Supplementary Material (ESI) for Chemical Communications
This journal is © The Royal Society of Chemistry 2002

data_global

_journal_coden_Cambridge      182

loop_
_publ_author_name
_publ_author_address
'Chivers, Tristram' 
; 
Department of Chemistry
University of Calgary
Calgary Alberta T2N 1N4
Canada
;

'Armstrong, Andrea' 
; 
Department of Chemistry
University of Calgary
Calgary Alberta T2N 1N4
Canada
;

'Krahn, Mark' 
; 
Department of Chemistry
University of Calgary
Calgary Alberta T2N 1N4
Canada
;

'Parvez, Masood' 
; 
Department of Chemistry
University of Calgary
Calgary Alberta T2N 1N4
Canada
;

'Schatte, Gabriele' 
; 
Department of Chemistry
University of Calgary
Calgary Alberta T2N 1N4
Canada
;

_publ_contact_author_name         'Dr Tristram Chivers'
_publ_contact_author_address 
;
Department of Chemistry
University of Calgary
Calgary Alberta T2N 1N4
Canada
;
_publ_contact_author_email        chivers@ucalgary.ca
_publ_contact_author_fax          '001 403 289 9488'
_publ_contact_author_phone        '001 403 220 5741'
_publ_contact_letter
; 
To: Cambridge Crystallographic Data Centre
Please accept the following CIF file which is being submitted
in support of an upcoming communication to be published in
Chem. Commun..
Please forward any questions concerning 
this CIF to Dr. Gabriele Schatte
(schatte@ucalgary.ca).
;
_publ_requested_journal
'Chem. Commun.'

# TITLE AND AUTHOR LIST

_publ_section_title
; 
Syntheses and Structures of an Unsolvated Tetrakisimidophosphate
{Li3[P(NtBu)3(NSiMe3)]}2 and the Face-sharing Double-cubane
{Li2(THF)[P(O)(NtBu)2(NHtBu)]}2
;

_publ_section_acknowledgements
; 
NSERC (financial support)
Dr. R. McDonald (University of Alberta, Canada; for X-ray
data collection)
; 

data_3

_database_code_CSD	190648

_audit_creation_method            'manual editing of SHELXL template'

_chemical_name_systematic
;
?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          'C32 H72 Li4 N6 O4 P2'
_chemical_formula_sum             'C32 H72 Li4 N6 O4 P2'
_chemical_formula_weight          694.66

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
'C'  'C'   0.0033   0.0016
'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'  -0.0003   0.0001
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'N'  'N'   0.0061   0.0033
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'O'  'O'   0.0106   0.0060
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'P'  'P'   0.1023   0.0942
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

# CRYSTAL DATA

_symmetry_cell_setting           'Triclinic'
_symmetry_space_group_name_H-M   'P-1   '

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                    10.3775(15)
_cell_length_b                    10.5873(16)
_cell_length_c                    11.5111(17)
_cell_angle_alpha                 103.906(2)
_cell_angle_beta                  92.088(2)
_cell_angle_gamma                 119.424(2)
_cell_volume                      1051.3(3)
_cell_formula_units_Z             1
_cell_measurement_temperature     193(2)
_cell_measurement_reflns_used     3012
_cell_measurement_theta_min       ?
_cell_measurement_theta_max       ?

_exptl_crystal_description       'fragment'
_exptl_crystal_colour            'colorless'
_exptl_crystal_size_max           0.43
_exptl_crystal_size_mid           0.40
_exptl_crystal_size_min           0.17
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.097
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              380
_exptl_absorpt_coefficient_mu     0.142
_exptl_absorpt_correction_type    'Gaussian integration'
_exptl_absorpt_correction_T_min   0.9302
_exptl_absorpt_correction_T_max   0.9766
_exptl_absorpt_process_details    
;
(a) Busing, W. R. & Levy, H. A. (1957) Acta Cryst. 10, 180-182.
(b) Coppens, P., Leiserowitz, L. & Rabinovich, D. (1965) Acta Cryst.
18, 1035-1038.
;
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1.00    0.00    0.00    0.0850
-1.00    0.00    0.00    0.0850
-1.00    2.00   -1.00    0.2150
1.00   -2.00    1.00    0.2150
1.00    1.00   -2.00    0.1550
1.00   -1.00    1.00    0.1750
0.00    0.00    1.00    0.1800
1.00   -2.00   -2.00    0.2000

_exptl_special_details
;
?
;

# EXPERIMENTAL DATA

_diffrn_ambient_temperature       193(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source          'fine-focus rotating anode'
_diffrn_radiation_monochromator   graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean  ?
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         'no decay'
_diffrn_reflns_number             5177
_diffrn_reflns_av_R_equivalents   0.0270
_diffrn_reflns_av_sigmaI/netI     0.0755
_diffrn_reflns_limit_h_min        -11
_diffrn_reflns_limit_h_max        12
_diffrn_reflns_limit_k_min        -12
_diffrn_reflns_limit_k_max        13
_diffrn_reflns_limit_l_min        -12
_diffrn_reflns_limit_l_max        14
_diffrn_reflns_theta_min          1.85
_diffrn_reflns_theta_max          26.42
_reflns_number_total              4223
_reflns_number_gt                 2837
_reflns_threshold_expression      >2sigma(I)

_computing_data_collection      'Bruker SMART'
_computing_cell_refinement      'Bruker SMART'
_computing_data_reduction       'Bruker SHELXTL'
_computing_structure_solution   'Bruker SHELXTL'
_computing_structure_refinement 'Bruker SHELXTL'
_computing_molecular_graphics   'Bruker SHELXTL'
_computing_publication_material 'Bruker SHELXTL'

# REFINEMENT DATA

_refine_special_details
;
Refinement of F^2^ against ALL reflections.  The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0825P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     mixed
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        ?
_refine_ls_number_reflns          4223
_refine_ls_number_parameters      217
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0854
_refine_ls_R_factor_gt            0.0552
_refine_ls_wR_factor_ref          0.1534
_refine_ls_wR_factor_gt           0.1392
_refine_ls_goodness_of_fit_ref    0.973
_refine_ls_restrained_S_all       0.973
_refine_ls_shift/su_max           0.000
_refine_ls_shift/su_mean          0.000

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.04990(7) 0.07562(7) 0.34491(5) 0.02520(19) Uani 1 1 d . . .
O1 O 0.09058(16) 0.15932(17) 0.48323(13) 0.0273(4) Uani 1 1 d . . .
O2 O 0.1697(2) 0.41952(19) 0.75056(16) 0.0440(5) Uani 1 1 d . . .
N1 N 0.1299(2) 0.2072(2) 0.27200(17) 0.0303(5) Uani 1 1 d . . .
H1N H 0.1475 0.1750 0.2000 0.036 Uiso 1 1 calc R . .
N2 N 0.1072(2) -0.0441(2) 0.31734(17) 0.0256(4) Uani 1 1 d . . .
N3 N -0.1315(2) -0.0233(2) 0.31867(17) 0.0281(5) Uani 1 1 d . . .
C10 C 0.1751(3) 0.3692(3) 0.3105(2) 0.0347(6) Uani 1 1 d . . .
C11 C 0.0618(3) 0.3955(3) 0.3766(3) 0.0462(7) Uani 1 1 d . . .
H11A H -0.0375 0.3348 0.3236 0.055 Uiso 1 1 calc R . .
H11B H 0.0939 0.5033 0.3974 0.055 Uiso 1 1 calc R . .
H11C H 0.0560 0.3653 0.4512 0.055 Uiso 1 1 calc R . .
C12 C 0.3292(3) 0.4643(3) 0.3942(3) 0.0559(8) Uani 1 1 d . . .
H12A H 0.4027 0.4475 0.3527 0.067 Uiso 1 1 calc R . .
H12B H 0.3225 0.4343 0.4690 0.067 Uiso 1 1 calc R . .
H12C H 0.3613 0.5721 0.4146 0.067 Uiso 1 1 calc R . .
C13 C 0.1867(4) 0.4181(3) 0.1954(3) 0.0548(8) Uani 1 1 d . . .
H13A H 0.0883 0.3580 0.1413 0.066 Uiso 1 1 calc R . .
H13B H 0.2604 0.4018 0.1537 0.066 Uiso 1 1 calc R . .
H13C H 0.2190 0.5260 0.2170 0.066 Uiso 1 1 calc R . .
C20 C 0.2569(3) -0.0201(3) 0.3003(2) 0.0330(6) Uani 1 1 d . . .
C21 C 0.3893(3) 0.1318(3) 0.3811(3) 0.0479(8) Uani 1 1 d . . .
H21A H 0.3856 0.2156 0.3623 0.057 Uiso 1 1 calc R . .
H21B H 0.4842 0.1381 0.3658 0.057 Uiso 1 1 calc R . .
H21C H 0.3826 0.1387 0.4669 0.057 Uiso 1 1 calc R . .
C22 C 0.2733(3) -0.0329(4) 0.1674(3) 0.0520(8) Uani 1 1 d . . .
H22A H 0.1900 -0.1303 0.1151 0.062 Uiso 1 1 calc R . .
H22B H 0.3690 -0.0272 0.1559 0.062 Uiso 1 1 calc R . .
H22C H 0.2716 0.0504 0.1459 0.062 Uiso 1 1 calc R . .
C23 C 0.2663(3) -0.1475(3) 0.3324(3) 0.0547(8) Uani 1 1 d . . .
H23A H 0.1827 -0.2459 0.2818 0.066 Uiso 1 1 calc R . .
H23B H 0.2602 -0.1387 0.4185 0.066 Uiso 1 1 calc R . .
H23C H 0.3620 -0.1396 0.3175 0.066 Uiso 1 1 calc R . .
C30 C -0.2356(3) -0.0855(3) 0.2022(2) 0.0342(6) Uani 1 1 d . . .
C31 C -0.2733(4) 0.0307(4) 0.1803(3) 0.0560(9) Uani 1 1 d . . .
H31A H -0.3107 0.0656 0.2506 0.067 Uiso 1 1 calc R . .
H31B H -0.3508 -0.0166 0.1071 0.067 Uiso 1 1 calc R . .
H31C H -0.1826 0.1174 0.1694 0.067 Uiso 1 1 calc R . .
C32 C -0.1781(3) -0.1382(4) 0.0921(2) 0.0501(8) Uani 1 1 d . . .
H32A H -0.1528 -0.2122 0.1050 0.060 Uiso 1 1 calc R . .
H32B H -0.0882 -0.0508 0.0810 0.060 Uiso 1 1 calc R . .
H32C H -0.2564 -0.1855 0.0193 0.060 Uiso 1 1 calc R . .
C33 C -0.3814(3) -0.2216(4) 0.2133(3) 0.0569(9) Uani 1 1 d . . .
H33A H -0.4188 -0.1894 0.2846 0.068 Uiso 1 1 calc R . .
H33B H -0.3617 -0.3006 0.2224 0.068 Uiso 1 1 calc R . .
H33C H -0.4570 -0.2621 0.1399 0.068 Uiso 1 1 calc R . .
C41 C 0.2966(3) 0.5507(3) 0.7340(3) 0.0549(8) Uani 1 1 d . . .
H41A H 0.2636 0.5993 0.6862 0.066 Uiso 1 1 calc R . .
H41B H 0.3642 0.5230 0.6911 0.066 Uiso 1 1 calc R . .
C42 C 0.3740(4) 0.6543(4) 0.8592(3) 0.0767(12) Uani 1 1 d . . .
H42A H 0.4632 0.6495 0.8849 0.092 Uiso 1 1 calc R . .
H42B H 0.4071 0.7604 0.8627 0.092 Uiso 1 1 calc R . .
C43 C 0.2636(4) 0.6015(5) 0.9377(3) 0.0985(16) Uani 1 1 d . . .
H43A H 0.2432 0.6822 0.9774 0.118 Uiso 1 1 calc R . .
H43B H 0.3017 0.5740 1.0018 0.118 Uiso 1 1 calc R . .
C44 C 0.1261(3) 0.4684(3) 0.8603(3) 0.0507(8) Uani 1 1 d . . .
H44A H 0.0830 0.3871 0.9004 0.061 Uiso 1 1 calc R . .
H44B H 0.0501 0.4954 0.8435 0.061 Uiso 1 1 calc R . .
Li1 Li -0.1364(5) 0.0011(5) 0.4894(4) 0.0336(9) Uani 1 1 d . . .
Li2 Li 0.0915(4) 0.2083(4) 0.6566(4) 0.0330(10) Uani 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
P1 0.0270(3) 0.0288(3) 0.0236(3) 0.0095(2) 0.0074(2) 0.0162(3)
O1 0.0298(9) 0.0313(9) 0.0228(9) 0.0086(7) 0.0071(7) 0.0168(7)
O2 0.0450(11) 0.0319(10) 0.0407(11) 0.0044(8) 0.0131(8) 0.0119(8)
N1 0.0426(12) 0.0303(11) 0.0250(11) 0.0108(8) 0.0141(9) 0.0223(9)
N2 0.0269(10) 0.0274(10) 0.0269(10) 0.0108(8) 0.0087(8) 0.0157(8)
N3 0.0242(10) 0.0380(11) 0.0240(10) 0.0111(8) 0.0050(8) 0.0165(9)
C10 0.0438(15) 0.0320(13) 0.0343(14) 0.0144(11) 0.0138(11) 0.0215(12)
C11 0.0601(19) 0.0408(16) 0.0511(18) 0.0164(13) 0.0215(14) 0.0337(14)
C12 0.0500(18) 0.0373(16) 0.068(2) 0.0071(14) 0.0090(15) 0.0174(14)
C13 0.089(2) 0.0480(17) 0.0528(19) 0.0303(14) 0.0331(17) 0.0457(17)
C20 0.0307(13) 0.0335(13) 0.0375(14) 0.0105(11) 0.0114(11) 0.0182(11)
C21 0.0271(14) 0.0465(17) 0.064(2) 0.0107(14) 0.0068(13) 0.0169(12)
C22 0.0492(18) 0.066(2) 0.0483(18) 0.0154(15) 0.0256(14) 0.0345(15)
C23 0.0421(17) 0.0522(18) 0.086(2) 0.0280(17) 0.0175(15) 0.0327(14)
C30 0.0327(13) 0.0464(15) 0.0256(13) 0.0101(11) 0.0018(10) 0.0223(12)
C31 0.063(2) 0.068(2) 0.0469(18) 0.0122(15) -0.0066(15) 0.0442(17)
C32 0.0509(17) 0.071(2) 0.0300(15) 0.0082(14) 0.0015(13) 0.0363(15)
C33 0.0354(16) 0.068(2) 0.0483(18) 0.0145(15) -0.0052(13) 0.0146(14)
C41 0.0511(18) 0.0478(17) 0.056(2) 0.0193(14) 0.0185(15) 0.0164(14)
C42 0.065(2) 0.058(2) 0.061(2) 0.0102(17) -0.0062(18) 0.0028(18)
C43 0.085(3) 0.087(3) 0.047(2) -0.0092(19) 0.011(2) 0.001(2)
C44 0.0530(18) 0.0491(17) 0.0487(18) 0.0110(14) 0.0186(14) 0.0262(14)
Li1 0.034(2) 0.045(2) 0.031(2) 0.0140(18) 0.0101(17) 0.0255(19)
Li2 0.035(2) 0.028(2) 0.034(2) 0.0076(17) 0.0041(17) 0.0152(18)

_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix.  The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry.  An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

# MOLECULAR GEOMETRY 

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P1 O1 1.5504(16) . ?
P1 N3 1.6126(19) . ?
P1 N2 1.619(2) . ?
P1 N1 1.677(2) . ?
P1 Li1 2.538(4) 2_556 ?
P1 Li1 2.548(4) . ?
P1 Li2 2.613(4) 2_556 ?
O1 Li2 1.936(4) . ?
O1 Li1 2.061(4) 2_556 ?
O1 Li1 2.134(4) . ?
O2 C44 1.423(3) . ?
O2 C41 1.431(3) . ?
O2 Li2 1.954(4) . ?
N1 C10 1.478(3) . ?
N2 C20 1.475(3) . ?
N2 Li2 2.034(4) 2_556 ?
N2 Li1 2.140(4) 2_556 ?
N3 C30 1.473(3) . ?
N3 Li1 1.925(4) . ?
N3 Li2 2.270(5) 2_556 ?
C10 C13 1.522(4) . ?
C10 C11 1.525(4) . ?
C10 C12 1.530(4) . ?
C20 C23 1.526(4) . ?
C20 C22 1.527(4) . ?
C20 C21 1.535(3) . ?
C20 Li1 2.774(5) 2_556 ?
C30 C32 1.522(4) . ?
C30 C31 1.530(4) . ?
C30 C33 1.531(4) . ?
C41 C42 1.489(4) . ?
C42 C43 1.460(5) . ?
C43 C44 1.464(4) . ?
Li1 O1 2.061(4) 2_556 ?
Li1 N2 2.140(4) 2_556 ?
Li1 P1 2.538(4) 2_556 ?
Li1 Li2 2.579(5) . ?
Li1 Li2 2.690(6) 2_556 ?
Li1 C20 2.774(5) 2_556 ?
Li1 Li1 2.845(8) 2_556 ?
Li2 N2 2.034(4) 2_556 ?
Li2 N3 2.270(5) 2_556 ?
Li2 P1 2.613(4) 2_556 ?
Li2 Li1 2.690(6) 2_556 ?

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
_geom_angle_publ_flag
O1 P1 N3 103.60(9) . . ?
O1 P1 N2 109.80(9) . . ?
N3 P1 N2 106.69(10) . . ?
O1 P1 N1 107.72(9) . . ?
N3 P1 N1 116.59(10) . . ?
N2 P1 N1 112.03(10) . . ?
O1 P1 Li1 54.28(11) . 2_556 ?
N3 P1 Li1 106.23(12) . 2_556 ?
N2 P1 Li1 56.93(11) . 2_556 ?
N1 P1 Li1 136.84(12) . 2_556 ?
O1 P1 Li1 56.65(11) . . ?
N2 P1 Li1 107.82(12) . . ?
N1 P1 Li1 140.15(12) . . ?
Li1 P1 Li1 68.02(15) 2_556 . ?
O1 P1 Li2 101.51(11) . 2_556 ?
N3 P1 Li2 59.49(12) . 2_556 ?
N2 P1 Li2 51.11(11) . 2_556 ?
N1 P1 Li2 150.33(12) . 2_556 ?
Li1 P1 Li2 60.07(13) 2_556 2_556 ?
Li1 P1 Li2 62.81(13) . 2_556 ?
P1 O1 Li2 163.27(15) . . ?
P1 O1 Li1 88.09(13) . 2_556 ?
Li2 O1 Li1 84.54(18) . 2_556 ?
P1 O1 Li1 85.98(13) . . ?
Li2 O1 Li1 78.49(17) . . ?
Li1 O1 Li1 85.38(17) 2_556 . ?
C44 O2 C41 107.3(2) . . ?
C44 O2 Li2 125.5(2) . . ?
C41 O2 Li2 126.5(2) . . ?
C10 N1 P1 129.77(16) . . ?
C20 N2 P1 130.13(16) . . ?
C20 N2 Li2 138.64(19) . 2_556 ?
P1 N2 Li2 90.60(15) . 2_556 ?
C20 N2 Li1 98.61(17) . 2_556 ?
P1 N2 Li1 83.70(13) . 2_556 ?
Li2 N2 Li1 76.28(17) 2_556 2_556 ?
C30 N3 P1 128.38(17) . . ?
C30 N3 Li1 139.6(2) . . ?
P1 N3 Li1 91.71(15) . . ?
C30 N3 Li2 107.43(18) . 2_556 ?
P1 N3 Li2 82.76(13) . 2_556 ?
Li1 N3 Li2 79.30(18) . 2_556 ?
N1 C10 C13 106.8(2) . . ?
N1 C10 C11 112.2(2) . . ?
C13 C10 C11 109.9(2) . . ?
N1 C10 C12 110.1(2) . . ?
C13 C10 C12 108.9(2) . . ?
C11 C10 C12 108.9(2) . . ?
N2 C20 C23 106.7(2) . . ?
N2 C20 C22 110.5(2) . . ?
C23 C20 C22 108.2(2) . . ?
N2 C20 C21 114.5(2) . . ?
C23 C20 C21 107.9(2) . . ?
C22 C20 C21 108.9(2) . . ?
C23 C20 Li1 84.07(19) . 2_556 ?
C22 C20 Li1 159.9(2) . 2_556 ?
C21 C20 Li1 81.21(18) . 2_556 ?
N3 C30 C32 114.2(2) . . ?
N3 C30 C31 110.9(2) . . ?
C32 C30 C31 108.5(2) . . ?
N3 C30 C33 106.6(2) . . ?
C32 C30 C33 108.7(2) . . ?
C31 C30 C33 107.7(2) . . ?
O2 C41 C42 105.1(2) . . ?
C43 C42 C41 105.9(3) . . ?
C42 C43 C44 107.1(3) . . ?
O2 C44 C43 105.9(3) . . ?
N3 Li1 O1 101.69(19) . 2_556 ?
N3 Li1 O1 75.34(16) . . ?
O1 Li1 O1 94.62(17) 2_556 . ?
N3 Li1 N2 171.7(2) . 2_556 ?
O1 Li1 N2 76.23(15) 2_556 2_556 ?
O1 Li1 N2 96.72(17) . 2_556 ?
N3 Li1 P1 136.8(2) . 2_556 ?
O1 Li1 P1 37.63(8) 2_556 2_556 ?
O1 Li1 P1 91.29(15) . 2_556 ?
N2 Li1 P1 39.37(9) 2_556 2_556 ?
N3 Li1 P1 39.24(10) . . ?
O1 Li1 P1 92.71(16) 2_556 . ?
O1 Li1 P1 37.37(8) . . ?
N2 Li1 P1 132.49(19) 2_556 . ?
P1 Li1 P1 111.98(15) 2_556 . ?
N3 Li1 Li2 122.4(2) . . ?
O1 Li1 Li2 89.73(17) 2_556 . ?
O1 Li1 Li2 47.34(13) . . ?
N2 Li1 Li2 50.01(14) 2_556 . ?
P1 Li1 Li2 61.42(13) 2_556 . ?
P1 Li1 Li2 84.56(16) . . ?
N3 Li1 Li2 56.00(15) . 2_556 ?
O1 Li1 Li2 45.75(13) 2_556 2_556 ?
O1 Li1 Li2 85.31(16) . 2_556 ?
N2 Li1 Li2 121.8(2) 2_556 2_556 ?
P1 Li1 Li2 82.51(15) 2_556 2_556 ?
P1 Li1 Li2 59.78(13) . 2_556 ?
Li2 Li1 Li2 114.68(17) . 2_556 ?
N3 Li1 C20 156.1(2) . 2_556 ?
O1 Li1 C20 93.20(16) 2_556 2_556 ?
O1 Li1 C20 122.32(18) . 2_556 ?
N2 Li1 C20 31.70(9) 2_556 2_556 ?
P1 Li1 C20 63.60(11) 2_556 2_556 ?
P1 Li1 C20 159.35(18) . 2_556 ?
Li2 Li1 C20 75.70(15) . 2_556 ?
Li2 Li1 C20 134.72(19) 2_556 2_556 ?
N3 Li1 Li1 87.5(2) . 2_556 ?
O1 Li1 Li1 48.38(13) 2_556 2_556 ?
O1 Li1 Li1 46.24(13) . 2_556 ?
N2 Li1 Li1 85.14(19) 2_556 2_556 ?
P1 Li1 Li1 56.16(14) 2_556 2_556 ?
P1 Li1 Li1 55.82(14) . 2_556 ?
Li2 Li1 Li1 59.22(17) . 2_556 ?
Li2 Li1 Li1 55.46(16) 2_556 2_556 ?
C20 Li1 Li1 116.2(2) 2_556 2_556 ?
O1 Li2 O2 119.1(2) . . ?
O1 Li2 N2 107.11(18) . 2_556 ?
O2 Li2 N2 118.8(2) . 2_556 ?
O1 Li2 N3 94.36(18) . 2_556 ?
O2 Li2 N3 133.9(2) . 2_556 ?
N2 Li2 N3 73.87(15) 2_556 2_556 ?
O1 Li2 Li1 54.17(14) . . ?
O2 Li2 Li1 136.9(2) . . ?
N2 Li2 Li1 53.70(14) 2_556 . ?
N3 Li2 Li1 87.68(16) 2_556 . ?
O1 Li2 P1 93.76(15) . 2_556 ?
O2 Li2 P1 146.8(2) . 2_556 ?
N2 Li2 P1 38.29(9) 2_556 2_556 ?
N3 Li2 P1 37.75(8) 2_556 2_556 ?
Li1 Li2 P1 58.52(12) . 2_556 ?
O1 Li2 Li1 49.72(13) . 2_556 ?
O2 Li2 Li1 149.1(2) . 2_556 ?
N2 Li2 Li1 91.40(17) 2_556 2_556 ?
N3 Li2 Li1 44.69(13) 2_556 2_556 ?
Li1 Li2 Li1 65.32(17) . 2_556 ?
P1 Li2 Li1 57.41(12) 2_556 2_556 ?

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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N3 P1 O1 Li2 36.6(6) . . . . ?
N2 P1 O1 Li2 -77.1(6) . . . . ?
N1 P1 O1 Li2 160.7(5) . . . . ?
Li1 P1 O1 Li2 -63.8(6) 2_556 . . . ?
Li1 P1 O1 Li2 21.7(5) . . . . ?
Li2 P1 O1 Li2 -24.5(6) 2_556 . . . ?
N3 P1 O1 Li1 100.38(15) . . . 2_556 ?
N2 P1 O1 Li1 -13.27(15) . . . 2_556 ?
N1 P1 O1 Li1 -135.52(14) . . . 2_556 ?
Li1 P1 O1 Li1 85.50(17) . . . 2_556 ?
Li2 P1 O1 Li1 39.31(16) 2_556 . . 2_556 ?
N3 P1 O1 Li1 14.88(14) . . . . ?
N2 P1 O1 Li1 -98.77(14) . . . . ?
N1 P1 O1 Li1 138.99(14) . . . . ?
Li1 P1 O1 Li1 -85.50(17) 2_556 . . . ?
Li2 P1 O1 Li1 -46.19(15) 2_556 . . . ?
O1 P1 N1 C10 -24.7(2) . . . . ?
N3 P1 N1 C10 91.1(2) . . . . ?
N2 P1 N1 C10 -145.6(2) . . . . ?
Li1 P1 N1 C10 -81.0(3) 2_556 . . . ?
Li1 P1 N1 C10 34.1(3) . . . . ?
Li2 P1 N1 C10 165.6(2) 2_556 . . . ?
O1 P1 N2 C20 -83.1(2) . . . . ?
N3 P1 N2 C20 165.23(19) . . . . ?
N1 P1 N2 C20 36.5(2) . . . . ?
Li1 P1 N2 C20 -96.0(2) 2_556 . . . ?
Li1 P1 N2 C20 -143.3(2) . . . . ?
Li2 P1 N2 C20 -172.1(3) 2_556 . . . ?
O1 P1 N2 Li2 88.98(14) . . . 2_556 ?
N3 P1 N2 Li2 -22.67(15) . . . 2_556 ?
N1 P1 N2 Li2 -151.38(14) . . . 2_556 ?
Li1 P1 N2 Li2 76.13(17) 2_556 . . 2_556 ?
Li1 P1 N2 Li2 28.84(16) . . . 2_556 ?
O1 P1 N2 Li1 12.85(14) . . . 2_556 ?
N3 P1 N2 Li1 -98.80(14) . . . 2_556 ?
N1 P1 N2 Li1 132.49(14) . . . 2_556 ?
Li1 P1 N2 Li1 -47.3(2) . . . 2_556 ?
Li2 P1 N2 Li1 -76.13(17) 2_556 . . 2_556 ?
O1 P1 N3 C30 158.0(2) . . . . ?
N2 P1 N3 C30 -86.2(2) . . . . ?
N1 P1 N3 C30 39.9(2) . . . . ?
Li1 P1 N3 C30 -145.8(2) 2_556 . . . ?
Li1 P1 N3 C30 174.5(3) . . . . ?
Li2 P1 N3 C30 -106.5(2) 2_556 . . . ?
O1 P1 N3 Li1 -16.50(16) . . . . ?
N2 P1 N3 Li1 99.37(16) . . . . ?
N1 P1 N3 Li1 -134.62(15) . . . . ?
Li1 P1 N3 Li1 39.8(2) 2_556 . . . ?
Li2 P1 N3 Li1 78.99(18) 2_556 . . . ?
O1 P1 N3 Li2 -95.49(13) . . . 2_556 ?
N2 P1 N3 Li2 20.38(14) . . . 2_556 ?
N1 P1 N3 Li2 146.39(13) . . . 2_556 ?
Li1 P1 N3 Li2 -39.22(15) 2_556 . . 2_556 ?
Li1 P1 N3 Li2 -78.99(18) . . . 2_556 ?
P1 N1 C10 C13 -159.6(2) . . . . ?
P1 N1 C10 C11 -39.2(3) . . . . ?
P1 N1 C10 C12 82.3(3) . . . . ?
P1 N2 C20 C23 155.68(19) . . . . ?
Li2 N2 C20 C23 -12.3(4) 2_556 . . . ?
Li1 N2 C20 C23 66.7(2) 2_556 . . . ?
P1 N2 C20 C22 -87.0(3) . . . . ?
Li2 N2 C20 C22 105.0(3) 2_556 . . . ?
Li1 N2 C20 C22 -176.0(2) 2_556 . . . ?
P1 N2 C20 C21 36.3(3) . . . . ?
Li2 N2 C20 C21 -131.7(3) 2_556 . . . ?
Li1 N2 C20 C21 -52.7(3) 2_556 . . . ?
P1 N2 C20 Li1 89.0(2) . . . 2_556 ?
Li2 N2 C20 Li1 -79.0(3) 2_556 . . 2_556 ?
P1 N3 C30 C32 35.5(3) . . . . ?
Li1 N3 C30 C32 -153.0(3) . . . . ?
Li2 N3 C30 C32 -59.1(3) 2_556 . . . ?
P1 N3 C30 C31 -87.4(3) . . . . ?
Li1 N3 C30 C31 84.0(4) . . . . ?
Li2 N3 C30 C31 178.0(2) 2_556 . . . ?
P1 N3 C30 C33 155.6(2) . . . . ?
Li1 N3 C30 C33 -33.0(4) . . . . ?
Li2 N3 C30 C33 61.0(3) 2_556 . . . ?
C44 O2 C41 C42 29.3(3) . . . . ?
Li2 O2 C41 C42 -141.2(3) . . . . ?
O2 C41 C42 C43 -18.3(4) . . . . ?
C41 C42 C43 C44 1.1(5) . . . . ?
C41 O2 C44 C43 -28.8(4) . . . . ?
Li2 O2 C44 C43 141.8(3) . . . . ?
C42 C43 C44 O2 16.6(5) . . . . ?
C30 N3 Li1 O1 106.9(3) . . . 2_556 ?
P1 N3 Li1 O1 -79.81(17) . . . 2_556 ?
Li2 N3 Li1 O1 2.50(17) 2_556 . . 2_556 ?
C30 N3 Li1 O1 -161.3(3) . . . . ?
P1 N3 Li1 O1 11.97(11) . . . . ?
Li2 N3 Li1 O1 94.27(15) 2_556 . . . ?
C30 N3 Li1 P1 122.8(3) . . . 2_556 ?
P1 N3 Li1 P1 -63.9(3) . . . 2_556 ?
Li2 N3 Li1 P1 18.4(3) 2_556 . . 2_556 ?
C30 N3 Li1 P1 -173.3(3) . . . . ?
Li2 N3 Li1 P1 82.30(13) 2_556 . . . ?
C30 N3 Li1 Li2 -155.9(3) . . . . ?
P1 N3 Li1 Li2 17.4(2) . . . . ?
Li2 N3 Li1 Li2 99.7(2) 2_556 . . . ?
C30 N3 Li1 Li2 104.4(3) . . . 2_556 ?
P1 N3 Li1 Li2 -82.30(13) . . . 2_556 ?
C30 N3 Li1 C20 -20.6(7) . . . 2_556 ?
P1 N3 Li1 C20 152.7(5) . . . 2_556 ?
Li2 N3 Li1 C20 -125.0(5) 2_556 . . 2_556 ?
C30 N3 Li1 Li1 153.4(3) . . . 2_556 ?
P1 N3 Li1 Li1 -33.26(18) . . . 2_556 ?
Li2 N3 Li1 Li1 49.04(18) 2_556 . . 2_556 ?
P1 O1 Li1 N3 -12.48(12) . . . . ?
Li2 O1 Li1 N3 173.76(19) . . . . ?
Li1 O1 Li1 N3 -100.89(18) 2_556 . . . ?
P1 O1 Li1 O1 88.41(14) . . . 2_556 ?
Li2 O1 Li1 O1 -85.35(18) . . . 2_556 ?
Li1 O1 Li1 O1 0.0 2_556 . . 2_556 ?
P1 O1 Li1 N2 165.06(15) . . . 2_556 ?
Li2 O1 Li1 N2 -8.71(18) . . . 2_556 ?
Li1 O1 Li1 N2 76.65(17) 2_556 . . 2_556 ?
P1 O1 Li1 P1 125.95(11) . . . 2_556 ?
Li2 O1 Li1 P1 -47.81(16) . . . 2_556 ?
Li1 O1 Li1 P1 37.54(9) 2_556 . . 2_556 ?
Li2 O1 Li1 P1 -173.76(16) . . . . ?
Li1 O1 Li1 P1 -88.41(14) 2_556 . . . ?
P1 O1 Li1 Li2 173.76(16) . . . . ?
Li1 O1 Li1 Li2 85.35(18) 2_556 . . . ?
P1 O1 Li1 Li2 43.57(13) . . . 2_556 ?
Li2 O1 Li1 Li2 -130.19(14) . . . 2_556 ?
Li1 O1 Li1 Li2 -44.84(13) 2_556 . . 2_556 ?
P1 O1 Li1 C20 -174.85(19) . . . 2_556 ?
Li2 O1 Li1 C20 11.4(2) . . . 2_556 ?
Li1 O1 Li1 C20 96.7(2) 2_556 . . 2_556 ?
P1 O1 Li1 Li1 88.41(14) . . . 2_556 ?
Li2 O1 Li1 Li1 -85.35(18) . . . 2_556 ?
O1 P1 Li1 N3 160.70(18) . . . . ?
N2 P1 Li1 N3 -96.92(14) . . . . ?
N1 P1 Li1 N3 83.4(2) . . . . ?
Li1 P1 Li1 N3 -138.5(2) 2_556 . . . ?
Li2 P1 Li1 N3 -71.95(16) 2_556 . . . ?
O1 P1 Li1 O1 -94.07(15) . . . 2_556 ?
N3 P1 Li1 O1 105.23(19) . . . 2_556 ?
N2 P1 Li1 O1 8.31(16) . . . 2_556 ?
N1 P1 Li1 O1 -171.37(12) . . . 2_556 ?
Li1 P1 Li1 O1 -33.29(9) 2_556 . . 2_556 ?
Li2 P1 Li1 O1 33.28(13) 2_556 . . 2_556 ?
N3 P1 Li1 O1 -160.70(18) . . . . ?
N2 P1 Li1 O1 102.38(12) . . . . ?
N1 P1 Li1 O1 -77.30(19) . . . . ?
Li1 P1 Li1 O1 60.78(14) 2_556 . . . ?
Li2 P1 Li1 O1 127.35(15) 2_556 . . . ?
O1 P1 Li1 N2 -20.3(2) . . . 2_556 ?
N3 P1 Li1 N2 179.0(3) . . . 2_556 ?
N2 P1 Li1 N2 82.1(3) . . . 2_556 ?
N1 P1 Li1 N2 -97.6(3) . . . 2_556 ?
Li1 P1 Li1 N2 40.46(17) 2_556 . . 2_556 ?
Li2 P1 Li1 N2 107.0(3) 2_556 . . 2_556 ?
O1 P1 Li1 P1 -60.78(14) . . . 2_556 ?
N3 P1 Li1 P1 138.5(2) . . . 2_556 ?
N2 P1 Li1 P1 41.60(17) . . . 2_556 ?
N1 P1 Li1 P1 -138.08(15) . . . 2_556 ?
Li1 P1 Li1 P1 0.0 2_556 . . 2_556 ?
Li2 P1 Li1 P1 66.57(16) 2_556 . . 2_556 ?
O1 P1 Li1 Li2 -4.60(12) . . . . ?
N3 P1 Li1 Li2 -165.3(2) . . . . ?
N2 P1 Li1 Li2 97.78(14) . . . . ?
N1 P1 Li1 Li2 -81.9(2) . . . . ?
Li1 P1 Li1 Li2 56.17(15) 2_556 . . . ?
Li2 P1 Li1 Li2 122.74(14) 2_556 . . . ?
O1 P1 Li1 Li2 -127.35(15) . . . 2_556 ?
N3 P1 Li1 Li2 71.95(16) . . . 2_556 ?
N2 P1 Li1 Li2 -24.97(14) . . . 2_556 ?
N1 P1 Li1 Li2 155.35(17) . . . 2_556 ?
Li1 P1 Li1 Li2 -66.57(16) 2_556 . . 2_556 ?
O1 P1 Li1 C20 12.4(5) . . . 2_556 ?
N3 P1 Li1 C20 -148.3(6) . . . 2_556 ?
N2 P1 Li1 C20 114.8(5) . . . 2_556 ?
N1 P1 Li1 C20 -64.9(6) . . . 2_556 ?
Li1 P1 Li1 C20 73.2(5) 2_556 . . 2_556 ?
Li2 P1 Li1 C20 139.8(6) 2_556 . . 2_556 ?
O1 P1 Li1 Li1 -60.78(14) . . . 2_556 ?
N3 P1 Li1 Li1 138.5(2) . . . 2_556 ?
N2 P1 Li1 Li1 41.60(17) . . . 2_556 ?
N1 P1 Li1 Li1 -138.08(15) . . . 2_556 ?
Li2 P1 Li1 Li1 66.57(16) 2_556 . . 2_556 ?
P1 O1 Li2 O2 -151.1(4) . . . . ?
Li1 O1 Li2 O2 144.7(3) 2_556 . . . ?
Li1 O1 Li2 O2 -129.0(3) . . . . ?
P1 O1 Li2 N2 -12.6(7) . . . 2_556 ?
Li1 O1 Li2 N2 -76.9(2) 2_556 . . 2_556 ?
Li1 O1 Li2 N2 9.52(19) . . . 2_556 ?
P1 O1 Li2 N3 61.8(6) . . . 2_556 ?
Li1 O1 Li2 N3 -2.41(16) 2_556 . . 2_556 ?
Li1 O1 Li2 N3 83.97(17) . . . 2_556 ?
P1 O1 Li2 Li1 -22.1(5) . . . . ?
Li1 O1 Li2 Li1 -86.38(17) 2_556 . . . ?
P1 O1 Li2 P1 24.0(6) . . . 2_556 ?
Li1 O1 Li2 P1 -40.25(15) 2_556 . . 2_556 ?
Li1 O1 Li2 P1 46.13(15) . . . 2_556 ?
P1 O1 Li2 Li1 64.3(5) . . . 2_556 ?
Li1 O1 Li2 Li1 86.38(17) . . . 2_556 ?
C44 O2 Li2 O1 153.0(2) . . . . ?
C41 O2 Li2 O1 -38.1(4) . . . . ?
C44 O2 Li2 N2 19.3(4) . . . 2_556 ?
C41 O2 Li2 N2 -171.8(2) . . . 2_556 ?
C44 O2 Li2 N3 -75.8(4) . . . 2_556 ?
C41 O2 Li2 N3 93.1(4) . . . 2_556 ?
C44 O2 Li2 Li1 85.7(4) . . . . ?
C41 O2 Li2 Li1 -105.5(4) . . . . ?
C44 O2 Li2 P1 -18.0(5) . . . 2_556 ?
C41 O2 Li2 P1 150.9(3) . . . 2_556 ?
C44 O2 Li2 Li1 -147.7(4) . . . 2_556 ?
C41 O2 Li2 Li1 21.2(6) . . . 2_556 ?
N3 Li1 Li2 O1 -7.2(2) . . . . ?
O1 Li1 Li2 O1 96.54(18) 2_556 . . . ?
N2 Li1 Li2 O1 168.7(2) 2_556 . . . ?
P1 Li1 Li2 O1 122.48(17) 2_556 . . . ?
P1 Li1 Li2 O1 3.80(10) . . . . ?
Li2 Li1 Li2 O1 56.92(15) 2_556 . . . ?
C20 Li1 Li2 O1 -170.08(19) 2_556 . . . ?
Li1 Li1 Li2 O1 56.92(15) 2_556 . . . ?
N3 Li1 Li2 O2 89.0(4) . . . . ?
O1 Li1 Li2 O2 -167.3(3) 2_556 . . . ?
O1 Li1 Li2 O2 96.2(3) . . . . ?
N2 Li1 Li2 O2 -95.1(3) 2_556 . . . ?
P1 Li1 Li2 O2 -141.4(3) 2_556 . . . ?
P1 Li1 Li2 O2 100.0(3) . . . . ?
Li2 Li1 Li2 O2 153.1(4) 2_556 . . . ?
C20 Li1 Li2 O2 -73.9(3) 2_556 . . . ?
Li1 Li1 Li2 O2 153.1(4) 2_556 . . . ?
N3 Li1 Li2 N2 -175.8(3) . . . 2_556 ?
O1 Li1 Li2 N2 -72.14(16) 2_556 . . 2_556 ?
O1 Li1 Li2 N2 -168.7(2) . . . 2_556 ?
P1 Li1 Li2 N2 -46.21(10) 2_556 . . 2_556 ?
P1 Li1 Li2 N2 -164.89(19) . . . 2_556 ?
Li2 Li1 Li2 N2 -111.8(2) 2_556 . . 2_556 ?
C20 Li1 Li2 N2 21.23(10) 2_556 . . 2_556 ?
Li1 Li1 Li2 N2 -111.8(2) 2_556 . . 2_556 ?
N3 Li1 Li2 N3 -104.2(2) . . . 2_556 ?
O1 Li1 Li2 N3 -0.52(17) 2_556 . . 2_556 ?
O1 Li1 Li2 N3 -97.06(18) . . . 2_556 ?
N2 Li1 Li2 N3 71.62(15) 2_556 . . 2_556 ?
P1 Li1 Li2 N3 25.42(10) 2_556 . . 2_556 ?
P1 Li1 Li2 N3 -93.26(15) . . . 2_556 ?
Li2 Li1 Li2 N3 -40.15(16) 2_556 . . 2_556 ?
C20 Li1 Li2 N3 92.85(15) 2_556 . . 2_556 ?
Li1 Li1 Li2 N3 -40.15(16) 2_556 . . 2_556 ?
N3 Li1 Li2 P1 -129.6(3) . . . 2_556 ?
O1 Li1 Li2 P1 -25.94(10) 2_556 . . 2_556 ?
O1 Li1 Li2 P1 -122.48(17) . . . 2_556 ?
N2 Li1 Li2 P1 46.21(10) 2_556 . . 2_556 ?
P1 Li1 Li2 P1 -118.68(14) . . . 2_556 ?
Li2 Li1 Li2 P1 -65.57(14) 2_556 . . 2_556 ?
C20 Li1 Li2 P1 67.43(10) 2_556 . . 2_556 ?
Li1 Li1 Li2 P1 -65.57(14) 2_556 . . 2_556 ?
N3 Li1 Li2 Li1 -64.1(2) . . . 2_556 ?
O1 Li1 Li2 Li1 39.63(11) 2_556 . . 2_556 ?
O1 Li1 Li2 Li1 -56.92(15) . . . 2_556 ?
N2 Li1 Li2 Li1 111.8(2) 2_556 . . 2_556 ?
P1 Li1 Li2 Li1 65.57(14) 2_556 . . 2_556 ?
P1 Li1 Li2 Li1 -53.12(12) . . . 2_556 ?
Li2 Li1 Li2 Li1 0.0 2_556 . . 2_556 ?
C20 Li1 Li2 Li1 133.0(2) 2_556 . . 2_556 ?

_diffrn_measured_fraction_theta_max    0.978
_diffrn_reflns_theta_full              26.42
_diffrn_measured_fraction_theta_full   0.978
_refine_diff_density_max    0.267
_refine_diff_density_min   -0.331
_refine_diff_density_rms    0.056


data_Compound_2

_database_code_CSD	190649


_audit_creation_method            SHELXL-97 

#-----------------------------------------------------------------------------
_computing_data_collection                           'COLLECT (Hooft, 1998)'
_computing_cell_refinement            'HKL DENZO (Otwinowski & Minor, 1997)'
_computing_data_reduction             'SCALEPACK (Otwinowski & Minor, 1997)'
_computing_structure_solution                           'SAPI91 (Fan, 1991)'
_computing_structure_refinement                'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material                'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics   	           'TEXSAN (M. S. C., 1994)'
#-----------------------------------------------------------------------------
_chemical_name_systematic      ' ? '
_chemical_name_common          ' ? '
_chemical_melting_point        ' ? '
_chemical_formula_sum          'C15 H36 Li3 N4 P Si'
_chemical_formula_weight          352.36
_chemical_compound_source      'synthesized by authors '

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
'C'  'C'   0.0033   0.0016
'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'
'N'  'N'   0.0061   0.0033
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'P'  'P'   0.1023   0.0942
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'Si'  'Si'   0.0817   0.0704
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'Li'  'Li'  -0.0003   0.0001
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting            trigonal 
_symmetry_space_group_name_H-M    ' R -3 ' 

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                    14.8927(4)
_cell_length_b                    14.8927(4)
_cell_length_c                    16.0178(6)
_cell_angle_alpha                 90.00
_cell_angle_beta                  90.00
_cell_angle_gamma                 120.00
_cell_volume                      3076.66(16)
_cell_formula_units_Z             6
_cell_measurement_temperature     173(2)
_cell_measurement_reflns_used     6543
_cell_measurement_theta_min       1.0
_cell_measurement_theta_max       30.0

_exptl_crystal_description        'prism'
_exptl_crystal_colour             'colourless'
_exptl_crystal_size_max           0.25
_exptl_crystal_size_mid           0.20
_exptl_crystal_size_min           0.15
_exptl_crystal_density_meas       'not measured'
_exptl_crystal_density_diffrn     1.141
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              1152
_exptl_absorpt_coefficient_mu     0.195
_exptl_absorpt_correction_type    'multi-scan'
_exptl_absorpt_correction_T_min   0.9529
_exptl_absorpt_correction_T_max   0.9713
_exptl_absorpt_process_details    '(SORTAV: Blessing, 1997)'


_diffrn_ambient_temperature       173(2)
_diffrn_radiation_wavelength      0.71069
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source          'fine-focus sealed tube'
_diffrn_radiation_monochromator   graphite
_diffrn_measurement_device_type   'Nonius KappaCCD Diffractometer'
_diffrn_measurement_method        ' \w & \f ' 
_diffrn_standards_decay_%         ' < 0.1 '
_diffrn_reflns_number             6937
_diffrn_reflns_av_R_equivalents   0.0324
_diffrn_reflns_av_sigmaI/netI     0.0401
_diffrn_reflns_limit_h_min        -16
_diffrn_reflns_limit_h_max        20
_diffrn_reflns_limit_k_min        -20
_diffrn_reflns_limit_k_max        15
_diffrn_reflns_limit_l_min        -22
_diffrn_reflns_limit_l_max        22
_diffrn_reflns_theta_min          4.37
_diffrn_reflns_theta_max          29.91
_reflns_number_total              1986
_reflns_number_gt                 1642
_reflns_threshold_expression      >2sigma(I)

_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
;
calc w=1/[\s^2^(Fo^2^)+(0.0727P)^2^+1.8196P] where 
P=(Fo^2^+2Fc^2^)/3
;
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     'constr'
_refine_ls_extinction_method      none
_refine_ls_number_reflns          1986
_refine_ls_number_parameters      73
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0501
_refine_ls_R_factor_gt            0.0384
_refine_ls_wR_factor_ref          0.1215
_refine_ls_wR_factor_gt           0.1138
_refine_ls_goodness_of_fit_ref    1.022
_refine_ls_restrained_S_all       1.022
_refine_ls_shift/su_max           0.000
_refine_ls_shift/su_mean          0.000
_refine_diff_density_max          0.331
_refine_diff_density_min         -0.450
_refine_diff_density_rms          0.050
_diffrn_measured_fraction_theta_max    0.996
_diffrn_reflns_theta_full              29.91
_diffrn_measured_fraction_theta_full   0.996

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.0000 0.0000 0.13662(3) 0.01793(16) Uani 1 3 d S . .
Si1 Si 0.0000 0.0000 0.33695(4) 0.02625(18) Uani 1 3 d S . .
N1 N 0.0000 0.0000 0.23340(11) 0.0234(4) Uani 1 3 d S . .
N2 N 0.01398(8) -0.09471(8) 0.09003(6) 0.0197(2) Uani 1 1 d . . .
C1 C 0.05793(9) -0.15212(9) 0.13439(8) 0.0218(3) Uani 1 1 d . . .
C2 C -0.01262(11) -0.22198(10) 0.20418(9) 0.0287(3) Uani 1 1 d . . .
H2A H -0.0820 -0.2683 0.1817 0.043 Uiso 1 1 calc R . .
H2B H -0.0172 -0.1791 0.2485 0.043 Uiso 1 1 calc R . .
H2C H 0.0161 -0.2633 0.2271 0.043 Uiso 1 1 calc R . .
C3 C 0.16676(10) -0.07967(11) 0.16975(9) 0.0298(3) Uani 1 1 d . . .
H3A H 0.2120 -0.0349 0.1251 0.045 Uiso 1 1 calc R . .
H3B H 0.1954 -0.1212 0.1926 0.045 Uiso 1 1 calc R . .
H3C H 0.1623 -0.0368 0.2141 0.045 Uiso 1 1 calc R . .
C4 C 0.06770(11) -0.22250(11) 0.06919(9) 0.0303(3) Uani 1 1 d . . .
H4A H 0.1125 -0.1800 0.0234 0.045 Uiso 1 1 calc R . .
H4B H -0.0011 -0.2717 0.0472 0.045 Uiso 1 1 calc R . .
H4C H 0.0980 -0.2607 0.0954 0.045 Uiso 1 1 calc R . .
C5 C 0.10619(13) -0.01948(14) 0.38196(9) 0.0392(4) Uani 1 1 d . . .
H5A H 0.0994 -0.0842 0.3603 0.059 Uiso 1 1 calc R . .
H5B H 0.1004 -0.0232 0.4430 0.059 Uiso 1 1 calc R . .
H5C H 0.1739 0.0388 0.3659 0.059 Uiso 1 1 calc R . .
Li1 Li -0.12121(17) -0.14419(17) 0.03723(13) 0.0246(4) Uani 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
P1 0.01806(19) 0.01806(19) 0.0177(3) 0.000 0.000 0.00903(10)
Si1 0.0305(2) 0.0305(2) 0.0178(3) 0.000 0.000 0.01523(12)
N1 0.0256(6) 0.0256(6) 0.0189(8) 0.000 0.000 0.0128(3)
N2 0.0220(5) 0.0197(5) 0.0199(5) 0.0009(4) -0.0003(4) 0.0123(4)
C1 0.0220(6) 0.0206(6) 0.0246(6) 0.0025(4) -0.0003(5) 0.0119(5)
C2 0.0310(7) 0.0247(6) 0.0309(7) 0.0068(5) 0.0024(5) 0.0142(5)
C3 0.0226(6) 0.0310(7) 0.0361(7) 0.0020(6) -0.0046(5) 0.0135(5)
C4 0.0360(7) 0.0280(7) 0.0350(7) -0.0003(6) 0.0001(6) 0.0221(6)
C5 0.0446(9) 0.0508(10) 0.0259(7) 0.0006(6) -0.0075(6) 0.0265(8)
Li1 0.0242(10) 0.0225(10) 0.0256(10) -0.0027(8) -0.0013(8) 0.0106(9)

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P1 N1 1.5502(18) . ?
P1 N2 1.6980(10) 3 ?
P1 N2 1.6980(10) 2 ?
P1 N2 1.6980(10) . ?
P1 Li1 2.555(2) 3 ?
P1 Li1 2.555(2) . ?
P1 Li1 2.555(2) 2 ?
Si1 N1 1.6586(18) . ?
Si1 C5 1.8879(15) 2 ?
Si1 C5 1.8879(15) . ?
Si1 C5 1.8879(15) 3 ?
N2 C1 1.4912(15) . ?
N2 Li1 1.957(2) . ?
N2 Li1 2.037(2) 2 ?
N2 Li1 2.093(2) 12 ?
C1 C2 1.5308(17) . ?
C1 C3 1.5372(18) . ?
C1 C4 1.5373(17) . ?
C1 Li1 2.743(2) 2 ?
Li1 N2 2.037(2) 3 ?
Li1 N2 2.093(2) 11 ?
Li1 Li1 2.327(3) 11 ?
Li1 Li1 2.327(3) 12 ?
Li1 C4 2.575(3) 11 ?
Li1 C3 2.733(3) 3 ?
Li1 C1 2.743(2) 3 ?
Li1 Li1 3.461(4) 3 ?
Li1 Li1 3.461(4) 2 ?

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
_geom_angle_publ_flag
N1 P1 N2 116.07(4) . 3 ?
N1 P1 N2 116.07(4) . 2 ?
N2 P1 N2 102.14(4) 3 2 ?
N1 P1 N2 116.07(4) . . ?
N2 P1 N2 102.14(4) 3 . ?
N2 P1 N2 102.14(4) 2 . ?
N1 P1 Li1 128.54(5) . 3 ?
N2 P1 Li1 49.95(6) 3 3 ?
N2 P1 Li1 52.67(6) 2 3 ?
N2 P1 Li1 115.37(6) . 3 ?
N1 P1 Li1 128.54(5) . . ?
N2 P1 Li1 52.67(6) 3 . ?
N2 P1 Li1 115.37(6) 2 . ?
N2 P1 Li1 49.95(6) . . ?
Li1 P1 Li1 85.28(7) 3 . ?
N1 P1 Li1 128.54(5) . 2 ?
N2 P1 Li1 115.37(6) 3 2 ?
N2 P1 Li1 49.95(6) 2 2 ?
N2 P1 Li1 52.67(6) . 2 ?
Li1 P1 Li1 85.28(7) 3 2 ?
Li1 P1 Li1 85.28(7) . 2 ?
N1 Si1 C5 112.45(5) . 2 ?
N1 Si1 C5 112.45(5) . . ?
C5 Si1 C5 106.33(6) 2 . ?
N1 Si1 C5 112.45(5) . 3 ?
C5 Si1 C5 106.33(6) 2 3 ?
C5 Si1 C5 106.33(6) . 3 ?
P1 N1 Si1 180.0 . . ?
C1 N2 P1 122.56(8) . . ?
C1 N2 Li1 130.84(10) . . ?
P1 N2 Li1 88.42(8) . . ?
C1 N2 Li1 100.91(9) . 2 ?
P1 N2 Li1 85.82(7) . 2 ?
Li1 N2 Li1 120.15(13) . 2 ?
C1 N2 Li1 105.54(9) . 12 ?
P1 N2 Li1 129.09(8) . 12 ?
Li1 N2 Li1 70.06(7) . 12 ?
Li1 N2 Li1 68.58(7) 2 12 ?
N2 C1 C2 112.88(10) . . ?
N2 C1 C3 112.59(10) . . ?
C2 C1 C3 109.42(11) . . ?
N2 C1 C4 106.60(10) . . ?
C2 C1 C4 107.43(10) . . ?
C3 C1 C4 107.63(11) . . ?
N2 C1 Li1 46.82(7) . 2 ?
C2 C1 Li1 153.72(10) . 2 ?
C3 C1 Li1 73.35(8) . 2 ?
C4 C1 Li1 95.96(9) . 2 ?
N2 Li1 N2 82.81(10) . 3 ?
N2 Li1 N2 107.29(11) . 11 ?
N2 Li1 N2 104.35(10) 3 11 ?
N2 Li1 Li1 116.88(7) . 11 ?
N2 Li1 Li1 56.86(6) 3 11 ?
N2 Li1 Li1 52.21(10) 11 11 ?
N2 Li1 Li1 57.73(6) . 12 ?
N2 Li1 Li1 115.74(6) 3 12 ?
N2 Li1 Li1 54.56(10) 11 12 ?
Li1 Li1 Li1 96.08(12) 11 12 ?
N2 Li1 P1 41.63(5) . . ?
N2 Li1 P1 41.52(5) 3 . ?
N2 Li1 P1 115.45(10) 11 . ?
Li1 Li1 P1 89.06(6) 11 . ?
Li1 Li1 P1 89.06(6) 12 . ?
N2 Li1 C4 131.48(11) . 11 ?
N2 Li1 C4 144.59(11) 3 11 ?
N2 Li1 C4 61.67(7) 11 11 ?
Li1 Li1 C4 93.69(12) 11 11 ?
Li1 Li1 C4 83.85(12) 12 11 ?
P1 Li1 C4 172.62(10) . 11 ?
N2 Li1 C3 102.77(9) . 3 ?
N2 Li1 C3 61.74(7) 3 3 ?
N2 Li1 C3 144.91(11) 11 3 ?
Li1 Li1 C3 97.90(10) 11 3 ?
Li1 Li1 C3 159.86(13) 12 3 ?
P1 Li1 C3 76.78(7) . 3 ?
C4 Li1 C3 109.55(9) 11 3 ?
N2 Li1 C1 102.99(9) . 3 ?
N2 Li1 C1 32.27(5) 3 3 ?
N2 Li1 C1 120.56(10) 11 3 ?
Li1 Li1 C1 68.59(8) 11 3 ?
Li1 Li1 C1 147.96(8) 12 3 ?
P1 Li1 C1 63.66(6) . 3 ?
C4 Li1 C1 123.72(9) 11 3 ?
C3 Li1 C1 32.61(5) 3 3 ?
N2 Li1 Li1 78.59(6) . 3 ?
N2 Li1 Li1 29.26(7) 3 3 ?
N2 Li1 Li1 78.05(6) 11 3 ?
Li1 Li1 Li1 41.96(6) 11 3 ?
Li1 Li1 Li1 90.0 12 3 ?
P1 Li1 Li1 47.36(4) . 3 ?
C4 Li1 Li1 134.35(7) 11 3 ?
C3 Li1 Li1 90.76(8) 3 3 ?
C1 Li1 Li1 59.50(7) 3 3 ?
N2 Li1 Li1 30.59(7) . 2 ?
N2 Li1 Li1 77.71(6) 3 2 ?
N2 Li1 Li1 79.34(6) 11 2 ?
Li1 Li1 Li1 90.0 11 2 ?
Li1 Li1 Li1 41.96(6) 12 2 ?
P1 Li1 Li1 47.36(4) . 2 ?
C4 Li1 Li1 125.71(9) 11 2 ?
C3 Li1 Li1 123.51(5) 3 2 ?
C1 Li1 Li1 107.93(6) 3 2 ?
Li1 Li1 Li1 60.0 3 2 ?

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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2 P1 N1 Si1 0(29) 3 . . . ?
N2 P1 N1 Si1 0(77) 2 . . . ?
N2 P1 N1 Si1 0(32) . . . . ?
Li1 P1 N1 Si1 0(49) 3 . . . ?
Li1 P1 N1 Si1 0(26) . . . . ?
Li1 P1 N1 Si1 0(57) 2 . . . ?
C5 Si1 N1 P1 0(57) 2 . . . ?
C5 Si1 N1 P1 0(50) . . . . ?
C5 Si1 N1 P1 0(23) 3 . . . ?
N1 P1 N2 C1 -19.67(10) . . . . ?
N2 P1 N2 C1 -146.95(10) 3 . . . ?
N2 P1 N2 C1 107.60(12) 2 . . . ?
Li1 P1 N2 C1 161.84(10) 3 . . . ?
Li1 P1 N2 C1 -139.34(13) . . . . ?
Li1 P1 N2 C1 100.28(11) 2 . . . ?
N1 P1 N2 Li1 119.66(7) . . . . ?
N2 P1 N2 Li1 -7.61(8) 3 . . . ?
N2 P1 N2 Li1 -113.06(7) 2 . . . ?
Li1 P1 N2 Li1 -58.83(9) 3 . . . ?
Li1 P1 N2 Li1 -120.39(13) 2 . . . ?
N1 P1 N2 Li1 -119.95(6) . . . 2 ?
N2 P1 N2 Li1 112.77(6) 3 . . 2 ?
N2 P1 N2 Li1 7.33(8) 2 . . 2 ?
Li1 P1 N2 Li1 61.56(8) 3 . . 2 ?
Li1 P1 N2 Li1 120.39(13) . . . 2 ?
N1 P1 N2 Li1 -177.86(9) . . . 12 ?
N2 P1 N2 Li1 54.87(10) 3 . . 12 ?
N2 P1 N2 Li1 -50.58(10) 2 . . 12 ?
Li1 P1 N2 Li1 3.65(15) 3 . . 12 ?
Li1 P1 N2 Li1 62.48(11) . . . 12 ?
Li1 P1 N2 Li1 -57.91(12) 2 . . 12 ?
P1 N2 C1 C2 67.82(13) . . . . ?
Li1 N2 C1 C2 -52.75(16) . . . . ?
Li1 N2 C1 C2 159.82(11) 2 . . . ?
Li1 N2 C1 C2 -129.60(11) 12 . . . ?
P1 N2 C1 C3 -56.68(13) . . . . ?
Li1 N2 C1 C3 -177.25(12) . . . . ?
Li1 N2 C1 C3 35.33(12) 2 . . . ?
Li1 N2 C1 C3 105.90(12) 12 . . . ?
P1 N2 C1 C4 -174.47(8) . . . . ?
Li1 N2 C1 C4 64.96(15) . . . . ?
Li1 N2 C1 C4 -82.47(11) 2 . . . ?
Li1 N2 C1 C4 -11.89(12) 12 . . . ?
P1 N2 C1 Li1 -92.00(10) . . . 2 ?
Li1 N2 C1 Li1 147.43(16) . . . 2 ?
Li1 N2 C1 Li1 70.58(7) 12 . . 2 ?
C1 N2 Li1 N2 139.70(10) . . . 3 ?
P1 N2 Li1 N2 6.25(7) . . . 3 ?
Li1 N2 Li1 N2 -77.99(12) 2 . . 3 ?
Li1 N2 Li1 N2 -126.68(8) 12 . . 3 ?
C1 N2 Li1 N2 -117.45(12) . . . 11 ?
P1 N2 Li1 N2 109.10(9) . . . 11 ?
Li1 N2 Li1 N2 24.86(15) 2 . . 11 ?
Li1 N2 Li1 N2 -23.83(11) 12 . . 11 ?
C1 N2 Li1 Li1 -173.28(12) . . . 11 ?
P1 N2 Li1 Li1 53.27(14) . . . 11 ?
Li1 N2 Li1 Li1 -31.0(2) 2 . . 11 ?
Li1 N2 Li1 Li1 -79.66(16) 12 . . 11 ?
C1 N2 Li1 Li1 -93.62(12) . . . 12 ?
P1 N2 Li1 Li1 132.93(8) . . . 12 ?
Li1 N2 Li1 Li1 48.69(6) 2 . . 12 ?
C1 N2 Li1 P1 133.45(13) . . . . ?
Li1 N2 Li1 P1 -84.24(10) 2 . . . ?
Li1 N2 Li1 P1 -132.93(8) 12 . . . ?
C1 N2 Li1 C4 -50.3(2) . . . 11 ?
P1 N2 Li1 C4 176.26(13) . . . 11 ?
Li1 N2 Li1 C4 92.02(15) 2 . . 11 ?
Li1 N2 Li1 C4 43.33(15) 12 . . 11 ?
C1 N2 Li1 C3 80.89(13) . . . 3 ?
P1 N2 Li1 C3 -52.57(8) . . . 3 ?
Li1 N2 Li1 C3 -136.80(10) 2 . . 3 ?
Li1 N2 Li1 C3 174.51(9) 12 . . 3 ?
C1 N2 Li1 C1 114.36(12) . . . 3 ?
P1 N2 Li1 C1 -19.09(8) . . . 3 ?
Li1 N2 Li1 C1 -103.33(11) 2 . . 3 ?
Li1 N2 Li1 C1 -152.02(8) 12 . . 3 ?
C1 N2 Li1 Li1 169.06(12) . . . 3 ?
P1 N2 Li1 Li1 35.60(4) . . . 3 ?
Li1 N2 Li1 Li1 -48.63(8) 2 . . 3 ?
Li1 N2 Li1 Li1 -97.32(5) 12 . . 3 ?
C1 N2 Li1 Li1 -142.31(17) . . . 2 ?
P1 N2 Li1 Li1 84.24(10) . . . 2 ?
Li1 N2 Li1 Li1 -48.69(6) 12 . . 2 ?
N1 P1 Li1 N2 -93.69(7) . . . . ?
N2 P1 Li1 N2 170.63(11) 3 . . . ?
N2 P1 Li1 N2 84.58(6) 2 . . . ?
Li1 P1 Li1 N2 129.13(6) 3 . . . ?
Li1 P1 Li1 N2 43.49(9) 2 . . . ?
N1 P1 Li1 N2 95.68(6) . . . 3 ?
N2 P1 Li1 N2 -86.05(6) 2 . . 3 ?
N2 P1 Li1 N2 -170.63(11) . . . 3 ?
Li1 P1 Li1 N2 -41.50(8) 3 . . 3 ?
Li1 P1 Li1 N2 -127.14(6) 2 . . 3 ?
N1 P1 Li1 N2 178.59(6) . . . 11 ?
N2 P1 Li1 N2 82.91(11) 3 . . 11 ?
N2 P1 Li1 N2 -3.14(13) 2 . . 11 ?
N2 P1 Li1 N2 -87.72(12) . . . 11 ?
Li1 P1 Li1 N2 41.41(7) 3 . . 11 ?
Li1 P1 Li1 N2 -44.22(6) 2 . . 11 ?
N1 P1 Li1 Li1 131.95(6) . . . 11 ?
N2 P1 Li1 Li1 36.27(8) 3 . . 11 ?
N2 P1 Li1 Li1 -49.78(9) 2 . . 11 ?
N2 P1 Li1 Li1 -134.36(11) . . . 11 ?
Li1 P1 Li1 Li1 -5.23(8) 3 . . 11 ?
Li1 P1 Li1 Li1 -90.87(5) 2 . . 11 ?
N1 P1 Li1 Li1 -131.95(6) . . . 12 ?
N2 P1 Li1 Li1 132.37(10) 3 . . 12 ?
N2 P1 Li1 Li1 46.32(10) 2 . . 12 ?
N2 P1 Li1 Li1 -38.26(8) . . . 12 ?
Li1 P1 Li1 Li1 90.87(5) 3 . . 12 ?
Li1 P1 Li1 Li1 5.23(8) 2 . . 12 ?
N1 P1 Li1 C4 -116.1(8) . . . 11 ?
N2 P1 Li1 C4 148.3(8) 3 . . 11 ?
N2 P1 Li1 C4 62.2(8) 2 . . 11 ?
N2 P1 Li1 C4 -22.4(8) . . . 11 ?
Li1 P1 Li1 C4 106.8(7) 3 . . 11 ?
Li1 P1 Li1 C4 21.1(8) 2 . . 11 ?
N1 P1 Li1 C3 33.61(8) . . . 3 ?
N2 P1 Li1 C3 -62.08(7) 3 . . 3 ?
N2 P1 Li1 C3 -148.13(5) 2 . . 3 ?
N2 P1 Li1 C3 127.30(9) . . . 3 ?
Li1 P1 Li1 C3 -103.57(9) 3 . . 3 ?
Li1 P1 Li1 C3 170.79(8) 2 . . 3 ?
N1 P1 Li1 C1 65.48(6) . . . 3 ?
N2 P1 Li1 C1 -30.21(5) 3 . . 3 ?
N2 P1 Li1 C1 -116.26(5) 2 . . 3 ?
N2 P1 Li1 C1 159.17(8) . . . 3 ?
Li1 P1 Li1 C1 -71.71(8) 3 . . 3 ?
Li1 P1 Li1 C1 -157.34(6) 2 . . 3 ?
N1 P1 Li1 Li1 137.18(3) . . . 3 ?
N2 P1 Li1 Li1 41.50(8) 3 . . 3 ?
N2 P1 Li1 Li1 -44.55(8) 2 . . 3 ?
N2 P1 Li1 Li1 -129.13(6) . . . 3 ?
Li1 P1 Li1 Li1 -85.64(6) 2 . . 3 ?
N1 P1 Li1 Li1 -137.18(3) . . . 2 ?
N2 P1 Li1 Li1 127.14(6) 3 . . 2 ?
N2 P1 Li1 Li1 41.09(8) 2 . . 2 ?
N2 P1 Li1 Li1 -43.49(9) . . . 2 ?
Li1 P1 Li1 Li1 85.64(6) 3 . . 2 ?

#-----------------------------------------------------------------------------
data_Compound_1a 

_database_code_CSD	190650

#-----------------------------------------------------------------------------
_computing_data_collection                           'COLLECT (Hooft, 1998)'
_computing_cell_refinement            'HKL DENZO (Otwinowski & Minor, 1997)'
_computing_data_reduction             'SCALEPACK (Otwinowski & Minor, 1997)'
_computing_structure_solution                           'SAPI91 (Fan, 1991)'
_computing_structure_refinement                'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material                'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics   	           'TEXSAN (M. S. C., 1994)'
#-----------------------------------------------------------------------------
_chemical_name_systematic      ' ? ' 
_chemical_name_common          ' ? ' 
_chemical_melting_point        ' ? ' 
_chemical_formula_sum          'C15 H39 N4 P Si'
_chemical_formula_weight          334.56
_chemical_compound_source      'synthesized by authors '

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
'C'  'C'   0.0033   0.0016
'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'
'N'  'N'   0.0061   0.0033
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'P'  'P'   0.1023   0.0942
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'Si'  'Si'   0.0817   0.0704
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting            trigonal 
_symmetry_space_group_name_H-M    ' R -3 ' 

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                    14.7950(4)
_cell_length_b                    14.7950(4)
_cell_length_c                    16.3978(4)
_cell_angle_alpha                 90.00
_cell_angle_beta                  90.00
_cell_angle_gamma                 120.00
_cell_volume                      3108.46(14)
_cell_formula_units_Z             6
_cell_measurement_temperature     173(2)
_cell_measurement_reflns_used     6136
_cell_measurement_theta_min       1.0
_cell_measurement_theta_max       27.5

_exptl_crystal_description        'block'
_exptl_crystal_colour             'colourless'
_exptl_crystal_size_max           0.25
_exptl_crystal_size_mid           0.25
_exptl_crystal_size_min           0.20
_exptl_crystal_density_meas       'not measured'
_exptl_crystal_density_diffrn     1.072
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              1116
_exptl_absorpt_coefficient_mu     0.192
_exptl_absorpt_correction_type    'multi-scan'
_exptl_absorpt_correction_T_min   0.9535
_exptl_absorpt_correction_T_max   0.9626
_exptl_absorpt_process_details    '(SORTAV: Blessing, 1997)'

_diffrn_ambient_temperature       173(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source          'fine-focus sealed tube'
_diffrn_radiation_monochromator   graphite
_diffrn_measurement_device_type   'Nonius KappaCCD Diffractometer'
_diffrn_measurement_method        ' \w & \f '
_diffrn_standards_decay_%         '< 0.01'
_diffrn_reflns_number             6136
_diffrn_reflns_av_R_equivalents   0.0318
_diffrn_reflns_av_sigmaI/netI     0.0323
_diffrn_reflns_limit_h_min        -19
_diffrn_reflns_limit_h_max        18
_diffrn_reflns_limit_k_min        -18
_diffrn_reflns_limit_k_max        17
_diffrn_reflns_limit_l_min        -20
_diffrn_reflns_limit_l_max        21
_diffrn_reflns_theta_min          3.41
_diffrn_reflns_theta_max          27.52
_reflns_number_total              1565
_reflns_number_gt                 1312
_reflns_threshold_expression      >2sigma(I)

_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.054P)^2^+2.188P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     'constr'
_refine_ls_extinction_method      none
_refine_ls_number_reflns          1565
_refine_ls_number_parameters      64
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0450
_refine_ls_R_factor_gt            0.0361
_refine_ls_wR_factor_ref          0.1075
_refine_ls_wR_factor_gt           0.1025
_refine_ls_goodness_of_fit_ref    1.098
_refine_ls_restrained_S_all       1.098
_refine_ls_shift/su_max           0.000
_refine_ls_shift/su_mean          0.000
_refine_diff_density_max          0.295
_refine_diff_density_min         -0.316
_refine_diff_density_rms          0.044
_diffrn_measured_fraction_theta_max    0.984
_diffrn_reflns_theta_full              27.52
_diffrn_measured_fraction_theta_full   0.984

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.0000 0.0000 0.35095(3) 0.02012(19) Uani 1 3 d S . .
Si1 Si 0.0000 0.0000 0.15657(4) 0.0267(2) Uani 1 3 d S . .
N1 N 0.10163(9) 0.00018(9) 0.39501(6) 0.0250(3) Uani 1 1 d . . .
H1 H 0.0896 -0.0325 0.4420 0.030 Uiso 1 1 calc R . .
N2 N 0.0000 0.0000 0.25826(11) 0.0254(4) Uani 1 3 d S . .
C1 C 0.21023(10) 0.04945(10) 0.36368(8) 0.0240(3) Uani 1 1 d . . .
C2 C 0.21758(12) -0.01038(12) 0.29001(8) 0.0322(3) Uani 1 1 d . . .
H2A H 0.2900 0.0233 0.2709 0.039 Uiso 1 1 calc R . .
H2B H 0.1727 -0.0102 0.2461 0.039 Uiso 1 1 calc R . .
H2C H 0.1947 -0.0825 0.3059 0.039 Uiso 1 1 calc R . .
C3 C 0.24842(11) 0.16265(11) 0.33969(9) 0.0336(4) Uani 1 1 d . . .
H3A H 0.3202 0.1945 0.3193 0.040 Uiso 1 1 calc R . .
H3B H 0.2464 0.2014 0.3874 0.040 Uiso 1 1 calc R . .
H3C H 0.2032 0.1646 0.2969 0.040 Uiso 1 1 calc R . .
C4 C 0.27804(12) 0.04659(13) 0.43265(9) 0.0362(4) Uani 1 1 d . . .
H4A H 0.3505 0.0783 0.4140 0.043 Uiso 1 1 calc R . .
H4B H 0.2528 -0.0260 0.4486 0.043 Uiso 1 1 calc R . .
H4C H 0.2743 0.0856 0.4796 0.043 Uiso 1 1 calc R . .
C5 C 0.12399(13) 0.11143(14) 0.11504(9) 0.0407(4) Uani 1 1 d . . .
H5A H 0.1218 0.1095 0.0553 0.049 Uiso 1 1 calc R . .
H5B H 0.1836 0.1054 0.1341 0.049 Uiso 1 1 calc R . .
H5C H 0.1313 0.1776 0.1341 0.049 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
P1 0.0214(3) 0.017 0.0202(3) 0.000 0.000 0.009
Si1 0.0317(4) 0.027 0.0198(3) 0.000 0.000 0.014
N1 0.0232(6) 0.0296(6) 0.0233(5) 0.0061(4) 0.0013(4) 0.0139(5)
N2 0.0275(10) 0.026 0.0221(10) 0.000 0.000 0.013
C1 0.0198(6) 0.0243(7) 0.0279(7) 0.0006(5) 0.0006(5) 0.0110(5)
C2 0.0317(8) 0.0349(8) 0.0359(8) -0.0025(6) 0.0022(6) 0.0210(7)
C3 0.0271(7) 0.0243(7) 0.0457(9) 0.0023(6) 0.0043(6) 0.0101(6)
C4 0.0283(8) 0.0460(9) 0.0372(8) -0.0005(7) -0.0047(6) 0.0208(7)
C5 0.0424(9) 0.0445(9) 0.0303(8) 0.0077(6) 0.0075(6) 0.0180(8)

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P1 N2 1.5200(18) . ?
P1 N1 1.6670(11) 2 ?
P1 N1 1.6670(11) . ?
P1 N1 1.6670(11) 3 ?
Si1 N2 1.6674(18) . ?
Si1 C5 1.8769(16) . ?
Si1 C5 1.8769(16) 3 ?
Si1 C5 1.8769(16) 2 ?
N1 C1 1.4851(16) . ?
C1 C4 1.5263(18) . ?
C1 C3 1.5273(19) . ?
C1 C2 1.5334(18) . ?

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
_geom_angle_publ_flag
N2 P1 N1 115.68(4) . 2 ?
N2 P1 N1 115.68(4) . . ?
N1 P1 N1 102.61(5) 2 . ?
N2 P1 N1 115.68(4) . 3 ?
N1 P1 N1 102.61(5) 2 3 ?
N1 P1 N1 102.61(5) . 3 ?
N2 Si1 C5 111.28(5) . . ?
N2 Si1 C5 111.28(5) . 3 ?
C5 Si1 C5 107.61(5) . 3 ?
N2 Si1 C5 111.28(5) . 2 ?
C5 Si1 C5 107.61(5) . 2 ?
C5 Si1 C5 107.61(5) 3 2 ?
C1 N1 P1 127.19(9) . . ?
P1 N2 Si1 180.0 . . ?
N1 C1 C4 107.15(11) . . ?
N1 C1 C3 110.10(11) . . ?
C4 C1 C3 109.47(12) . . ?
N1 C1 C2 111.15(11) . . ?
C4 C1 C2 109.30(11) . . ?
C3 C1 C2 109.63(11) . . ?

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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2 P1 N1 C1 32.15(12) . . . . ?
N1 P1 N1 C1 -94.75(14) 2 . . . ?
N1 P1 N1 C1 159.04(11) 3 . . . ?
N1 P1 N2 Si1 0(52) 2 . . . ?
N1 P1 N2 Si1 0(52) . . . . ?
N1 P1 N2 Si1 0(27) 3 . . . ?
C5 Si1 N2 P1 0(76) . . . . ?
C5 Si1 N2 P1 0(28) 3 . . . ?
C5 Si1 N2 P1 0(31) 2 . . . ?
P1 N1 C1 C4 169.18(10) . . . . ?
P1 N1 C1 C3 50.21(15) . . . . ?
P1 N1 C1 C2 -71.47(14) . . . . ?