Counter-ligand control of the electronic structure in dinuclear copper-tetrakisguanidine complexes.
Ziesak, Alexandra; Wesp, Tobias; Hübner, Olaf; Kaifer, Elisabeth; Wadepohl, Hubert; Himmel, Hans-Jörg; Dalton transactions (Cambridge, England : 2003) 44 (2015) 19111–19125; doi:10.1039/c5dt03270a

data_7037110
_publ_section_title
;
 Counter-ligand control of the electronic structure in dinuclear
 copper-tetrakisguanidine complexes.
;
_journal_issue                   44
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              19111
_journal_page_last               19125
_journal_paper_doi               10.1039/c5dt03270a
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C38 H64 Cu2 N12 O8, 4(C2 H3 N)'
_chemical_formula_sum            'C46 H76 Cu2 N16 O8'
_chemical_formula_weight         1108.30
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_block_code                hi_az12
_audit_creation_date
;
'Wed Apr 15 11:39:03 2015'
;
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3151 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-07-20 deposited with the CCDC.
2015-10-09 downloaded from the CCDC.
;
_cell_angle_alpha                85.405(3)
_cell_angle_beta                 78.567(3)
_cell_angle_gamma                63.473(3)
_cell_formula_units_Z            2
_cell_length_a                   12.3650(4)
_cell_length_b                   12.5243(5)
_cell_length_c                   20.2731(6)
_cell_measurement_reflns_used    26388
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      70.6050
_cell_measurement_theta_min      4.0140
_cell_volume                     2753.17(18)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material
'encif (Wadepohl, 2009-14); encifer 1.5 (CCDC, 2014)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_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
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_details
;
  1 omega   -8.00   19.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000  120.0000 27

  2 omega  -37.00   73.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   19.0000  -60.0000 110

  3 omega  -65.00  -17.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000  120.0000 48

  4 omega  -13.00   68.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       10.0000   71.0000   90.4468 81

  5 omega  -50.00   42.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       14.0000  -75.0000  -56.3832 92

  6 omega   -6.00   42.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       14.0000   79.0000 -106.7781 48

  7 omega    3.00   28.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       34.0000   79.0000 -110.1131 25

  8 omega    6.00   31.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       38.0000   80.0000  -87.3739 25

  9 omega   10.00   40.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   80.0000  -13.4418 30

 10 omega   11.00   36.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   78.0000   57.3528 25

 11 omega   10.00   35.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   80.0000  153.2762 25

 12 omega   10.00   35.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   80.0000  116.4630 25

 13 omega   15.00   40.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   78.0000  168.6758 25

 14 omega   15.00   40.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   79.0000   29.8311 25

 15 omega   15.00   40.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   78.0000   69.2885 25

 16 omega   14.00   39.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   80.0000  -74.2967 25

 17 omega   19.00   44.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   78.0000 -163.8144 25

 18 omega   19.00   44.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   79.0000 -138.1272 25

 19 omega   19.00   44.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   79.0000   -7.4846 25

 20 omega   24.00   51.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  -30.0000 27

 21 omega   25.00   52.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  150.0000 27

 22 omega   25.00   52.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   75.0000  142.8992 27

 23 omega   27.00   54.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000 -150.0000 27

 24 omega  -17.00   85.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -80.0000   68.6488 102

 25 omega   25.00   52.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  120.0000 27

 26 omega   23.00   48.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   78.0000 -102.5566 25

 27 omega   26.00   53.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000   90.0000 27

 28 omega   26.00   53.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000   60.0000 27

 29 omega   26.00   51.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   75.0000  116.2096 25

 30 omega   28.00   55.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000    0.0000 27

 31 omega  -16.00   84.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -77.0000 -150.0000 100

 32 omega   32.00   59.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  -90.0000 27

 33 omega   26.00   51.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   76.0000   74.9624 25

 34 omega   25.00   52.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  -60.0000 27

 35 omega   31.00   74.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   74.0000  -16.8160 43

 36 omega   31.00   56.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   74.0000  157.5927 25

 37 omega   29.00   55.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   76.0000   39.6624 26

 38 omega   32.00   59.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   76.0000 -175.4152 27

 39 omega  -12.00   72.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000  -80.0000  147.0972 84

 40 omega   35.00   62.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000  -52.9777 27

 41 omega   35.00   62.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   71.0000   75.4356 27

 42 omega   40.00   67.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   74.0000  -96.9302 27

 43 omega   29.00   54.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000 -120.6436 25

 44 omega   36.00   61.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   71.0000  -62.5651 25

 45 omega    9.00   82.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000  -79.0000  -42.7898 73

 46 omega   36.00   63.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   75.0000  169.4725 27

 47 omega   35.00   61.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   73.0000 -145.4414 26

 48 omega   34.00   59.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   76.0000  -24.1646 25

 49 omega   41.00   68.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   64.0000  -86.0367 27

 50 omega   43.00   68.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   64.0000   61.8586 25

 51 omega   46.00   73.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   65.0000  104.6077 27

 52 omega   43.00   68.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   67.0000  -63.2980 25

 53 omega   38.00   65.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   74.0000   74.8605 27

 54 omega   59.00   86.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   49.0000  -80.5202 27

 55 omega   58.00   83.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000  -80.0000 -102.5694 25

 56 omega  103.00  133.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   66.0000 -121.1015 30

 57 omega   46.00   73.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   66.0000 -121.1015 27

 58 omega   37.00   64.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   76.0000  118.9133 27

 59 omega   36.00   62.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   77.0000   10.3735 26

 60 omega   37.00   62.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   77.0000  145.2330 25

 61 omega   48.00   97.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   64.0000 -127.5289 49

 62 omega   45.00   71.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   72.0000   31.9328 26

 63 omega   49.00   79.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   61.0000   80.3515 30

 64 omega   45.00   71.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   71.0000  -70.9242 26

 65 omega   48.00   75.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   74.0000  151.8414 27

 66 omega   43.00   89.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   75.0000  -57.2078 46

 67 omega   53.00   78.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   68.0000   95.2710 25

 68 omega   48.00  108.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   73.0000  163.6336 60

 69 omega   53.00  112.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   51.0000   -1.4443 59

 70 omega   51.00  100.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   64.0000  130.5663 49

 71 omega   53.00   79.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   62.0000   38.1969 26

 72 omega   52.00   79.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   71.0000   67.0622 27

 73 omega   48.00   74.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   77.0000  -10.2780 26

 74 omega   55.00  149.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   42.0000  -57.2975 94

 75 omega   60.00   88.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   61.0000  153.2456 28

 76 omega   55.00  117.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   72.0000 -176.7349 62

 77 omega   95.00  126.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   74.0000   74.3815 31

 78 omega   55.00   90.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   74.0000   74.3815 35

 79 omega   63.00   88.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000  -80.0000 -140.0754 25

 80 omega   57.00   87.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   76.0000  -75.7343 30

 81 omega   55.00   82.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000  -80.0000  146.3827 27

 82 omega   65.00   93.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   55.0000   23.9426 28

 83 omega   62.00   92.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   68.0000  106.1133 30

 84 omega   60.00  155.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   71.0000   81.5281 95

 85 omega   63.00   90.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   77.0000 -138.4419 27

 86 omega   68.00  111.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   64.0000  142.8403 43

 87 omega   62.00   92.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   73.0000   73.1092 30

 88 omega   67.00  112.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   66.0000  -12.6719 45

 89 omega   62.00   99.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   74.0000  117.7472 37

 90 omega   78.00  103.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   51.0000  -38.3688 25

 91 omega   64.00   97.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   70.0000   21.5637 33

 92 omega   62.00   93.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   73.0000 -149.3997 31

 93 omega   63.00  147.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   71.0000   38.9755 84

 94 omega   73.00  100.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       94.0000   49.0000  -52.1947 27

 95 omega   74.00  107.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       94.0000   55.0000 -162.5347 33

 96 omega   68.00  151.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       94.0000   72.0000  148.6443 83

 97 omega   69.00  110.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       98.0000   75.0000 -153.1977 41

 98 omega   69.00   98.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       98.0000   77.0000   96.4146 29

 99 omega   86.00  113.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   63.0000   30.0000 27

100 omega   86.00  113.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   63.0000  -30.0000 27

101 omega  121.00  175.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   63.0000  -60.0000 54

102 omega   86.00  118.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   63.0000  -60.0000 32

103 omega   81.00  129.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   90.0000 48

104 omega   80.00  107.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -180.0000 27

105 omega   78.00  105.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  120.0000 27

106 omega   79.00  177.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -90.0000 98

107 omega  112.00  166.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -120.0000 54

108 omega   79.00  107.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -120.0000 28

109 omega   81.00  137.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000   89.6706 56

110 omega   79.00  104.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -30.0000 25

111 omega  143.00  170.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   60.0000 27

112 omega   79.00  106.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   60.0000 27

113 omega   79.00  167.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   30.0000 88

114 omega  108.00  177.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  150.0000 69

115 omega   79.00  104.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  150.0000 25

116 omega   78.00  178.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -150.0000 100

117 omega   78.00  178.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000    0.0000 100

118 omega  142.00  169.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -60.0000 27

119 omega   78.00  104.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -60.0000 26

120 omega   87.00  176.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   63.0000 -180.0000 89

121 omega   86.00  176.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   63.0000   60.0000 90

122 omega   69.00  123.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000 -122.2753 54

123 omega  125.00  176.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   70.0000  103.2333 51

124 omega   84.00  122.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   70.0000  103.2333 38

125 omega   42.00  123.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000  -40.5377 81

126 omega   85.00  112.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   71.0000  133.3029 27

127 omega   88.00  177.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   54.0000  -24.0144 89

128 omega   76.00  104.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -79.0000  105.1003 28

129 omega   71.00  139.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000   69.6561 68

130 omega   80.00  106.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   74.0000 -127.6946 26

131 omega   37.00  140.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000    1.5913 103

132 omega   37.00   63.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000   69.6561 26

133 omega   37.00   90.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000 -143.9925 53

134 omega   64.00   91.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -79.0000  -57.9241 27

135 omega   37.00   63.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -79.0000  -57.9241 26

136 omega   48.00  139.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -79.0000  150.3644 91

137 omega   83.00  108.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000  -60.0000 25

138 omega   87.00  117.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   63.0000  150.0000 30

139 omega   89.00  175.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   63.0000  120.0000 86

140 omega   48.00  105.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -79.0000  -78.2762 57

141 omega  -72.00   26.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -38.0000  -30.0000 98

142 omega  -44.00   73.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   19.0000   30.0000 117

143 omega  -26.00   72.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   38.0000 -180.0000 98

144 omega  -15.00   84.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       14.0000   76.0000 -162.9406 99

145 omega   -7.00   92.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       22.0000   76.0000  -40.2728 99

146 omega   -6.00   46.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       26.0000   80.0000   97.5411 52

147 omega   -4.00   96.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       26.0000   77.0000  -89.7379 100

148 omega   10.00   46.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   80.0000  116.4630 36

149 omega   15.00   47.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   79.0000   29.8311 32

150 omega   14.00   46.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   80.0000  -74.2967 32

151 omega   19.00   47.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   79.0000   -7.4846 28

152 omega   19.00   49.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   78.0000 -163.8144 30

153 omega   19.00   47.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   79.0000 -138.1272 28

154 omega   24.00  124.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  -60.0000 100

155 omega  -15.00   75.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -57.0000  -60.0000 90

156 omega  -18.00   80.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -38.0000   90.0000 98

157 omega   30.00  128.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   74.0000  -16.8160 98

158 omega   28.00  128.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000 -120.6436 100

159 omega   30.00  128.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   74.0000  157.5927 98

160 omega   33.00  132.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   76.0000  -24.1646 99

161 omega   39.00  129.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   64.0000  -86.0367 90

162 omega   34.00  131.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   73.0000 -145.4414 97

163 omega   -9.00   93.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000  -79.0000  -42.7898 102

164 omega   39.00  129.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   64.0000   61.8586 90

165 omega   35.00  131.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   71.0000  -62.5651 96

166 omega   43.00  134.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   65.0000  104.6077 91

167 omega   36.00  136.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   77.0000  145.2330 100

168 omega   42.00  134.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   67.0000  -63.2980 92

169 omega   -5.00   98.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000  -80.0000 -102.5694 103

170 omega   37.00  136.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   76.0000  118.9133 99

171 omega   47.00  137.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   64.0000 -127.5289 90

172 omega   41.00  140.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   75.0000  -57.2078 99

173 omega   48.00  138.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   61.0000   80.3515 90

174 omega   43.00  139.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   71.0000  -70.9242 96

175 omega   52.00  144.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   51.0000   -1.4443 92

176 omega   52.00  142.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   62.0000   38.1969 90

177 omega   46.00  143.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   73.0000  163.6336 97

178 omega   50.00  142.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   68.0000   95.2710 92

179 omega   51.00  141.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   64.0000  130.5663 90

180 omega   52.00  142.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   63.0000   50.1555 90

181 omega   48.00  148.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   77.0000  -10.2780 100

182 omega   56.00  146.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   61.0000  153.2456 90

183 omega   51.00  147.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   71.0000   67.0622 96

184 omega    7.00  109.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000  -79.0000  160.5231 102

185 omega   54.00  150.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   42.0000  -57.2975 96

186 omega   57.00  147.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   56.0000 -157.1409 90

187 omega   56.00  146.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   62.0000   13.8303 90

188 omega   45.00  151.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   26.0000  -92.5536 106

189 omega   55.00  149.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   48.0000  -50.2314 94

190 omega   55.00  151.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   72.0000 -176.7349 96

191 omega   57.00  156.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   76.0000  -75.7343 99

192 omega   67.00  157.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   64.0000  142.8403 90

193 omega   64.00  159.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   70.0000   21.5637 95

194 omega   67.00  158.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   66.0000  -12.6719 91

195 omega   60.00  160.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   77.0000 -138.4419 100

196 omega   67.00  163.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       94.0000   72.0000  148.6443 96

197 omega   73.00  163.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       94.0000   55.0000 -162.5347 90

198 omega   68.00  168.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       98.0000   77.0000   96.4146 100

199 omega   37.00  140.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000   69.6561 103

200 omega   86.00  176.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   63.0000  120.0000 90

201 omega   78.00  178.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -60.0000 100

202 omega   86.00  176.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   63.0000   90.0000 90

203 omega   86.00  176.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   63.0000  -90.0000 90

204 omega   35.00  178.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -12.0000 -120.0000 143

205 omega   37.00  139.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -79.0000  150.3644 102

206 omega   35.00   93.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000   30.0000 58

207 phi      0.00  120.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
 108.0000  108.0000   20.0000     -     120

208 omega   35.00   93.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000 -120.0000 58

209 omega   35.00   93.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000  120.0000 58

210 omega   37.00  140.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000    1.5913 103

211 omega   35.00   93.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000 -180.0000 58

212 omega   35.00   93.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000  -30.0000 58

213 omega   80.00  118.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   74.0000 -127.6946 38

214 omega   86.00  176.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   63.0000   60.0000 90

215 omega   78.00  178.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -120.0000 100

216 omega   78.00  178.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   30.0000 100

217 omega   78.00  178.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  150.0000 100

218 omega   78.00  178.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000    0.0000 100

219 omega   37.00  139.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -79.0000  -98.6655 102

220 omega   78.00  178.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -30.0000 100

221 omega   78.00  178.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -180.0000 100

;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Agilent SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w and \p scans'
_diffrn_measurement_specimen_support 'polyimid foil'
_diffrn_orient_matrix_UB_11      0.0198751000
_diffrn_orient_matrix_UB_12      -0.0094996000
_diffrn_orient_matrix_UB_13      -0.0771688000
_diffrn_orient_matrix_UB_21      0.1351797000
_diffrn_orient_matrix_UB_22      -0.0904992000
_diffrn_orient_matrix_UB_23      -0.0014196000
_diffrn_orient_matrix_UB_31      -0.0372449000
_diffrn_orient_matrix_UB_32      -0.1030618000
_diffrn_orient_matrix_UB_33      0.0073659000
_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  0.072
_diffrn_reflns_av_unetI/netI     0.0500
_diffrn_reflns_laue_measured_fraction_full 0.992
_diffrn_reflns_laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            156958
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.920
_diffrn_reflns_theta_min         3.945
_diffrn_source                   'microfocus X-Ray tube'
_diffrn_source_type              'Agilent SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.476
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81047
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light blue'
_exptl_crystal_density_diffrn    1.337
_exptl_crystal_description       needle
_exptl_crystal_F_000             1172
_exptl_crystal_size_max          0.225
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.025
_refine_diff_density_max         1.503
_refine_diff_density_min         -0.666
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.973
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     674
_refine_ls_number_reflns         12848
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.973
_refine_ls_R_factor_all          0.0519
_refine_ls_R_factor_gt           0.0410
_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^)+(0.0632P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0966
_refine_ls_wR_factor_ref         0.0992
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10602
_reflns_number_total             12848
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt03270a2.cif
_cod_data_source_block           hi_az12_5
_cod_original_cell_volume        2753.18(17)
_cod_database_code               7037110
_audit_block_refno               2403
_audit_block_usercomment         'hi_az240, needle light blue'
_chemical_oxdiff_formula         'C46 H76 Cu2 N16 O8'
_chemical_oxdiff_usercomment     'hi_az240, needle light blue'
_shelx_estimated_absorpt_t_max   0.866
_shelx_estimated_absorpt_t_min   0.866
_diffrn_oxdiff_twin_integration_method simultaneous
_shelxl_version_number           2014/7
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5853(8) 0.4147(8)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C9(H9), C10(H10)
3.b Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,
 H15C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,
 H20B,H20C), C22(H22A,H22B,H22C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C),
 C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C31(H31A,H31B,
 H31C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C36(H36A,
 H36B,H36C), C38(H38A,H38B,H38C), C52(H52A,H52B,H52C), C62(H62A,H62B,H62C),
 C72(H72A,H72B,H72C), C42(H42A,H42B,H42C)
;
_shelx_res_checksum              36057
_olex2_submission_special_instructions 'No special instructions were received'
_cell_oxdiff_length_a            12.3650(3)
_cell_oxdiff_length_b            12.5243(5)
_cell_oxdiff_length_c            20.2731(6)
_cell_oxdiff_angle_alpha         85.405(3)
_cell_oxdiff_angle_beta          78.567(2)
_cell_oxdiff_angle_gamma         63.473(3)
_cell_oxdiff_volume              2753.18(15)
_cell_oxdiff_measurement_reflns_used 26388
_cell_oxdiff_twin_number         2