'
_cell_oxdiff_length_a            8.16795(14)
_cell_oxdiff_length_b            17.8145(3)
_cell_oxdiff_length_c            23.4233(4)
_cell_oxdiff_angle_alpha         79.0943(15)
_cell_oxdiff_angle_beta          89.6706(14)
_cell_oxdiff_angle_gamma         77.4838(15)
_cell_oxdiff_volume              3264.98(10)
_cell_oxdiff_measurement_reflns_used 27385