Cyclometalated titanium and zirconium complexes stabilised by a new silylmethylene-linked tetradentate triamidophosphine.
Sietzen, M.; Federmann, P.; Sonnenschein, C.; Wadepohl, H.; Ballmann, J.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 3013–3023; doi:10.1039/c5dt04561d

data_7037957
_publ_section_title
;
 Cyclometalated titanium and zirconium complexes stabilised by a new
 silylmethylene-linked tetradentate triamidophosphine.
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3013
_journal_page_last               3023
_journal_paper_doi               10.1039/c5dt04561d
_journal_volume                  45
_journal_year                    2016
_chemical_formula_sum            'C39 H63 Li3 N3 O6 P Si3'
_chemical_formula_weight         805.98
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_code                ba_jb7
_audit_creation_date
;
'Wed Mar 20 17:58:34 2013'
;
_audit_creation_method           olex2
_audit_update_record
;
2015-12-14 deposited with the CCDC.
2015-12-28 downloaded from the CCDC.
;
_cell_angle_alpha                106.9639(16)
_cell_angle_beta                 92.2955(16)
_cell_angle_gamma                98.2181(15)
_cell_formula_units_Z            2
_cell_length_a                   12.4277(2)
_cell_length_b                   13.1483(2)
_cell_length_c                   14.8044(3)
_cell_measurement_reflns_used    23109
_cell_measurement_temperature    110(1)
_cell_measurement_theta_max      70.4230
_cell_measurement_theta_min      3.5730
_cell_volume                     2281.51(7)
_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_publication_material
'encif (Wadepohl, 2012); encifer 1.4 (CCDC, 2011)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXT (Sheldrick, 2013)'
_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 0.985
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_details
;
  1 omega  -26.00   25.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   38.0000  -60.0000 51

  2 omega  -58.00  -21.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000  120.0000 37

  3 omega  -15.00   15.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000  120.0000 30

  4 omega  -21.00   69.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000  150.0000 90

  5 omega  -16.00   10.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000   60.0000 26

  6 omega   37.00   62.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000   60.0000 25

  7 omega   41.00   66.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   38.0000  -60.0000 25

  8 omega  -72.00  -30.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       -3.5000  -77.0000   30.0000 42

  9 omega  -26.00   23.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       -3.5000  -77.0000   30.0000 49

 10 omega  -12.00   29.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0000   79.0000    0.9048 41

 11 omega    7.00   43.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       38.0000   79.0000  139.9541 36

 12 omega    7.00   32.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       38.0000   79.0000   74.6890 25

 13 omega   10.00   35.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   80.0000  -43.5485 25

 14 omega   10.00   41.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   80.0000 -126.2892 31

 15 omega   15.00   46.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   78.0000  -90.8289 31

 16 omega   14.00   39.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   80.0000   32.0770 25

 17 omega   17.00   48.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   77.0000 -178.4029 31

 18 omega   15.00   40.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   78.0000   86.6376 25

 19 omega   14.00   39.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   80.0000 -135.5268 25

 20 omega   15.00   44.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   80.0000  -11.3574 29

 21 omega   19.00   44.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   79.0000  -57.5532 25

 22 omega   19.00   44.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   79.0000  133.4643 25

 23 omega   27.00   82.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -77.0000   30.0000 55

 24 omega   93.00  120.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000 -119.5413 27

 25 omega   30.00   57.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   75.0000  108.5268 27

 26 omega   30.00   55.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   76.0000 -171.8181 25

 27 omega   84.00  121.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   74.0000  -18.8040 37

 28 omega   30.00   56.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   74.0000   92.0111 26

 29 omega   30.00   57.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000  134.5465 27

 30 omega   83.00  128.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   75.0000  108.5268 45

 31 omega   29.00   56.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000 -119.5413 27

 32 omega   46.00   71.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   74.0000  -18.8040 25

 33 omega   29.00   62.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000  -33.1165 33

 34 omega   34.00   62.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   76.0000   53.8918 28

 35 omega   55.00   82.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   64.0000 -129.2418 27

 36 omega   32.00   59.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   77.0000  162.2873 27

 37 omega   39.00   87.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   65.0000  -96.7319 48

 38 omega   42.00   69.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   74.0000  139.3136 27

 39 omega   -8.00   93.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000  -80.0000  -23.5027 101

 40 omega   34.00   61.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   73.0000  -76.3552 27

 41 omega   37.00   63.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   76.0000   12.8870 26

 42 omega   38.00   74.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   76.0000  -67.9200 36

 43 omega   91.00  118.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   76.0000  -67.9200 27

 44 omega   39.00   71.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   73.0000 -150.1490 32

 45 omega   44.00   80.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   66.0000   41.0861 36

 46 omega   88.00  133.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   66.0000   41.0861 45

 47 omega   46.00   76.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   63.0000   96.2241 30

 48 omega   45.00   71.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   69.0000  174.7436 26

 49 omega   47.00  133.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   68.0000  -46.3085 86

 50 omega   -1.00  100.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000  -79.0000 -155.8319 101

 51 omega   53.00   81.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   58.0000  165.6294 28

 52 omega   59.00   92.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   58.0000  141.0518 33

 53 omega   47.00  109.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   73.0000  -92.0697 62

 54 omega   55.00   94.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   58.0000   12.3433 39

 55 omega   49.00   77.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   69.0000  -16.5278 28

 56 omega   45.00   74.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   76.0000 -173.3292 29

 57 omega   54.00  103.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   68.0000   22.1661 49

 58 omega   58.00   83.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   54.0000  158.5506 25

 59 omega   56.00   90.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   63.0000   97.3940 34

 60 omega   51.00   79.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000  -78.0000   53.4230 28

 61 omega   51.00  146.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   71.0000  177.3271 95

 62 omega   57.00  145.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   55.0000   67.1198 88

 63 omega   20.00   49.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000  -78.0000   53.4230 29

 64 omega   58.00   85.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   60.0000 -133.7685 27

 65 omega   49.00   76.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   75.0000  103.1923 27

 66 omega   55.00  145.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   68.0000  -50.6783 90

 67 omega   54.00   81.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000  -80.0000  178.4211 27

 68 omega   62.00   89.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   44.0000  169.2628 27

 69 omega   67.00  151.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   53.0000  -91.5182 84

 70 omega   69.00  109.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   54.0000  133.7861 40

 71 omega   16.00   81.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000  -80.0000   83.7515 65

 72 omega   64.00   98.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   48.0000   62.6359 34

 73 omega   65.00  100.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   56.0000 -139.3187 35

 74 omega   70.00  136.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       94.0000   69.0000 -133.0506 66

 75 omega   73.00  103.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       94.0000   56.0000  106.8157 30

 76 omega   85.00  112.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000 -180.0000 27

 77 omega   90.00  115.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   50.0000    0.0000 25

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

 79 omega   64.00   96.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000 -131.8082 32

 80 omega   80.00  107.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -77.0000 -180.0000 27

 81 omega  119.00  156.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000  -60.0000 37

 82 omega   39.00  139.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000  -34.5427 100

 83 omega   82.00  157.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000 -150.0000 75

 84 omega   86.00  126.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000   30.0000 40

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

 86 omega   86.00  111.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000 -120.0000 25

 87 omega   86.00  111.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000 -180.0000 25

 88 omega   86.00  111.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  -90.0000 25

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

 90 omega   85.00  156.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000   60.0000 71

 91 omega   86.00  173.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000    0.0000 87

 92 omega  112.00  177.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  150.0000 65

 93 omega   78.00  107.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  150.0000 29

 94 omega   79.00  106.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -150.0000 27

 95 omega  133.00  159.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -180.0000 26

 96 omega   78.00  105.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -180.0000 27

 97 omega   78.00  105.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   90.0000 27

 98 omega   74.00  138.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -79.0000   36.0281 64

 99 omega  153.00  178.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -60.0000 25

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

101 omega   39.00   66.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -79.0000   36.0281 27

102 omega  152.00  178.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -30.0000 26

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

104 omega   78.00  177.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -120.0000 99

105 omega  146.00  177.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   60.0000 31

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

107 omega  134.00  160.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -90.0000 26

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

109 omega  108.00  174.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  120.0000 66

110 omega   85.00  112.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  120.0000 27

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

112 omega  153.00  178.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000    0.0000 25

113 omega   63.00  106.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000  -87.3038 43

114 omega   79.00  104.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000    0.0000 25

115 omega   85.00  174.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000   90.0000 89

116 omega  120.00  174.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  -60.0000 54

117 omega   86.00  113.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  -60.0000 27

118 omega   82.00  116.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000  -60.0000 34

119 omega   85.00  112.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  150.0000 27

120 omega   83.00  110.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000    0.0000 27

121 omega   39.00  140.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000  124.8496 101

122 omega   84.00  109.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000  -90.0000 25

123 omega  114.00  139.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -79.0000   80.3130 25

124 omega   72.00   99.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -79.0000   80.3130 27

125 omega   43.00   70.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -79.0000   80.3130 27

126 omega   82.00  178.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000  -30.0000 96

127 omega   82.00  176.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   73.0000   39.1504 94

128 omega   84.00  111.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000  150.0000 27

129 phi      0.00  120.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
   0.0000    0.0000  -20.0000     -     120

130 omega  -72.00   26.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -38.0000   30.0000 98

131 omega  -21.00   69.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000 -180.0000 90

132 omega   -8.00   92.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       22.0000   77.0000  -87.2704 100

133 omega   -3.00   96.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       26.0000   76.0000  133.0261 99

134 omega    5.00   95.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       26.0000   55.0000   43.5068 90

135 omega   10.00   44.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   80.0000  151.2171 34

136 omega   14.00   46.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   80.0000 -135.5268 32

137 omega   19.00   47.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   79.0000  -57.5532 28

138 omega   -9.00   94.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000  -80.0000  -23.5027 103

139 omega   46.00  143.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   73.0000  -92.0697 97

140 omega   57.00  147.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   54.0000  158.5506 90

141 omega    7.00  110.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000  -80.0000  178.4211 103

142 omega    8.00  109.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000  -78.0000   53.4230 101

143 omega   57.00  146.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   60.0000 -133.7685 89

144 omega   57.00  147.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   55.0000   67.1198 90

145 omega   54.00  146.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   68.0000   22.1661 92

146 omega   49.00  148.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   75.0000  103.1923 99

147 omega   54.00  150.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   42.0000  -14.5033 96

148 omega   51.00  147.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   71.0000  177.3271 96

;
_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      -0.1011888000
_diffrn_orient_matrix_UB_12      -0.0838219000
_diffrn_orient_matrix_UB_13      -0.0025361000
_diffrn_orient_matrix_UB_21      0.0714559000
_diffrn_orient_matrix_UB_22      -0.0893564000
_diffrn_orient_matrix_UB_23      -0.0192494000
_diffrn_orient_matrix_UB_31      0.0214449000
_diffrn_orient_matrix_UB_32      0.0199627000
_diffrn_orient_matrix_UB_33      0.1074634000
_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  0.059
_diffrn_reflns_av_unetI/netI     0.0382
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            67698
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.142
_diffrn_reflns_theta_min         3.561
_diffrn_source                   'microfocus X-Ray tube'
_diffrn_source_type              'Agilent SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.639
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56582
_exptl_absorpt_correction_type   multi-scan
_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)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.173
_exptl_crystal_description       plate
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.104
_refine_diff_density_min         -0.626
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     503
_refine_ls_number_reflns         9598
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0773
_refine_ls_R_factor_gt           0.0598
_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^)+(0.0874P)^2^+1.4587P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1485
_refine_ls_wR_factor_ref         0.1576
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7720
_reflns_number_total             9598
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt04561d2.cif
_cod_data_source_block           ba_jb7_5
_cod_depositor_comments
'Adding full bibliography for 7037956--7037963.cif.'
_cod_original_cell_volume        2281.50(7)
_cod_database_code               7037957
_audit_block_refno               1731
_audit_block_usercomment         'jb109, plate, colourless'
_shelx_estimated_absorpt_t_min   0.853
_shelx_estimated_absorpt_t_max   0.853
_shelxl_version_number           2013-2
_shelx_res_checksum              45851
_cell_oxdiff_length_a            12.4277(2)
_cell_oxdiff_length_b            13.1483(2)
_cell_oxdiff_length_c            14.8044(3)
_cell_oxdiff_angle_alpha         106.9639(16)
_cell_oxdiff_angle_beta          92.2955(16)
_cell_oxdiff_angle_gamma         98.2181(15)
_cell_oxdiff_volume              2281.50(7)
_cell_oxdiff_measurement_reflns_used 23109
_cell_oxdiff_twin_number         2