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_4338080
_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         'C30 H46 Cl2 N3 P Si3 Ti'
_chemical_formula_sum            'C34 H50 Cl2 N3 P Si3 Ti'
_chemical_formula_weight         734.81
_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_jb10
_audit_creation_date
;
'Mon Jun 03 16:24:23 2013'
;
_audit_update_record             'Mon Jun  3 16:47:38 CEST 2013'
_cell_angle_alpha                107.384(3)
_cell_angle_beta                 101.288(4)
_cell_angle_gamma                92.178(3)
_cell_formula_units_Z            2
_cell_length_a                   9.7694(5)
_cell_length_b                   11.3071(4)
_cell_length_c                   18.5921(7)
_cell_measurement_reflns_used    12569
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      70.6030
_cell_measurement_theta_min      4.1000
_cell_volume                     1911.79(15)
_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(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9621
_diffrn_detector_type            'Agilent EOS'
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_details
;
  1 omega  -69.00  -34.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -38.0000    0.0000 35

  2 omega   17.00   67.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   77.0000  -90.0000 50

  3 omega  -23.00   16.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   77.0000  -90.0000 39

  4 omega   -8.00   22.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000  150.0000 30

  5 omega  -23.00   17.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -38.0000    0.0000 40

  6 omega   40.00   69.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000  150.0000 29

  7 omega   32.00   63.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000   90.0000 31

  8 omega  -53.00   43.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       14.0000  -75.0000  117.2096 96

  9 omega   -2.00   26.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       22.0000   78.0000   83.1849 28

 10 omega    4.00   39.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       30.0000   80.0000 -112.3803 35

 11 omega    4.00   31.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       34.0000   79.0000  -39.4395 27

 12 omega    7.00   32.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       38.0000   79.0000  -17.8224 25

 13 omega    8.00   33.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       38.0000   78.0000  120.0619 25

 14 omega   10.00   38.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   80.0000  155.1364 28

 15 omega   11.00   36.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   79.0000  -64.0103 25

 16 omega   11.00   36.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   78.0000   40.7636 25

 17 omega   76.00  103.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   77.0000   95.4522 27

 18 omega   18.00   45.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   77.0000   41.4302 27

 19 omega   19.00   45.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   77.0000  -74.4504 26

 20 omega   15.00   40.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   79.0000 -142.2404 25

 21 omega   22.00   49.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   77.0000   95.4522 27

 22 omega   15.00   40.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   79.0000  172.0256 25

 23 omega   18.00   43.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   80.0000  125.9457 25

 24 omega   19.00   44.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   80.0000  173.0660 25

 25 omega   20.00   51.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   77.0000   73.3539 31

 26 omega   19.00   44.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   78.0000   -0.3040 25

 27 omega   19.00   74.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -57.0000 -180.0000 55

 28 omega   42.00   91.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   66.0000   34.9798 49

 29 omega   28.00   63.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000 -122.1106 35

 30 omega   30.00   57.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   73.0000   -6.3764 27

 31 omega  103.00  128.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000 -122.1106 25

 32 omega   29.00   56.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   75.0000 -168.2927 27

 33 omega   44.00   71.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   71.0000  150.1120 27

 34 omega   37.00   64.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   60.0000   94.1154 27

 35 omega  103.00  128.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   75.0000 -168.2927 25

 36 omega   30.00   57.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   76.0000  134.9114 27

 37 omega  -13.00   88.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000  -80.0000  126.6032 101

 38 omega  104.00  129.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   64.0000  102.0125 25

 39 omega   39.00   67.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   64.0000  102.0125 28

 40 omega   47.00   99.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   66.0000  -71.3381 52

 41 omega   35.00   63.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   73.0000   12.8172 28

 42 omega   36.00   64.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   71.0000  -51.9248 28

 43 omega  103.00  130.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   66.0000  -71.3381 27

 44 omega   45.00  131.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   62.0000  164.3125 86

 45 omega   40.00   97.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   72.0000  112.6815 57

 46 omega   56.00   83.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   65.0000 -159.3810 27

 47 omega   53.00   81.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   67.0000  -49.1856 28

 48 omega   43.00   70.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   72.0000  171.8904 27

 49 omega   45.00   80.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   69.0000  -20.2104 35

 50 omega   -1.00  102.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000  -80.0000  -71.3010 103

 51 omega   47.00   95.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   48.0000  -82.5432 48

 52 omega   44.00   71.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   70.0000   98.8126 27

 53 omega  112.00  137.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   76.0000  151.3657 25

 54 omega   41.00   68.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   76.0000  151.3657 27

 55 omega   45.00   74.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   77.0000  169.9173 29

 56 omega   55.00   86.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   67.0000    3.6470 31

 57 omega   47.00   74.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   72.0000  -98.2494 27

 58 omega   62.00   89.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   58.0000 -160.8031 27

 59 omega   48.00  100.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   77.0000   90.7044 52

 60 omega   48.00  148.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   77.0000   27.1330 100

 61 omega   62.00   92.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   63.0000   12.7027 30

 62 omega   55.00   85.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   72.0000  -74.5725 30

 63 omega   53.00  146.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   76.0000  -34.9668 93

 64 omega   63.00   90.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   64.0000   16.6470 27

 65 omega   74.00  153.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   59.0000 -140.8075 79

 66 omega   57.00   84.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   76.0000 -163.5526 27

 67 omega   17.00   98.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000  -79.0000   21.1608 81

 68 omega   67.00  143.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   68.0000  112.2466 76

 69 omega   72.00  103.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       94.0000   51.0000   69.8357 31

 70 omega   71.00  113.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       94.0000   65.0000  -79.3435 42

 71 omega   71.00  166.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       98.0000   74.0000    3.9167 95

 72 omega   72.00  125.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000  -27.5151 53

 73 omega   43.00  115.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -78.0000  -51.8333 72

 74 omega   71.00   99.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -77.0000   30.0000 28

 75 omega   86.00  113.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -30.0000 27

 76 omega   82.00  110.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000   60.0000 28

 77 omega   83.00  108.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000 -150.0000 25

 78 omega   95.00  132.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   50.0000 -120.0000 37

 79 omega   87.00  171.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000    0.0000 84

 80 omega   86.00  175.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000 -120.0000 89

 81 omega   37.00  106.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000   73.7111 69

 82 omega   86.00  114.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000 -150.0000 28

 83 omega   86.00  111.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000 -180.0000 25

 84 omega   85.00  113.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000   60.0000 28

 85 omega   79.00  107.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  120.0000 28

 86 omega   83.00  177.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000  -90.0000 94

 87 omega   83.00  108.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000 -180.0000 25

 88 omega  119.00  177.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -60.0000 58

 89 omega  110.00  177.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   30.0000 67

 90 omega   78.00  105.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   30.0000 27

 91 omega   80.00  107.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000    0.0000 27

 92 omega   78.00  116.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -90.0000 38

 93 omega  117.00  174.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  -30.0000 57

 94 omega   78.00  105.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -60.0000 27

 95 omega   85.00  115.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  -30.0000 30

 96 omega   78.00  105.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   90.0000 27

 97 omega  131.00  158.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -150.0000 27

 98 omega   78.00  105.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -150.0000 27

 99 omega  119.00  176.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   60.0000 57

100 omega   79.00  105.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   60.0000 26

101 omega   38.00  100.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000 -155.4410 62

102 omega   85.00  131.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  -60.0000 46

103 omega   78.00  104.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -120.0000 26

104 omega  110.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  150.0000 68

105 omega   85.00  173.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000   90.0000 88

106 omega   78.00  108.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  150.0000 30

107 omega   85.00  172.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  120.0000 87

108 omega  108.00  177.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -180.0000 69

109 omega   78.00  105.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -180.0000 27

110 omega   85.00  112.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  150.0000 27

111 omega   95.00  122.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   50.0000   90.0000 27

112 omega   95.00  122.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   50.0000  150.0000 27

113 omega  153.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   75.0000  -98.0593 25

114 omega   37.00  139.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000  129.0409 102

115 omega   80.00  107.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   75.0000  -98.0593 27

116 omega   97.00  138.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000  -12.9855 41

117 omega   70.00  137.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -79.0000 -119.5155 67

118 phi      0.00  120.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
 -40.0000    0.0000    0.0000     -     120

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

120 omega  -56.00   43.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       14.0000  -75.0000  117.2096 99

121 omega    0.00   90.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       22.0000   62.0000   53.5973 90

122 omega   -5.00   49.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       26.0000   78.0000  -44.9288 54

123 omega   -3.00   96.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       26.0000   75.0000   83.8928 99

124 omega   -4.00   96.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       26.0000   77.0000 -149.6064 100

125 omega   45.00  138.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   69.0000  -20.2104 93

126 omega   52.00  142.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   62.0000  125.5822 90

;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Agilent SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w and \p scans'
_diffrn_measurement_specimen_support 'polyimid foil'
_diffrn_orient_matrix_UB_11      0.1229972000
_diffrn_orient_matrix_UB_12      -0.0202210000
_diffrn_orient_matrix_UB_13      -0.0415993000
_diffrn_orient_matrix_UB_21      0.0036884000
_diffrn_orient_matrix_UB_22      0.1358278000
_diffrn_orient_matrix_UB_23      -0.0009910000
_diffrn_orient_matrix_UB_31      0.1048505000
_diffrn_orient_matrix_UB_32      0.0417587000
_diffrn_orient_matrix_UB_33      0.0786164000
_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  0.0516
_diffrn_reflns_av_unetI/netI     0.0337
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            42442
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.670
_diffrn_reflns_theta_min         4.112
_diffrn_source                   'microfocus X-Ray tube'
_diffrn_source_type              'Agilent SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.684
_exptl_absorpt_correction_T_max  0.901
_exptl_absorpt_correction_T_min  0.514
_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    1.276
_exptl_crystal_description       plate
_exptl_crystal_F_000             776
_exptl_crystal_size_max          0.1870
_exptl_crystal_size_mid          0.0976
_exptl_crystal_size_min          0.0222
_refine_diff_density_max         0.526
_refine_diff_density_min         -0.359
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     374
_refine_ls_number_reflns         7095
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0532
_refine_ls_R_factor_gt           0.0479
_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^)+(0.0481P)^2^+1.8206P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1088
_refine_ls_wR_factor_ref         0.1116
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6483
_reflns_number_total             7095
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic500163c_si_001.cif
_cod_data_source_block           ba_jb10_sq
_cod_depositor_comments
'Adding full bibliography for 4338072--4338082.cif.'
_cod_original_cell_volume        1911.78(14)
_cod_database_code               4338080
_audit_block_refno               1771
_audit_block_usercomment         'jb112Ti, plate, 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)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C9(H9), C15(H15), C16(H16), C17(H17), C18(H18),
 C24(H24), C25(H25), C26(H26), C27(H27)
2.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C19(H19A,H19B,
 H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C28(H28A,H28B,H28C), C29(H29A,
 H29B,H29C), C30(H30A,H30B,H30C)
;
_shelx_estimated_absorpt_t_max   0.652
_shelx_estimated_absorpt_t_min   0.652
_shelx_fab_checksum              63410
_cell_oxdiff_length_a            9.7694(5)
_cell_oxdiff_length_b            11.3071(4)
_cell_oxdiff_length_c            18.5921(7)
_cell_oxdiff_angle_alpha         107.384(3)
_cell_oxdiff_angle_beta          101.288(4)
_cell_oxdiff_angle_gamma         92.178(3)
_cell_oxdiff_volume              1911.78(13)
_cell_oxdiff_measurement_reflns_used 12569
_reflns_odcompleteness_completeness 98.11
_reflns_odcompleteness_theta     66.97
_reflns_odcompleteness_iscentric 1