Phospha Derivatives of Tris(2-aminoethyl)amine (tren) and Tris(3-aminopropyl)amine (trpn): Synthesis and Complexation Studies with Group 4 Metals
Sietzen, Malte; Batke, Sonja; Merz, Lukas; Wadepohl, Hubert; Ballmann, Joachim; Organometallics 34 (2015) 1118–; doi:10.1021/acs.organomet.5b00065

data_1518840
_publ_section_title
;
 Phospha Derivatives of Tris(2-aminoethyl)amine (tren) and
 Tris(3-aminopropyl)amine (trpn): Synthesis and Complexation Studies with
 Group 4 Metals
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              1118
_journal_paper_doi               10.1021/acs.organomet.5b00065
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C29 H39 N4 P Ti'
_chemical_formula_sum            'C29 H39 N4 P Ti'
_chemical_formula_weight         522.51
_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   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_block_code                ba_jb9
_audit_creation_date
;
'Tue Apr 23 12:03:56 2013'
;
_audit_update_record             'Tue Apr 23 12:08:07 CEST 2013'
_cell_angle_alpha                81.9190(17)
_cell_angle_beta                 81.3926(18)
_cell_angle_gamma                70.9432(19)
_cell_formula_units_Z            2
_cell_length_a                   8.48075(19)
_cell_length_b                   12.3163(2)
_cell_length_c                   13.7435(3)
_cell_measurement_reflns_used    35299
_cell_measurement_temperature    110(1)
_cell_measurement_theta_max      70.5970
_cell_measurement_theta_min      3.8120
_cell_volume                     1335.10(5)
_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 0.973
_diffrn_measurement_details
;
  1 omega  -69.00  -21.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000 -180.0000 48

  2 omega  -11.00   20.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000 -180.0000 31

  3 omega  -69.00   21.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -19.0000   60.0000 90

  4 omega   34.00   65.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       -3.5000   57.0000 -150.0000 31

  5 omega   18.00   65.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       -3.5000   57.0000  -30.0000 47

  6 omega  -17.00   10.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       -3.5000   57.0000  -30.0000 27

  7 omega  -22.00   31.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       -3.5000   57.0000 -150.0000 53

  8 omega   -9.00   40.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0000   80.0000  125.2567 49

  9 omega    7.00   32.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       38.0000   78.0000   65.7161 25

 10 omega    6.00   31.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       38.0000   80.0000 -145.1327 25

 11 omega   10.00   35.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   80.0000  -24.8646 25

 12 omega   11.00   36.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   79.0000  126.5212 25

 13 omega   15.00   42.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   77.0000  172.6813 27

 14 omega   11.00   36.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   79.0000  -72.8887 25

 15 omega   15.00   40.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   78.0000 -166.3414 25

 16 omega   18.00   45.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   77.0000   77.1336 27

 17 omega   15.00   40.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   79.0000 -121.2502 25

 18 omega   24.00   49.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   77.0000  -38.6373 25

 19 omega   19.00   44.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   78.0000   90.0959 25

 20 omega   19.00   46.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   78.0000  123.4662 27

 21 omega   20.00   47.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   77.0000   19.9761 27

 22 omega   20.00   55.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   77.0000  160.9291 35

 23 omega   19.00   48.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -77.0000 -180.0000 29

 24 omega   30.00   56.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   73.0000   44.9127 26

 25 omega  103.00  128.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   75.0000  -19.9968 25

 26 omega   30.00   59.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   75.0000  140.8980 29

 27 omega   29.00   56.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   76.0000  -68.4981 27

 28 omega   29.00   60.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000 -167.7320 31

 29 omega   30.00   55.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   75.0000  -19.9968 25

 30 omega   40.00   67.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   64.0000 -136.2514 27

 31 omega   78.00  105.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   64.0000 -136.2514 27

 32 omega   35.00   62.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000  -52.8667 27

 33 omega   84.00  132.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   75.0000   94.1406 48

 34 omega   38.00   63.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   76.0000 -176.8047 25

 35 omega   34.00   68.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   75.0000   94.1406 34

 36 omega   33.00   60.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   77.0000  154.5957 27

 37 omega  110.00  135.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   71.0000   -0.1302 25

 38 omega   40.00   67.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   71.0000   -0.1302 27

 39 omega   36.00   63.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   77.0000  -74.4438 27

 40 omega   88.00  132.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   77.0000  -74.4438 44

 41 omega   46.00   74.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   58.0000  157.9099 28

 42 omega   45.00   70.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   51.0000 -130.5233 25

 43 omega   57.00  123.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   62.0000   27.9191 66

 44 omega   -4.00   82.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000  -78.0000 -111.2104 86

 45 omega   38.00   72.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   73.0000   63.7034 34

 46 omega   -5.00   95.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000  -80.0000    7.4365 100

 47 omega   48.00  112.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   64.0000   57.3955 64

 48 omega   49.00   75.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   56.0000 -142.7659 26

 49 omega  114.00  139.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   70.0000  -22.2994 25

 50 omega   45.00   73.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   70.0000  -22.2994 28

 51 omega  115.00  140.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   77.0000  -58.3987 25

 52 omega   40.00   67.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   77.0000  -58.3987 27

 53 omega   42.00   76.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   75.0000  153.2555 34

 54 omega   48.00  138.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   61.0000 -113.8888 90

 55 omega   71.00   98.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   45.0000   77.0672 27

 56 omega   87.00  121.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   56.0000   11.4911 34

 57 omega   54.00   82.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   56.0000   11.4911 28

 58 omega   50.00  121.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   75.0000  138.5129 71

 59 omega   57.00  137.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   51.0000 -145.5410 80

 60 omega   57.00   90.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   50.0000   51.0027 33

 61 omega   59.00   86.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   46.0000  -63.5300 27

 62 omega   56.00   91.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   71.0000  -70.2765 35

 63 omega   16.00   96.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000  -79.0000  109.6150 80

 64 omega   62.00   96.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   74.0000  109.0048 34

 65 omega   68.00  103.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   45.0000   92.1766 35

 66 omega   74.00  101.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       94.0000   43.0000  -82.4576 27

 67 omega   82.00  171.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      102.0000   58.0000  -19.7429 89

 68 omega   86.00  111.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000 -180.0000 25

 69 omega   48.00  133.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000  121.3772 85

 70 omega   83.00  114.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000   60.0000 31

 71 omega   84.00  112.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000    0.0000 28

 72 omega  115.00  153.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000 -150.0000 38

 73 omega   83.00  112.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000 -150.0000 29

 74 omega   72.00  139.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -79.0000  -73.0175 67

 75 omega   85.00  115.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000   60.0000 30

 76 omega   85.00  146.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000 -150.0000 61

 77 omega   37.00   64.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -79.0000  -73.0175 27

 78 omega   82.00  109.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000 -180.0000 27

 79 omega   46.00   92.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -77.0000 -180.0000 46

 80 omega   37.00  112.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -79.0000 -134.8696 75

 81 omega   86.00  113.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  150.0000 27

 82 omega   83.00  110.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000 -120.0000 27

 83 omega   79.00  104.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -90.0000 25

 84 omega  133.00  161.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   60.0000 28

 85 omega   78.00  105.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   60.0000 27

 86 omega   79.00  106.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000    0.0000 27

 87 omega  112.00  176.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   30.0000 64

 88 omega   80.00  107.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   30.0000 27

 89 omega  111.00  178.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -60.0000 67

 90 omega   78.00  104.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -60.0000 26

 91 omega  150.00  177.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -120.0000 27

 92 omega  110.00  149.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -120.0000 39

 93 omega   78.00  104.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -120.0000 26

 94 omega  140.00  178.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -180.0000 38

 95 omega   78.00  104.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -180.0000 26

 96 omega   78.00  104.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -30.0000 26

 97 omega  140.00  176.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   90.0000 36

 98 omega   84.00  111.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   90.0000 27

 99 omega   85.00  175.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  -90.0000 90

100 omega   71.00  117.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -79.0000   52.4021 46

101 omega   79.00  177.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -150.0000 98

102 omega  111.00  177.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  150.0000 66

103 omega   79.00  104.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  150.0000 25

104 omega   86.00  170.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000    0.0000 84

105 omega   85.00  152.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000   90.0000 67

106 omega   94.00  121.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   49.0000  -30.0000 27

107 omega   67.00  103.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000    3.8790 36

108 omega   92.00  141.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   50.0000   90.0000 49

109 omega   79.00  175.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  120.0000 96

110 omega   85.00  122.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000   30.0000 37

111 omega   85.00  115.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  -60.0000 30

112 omega   87.00  119.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000   30.0000 32

113 omega  -21.00   69.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000  -30.0000 90

114 omega  -25.00   65.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       -3.5000   57.0000 -180.0000 90

115 omega   -8.00   92.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       22.0000   77.0000 -132.2760 100

116 omega   -5.00   91.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       22.0000   71.0000 -178.2976 96

117 omega    3.00   97.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       26.0000   46.0000  114.6819 94

118 omega   11.00   47.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   79.0000  126.5212 36

119 omega   15.00   49.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   78.0000 -166.3414 34

120 omega   19.00   49.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   78.0000  123.4662 30

121 omega   19.00   49.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   78.0000   90.0959 30

122 omega  -19.00  127.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000    0.0000  240.0000 146

123 omega  -19.00  127.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000    0.0000    0.0000 146

124 omega  -19.00  127.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000    0.0000  120.0000 146

125 omega   29.00  128.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   76.0000  -68.4981 99

126 omega   28.00  128.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000 -167.7320 100

127 omega   30.00  127.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   73.0000   44.9127 97

128 omega   28.00  128.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000  -52.8667 100

129 omega   29.00  128.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   75.0000  140.8980 99

130 omega   32.00  132.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   77.0000  154.5957 100

131 omega   33.00  132.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   76.0000 -176.8047 99

132 omega   33.00  132.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   75.0000   94.1406 99

133 omega   44.00  134.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   62.0000   27.9191 90

134 omega   38.00  135.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   73.0000   63.7034 97

135 omega   45.00  135.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   58.0000  157.9099 90

136 omega   39.00  135.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   71.0000   -0.1302 96

137 omega   36.00  136.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   77.0000  -74.4438 100

138 omega   -4.00   97.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000  -78.0000 -111.2104 101

139 omega   44.00  136.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   51.0000 -130.5233 92

140 omega   -5.00   98.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000  -80.0000    7.4365 103

141 omega   41.00  140.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   75.0000  153.2555 99

142 omega   49.00  139.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   56.0000 -142.7659 90

143 omega   48.00  138.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   61.0000 -113.8888 90

144 omega   44.00  139.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   70.0000  -22.2994 95

145 omega   40.00  140.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   77.0000  -58.3987 100

146 omega   47.00  137.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   64.0000   57.3955 90

147 omega   47.00  147.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   33.0000 -154.1062 100

148 omega   51.00  145.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   45.0000   77.0672 94

149 omega   53.00  143.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   56.0000   11.4911 90

150 omega   56.00  148.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   50.0000   51.0027 92

151 omega   49.00  148.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   75.0000  138.5129 99

152 omega   56.00  148.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   51.0000 -145.5410 92

153 omega   15.00  117.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000  -79.0000  109.6150 102

154 omega   86.00  168.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   50.0000   60.0000 82

155 omega   78.00  178.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -150.0000 100

156 omega   36.00   93.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -38.0000  -30.0000 57

157 omega   82.00  178.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000  -60.0000 96

158 omega   35.00   94.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000  150.0000 59

159 omega   37.00  139.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -79.0000 -134.8696 102

160 omega   82.00  178.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000  150.0000 96

161 omega   37.00  139.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -79.0000   52.4021 102

162 omega   35.00   94.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000 -150.0000 59

163 omega   38.00  104.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -50.0000  150.0000 66

164 omega   35.00   94.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000    0.0000 59

165 omega   36.00   93.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -38.0000  -90.0000 57

166 omega   35.00   94.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000   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      -0.1612284000
_diffrn_orient_matrix_UB_12      -0.0350800000
_diffrn_orient_matrix_UB_13      0.0163162000
_diffrn_orient_matrix_UB_21      0.0874701000
_diffrn_orient_matrix_UB_22      -0.1084612000
_diffrn_orient_matrix_UB_23      0.0660948000
_diffrn_orient_matrix_UB_31      -0.0612362000
_diffrn_orient_matrix_UB_32      0.0684741000
_diffrn_orient_matrix_UB_33      0.0913413000
_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  0.0375
_diffrn_reflns_av_unetI/netI     0.0160
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            56268
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.809
_diffrn_reflns_theta_min         3.816
_diffrn_source                   'microfocus X-Ray tube'
_diffrn_source_type              'Agilent SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.461
_exptl_absorpt_correction_T_max  0.800
_exptl_absorpt_correction_T_min  0.661
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.300
_exptl_crystal_description       irregular
_exptl_crystal_F_000             556
_exptl_crystal_size_max          0.1698
_exptl_crystal_size_mid          0.0887
_exptl_crystal_size_min          0.0821
_refine_diff_density_max         0.263
_refine_diff_density_min         -0.293
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     419
_refine_ls_number_reflns         5001
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0265
_refine_ls_R_factor_gt           0.0260
_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^)+(0.0315P)^2^+0.7090P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0666
_refine_ls_wR_factor_ref         0.0669
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4905
_reflns_number_total             5001
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00065_si_002.cif
_cod_data_source_block           ba_jb9
_cod_depositor_comments
'Adding full bibliography for 1518840--1518841.cif.'
_cod_original_cell_volume        1335.09(5)
_cod_database_code               1518840
_audit_block_refno               1757
_audit_block_usercomment         'jb118, irregular, 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 Idealised Me refined as rotating group with stretchable bonds:
 C28(H28A,H28B,H28C), C29(H29A,H29B,H29C)
;
_shelx_estimated_absorpt_t_max   0.723
_shelx_estimated_absorpt_t_min   0.723
_shelx_hkl_checksum              54652
_cell_oxdiff_length_a            8.48075(19)
_cell_oxdiff_length_b            12.3163(2)
_cell_oxdiff_length_c            13.7435(3)
_cell_oxdiff_angle_alpha         81.9190(17)
_cell_oxdiff_angle_beta          81.3926(18)
_cell_oxdiff_angle_gamma         70.9432(19)
_cell_oxdiff_volume              1335.09(5)
_cell_oxdiff_measurement_reflns_used 35299
_reflns_odcompleteness_completeness 98.36
_reflns_odcompleteness_theta     66.97
_reflns_odcompleteness_iscentric 1