Synthesis and Reactivity of Group 4 Metal Benzyl Complexes Supported by Carbazolide-Based PNP Pincer Ligands.
Plundrich, Gudrun T.; Wadepohl, Hubert; Gade, Lutz H.; Inorganic chemistry 55 (2015) 353–; doi:10.1021/acs.inorgchem.5b02498

data_4344794
_publ_section_title
;
 Synthesis and Reactivity of Group 4 Metal Benzyl Complexes Supported by
 Carbazolide-Based PNP Pincer Ligands.
;
_journal_issue                   1
_journal_name_full               'Inorganic chemistry'
_journal_page_first              353
_journal_paper_doi               10.1021/acs.inorgchem.5b02498
_journal_volume                  55
_journal_year                    2015
_chemical_formula_moiety         'C34 H54 I3 N P2 Zr'
_chemical_formula_sum            'C34 H54 I3 N P2 Zr'
_chemical_formula_weight         1010.64
_chemical_properties_physical    'air-sensitive, moisture-sensitive'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
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'Thu Apr 30 15:37:01 2015'
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Olex2 1.2
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;
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_cell_angle_alpha                90
_cell_angle_beta                 92.1938(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.12353(13)
_cell_length_b                   13.48168(12)
_cell_length_c                   22.15079(19)
_cell_measurement_reflns_used    31776
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      70.2220
_cell_measurement_theta_min      3.8240
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;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
;
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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)'
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'encif (Wadepohl, 2009-15); encifer 1.5 (CCDC, 2014)'
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_computing_structure_solution    'SUPERFLIP (Palatinus, 2007-2009)'
_diffrn_ambient_environment      'perfluoro polyether oil / N~2~'
_diffrn_ambient_temperature      120(1)
_diffrn_detector                 'CCD plate'
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_diffrn_measurement_details
;
  1 omega    9.00   72.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   19.0000    0.0000 63

  2 omega  -24.00   41.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
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  3 omega  -67.00  -42.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
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  4 omega  -42.00    6.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
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  5 omega  -70.00    0.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
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  6 omega  -25.00   28.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
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  7 omega  -18.00   40.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
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  8 omega    5.00   35.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
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  9 omega    6.00   31.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       38.0000   80.0000 -132.9548 25

 10 omega   10.00   35.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   80.0000   17.6708 25

 11 omega   10.00   35.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   80.0000   80.5480 25

 12 omega   10.00   35.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   80.0000  117.9667 25

 13 omega   14.00   39.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   80.0000  161.0910 25

 14 omega   15.00   40.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   79.0000 -107.1432 25

 15 omega   14.00   39.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   80.0000  -35.1444 25

 16 omega   19.00   44.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   79.0000 -156.9168 25

 17 omega   19.00   44.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   79.0000  -61.9927 25

 18 omega   19.00   44.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   79.0000 -121.6849 25

 19 omega   19.00   49.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   78.0000   31.4524 30

 20 omega   19.00   44.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   79.0000  -10.4533 25

 21 omega   18.00   43.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   80.0000   76.0170 25

 22 omega   21.00   46.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   77.0000   63.9120 25

 23 omega   19.00   45.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   80.0000  -91.8957 26

 24 omega   24.00   51.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000   60.0000 27

 25 omega  -15.00   84.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -77.0000  120.0000 99

 26 omega   23.00   48.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   78.0000  142.2860 25

 27 omega   23.00   48.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   78.0000  -27.1951 25

 28 omega   33.00   60.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000 -120.0000 27

 29 omega   25.00   50.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000 -180.0000 25

 30 omega   26.00   53.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  -60.0000 27

 31 omega   -6.00   65.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -77.0000 -150.0000 71

 32 omega  -17.00   86.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -80.0000   -4.8059 103

 33 omega   25.00   52.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000    0.0000 27

 34 omega   24.00   51.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  101.8428 27

 35 omega   27.00   54.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000 -150.0000 27

 36 omega   29.00   56.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   76.0000  136.6014 27

 37 omega   28.00   55.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000  -94.6956 27

 38 omega   29.00   54.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000  -36.8730 25

 39 omega   33.00   58.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   73.0000  -71.6871 25

 40 omega  -13.00   89.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000  -80.0000  -77.3103 102

 41 omega   29.00   54.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000  -13.7423 25

 42 omega   30.00   55.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   76.0000 -146.7629 25

 43 omega   29.00   56.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000 -133.0986 27

 44 omega   30.00   58.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   75.0000  177.2855 28

 45 omega   29.00   54.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000  109.7313 25

 46 omega   29.00   56.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   75.0000   81.6793 27

 47 omega   28.00   59.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000    9.4233 31

 48 omega   36.00   63.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   75.0000 -165.4964 27

 49 omega   33.00   68.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   75.0000   66.1642 35

 50 omega   33.00   59.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   76.0000 -108.3938 26

 51 omega   37.00   64.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   76.0000  -54.0572 27

 52 omega   45.00   91.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   61.0000  -62.0838 46

 53 omega   41.00   68.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   69.0000  -55.4286 27

 54 omega   38.00   65.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   73.0000   29.5584 27

 55 omega   38.00   65.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   76.0000   38.0933 27

 56 omega   39.00   64.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   73.0000  -13.4963 25

 57 omega   38.00   90.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   76.0000  160.4868 52

 58 omega   47.00   74.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   67.0000  -67.2141 27

 59 omega   51.00  106.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   56.0000  -79.8725 55

 60 omega   41.00   66.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   77.0000  -40.4927 25

 61 omega   41.00   68.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   75.0000  123.8632 27

 62 omega   49.00   79.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   63.0000  114.5617 30

 63 omega   44.00  127.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   70.0000   82.8892 83

 64 omega   40.00   82.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   77.0000  169.1135 42

 65 omega   51.00   78.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000  -80.0000 -100.1259 27

 66 omega   48.00   79.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   65.0000   18.7976 31

 67 omega   52.00  120.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   60.0000 -123.3413 68

 68 omega   48.00   73.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   71.0000 -172.5669 25

 69 omega   46.00   75.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   75.0000   25.4458 29

 70 omega   48.00   75.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   76.0000 -128.1413 27

 71 omega   45.00   70.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   77.0000 -168.0180 25

 72 omega   44.00   96.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   77.0000  -18.3269 52

 73 omega   49.00   76.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   70.0000   56.1348 27

 74 omega   50.00   76.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   74.0000  103.1957 26

 75 omega   58.00  101.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   60.0000   26.7936 43

 76 omega   52.00   79.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   72.0000 -162.6769 27

 77 omega   95.00  122.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   55.0000 -160.5224 27

 78 omega   60.00   88.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   55.0000 -160.5224 28

 79 omega   53.00   88.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   69.0000   -7.3766 35

 80 omega   54.00   81.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000  -79.0000   23.3001 27

 81 omega   50.00  116.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   75.0000   42.2796 66

 82 omega   53.00  109.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   75.0000  124.1924 56

 83 omega   56.00   83.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   75.0000  100.4846 27

 84 omega   58.00   95.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   68.0000  -31.3717 37

 85 omega   55.00   81.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   71.0000 -173.0111 26

 86 omega   60.00   87.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   64.0000   35.8121 27

 87 omega   55.00   82.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   75.0000 -139.4453 27

 88 omega   60.00   87.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   61.0000  -54.6083 27

 89 omega   54.00   89.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   76.0000 -125.5462 35

 90 omega   57.00   90.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   75.0000 -163.8617 33

 91 omega   56.00   82.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   77.0000  -96.8043 26

 92 omega   59.00   97.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   73.0000  132.3591 38

 93 omega   59.00  154.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   75.0000  -15.9555 95

 94 omega   61.00   87.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   75.0000  -23.5148 26

 95 omega   71.00  135.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   43.0000  -25.8623 64

 96 omega   69.00   97.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   58.0000 -111.3428 28

 97 omega   67.00   93.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   69.0000  173.8409 26

 98 omega   64.00   89.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   71.0000   15.1306 25

 99 omega   70.00   95.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   55.0000  175.1922 25

100 omega   63.00  123.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   72.0000   35.0717 60

101 omega   66.00  101.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   69.0000   83.6443 35

102 omega   77.00  156.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   63.0000 -162.4931 79

103 omega   62.00  104.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   76.0000  132.6174 42

104 omega   69.00   95.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       94.0000   70.0000   65.9143 26

105 omega   74.00  100.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       94.0000   64.0000  -98.5424 26

106 omega   74.00  101.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       94.0000   53.0000  -97.5492 27

107 omega   84.00  111.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       94.0000   59.0000  -76.6772 27

108 omega   78.00  110.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       98.0000   56.0000  134.8001 32

109 omega   78.00  107.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      102.0000   68.0000  -98.1720 29

110 omega   78.00  177.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -120.0000 99

111 omega   76.00  139.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000   79.3198 63

112 omega  110.00  177.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   90.0000 67

113 omega   78.00  104.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   90.0000 26

114 omega   78.00  175.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   30.0000 97

115 omega  146.00  172.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -60.0000 26

116 omega   78.00  104.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -60.0000 26

117 omega   79.00  177.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -90.0000 98

118 omega  104.00  130.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -79.0000   10.0990 26

119 omega   78.00  175.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  120.0000 97

120 omega   38.00   96.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -79.0000   10.0990 58

121 omega   78.00  175.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000    0.0000 97

122 omega   86.00  175.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   63.0000  -30.0000 89

123 omega  151.00  177.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   60.0000 26

124 omega   86.00  112.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   63.0000 -150.0000 26

125 omega   78.00  104.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   60.0000 26

126 omega   78.00  105.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -180.0000 27

127 omega   86.00  120.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   63.0000   90.0000 34

128 omega   86.00  175.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   63.0000  -60.0000 89

129 omega   78.00  163.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  140.9524 85

130 omega   72.00   99.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000  -86.2818 27

131 omega   81.00  108.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   71.0000  -13.9935 27

132 omega   86.00  113.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   71.0000 -141.5341 27

133 omega   45.00  100.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000   45.8407 55

134 omega   63.00  102.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000 -107.8499 39

135 omega   67.00  139.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000 -150.9000 72

136 omega   72.00  109.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000  -64.2948 37

137 omega   39.00   65.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000 -150.9000 26

138 omega   75.00  102.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -77.0000  -30.0000 27

139 omega   82.00  160.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000 -120.0000 78

140 omega   63.00  104.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000  168.3112 41

141 omega   87.00  112.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   63.0000  -90.0000 25

142 omega   88.00  175.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   63.0000   60.0000 87

143 omega   88.00  127.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   63.0000 -120.0000 39

144 omega   81.00  134.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   72.0000   24.0000 53

145 omega   86.00  112.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   63.0000  120.0000 26

146 omega   65.00  103.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -77.0000  120.0000 38

147 omega  135.00  177.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -150.0000 42

148 omega   78.00  104.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -150.0000 26

149 omega   78.00  104.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -30.0000 26

150 omega   86.00  175.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   63.0000 -180.0000 89

151 omega   78.00  160.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  150.0000 82

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

153 omega  -73.00   44.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -19.0000  150.0000 117

154 omega  -26.00   72.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   38.0000  -60.0000 98

155 omega  -21.00   69.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000 -180.0000 90

156 omega   -6.00   91.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       22.0000   73.0000  105.6480 97

157 omega   -4.00   96.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       26.0000   77.0000   24.1786 100

158 omega   -4.00   96.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       26.0000   77.0000  -78.0294 100

159 omega   -3.00   96.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       26.0000   76.0000  152.1191 99

160 omega   -1.00  102.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000  -80.0000 -100.1259 103

161 omega   46.00  138.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   67.0000  -67.2141 92

162 omega   53.00  143.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   56.0000  137.5705 90

163 omega   48.00  143.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   70.0000   56.1348 95

164 omega    7.00  109.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000  -79.0000   23.3001 102

165 omega   51.00  147.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   72.0000 -162.6769 96

166 omega   55.00  149.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   45.0000  -15.5189 94

167 omega   50.00  144.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   74.0000  103.1957 94

168 omega   56.00  148.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   50.0000 -103.2338 92

169 omega   53.00  146.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   69.0000   -7.3766 93

;
_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      -0.0870789000
_diffrn_orient_matrix_UB_12      0.0195921000
_diffrn_orient_matrix_UB_13      0.0431810000
_diffrn_orient_matrix_UB_21      -0.0300203000
_diffrn_orient_matrix_UB_22      0.0938017000
_diffrn_orient_matrix_UB_23      -0.0361546000
_diffrn_orient_matrix_UB_31      -0.0729252000
_diffrn_orient_matrix_UB_32      -0.0621840000
_diffrn_orient_matrix_UB_33      -0.0409241000
_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  0.0783
_diffrn_reflns_av_unetI/netI     0.0251
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            131015
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.951
_diffrn_reflns_theta_min         3.839
_diffrn_source                   'microfocus X-Ray tube'
_diffrn_source_type              'Agilent SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    21.799
_exptl_absorpt_correction_T_max  0.613
_exptl_absorpt_correction_T_min  0.210
_exptl_absorpt_correction_type   gaussian
_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)
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    1.714
_exptl_crystal_description       plate
_exptl_crystal_F_000             1976
_exptl_crystal_size_max          0.106
_exptl_crystal_size_mid          0.051
_exptl_crystal_size_min          0.029
_refine_diff_density_max         1.280
_refine_diff_density_min         -1.170
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     384
_refine_ls_number_reflns         7502
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0495
_refine_ls_R_factor_gt           0.0438
_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^)+(0.0455P)^2^+20.3277P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1041
_refine_ls_wR_factor_ref         0.1072
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6840
_reflns_number_total             7502
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02498_si_002.cif
_cod_data_source_block           ga_gp32
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4344794
_audit_block_refno               2425
_audit_block_usercomment         'gp-II-08, plate, red'
_chemical_oxdiff_formula         'C34 H54 I3 N P2 Zr'
_chemical_oxdiff_usercomment     'gp-II-08, plate, red'
_shelx_estimated_absorpt_t_max   0.219
_shelx_estimated_absorpt_t_min   0.219
_reflns_odcompleteness_completeness 99.96
_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 1.5 times of:
  All C(H,H,H) groups
2. Rigid body (RIGU) restrains
 C24, C25, C26
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C27, C28, C29
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C30, C31, C32
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C33, C34, C35
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3.a Ternary CH refined with riding coordinates:
 C24(H24), C27(H27), C30(H30), C33(H33)
3.b Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C15(H15A,H15B)
3.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C9(H9), C11(H11)
3.d Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C21(H21A,H21B,
 H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C25(H25A,H25B,H25C), C26(H26A,
 H26B,H26C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C31(H31A,H31B,H31C),
 C32(H32A,H32B,H32C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C)
;
_shelx_res_checksum              75038
_olex2_submission_special_instructions 'No special instructions were received'
_cell_oxdiff_length_a            13.1226(2)
_cell_oxdiff_length_b            13.48599(19)
_cell_oxdiff_length_c            22.1450(4)
_cell_oxdiff_angle_alpha         89.9941(12)
_cell_oxdiff_angle_beta          92.1695(14)
_cell_oxdiff_angle_gamma         90.0547(13)
_cell_oxdiff_volume              3916.20(11)
_cell_oxdiff_measurement_reflns_used 31776