Synthesis of NPN-Coordinated Tantalum Alkyl Complexes and Their Hydrogenolysis: Isolation of a Terminal Tantalum Hydride Incorporating a Doubly Cyclometalated NPN Scaffold
Batke, Sonja; Sietzen, Malte; Wadepohl, Hubert; Ballmann, Joachim; Inorganic Chemistry  (2017) –; doi:10.1021/acs.inorgchem.7b00277

data_4345726
_publ_section_title
;
 Synthesis of NPN-Coordinated Tantalum Alkyl Complexes and Their
 Hydrogenolysis: Isolation of a Terminal Tantalum Hydride Incorporating a
 Doubly Cyclometalated NPN Scaffold
;
_journal_name_full               'Inorganic Chemistry'
_journal_paper_doi               10.1021/acs.inorgchem.7b00277
_journal_year                    2017
_chemical_formula_moiety         'C43 H53 N2 P2 Si Ta, C4 H10 O'
_chemical_formula_sum            'C47 H63 N2 O P2 Si Ta'
_chemical_formula_weight         942.97
_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   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_block_code                ba_ms39
_audit_creation_date
;
'Wed Aug 26 10:11:38 2015'
;
_audit_creation_method
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Olex2 1.2
(compiled 2015.01.26 svn.r3151 for OlexSys, GUI svn.r4998)
;
_audit_update_record
'26.08.2015 10:16:29 CEST UTC+02:00  encif 1.32'
_cell_angle_alpha                87.6364(7)
_cell_angle_beta                 82.5388(7)
_cell_angle_gamma                84.0719(7)
_cell_formula_units_Z            4
_cell_length_a                   9.39598(8)
_cell_length_b                   21.86855(18)
_cell_length_c                   22.49629(19)
_cell_measurement_reflns_used    119207
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      70.6380
_cell_measurement_theta_min      4.4580
_cell_volume                     4556.99(7)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material
'encif (Wadepohl, 2009-14); encifer 1.5 (CCDC, 2014)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'SUPERFLIP (Palatinus, 2007-2009)'
_diffrn_ambient_environment      'perfluoro polyether oil / N~2~'
_diffrn_ambient_temperature      120(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9621
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_details
;
  1 omega   31.00   60.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   77.0000  150.0000 29

  2 omega  -71.00  -31.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -19.0000    0.0000 40

  3 omega  -39.00   26.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -38.0000  -90.0000 65

  4 omega  -59.00   25.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -38.0000 -180.0000 84

  5 omega  -25.00   41.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -19.0000    0.0000 66

  6 omega  -68.00  -41.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -38.0000  -90.0000 27

  7 omega  -11.00   78.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       10.0000   71.0000  -32.4486 89

  8 omega   -5.00   38.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       22.0000   79.0000   29.9031 43

  9 omega    7.00   32.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       38.0000   78.0000  100.6913 25

 10 omega    9.00   45.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       38.0000   78.0000  140.8030 36

 11 omega   10.00   35.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   80.0000   15.9582 25

 12 omega   15.00   40.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   77.0000 -115.0817 25

 13 omega   10.00   35.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   80.0000  171.3301 25

 14 omega   10.00   35.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   80.0000  -90.3718 25

 15 omega   11.00   36.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   78.0000 -126.1122 25

 16 omega   11.00   36.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   78.0000  -42.7832 25

 17 omega   14.00   39.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   80.0000  -89.6495 25

 18 omega   19.00   45.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   79.0000 -158.7298 26

 19 omega   19.00   44.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   79.0000   60.5060 25

 20 omega   18.00   43.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   80.0000  -99.7837 25

 21 omega   21.00   47.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   77.0000 -114.8495 26

 22 omega   18.00   43.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   80.0000  116.0672 25

 23 omega   19.00   44.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   78.0000    7.8454 25

 24 omega   29.00   55.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000    0.0000 26

 25 omega   23.00   48.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   78.0000  -73.1521 25

 26 omega   23.00   48.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   78.0000  -39.9490 25

 27 omega   25.00   53.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000 -106.6588 28

 28 omega   23.00   48.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   78.0000   51.3225 25

 29 omega   26.00   52.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  -60.0000 26

 30 omega   24.00   50.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000   90.0000 26

 31 omega   25.00   50.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000   93.3928 25

 32 omega   26.00   52.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000 -120.0000 26

 33 omega   23.00   48.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   78.0000  138.2309 25

 34 omega   24.00   50.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000 -150.0000 26

 35 omega   23.00   48.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   78.0000  174.7939 25

 36 omega   28.00   54.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  -90.0000 26

 37 omega  -17.00   86.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -80.0000  111.4728 103

 38 omega   30.00   56.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   75.0000  -66.1296 26

 39 omega   28.00   54.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000  -31.9160 26

 40 omega   29.00   55.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   76.0000 -118.5820 26

 41 omega   32.00   63.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   74.0000   35.1966 31

 42 omega  103.00  128.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   75.0000  -66.1296 25

 43 omega   36.00   62.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000   78.8911 26

 44 omega   38.00   63.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   66.0000  -86.5767 25

 45 omega   29.00   55.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   76.0000   72.0466 26

 46 omega   30.00   62.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   76.0000  176.6908 32

 47 omega   28.00   54.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000   11.9268 26

 48 omega   81.00  107.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000  134.6036 26

 49 omega   29.00   55.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000  134.6036 26

 50 omega   30.00   57.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   75.0000 -151.3302 27

 51 omega   71.00  128.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   76.0000   72.0466 57

 52 omega  -12.00   89.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000  -80.0000   -4.7380 101

 53 omega   30.00   56.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   76.0000  -56.7443 26

 54 omega   35.00   61.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   71.0000  -65.8094 26

 55 omega   32.00   72.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000  -80.0000 -162.9750 40

 56 omega   33.00   62.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   76.0000    1.8399 29

 57 omega   36.00   66.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   71.0000   81.0329 30

 58 omega   33.00   59.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   76.0000 -146.9461 26

 59 omega   -9.00   17.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000  -80.0000 -162.9750 26

 60 omega   47.00   88.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   61.0000 -136.1421 41

 61 omega  100.00  126.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   76.0000  112.5101 26

 62 omega   37.00   63.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   76.0000  112.5101 26

 63 omega   68.00   95.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000  -80.0000 -118.1798 27

 64 omega   39.00   94.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   71.0000 -125.8141 55

 65 omega   37.00   63.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   75.0000  156.3269 26

 66 omega   37.00   63.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   77.0000  -65.7789 26

 67 omega   43.00   74.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   66.0000   57.7125 31

 68 omega   45.00  133.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   69.0000   -4.6683 88

 69 omega   48.00  102.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   63.0000  -98.1465 54

 70 omega   42.00   69.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   73.0000  -44.0090 27

 71 omega   47.00   75.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   72.0000   60.0841 28

 72 omega   46.00   72.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   75.0000   -9.5084 26

 73 omega   52.00   78.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000  -79.0000  -58.0817 26

 74 omega   44.00   70.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   77.0000 -110.6440 26

 75 omega   49.00   75.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   72.0000  138.3417 26

 76 omega   46.00   72.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   76.0000  -43.9023 26

 77 omega   53.00  141.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   54.0000   47.3201 88

 78 omega   49.00   75.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   75.0000  -98.8318 26

 79 omega   53.00   79.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   70.0000   81.7284 26

 80 omega    8.00  109.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000  -80.0000 -157.2937 101

 81 omega   50.00   76.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   74.0000  173.8944 26

 82 omega   57.00   86.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   64.0000  172.1060 29

 83 omega   57.00   85.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   69.0000  -77.7629 28

 84 omega   56.00   82.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   51.0000  135.3644 26

 85 omega   62.00  150.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   57.0000  -98.0620 88

 86 omega   53.00   79.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   76.0000 -102.3022 26

 87 omega   55.00   98.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   72.0000  -13.5253 43

 88 omega   57.00   90.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   74.0000  -54.5312 33

 89 omega   58.00   98.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   69.0000  148.1969 40

 90 omega   60.00   88.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   61.0000 -118.4721 28

 91 omega   54.00   80.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   74.0000   80.7006 26

 92 omega   54.00   80.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   74.0000 -163.3450 26

 93 omega   72.00   97.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   51.0000 -130.0524 25

 94 omega   68.00  112.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   57.0000 -113.7108 44

 95 omega   58.00   89.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   73.0000  143.7709 31

 96 omega   65.00  143.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   55.0000 -163.5476 78

 97 omega   57.00   83.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   76.0000  113.7622 26

 98 omega   50.00  106.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000  -80.0000   68.7347 56

 99 omega   59.00   85.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   72.0000  -32.5834 26

100 omega   65.00   98.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   66.0000    6.6628 33

101 omega   56.00   84.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   77.0000  -85.8371 28

102 omega   67.00   94.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   59.0000  116.6794 27

103 omega   59.00   85.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   72.0000  112.6952 26

104 omega   64.00   89.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   74.0000  -24.9943 25

105 omega   60.00   86.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   77.0000  116.4329 26

106 omega   69.00   99.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   51.0000   72.7491 30

107 omega   61.00   88.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   75.0000  -75.5958 27

108 omega   66.00   91.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   68.0000   99.1875 25

109 omega   73.00  163.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       94.0000   54.0000  -22.3278 90

110 omega   78.00  104.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       98.0000   52.0000   90.9063 26

111 omega   76.00  107.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       98.0000   50.0000 -157.2183 31

112 omega   70.00   96.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       98.0000   73.0000   27.8212 26

113 omega   75.00  101.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      102.0000   72.0000    4.6708 26

114 omega  143.00  169.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      102.0000   68.0000  -80.3212 26

115 omega   78.00  104.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      102.0000   68.0000  -80.3212 26

116 omega   81.00  108.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      102.0000   58.0000  157.6635 27

117 omega   79.00  171.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  150.0000 92

118 omega   78.00  104.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   30.0000 26

119 omega   78.00  178.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -60.0000 100

120 omega   78.00  103.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -30.0000 25

121 omega  110.00  177.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -150.0000 67

122 omega   78.00  104.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -150.0000 26

123 omega   79.00  177.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  120.0000 98

124 omega  135.00  161.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -120.0000 26

125 omega   79.00  105.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -120.0000 26

126 omega   85.00  111.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000   90.0000 26

127 omega   78.00  104.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -180.0000 26

128 omega   83.00  110.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   76.0000   -8.3927 27

129 omega   37.00  123.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000  108.9597 86

130 omega   79.00  117.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000   14.9868 38

131 omega   38.00  140.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000 -151.9265 102

132 omega   68.00  108.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -79.0000  153.4855 40

133 omega   37.00   63.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -79.0000  153.4855 26

134 omega   82.00  109.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000   46.9039 27

135 omega   45.00   71.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000   46.9039 26

136 omega   83.00  158.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000   30.0000 75

137 omega   51.00  140.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000  -78.5490 89

138 omega   75.00  135.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000  -33.3793 60

139 omega   84.00  157.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000  -90.0000 73

140 omega   86.00  113.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  150.0000 27

141 omega   86.00  174.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000   30.0000 88

142 omega   46.00   93.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -38.0000 -180.0000 47

143 omega   86.00  175.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  -90.0000 89

144 omega   86.00  112.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000 -120.0000 26

145 omega   86.00  143.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  120.0000 57

146 omega   86.00  174.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000 -180.0000 88

147 omega  141.00  173.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  -30.0000 32

148 omega   85.00  111.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  -30.0000 26

149 omega   85.00  112.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000  -30.0000 27

150 omega   85.00  178.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000    0.0000 93

151 omega   85.00  112.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  -60.0000 27

152 omega   78.00  177.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   60.0000 99

153 omega   78.00  104.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000    0.0000 26

154 omega   85.00  119.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000 -150.0000 34

155 omega   78.00  166.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   90.0000 88

156 omega   79.00  105.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -90.0000 26

157 omega  -44.00   73.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   19.0000  -30.0000 117

158 omega  -44.00   73.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   19.0000 -120.0000 117

159 omega  -30.00   70.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   77.0000  -30.0000 100

160 omega  -13.00   83.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       14.0000   71.0000  -30.4838 96

161 omega  -16.00   84.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       14.0000   77.0000  -74.0353 100

162 omega   -1.00   90.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       22.0000   65.0000 -114.1911 91

163 omega   -4.00   96.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       26.0000   77.0000 -162.4844 100

164 omega   -3.00   96.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       26.0000   76.0000  117.8718 99

165 omega   -4.00   96.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       26.0000   77.0000   23.7090 100

166 omega   10.00   46.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   80.0000  171.3301 36

167 omega   10.00   46.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   80.0000  -90.3718 36

168 omega   10.00   46.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   80.0000   15.9582 36

169 omega   14.00   46.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   80.0000  -89.6495 32

170 omega   19.00   49.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   78.0000    7.8454 30

171 omega   19.00   47.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   79.0000   60.5060 28

172 omega   19.00   47.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   79.0000 -158.7298 28

173 omega   18.00   46.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   80.0000  -99.7837 28

174 omega   23.00   49.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   78.0000   51.3225 26

175 omega   23.00   49.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   78.0000  138.2309 26

176 omega  -19.00  127.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000    0.0000  240.0000 146

177 omega  -18.00   80.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -38.0000  150.0000 98

178 omega   23.00   49.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   78.0000  174.7939 26

179 omega  -19.00  127.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000    0.0000    0.0000 146

180 omega  -19.00  127.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000    0.0000  120.0000 146

181 omega   24.00  124.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  120.0000 100

182 omega  -19.00   52.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000    0.0000    0.0000 71

183 omega   23.00   49.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   78.0000  -73.1521 26

184 omega   24.00  124.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000 -120.0000 100

185 omega   29.00  128.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   76.0000  176.6908 99

186 omega   29.00  128.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   76.0000   72.0466 99

187 omega   35.00  126.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   66.0000  -86.5767 91

188 omega   28.00  128.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000  134.6036 100

189 omega   28.00  128.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000   78.8911 100

190 omega   -9.00   94.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000  -80.0000 -162.9750 103

191 omega   33.00  132.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   76.0000    1.8399 99

192 omega   44.00  134.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   61.0000 -136.1421 90

193 omega   36.00  136.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   77.0000  -65.7789 100

194 omega   43.00  134.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   66.0000   57.7125 91

195 omega   39.00  135.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   71.0000 -125.8141 96

196 omega   -5.00   98.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000  -80.0000 -118.1798 103

197 omega   37.00  136.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   76.0000  112.5101 99

198 omega   47.00  137.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   64.0000  176.6787 90

199 omega   48.00  138.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   63.0000  -98.1465 90

200 omega    3.00  105.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000  -79.0000   70.7989 102

201 omega   53.00  143.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   55.0000 -133.1784 90

202 omega   51.00  145.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   47.0000 -120.1477 94

203 omega   52.00  144.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   49.0000  117.6972 92

204 omega   51.00  145.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   46.0000   21.6788 94

205 omega   45.00  144.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   75.0000   -9.5084 99

206 omega   47.00  143.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   72.0000  138.3417 96

207 omega   47.00  143.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   72.0000   60.0841 96

208 omega   44.00  144.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   77.0000 -110.6440 100

209 omega   53.00  143.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   54.0000   47.3201 90

210 omega    3.00  105.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000  -79.0000  -58.0817 102

211 omega   51.00  145.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   46.0000 -105.9314 94

212 omega   45.00  144.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   76.0000  -43.9023 99

213 omega   52.00  147.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   70.0000   81.7284 95

214 omega   53.00  146.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   69.0000  -77.7629 93

215 omega    7.00  110.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000  -80.0000 -157.2937 103

216 omega   50.00  148.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   74.0000  173.8944 98

217 omega   55.00  145.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   64.0000  172.1060 90

218 omega   56.00  148.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   51.0000  135.3644 92

219 omega   49.00  148.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   75.0000  -98.8318 99

;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Agilent SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'polyimid foil'
_diffrn_orient_matrix_UB_11      0.0295987000
_diffrn_orient_matrix_UB_12      -0.0206235000
_diffrn_orient_matrix_UB_13      -0.0654829000
_diffrn_orient_matrix_UB_21      -0.1263768000
_diffrn_orient_matrix_UB_22      -0.0403451000
_diffrn_orient_matrix_UB_23      0.0115557000
_diffrn_orient_matrix_UB_31      -0.1037618000
_diffrn_orient_matrix_UB_32      0.0544716000
_diffrn_orient_matrix_UB_33      -0.0187697000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0480
_diffrn_reflns_av_unetI/netI     0.0189
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            235871
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.807
_diffrn_reflns_theta_min         3.965
_diffrn_source                   'microfocus X-Ray tube'
_diffrn_source_type              'Agilent SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.631
_exptl_absorpt_correction_T_max  0.853
_exptl_absorpt_correction_T_min  0.483
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.374
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1936
_exptl_crystal_size_max          0.173
_exptl_crystal_size_mid          0.059
_exptl_crystal_size_min          0.033
_refine_diff_density_max         0.527
_refine_diff_density_min         -0.654
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1009
_refine_ls_number_reflns         17144
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0235
_refine_ls_R_factor_gt           0.0210
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0189P)^2^+4.1829P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0473
_refine_ls_wR_factor_ref         0.0483
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16094
_reflns_number_total             17144
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic7b00277_si_002.cif
_cod_data_source_block           ba_ms39
_cod_database_code               4345726
_audit_block_refno               2501
_audit_block_usercomment         'MS374, irregular, yellow'
_chemical_oxdiff_formula         'C47 H63 N2 O1 P2 Si1 Ta1'
_chemical_oxdiff_usercomment     'MS374, irregular, yellow'
_shelx_estimated_absorpt_t_max   0.603
_shelx_estimated_absorpt_t_min   0.603
_reflns_odcompleteness_completeness 98.61
_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:
 C37(H37A,H37B), C87(H87A,H87B), C201(H20A,H20B), C203(H20F,H20G), C101(H10A,
 H10B), C103(H10F,H10G)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C11(H11), C13(H13), C18(H18),
 C19(H19), C20(H20), C21(H21), C24(H24), C26(H26), C28(H28), C32(H32), C33(H33),
  C34(H34), C35(H35), C36(H36), C53(H53), C54(H54), C55(H55), C56(H56),
 C59(H59), C61(H61), C63(H63), C68(H68), C69(H69), C70(H70), C71(H71), C74(H74),
  C76(H76), C78(H78), C82(H82), C83(H83), C84(H84), C85(H85), C86(H86)
2.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C29(H29A,H29B,H29C), C30(H30A,H30B,
 H30C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C41(H41A,
 H41B,H41C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C64(H64A,H64B,H64C),
 C65(H65A,H65B,H65C), C79(H79A,H79B,H79C), C80(H80A,H80B,H80C), C88(H88A,H88B,
 H88C), C89(H89A,H89B,H89C), C90(H90A,H90B,H90C), C91(H91A,H91B,H91C), C92(H92A,
 H92B,H92C), C93(H93A,H93B,H93C), C202(H20C,H20D,H20E), C204(H20H,H20I,H20J),
 C102(H10C,H10D,H10E), C104(H10H,H10I,H10J)
;
_shelx_res_checksum              51836
_olex2_submission_special_instructions 'No special instructions were received'
_cell_oxdiff_length_a            9.39597(8)
_cell_oxdiff_length_b            21.86855(18)
_cell_oxdiff_length_c            22.49629(19)
_cell_oxdiff_angle_alpha         87.6364(7)
_cell_oxdiff_angle_beta          82.5388(7)
_cell_oxdiff_angle_gamma         84.0719(7)
_cell_oxdiff_volume              4556.99(7)
_cell_oxdiff_measurement_reflns_used 119207