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_7037960
_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_moiety         'C31 H46 N3 O P Si3 Zr'
_chemical_formula_sum            'C31 H46 N3 O P Si3 Zr'
_chemical_formula_weight         683.17
_chemical_properties_physical    'air-sensitive, moisture-sensitive'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_block_code                ba_ms11
_audit_creation_date
;
'Mon May 05 14:33:13 2014'
;
_audit_update_record
;
2015-12-14 deposited with the CCDC.
2015-12-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.1509(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.51494(10)
_cell_length_b                   15.79043(15)
_cell_length_c                   20.4802(2)
_cell_measurement_reflns_used    45793
_cell_measurement_temperature    110(1)
_cell_measurement_theta_max      70.6650
_cell_measurement_theta_min      4.3210
_cell_volume                     3297.25(6)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material
'encif (Wadepohl, 2009-14); encifer 1.4 (CCDC, 2011)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'SUPERFLIP (Palatinus, 2007-2009)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      110(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9621
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
;
  1 omega  -23.00   28.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   45.0000  104.0000 51

  2 omega  -69.00   23.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -45.0000  -46.0000 92

  3 omega   54.00   79.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   45.0000  104.0000 25

  4 omega   30.00   55.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -45.0000  -46.0000 25

  5 omega   37.00   83.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000  -46.0000 46

  6 omega  107.00  132.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000  104.0000 25

  7 omega  -43.00   49.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   19.0000 -180.0000 92

  8 omega  -71.00  -45.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -38.0000   30.0000 26

  9 omega  -64.00    1.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000  -90.0000 65

 10 omega  -33.00   24.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -38.0000   30.0000 57

 11 omega    8.00   34.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       10.0000   69.0000  128.0153 26

 12 omega  -11.00   48.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       14.0000   78.0000  -29.1734 59

 13 omega   -7.00   19.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       22.0000   79.0000 -121.0816 26

 14 omega    3.00   30.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       26.0000   78.0000  -87.9553 27

 15 omega    4.00   37.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       34.0000   80.0000 -164.4721 33

 16 omega    3.00   34.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       34.0000   80.0000  102.8164 31

 17 omega   13.00   39.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       38.0000   77.0000  -28.3984 26

 18 omega   17.00   43.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   76.0000  -55.8477 26

 19 omega   14.00   39.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   80.0000  -21.6910 25

 20 omega   14.00   39.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   80.0000   90.7822 25

 21 omega   17.00   43.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   80.0000 -152.5700 26

 22 omega   18.00   43.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   80.0000  -62.8959 25

 23 omega   19.00   44.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   79.0000 -130.5766 25

 24 omega   21.00   48.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   77.0000  136.2841 27

 25 omega   18.00   43.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   80.0000    2.0191 25

 26 omega   18.00   43.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   80.0000 -146.9455 25

 27 omega   19.00   45.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   79.0000  174.1325 26

 28 omega   19.00   45.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   80.0000   36.3242 26

 29 omega   24.00   49.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   78.0000   99.1177 25

 30 omega   25.00   51.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   76.0000 -105.3498 26

 31 omega   26.00   52.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  -70.4795 26

 32 omega   25.00   50.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  120.0000 25

 33 omega   31.00   57.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000   60.0000 26

 34 omega   12.00   84.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -77.0000   60.0000 72

 35 omega   25.00   51.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000 -120.0000 26

 36 omega   24.00   50.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  150.0000 26

 37 omega   24.00   50.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000    9.6462 26

 38 omega   79.00  109.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  150.0000 30

 39 omega   28.00   55.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000  -18.3284 27

 40 omega   29.00   56.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   76.0000  103.6400 27

 41 omega   29.00   56.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   76.0000   74.8268 27

 42 omega  -13.00   88.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000  -79.0000    4.7805 101

 43 omega   31.00   57.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   75.0000 -103.3673 26

 44 omega   29.00   55.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   76.0000  -51.9153 26

 45 omega   29.00   63.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   76.0000 -146.5075 34

 46 omega   29.00   87.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   75.0000 -173.9755 58

 47 omega   29.00   55.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000   13.6737 26

 48 omega   28.00   57.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000   42.6015 29

 49 omega  106.00  131.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   73.0000  123.1364 25

 50 omega   -9.00   93.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000  -79.0000 -171.7088 102

 51 omega   33.00   58.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   76.0000  130.7482 25

 52 omega   87.00  113.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   77.0000  -38.3724 26

 53 omega   32.00   69.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   77.0000  -38.3724 37

 54 omega   38.00   68.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   74.0000  176.4097 30

 55 omega   39.00   73.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   71.0000   25.7939 34

 56 omega   39.00   92.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   71.0000 -105.7417 53

 57 omega   38.00   81.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   73.0000  -58.5168 43

 58 omega   40.00   66.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   77.0000   56.6276 26

 59 omega   42.00  104.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   75.0000   67.5394 62

 60 omega   42.00   68.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   75.0000  103.3359 26

 61 omega   42.00   85.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   75.0000   -7.8851 43

 62 omega   48.00   98.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   73.0000 -132.5671 50

 63 omega   45.00   70.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   73.0000 -107.3383 25

 64 omega   40.00   66.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   77.0000 -157.1243 26

 65 omega   40.00   66.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   77.0000   45.1351 26

 66 omega   69.00   95.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000  -79.0000  -60.3505 26

 67 omega   54.00   80.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   55.0000 -142.8335 26

 68 omega   46.00   90.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   76.0000 -102.1681 44

 69 omega   45.00   77.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   76.0000  144.8589 32

 70 omega   46.00   73.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   75.0000  -27.6863 27

 71 omega   52.00  113.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   71.0000  110.4039 61

 72 omega   59.00   92.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   60.0000  179.9027 33

 73 omega   49.00   75.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   75.0000 -106.7858 26

 74 omega   54.00  103.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   70.0000   45.8960 49

 75 omega   49.00   75.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   76.0000 -155.3264 26

 76 omega   58.00  146.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   51.0000  108.2986 88

 77 omega   60.00   86.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000  -79.0000 -124.5874 26

 78 omega   61.00  104.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   68.0000  -82.5663 43

 79 omega   49.00  123.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   75.0000  -53.9518 74

 80 omega   57.00   83.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   77.0000  -60.3435 26

 81 omega   54.00   81.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   74.0000  111.0299 27

 82 omega   55.00   87.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   74.0000 -151.1602 32

 83 omega   54.00   85.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   74.0000    9.7748 31

 84 omega   62.00   90.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   57.0000  151.5371 28

 85 omega   54.00   89.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   74.0000  -23.6796 35

 86 omega   61.00   87.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   63.0000  162.0219 26

 87 omega   57.00   90.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   76.0000 -142.6389 33

 88 omega   61.00   87.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   38.0000 -139.9877 26

 89 omega   66.00  131.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   56.0000 -146.6562 65

 90 omega   58.00   84.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   74.0000  -11.3622 26

 91 omega   60.00   90.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   70.0000   87.2571 30

 92 omega   70.00  103.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   61.0000   27.9832 33

 93 omega   75.00  101.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   59.0000 -111.4885 26

 94 omega   62.00  159.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   74.0000   46.0303 97

 95 omega   67.00   97.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   65.0000  113.0799 30

 96 omega   72.00   98.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   61.0000   13.0451 26

 97 omega   68.00  138.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   66.0000 -102.1048 70

 98 omega   74.00   99.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       94.0000   54.0000  147.3546 25

 99 omega   65.00  125.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       94.0000   75.0000   27.7766 60

100 omega   71.00   97.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       94.0000   73.0000  -14.5369 26

101 omega   66.00  133.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       94.0000   74.0000  -61.1501 67

102 omega   71.00  125.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       94.0000   68.0000 -136.2851 54

103 omega   76.00  102.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       98.0000   64.0000  -13.7634 26

104 omega   77.00  111.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       98.0000   68.0000  143.7009 34

105 omega   78.00  110.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      102.0000   67.0000   47.0128 32

106 omega   78.00  104.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      102.0000   72.0000  165.9104 26

107 omega   72.00  107.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      102.0000   77.0000  -95.4903 35

108 omega   79.00  107.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      106.0000   71.0000  174.9911 28

109 omega   85.00  162.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000  150.0000 77

110 omega  116.00  176.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -60.0000 60

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

112 omega  148.00  174.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  120.0000 26

113 omega   87.00  113.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  120.0000 26

114 omega   79.00  178.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   30.0000 99

115 omega   87.00  112.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  -30.0000 25

116 omega   49.00  140.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000  -55.1860 91

117 omega   85.00  142.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000   90.0000 57

118 omega   85.00  175.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000 -120.0000 90

119 omega   74.00  105.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000 -126.0378 31

120 omega   44.00   70.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000 -126.0378 26

121 omega   85.00  140.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  -60.0000 55

122 omega   88.00  120.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000   60.0000 32

123 omega   85.00  174.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000 -150.0000 89

124 omega  112.00  178.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   60.0000 66

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

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

127 omega   78.00  178.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -180.0000 100

128 omega   80.00  167.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -90.0000 87

129 omega   69.00  133.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000   36.9520 64

130 omega  131.00  177.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   90.0000 46

131 omega  117.00  174.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000    0.0000 57

132 omega   37.00  101.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -79.0000   89.1744 64

133 omega   78.00  104.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000    0.0000 26

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

135 omega   85.00  112.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000    0.0000 27

136 omega   79.00  105.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000   -4.5384 26

137 omega   87.00  177.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -30.0000 90

138 omega   81.00  173.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   72.0000   18.2055 92

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

140 omega   69.00  111.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000 -175.7374 42

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

142 omega   78.00  176.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  150.0000 98

143 omega   37.00  128.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -79.0000  128.3665 91

144 omega  -21.00   69.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000  -60.0000 90

145 omega  -21.00   69.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000   30.0000 90

146 omega  -44.00   73.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   19.0000 -120.0000 117

147 omega  -72.00   26.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -38.0000 -180.0000 98

148 omega  -70.00   30.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -77.0000  -60.0000 100

149 omega   -7.00   86.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0000   69.0000  -32.5876 93

150 omega   -8.00   87.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0000   70.0000   71.7442 95

151 omega   -7.00   92.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       22.0000   76.0000    2.0208 99

152 omega   -3.00   96.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       26.0000   76.0000   81.6941 99

153 omega   -4.00   96.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       26.0000   77.0000 -163.5961 100

154 omega    7.00   49.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       38.0000   78.0000 -146.5211 42

155 omega    7.00   47.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       38.0000   79.0000  169.9867 40

156 omega    6.00   46.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       38.0000   80.0000  -74.3617 40

157 omega   14.00   46.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   80.0000  -21.6910 32

158 omega   14.00   46.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   80.0000   90.7822 32

159 omega   19.00   47.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   79.0000  174.1325 28

160 omega   18.00   46.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   80.0000 -146.9455 28

161 omega   18.00   46.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   80.0000    2.0191 28

162 omega   18.00   46.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   80.0000  -62.8959 28

163 omega   18.00   46.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   80.0000   36.3242 28

164 omega  -15.00   75.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -57.0000  -90.0000 90

165 omega   23.00   49.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   78.0000  -97.2918 26

166 omega  -16.00   84.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -77.0000  120.0000 100

167 omega   23.00   49.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   78.0000   99.1177 26

168 omega   28.00  128.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000  -18.3284 100

169 omega   28.00  128.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000   42.6015 100

170 omega  -13.00   89.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000  -79.0000    4.7805 102

171 omega   34.00   59.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   74.0000  176.4097 25

172 omega   34.00  131.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   73.0000  123.1364 97

173 omega   43.00  134.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   66.0000  125.2574 91

174 omega   38.00  135.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   73.0000  -58.5168 97

175 omega   39.00  135.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   71.0000   25.7939 96

176 omega   40.00  140.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   77.0000   45.1351 100

177 omega   41.00  140.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   75.0000   67.5394 99

178 omega   42.00  139.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   73.0000 -107.3383 97

179 omega   -1.00  101.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000  -79.0000  -60.3505 102

180 omega   41.00  140.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   75.0000   -7.8851 99

181 omega   40.00  140.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   77.0000 -157.1243 100

182 omega   47.00  143.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   71.0000  110.4039 96

183 omega   45.00  144.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   75.0000  -27.6863 99

184 omega   45.00  144.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   76.0000  144.8589 99

185 omega   57.00  147.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   57.0000  155.0105 90

186 omega   54.00  146.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   68.0000  -82.5663 92

187 omega   51.00  147.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   71.0000   16.1732 96

188 omega   56.00  146.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   62.0000 -141.5224 90

189 omega   49.00  148.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   76.0000 -155.3264 99

190 omega   52.00  147.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   70.0000   45.8960 95

191 omega   57.00  146.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   60.0000  179.9027 89

192 omega   56.00  148.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   51.0000  108.2986 92

193 omega   55.00  149.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   46.0000  153.7301 94

194 omega   56.00  146.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   63.0000  -70.7009 90

195 omega   49.00  148.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   75.0000 -106.7858 99

196 omega   49.00  148.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   75.0000  -53.9518 99

197 omega    7.00  109.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000  -79.0000 -124.5874 102

;
_diffrn_measurement_device       'four-circle 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      0.1457638000
_diffrn_orient_matrix_UB_12      0.0078494000
_diffrn_orient_matrix_UB_13      0.0372218000
_diffrn_orient_matrix_UB_21      0.0011823000
_diffrn_orient_matrix_UB_22      -0.0937266000
_diffrn_orient_matrix_UB_23      0.0208916000
_diffrn_orient_matrix_UB_31      0.0398773000
_diffrn_orient_matrix_UB_32      -0.0258310000
_diffrn_orient_matrix_UB_33      -0.0647854000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0933
_diffrn_reflns_av_unetI/netI     0.0293
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            146326
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.839
_diffrn_reflns_theta_min         3.576
_diffrn_source                   'microfocus X-Ray tube'
_diffrn_source_type              'Agilent SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.456
_exptl_absorpt_correction_T_max  0.820
_exptl_absorpt_correction_T_min  0.597
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.376
_exptl_crystal_description       plate
_exptl_crystal_F_000             1432
_exptl_crystal_size_max          0.1420
_exptl_crystal_size_mid          0.1075
_exptl_crystal_size_min          0.0484
_refine_diff_density_max         0.633
_refine_diff_density_min         -0.822
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     367
_refine_ls_number_reflns         6306
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0374
_refine_ls_R_factor_gt           0.0323
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0304P)^2^+3.0918P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0704
_refine_ls_wR_factor_ref         0.0723
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5815
_reflns_number_total             6306
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt04561d2.cif
_cod_data_source_block           ba_ms11
_cod_depositor_comments
'Adding full bibliography for 7037956--7037963.cif.'
_cod_original_cell_volume        3297.26(6)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7037960
_audit_block_refno               2031
_audit_block_usercomment         'pf34 plate yellow'
_shelxl_version_number           2014-3
_chemical_oxdiff_formula         'C31 H46 N3 O1 P1 Si3 Zr1'
_chemical_oxdiff_usercomment     'pf34 plate yellow'
_shelx_estimated_absorpt_t_max   0.664
_shelx_estimated_absorpt_t_min   0.664
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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), C28(H28A,H28B), C29(H29A,H29B),
 C30(H30A,H30B), C31(H31A,H31B)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C9(H9), C13(H13), C14(H14), C15(H15), C16(H16),
 C17(H17), C21(H21), C22(H22), C23(H23), C24(H24), C25(H25)
2.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C18(H18A,H18B,H18C), C19(H19A,H19B,
 H19C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C)
;
_shelx_res_checksum              21203
_cell_oxdiff_length_a            10.51309(19)
_cell_oxdiff_length_b            15.7946(3)
_cell_oxdiff_length_c            20.4786(4)
_cell_oxdiff_angle_alpha         90.0557(17)
_cell_oxdiff_angle_beta          104.1530(17)
_cell_oxdiff_angle_gamma         89.9987(16)
_cell_oxdiff_volume              3297.26(11)
_cell_oxdiff_measurement_reflns_used 45793