Zirconium and Hafnium Hydrazinediido Half-Sandwich Complexes: Synthesis and Reactivity
Schweizer, Peter D.; Wadepohl, Hubert; Gade, Lutz H.; Organometallics 33 (2014) 1726–; doi:10.1021/om500087s

data_4082805
_publ_section_title
;
 Zirconium and Hafnium Hydrazinediido Half-Sandwich Complexes: Synthesis
 and Reactivity
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              1726
_journal_paper_doi               10.1021/om500087s
_journal_volume                  33
_journal_year                    2014
_chemical_formula_sum            'C40 H65 N7 Si2 Zr'
_chemical_formula_weight         791.39
_chemical_properties_physical    air-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
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_block_code                ga_psch27
_audit_creation_date
;
'Fri Sep 13 12:06:49 2013'
;
_audit_creation_method           SHELXL-2013
_audit_update_record             'Fri Sep 13 15:07:05 CEST 2013'
_cell_angle_alpha                69.7957(9)
_cell_angle_beta                 83.7816(9)
_cell_angle_gamma                89.9914(9)
_cell_formula_units_Z            4
_cell_length_a                   10.97715(14)
_cell_length_b                   18.92432(18)
_cell_length_c                   22.6228(2)
_cell_measurement_reflns_used    47366
_cell_measurement_temperature    110(1)
_cell_measurement_theta_max      70.8380
_cell_measurement_theta_min      3.7200
_cell_volume                     4380.93(8)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_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(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9241
_diffrn_detector_type            'Agilent EOS'
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_details
;
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omega____ theta____ kappa____ phi______ frames
    -       -3.5000   57.0000  -30.0000 54

  2 omega  -34.00   56.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       -3.5000   25.0000 -120.0000 180

  3 omega  -49.00   17.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       -3.5000  -64.0000    0.0000 132

  4 omega  -13.00   19.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       -3.5000  -64.0000  120.0000 64

  5 omega  -29.00   69.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
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  6 omega  -24.00   32.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
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  7 omega  -71.00  -24.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
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  8 omega   -5.00   24.00   0.5000    0.5000
omega____ theta____ kappa____ phi______ frames
    -       26.0000   79.0000 -155.8434 58

  9 omega    6.00   31.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       38.0000   80.0000  -32.8697 50

 10 omega    7.00   32.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       38.0000   78.0000   17.7188 50

 11 omega   11.00   39.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   80.0000  -93.3494 56

 12 omega   10.00   35.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   80.0000  176.6355 50

 13 omega   11.00   36.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   78.0000 -126.8652 50

 14 omega   15.00   40.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   79.0000   46.6272 50

 15 omega   14.00   39.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   80.0000   66.8115 50

 16 omega   15.00   41.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   78.0000  -78.8823 52

 17 omega   15.00   40.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   79.0000  179.8678 50

 18 omega   15.00   40.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   79.0000   21.7340 50

 19 omega   15.00   40.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   78.0000  102.2497 50

 20 omega   17.00   46.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   80.0000  113.1069 58

 21 omega   15.00   40.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   78.0000 -122.9196 50

 22 omega   20.00   47.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   77.0000    0.6618 54

 23 omega   19.00   44.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   79.0000 -131.9637 50

 24 omega   19.00   44.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   78.0000  134.4575 50

 25 omega   19.00   82.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -77.0000 -180.0000 126

 26 omega   33.00   62.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   69.0000  -92.2211 58

 27 omega   29.00   54.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000   73.2697 50

 28 omega   29.00   56.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   75.0000   52.7466 54

 29 omega   29.00   54.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000   94.2327 50

 30 omega   30.00   55.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   76.0000   62.2036 50

 31 omega   83.00  110.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000  -73.0767 54

 32 omega   28.00   55.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000  -73.0767 54

 33 omega   30.00   55.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   76.0000   39.6696 50

 34 omega   42.00   69.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   63.0000  176.3145 54

 35 omega   29.00   56.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   76.0000  -62.9249 54

 36 omega   31.00   56.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   74.0000  -43.5280 50

 37 omega   34.00   61.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   68.0000 -160.2646 54

 38 omega   28.00   55.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000   22.6392 54

 39 omega   35.00   62.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   72.0000 -127.0876 54

 40 omega   60.00   94.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000  -80.0000    1.1459 68

 41 omega   31.00   58.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000  -80.0000    1.1459 54

 42 omega   34.00   61.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   76.0000  -43.0543 54

 43 omega   41.00   75.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   61.0000   42.2084 68

 44 omega   33.00   59.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   75.0000 -162.4839 52

 45 omega   40.00   67.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   64.0000   52.9937 54

 46 omega   34.00   60.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   74.0000  120.3093 52

 47 omega   33.00   59.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   76.0000 -150.5959 52

 48 omega   40.00   77.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   70.0000  -76.1111 74

 49 omega   45.00  111.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   67.0000 -151.3523 132

 50 omega   45.00   72.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   67.0000  -36.6209 54

 51 omega   50.00   80.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   56.0000   50.3387 60

 52 omega   86.00  113.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   77.0000   76.8385 54

 53 omega   40.00   67.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   72.0000 -126.9784 54

 54 omega   40.00   90.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   70.0000  171.1287 100

 55 omega   46.00   73.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   59.0000  161.9478 54

 56 omega   36.00   85.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   77.0000   76.8385 98

 57 omega   69.00   96.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000  -80.0000 -122.5533 54

 58 omega   46.00  114.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   69.0000  -35.4641 136

 59 omega   43.00   79.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   72.0000 -172.4559 72

 60 omega   41.00   67.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   76.0000  -27.8472 52

 61 omega   49.00   90.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   58.0000   52.8647 82

 62 omega    1.00  101.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000  -79.0000  -74.6825 200

 63 omega   -1.00  101.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000  -80.0000  150.3900 204

 64 omega   41.00   70.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   75.0000   -3.8161 58

 65 omega   51.00  141.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   65.0000 -139.7708 180

 66 omega   68.00  108.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   58.0000   97.4360 80

 67 omega   52.00  136.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   49.0000  -26.5924 168

 68 omega   46.00   71.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   75.0000  136.9595 50

 69 omega   53.00  136.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   53.0000  -77.2385 166

 70 omega   52.00   79.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   68.0000 -122.2030 54

 71 omega   51.00   76.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   73.0000  -84.7802 50

 72 omega   56.00   81.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   65.0000  -89.1624 50

 73 omega   49.00   77.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   77.0000  140.7002 56

 74 omega   57.00  140.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   68.0000    9.0883 166

 75 omega   53.00   82.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   69.0000   67.1227 58

 76 omega   50.00   78.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   74.0000  -47.0368 56

 77 omega   61.00  149.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   61.0000   62.6264 176

 78 omega   56.00   85.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   70.0000   74.0603 58

 79 omega   61.00   87.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   56.0000   -2.1060 52

 80 omega   60.00   91.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   65.0000 -133.2352 62

 81 omega   61.00   92.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   66.0000  -75.7079 62

 82 omega   54.00  150.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   73.0000  124.0131 192

 83 omega   60.00  119.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   61.0000   -1.4411 118

 84 omega   68.00   93.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   37.0000  138.5617 50

 85 omega   62.00  150.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   67.0000   35.2343 176

 86 omega   61.00   88.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000  -79.0000  -64.9949 54

 87 omega   16.00   87.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000  -80.0000   40.7291 142

 88 omega   63.00  153.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   67.0000 -130.0904 180

 89 omega   59.00  136.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   72.0000 -172.4746 154

 90 omega   69.00  119.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   58.0000  -54.3523 100

 91 omega   68.00   95.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   61.0000   82.5174 54

 92 omega   61.00   91.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   76.0000  168.5790 60

 93 omega   73.00  114.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       94.0000   57.0000   78.2596 82

 94 omega   66.00   96.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       94.0000   75.0000 -146.5209 60

 95 omega   69.00   95.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       98.0000   76.0000   -6.1893 52

 96 omega   73.00  118.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      102.0000   77.0000   -3.3599 90

 97 omega  143.00  170.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -180.0000 54

 98 omega   78.00  105.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -180.0000 54

 99 omega  144.00  174.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  -90.0000 60

100 omega   37.00  106.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000  -91.8519 138

101 omega   79.00  104.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   30.0000 50

102 omega   79.00  104.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -30.0000 50

103 omega   72.00  140.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000  136.7241 136

104 omega   78.00  104.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -120.0000 52

105 omega   42.00   69.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000  136.7241 54

106 omega   79.00  177.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  150.0000 196

107 omega   78.00  104.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  120.0000 52

108 omega   78.00  165.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -150.0000 174

109 omega   79.00  104.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -90.0000 50

110 omega  127.00  178.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -60.0000 102

111 omega   37.00  109.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000   -4.2563 144

112 omega   79.00  104.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -60.0000 50

113 omega  120.00  177.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   60.0000 114

114 omega   79.00  104.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   60.0000 50

115 omega   85.00  136.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000 -180.0000 102

116 omega  125.00  178.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -120.0000 106

117 omega   85.00  112.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000   30.0000 54

118 omega   85.00  138.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000 -120.0000 106

119 omega  131.00  177.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   90.0000 92

120 omega   78.00  104.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   90.0000 52

121 omega  136.00  166.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   30.0000 60

122 omega   85.00  112.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  -90.0000 54

123 omega  139.00  166.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  -30.0000 54

124 omega   85.00  111.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  -30.0000 52

125 omega   86.00  157.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  -60.0000 142

126 omega   79.00  177.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000    0.0000 196

127 omega   81.00  175.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   73.0000 -165.7936 188

128 omega   79.00  129.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   75.0000  140.2402 100

129 omega   39.00  106.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000   81.8344 134

130 omega   75.00  139.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000 -165.5877 128

131 omega   37.00   65.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000 -165.5877 56

132 omega   85.00  135.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000   41.6550 100

133 omega   88.00  174.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   56.0000  127.1006 172

134 omega   87.00  114.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -79.0000  -49.0656 54

135 omega   38.00   66.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -79.0000  -49.0656 56

136 omega   85.00  112.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -79.0000 -123.1595 54

137 omega   83.00  148.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000  150.0000 130

138 omega   84.00  162.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000    0.0000 156

139 omega   83.00  158.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000  -60.0000 150

140 omega   84.00  176.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000  120.0000 184

141 omega   83.00  162.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000   60.0000 158

142 omega   85.00  114.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  120.0000 58

143 omega   85.00  174.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000   60.0000 178

144 omega   85.00  111.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000   90.0000 52

145 omega  -73.00   44.00   0.5000    0.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -19.0000   30.0000 234

146 omega  -76.00   31.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       -3.5000  -25.0000  -90.0000 214

147 omega    3.00   49.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       34.0000   78.0000  127.3703 92

148 omega   15.00   47.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   79.0000  179.8678 64

149 omega   15.00   49.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   78.0000  -78.8823 68

150 omega   19.00   49.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   78.0000  134.4575 60

151 omega   19.00   47.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   79.0000 -131.9637 56

152 omega   -5.00   98.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000  -80.0000 -122.5533 206

153 omega   -5.00   98.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000  -80.0000  -42.6137 206

154 omega   49.00  139.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   58.0000   52.8647 180

155 omega   -1.00  102.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000  -80.0000  150.3900 206

156 omega   43.00  139.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   72.0000 -172.4559 192

157 omega   50.00  142.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   68.0000 -122.2030 184

158 omega   53.00  143.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   58.0000   97.4360 180

159 omega   58.00  146.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   59.0000 -127.9423 176

160 omega   52.00  150.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   38.0000   97.9577 196

161 omega   50.00   75.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   73.0000  -84.7802 50

162 omega   50.00  148.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   74.0000  -47.0368 196

163 omega   54.00  146.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   68.0000    9.0883 184

164 omega   55.00  146.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   65.0000  -89.1624 182

165 omega   48.00  148.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   77.0000  140.7002 200

;
_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      0.0191962000
_diffrn_orient_matrix_UB_12      -0.0687912000
_diffrn_orient_matrix_UB_13      0.0588051000
_diffrn_orient_matrix_UB_21      0.0273705000
_diffrn_orient_matrix_UB_22      -0.0478320000
_diffrn_orient_matrix_UB_23      -0.0425138000
_diffrn_orient_matrix_UB_31      0.1372738000
_diffrn_orient_matrix_UB_32      0.0227251000
_diffrn_orient_matrix_UB_33      -0.0084203000
_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  0.032
_diffrn_reflns_av_unetI/netI     0.0179
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            217541
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.963
_diffrn_reflns_theta_min         3.772
_diffrn_source                   'microfocus X-Ray tube'
_diffrn_source_type              'Agilent SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.839
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68009
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.200
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1688
_exptl_crystal_size_max          0.2141
_exptl_crystal_size_mid          0.1969
_exptl_crystal_size_min          0.0808
_refine_diff_density_max         1.773
_refine_diff_density_min         -1.334
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     982
_refine_ls_number_reflns         29649
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0582
_refine_ls_R_factor_gt           0.0501
_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^)+(0.0777P)^2^+4.6216P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1340
_refine_ls_wR_factor_ref         0.1415
_reflns_Friedel_coverage         0.000
_reflns_number_gt                25914
_reflns_number_total             29649
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om500087s_si_002.cif
_cod_data_source_block           ga_complex_12
_cod_depositor_comments          'Adding full bibliography for 4082805.cif.'
_cod_database_code               4082805
_audit_block_refno               1846
_audit_block_usercomment         'PD506_1, irregular, light yellow'
_shelx_estimated_absorpt_t_min   0.764
_shelx_estimated_absorpt_t_max   0.764
_shelxl_version_number           2013-4
_shelx_res_checksum              33130
_cell_oxdiff_length_a            10.97715(14)
_cell_oxdiff_length_b            18.92432(18)
_cell_oxdiff_length_c            22.6228(2)
_cell_oxdiff_angle_alpha         69.7957(9)
_cell_oxdiff_angle_beta          83.7816(9)
_cell_oxdiff_angle_gamma         89.9914(9)
_cell_oxdiff_volume              4380.93(8)
_cell_oxdiff_measurement_reflns_used 47366
_cell_oxdiff_twin_number         2