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_4344797
_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         'C53 H53 Cl2 N P2 Zr, 0.5(C6 H14)'
_chemical_formula_sum            'C56 H60 Cl2 N P2 Zr'
_chemical_formula_weight         971.11
_chemical_properties_physical    'air-sensitive, moisture-sensitive'
_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
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'Tue Jan 29 10:31:07 2013'
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Olex2 1.2
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;
_audit_update_record
'26.10.2015 09:08:45 CET UTC+01:00  encif 1.36'
_cell_angle_alpha                98.0613(9)
_cell_angle_beta                 101.1523(12)
_cell_angle_gamma                96.3265(14)
_cell_formula_units_Z            4
_cell_length_a                   15.0656(3)
_cell_length_b                   15.5282(2)
_cell_length_c                   21.92283(17)
_cell_measurement_reflns_used    43338
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      70.9180
_cell_measurement_theta_min      4.1650
_cell_volume                     4932.07(13)
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;
CrysAlisPro, Agilent Technologies,
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
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'encif (Wadepohl, 2009-15); encifer 1.5 (CCDC, 2014)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SUPERFLIP (Palatinus, 2007-2009)'
_diffrn_ambient_temperature      110(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9241
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;
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omega____ theta____ kappa____ phi______ frames
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  2 omega   -6.00   33.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
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  3 omega  -30.00   72.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
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  4 omega  -70.00   30.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
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  5 omega   31.00   61.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
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  6 omega  -30.00   26.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
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  7 omega  -72.00  -37.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
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  8 omega  -35.00    2.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
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  9 omega  -17.00   19.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       16.0000   80.0000  -29.5213 72

 10 omega  -24.00    1.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -32.0000  -80.0000   93.5119 50

 11 omega   -2.00   23.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       32.0000   78.0000  -11.4138 50

 12 omega   12.00   39.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       40.0000   77.0000    3.8126 54

 13 omega    6.00   38.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       40.0000   80.0000 -162.1892 64

 14 omega    9.00   34.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       44.0000   80.0000   30.3562 50

 15 omega    9.00   34.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       44.0000   80.0000  146.1756 50

 16 omega   10.00   35.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       44.0000   78.0000  121.3767 50

 17 omega   72.00  108.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       44.0000   77.0000 -118.9355 72

 18 omega   10.00   39.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       44.0000   79.0000   80.9374 58

 19 omega   11.00   42.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       44.0000   77.0000 -118.9355 62

 20 omega  -42.00  -16.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -48.0000  -76.0000 -108.5475 52

 21 omega   13.00   38.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       48.0000   80.0000   58.9090 50

 22 omega   16.00   41.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       48.0000   77.0000  -70.5759 50

 23 omega   13.00   38.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       48.0000   80.0000  152.9259 50

 24 omega   13.00   38.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       48.0000   80.0000 -131.9298 50

 25 omega   13.00   38.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       48.0000   80.0000  -46.0433 50

 26 omega   17.00   42.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       52.0000   80.0000   11.3060 50

 27 omega   17.00   42.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       52.0000   80.0000 -107.5909 50

 28 omega  -51.00  -25.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -55.5967  -77.0000 -120.0000 52

 29 omega  -88.00   17.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -55.5967   77.0000   60.0000 210

 30 omega  -58.00  -24.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -55.5967  -77.0000 -150.0000 68

 31 omega   21.00   46.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       55.5967   79.0000   57.2876 50

 32 omega   24.00   50.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       55.5967   77.0000  -90.0000 52

 33 omega   23.00   64.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       55.5967   77.0000  120.0000 82

 34 omega   23.00   49.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       55.5967   77.0000   30.0000 52

 35 omega   30.00   80.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       55.5967  -80.0000 -156.8516 100

 36 omega   23.00   49.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       55.5967   77.0000  -60.0000 52

 37 omega   -7.00   26.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       55.5967  -80.0000 -156.8516 66

 38 omega   24.00   49.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       55.5967   77.0000  150.0000 50

 39 omega   24.00   51.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       55.5967   77.0000   90.0000 54

 40 omega   21.00   46.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       55.5967   79.0000 -173.1260 50

 41 omega  -62.00  -27.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -56.0000  -74.0000  148.0156 70

 42 omega  -55.00  -25.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -56.0000  -75.0000  157.1683 60

 43 omega -122.00  -97.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -56.0000  -75.0000  157.1683 50

 44 omega   22.00   47.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       56.0000   78.0000   -9.2973 50

 45 omega   22.00   47.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
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 46 omega  -53.00  -27.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
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 47 omega  -67.00  -31.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
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 48 omega  -59.00  -31.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -60.0000  -71.0000  114.3242 56

 49 omega  -58.00  -27.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -60.0000  -76.0000  -73.7437 62

 50 omega -131.00  -27.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -60.0000  -76.0000   15.8761 208

 51 omega  -62.00  -27.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -60.0000  -77.0000  -25.3534 70

 52 omega  -81.00  -31.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -60.0000  -72.0000  174.5948 100

 53 omega  -63.00  -29.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -60.0000  -74.0000  140.1650 68

 54 omega   57.00   84.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       60.0000   77.0000   77.2048 54

 55 omega   27.00   53.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       60.0000   77.0000   77.2048 52

 56 omega  -57.00  -31.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.0000  -76.0000 -110.3175 52

 57 omega  -62.00  -33.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.0000  -73.0000   59.9748 58

 58 omega  -59.00  -33.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.5000  -77.0000  -90.0000 52

 59 omega  -57.00  -31.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.5000  -77.0000  -49.4526 52

 60 omega  -58.00  -32.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.5000  -77.0000  -83.3516 52

 61 omega  -58.00  -32.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.5000  -76.0000  -16.0635 52

 62 omega -131.00 -105.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.5000  -76.0000  -16.0635 52

 63 omega  -57.00  -31.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.5000  -77.0000 -146.0437 52

 64 omega  -57.00  -31.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.5000  -77.0000   98.6814 52

 65 omega -135.00 -108.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.5000  -77.0000   98.6814 54

 66 omega  -57.00  -31.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.5000  -77.0000   33.0917 52

 67 omega  -64.00  -32.00   0.5000   10.0000
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 68 omega  -61.00  -35.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.5000  -77.0000 -120.0000 52

 69 omega  -61.00  -35.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.5000  -71.0000  151.7507 52

 70 omega  -61.00  -35.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.5000  -77.0000   90.0000 52

 71 omega  -58.00  -32.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.5000  -77.0000  -30.0000 52

 72 omega  -56.00  -31.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.5000  -77.0000  150.0000 50

 73 omega  -57.00  -31.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.5000  -77.0000   60.0000 52

 74 omega  -57.00  -31.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.5000  -77.0000    0.0000 52

 75 omega  -62.00  -36.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.5000  -77.0000   30.0000 52

 76 omega  -57.00  -31.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.5000  -77.0000  120.0000 52

 77 omega  -57.00  -31.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.5000  -77.0000 -180.0000 52

 78 omega  -99.00    8.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.5000   80.0000 -148.4714 214

 79 omega   44.00   77.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       68.0000   61.0000  151.7685 66

 80 omega   41.00  140.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       68.0000   72.0000  111.0948 198

 81 omega   38.00   64.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       68.0000   77.0000   30.3486 52

 82 omega   41.00   71.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       68.0000   67.0000   -9.0611 60

 83 omega   48.00  142.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       72.0000   62.0000 -106.8960 188

 84 omega   57.00  142.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       72.0000   56.0000   73.8846 170

 85 omega   42.00   71.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       72.0000   71.0000  152.9820 58

 86 omega   63.00   88.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       72.0000  -79.0000 -124.5343 50

 87 omega   52.00   84.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       72.0000   52.0000 -139.7403 64

 88 omega   49.00   78.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       72.0000   56.0000  -38.2252 58

 89 omega   43.00   69.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       76.0000   77.0000  -51.8922 52

 90 omega   46.00  106.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       76.0000   71.0000  178.3855 120

 91 omega   55.00   85.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       76.0000   55.0000 -131.9342 60

 92 omega   43.00   73.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       76.0000   77.0000   78.5616 60

 93 omega   69.00  111.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       76.0000  -80.0000  131.8610 84

 94 omega   43.00   69.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       76.0000   77.0000   12.2164 52

 95 omega   59.00  146.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       76.0000   56.0000    0.9798 174

 96 omega   48.00   74.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       80.0000   75.0000 -118.0032 52

 97 omega   74.00  100.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       80.0000   47.0000  114.9007 52

 98 omega   54.00   87.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       80.0000   66.0000  150.6723 66

 99 omega   59.00   85.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       80.0000   65.0000   43.7974 52

100 omega   55.00   85.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       80.0000   62.0000  126.3806 60

101 omega   70.00   97.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       84.0000  -80.0000 -176.7069 54

102 omega   58.00  154.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       84.0000   66.0000   70.3754 192

103 omega   67.00   93.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       84.0000   49.0000  -24.2644 52

104 omega   61.00   87.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       84.0000   48.0000 -133.6527 52

105 omega   52.00   82.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       84.0000  -80.0000   16.4681 60

106 omega   52.00   84.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       84.0000   75.0000   19.6022 64

107 omega   54.00   80.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       84.0000   72.0000  124.7327 52

108 omega   65.00  151.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       88.0000   62.0000  -53.7289 172

109 omega   63.00   89.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       88.0000   62.0000  -59.2595 52

110 omega   60.00  160.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       88.0000   72.0000 -131.8576 200

111 omega   17.00  109.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       88.0000  -80.0000  -79.8540 184

112 omega   62.00   93.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       88.0000   50.0000 -132.6118 62

113 omega   57.00  160.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       88.0000   73.0000  164.8676 206

114 omega   58.00   84.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       88.0000   72.0000   64.8005 52

115 omega   70.00  125.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       92.0000  -80.0000   42.8019 110

116 omega   68.00  143.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       92.0000   60.0000  136.1589 150

117 omega   68.00   93.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       92.0000   53.0000  -61.7251 50

118 omega   59.00   85.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       92.0000   76.0000  138.8021 52

119 omega   67.00   93.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       92.0000   53.0000  -69.6114 52

120 omega   62.00   88.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       92.0000   71.0000 -107.2564 52

121 omega   64.00   91.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       96.0000   75.0000    9.7074 54

122 omega   63.00   89.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       96.0000   77.0000  -47.5701 52

123 omega   71.00   96.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      100.0000   69.0000 -110.7573 50

124 omega   73.00  135.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      100.0000   67.0000   57.7448 124

125 omega   75.00  101.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      100.0000   52.0000 -160.2451 52

126 omega   67.00   93.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      100.0000   76.0000 -156.1152 52

127 omega   78.00  104.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.1934   77.0000  -60.0000 52

128 omega   78.00  104.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.1934   77.0000  120.0000 52

129 omega   78.00  178.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.1934   77.0000 -150.0000 200

130 omega   78.00  104.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.1934   77.0000   60.0000 52

131 omega   78.00  104.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.1934   77.0000  -90.0000 52

132 omega   78.00  178.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.1934   77.0000   90.0000 200

133 omega   78.00  105.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.1934   77.0000    0.0000 54

134 omega   78.00  104.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.1934   77.0000  150.0000 52

135 omega   85.00  177.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.1934   64.0000  -30.0000 184

136 omega   80.00  105.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.1934   75.0000 -121.0915 50

137 omega   88.00  178.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.1934   75.0000   35.9231 180

138 omega   71.00  144.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.1934  -80.0000 -122.1844 146

139 omega   42.00   68.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.1934  -80.0000 -122.1844 52

140 omega   85.00  110.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.1934   66.0000  -71.8792 50

141 omega  111.00  138.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.1934  -80.0000   99.1262 54

142 omega   80.00  107.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.1934  -80.0000   99.1262 54

143 omega   89.00  115.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.1934  -80.0000  -82.3471 52

144 omega   49.00   75.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.1934  -80.0000  -82.3471 52

145 omega   84.00  143.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.1934  -79.0000   26.3294 118

146 omega   42.00   75.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.1934  -79.0000   26.3294 66

147 omega   39.00  136.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.1934  -80.0000 -176.5715 194

148 omega   86.00  124.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.1934  -80.0000   54.7432 76

149 omega   43.00   81.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.1934  -80.0000   54.7432 76

150 omega   81.00  106.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.1934   71.0000   80.9834 50

151 omega   74.00  101.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.1934  -80.0000  133.8526 54

152 omega   42.00   68.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.1934  -80.0000  133.8526 52

153 omega   87.00  178.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.1934   64.0000    0.0000 182

154 omega   87.00  178.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.1934   64.0000  -60.0000 182

155 omega   85.00  112.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.1934   64.0000 -120.0000 54

156 omega   87.00  177.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.1934   64.0000   60.0000 180

157 omega   78.00  177.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.1934   77.0000 -120.0000 198

158 omega   86.00  177.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.1934   64.0000  120.0000 182

159 omega   86.00  178.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.1934   64.0000 -180.0000 184

160 omega   85.00  178.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.1934   64.0000  150.0000 186

161 omega   85.00  177.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.1934   64.0000  -90.0000 184

162 omega   78.00  103.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.1934   77.0000   30.0000 50

163 omega   78.00  104.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.1934   77.0000 -180.0000 52

164 omega   85.00  131.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.1934   64.0000   30.0000 92

165 omega   55.00  123.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.1934  -80.0000  -30.5820 136

166 omega   78.00  103.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.1934   77.0000  -30.0000 50

167 omega   61.00   88.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -80.0000  121.9888 54

168 omega  -24.00   71.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000 -120.0000 190

169 omega   -9.00   96.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       24.0000   77.0000  128.5516 210

170 omega   -6.00   56.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       24.0000   72.0000   67.2221 124

171 omega   -9.00   96.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       24.0000   76.0000   -9.4978 210

;
_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      -0.0224055000
_diffrn_orient_matrix_UB_12      -0.0933274000
_diffrn_orient_matrix_UB_13      -0.0387843000
_diffrn_orient_matrix_UB_21      0.0540383000
_diffrn_orient_matrix_UB_22      -0.0359562000
_diffrn_orient_matrix_UB_23      0.0556777000
_diffrn_orient_matrix_UB_31      -0.0875682000
_diffrn_orient_matrix_UB_32      -0.0155233000
_diffrn_orient_matrix_UB_33      0.0258296000
_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  0.049
_diffrn_reflns_av_unetI/netI     0.0343
_diffrn_reflns_laue_measured_fraction_full 0.992
_diffrn_reflns_laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            211558
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.512
_diffrn_reflns_theta_max         67.512
_diffrn_reflns_theta_min         3.845
_diffrn_source                   'microfocus X-Ray tube'
_diffrn_source_type              'Agilent SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.713
_exptl_absorpt_correction_T_max  0.989
_exptl_absorpt_correction_T_min  0.752
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
;
_exptl_crystal_colour            'dark yellow'
_exptl_crystal_density_diffrn    1.308
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2028
_exptl_crystal_size_max          0.214
_exptl_crystal_size_mid          0.147
_exptl_crystal_size_min          0.077
_refine_diff_density_max         3.869
_refine_diff_density_min         -2.013
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1132
_refine_ls_number_reflns         30987
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0792
_refine_ls_R_factor_gt           0.0649
_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^)+(0.1299P)^2^+0.5612P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1813
_refine_ls_wR_factor_ref         0.1902
_reflns_Friedel_coverage         0.000
_reflns_number_gt                24377
_reflns_number_total             30987
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02498_si_002.cif
_cod_data_source_block           ga_gp8a_5
_cod_original_cell_volume        4932.04(13)
_cod_database_code               4344797
_audit_block_refno               1684
_audit_block_usercomment         'gp396_4 gelb irregular Zwilling'
_chemical_oxdiff_formula         'C56 H60 cl2 N1 P2 Zr1'
_chemical_oxdiff_usercomment     'gp396_4 gelb irregular Zwilling'
_shelx_estimated_absorpt_t_max   0.708
_shelx_estimated_absorpt_t_min   0.708
_shelxl_version_number           2014/7
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5669(8) 0.4331(8)
2. 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
3. Restrained distances
 C201-C202 \\sim C205-C206 \\sim C202-C203 \\sim C204-C205 \\sim C203-C204
 with sigma of 0.02
4. Rigid body (RIGU) restrains
 C16, C17, C18, C19
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C15(H15A,H15B), C48(H48A,H48B), C74(H74A,H74B), C75(H75A,
 H75B), C108(H10A,H10B), C202(H20D,H20E), C203(H20F,H20G), C204(H20H,H20I),
 C205(H20J,H20K)
5.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C9(H9), C11(H11), C25(H25), C26(H26), C27(H27), C28(H28),
 C29(H29), C31(H31), C32(H32), C33(H33), C34(H34), C35(H35), C37(H37), C38(H38),
  C39(H39), C40(H40), C41(H41), C43(H43), C44(H44), C45(H45), C46(H46),
 C47(H47), C50(H50), C51(H51), C52(H52), C53(H53), C54(H54), C64(H64), C66(H66),
  C69(H69), C71(H71), C85(H85), C86(H86), C87(H87), C88(H88), C89(H89),
 C91(H91), C92(H92), C93(H93), C94(H94), C95(H95), C97(H97), C98(H98), C99(H99),
  C100(H100), C101(H101), C103(H103), C104(H104), C105(H105), C106(H106),
 C107(H107), C110(H110), C111(H111), C112(H112), C113(H113), C114(H114)
5.c 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), C77(H77A,H77B,H77C), C78(H78A,
 H78B,H78C), C79(H79A,H79B,H79C), C81(H81A,H81B,H81C), C82(H82A,H82B,H82C),
 C83(H83A,H83B,H83C), C201(H20A,H20B,H20C), C206(H20L,H20M,H20N)
;
_shelx_res_checksum              50977
_olex2_submission_special_instructions 'No special instructions were received'
_cell_oxdiff_length_a            15.0588(2)
_cell_oxdiff_length_b            15.5292(2)
_cell_oxdiff_length_c            21.92556(15)
_cell_oxdiff_angle_alpha         98.0614(8)
_cell_oxdiff_angle_beta          101.0976(10)
_cell_oxdiff_angle_gamma         96.3392(12)
_cell_oxdiff_volume              4931.65(11)
_cell_oxdiff_measurement_reflns_used 43338
_cell_oxdiff_twin_number         2