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_4343173
_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         'C45 H44 N3 P Ta, 1.5(C6 H6)'
_chemical_formula_sum            'C54 H54 N3 P Ta'
_chemical_formula_weight         956.92
_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_ms7
_audit_creation_date
;
'Wed Dec 04 12:29:14 2013'
;
_audit_creation_method
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Olex2 1.2
(compiled 2015.01.26 svn.r3151 for OlexSys, GUI svn.r4998)
;
_audit_update_record
'10.02.2015 17:26:42 CET UTC+01:00  encif 1.29'
_cell_angle_alpha                77.885(5)
_cell_angle_beta                 68.693(5)
_cell_angle_gamma                70.190(5)
_cell_formula_units_Z            2
_cell_length_a                   12.0019(6)
_cell_length_b                   13.7239(7)
_cell_length_c                   15.1796(9)
_cell_measurement_reflns_used    5944
_cell_measurement_temperature    110(1)
_cell_measurement_theta_max      65.7680
_cell_measurement_theta_min      4.1220
_cell_volume                     2180.8(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
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'encif (Wadepohl, 2009-14); encifer 1.5 (CCDC, 2014)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'SUPERFLIP (Palatinus, 2007-2009)'
_diffrn_ambient_temperature      110(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9621
_diffrn_detector_type            'Agilent EOS'
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_details
;
  1 omega   21.00   68.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   77.0000   60.0000 47

  2 omega   29.00   57.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   77.0000 -150.0000 28

  3 omega  -21.00   23.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -38.0000   90.0000 44

  4 omega  -26.00    5.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   77.0000 -150.0000 31

  5 omega  -72.00   24.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -38.0000    0.0000 96

  6 omega  -28.00   13.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   77.0000   60.0000 41

  7 omega  -71.00  -30.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -38.0000   90.0000 41

  8 omega    9.00   44.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       14.0000   80.0000  169.0480 35

  9 omega    2.00   27.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       34.0000   80.0000   58.4681 25

 10 omega    3.00   28.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       34.0000   79.0000 -133.1489 25

 11 omega    7.00   32.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       38.0000   79.0000  -21.2501 25

 12 omega   11.00   36.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   79.0000  -64.4155 25

 13 omega   11.00   36.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   80.0000  120.6364 25

 14 omega   16.00   44.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   79.0000 -119.0204 28

 15 omega   15.00   40.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   79.0000    4.6958 25

 16 omega   15.00   40.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   78.0000  155.6109 25

 17 omega   14.00   39.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   80.0000 -173.9831 25

 18 omega   17.00   44.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   79.0000  -79.7637 27

 19 omega   19.00   44.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   79.0000   35.9051 25

 20 omega   19.00   44.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   79.0000  -62.0256 25

 21 omega   19.00   44.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   78.0000  102.5199 25

 22 omega   19.00   44.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   78.0000   82.5653 25

 23 omega   33.00   59.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000   60.0000 26

 24 omega   30.00   57.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000   30.0000 27

 25 omega   29.00   56.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  -90.0000 27

 26 omega   29.00   56.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000 -150.0000 27

 27 omega   25.00   52.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000 -180.0000 27

 28 omega   23.00   48.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   78.0000   19.4680 25

 29 omega  -16.00   83.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -77.0000 -180.0000 99

 30 omega   29.00   56.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  -30.0000 27

 31 omega   28.00   55.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  120.0000 27

 32 omega   28.00   55.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  150.0000 27

 33 omega   31.00   58.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000 -120.0000 27

 34 omega   29.00  116.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  -60.0000 87

 35 omega   83.00  108.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   76.0000   76.6414 25

 36 omega   29.00   56.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   76.0000   76.6414 27

 37 omega   32.00   59.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   76.0000  129.9270 27

 38 omega   91.00  118.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000  179.4548 27

 39 omega   31.00   58.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000  179.4548 27

 40 omega   35.00   62.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   77.0000  -86.9474 27

 41 omega   83.00  110.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   77.0000  -86.9474 27

 42 omega   41.00   71.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   60.0000   93.2028 30

 43 omega   33.00   61.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   77.0000  161.2105 28

 44 omega   36.00   63.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   75.0000 -106.7395 27

 45 omega  103.00  130.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   60.0000   93.2028 27

 46 omega   34.00   59.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   76.0000   -0.6424 25

 47 omega   38.00   65.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   67.0000  135.9502 27

 48 omega   35.00   60.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   74.0000 -165.1211 25

 49 omega   35.00   67.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   76.0000  -35.1715 32

 50 omega   79.00  135.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   75.0000 -162.1954 56

 51 omega   39.00   65.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   75.0000 -162.1954 26

 52 omega   45.00   71.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   67.0000 -119.2518 26

 53 omega   40.00   68.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   70.0000   39.6074 28

 54 omega   43.00   75.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   67.0000  147.4887 32

 55 omega   44.00   70.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   63.0000  113.5439 26

 56 omega   41.00   70.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   76.0000 -159.5963 29

 57 omega    1.00   81.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000  -78.0000   75.3884 80

 58 omega   47.00   74.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   65.0000   14.5712 27

 59 omega   53.00  108.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   58.0000  176.5176 55

 60 omega   52.00   82.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   63.0000  113.9986 30

 61 omega   45.00   71.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   75.0000 -162.0037 26

 62 omega   57.00  108.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   67.0000  149.2596 51

 63 omega   46.00   72.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   76.0000  114.0154 26

 64 omega   42.00  106.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000  -80.0000 -142.4328 64

 65 omega   50.00  135.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   67.0000  -72.8967 85

 66 omega   52.00  141.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   61.0000   66.2594 89

 67 omega   48.00   74.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   71.0000 -106.5558 26

 68 omega   47.00   80.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   73.0000  -23.5875 33

 69 omega   56.00   83.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   62.0000   10.7507 27

 70 omega   54.00   79.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   69.0000 -138.8013 25

 71 omega   10.00   82.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000  -80.0000  -23.5065 72

 72 omega   49.00   76.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000  -77.0000  -66.2989 27

 73 omega   73.00  103.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   54.0000   28.1209 30

 74 omega   56.00   82.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   77.0000 -119.1937 26

 75 omega   63.00   91.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   65.0000 -159.4726 28

 76 omega   57.00  138.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   75.0000  102.9869 81

 77 omega   56.00   85.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   77.0000  -62.0276 29

 78 omega   58.00   84.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   74.0000   -4.8345 26

 79 omega   70.00  153.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   58.0000   17.3108 83

 80 omega   71.00  139.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -       94.0000   46.0000  178.7875 68

 81 omega   72.00  108.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -       94.0000   64.0000 -108.0202 36

 82 omega   75.00  110.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -       98.0000   66.0000   65.8869 35

 83 omega   76.00  102.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      102.0000   71.0000  -62.5529 26

 84 omega   81.00  118.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      102.0000   56.0000    8.4613 37

 85 omega   83.00  110.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -77.0000 -180.0000 27

 86 omega   38.00  106.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -79.0000   30.2842 68

 87 omega   84.00  111.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -79.0000  -62.3203 27

 88 omega   76.00  125.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000  163.0640 49

 89 omega   47.00   74.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000  163.0640 27

 90 omega   84.00  154.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000 -120.0000 70

 91 omega   93.00  150.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   50.0000   30.0000 57

 92 omega   85.00  112.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000    0.0000 27

 93 omega  116.00  177.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -30.0000 61

 94 omega   78.00  104.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -30.0000 26

 95 omega   85.00  112.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000 -180.0000 27

 96 omega   78.00  104.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -150.0000 26

 97 omega   85.00  174.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000   30.0000 89

 98 omega  153.00  178.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -90.0000 25

 99 omega   79.00  104.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -90.0000 25

100 omega  153.00  178.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   90.0000 25

101 omega   78.00  104.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   90.0000 26

102 omega   79.00  176.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -120.0000 97

103 omega  117.00  174.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  120.0000 57

104 omega   78.00  104.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  120.0000 26

105 omega   80.00  107.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   30.0000 27

106 omega   79.00  177.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -60.0000 98

107 omega   85.00  174.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  -90.0000 89

108 omega  125.00  171.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000    0.0000 46

109 omega   78.00  105.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000    0.0000 27

110 omega   90.00  117.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000 -120.0000 27

111 omega  147.00  177.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   60.0000 30

112 omega   84.00  109.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000  -29.0823 25

113 omega   78.00  104.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   60.0000 26

114 omega   49.00   75.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000  -29.0823 26

115 omega   79.00  163.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -180.0000 84

116 omega   85.00  173.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000   90.0000 88

117 omega   37.00  130.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -79.0000 -105.9044 93

118 omega   82.00  177.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000   60.0000 95

119 omega   78.00  172.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  150.0000 94

120 omega   86.00  134.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  -30.0000 48

121 omega   41.00  138.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000   88.5149 97

122 omega  117.00  175.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000 -150.0000 58

123 omega   86.00  111.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000 -150.0000 25

124 omega   86.00  133.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  120.0000 47

;
_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      -0.0214934000
_diffrn_orient_matrix_UB_12      0.0384684000
_diffrn_orient_matrix_UB_13      -0.0970589000
_diffrn_orient_matrix_UB_21      -0.0334217000
_diffrn_orient_matrix_UB_22      -0.0998390000
_diffrn_orient_matrix_UB_23      0.0030096000
_diffrn_orient_matrix_UB_31      -0.1382927000
_diffrn_orient_matrix_UB_32      0.0541212000
_diffrn_orient_matrix_UB_33      0.0505430000
_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  0.1702
_diffrn_reflns_av_unetI/netI     0.1426
_diffrn_reflns_laue_measured_fraction_full 0.974
_diffrn_reflns_laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            48943
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        67.564
_diffrn_reflns_theta_max         67.564
_diffrn_reflns_theta_min         4.129
_diffrn_source                   'microfocus X-Ray tube'
_diffrn_source_type              'Agilent SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.300
_exptl_absorpt_correction_T_max  0.811
_exptl_absorpt_correction_T_min  0.623
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.457
_exptl_crystal_description       irregular
_exptl_crystal_F_000             974
_exptl_crystal_size_max          0.127
_exptl_crystal_size_mid          0.094
_exptl_crystal_size_min          0.045
_refine_diff_density_max         1.868
_refine_diff_density_min         -3.895
_refine_diff_density_rms         0.228
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     544
_refine_ls_number_reflns         7677
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.1089
_refine_ls_R_factor_gt           0.0672
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0637P)^2^+8.4041P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1472
_refine_ls_wR_factor_ref         0.1948
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5378
_reflns_number_total             7677
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b00333_si_001.cif
_cod_data_source_block           ba_ms7
_cod_depositor_comments
;

2021-04-15
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C108 H108 N6 P2 Ta2'
_cod_original_formula_weight         1913.84
_cod_original_formula_moiety         'C90 H88 N6 P2 Ta2, 3(C6 H6)'
_cod_original_formula_units_Z            1
_cod_database_code               4343173
_audit_block_refno               1917
_audit_block_usercomment         'MS281, irregular, orange'
_chemical_oxdiff_formula         'C108 H106 N6 P2 Ta2 '
_chemical_oxdiff_usercomment     'MS281, irregular, orange'
_shelx_estimated_absorpt_t_max   0.619
_shelx_estimated_absorpt_t_min   0.619
_reflns_odcompleteness_completeness 98.36
_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. Restrained distances
 C81-C82 \\sim C82-C83 \\sim C81-C83_$1
 with sigma of 0.01
 C83_$1-C82 \\sim C81-C83 \\sim C82-C81_$1
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 N1, C2, C7
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N2, C22
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N3, C38
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C81, C82, C83
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Ternary CH refined with riding coordinates:
 C7(H7)
4.b Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B)
4.c 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), C33(H33), C34(H34),
  C35(H35), C36(H36), C39(H39), C41(H41), C43(H43), C51(H51), C52(H52),
 C53(H53), C54(H54), C55(H55), C56(H56), C81(H81), C82(H82), C83(H83)
4.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C29(H29A,H29B,H29C), C30(H30A,H30B,
 H30C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C)
;
_shelx_res_checksum              11035
_olex2_submission_special_instructions 'No special instructions were received'
_cell_oxdiff_length_a            12.0019(6)
_cell_oxdiff_length_b            13.7239(7)
_cell_oxdiff_length_c            15.1796(9)
_cell_oxdiff_angle_alpha         77.885(5)
_cell_oxdiff_angle_beta          68.693(5)
_cell_oxdiff_angle_gamma         70.190(5)
_cell_oxdiff_volume              2180.8(2)
_cell_oxdiff_measurement_reflns_used 5944