Synthesis and reactivity of cyclometalated triamidophosphine complexes of niobium and tantalum.
Sietzen, Malte; Wadepohl, Hubert; Ballmann, Joachim; Inorganic chemistry 54 (2015) 4094–4103; doi:10.1021/acs.inorgchem.5b00333

data_4343175
_publ_section_title
;
 Synthesis and reactivity of cyclometalated triamidophosphine complexes of
 niobium and tantalum.
;
_journal_issue                   8
_journal_name_full               'Inorganic chemistry'
_journal_page_first              4094
_journal_page_last               4103
_journal_paper_doi               10.1021/acs.inorgchem.5b00333
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C53 H59 N5 Nb P Si'
_chemical_formula_sum            'C53 H59 N5 Nb P Si'
_chemical_formula_weight         918.02
_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'
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_cell_measurement_reflns_used    52233
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CrysAlisPro, Agilent Technologies,
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omega____ theta____ kappa____ phi______ frames
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  2 omega   -9.00   21.00   1.0000    5.0000
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  3 omega  -67.00  -15.00   1.0000    5.0000
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  4 omega  -24.00   32.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
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  5 omega   39.00   65.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
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  6 omega  -28.00    9.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
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  7 omega   17.00   44.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       -3.5000   38.0000   30.0000 27

  8 omega  -13.00   47.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
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  9 omega   -5.00   48.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       26.0000   78.0000  131.4505 53

 10 omega    7.00   38.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       38.0000   79.0000   59.0052 31

 11 omega    6.00   31.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       38.0000   80.0000 -136.6938 25

 12 omega   11.00   36.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   78.0000  139.7759 25

 13 omega   15.00   40.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   79.0000 -164.3077 25

 14 omega   16.00   42.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   78.0000 -104.2463 26

 15 omega   15.00   40.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   78.0000  -62.6915 25

 16 omega   18.00   43.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   80.0000   -6.2606 25

 17 omega   18.00   43.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   80.0000   64.1821 25

 18 omega   18.00   43.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   80.0000 -161.5012 25

 19 omega   22.00   48.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   77.0000   37.0187 26

 20 omega   19.00   45.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   80.0000  140.5717 26

 21 omega   18.00   43.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   80.0000  -38.7475 25

 22 omega   29.00   55.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000  -64.5277 26

 23 omega   30.00   66.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   75.0000   24.0599 36

 24 omega   30.00   56.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000  -90.2269 26

 25 omega   28.00   53.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000  -11.1393 25

 26 omega   29.00   55.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000 -138.5725 26

 27 omega   76.00  103.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000  -90.2269 27

 28 omega   28.00   54.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000   84.6781 26

 29 omega   30.00   56.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000  158.0152 26

 30 omega   78.00  117.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000  -11.1393 39

 31 omega   24.00   90.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000  -80.0000 -124.5458 66

 32 omega  -11.00   17.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000  -80.0000 -124.5458 28

 33 omega   42.00   69.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   73.0000   98.6982 27

 34 omega   28.00   54.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000  137.8035 26

 35 omega   31.00   57.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   75.0000   41.3439 26

 36 omega   32.00   63.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   76.0000 -172.1139 31

 37 omega   28.00   55.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000   62.1351 27

 38 omega   89.00  115.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000  158.0152 26

 39 omega  -13.00   89.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000  -80.0000   43.3379 102

 40 omega   53.00  130.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   58.0000  137.5972 77

 41 omega   35.00   71.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   74.0000  -13.6069 36

 42 omega   33.00   64.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   76.0000  157.3473 31

 43 omega   47.00   73.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   77.0000  -87.0787 26

 44 omega   33.00   59.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   75.0000   89.6371 26

 45 omega   41.00   67.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   73.0000   50.9194 26

 46 omega   39.00   65.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
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 47 omega   46.00   72.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   65.0000  101.0341 26

 48 omega   48.00   94.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   58.0000  -51.0596 46

 49 omega   46.00   95.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   56.0000 -137.1609 49

 50 omega   63.00   89.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   66.0000  178.4043 26

 51 omega   36.00   61.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   77.0000  -18.5055 25

 52 omega   38.00   68.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   73.0000 -117.1224 30

 53 omega   42.00   69.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   74.0000  -13.1053 27

 54 omega   49.00   75.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   64.0000   91.0710 26

 55 omega   41.00   69.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   77.0000 -109.3590 28

 56 omega    0.00  101.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000  -80.0000  119.5682 101

 57 omega   57.00   84.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000  -80.0000  -35.2093 27

 58 omega   45.00   72.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   77.0000  -67.5878 27

 59 omega   53.00  143.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   55.0000   61.1228 90

 60 omega   53.00   80.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   69.0000  -23.2095 27

 61 omega   50.00   79.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   73.0000   89.2276 29

 62 omega   59.00   86.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000  -80.0000  179.1246 27

 63 omega   61.00  111.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   65.0000   -9.6161 50

 64 omega   53.00  130.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   76.0000 -120.9391 77

 65 omega   52.00   80.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   77.0000  138.3109 28

 66 omega   57.00  103.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   69.0000   -1.9163 46

 67 omega   57.00   83.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   40.0000 -121.9214 26

 68 omega   52.00   91.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000  -80.0000  -55.1020 39

 69 omega   65.00  152.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   58.0000   23.5388 87

 70 omega   59.00   85.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   74.0000 -150.4074 26

 71 omega   65.00  140.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   55.0000  -16.0000 75

 72 omega   56.00  127.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   77.0000  145.6308 71

 73 omega   61.00   89.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   70.0000   81.1924 28

 74 omega   56.00  155.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   77.0000  -74.3167 99

 75 omega   62.00  159.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   73.0000  103.7408 97

 76 omega   70.00  110.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   59.0000 -156.3821 40

 77 omega   67.00  151.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   45.0000   88.7116 84

 78 omega   70.00  107.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       94.0000   43.0000 -166.4020 37

 79 omega   66.00   92.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       94.0000   74.0000   18.6305 26

 80 omega   81.00  106.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000  110.0717 25

 81 omega   77.00  104.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -77.0000  -90.0000 27

 82 omega   83.00  108.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000    0.0000 25

 83 omega   43.00   69.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000  110.0717 26

 84 omega  119.00  153.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  150.0000 34

 85 omega   86.00  111.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  150.0000 25

 86 omega  122.00  174.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000   60.0000 52

 87 omega   86.00  118.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000   60.0000 32

 88 omega   85.00  111.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000    0.0000 26

 89 omega   86.00  175.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000   30.0000 89

 90 omega   46.00  102.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000   78.1221 56

 91 omega  118.00  173.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  120.0000 55

 92 omega   78.00  106.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  120.0000 28

 93 omega   86.00  111.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  -90.0000 25

 94 omega   85.00  112.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  -60.0000 27

 95 omega   85.00  175.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000 -120.0000 90

 96 omega   78.00  165.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000    0.0000 87

 97 omega  109.00  178.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   90.0000 69

 98 omega   78.00  105.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   90.0000 27

 99 omega   79.00  104.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -120.0000 25

100 omega   85.00  112.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  120.0000 27

101 omega   78.00  177.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -30.0000 99

102 omega   81.00  177.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -90.0000 96

103 omega  153.00  178.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   30.0000 25

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

105 omega   78.00  177.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  150.0000 99

106 omega  116.00  160.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -60.0000 44

107 omega   75.00  138.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000   42.6111 63

108 omega   80.00  107.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -60.0000 27

109 omega   85.00  174.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000 -180.0000 89

110 omega   85.00  175.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000 -150.0000 90

111 omega  153.00  178.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   60.0000 25

112 omega   44.00   72.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000   42.6111 28

113 omega   81.00  108.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   60.0000 27

114 omega   78.00  105.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -150.0000 27

115 omega   85.00  128.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000   90.0000 43

116 omega   78.00  104.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -180.0000 26

117 omega   37.00  138.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000 -121.1641 101

118 omega   82.00  113.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000 -180.0000 31

119 omega   85.00  144.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  -30.0000 59

120 omega   73.00  138.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000  -19.7808 65

121 omega   39.00  106.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000  170.1057 67

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

123 omega  -69.00   21.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000  -30.0000 90

124 omega  -25.00   67.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       -3.5000   50.0000   90.0000 92

125 omega   -7.00   92.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       22.0000   76.0000  -33.3474 99

126 omega   -6.00   92.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       22.0000   74.0000 -107.2428 98

127 omega    5.00   95.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       26.0000   56.0000   67.6897 90

128 omega    5.00   95.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       26.0000   55.0000  118.0348 90

129 omega    7.00   49.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       38.0000   78.0000  -77.5464 42

130 omega   11.00   49.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   78.0000  139.7759 38

131 omega   15.00   47.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   79.0000    6.0476 32

132 omega   14.00   46.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   80.0000  132.9154 32

133 omega   18.00   46.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   80.0000   64.1821 28

134 omega   18.00   46.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   80.0000 -161.5012 28

135 omega   18.00   46.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   80.0000  140.5717 28

136 omega   18.00   46.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   80.0000  -38.7475 28

137 omega   20.00   90.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   77.0000   37.0187 70

138 omega  -13.00   90.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000  -80.0000 -124.5458 103

139 omega   28.00  128.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000 -138.5725 100

140 omega   28.00  128.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000  137.8035 100

141 omega   29.00  128.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   75.0000   41.3439 99

142 omega   33.00  132.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   76.0000  157.3473 99

143 omega   34.00  131.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   73.0000   50.9194 97

144 omega   34.00  132.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   74.0000  -13.6069 98

145 omega   33.00  132.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   75.0000   89.6371 99

146 omega   43.00  134.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   66.0000  178.4043 91

147 omega   45.00  135.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   56.0000 -137.1609 90

148 omega   38.00  135.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   73.0000 -117.1224 97

149 omega   44.00  134.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   61.0000   20.7625 90

150 omega   45.00  135.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   58.0000  -51.0596 90

151 omega   40.00  140.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   77.0000 -109.3590 100

152 omega   -1.00  102.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000  -80.0000  -35.2093 103

153 omega   -1.00  102.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000  -80.0000  -80.0911 103

154 omega   53.00  143.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   55.0000   61.1228 90

155 omega   53.00  144.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   52.0000  123.5469 91

156 omega   51.00  141.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   64.0000    1.4709 90

157 omega   44.00  144.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   77.0000  -67.5878 100

158 omega    7.00  110.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000  -80.0000  179.1246 103

159 omega   55.00  146.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   65.0000   -9.6161 91

160 omega   50.00  147.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   73.0000   89.2276 97

161 omega   53.00  146.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   69.0000  -23.2095 93

162 omega   58.00  146.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   59.0000  -52.8053 88

;
_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      0.0615867000
_diffrn_orient_matrix_UB_12      -0.1219847000
_diffrn_orient_matrix_UB_13      0.0143895000
_diffrn_orient_matrix_UB_21      -0.0117386000
_diffrn_orient_matrix_UB_22      0.0026999000
_diffrn_orient_matrix_UB_23      0.0936123000
_diffrn_orient_matrix_UB_31      -0.1217077000
_diffrn_orient_matrix_UB_32      -0.0334959000
_diffrn_orient_matrix_UB_33      0.0331249000
_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  0.0431
_diffrn_reflns_av_unetI/netI     0.0213
_diffrn_reflns_laue_measured_fraction_full 0.985
_diffrn_reflns_laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            88872
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.698
_diffrn_reflns_theta_min         3.630
_diffrn_source                   'microfocus X-Ray tube'
_diffrn_source_type              'Agilent SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.955
_exptl_absorpt_correction_T_max  0.929
_exptl_absorpt_correction_T_min  0.646
_exptl_absorpt_correction_type   gaussian
_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)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.294
_exptl_crystal_description       plate
_exptl_crystal_F_000             964
_exptl_crystal_size_max          0.184
_exptl_crystal_size_mid          0.093
_exptl_crystal_size_min          0.025
_refine_diff_density_max         0.806
_refine_diff_density_min         -0.731
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     559
_refine_ls_number_reflns         8834
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0329
_refine_ls_R_factor_gt           0.0308
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0397P)^2^+2.1636P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0808
_refine_ls_wR_factor_ref         0.0820
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8386
_reflns_number_total             8834
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b00333_si_001.cif
_cod_data_source_block           ba_ms3
_cod_database_code               4343175
_audit_block_refno               1730
_audit_block_usercomment         'MS136, plate, yellow'
_chemical_oxdiff_formula         'C53 H59 N5 Nb1 P1 Si1'
_chemical_oxdiff_usercomment     'MS136, plate, yellow'
_shelx_estimated_absorpt_t_max   0.757
_shelx_estimated_absorpt_t_min   0.757
_reflns_odcompleteness_completeness 98.50
_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.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C9(H9), C12(H12), C13(H13), C14(H14), C15(H15),
 C18(H18), C19(H19), C20(H20), C21(H21), C23(H23), C25(H25), C27(H27), C31(H31),
  C33(H33), C35(H35), C39(H39), C41(H41), C43(H43), C49(H49), C50(H50),
 C51(H51), C52(H52), C53(H53)
2.c Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C36(H36A,H36B,H36C), C37(H37A,H37B,
 H37C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C46(H46A,H46B,H46C), C47(H47A,
 H47B,H47C), C48(H48A,H48B,H48C)
;
_shelx_res_checksum              69995
_olex2_submission_special_instructions 'No special instructions were received'
_cell_oxdiff_length_a            12.33713(18)
_cell_oxdiff_length_b            12.97373(17)
_cell_oxdiff_length_c            16.8536(2)
_cell_oxdiff_angle_alpha         73.3096(11)
_cell_oxdiff_angle_beta          68.5804(12)
_cell_oxdiff_angle_gamma         73.5376(12)
_cell_oxdiff_volume              2356.76(5)
_cell_oxdiff_measurement_reflns_used 52261