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_7037956
_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            'C24 H42 N2 P2 Si4'
_chemical_formula_weight         532.89
_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_cs2
_audit_creation_date
;
'Mon Mar 04 15:40:02 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                86.273(2)
_cell_angle_beta                 78.908(2)
_cell_angle_gamma                73.161(3)
_cell_formula_units_Z            1
_cell_length_a                   7.1947(2)
_cell_length_b                   8.3354(2)
_cell_length_c                   13.4789(3)
_cell_measurement_reflns_used    15413
_cell_measurement_temperature    110(1)
_cell_measurement_theta_max      70.7340
_cell_measurement_theta_min      5.5080
_cell_volume                     759.19(4)
_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    '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 0.980
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_details
;
  1 omega  -66.00   19.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000    0.0000 85

  2 omega  -67.00  -40.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000 -120.0000 27

  3 omega  -39.00   21.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000 -120.0000 60

  4 omega  -22.00   60.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       -3.5000   57.0000   30.0000 82

  5 omega   -6.00   19.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       26.0000   80.0000    6.9416 25

  6 omega    8.00   35.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       38.0000   80.0000  -21.9304 27

  7 omega    7.00   32.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       38.0000   79.0000  -94.2727 25

  8 omega    8.00   38.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       38.0000   79.0000  164.4443 30

  9 omega   14.00   41.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   78.0000   78.6284 27

 10 omega   14.00   39.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   80.0000 -144.5204 25

 11 omega   14.00   40.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   80.0000   19.9077 26

 12 omega   21.00   57.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   75.0000  -56.8140 36

 13 omega   18.00   43.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   80.0000  147.9313 25

 14 omega   91.00  118.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   75.0000  -56.8140 27

 15 omega   30.00   58.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -57.0000 -180.0000 28

 16 omega   28.00   55.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000 -124.8147 27

 17 omega   99.00  128.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000 -124.8147 29

 18 omega   32.00   65.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   71.0000  131.4379 33

 19 omega  102.00  127.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   71.0000  131.4379 25

 20 omega   30.00   57.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   73.0000   28.2664 27

 21 omega   38.00   90.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   69.0000  153.4029 52

 22 omega   33.00   58.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   77.0000  -17.0796 25

 23 omega   86.00  125.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   75.0000   96.4571 39

 24 omega   96.00  130.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   69.0000  153.4029 34

 25 omega   -8.00   93.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000  -80.0000  124.2867 101

 26 omega   46.00   73.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   42.0000  -17.8207 27

 27 omega   91.00  130.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   61.0000 -149.3710 39

 28 omega   34.00   66.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   76.0000 -124.3660 32

 29 omega   33.00   61.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   75.0000   96.4571 28

 30 omega   42.00   76.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   61.0000 -149.3710 34

 31 omega   44.00   71.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   61.0000  -76.5220 27

 32 omega   53.00   80.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   68.0000   23.4079 27

 33 omega   47.00   76.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   43.0000  -44.6197 29

 34 omega   44.00  139.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   73.0000   45.4909 95

 35 omega   28.00   73.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000  -80.0000  -74.8450 45

 36 omega    5.00  105.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000  -78.0000 -130.3116 100

 37 omega   44.00   73.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   77.0000  138.7883 29

 38 omega   57.00   87.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   58.0000 -111.8009 30

 39 omega   55.00  126.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   66.0000  -31.8255 71

 40 omega   15.00   97.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000  -79.0000   -3.7954 82

 41 omega   55.00   90.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   74.0000  172.1519 35

 42 omega  105.00  145.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   73.0000  -16.5479 40

 43 omega   58.00   99.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   73.0000  -16.5479 41

 44 omega   65.00   94.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   57.0000 -143.7746 29

 45 omega   83.00  119.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      106.0000   64.0000   89.8321 36

 46 omega   79.00  104.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -90.0000 25

 47 omega  138.00  165.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  120.0000 27

 48 omega   87.00  119.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  120.0000 32

 49 omega   79.00  104.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000    0.0000 25

 50 omega   79.00  106.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  150.0000 27

 51 omega   42.00   86.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000   -2.0499 44

 52 omega   78.00  104.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -60.0000 26

 53 omega   86.00  174.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000 -150.0000 88

 54 omega  139.00  173.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   60.0000 34

 55 omega   78.00  104.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   60.0000 26

 56 omega  131.00  174.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000 -120.0000 43

 57 omega   87.00  116.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000 -120.0000 29

 58 omega  121.00  168.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000    0.0000 47

 59 omega   85.00  175.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000   30.0000 90

 60 omega   37.00  139.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -79.0000  -34.6646 102

 61 omega   77.00  105.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000   42.1797 28

 62 omega   83.00  119.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -77.0000 -150.0000 36

 63 omega  108.00  139.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -79.0000 -122.2935 31

 64 omega   40.00   65.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000   42.1797 25

 65 omega   82.00  163.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000   90.0000 81

 66 omega   50.00  100.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -79.0000 -122.2935 50

 67 omega   93.00  143.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   50.0000  -90.0000 50

 68 omega  137.00  174.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000 -180.0000 37

 69 omega   85.00  121.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000   30.0000 36

 70 omega   85.00  174.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  150.0000 89

 71 omega   85.00  175.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  -60.0000 90

 72 omega   85.00  174.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  -90.0000 89

 73 omega   82.00  109.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  120.0000 27

 74 omega   38.00  138.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -79.0000  119.7465 100

 75 omega   85.00  174.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  -30.0000 89

 76 omega   86.00  113.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   50.0000 -120.0000 27

 77 omega   85.00  111.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000   60.0000 26

 78 omega   85.00  134.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000 -180.0000 49

 79 omega   52.00   96.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -77.0000 -180.0000 44

 80 omega   80.00  164.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   90.0000 84

 81 omega   78.00  105.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -120.0000 27

 82 omega   83.00  110.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000  150.0000 27

 83 omega  115.00  143.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000  150.0000 28

 84 omega   79.00  106.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -30.0000 27

 85 omega   83.00  110.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -180.0000 27

 86 omega   57.00   92.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -77.0000  150.0000 35

 87 omega   79.00  106.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   30.0000 27

 88 omega  -72.00   26.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -38.0000   60.0000 98

 89 omega  -25.00   65.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       -3.5000   57.0000 -180.0000 90

 90 omega   -2.00   90.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       22.0000   67.0000   40.2977 92

 91 omega   -6.00   46.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       26.0000   80.0000    6.9416 52

 92 omega   -4.00   96.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       26.0000   77.0000 -131.8738 100

 93 omega    7.00   47.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       38.0000   79.0000  -94.2727 40

 94 omega    6.00   46.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       38.0000   80.0000  -21.9304 40

 95 omega   10.00   46.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   80.0000   99.4925 36

 96 omega   14.00   46.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   80.0000 -144.5204 32

 97 omega  -19.00  127.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000    0.0000    0.0000 146

 98 omega  -19.00  127.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000    0.0000  120.0000 146

 99 omega  -19.00  127.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000    0.0000    0.0000 146

100 omega  -19.00  127.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000    0.0000  120.0000 146

101 omega  -19.00  127.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000    0.0000  240.0000 146

102 omega   29.00  128.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   76.0000 -139.8469 99

103 omega   31.00  127.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   71.0000  131.4379 96

104 omega  -12.00   89.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000  -78.0000 -177.7045 101

105 omega   33.00  132.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   76.0000 -124.3660 99

106 omega   -9.00   94.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000  -80.0000  124.2867 103

107 omega   37.00  130.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   69.0000  153.4029 93

108 omega   32.00  132.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   77.0000  -17.0796 100

109 omega   40.00  130.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   61.0000 -149.3710 90

110 omega   44.00  134.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   61.0000  -76.5220 90

111 omega   42.00  138.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   42.0000  178.8996 96

112 omega   42.00  134.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   68.0000   23.4079 92

113 omega   42.00  139.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   73.0000   45.4909 97

114 omega   46.00  142.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   43.0000  -44.6197 96

115 omega    4.00  105.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000  -78.0000 -130.3116 101

116 omega   44.00  144.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   77.0000  138.7883 100

117 omega    3.00  106.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000  -80.0000  -74.8450 103

118 omega   55.00  146.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   66.0000  -31.8255 91

119 omega   57.00  147.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   58.0000 -111.8009 90

120 omega   86.00  166.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   50.0000   90.0000 80

121 omega   38.00  104.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -50.0000   90.0000 66

;
_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      -0.0247107000
_diffrn_orient_matrix_UB_12      -0.1187391000
_diffrn_orient_matrix_UB_13      0.0909153000
_diffrn_orient_matrix_UB_21      -0.0476067000
_diffrn_orient_matrix_UB_22      -0.1189281000
_diffrn_orient_matrix_UB_23      -0.0679146000
_diffrn_orient_matrix_UB_31      0.2210908000
_diffrn_orient_matrix_UB_32      -0.0951275000
_diffrn_orient_matrix_UB_33      -0.0262426000
_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  0.0325
_diffrn_reflns_av_unetI/netI     0.0143
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            22999
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.888
_diffrn_reflns_theta_min         3.341
_diffrn_source                   'microfocus X-Ray tube'
_diffrn_source_type              'Agilent SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.920
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72195
_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    1.166
_exptl_crystal_description       irregular
_exptl_crystal_F_000             286
_exptl_crystal_size_max          0.2107
_exptl_crystal_size_mid          0.0953
_exptl_crystal_size_min          0.0816
_refine_diff_density_max         1.082
_refine_diff_density_min         -0.312
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     177
_refine_ls_number_reflns         2845
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0488
_refine_ls_R_factor_gt           0.0446
_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^)+(0.0462P)^2^+0.9522P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1089
_refine_ls_wR_factor_ref         0.1112
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2583
_reflns_number_total             2845
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt04561d2.cif
_cod_data_source_block           ba_cs2_4
_cod_depositor_comments
'Adding full bibliography for 7037956--7037963.cif.'
_cod_database_code               7037956
_audit_block_refno               1716
_audit_block_usercomment         'cs07, irregular, colourless'
_shelx_estimated_absorpt_t_min   0.578
_shelx_estimated_absorpt_t_max   0.797
_shelxl_version_number           2013-2
_shelx_res_checksum              58105
_cell_oxdiff_length_a            7.1947(2)
_cell_oxdiff_length_b            8.3354(2)
_cell_oxdiff_length_c            13.4789(3)
_cell_oxdiff_angle_alpha         86.273(2)
_cell_oxdiff_angle_beta          78.908(2)
_cell_oxdiff_angle_gamma         73.161(2)
_cell_oxdiff_volume              759.19(3)
_cell_oxdiff_measurement_reflns_used 15413
_cell_oxdiff_twin_number         2