A Tripodal Benzylene-Linked Trisamidophosphine Ligand Scaffold: Synthesis and Coordination Chemistry with Group(IV) Metals.
Batke, Sonja; Sietzen, Malte; Wadepohl, Hubert; Ballmann, Joachim; Inorganic chemistry 53 (2014) 4144–4153; doi:10.1021/ic500163c

data_4338082
_publ_section_title
;
 A Tripodal Benzylene-Linked Trisamidophosphine Ligand Scaffold: Synthesis
 and Coordination Chemistry with Group(IV) Metals.
;
_journal_issue                   8
_journal_name_full               'Inorganic chemistry'
_journal_page_first              4144
_journal_page_last               4153
_journal_paper_doi               10.1021/ic500163c
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'C48 H54 Cl2 N6 P2 Si2 Ti3, 3(C6 D6)'
_chemical_formula_sum            'C66 H54 Cl2 D18 N6 P2 Si2 Ti3'
_chemical_formula_weight         1300.12
_chemical_properties_physical    air-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_block_code                ba_sb3
_audit_creation_date
;
'Fri Jul 19 13:38:38 2013'
;
_audit_update_record             'Fri Jul 19 13:44:40 CEST 2013'
_cell_angle_alpha                74.457(2)
_cell_angle_beta                 66.589(3)
_cell_angle_gamma                68.283(2)
_cell_formula_units_Z            2
_cell_length_a                   15.4536(4)
_cell_length_b                   15.5687(4)
_cell_length_c                   15.9472(4)
_cell_measurement_reflns_used    16332
_cell_measurement_temperature    110(1)
_cell_measurement_theta_max      70.4950
_cell_measurement_theta_min      4.6430
_cell_volume                     3237.94(16)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
'encif (Wadepohl, 2009-13); encifer 1.4 (CCDC, 2011)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SUPERFLIP (Palatinus, 2007-2009)'
_diffrn_ambient_temperature      110(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9621
_diffrn_detector_type            'Agilent EOS'
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_details
;
  1 omega  -71.00   26.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -38.0000 -120.0000 97

  2 omega  -23.00   19.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000 -180.0000 42

  3 omega  -38.00   62.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       -3.5000   25.0000    0.0000 100

  4 omega  -25.00   52.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       -3.5000   57.0000   60.0000 77

  5 omega  -50.00  -16.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       -3.5000  -57.0000    0.0000 34

  6 omega  -15.00   31.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       14.0000   78.0000   97.3631 46

  7 omega    7.00   32.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       38.0000   79.0000   88.6819 25

  8 omega    6.00   31.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       38.0000   80.0000  176.2971 25

  9 omega    7.00   37.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       38.0000   78.0000  -12.9881 30

 10 omega   11.00   36.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   79.0000   35.9206 25

 11 omega   11.00   36.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   79.0000  -68.2381 25

 12 omega   15.00   40.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   78.0000  -98.6724 25

 13 omega   15.00   40.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   79.0000  -29.5988 25

 14 omega   15.00   40.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   79.0000 -163.6977 25

 15 omega   15.00   40.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   79.0000  118.8836 25

 16 omega   20.00   82.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   77.0000   94.4208 62

 17 omega   19.00   44.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   78.0000    2.4505 25

 18 omega   18.00   43.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   80.0000   53.5385 25

 19 omega   19.00   44.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   78.0000 -143.6156 25

 20 omega   18.00   43.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   80.0000  138.3107 25

 21 omega   18.00   43.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   80.0000  115.5852 25

 22 omega   20.00   45.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   78.0000  156.6238 25

 23 omega   19.00   44.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   79.0000  -79.5078 25

 24 omega   18.00   43.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   80.0000  -14.8156 25

 25 omega   30.00   66.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -57.0000   30.0000 36

 26 omega   28.00   55.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000   74.6016 27

 27 omega   28.00   55.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000    0.1738 27

 28 omega   85.00  114.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000    0.1738 29

 29 omega   31.00   56.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   74.0000  -75.8608 25

 30 omega   31.00   57.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   72.0000 -177.1804 26

 31 omega  103.00  128.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   75.0000  126.4133 25

 32 omega   30.00   57.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   73.0000  -10.2784 27

 33 omega   30.00   57.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   75.0000  -91.7997 27

 34 omega   35.00   61.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000  144.2247 26

 35 omega   42.00   69.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   69.0000 -167.5632 27

 36 omega   29.00   56.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   75.0000  126.4133 27

 37 omega   44.00  107.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   72.0000  173.4690 63

 38 omega   32.00   57.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   77.0000   48.2003 25

 39 omega   99.00  125.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   71.0000  -45.1898 26

 40 omega   36.00   62.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   71.0000  -45.1898 26

 41 omega   32.00   58.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   77.0000 -143.2247 26

 42 omega   48.00  135.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   57.0000 -147.9445 87

 43 omega   38.00   64.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   75.0000 -142.7145 26

 44 omega   38.00   71.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   76.0000  159.8431 33

 45 omega   38.00   64.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   73.0000  120.1495 26

 46 omega   36.00   62.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   77.0000 -119.3573 26

 47 omega   41.00   67.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   76.0000  -34.3785 26

 48 omega   -4.00   95.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000  -80.0000 -147.4158 99

 49 omega   40.00   77.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   71.0000   21.7494 37

 50 omega   36.00   98.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000  -80.0000   31.5852 62

 51 omega   45.00   71.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   76.0000 -133.1539 26

 52 omega   48.00   75.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   71.0000   -2.1351 27

 53 omega  110.00  136.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   76.0000 -133.1539 26

 54 omega   41.00   69.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   76.0000  -86.9771 28

 55 omega   40.00  136.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   77.0000   77.7177 96

 56 omega   47.00   79.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   65.0000  113.7289 32

 57 omega   44.00   76.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   77.0000  119.0018 32

 58 omega   48.00   87.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   74.0000   43.2147 39

 59 omega    4.00  104.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000  -79.0000  -61.0445 100

 60 omega   53.00  137.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   54.0000  -79.7328 84

 61 omega   58.00  102.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   63.0000   19.3746 44

 62 omega   48.00   75.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   70.0000  -75.1824 27

 63 omega   49.00  142.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   72.0000  -43.9507 93

 64 omega   51.00   76.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   73.0000 -158.9851 25

 65 omega   48.00   74.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   77.0000  -29.6847 26

 66 omega   48.00   74.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   77.0000   26.5860 26

 67 omega   53.00   80.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000  -80.0000 -148.1763 27

 68 omega   50.00   77.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   74.0000 -100.1281 27

 69 omega   51.00  124.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   71.0000  155.8378 73

 70 omega   57.00   93.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   69.0000  -13.9080 36

 71 omega   64.00  123.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   60.0000   91.1674 59

 72 omega   55.00  150.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   71.0000  104.9183 95

 73 omega   57.00   83.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   70.0000 -133.5081 26

 74 omega   56.00   86.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   70.0000  -60.6730 30

 75 omega   62.00   88.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   71.0000  -19.0635 26

 76 omega   54.00   81.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000  -80.0000 -178.9943 27

 77 omega   71.00  103.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000  -80.0000   45.5311 32

 78 omega  113.00  151.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   74.0000   60.0150 38

 79 omega   58.00  109.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   74.0000   60.0150 51

 80 omega   62.00   88.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   76.0000   -2.4754 26

 81 omega   76.00  164.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       94.0000   50.0000  -84.3595 88

 82 omega   65.00   91.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       94.0000   77.0000 -151.2207 26

 83 omega   64.00  120.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       94.0000   77.0000   41.8742 56

 84 omega   68.00  102.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       94.0000   71.0000   10.5642 34

 85 omega   73.00  107.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       94.0000   55.0000 -145.6472 34

 86 omega   66.00  131.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       94.0000   73.0000  158.5906 65

 87 omega   80.00  134.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000   56.6286 54

 88 omega   42.00   73.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000   56.6286 31

 89 omega   38.00  104.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000  -35.9052 66

 90 omega   86.00  175.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  150.0000 89

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

 92 omega   86.00  174.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000 -150.0000 88

 93 omega   79.00  106.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -78.0000  -80.9189 27

 94 omega   85.00  121.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000 -120.0000 36

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

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

 97 omega   85.00  175.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  -60.0000 90

 98 omega   85.00  111.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  -90.0000 26

 99 omega   79.00  105.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  120.0000 26

100 omega   78.00  104.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   90.0000 26

101 omega   79.00  104.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -180.0000 25

102 omega   78.00  105.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000    0.0000 27

103 omega   78.00  104.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -60.0000 26

104 omega   78.00  104.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  150.0000 26

105 omega  136.00  167.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -90.0000 31

106 omega   79.00  104.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -90.0000 25

107 omega   85.00  113.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  120.0000 28

108 omega   82.00  177.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   30.0000 95

109 omega   78.00  104.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -150.0000 26

110 omega  108.00  178.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -120.0000 70

111 omega   78.00  104.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -120.0000 26

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

113 omega   86.00  172.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000   90.0000 86

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

115 omega  118.00  173.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   60.0000 55

116 omega   78.00  114.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   60.0000 36

117 omega   75.00  102.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000 -138.0534 27

118 omega   39.00  140.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000   27.3883 101

119 omega  111.00  137.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -79.0000 -117.7914 26

120 omega   79.00  108.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -79.0000 -117.7914 29

121 omega   43.00   94.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000   83.7442 51

122 omega   37.00   63.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -79.0000 -117.7914 26

123 omega   86.00  177.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   49.0000  135.0000 91

124 omega   66.00  109.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000  128.3485 43

125 omega   83.00  112.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000  -90.0000 29

126 omega   86.00  175.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000    0.0000 89

127 omega   38.00  139.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000 -171.0052 101

128 omega   83.00  120.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000  120.0000 37

129 omega   83.00  139.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000  -30.0000 56

130 omega   84.00  143.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000  -60.0000 59

;
_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      0.1083441000
_diffrn_orient_matrix_UB_12      -0.0010731000
_diffrn_orient_matrix_UB_13      -0.0311176000
_diffrn_orient_matrix_UB_21      -0.0249197000
_diffrn_orient_matrix_UB_22      0.0976121000
_diffrn_orient_matrix_UB_23      -0.0562528000
_diffrn_orient_matrix_UB_31      -0.0243436000
_diffrn_orient_matrix_UB_32      0.0452618000
_diffrn_orient_matrix_UB_33      0.0847148000
_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  0.0798
_diffrn_reflns_av_unetI/netI     0.0514
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            81874
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.018
_diffrn_reflns_theta_min         3.652
_diffrn_source                   'microfocus X-Ray tube'
_diffrn_source_type              'Agilent SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.997
_exptl_absorpt_correction_T_max  0.927
_exptl_absorpt_correction_T_min  0.644
_exptl_absorpt_correction_type   analytical
_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)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.334
_exptl_crystal_description       needle
_exptl_crystal_F_000             1336
_exptl_crystal_size_max          0.1253
_exptl_crystal_size_mid          0.0393
_exptl_crystal_size_min          0.0155
_refine_diff_density_max         0.454
_refine_diff_density_min         -0.459
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     736
_refine_ls_number_reflns         12137
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0581
_refine_ls_R_factor_gt           0.0383
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0428P)^2^+0.6935P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0846
_refine_ls_wR_factor_ref         0.0934
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9441
_reflns_number_total             12137
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic500163c_si_001.cif
_cod_data_source_block           ba_sb3
_cod_depositor_comments
'Adding full bibliography for 4338072--4338082.cif.'
_cod_original_cell_volume        3237.94(17)
_cod_database_code               4338082
_audit_block_refno               1813
_audit_block_usercomment         'sb25, needle, red'
_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), C25(H25A,H25B), C26(H26A,H26B),
 C27(H27A,H27B)
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), C30(H30), C31(H31), C32(H32), C33(H33),
  C36(H36), C37(H37), C38(H38), C39(H39), C42(H42), C43(H43), C44(H44),
 C45(H45), C51(D51), C52(D52), C53(D53), C54(D54), C55(D55), C56(D56), C61(D61),
  C62(D62), C63(D63), C64(D64), C65(D65), C66(D66), C71(D71), C72(D72),
 C73(D73), C74(D74), C75(D75), C76(D76)
2.c Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C46(H46A,H46B,
 H46C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C)
;
_shelx_estimated_absorpt_t_max   0.635
_shelx_estimated_absorpt_t_min   0.635
_shelx_res_checksum              46896
_shelxl_version_number           2013-4
_cell_oxdiff_length_a            15.4536(4)
_cell_oxdiff_length_b            15.5687(4)
_cell_oxdiff_length_c            15.9472(4)
_cell_oxdiff_angle_alpha         74.457(2)
_cell_oxdiff_angle_beta          66.589(3)
_cell_oxdiff_angle_gamma         68.282(2)
_cell_oxdiff_volume              3237.94(14)
_cell_oxdiff_measurement_reflns_used 16332
_reflns_odcompleteness_completeness 98.41
_reflns_odcompleteness_theta     66.97
_reflns_odcompleteness_iscentric 1