#------------------------------------------------------------------------------
#$Date: 2016-03-05 11:29:23 +0200 (Sat, 05 Mar 2016) $
#$Revision: 177783 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/79/7037957.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7037957
loop_
_publ_author_name
'Sietzen, M.'
'Federmann, P.'
'Sonnenschein, C.'
'Wadepohl, H.'
'Ballmann, J.'
_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       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'Agilent SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω and π 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/[σ²(Fo²)+(0.0874P)²+1.4587P]
 where P=(Fo²+2Fc²)/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 > 2σ(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_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.853
_shelx_estimated_absorpt_t_max   0.853
_shelxl_version_number           2013-2
_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
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_disorder_assembly
_atom_site_disorder_group
P P 0.68668(5) 0.75941(6) 0.74779(5) 0.02181(18) Uani 1 1 d . . . .
Si1 Si 0.64525(6) 0.97101(6) 0.70588(6) 0.02377(19) Uani 1 1 d . . . .
Si2 Si 0.87855(6) 0.68203(6) 0.64145(6) 0.02291(19) Uani 1 1 d . . . .
Si3 Si 0.57125(6) 0.65462(6) 0.89404(6) 0.02275(19) Uani 1 1 d . . . .
O1 O 0.92617(17) 0.92839(17) 0.53182(15) 0.0286(5) Uani 1 1 d . . . .
O2 O 0.91512(18) 0.94628(17) 0.93002(15) 0.0301(5) Uani 1 1 d . . . .
O3 O 0.74221(15) 0.46152(16) 0.99886(15) 0.0267(5) Uani 1 1 d . . . .
O4 O 0.92519(18) 0.36431(19) 1.02186(18) 0.0379(6) Uani 1 1 d . . . .
N1 N 0.78430(18) 0.99376(18) 0.73324(16) 0.0197(5) Uani 1 1 d . . . .
N2 N 0.94900(18) 0.80831(18) 0.70015(17) 0.0208(5) Uani 1 1 d . . . .
N3 N 0.51168(18) 0.53224(19) 0.90336(18) 0.0229(5) Uani 1 1 d . . . .
C1 C 0.5863(2) 0.8415(2) 0.7294(2) 0.0273(7) Uani 1 1 d . . . .
H1A H 0.5459 0.8590 0.7852 0.033 Uiso 1 1 calc R U . .
H1B H 0.5349 0.7990 0.6763 0.033 Uiso 1 1 calc R U . .
C2 C 0.7331(2) 0.7040(2) 0.6284(2) 0.0240(6) Uani 1 1 d . . . .
H2A H 0.7281 0.7539 0.5920 0.029 Uiso 1 1 calc R U . .
H2B H 0.6869 0.6363 0.5950 0.029 Uiso 1 1 calc R U . .
C3 C 0.6060(2) 0.6414(2) 0.7685(2) 0.0253(6) Uani 1 1 d . . . .
H3A H 0.6456 0.5814 0.7482 0.030 Uiso 1 1 calc R U . .
H3B H 0.5383 0.6230 0.7282 0.030 Uiso 1 1 calc R U . .
C4 C 0.5757(3) 1.0785(3) 0.7819(3) 0.0427(9) Uani 1 1 d . . . .
H4A H 0.6003 1.0921 0.8472 0.064 Uiso 1 1 calc R U . .
H4B H 0.4982 1.0550 0.7729 0.064 Uiso 1 1 calc R U . .
H4C H 0.5929 1.1434 0.7644 0.064 Uiso 1 1 calc R U . .
C5 C 0.6024(3) 0.9545(3) 0.5788(3) 0.0387(8) Uani 1 1 d . . . .
H5A H 0.6256 1.0208 0.5650 0.058 Uiso 1 1 calc R U . .
H5B H 0.5244 0.9361 0.5681 0.058 Uiso 1 1 calc R U . .
H5C H 0.6352 0.8981 0.5383 0.058 Uiso 1 1 calc R U . .
C6 C 0.8477(2) 1.0919(2) 0.7384(2) 0.0208(6) Uani 1 1 d . . . .
C7 C 0.8135(2) 1.1727(2) 0.7029(2) 0.0249(6) Uani 1 1 d . . . .
H7 H 0.7422 1.1627 0.6764 0.030 Uiso 1 1 calc R U . .
C8 C 0.8843(3) 1.2663(2) 0.7068(2) 0.0278(7) Uani 1 1 d . . . .
H8 H 0.8591 1.3178 0.6835 0.033 Uiso 1 1 calc R U . .
C9 C 0.9914(3) 1.2843(2) 0.7446(2) 0.0312(7) Uani 1 1 d . . . .
H9 H 1.0385 1.3463 0.7456 0.037 Uiso 1 1 calc R U . .
C10 C 1.0269(2) 1.2076(3) 0.7809(2) 0.0294(7) Uani 1 1 d . . . .
H10 H 1.0986 1.2183 0.8067 0.035 Uiso 1 1 calc R U . .
C11 C 0.9562(2) 1.1152(2) 0.7791(2) 0.0234(6) Uani 1 1 d . . . .
H11 H 0.9816 1.0664 0.8059 0.028 Uiso 1 1 calc R U . .
C12 C 0.9271(3) 0.6264(3) 0.5214(3) 0.0368(8) Uani 1 1 d . . . .
H12A H 0.9132 0.6711 0.4827 0.055 Uiso 1 1 calc R U . .
H12B H 0.8889 0.5545 0.4923 0.055 Uiso 1 1 calc R U . .
H12C H 1.0040 0.6250 0.5279 0.055 Uiso 1 1 calc R U . .
C13 C 0.8772(3) 0.5731(3) 0.7011(3) 0.0349(8) Uani 1 1 d . . . .
H13A H 0.9432 0.5428 0.6911 0.052 Uiso 1 1 calc R U . .
H13B H 0.8155 0.5176 0.6747 0.052 Uiso 1 1 calc R U . .
H13C H 0.8721 0.6034 0.7679 0.052 Uiso 1 1 calc R U . .
C14 C 1.0602(2) 0.8263(2) 0.7284(2) 0.0245(6) Uani 1 1 d . . . .
C15 C 1.1258(2) 0.9250(2) 0.7329(2) 0.0265(6) Uani 1 1 d . . . .
H15 H 1.0941 0.9759 0.7135 0.032 Uiso 1 1 calc R U . .
C16 C 1.2354(2) 0.9491(3) 0.7651(3) 0.0357(8) Uani 1 1 d . . . .
H16 H 1.2752 1.0154 0.7671 0.043 Uiso 1 1 calc R U . .
C17 C 1.2863(3) 0.8757(3) 0.7944(3) 0.0464(10) Uani 1 1 d . . . .
H17 H 1.3596 0.8917 0.8169 0.056 Uiso 1 1 calc R U . .
C18 C 1.2242(3) 0.7775(3) 0.7889(3) 0.0508(11) Uani 1 1 d . . . .
H18 H 1.2571 0.7264 0.8070 0.061 Uiso 1 1 calc R U . .
C19 C 1.1147(3) 0.7532(3) 0.7572(3) 0.0399(9) Uani 1 1 d . . . .
H19 H 1.0760 0.6864 0.7549 0.048 Uiso 1 1 calc R U . .
C20 C 0.7033(3) 0.6998(3) 0.9705(3) 0.0348(8) Uani 1 1 d . . . .
H20A H 0.6909 0.6973 1.0335 0.052 Uiso 1 1 calc R U . .
H20B H 0.7322 0.7723 0.9726 0.052 Uiso 1 1 calc R U . .
H20C H 0.7544 0.6531 0.9446 0.052 Uiso 1 1 calc R U . .
C21 C 0.4882(3) 0.7650(3) 0.9386(3) 0.0342(7) Uani 1 1 d . . . .
H21A H 0.4255 0.7539 0.8947 0.051 Uiso 1 1 calc R U . .
H21B H 0.5319 0.8334 0.9443 0.051 Uiso 1 1 calc R U . .
H21C H 0.4649 0.7641 0.9994 0.051 Uiso 1 1 calc R U . .
C22 C 0.4396(2) 0.4599(2) 0.8314(2) 0.0236(6) Uani 1 1 d . . . .
C23 C 0.4312(3) 0.3480(3) 0.8169(3) 0.0360(8) Uani 1 1 d . . . .
H23 H 0.4759 0.3238 0.8554 0.043 Uiso 1 1 calc R U . .
C24 C 0.3588(3) 0.2729(3) 0.7474(3) 0.0467(10) Uani 1 1 d . . . .
H24 H 0.3561 0.1999 0.7402 0.056 Uiso 1 1 calc R U . .
C25 C 0.2909(3) 0.3047(3) 0.6889(3) 0.0425(9) Uani 1 1 d . . . .
H25 H 0.2427 0.2541 0.6421 0.051 Uiso 1 1 calc R U . .
C26 C 0.2961(3) 0.4144(3) 0.7014(3) 0.0367(8) Uani 1 1 d . . . .
H26 H 0.2504 0.4375 0.6629 0.044 Uiso 1 1 calc R U . .
C27 C 0.3679(2) 0.4891(3) 0.7702(2) 0.0289(7) Uani 1 1 d . . . .
H27 H 0.3693 0.5618 0.7768 0.035 Uiso 1 1 calc R U . .
C28 C 1.0281(3) 0.9004(3) 0.4980(2) 0.0316(7) Uani 1 1 d . . . .
H28A H 1.0173 0.8620 0.4307 0.038 Uiso 1 1 calc R U . .
H28B H 1.0540 0.8532 0.5305 0.038 Uiso 1 1 calc R U . .
C29 C 0.8882(3) 1.0000(3) 0.4852(2) 0.0313(7) Uani 1 1 d . . . .
H29A H 0.8203 1.0200 0.5093 0.038 Uiso 1 1 calc R U . .
H29B H 0.8744 0.9638 0.4177 0.038 Uiso 1 1 calc R U . .
C30 C 0.9825(3) 0.8869(2) 0.9696(2) 0.0325(7) Uani 1 1 d . . . .
H30A H 0.9889 0.8197 0.9222 0.039 Uiso 1 1 calc R U . .
H30B H 0.9494 0.8699 1.0228 0.039 Uiso 1 1 calc R U . .
C31 C 0.9068(3) 1.0471(3) 0.9980(2) 0.0330(7) Uani 1 1 d . . . .
H31A H 0.8720 1.0341 1.0521 0.040 Uiso 1 1 calc R U . .
H31B H 0.8618 1.0862 0.9699 0.040 Uiso 1 1 calc R U . .
C32 C 0.8353(2) 0.5207(2) 1.0631(2) 0.0283(7) Uani 1 1 d . . . .
H32A H 0.8117 0.5731 1.1163 0.034 Uiso 1 1 calc R U . .
H32B H 0.8850 0.5592 1.0309 0.034 Uiso 1 1 calc R U . .
C33 C 0.8927(3) 0.4448(3) 1.0983(3) 0.0351(7) Uani 1 1 d . . . .
H33A H 0.9566 0.4851 1.1400 0.042 Uiso 1 1 calc R U . .
H33B H 0.8444 0.4105 1.1346 0.042 Uiso 1 1 calc R U . .
C34 C 0.8338(3) 0.3076(3) 0.9583(3) 0.0380(8) Uani 1 1 d . . . .
H34A H 0.7832 0.2698 0.9904 0.046 Uiso 1 1 calc R U . .
H34B H 0.8573 0.2545 0.9056 0.046 Uiso 1 1 calc R U . .
C35 C 0.7768(3) 0.3821(3) 0.9213(2) 0.0348(7) Uani 1 1 d . . . .
H35A H 0.8258 0.4174 0.8862 0.042 Uiso 1 1 calc R U . .
H35B H 0.7139 0.3413 0.8785 0.042 Uiso 1 1 calc R U . .
Li1 Li 0.8849(4) 0.9112(4) 0.6473(4) 0.0274(11) Uani 1 1 d . . . .
Li2 Li 0.8530(4) 0.8947(4) 0.8031(4) 0.0241(10) Uani 1 1 d . . . .
Li3 Li 0.5966(4) 0.4892(4) 0.9993(4) 0.0258(10) Uani 1 1 d . . . .
O5 O 0.6289(5) 0.4276(3) 0.5144(4) 0.128(2) Uani 1 1 d D . A 1
O6 O 0.6521(3) 0.2196(3) 0.5133(3) 0.0858(11) Uani 1 1 d D . A 1
C36 C 0.5500(5) 0.3684(6) 0.5537(5) 0.115(3) Uani 1 1 d D . A 1
H36A H 0.4902 0.3307 0.5063 0.139 Uiso 1 1 calc R U A 1
H36B H 0.5211 0.4168 0.6064 0.139 Uiso 1 1 calc R U A 1
C37 C 0.6013(4) 0.2925(5) 0.5859(4) 0.0831(17) Uani 1 1 d D . A 1
H37A H 0.5468 0.2503 0.6112 0.100 Uiso 1 1 calc R U A 1
H37B H 0.6563 0.3320 0.6372 0.100 Uiso 1 1 calc R U A 1
C38 C 0.7260(4) 0.2803(4) 0.4752(4) 0.0691(13) Uani 1 1 d D . A 1
H38A H 0.7565 0.2322 0.4234 0.083 Uiso 1 1 calc R U A 1
H38B H 0.7853 0.3179 0.5232 0.083 Uiso 1 1 calc R U A 1
C39 C 0.6794(4) 0.3603(4) 0.4396(4) 0.0715(14) Uani 1 1 d D . A 1
H39A H 0.7367 0.4039 0.4183 0.086 Uiso 1 1 calc R U A 1
H39B H 0.6259 0.3237 0.3863 0.086 Uiso 1 1 calc R U A 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Li Li 0.0008 0.0003 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
C1 P C3 104.63(13) . .
C1 P C2 104.17(14) . .
C3 P C2 103.26(13) . .
C1 P Li2 102.03(15) . .
C3 P Li2 143.82(15) . .
C2 P Li2 93.34(15) . .
N1 Si1 C4 112.94(15) . .
N1 Si1 C5 114.56(14) . .
C4 Si1 C5 107.84(18) . .
N1 Si1 C1 108.36(12) . .
C4 Si1 C1 106.10(15) . .
C5 Si1 C1 106.53(15) . .
N2 Si2 C12 111.77(14) . .
N2 Si2 C2 104.09(12) . .
C12 Si2 C2 109.70(15) . .
N2 Si2 C13 118.25(14) . .
C12 Si2 C13 106.18(16) . .
C2 Si2 C13 106.58(13) . .
N2 Si2 Li1 39.75(13) . .
C12 Si2 Li1 100.12(15) . .
C2 Si2 Li1 72.83(13) . .
C13 Si2 Li1 151.89(16) . .
N2 Si2 Li2 39.20(12) . .
C12 Si2 Li2 145.32(14) . .
C2 Si2 Li2 72.62(13) . .
C13 Si2 Li2 106.01(15) . .
Li1 Si2 Li2 46.26(13) . .
N3 Si3 C20 108.90(13) . .
N3 Si3 C21 113.52(14) . .
C20 Si3 C21 105.27(16) . .
N3 Si3 C3 110.54(13) . .
C20 Si3 C3 106.62(14) . .
C21 Si3 C3 111.59(14) . .
N3 Si3 Li3 37.35(12) . .
C20 Si3 Li3 71.68(13) . .
C21 Si3 Li3 121.71(15) . .
C3 Si3 Li3 125.29(14) . .
C29 O1 C28 109.9(2) . .
C29 O1 Li1 126.4(2) . .
C28 O1 Li1 120.3(2) . .
C31 O2 C30 110.8(2) . .
C31 O2 Li2 126.9(2) . .
C30 O2 Li2 122.3(2) . .
C35 O3 C32 109.7(2) . .
C35 O3 Li3 121.4(2) . .
C32 O3 Li3 128.4(2) . .
C34 O4 C33 110.2(2) . .
C6 N1 Si1 121.38(18) . .
C6 N1 Li1 91.7(2) . .
Si1 N1 Li1 122.0(2) . .
C6 N1 Li2 116.8(2) . .
Si1 N1 Li2 118.83(17) . .
Li1 N1 Li2 71.4(2) . .
C14 N2 Si2 122.36(19) . .
C14 N2 Li1 120.4(2) . .
Si2 N2 Li1 106.6(2) . .
C14 N2 Li2 114.5(2) . .
Si2 N2 Li2 110.19(17) . .
Li1 N2 Li2 71.8(2) . .
C22 N3 Si3 121.62(19) . .
C22 N3 Li3 123.7(2) . .
Si3 N3 Li3 111.11(19) . .
C22 N3 Li3 89.5(2) . 2_667
Si3 N3 Li3 125.3(2) . 2_667
Li3 N3 Li3 74.6(2) . 2_667
P C1 Si1 114.79(15) . .
P C2 Si2 109.05(15) . .
P C3 Si3 116.93(16) . .
N1 C6 C11 119.5(2) . .
N1 C6 C7 125.4(3) . .
C11 C6 C7 115.1(2) . .
N1 C6 Li1 54.25(17) . .
C11 C6 Li1 88.0(2) . .
C7 C6 Li1 128.2(2) . .
C8 C7 C6 121.5(3) . .
C9 C8 C7 121.4(3) . .
C8 C9 C10 118.5(3) . .
C11 C10 C9 120.4(3) . .
C10 C11 C6 123.0(3) . .
N2 C14 C19 124.5(3) . .
N2 C14 C15 120.4(3) . .
C19 C14 C15 115.0(3) . .
C16 C15 C14 122.8(3) . .
C17 C16 C15 120.7(3) . .
C16 C17 C18 117.7(3) . .
C19 C18 C17 121.8(3) . .
C18 C19 C14 122.0(3) . .
N3 C22 C23 120.3(3) . .
N3 C22 C27 124.9(3) . .
C23 C22 C27 114.7(3) . .
N3 C22 Li3 56.39(18) . 2_667
C23 C22 Li3 97.2(2) . 2_667
C27 C22 Li3 116.0(2) . 2_667
C24 C23 C22 122.4(3) . .
C25 C24 C23 121.0(3) . .
C24 C25 C26 118.4(3) . .
C27 C26 C25 120.7(3) . .
C26 C27 C22 122.8(3) . .
O1 C28 C29 110.5(3) . 2_776
O1 C29 C28 110.3(3) . 2_776
O2 C30 C31 109.4(3) . 2_777
O2 C31 C30 110.4(3) . 2_777
O3 C32 C33 109.9(2) . .
O4 C33 C32 111.3(3) . .
O4 C34 C35 111.4(3) . .
O3 C35 C34 109.7(3) . .
O1 Li1 N2 119.8(3) . .
O1 Li1 N1 126.8(3) . .
N2 Li1 N1 113.3(3) . .
O1 Li1 Li2 173.6(3) . .
N2 Li1 Li2 56.92(18) . .
N1 Li1 Li2 56.42(18) . .
O1 Li1 C6 104.0(2) . .
N2 Li1 C6 126.3(3) . .
N1 Li1 C6 34.05(12) . .
Li2 Li1 C6 76.1(2) . .
O1 Li1 Si2 109.4(2) . .
N2 Li1 Si2 33.61(11) . .
N1 Li1 Si2 116.3(2) . .
Li2 Li1 Si2 71.08(17) . .
C6 Li1 Si2 146.4(2) . .
O2 Li2 N1 123.0(3) . .
O2 Li2 N2 116.8(2) . .
N1 Li2 N2 103.3(2) . .
O2 Li2 Li1 141.1(3) . .
N1 Li2 Li1 52.15(17) . .
N2 Li2 Li1 51.24(17) . .
O2 Li2 P 124.3(2) . .
N1 Li2 P 88.66(18) . .
N2 Li2 P 94.14(19) . .
Li1 Li2 P 94.6(2) . .
O2 Li2 Si2 129.5(2) . .
N1 Li2 Si2 105.81(19) . .
N2 Li2 Si2 30.61(9) . .
Li1 Li2 Si2 62.66(17) . .
P Li2 Si2 63.93(11) . .
O3 Li3 N3 128.5(3) . .
O3 Li3 N3 125.9(3) . 2_667
N3 Li3 N3 105.4(2) . 2_667
O3 Li3 Li3 175.5(4) . 2_667
N3 Li3 Li3 53.96(19) . 2_667
N3 Li3 Li3 51.42(19) 2_667 2_667
O3 Li3 C22 104.6(2) . 2_667
N3 Li3 C22 122.1(2) . 2_667
N3 Li3 C22 34.15(12) 2_667 2_667
Li3 Li3 C22 74.8(2) 2_667 2_667
O3 Li3 Si3 109.9(2) . .
N3 Li3 Si3 31.54(10) . .
N3 Li3 Si3 119.8(2) 2_667 .
Li3 Li3 Si3 74.1(2) 2_667 .
C22 Li3 Si3 116.8(2) 2_667 .
C36 O5 C39 112.9(4) . .
C38 O6 C37 108.2(4) . .
O5 C36 C37 108.4(5) . .
C36 C37 O6 114.4(5) . .
O6 C38 C39 114.2(4) . .
O5 C39 C38 108.9(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
P C1 1.824(3) .
P C3 1.834(3) .
P C2 1.854(3) .
P Li2 2.463(5) .
Si1 N1 1.722(2) .
Si1 C4 1.873(3) .
Si1 C5 1.876(4) .
Si1 C1 1.889(3) .
Si2 N2 1.720(2) .
Si2 C12 1.873(3) .
Si2 C2 1.883(3) .
Si2 C13 1.888(3) .
Si2 Li1 2.978(5) .
Si2 Li2 3.171(5) .
Si3 N3 1.719(2) .
Si3 C20 1.873(3) .
Si3 C21 1.879(3) .
Si3 C3 1.888(3) .
Si3 Li3 3.065(5) .
O1 C29 1.437(4) .
O1 C28 1.438(4) .
O1 Li1 1.871(5) .
O2 C31 1.432(4) .
O2 C30 1.438(4) .
O2 Li2 1.891(5) .
O3 C35 1.436(4) .
O3 C32 1.439(4) .
O3 Li3 1.896(5) .
O4 C34 1.412(4) .
O4 C33 1.423(4) .
N1 C6 1.392(3) .
N1 Li1 2.017(6) .
N1 Li2 2.129(5) .
N2 C14 1.394(4) .
N2 Li1 1.988(5) .
N2 Li2 2.136(5) .
N3 C22 1.390(4) .
N3 Li3 1.993(5) .
N3 Li3 2.062(5) 2_667
C6 C11 1.409(4) .
C6 C7 1.422(4) .
C6 Li1 2.485(6) .
C7 C8 1.392(4) .
C8 C9 1.383(4) .
C9 C10 1.387(5) .
C10 C11 1.387(4) .
C14 C19 1.402(4) .
C14 C15 1.413(4) .
C15 C16 1.385(4) .
C16 C17 1.384(5) .
C17 C18 1.385(5) .
C18 C19 1.383(5) .
C22 C23 1.411(4) .
C22 C27 1.413(4) .
C22 Li3 2.475(6) 2_667
C23 C24 1.387(5) .
C24 C25 1.374(5) .
C25 C26 1.392(5) .
C26 C27 1.375(5) .
C28 C29 1.502(4) 2_776
C29 C28 1.502(4) 2_776
C30 C31 1.497(5) 2_777
C31 C30 1.497(5) 2_777
C32 C33 1.502(4) .
C34 C35 1.496(5) .
Li1 Li2 2.422(7) .
Li3 N3 2.062(5) 2_667
Li3 Li3 2.458(9) 2_667
Li3 C22 2.475(6) 2_667
O5 C36 1.412(8) .
O5 C39 1.430(7) .
O6 C38 1.376(6) .
O6 C37 1.449(6) .
C36 C37 1.436(9) .
C38 C39 1.482(6) .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
C4 Si1 N1 C6 -51.7(3) . .
C5 Si1 N1 C6 72.3(3) . .
C1 Si1 N1 C6 -169.0(2) . .
C4 Si1 N1 Li1 -166.7(2) . .
C5 Si1 N1 Li1 -42.7(3) . .
C1 Si1 N1 Li1 76.0(2) . .
C4 Si1 N1 Li2 108.1(2) . .
C5 Si1 N1 Li2 -127.9(2) . .
C1 Si1 N1 Li2 -9.1(2) . .
C12 Si2 N2 C14 -65.2(3) . .
C2 Si2 N2 C14 176.5(2) . .
C13 Si2 N2 C14 58.5(3) . .
Li1 Si2 N2 C14 -144.6(3) . .
Li2 Si2 N2 C14 139.1(3) . .
C12 Si2 N2 Li1 79.4(2) . .
C2 Si2 N2 Li1 -38.9(2) . .
C13 Si2 N2 Li1 -156.9(2) . .
Li2 Si2 N2 Li1 -76.3(2) . .
C12 Si2 N2 Li2 155.69(19) . .
C2 Si2 N2 Li2 37.4(2) . .
C13 Si2 N2 Li2 -80.6(2) . .
Li1 Si2 N2 Li2 76.3(2) . .
C20 Si3 N3 C22 -154.4(2) . .
C21 Si3 N3 C22 88.7(3) . .
C3 Si3 N3 C22 -37.6(3) . .
Li3 Si3 N3 C22 -159.3(3) . .
C20 Si3 N3 Li3 4.9(2) . .
C21 Si3 N3 Li3 -112.0(2) . .
C3 Si3 N3 Li3 121.7(2) . .
C20 Si3 N3 Li3 90.6(2) . 2_667
C21 Si3 N3 Li3 -26.3(3) . 2_667
C3 Si3 N3 Li3 -152.6(2) . 2_667
Li3 Si3 N3 Li3 85.7(3) . 2_667
C3 P C1 Si1 -179.98(17) . .
C2 P C1 Si1 -71.9(2) . .
Li2 P C1 Si1 24.7(2) . .
N1 Si1 C1 P -13.0(2) . .
C4 Si1 C1 P -134.6(2) . .
C5 Si1 C1 P 110.7(2) . .
C1 P C2 Si2 150.23(14) . .
C3 P C2 Si2 -100.67(15) . .
Li2 P C2 Si2 46.93(17) . .
N2 Si2 C2 P -60.11(16) . .
C12 Si2 C2 P -179.84(15) . .
C13 Si2 C2 P 65.61(19) . .
Li1 Si2 C2 P -84.99(16) . .
Li2 Si2 C2 P -36.41(14) . .
C1 P C3 Si3 -85.55(19) . .
C2 P C3 Si3 165.70(16) . .
Li2 P C3 Si3 50.7(3) . .
N3 Si3 C3 P -172.07(14) . .
C20 Si3 C3 P -53.9(2) . .
C21 Si3 C3 P 60.6(2) . .
Li3 Si3 C3 P -132.87(16) . .
Si1 N1 C6 C11 167.3(2) . .
Li1 N1 C6 C11 -62.9(3) . .
Li2 N1 C6 C11 7.1(4) . .
Si1 N1 C6 C7 -14.8(4) . .
Li1 N1 C6 C7 115.0(3) . .
Li2 N1 C6 C7 -175.0(3) . .
Si1 N1 C6 Li1 -129.8(3) . .
Li2 N1 C6 Li1 70.0(2) . .
N1 C6 C7 C8 -176.6(3) . .
C11 C6 C7 C8 1.3(4) . .
Li1 C6 C7 C8 -107.3(3) . .
C6 C7 C8 C9 0.7(5) . .
C7 C8 C9 C10 -1.5(5) . .
C8 C9 C10 C11 0.1(5) . .
C9 C10 C11 C6 2.1(5) . .
N1 C6 C11 C10 175.3(3) . .
C7 C6 C11 C10 -2.8(4) . .
Li1 C6 C11 C10 129.1(3) . .
Si2 N2 C14 C19 -33.2(4) . .
Li1 N2 C14 C19 -173.1(3) . .
Li2 N2 C14 C19 104.3(4) . .
Si2 N2 C14 C15 149.1(2) . .
Li1 N2 C14 C15 9.2(4) . .
Li2 N2 C14 C15 -73.3(3) . .
N2 C14 C15 C16 176.6(3) . .
C19 C14 C15 C16 -1.2(5) . .
C14 C15 C16 C17 0.3(6) . .
C15 C16 C17 C18 0.9(6) . .
C16 C17 C18 C19 -1.2(7) . .
C17 C18 C19 C14 0.2(7) . .
N2 C14 C19 C18 -176.8(4) . .
C15 C14 C19 C18 1.0(6) . .
Si3 N3 C22 C23 150.1(2) . .
Li3 N3 C22 C23 -6.5(4) . .
Li3 N3 C22 C23 -77.6(3) 2_667 .
Si3 N3 C22 C27 -32.1(4) . .
Li3 N3 C22 C27 171.3(3) . .
Li3 N3 C22 C27 100.2(3) 2_667 .
Si3 N3 C22 Li3 -132.3(3) . 2_667
Li3 N3 C22 Li3 71.0(3) . 2_667
N3 C22 C23 C24 178.6(3) . .
C27 C22 C23 C24 0.6(5) . .
Li3 C22 C23 C24 123.5(4) 2_667 .
C22 C23 C24 C25 -0.1(6) . .
C23 C24 C25 C26 -0.4(6) . .
C24 C25 C26 C27 0.5(5) . .
C25 C26 C27 C22 0.0(5) . .
N3 C22 C27 C26 -178.4(3) . .
C23 C22 C27 C26 -0.5(4) . .
Li3 C22 C27 C26 -112.6(3) 2_667 .
C29 O1 C28 C29 58.1(4) . 2_776
Li1 O1 C28 C29 -102.2(3) . 2_776
C28 O1 C29 C28 -58.0(4) . 2_776
Li1 O1 C29 C28 100.9(3) . 2_776
C31 O2 C30 C31 -58.0(4) . 2_777
Li2 O2 C30 C31 120.1(3) . 2_777
C30 O2 C31 C30 58.6(4) . 2_777
Li2 O2 C31 C30 -119.4(3) . 2_777
C35 O3 C32 C33 -57.9(3) . .
Li3 O3 C32 C33 130.4(3) . .
C34 O4 C33 C32 -56.7(3) . .
O3 C32 C33 O4 57.3(3) . .
C33 O4 C34 C35 57.4(4) . .
C32 O3 C35 C34 58.4(3) . .
Li3 O3 C35 C34 -129.2(3) . .
O4 C34 C35 O3 -58.7(4) . .
C29 O1 Li1 N2 -179.3(3) . .
C28 O1 Li1 N2 -22.4(4) . .
C29 O1 Li1 N1 -3.0(5) . .
C28 O1 Li1 N1 153.9(3) . .
C29 O1 Li1 C6 -31.3(4) . .
C28 O1 Li1 C6 125.5(3) . .
C29 O1 Li1 Si2 145.4(2) . .
C28 O1 Li1 Si2 -57.7(3) . .
C31 O2 Li2 N1 12.1(4) . .
C30 O2 Li2 N1 -165.6(3) . .
C31 O2 Li2 N2 141.6(3) . .
C30 O2 Li2 N2 -36.1(4) . .
C31 O2 Li2 Li1 81.0(5) . .
C30 O2 Li2 Li1 -96.8(5) . .
C31 O2 Li2 P -102.1(3) . .
C30 O2 Li2 P 80.2(4) . .
C31 O2 Li2 Si2 175.2(2) . .
C30 O2 Li2 Si2 -2.6(4) . .
C35 O3 Li3 N3 -56.5(5) . .
C32 O3 Li3 N3 114.4(4) . .
C35 O3 Li3 N3 117.9(4) . 2_667
C32 O3 Li3 N3 -71.2(4) . 2_667
C35 O3 Li3 C22 147.9(2) . 2_667
C32 O3 Li3 C22 -41.3(3) . 2_667
C35 O3 Li3 Si3 -86.0(3) . .
C32 O3 Li3 Si3 84.9(3) . .
C39 O5 C36 C37 56.4(7) . .
O5 C36 C37 O6 -56.8(6) . .
C38 O6 C37 C36 56.0(6) . .
C37 O6 C38 C39 -54.3(6) . .
C36 O5 C39 C38 -55.1(6) . .
O6 C38 C39 O5 55.2(6) . .
loop_
_cell_oxdiff_twin_id
_cell_oxdiff_twin_matrix_11
_cell_oxdiff_twin_matrix_12
_cell_oxdiff_twin_matrix_13
_cell_oxdiff_twin_matrix_21
_cell_oxdiff_twin_matrix_22
_cell_oxdiff_twin_matrix_23
_cell_oxdiff_twin_matrix_31
_cell_oxdiff_twin_matrix_32
_cell_oxdiff_twin_matrix_33
1 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000
2 -0.0470 -0.9504 -0.0014 -1.0481 0.0454 -0.0001 0.2626 -0.2600 -0.9993
loop_
_diffrn_oxdiff_twin_id
_diffrn_oxdiff_twin_ratio
_diffrn_oxdiff_twin_reflns_isolated
_diffrn_oxdiff_twin_reflns_overlapped
1 0.6104 60518 7180
2 0.3896 0 7180
