Ruthenium η4-Trimethylenemethane Complexes Containing Tripodal Phosphanomethylamine Ligands
Scherl, Peter; Kruckenberg, Achim; Mader, Steffen; Wadepohl, Hubert; Gade, Lutz H.; Organometallics 31 (2012) 7024–; doi:10.1021/om300794h

data_4079529
_publ_section_title
;
 Ruthenium \h4-Trimethylenemethane Complexes Containing Tripodal
 Phosphanomethylamine Ligands
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              7024
_journal_paper_doi               10.1021/om300794h
_journal_volume                  31
_journal_year                    2012
_chemical_absolute_configuration ad
_chemical_formula_sum            'C29 H56 N P3 Ru'
_chemical_formula_weight         612.73
_chemical_properties_physical    air-sensitive
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_block_code                ga_ps14
_audit_creation_date
;
'Mon Jan 16 11:33:41 2012'
;
_audit_creation_method
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_audit_update_record             'Mon Jan 16 11:44:00 CET 2012'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.26670(3)
_cell_length_b                   13.34070(5)
_cell_length_c                   22.72424(6)
_cell_measurement_reflns_used    116314
_cell_measurement_temperature    114.99(10)
_cell_measurement_theta_max      71.8874
_cell_measurement_theta_min      3.8390
_cell_volume                     3112.425(17)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR2011 (Giacovazzo et al., 2011)'
_diffrn_ambient_temperature      114.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9241
_diffrn_detector_type            'Agilent EOS'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
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omega____ theta____ kappa____ phi______ frames
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  3 omega  -57.00   -4.00   1.0000    3.0000
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  4 omega  -95.00  -62.00   1.0000    3.0000
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  5 omega    6.00   31.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
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  6 omega  -68.00   17.00   1.0000    3.0000
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  7 omega   10.00   35.00   1.0000    3.0000
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  8 omega   10.00   35.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   80.0000 -177.0000 25

  9 omega  -50.00   30.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000   25.0000 -120.0000 80

 10 omega  -69.00  -20.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
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 11 omega  -31.00   28.00   1.0000    3.0000
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 12 omega   14.00   39.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   80.0000 -145.0000 25

 13 omega   14.00   40.00   1.0000    3.0000
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 14 omega   19.00   44.00   1.0000    3.0000
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 15 omega   18.00   43.00   1.0000    3.0000
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 16 omega   19.00   44.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
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 17 omega   19.00   44.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
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 18 omega   23.00   48.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
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 19 omega   60.00  124.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
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 20 omega   23.00   48.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
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 21 omega   23.00   48.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
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 22 omega   25.00   51.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000   39.0000 26

 23 omega   30.00  108.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   76.0000   98.0000 78

 24 omega   83.00  124.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000  171.0000 41

 25 omega   30.00   66.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000  -65.0000 36

 26 omega   28.00   70.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000  171.0000 42

 27 omega   28.00   54.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
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 28 omega   76.00  124.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
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 29 omega   28.00   95.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
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 30 omega   28.00  123.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000 -141.0000 95

 31 omega   77.00  125.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   70.0000  153.0000 48

 32 omega   32.00   57.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   70.0000  153.0000 25

 33 omega   94.00  127.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000  -65.0000 33

 34 omega   -1.00   25.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
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 35 omega   -1.00  101.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
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 36 omega   73.00   99.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000  -80.0000   90.0000 26

 37 omega   35.00   87.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000  -80.0000  168.0000 52

 38 omega    8.00  104.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
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 39 omega   88.00  177.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   63.0000 -120.0000 89

 40 omega   87.00  113.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000   60.0000 26

 41 omega  121.00  175.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000  150.0000 54

 42 omega   80.00  106.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000  150.0000 26

 43 omega   80.00  106.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000  120.0000 26

 44 omega   80.00  106.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000  -30.0000 26

 45 omega   80.00  105.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000    0.0000 25

 46 omega   80.00  105.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000   30.0000 25

 47 omega  118.00  178.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000   90.0000 60

 48 omega   80.00  106.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000   90.0000 26

 49 omega   88.00  151.00   1.0000    6.0000
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 50 omega  119.00  176.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000 -180.0000 57

 51 omega   80.00  106.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000 -180.0000 26

 52 omega  153.00  178.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000 -120.0000 25

 53 omega   80.00  106.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000 -120.0000 26

 54 omega  123.00  172.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000    0.0000 49

 55 omega   80.00  178.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000   60.0000 98

 56 omega   80.00  178.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000  -90.0000 98

 57 omega  124.00  178.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000 -150.0000 54

 58 omega   80.00  106.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000 -150.0000 26

 59 omega   80.00  106.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000  -60.0000 26

 60 omega   91.00  117.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   50.0000 -150.0000 26

 61 omega   41.00  105.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -80.0000    3.0000 64

 62 omega   88.00  178.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   63.0000  -30.0000 90

 63 omega   78.00  140.00   1.0000    6.0000
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 64 omega   88.00  118.00   1.0000    6.0000
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    -      110.2342   63.0000    0.0000 30

 65 omega   42.00   67.00   1.0000    6.0000
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    -      110.2342  -79.0000  123.0000 25

 66 omega   73.00  100.00   1.0000    6.0000
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 67 omega   94.00  120.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   50.0000  -60.0000 26

 68 omega   72.00  130.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -80.0000 -103.0000 58

 69 omega   93.00  119.00   1.0000    6.0000
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    -      110.2342   50.0000  -90.0000 26

 70 omega   57.00  120.00   1.0000    6.0000
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    -      110.2342  -77.0000 -180.0000 63

 71 omega   40.00   66.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -80.0000 -103.0000 26

 72 omega   90.00  115.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   50.0000    0.0000 25

 73 omega   92.00  178.00   1.0000    6.0000
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    -      110.2342   50.0000   30.0000 86

 74 omega   95.00  121.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   50.0000   60.0000 26

 75 omega   48.00  142.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -80.0000   60.0000 94

 76 omega   88.00  129.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   63.0000   90.0000 41

 77 omega   88.00  116.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   63.0000  120.0000 28

 78 omega  119.00  177.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   63.0000  120.0000 58

 79 omega   85.00  111.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000 -150.0000 26

 80 omega   85.00  110.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000  -60.0000 25

 81 omega   85.00  124.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000 -120.0000 39

 82 omega   88.00  174.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   63.0000  -60.0000 86

 83 omega  -69.00   21.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
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 84 phi    240.00  360.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
 -40.0000    0.0000    0.0000     -     120

 85 omega    6.00   46.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       38.0000   80.0000  -87.0000 40

 86 omega   10.00   46.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   80.0000 -177.0000 36

 87 omega -110.00  -20.00   1.0000    3.0000
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    -      -42.5000  -63.0000   60.0000 90

 88 omega  -50.00   30.00   1.0000    3.0000
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    -      -42.5000   38.0000   30.0000 80

 89 omega -111.00  -21.00   1.0000    3.0000
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    -      -42.5000  -57.0000   30.0000 90

 90 omega  -50.00   30.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000   38.0000  -60.0000 80

 91 omega  -50.00   30.00   1.0000    3.0000
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 92 omega   14.00   46.00   1.0000    3.0000
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 93 omega   15.00   47.00   1.0000    3.0000
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 94 omega   14.00   46.00   1.0000    3.0000
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 95 omega   16.00  116.00   1.0000    3.0000
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 96 omega   19.00   47.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   79.0000  177.0000 28

 97 omega   19.00   49.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   78.0000   86.0000 30

 98 omega   19.00   47.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   79.0000    0.0000 28

 99 omega   18.00   46.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   80.0000  103.0000 28

100 omega   25.00  124.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   75.0000 -166.0000 99

101 omega   23.00   49.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   78.0000 -135.0000 26

102 omega   23.00   49.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   78.0000   64.0000 26

103 omega   24.00  124.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  124.0000 100

104 omega   24.00  124.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000   39.0000 100

105 omega   23.00   49.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   78.0000  105.0000 26

106 omega   34.00  124.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       55.1171   57.0000   60.0000 90

107 omega   28.00  128.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000  -65.0000 100

108 omega   29.00  128.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   76.0000   98.0000 99

109 omega   32.00  127.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   70.0000  153.0000 95

110 omega   28.00  128.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000  171.0000 100

111 omega   28.00  128.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000  -17.0000 100

112 omega   28.00  128.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000 -141.0000 100

113 omega   30.00  127.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   73.0000 -119.0000 97

114 omega   -5.00   98.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000  -80.0000 -107.0000 103

115 omega    7.00  110.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000  -80.0000   90.0000 103

116 omega    7.00  110.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000  -80.0000  168.0000 103

117 omega   11.00  114.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000  -80.0000  -89.0000 103

118 omega   11.00  113.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000  -79.0000  -15.0000 102

119 omega   80.00  178.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000   30.0000 98

120 omega   80.00  178.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000 -150.0000 98

121 omega   85.00  178.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000   30.0000 93

122 omega   80.00  178.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000  -90.0000 98

123 omega   80.00  178.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000 -120.0000 98

124 omega   80.00  178.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000 -180.0000 98

125 omega   88.00  178.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   50.0000 -120.0000 90

126 omega   88.00  178.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   63.0000   60.0000 90

127 omega   40.00  140.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -77.0000   90.0000 100

128 omega   88.00  178.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   50.0000  150.0000 90

129 omega   38.00   93.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -38.0000 -150.0000 55

130 omega   88.00  178.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   63.0000  -90.0000 90

131 omega   88.00  178.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   63.0000 -150.0000 90

132 omega   88.00  178.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   50.0000 -180.0000 90

133 omega   88.00  178.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   63.0000  -60.0000 90

134 omega   76.00  178.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   25.0000   60.0000 102

135 omega   40.00  140.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -77.0000 -120.0000 100

136 omega   88.00  178.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   50.0000  -30.0000 90

137 omega   85.00  178.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000  120.0000 93

138 omega   39.00  142.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -80.0000   18.0000 103

139 omega   37.00   94.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -25.0000   60.0000 57

140 omega   85.00  178.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000 -180.0000 93

141 omega   37.00   94.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -25.0000  -90.0000 57

142 omega   40.00  141.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -79.0000  140.0000 101

143 omega   88.00  178.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   50.0000  120.0000 90

144 omega   80.00  178.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000   90.0000 98

145 omega   37.00   94.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -25.0000  150.0000 57

146 omega   37.00   94.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -25.0000  -30.0000 57

147 omega   88.00  178.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   63.0000 -180.0000 90

148 omega   40.00  141.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -79.0000  -20.0000 101

149 omega   85.00  178.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000    0.0000 93

150 omega   85.00  178.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000  -90.0000 93

151 omega   88.00  178.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   63.0000   90.0000 90

152 omega   40.00  140.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -77.0000 -180.0000 100

153 omega   85.00  178.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000  150.0000 93

154 omega   85.00  178.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000  -30.0000 93

155 omega   88.00  178.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   63.0000   30.0000 90

156 omega   88.00  178.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   50.0000   90.0000 90

157 omega   88.00  178.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   50.0000   30.0000 90

158 omega   85.00  178.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000   90.0000 93

159 omega   80.00  178.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000  -60.0000 98

160 omega   88.00  178.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   50.0000    0.0000 90

161 omega  -68.00   22.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -63.0000 -148.0000 90

162 omega  -21.00   47.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       10.0000   79.0000  116.0000 68

163 omega -115.00   30.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000    0.0000    0.0000 145

164 omega -113.00  -12.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000 -180.0000 101

165 omega -115.00   23.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000    0.0000  120.0000 138

166 omega  -18.00  128.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       55.1171    0.0000    0.0000 146

167 omega  -18.00  128.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       55.1171    0.0000  240.0000 146

168 omega  -18.00  128.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       55.1171    0.0000    0.0000 146

169 omega  -18.00  128.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       55.1171    0.0000  240.0000 146

170 omega  -18.00  128.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       55.1171    0.0000  120.0000 146

171 omega  -18.00  128.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       55.1171    0.0000  120.0000 146

172 omega   28.00  128.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000  -88.0000 100

173 omega   -5.00   98.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000  -80.0000  -68.0000 103

174 omega   -1.00  102.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000  -80.0000   90.0000 103

;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Agilent SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w and \p scans'
_diffrn_measurement_specimen_support 'polyimid foil'
_diffrn_orient_matrix_UB_11      0.0069562000
_diffrn_orient_matrix_UB_12      0.0052591000
_diffrn_orient_matrix_UB_13      -0.0676748000
_diffrn_orient_matrix_UB_21      -0.1406514000
_diffrn_orient_matrix_UB_22      -0.0395304000
_diffrn_orient_matrix_UB_23      -0.0039876000
_diffrn_orient_matrix_UB_31      -0.0517002000
_diffrn_orient_matrix_UB_32      0.1083673000
_diffrn_orient_matrix_UB_33      0.0017942000
_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  0.0624
_diffrn_reflns_av_sigmaI/netI    0.0729
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            169021
_diffrn_reflns_theta_full        66.97
_diffrn_reflns_theta_max         71.8874
_diffrn_reflns_theta_min         3.8390
_diffrn_source                   'Agilent SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.649
_exptl_absorpt_correction_T_max  0.943
_exptl_absorpt_correction_T_min  0.927
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.308
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1304
_exptl_crystal_size_max          0.1423
_exptl_crystal_size_mid          0.1204
_exptl_crystal_size_min          0.1147
_refine_diff_density_max         0.239
_refine_diff_density_min         -0.356
_refine_diff_density_rms         0.039
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.015(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     339
_refine_ls_number_reflns         6117
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0132
_refine_ls_R_factor_gt           0.0132
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0175P)^2^+0.7866P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0338
_refine_ls_wR_factor_ref         0.0338
_reflns_number_gt                6104
_reflns_number_total             6117
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300794h_si_002.cif
_cod_data_source_block           compound_5
_cod_original_cell_volume        3112.423(17)
_cod_database_code               4079529
_audit_block_refno               1415
_audit_block_usercomment         PS315
_cell_oxdiff_length_a            10.26948(10)
_cell_oxdiff_length_b            13.34143(15)
_cell_oxdiff_length_c            22.7168(2)
_cell_oxdiff_angle_alpha         89.9719(8)
_cell_oxdiff_angle_beta          89.9850(8)
_cell_oxdiff_angle_gamma         89.9801(9)
_cell_oxdiff_volume              3112.42(5)
_cell_oxdiff_measurement_reflns_used 116314
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_theta     66.97
_reflns_odcompleteness_iscentric 1