Zirconium Complexes Supported by an N-Perfluoro-Arylated Diamidopyridyl Ligand: Synthesis of Hydrazinediido Complexes
Solveig A. Scholl; Gudrun T. Plundrich; Hubert Wadepohl; Lutz H. Gade; Inorganic Chemistry 52 (2013) 10158–10166; doi:10.1021/ic401603y

data_4335906
_publ_section_title
;
 Zirconium Complexes Supported by an N-Perfluoro-Arylated Diamidopyridyl
 Ligand: Synthesis of Hydrazinediido Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10158
_journal_page_last               10166
_journal_paper_doi               10.1021/ic401603y
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C37 H33 F8 N7 Zr, 0.5(C7 H8)'
_chemical_formula_sum            'C40.5 H37 F8 N7 Zr'
_chemical_formula_weight         864.99
_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                ga_ss47
_audit_creation_date
;
'Fri Feb 08 11:37:53 2013'
;
_audit_update_record             'Thu Jun 20 15:40:12 CEST 2013'
_cell_angle_alpha                112.625(2)
_cell_angle_beta                 105.1498(18)
_cell_angle_gamma                101.2234(18)
_cell_formula_units_Z            2
_cell_length_a                   11.2275(2)
_cell_length_b                   13.7650(3)
_cell_length_c                   14.1485(3)
_cell_measurement_reflns_used    34503
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      71.7390
_cell_measurement_theta_min      4.3080
_cell_volume                     1838.16(8)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24a (release 19-12-2012 CrysAlis171 .NET)
(compiled Dec 19 2012,11:08:27)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24a (release 19-12-2012 CrysAlis171 .NET)
(compiled Dec 19 2012,11:08:27)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24a (release 19-12-2012 CrysAlis171 .NET)
(compiled Dec 19 2012,11:08:27)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_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(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9621
_diffrn_detector_type            'Agilent EOS'
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_details
;
  1 omega  -65.00  -20.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000  -90.0000 45

  2 omega  -12.00   19.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000  -90.0000 31

  3 omega  -21.00   16.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000  -90.0000 37

  4 omega   18.00   69.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000  -90.0000 51

  5 omega  -17.00   13.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000    0.0000 30

  6 omega  -60.00  -35.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000    0.0000 25

  7 omega   -7.00   22.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       22.0000   77.0000  105.8477 29

  8 omega  -50.00   -8.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.0000  -77.0000  166.5518 42

  9 omega  -39.00  -12.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000   60.0000 27

 10 omega  -48.00  -20.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000  -90.0000 28

 11 omega -109.00  -59.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000    0.0000 50

 12 omega  -48.00  -12.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000  150.0000 36

 13 omega  -50.00   28.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000   77.0000   30.0000 78

 14 omega  -72.00   27.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000   77.0000  120.0000 99

 15 omega  -40.00  -13.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000  -60.0000 27

 16 omega  -39.00  -12.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000    0.0000 27

 17 omega   15.00   40.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   79.0000  -46.0175 25

 18 omega   15.00   40.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   79.0000  -74.4692 25

 19 omega   16.00   43.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   77.0000  113.9336 27

 20 omega   20.00   47.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   77.0000 -140.6715 27

 21 omega   19.00   44.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   79.0000  -31.6728 25

 22 omega   19.00   45.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   79.0000   24.7964 26

 23 omega   26.00   53.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   75.0000   -2.6771 27

 24 omega   27.00   53.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   75.0000  -23.0755 26

 25 omega   23.00   48.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   78.0000 -123.2424 25

 26 omega   99.00  124.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   76.0000   49.7545 25

 27 omega   99.00  124.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   75.0000  -23.0755 25

 28 omega   23.00   48.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   78.0000  -85.4914 25

 29 omega   26.00   55.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   76.0000   49.7545 29

 30 omega   24.00   50.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  145.6308 26

 31 omega  -15.00   84.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       55.1171  -77.0000  -90.0000 99

 32 omega   56.00   85.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       55.1171  -77.0000   60.0000 29

 33 omega   28.00   54.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       55.1171   77.0000 -180.0000 26

 34 omega   36.00   62.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   70.0000 -100.0542 26

 35 omega   29.00   55.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   76.0000  -73.7485 26

 36 omega   29.00   55.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   76.0000   93.6397 26

 37 omega   29.00   56.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   76.0000  -58.7244 27

 38 omega   28.00   54.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000 -167.1957 26

 39 omega   36.00   65.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   71.0000  117.4361 29

 40 omega   32.00   58.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   77.0000   -4.4269 26

 41 omega  105.00  131.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   77.0000   -4.4269 26

 42 omega   44.00   84.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   63.0000  172.6299 40

 43 omega   56.00   83.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   74.0000   -1.6903 27

 44 omega   40.00   69.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   71.0000  -67.4950 29

 45 omega   42.00   69.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   72.0000 -126.7084 27

 46 omega   50.00   76.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   52.0000   53.8654 26

 47 omega   48.00   75.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   64.0000  -80.3188 27

 48 omega   41.00   76.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   76.0000   -9.6428 35

 49 omega   51.00   76.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   58.0000  150.4852 25

 50 omega   46.00   84.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   69.0000 -107.1485 38

 51 omega   49.00   81.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   69.0000   76.6338 32

 52 omega   82.00  117.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   52.0000   53.8654 35

 53 omega   48.00   74.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   71.0000 -153.0248 26

 54 omega   57.00   85.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   64.0000  -81.8224 28

 55 omega   50.00  114.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   74.0000   91.2701 64

 56 omega   53.00  127.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   76.0000 -127.7683 74

 57 omega   59.00   87.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   43.0000 -143.7848 28

 58 omega   59.00  135.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   66.0000  140.5926 76

 59 omega   61.00  101.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   52.0000  171.5440 40

 60 omega   53.00   79.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   76.0000   26.9486 26

 61 omega   12.00  106.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000  -80.0000  131.7417 94

 62 omega   68.00  101.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   57.0000   74.6212 33

 63 omega  121.00  147.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   64.0000  -51.4528 26

 64 omega   63.00   89.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   64.0000  -51.4528 26

 65 omega   57.00  112.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   75.0000   35.8664 55

 66 omega   66.00   98.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   59.0000  -22.6866 32

 67 omega   61.00  130.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   76.0000  113.4447 69

 68 omega   67.00  125.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   44.0000   24.9128 58

 69 omega   67.00   93.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       94.0000   72.0000 -172.6544 26

 70 omega   68.00  106.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       94.0000   70.0000  -97.4180 38

 71 omega   70.00  100.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       98.0000   73.0000 -176.0582 30

 72 omega  114.00  140.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -80.0000   22.3417 26

 73 omega   79.00  107.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -80.0000   22.3417 28

 74 omega   46.00   72.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -80.0000   22.3417 26

 75 omega   65.00   92.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -77.0000  -60.0000 27

 76 omega   80.00  107.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000   90.0000 27

 77 omega   86.00  155.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000   60.0000 69

 78 omega   39.00  142.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -80.0000 -103.3219 103

 79 omega  117.00  142.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -80.0000   60.7129 25

 80 omega   89.00  177.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   64.0000  120.0000 88

 81 omega   88.00  115.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   64.0000   30.0000 27

 82 omega   88.00  118.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   64.0000    0.0000 30

 83 omega   88.00  174.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   64.0000 -120.0000 86

 84 omega   86.00  113.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -77.0000  150.0000 27

 85 omega   47.00   86.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -80.0000   60.7129 39

 86 omega  131.00  157.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000 -120.0000 26

 87 omega   86.00  129.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000 -120.0000 43

 88 omega   89.00  177.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   64.0000  -90.0000 88

 89 omega   81.00  106.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000  150.0000 25

 90 omega   55.00  115.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -80.0000   96.4607 60

 91 omega  112.00  138.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -80.0000 -160.3677 26

 92 omega   88.00  177.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   64.0000   60.0000 89

 93 omega   89.00  177.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   64.0000  -30.0000 88

 94 omega   88.00  177.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   64.0000  -60.0000 89

 95 omega   80.00  107.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000 -150.0000 27

 96 omega   39.00  142.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -80.0000  -19.4917 103

 97 omega  152.00  178.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   64.0000   90.0000 26

 98 omega   89.00  149.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   64.0000   90.0000 60

 99 omega   81.00  108.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000 -120.0000 27

100 omega   82.00  108.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000  -30.0000 26

101 omega   88.00  171.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   64.0000  150.0000 83

102 omega   80.00  106.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000  120.0000 26

103 omega  148.00  174.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000   60.0000 26

104 omega   42.00  104.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -80.0000 -160.3677 62

105 omega   81.00  106.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000   60.0000 25

106 omega   82.00  177.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000 -180.0000 95

107 omega   81.00  108.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000  -60.0000 27

108 omega  135.00  161.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000   30.0000 26

109 omega   80.00  106.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000   30.0000 26

110 omega   86.00  131.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000  -90.0000 45

111 omega  140.00  166.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   64.0000 -150.0000 26

112 omega   88.00  115.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   64.0000 -150.0000 27

113 omega  110.00  177.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000    0.0000 67

114 omega   82.00  108.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000    0.0000 26

115 omega   81.00  108.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000  -90.0000 27

116 omega  -21.00   69.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000  120.0000 90

117 omega  -72.00   26.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -38.0000  150.0000 98

118 omega  -26.00   72.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   38.0000  -30.0000 98

119 omega  -16.00   84.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       14.0000   77.0000  -37.3665 100

120 omega   -8.00   92.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       22.0000   77.0000 -151.0318 100

121 omega -113.00  -12.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000  150.0000 101

122 omega   15.00   47.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   79.0000  -74.4692 32

123 omega   15.00   47.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   79.0000  -46.0175 32

124 omega   19.00   47.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   79.0000  -31.6728 28

125 omega   18.00   46.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   80.0000   53.8720 28

126 omega   19.00   47.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   79.0000   24.7964 28

127 omega   19.00   47.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   79.0000  131.3842 28

128 omega   23.00   49.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   78.0000 -123.2424 26

129 omega   23.00   49.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   78.0000  -85.4914 26

130 omega   25.00  124.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   76.0000   49.7545 99

131 omega  -15.00   85.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       55.1171  -77.0000    0.0000 100

132 omega  -15.00   85.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       55.1171  -77.0000   60.0000 100

133 omega  -15.00   86.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       55.1171  -79.0000 -170.5298 101

134 omega  -15.00   85.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       55.1171  -77.0000  -90.0000 100

135 omega   28.00  128.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000 -167.1957 100

136 omega   32.00  132.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   77.0000   -4.4269 100

137 omega   35.00   60.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   71.0000  117.4361 25

138 omega   44.00  134.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   63.0000  172.6299 90

139 omega   39.00  135.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   71.0000  -67.4950 96

140 omega   41.00  140.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   76.0000   -9.6428 99

141 omega   45.00  138.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   69.0000 -107.1485 93

142 omega   45.00  138.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   69.0000   76.6338 93

143 omega   49.00  140.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   52.0000   53.8654 91

144 omega   51.00  141.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   64.0000  -81.8224 90

145 omega   47.00  143.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   71.0000 -153.0248 96

146 omega   50.00  148.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   74.0000   91.2701 98

147 omega   53.00  150.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   39.0000   19.6509 97

148 omega   61.00  151.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   57.0000   74.6212 90

149 omega   53.00  152.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   76.0000 -127.7683 99

150 omega   58.00  154.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   43.0000 -143.7848 96

151 omega   59.00  150.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   66.0000  140.5926 91

152 omega   53.00  152.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   76.0000   26.9486 99

153 omega   11.00  114.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000  -80.0000  131.7417 103

154 omega   61.00  152.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   52.0000  171.5440 91

;
_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      -0.0204444000
_diffrn_orient_matrix_UB_12      -0.0797182000
_diffrn_orient_matrix_UB_13      0.0509452000
_diffrn_orient_matrix_UB_21      0.1133292000
_diffrn_orient_matrix_UB_22      -0.0378566000
_diffrn_orient_matrix_UB_23      -0.0254425000
_diffrn_orient_matrix_UB_31      0.0971464000
_diffrn_orient_matrix_UB_32      0.0934124000
_diffrn_orient_matrix_UB_33      0.1135716000
_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  0.0424
_diffrn_reflns_av_unetI/netI     0.0223
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            63489
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.833
_diffrn_reflns_theta_min         3.645
_diffrn_source                   'microfocus X-Ray tube'
_diffrn_source_type              'Agilent SuperNova (Cu) x-ray Source'
_exptl_absorpt_coefficient_mu    3.173
_exptl_absorpt_correction_T_max  0.965
_exptl_absorpt_correction_T_min  0.749
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24a (release 19-12-2012 CrysAlis171 .NET)
(compiled Dec 19 2012,11:08:27)
numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.563
_exptl_crystal_description       irregular
_exptl_crystal_F_000             882
_exptl_crystal_size_max          0.1399
_exptl_crystal_size_mid          0.0662
_exptl_crystal_size_min          0.0111
_refine_diff_density_max         0.467
_refine_diff_density_min         -0.429
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     535
_refine_ls_number_reflns         7012
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0271
_refine_ls_R_factor_gt           0.0245
_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^)+(0.0255P)^2^+1.4306P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0588
_refine_ls_wR_factor_ref         0.0599
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6619
_reflns_number_total             7012
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic401603y_si_002_5.cif
_cod_data_source_block           ga_ss47
_cod_original_cell_volume        1838.17(8)
_cod_original_formula_sum        'C40.50 H37 F8 N7 Zr'
_cod_database_code               4335906
_audit_block_refno               1696
_audit_block_usercomment         'SOS701, irregular, colourless'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C87-C82 \\sim C87-C86
 with sigma of 0.02
3. Restrained atomic chiral volume
 C81
 fixed at 0 with sigma of 0.1
4. Rigid bond restraints
 C81, C82, C83, C84, C85, C86, C87
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
C81 \\sim C82 \\sim C83 \\sim C84 \\sim C85 \\sim C86 \\sim C87: within 1A 
with sigma of 0.01 and sigma for terminal atoms of 0.01
6. others
 Fixed Sof: C81(0.5) C82(0.5) H82(0.5) C83(0.5) H83(0.5) C84(0.5) H84(0.5)
 C85(0.5) H85(0.5) C86(0.5) H86(0.5) C87(0.5) H87A(0.5) H87B(0.5) H87C(0.5)
7.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C3(H3A,H3B)
7.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C9(H9), C27(H27), C28(H28), C29(H29), C30(H30),
 C31(H31), C33(H33), C34(H34), C35(H35), C36(H36), C37(H37), C82(H82), C83(H83),
  C84(H84), C85(H85), C86(H86)
7.c Fitted hexagon refined as free rotating group:
 C81(C82,C83,C84,C85,C86)
7.d Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C24(H24A,H24B,
 H24C), C25(H25A,H25B,H25C), C87(H87A,H87B,H87C)
;
_shelx_estimated_absorpt_t_max   0.742
_shelx_estimated_absorpt_t_min   0.742
_shelx_hkl_checksum              43422
_cell_oxdiff_length_a            11.2275(2)
_cell_oxdiff_length_b            13.7650(3)
_cell_oxdiff_length_c            14.1485(3)
_cell_oxdiff_angle_alpha         112.625(2)
_cell_oxdiff_angle_beta          105.1498(18)
_cell_oxdiff_angle_gamma         101.2234(18)
_cell_oxdiff_volume              1838.17(7)
_cell_oxdiff_measurement_reflns_used 34503
_reflns_odcompleteness_completeness 98.54
_reflns_odcompleteness_theta     66.97
_reflns_odcompleteness_iscentric 1