Supplementary Material (ESI) for Chemical Communications
This journal is © The Royal Society of Chemistry 2001
data_global
_journal_coden_Cambridge 182
loop_
_publ_author_name
_publ_author_address
'Scherer, W.'
;
Anorganisch-chemisches Institut
Technische Universitat Munchen
Lichtenbergstrasse 4
D-85747 Garching bei Munchen (Germany)
;
'Sirsch, P.'
;
Anorganisch-chemisches Institut
Technische Universitat Munchen
Lichtenbergstrasse 4
D-85747 Garching bei Munchen (Germany)
;
'Grosche, M.'
;
Anorganisch-chemisches Institut
Technische Universitat Munchen
Lichtenbergstrasse 4
D-85747 Garching bei Munchen (Germany)
;
'Spiegler, M.'
;
Anorganisch-chemisches Institut
Technische Universitat Munchen
Lichtenbergstrasse 4
D-85747 Garching bei Munchen (Germany)
;
'Mason, S. A.'
;
Institut Laue-Langevin
BP156
F-38042 Grenoble Cedex 9 (France)
;
'Gardiner, M.G.'
;
School of Chemistry
University of Sydney
Building F11
Sydney, 2006 (N. S. W. Australia)
;
# 0. AUDIT DETAILS
_audit_creation_date 'Apr 26 16:56:04 2001'
_audit_creation_method 'PLATON
option'
_audit_update_record
;
27.04.01 updated by author P. Sirsch
30.04.01 updated by author P. Sirsch
;
#===============================================================================
# 1. SUBMISSION DETAILS
_publ_contact_author_name # Name of author for correspondence
;
Dr. Wolfgang Scherer
;
_publ_contact_author_address # address of author for correspondence
;
Anorganisch-chemisches Institut
der Technischen Universitat Munchen
Lichtenbergstrasse 4
D-85747 Garching
GERMANY
;
_publ_contact_author_email wolfgang.scherer@ch.tum.de
_publ_contact_author_fax '49(89)28913473'
_publ_contact_author_phone '49(89)28913096'
_publ_requested_journal 'Chem. Commun.'
# Publication choise FI FM FO CI CM CO
_publ_requested_category ?
_publ_requested_coeditor_name ?
_publ_contact_letter # Include date of submission
;
Date of submission ?
Please consider this CIF submission for publication as a
Regular Structural Paper.
;
#===============================================================================
# 3. TITLE AND AUTHOR LIST
_publ_section_title
;
Agostic Deformations based on Electron Delocalization
in the Alkyllithium-complex [{2-(Me3Si)2CLiC5H4N}2]
;
_publ_section_title_footnote
;
?
;
# The loop structure below should contain the names and adresses of all
# authors, in the required order of publication. Repeat as necessary.
#===============================================================================
# 4. TEXT
_publ_section_synopsis
;
?
;
_publ_section_abstract
;
?
;
# Insert blank lines between paragraphs
_publ_section_comment
;
?
;
_publ_section_exptl_prep
;
?
;
_publ_section_exptl_refinement
;
?
;
# Insert blank lines between references
_publ_section_references
;
Blessing, R.H. (1995), Acta Cryst. A51, 33-37.
COLLECT. Data Collection Software. Nonius BV, 1998.
Koritsanszky, T., Howard, S.T., Richter, T., Mallinson, P.R., Su, Z.,
and Hansen, N.K. (1995). XD - a computer program package for multipole
refinement and analysis of charge densities from diffraction data.
Otwinowski, Z., Minor, W., Processing of X-ray Diffraction Data Collected
in Oscillation Mode, Methods in Enzymology, Volume 276: Macromolecular
Crystallography, part A, p. 307-326, 1997, Carter, C.W., Jr.,
Sweet, R.M., Eds., Academic Press.
Sheldrick, G.M. SHELXL97. Program for crystal structure
refinement. University of Gottingen, Germany, 1997.
Spek, A.L. (1990). Acta Cryst. A46, C-34.
Wilson, A.J.C. (1992) Ed. International Tables for Crystallography,
Volume C, Kluwer Academic Publishers, Dordrecht, The Netherlands.
;
_publ_section_acknowledgements
; ?
;
_publ_section_figure_captions
; View of the title compound with the atom numbering scheme.
Displacement ellipsoids for non-H atoms are drawn at the 50% probability level.
;
#===============================================================================
data_li_xd_115 # compound 1
_database_code_CSD 169890
#===============================================================================
# 5. CHEMICAL DATA
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety
'C24 H44 Li2 N2 Si4'
_chemical_formula_structural ?
# Ex: 'C12 H16 N2 O6, H2 O' and '(Cd 2+)3, (C6 N6 Cr 3-)2, 2(H2 O)'
_chemical_formula_sum
'C24 H44 Li2 N2 Si4'
_chemical_formula_weight 486.85
_chemical_compound_source 'see text'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Si Si 0.0817 0.0704
'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'
Li Li -0.0003 0.0001
'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'
C C 0.0033 0.0016
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
#===============================================================================
# 6. CRYSTAL DATA
_symmetry_cell_setting Monoclinic
_symmetry_space_group_name_Hall '-P 2yn'
_symmetry_space_group_name_H-M 'P 21/n'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
1/2-x,1/2+y,1/2-z
-x,-y,-z
1/2+x,1/2-y,1/2+z
_cell_length_a 11.7233(2)
_cell_length_b 9.8814(2)
_cell_length_c 12.7702(2)
_cell_angle_alpha 90
_cell_angle_beta 93.4810(11)
_cell_angle_gamma 90
_cell_volume 1476.60(5)
_cell_formula_units_Z 2
_cell_measurement_temperature 115
_cell_measurement_reflns_used 28093
_cell_measurement_theta_min ?
_cell_measurement_theta_max ?
_cell_special_details
; ?
;
_exptl_crystal_description 'prism'
_exptl_crystal_colour 'yellow'
_exptl_crystal_size_max 1.12
_exptl_crystal_size_mid 0.41
_exptl_crystal_size_min 0.28
_exptl_crystal_size_rad ?
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.095
_exptl_crystal_density_method 'Not Measured'
_exptl_crystal_F_000 528
_exptl_absorpt_coefficient_mu 0.215
_exptl_crystal_density_meas_temp ?
_exptl_absorpt_correction_type empirical
_exptl_absorpt_process_details 'SORTAV (R.H. Blessing, 1995)'
_exptl_absorpt_correction_T_min 0.795
_exptl_absorpt_correction_T_max 0.942
#===============================================================================
# 7. EXPERIMENTAL DATA
_exptl_special_details
; ?
;
_diffrn_ambient_temperature 115
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_source 'NONIUS FR 591 rotating anode'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'KappaCCD (Nonius)'
_diffrn_measurement_method 'rotation'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number none
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
? ? ?
# number of measured reflections (redundant set)
_diffrn_reflns_number 80348
_diffrn_reflns_av_R_equivalents 0.0344
_diffrn_reflns_av_sigmaI/netI 0.0510
_diffrn_reflns_limit_h_min -25
_diffrn_reflns_limit_h_max 23
_diffrn_reflns_limit_k_min -21
_diffrn_reflns_limit_k_max 19
_diffrn_reflns_limit_l_min -27
_diffrn_reflns_limit_l_max 22
_diffrn_reflns_theta_min 2.70
_diffrn_reflns_theta_max 50.61
_diffrn_reflns_theta_full 50.61
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measured_fraction_theta_full 0.975
_diffrn_reflns_reduction_process
;
?
;
# number of unique reflections
_reflns_number_total 15534
# number of observed reflections (> n sig(I))
_reflns_number_gt 8905
_reflns_threshold_expression 'F>3\s(F)'
_computing_data_collection 'COLLECT (Nonius, 1998)'
_computing_cell_refinement 'DENZO (Z. Otwinowski and W. Minor, 1997)'
_computing_data_reduction 'DENZO (Z. Otwinowski and W. Minor, 1997)'
_computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement 'XD (Koritsanszky et al, 1995)'
_computing_molecular_graphics 'PLATON (Spek, 1990)'
_computing_publication_material 'PLATON (Spek, 1990)'
#===============================================================================
# 8. REFINEMENT DATA
_refine_special_details
;
The lithium and hydrogen atom positions and their anisotropic thermal
parameters were fixed at the values obtained by neutron diffraction (100 K)
while the thermal parameters of the neutron study were scaled by the
average ratio (U(xray)/U(neutron)) = 1.30 for the heavy atoms to
account for the temperature difference.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'w=1/[\s^2^(Fo)]'
_refine_ls_hydrogen_treatment noref
_refine_ls_extinction_method none
_refine_ls_number_reflns 8905
_refine_ls_number_parameters 301
_refine_ls_number_restraints 0
_refine_ls_number_constraints 0
_refine_ls_R_factor_all 0.0817
_refine_ls_R_factor_gt 0.0250
_refine_ls_wR_factor_gt 0.0314
_refine_ls_R_Fsqd_factor 0.0265
_refine_ls_goodness_of_fit_ref 1.062
_refine_ls_restrained_S_all 1.062
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_diff_density_max 0.21
_refine_diff_density_min -0.20
#===============================================================================
# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_thermal_displace_type
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_U_iso_or_equiv
Si1 Si Uani 0.36009(1) 0.36447(1) 0.14265(1) 1.000 0.0184(1)
Si2 Si Uani 0.30228(1) 0.26310(1) -0.08625(1) 1.000 0.0194(1)
N N Uani 0.32170(4) 0.65175(5) 0.01422(4) 1.000 0.0173(1)
C1 C Uani 0.34445(3) 0.40747(4) 0.00109(3) 1.000 0.0154(1)
C2 C Uani 0.21836(5) 0.35769(7) 0.20396(4) 1.000 0.0363(2)
C3 C Uani 0.44800(8) 0.49177(8) 0.22359(5) 1.000 0.0328(2)
C4 C Uani 0.43410(5) 0.19839(7) 0.16947(5) 1.000 0.0349(2)
C5 C Uani 0.25199(5) 0.31911(7) -0.22208(4) 1.000 0.0343(1)
C6 C Uani 0.18768(5) 0.14550(5) -0.04195(5) 1.000 0.0312(1)
C7 C Uani 0.43079(6) 0.15207(8) -0.10675(7) 1.000 0.0326(2)
C11 C Uani 0.27294(3) 0.53035(4) -0.01261(3) 1.000 0.0150(1)
C12 C Uani 0.15600(4) 0.52954(5) -0.04788(4) 1.000 0.0225(1)
C13 C Uani 0.09272(4) 0.64778(5) -0.05310(4) 1.000 0.0265(1)
C14 C Uani 0.14460(4) 0.77001(5) -0.02328(4) 1.000 0.0240(1)
C15 C Uani 0.25923(4) 0.76603(5) 0.00900(3) 1.000 0.0210(1)
Li Li Uani 0.51919 0.39297 -0.05280 1.000 0.0284
H2A H Uani 0.22900 0.33521 0.28731 1.000 0.0886
H2B H Uani 0.16371 0.27859 0.16845 1.000 0.0689
H2C H Uani 0.17169 0.45205 0.19426 1.000 0.0742
H3A H Uani 0.45026 0.46178 0.30606 1.000 0.0701
H3B H Uani 0.41136 0.59432 0.22082 1.000 0.0653
H3C H Uani 0.53683 0.49804 0.20281 1.000 0.0657
H4A H Uani 0.44233 0.18219 0.25495 1.000 0.0736
H4B H Uani 0.52035 0.19701 0.14191 1.000 0.0685
H4C H Uani 0.38823 0.11186 0.13530 1.000 0.0686
H5A H Uani 0.23974 0.23074 -0.27289 1.000 0.0829
H5B H Uani 0.31118 0.38333 -0.25812 1.000 0.1003
H5C H Uani 0.17037 0.37072 -0.22631 1.000 0.0962
H6A H Uani 0.17366 0.06305 -0.09905 1.000 0.0671
H6B H Uani 0.10642 0.19677 -0.03671 1.000 0.0693
H6C H Uani 0.21003 0.09903 0.03440 1.000 0.0678
H7A H Uani 0.40248 0.06223 -0.15068 1.000 0.0783
H7B H Uani 0.47515 0.11794 -0.03447 1.000 0.0727
H7C H Uani 0.49471 0.19902 -0.15460 1.000 0.0667
H12 H Uani 0.11450 0.43384 -0.06803 1.000 0.0516
H13 H Uani 0.00191 0.64463 -0.08010 1.000 0.0564
H14 H Uani 0.09735 0.86567 -0.02670 1.000 0.0499
H15 H Uani 0.30452 0.85932 0.03114 1.000 0.0470
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
Si1 0.0171(1) 0.0209(1) 0.0171(1) 0.0037(1) -0.0005(1) 0.0004(1)
Si2 0.0152(1) 0.0196(1) 0.0232(1) -0.0053(1) 0.0000(1) -0.0006(1)
N 0.0158(1) 0.0158(2) 0.0203(2) -0.0018(1) -0.0002(1) 0.0005(1)
C1 0.0139(1) 0.0161(1) 0.0161(1) -0.0001(1) 0.0000(1) 0.0013(1)
C2 0.0262(2) 0.0590(4) 0.0244(2) 0.0090(2) 0.0080(2) 0.0003(2)
C3 0.0428(3) 0.0346(3) 0.0200(2) -0.0005(2) -0.0073(2) -0.0082(3)
C4 0.0370(3) 0.0277(2) 0.0389(3) 0.0106(2) -0.0079(2) 0.0071(2)
C5 0.0315(2) 0.0485(3) 0.0220(2) -0.0059(2) -0.0056(2) -0.0046(2)
C6 0.0262(2) 0.0222(2) 0.0453(3) -0.0046(2) 0.0033(2) -0.0072(2)
C7 0.0243(2) 0.0278(3) 0.0458(3) -0.0152(3) 0.0023(2) 0.0046(2)
C11 0.0123(1) 0.0162(1) 0.0166(1) 0.0012(1) 0.0008(1) 0.0004(1)
C12 0.0126(1) 0.0197(2) 0.0349(2) 0.0022(1) -0.0021(1) 0.0001(1)
C13 0.0145(1) 0.0239(2) 0.0407(2) 0.0050(2) -0.0015(1) 0.0035(1)
C14 0.0199(2) 0.0199(2) 0.0325(2) 0.0035(1) 0.0030(1) 0.0055(1)
C15 0.0210(2) 0.0168(2) 0.0252(2) -0.0010(1) 0.0015(1) 0.0022(1)
Li 0.0153 0.0408 0.0290 -0.0020 0.0010 0.0020
H2A 0.0671 0.1648 0.0348 0.0213 0.0097 -0.0034
H2B 0.0470 0.0813 0.0792 0.0035 0.0104 -0.0164
H2C 0.0557 0.0811 0.0879 -0.0007 0.0220 0.0216
H3A 0.0950 0.0813 0.0315 0.0079 -0.0155 -0.0168
H3B 0.0962 0.0444 0.0547 -0.0112 -0.0012 -0.0003
H3C 0.0445 0.0863 0.0652 0.0013 -0.0050 -0.0206
H4A 0.0991 0.0695 0.0501 0.0234 -0.0138 0.0130
H4B 0.0458 0.0704 0.0888 0.0085 0.0004 0.0204
H4C 0.0822 0.0351 0.0858 0.0011 -0.0168 0.0006
H5A 0.1170 0.0799 0.0504 -0.0276 -0.0074 -0.0074
H5B 0.1060 0.1347 0.0573 0.0358 -0.0198 -0.0664
H5C 0.0836 0.1469 0.0555 -0.0006 -0.0175 0.0551
H6A 0.0737 0.0506 0.0773 -0.0261 0.0062 -0.0229
H6B 0.0367 0.0547 0.1184 0.0028 0.0193 0.0010
H6C 0.0741 0.0627 0.0662 0.0164 0.0000 -0.0176
H7A 0.0579 0.0547 0.1220 -0.0519 0.0030 -0.0007
H7B 0.0666 0.0796 0.0704 0.0019 -0.0071 0.0358
H7C 0.0505 0.0635 0.0890 -0.0110 0.0274 0.0030
H12 0.0312 0.0320 0.0900 -0.0050 -0.0107 -0.0055
H13 0.0245 0.0514 0.0915 0.0040 -0.0116 0.0046
H14 0.0425 0.0331 0.0740 0.0039 0.0031 0.0154
H15 0.0411 0.0290 0.0697 -0.0085 -0.0064 -0.0034
#===============================================================================
# 10. MOLECULAR GEOMETRY
_geom_special_details
;
Bond distances, angles etc. have been calculated using the
rounded fractional coordinates. All esds are estimated
from the variances of the (full) variance-covariance matrix.
The cell esds are taken into account in the estimation of
distances, angles and torsion angles
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Si1 C1 1.8552(4) . . yes
Si1 C2 1.8804(6) . . yes
Si1 C3 1.8930(8) . . yes
Si1 C4 1.8781(7) . . yes
Si2 C1 1.8592(4) . . yes
Si2 C5 1.8811(5) . . yes
Si2 C6 1.8888(6) . . yes
Si2 C7 1.8947(7) . . yes
Si2 Li 2.8572 . . yes
N C11 1.3636(6) . . yes
N C15 1.3454(7) . . yes
N Li 1.9508 . 3_665 yes
C1 C11 1.4798(5) . . no
C1 Li 2.2049 . . yes
C11 C12 1.4168(6) . . no
C12 C13 1.3834(7) . . no
C13 C14 1.3948(7) . . no
C14 C15 1.3821(7) . . no
C2 H2A 1.0871 . . no
C2 H2B 1.0917 . . no
C2 H2C 1.0844 . . no
C3 H3A 1.0928 . . no
C3 H3B 1.1003 . . no
C3 H3C 1.0919 . . no
C4 H4A 1.1017 . . no
C4 H4B 1.0907 . . no
C4 H4C 1.0873 . . no
C5 H5A 1.0922 . . no
C5 H5B 1.0653 . . no
C5 H5C 1.0827 . . no
C6 H6A 1.0991 . . no
C6 H6B 1.0846 . . no
C6 H6C 1.0950 . . no
C7 H7A 1.0910 . . no
C7 H7B 1.0853 . . no
C7 H7C 1.0981 . . no
C12 H12 1.0872 . . no
C13 H13 1.0994 . . no
C14 H14 1.0951 . . no
C15 H15 1.0924 . . no
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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Si1 C2 112.11(2) . . . yes
C1 Si1 C3 113.46(2) . . . yes
C1 Si1 C4 113.27(2) . . . yes
C2 Si1 C3 105.18(3) . . . yes
C2 Si1 C4 107.64(3) . . . yes
C3 Si1 C4 104.53(3) . . . yes
C1 Si2 C5 112.61(2) . . . yes
C1 Si2 C6 117.42(2) . . . yes
C1 Si2 C7 110.03(3) . . . yes
C1 Si2 Li 50.50 . . . yes
C5 Si2 C6 105.57(3) . . . yes
C5 Si2 C7 104.50(3) . . . yes
C5 Si2 Li 103.41 . . . yes
C6 Si2 C7 105.73(3) . . . yes
C6 Si2 Li 150.96 . . . yes
C7 Si2 Li 64.71 . . . yes
C11 N C15 120.49(4) . . . yes
C11 N Li 104.12 . . 3_665 yes
C15 N Li 135.39 . . 3_665 yes
Si1 C1 Si2 114.57(2) . . . yes
Si1 C1 C11 108.96(3) . . . yes
Si1 C1 Li 104.51 . . . yes
Si2 C1 C11 115.50(3) . . . yes
Si2 C1 Li 88.92 . . . yes
C11 C1 Li 123.15 . . . yes
N C11 C1 117.79(3) . . . yes
N C11 C12 117.88(4) . . . yes
C1 C11 C12 124.28(4) . . . no
C11 C12 C13 121.08(4) . . . no
C12 C13 C14 119.64(4) . . . no
C13 C14 C15 117.18(4) . . . no
N C15 C14 123.72(5) . . . yes
H2A C2 H2C 108.34 . . . no
H2B C2 H2C 106.79 . . . no
Si1 C2 H2C 111.98 . . . no
Si1 C2 H2A 111.30 . . . no
Si1 C2 H2B 111.32 . . . no
H2A C2 H2B 106.86 . . . no
Si1 C3 H3A 109.06 . . . no
H3B C3 H3C 108.43 . . . no
Si1 C3 H3C 113.62 . . . no
H3A C3 H3B 105.50 . . . no
Si1 C3 H3B 113.32 . . . no
H3A C3 H3C 106.37 . . . no
Si1 C4 H4B 112.28 . . . no
Si1 C4 H4C 113.72 . . . no
Si1 C4 H4A 108.62 . . . no
H4A C4 H4B 106.90 . . . no
H4A C4 H4C 107.15 . . . no
H4B C4 H4C 107.83 . . . no
Si2 C5 H5B 113.44 . . . no
Si2 C5 H5C 114.28 . . . no
H5A C5 H5B 106.57 . . . no
Si2 C5 H5A 109.58 . . . no
H5A C5 H5C 105.25 . . . no
H5B C5 H5C 107.14 . . . no
Si2 C6 H6A 109.74 . . . no
H6A C6 H6C 107.33 . . . no
H6B C6 H6C 107.73 . . . no
H6A C6 H6B 106.90 . . . no
Si2 C6 H6B 111.99 . . . no
Si2 C6 H6C 112.87 . . . no
Si2 C7 H7A 108.82 . . . no
H7B C7 H7C 107.25 . . . no
Si2 C7 H7C 114.05 . . . no
H7A C7 H7B 107.43 . . . no
Si2 C7 H7B 113.98 . . . no
H7A C7 H7C 104.73 . . . no
C11 C12 H12 119.38 . . . no
C13 C12 H12 119.49 . . . no
C12 C13 H13 119.83 . . . no
C14 C13 H13 120.53 . . . no
C13 C14 H14 121.70 . . . no
C15 C14 H14 121.12 . . . no
N C15 H15 116.16 . . . no
C14 C15 H15 120.11 . . . no
N Li C1 145.90 3_665 . . yes
Si2 Li N 139.88 . . 3_665 yes
Si2 Li C1 40.59 . . . yes
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
C2 Si1 C1 Si2 -80.20(3) . . . . no
C2 Si1 C1 C11 50.92(4) . . . . no
C2 Si1 C1 Li -175.75 . . . . no
C3 Si1 C1 Si2 160.83(3) . . . . no
C3 Si1 C1 C11 -68.05(4) . . . . no
C3 Si1 C1 Li 65.27 . . . . no
C4 Si1 C1 Si2 41.86(3) . . . . no
C4 Si1 C1 C11 172.98(3) . . . . no
C4 Si1 C1 Li -53.70 . . . . no
C5 Si2 C1 Si1 165.53(2) . . . . no
C5 Si2 C1 C11 37.66(4) . . . . no
C5 Si2 C1 Li -88.99 . . . . no
C6 Si2 C1 Si1 42.61(3) . . . . no
C6 Si2 C1 C11 -85.26(3) . . . . no
C6 Si2 C1 Li 148.09 . . . . no
C7 Si2 C1 Si1 -78.34(3) . . . . no
C7 Si2 C1 C11 153.79(4) . . . . no
C7 Si2 C1 Li 27.14 . . . . no
Li Si2 C1 Si1 -105.48 . . . . no
Li Si2 C1 C11 126.65 . . . . no
C1 Si2 Li N 126.16 . . . 3_665 no
C5 Si2 Li C1 108.40 . . . . no
C5 Si2 Li N -125.44 . . . 3_665 no
C6 Si2 Li C1 -75.19 . . . . no
C6 Si2 Li N 50.97 . . . 3_665 no
C7 Si2 Li C1 -151.70 . . . . no
C7 Si2 Li N -25.54 . . . 3_665 no
C15 N C11 C1 -176.30(4) . . . . no
C15 N C11 C12 1.29(7) . . . . no
Li N C11 C1 4.19 3_665 . . . no
Li N C11 C12 -178.21 3_665 . . . no
C11 N C15 C14 -0.29(7) . . . . no
Li N C15 C14 179.02 3_665 . . . no
C11 N Li Si2 164.36 . . 3_665 3_665 no
C11 N Li C1 94.81 . . 3_665 3_665 no
C15 N Li Si2 -15.03 . . 3_665 3_665 no
C15 N Li C1 -84.58 . . 3_665 3_665 no
C11 N C15 H15 -179.51 . . . . no
Li N C15 H15 -0.20 3_665 . . . no
Si1 C1 C11 N 75.47(4) . . . . no
Si2 C1 C11 C12 28.65(5) . . . . no
Li C1 C11 N -47.27 . . . . no
Li C1 C11 C12 135.31 . . . . no
Si1 C1 Li Si2 115.13 . . . . no
Si1 C1 Li N 3.27 . . . 3_665 no
Si2 C1 Li N -111.86 . . . 3_665 no
C11 C1 Li Si2 -120.13 . . . . no
C11 C1 Li N 128.01 . . . 3_665 no
Si2 C1 C11 N -153.92(3) . . . . no
Si1 C1 C11 C12 -101.96(4) . . . . no
C1 C11 C12 C13 176.25(4) . . . . no
N C11 C12 C13 -1.17(7) . . . . no
C11 C12 C13 C14 0.04(9) . . . . no
C12 C13 C14 C15 0.95(7) . . . . no
C13 C14 C15 N -0.86(7) . . . . no
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
Si1 Li 3.0433 . 3_665 no
Si2 Li 4.3165 . 3_665 no
Si1 H6C 3.4044 . . no
Si2 H4C 3.3026 . . no
Si2 H12 2.7945 . . no
Si2 H3C 3.4183 . 3_665 no
N C3 3.3704(9) . . no
N H3B 2.8374 . . no
C3 N 3.3704(9) . . no
C3 Li 2.5107 . 3_665 no
C4 C7 3.5548(11) . . no
C5 C12 3.2928(8) . . no
C5 C14 3.5718(7) . 2_544 no
C7 C4 3.5548(11) . . no
C12 C5 3.2928(8) . . no
C14 C5 3.5718(7) . 2_554 no
C2 H13 2.9453 . 3_565 no
C3 H5B 3.0882 . 3_665 no
C4 H5C 3.0761 . 4_555 no
C4 H7B 2.7926 . . no
C5 H12 2.8528 . . no
C5 H3C 3.0627 . 3_665 no
C6 H2B 3.0198 . . no
C6 H12 2.9883 . . no
C6 H14 2.9716 . 1_545 no
C11 H2C 3.0606 . . no
C12 H5C 2.7803 . . no
C12 H13 3.0704 . 3_565 no
C13 H12 3.0661 . 3_565 no
C13 H6B 3.0741 . 3_565 no
C14 H6A 3.0785 . 1_565 no
C14 H5A 3.0320 . 2_554 no
C14 H5B 3.0808 . 2_554 no
C15 H2A 2.6849 . 2_555 no
C15 H5A 3.0360 . 2_554 no
Li Si2 4.3165 . 3_665 no
Li C3 2.5107 . 3_665 no
Li Si1 3.0433 . 3_665 no
Li Li 2.5630 . 3_665 no
Li H3C 3.4196 . . no
Li H4B 3.1509 . . no
Li H3B 2.3441 . 3_665 no
Li H3C 2.2601 . 3_665 no
H2A C15 2.6849 . 2_545 no
H2A H15 2.3868 . 2_545 no
H2B C6 3.0198 . . no
H2B H6C 2.5468 . . no
H2B H3B 2.4981 . 2_545 no
H2B H13 2.3135 . 3_565 no
H2C C11 3.0606 . . no
H3B N 2.8374 . . no
H3B H2B 2.4981 . 2_555 no
H3B Li 2.3441 . 3_665 no
H3B H7C 2.4922 . 3_665 no
H3C Li 3.4196 . . no
H3C Si2 3.4183 . 3_665 no
H3C C5 3.0627 . 3_665 no
H3C Li 2.2601 . 3_665 no
H3C H5B 2.2125 . 3_665 no
H4B Li 3.1509 . . no
H4B H7B 2.4124 . . no
H4B H5C 2.4523 . 4_555 no
H4C Si2 3.3026 . . no
H4C H6C 2.3903 . . no
H4C H7B 2.4516 . . no
H5A C14 3.0320 . 2_544 no
H5A C15 3.0360 . 2_544 no
H5B C14 3.0808 . 2_544 no
H5B H6A 2.5596 . 2_554 no
H5B C3 3.0882 . 3_665 no
H5B H3C 2.2125 . 3_665 no
H5C C12 2.7803 . . no
H5C H12 2.2504 . . no
H5C H7A 2.5720 . 2_554 no
H5C C4 3.0761 . 4_454 no
H5C H4B 2.4523 . 4_454 no
H6A C14 3.0785 . 1_545 no
H6A H14 2.3576 . 1_545 no
H6A H5B 2.5596 . 2_544 no
H6B H12 2.3793 . . no
H6B C13 3.0741 . 3_565 no
H6B H13 2.5542 . 3_565 no
H6C Si1 3.4044 . . no
H6C H2B 2.5468 . . no
H6C H4C 2.3903 . . no
H7A H5C 2.5720 . 2_544 no
H7B C4 2.7926 . . no
H7B H4B 2.4124 . . no
H7B H4C 2.4516 . . no
H7B H7B 2.5466 . 3_655 no
H7B H15 2.5905 . 3_665 no
H7C H3B 2.4922 . 3_665 no
H12 Si2 2.7945 . . no
H12 C5 2.8528 . . no
H12 C6 2.9883 . . no
H12 H5C 2.2504 . . no
H12 H6B 2.3793 . . no
H12 C13 3.0661 . 3_565 no
H12 H13 2.5210 . 3_565 no
H13 C2 2.9453 . 3_565 no
H13 C12 3.0704 . 3_565 no
H13 H2B 2.3135 . 3_565 no
H13 H6B 2.5542 . 3_565 no
H13 H12 2.5210 . 3_565 no
H14 C6 2.9716 . 1_565 no
H14 H6A 2.3576 . 1_565 no
H15 H2A 2.3868 . 2_555 no
H15 H7B 2.5905 . 3_665 no
loop_
_atom_rho_multipole_label
_atom_rho_multipole_coeff_Pv
_atom_rho_multipole_coeff_P00
_atom_rho_multipole_coeff_P11
_atom_rho_multipole_coeff_P1-1
_atom_rho_multipole_coeff_P10
_atom_rho_multipole_coeff_P20
_atom_rho_multipole_coeff_P21
_atom_rho_multipole_coeff_P2-1
_atom_rho_multipole_coeff_P22
_atom_rho_multipole_coeff_P2-2
_atom_rho_multipole_coeff_P30
_atom_rho_multipole_coeff_P31
_atom_rho_multipole_coeff_P3-1
_atom_rho_multipole_coeff_P32
_atom_rho_multipole_coeff_P3-2
_atom_rho_multipole_coeff_P33
_atom_rho_multipole_coeff_P3-3
_atom_rho_multipole_coeff_P40
_atom_rho_multipole_coeff_P41
_atom_rho_multipole_coeff_P4-1
_atom_rho_multipole_coeff_P42
_atom_rho_multipole_coeff_P4-2
_atom_rho_multipole_coeff_P43
_atom_rho_multipole_coeff_P4-3
_atom_rho_multipole_coeff_P44
_atom_rho_multipole_coeff_P4-4
_atom_rho_multipole_kappa_prime
_atom_rho_multipole_kappa_dprime0
_atom_rho_multipole_kappa_dprime1
_atom_rho_multipole_kappa_dprime2
_atom_rho_multipole_kappa_dprime3
_atom_rho_multipole_kappa_dprime4
SI(2) 3.26(10) 0.00 -0.05(2) 0.13(2) 0.06(2)
-0.02(2) 0.00(2) -0.01(2) -0.03(2) -0.11(2)
-0.01(3) -0.22(3) -0.30(3) 0.06(3) 0.01(2) 0.36(3) -0.01(2)
0.00 0.00 0.00 0.00 0.00 0.00 0.00
0.00 0.00
1.051(7) 1.00 1.00 1.00 1.00 1.00
SI(1) 3.23(11) 0.00 0.07(2) -0.01(2) 0.02(2)
-0.07(2) 0.171(19) -0.03(2) -0.045(19) 0.02(2)
-0.09(3) -0.21(3) -0.43(3) 0.13(2) -0.09(3) 0.28(3) 0.04(3)
0.00 0.00 0.00 0.00 0.00 0.00 0.00
0.00 0.00
1.031(7) 1.00 1.00 1.00 1.00 1.00
N 5.33(5) 0.00 -0.009(13) -0.064(12) 0.004(11)
-0.119(13) 0.018(11) 0.006(11) 0.022(12) 0.019(12)
0.002(11) -0.013(11) -0.018(11) -0.004(10) 0.015(10) 0.137(11) 0.014(11)
0.00 0.00 0.00 0.00 0.00 0.00 0.00
0.00 0.00
0.983(2) 1.00 1.00 1.00 1.00 1.00
C(1) 4.52(4) 0.00 0.024(13) -0.024(13) -0.019(13)
-0.029(13) -0.014(12) -0.021(12) -0.002(13) -0.045(12)
-0.035(14) -0.054(13) -0.097(13) -0.015(13) 0.091(13) 0.107(13) 0.000(13)
0.00 0.00 0.00 0.00 0.00 0.00 0.00
0.00 0.00
0.97 1.00 1.00 1.00 1.00 1.00
C(2) 4.44(6) 0.00 0.00 0.00 0.018(12)
0.043(12) 0.00 0.00 0.00 0.00
0.175(13) 0.00 0.00 0.00 0.00 0.004(11) 0.127(12)
0.00 0.00 0.00 0.00 0.00 0.00 0.00
0.00 0.00
0.986(3) 1.00 1.00 1.00 1.00 1.00
C(3) 4.46(4) 0.00 0.06(2) 0.025(16) 0.029(17)
0.052(16) -0.042(19) 0.005(14) 0.012(16) 0.077(19)
0.176(16) -0.039(17) 0.003(14) -0.007(15) 0.006(17) -0.017(16) 0.225(16)
0.00 0.00 0.00 0.00 0.00 0.00 0.00
0.00 0.00
0.98 1.00 1.00 1.00 1.00 1.00
C(4) 4.44 0.00 0.00 0.00 0.02
0.04 0.00 0.00 0.00 0.00
0.17 0.00 0.00 0.00 0.00 0.00 0.13
0.00 0.00 0.00 0.00 0.00 0.00 0.00
0.00 0.00
0.986(3) 1.00 1.00 1.00 1.00 1.00
C(5) 4.59(7) 0.00 0.00 0.00 0.014(12)
0.049(11) 0.00 0.00 0.00 0.00
0.236(12) 0.00 0.00 0.00 0.00 0.020(11) 0.144(11)
0.00 0.00 0.00 0.00 0.00 0.00 0.00
0.00 0.00
0.984(3) 1.00 1.00 1.00 1.00 1.00
C(6) 4.59 0.00 0.00 0.00 0.01
0.05 0.00 0.00 0.00 0.00
0.24 0.00 0.00 0.00 0.00 0.02 0.14
0.00 0.00 0.00 0.00 0.00 0.00 0.00
0.00 0.00
0.984(3) 1.00 1.00 1.00 1.00 1.00
C(7) 4.54(10) 0.00 0.10(2) 0.006(17) 0.024(17)
0.019(16) -0.007(19) 0.049(15) 0.014(18) 0.053(19)
0.179(19) -0.065(16) 0.007(15) 0.005(17) -0.033(17) -0.047(16) 0.163(17)
0.00 0.00 0.00 0.00 0.00 0.00 0.00
0.00 0.00
0.985(5) 1.00 1.00 1.00 1.00 1.00
C(11) 3.79(5) 0.00 0.000(11) 0.028(13) -0.040(14)
0.044(15) -0.006(12) 0.016(13) -0.143(12) 0.011(11)
0.184(16) 0.013(14) -0.004(15) 0.180(14) -0.022(13) 0.032(12) -0.013(12)
0.00 0.00 0.00 0.00 0.00 0.00 0.00
0.00 0.00
1.030(4) 1.00 1.00 1.00 1.00 1.00
C(12) 4.13(3) 0.00 0.005(11) -0.019(10) 0.00
-0.193(9) 0.00 0.00 0.007(10) 0.002(8)
0.00 0.032(10) 0.030(9) 0.00 0.00 0.249(8) -0.018(11)
0.00 0.00 0.00 0.00 0.00 0.00 0.00
0.00 0.00
1.009(2) 1.00 1.00 1.00 1.00 1.00
C(13) 4.13 0.00 0.01 -0.02 0.00
-0.19 0.00 0.00 0.01 0.00
0.00 0.03 0.03 0.00 0.00 0.25 -0.02
0.00 0.00 0.00 0.00 0.00 0.00 0.00
0.00 0.00
1.009(2) 1.00 1.00 1.00 1.00 1.00
C(14) 4.13 0.00 0.01 -0.02 0.00
-0.19 0.00 0.00 0.01 0.00
0.00 0.03 0.03 0.00 0.00 0.25 -0.02
0.00 0.00 0.00 0.00 0.00 0.00 0.00
0.00 0.00
1.009(2) 1.00 1.00 1.00 1.00 1.00
C(15) 4.02(4) 0.00 0.036(15) 0.040(15) 0.00
-0.182(15) 0.00 0.00 -0.021(14) 0.021(15)
0.00 0.009(14) 0.021(14) 0.00 0.00 0.300(15) -0.005(15)
0.00 0.00 0.00 0.00 0.00 0.00 0.00
0.00 0.00
1.009(2) 1.00 1.00 1.00 1.00 1.00
LI 0.90(11) 0.00 0.00 0.00 0.00
0.00 0.00 0.00 0.00 0.00
0.00 0.00 0.00 0.00 0.00 0.00 0.00
0.00 0.00 0.00 0.00 0.00 0.00 0.00
0.00 0.00
1.20 1.20 1.20 1.20 1.20 1.20
H(2A) 0.888(10) 0.00 0.00 0.00 0.099(6)
0.00 0.00 0.00 0.00 0.00
0.00 0.00 0.00 0.00 0.00 0.00 0.00
0.00 0.00 0.00 0.00 0.00 0.00 0.00
0.00 0.00
1.20 1.20 1.20 1.20 1.20 1.20
H(2B) 0.89 0.00 0.00 0.00 0.10
0.00 0.00 0.00 0.00 0.00
0.00 0.00 0.00 0.00 0.00 0.00 0.00
0.00 0.00 0.00 0.00 0.00 0.00 0.00
0.00 0.00
1.20 1.20 1.20 1.20 1.20 1.20
H(2C) 0.89 0.00 0.00 0.00 0.10
0.00 0.00 0.00 0.00 0.00
0.00 0.00 0.00 0.00 0.00 0.00 0.00
0.00 0.00 0.00 0.00 0.00 0.00 0.00
0.00 0.00
1.20 1.20 1.20 1.20 1.20 1.20
H(3A) 0.89 0.00 0.00 0.00 0.10
0.00 0.00 0.00 0.00 0.00
0.00 0.00 0.00 0.00 0.00 0.00 0.00
0.00 0.00 0.00 0.00 0.00 0.00 0.00
0.00 0.00
1.20 1.20 1.20 1.20 1.20 1.20
H(3B) 0.83(3) 0.00 0.00 0.00 0.06(2)
0.00 0.00 0.00 0.00 0.00
0.00 0.00 0.00 0.00 0.00 0.00 0.00
0.00 0.00 0.00 0.00 0.00 0.00 0.00
0.00 0.00
1.20 1.20 1.20 1.20 1.20 1.20
H(3C) 0.91(3) 0.00 0.00 0.00 0.10(2)
0.00 0.00 0.00 0.00 0.00
0.00 0.00 0.00 0.00 0.00 0.00 0.00
0.00 0.00 0.00 0.00 0.00 0.00 0.00
0.00 0.00
1.20 1.20 1.20 1.20 1.20 1.20
H(4A) 0.89 0.00 0.00 0.00 0.10
0.00 0.00 0.00 0.00 0.00
0.00 0.00 0.00 0.00 0.00 0.00 0.00
0.00 0.00 0.00 0.00 0.00 0.00 0.00
0.00 0.00
1.20 1.20 1.20 1.20 1.20 1.20
H(4B) 0.89 0.00 0.00 0.00 0.10
0.00 0.00 0.00 0.00 0.00
0.00 0.00 0.00 0.00 0.00 0.00 0.00
0.00 0.00 0.00 0.00 0.00 0.00 0.00
0.00 0.00
1.20 1.20 1.20 1.20 1.20 1.20
H(4C) 0.89 0.00 0.00 0.00 0.10
0.00 0.00 0.00 0.00 0.00
0.00 0.00 0.00 0.00 0.00 0.00 0.00
0.00 0.00 0.00 0.00 0.00 0.00 0.00
0.00 0.00
1.20 1.20 1.20 1.20 1.20 1.20
H(5A) 0.89 0.00 0.00 0.00 0.10
0.00 0.00 0.00 0.00 0.00
0.00 0.00 0.00 0.00 0.00 0.00 0.00
0.00 0.00 0.00 0.00 0.00 0.00 0.00
0.00 0.00
1.20 1.20 1.20 1.20 1.20 1.20
H(5B) 0.89 0.00 0.00 0.00 0.10
0.00 0.00 0.00 0.00 0.00
0.00 0.00 0.00 0.00 0.00 0.00 0.00
0.00 0.00 0.00 0.00 0.00 0.00 0.00
0.00 0.00
1.20 1.20 1.20 1.20 1.20 1.20
H(5C) 0.89 0.00 0.00 0.00 0.10
0.00 0.00 0.00 0.00 0.00
0.00 0.00 0.00 0.00 0.00 0.00 0.00
0.00 0.00 0.00 0.00 0.00 0.00 0.00
0.00 0.00
1.20 1.20 1.20 1.20 1.20 1.20
H(6A) 0.89 0.00 0.00 0.00 0.10
0.00 0.00 0.00 0.00 0.00
0.00 0.00 0.00 0.00 0.00 0.00 0.00
0.00 0.00 0.00 0.00 0.00 0.00 0.00
0.00 0.00
1.20 1.20 1.20 1.20 1.20 1.20
H(6B) 0.89 0.00 0.00 0.00 0.10
0.00 0.00 0.00 0.00 0.00
0.00 0.00 0.00 0.00 0.00 0.00 0.00
0.00 0.00 0.00 0.00 0.00 0.00 0.00
0.00 0.00
1.20 1.20 1.20 1.20 1.20 1.20
H(6C) 0.89 0.00 0.00 0.00 0.10
0.00 0.00 0.00 0.00 0.00
0.00 0.00 0.00 0.00 0.00 0.00 0.00
0.00 0.00 0.00 0.00 0.00 0.00 0.00
0.00 0.00
1.20 1.20 1.20 1.20 1.20 1.20
H(7A) 0.89 0.00 0.00 0.00 0.10
0.00 0.00 0.00 0.00 0.00
0.00 0.00 0.00 0.00 0.00 0.00 0.00
0.00 0.00 0.00 0.00 0.00 0.00 0.00
0.00 0.00
1.20 1.20 1.20 1.20 1.20 1.20
H(7B) 0.82(3) 0.00 0.00 0.00 0.11(2)
0.00 0.00 0.00 0.00 0.00
0.00 0.00 0.00 0.00 0.00 0.00 0.00
0.00 0.00 0.00 0.00 0.00 0.00 0.00
0.00 0.00
1.20 1.20 1.20 1.20 1.20 1.20
H(7C) 0.94(3) 0.00 0.00 0.00 0.17(2)
0.00 0.00 0.00 0.00 0.00
0.00 0.00 0.00 0.00 0.00 0.00 0.00
0.00 0.00 0.00 0.00 0.00 0.00 0.00
0.00 0.00
1.20 1.20 1.20 1.20 1.20 1.20
H(12) 0.888(12) 0.00 0.00 0.00 0.125(9)
0.00 0.00 0.00 0.00 0.00
0.00 0.00 0.00 0.00 0.00 0.00 0.00
0.00 0.00 0.00 0.00 0.00 0.00 0.00
0.00 0.00
1.20 1.20 1.20 1.20 1.20 1.20
H(13) 0.89 0.00 0.00 0.00 0.12
0.00 0.00 0.00 0.00 0.00
0.00 0.00 0.00 0.00 0.00 0.00 0.00
0.00 0.00 0.00 0.00 0.00 0.00 0.00
0.00 0.00
1.20 1.20 1.20 1.20 1.20 1.20
H(14) 0.89 0.00 0.00 0.00 0.12
0.00 0.00 0.00 0.00 0.00
0.00 0.00 0.00 0.00 0.00 0.00 0.00
0.00 0.00 0.00 0.00 0.00 0.00 0.00
0.00 0.00
1.20 1.20 1.20 1.20 1.20 1.20
H(15) 0.89 0.00 0.00 0.00 0.12
0.00 0.00 0.00 0.00 0.00
0.00 0.00 0.00 0.00 0.00 0.00 0.00
0.00 0.00 0.00 0.00 0.00 0.00 0.00
0.00 0.00
1.20 1.20 1.20 1.20 1.20 1.20
loop_
_atom_local_axes_label
_atom_local_axes_atom0
_atom_local_axes_ax1
_atom_local_axes_atom1
_atom_local_axes_atom2
_atom_local_axes_ax2
SI(2) C(7) X SI(2) C(1) Y
SI(1) C(3) X SI(1) C(1) Y
N C(11) X N C(15) Y
C(1) SI(2) X C(1) SI(1) Y
C(2) SI(1) Z C(2) C(1) Y
C(3) SI(1) Z C(3) C(1) Y
C(4) SI(1) Z C(4) C(1) Y
C(5) SI(2) Z C(5) C(1) Y
C(6) SI(2) Z C(6) C(1) Y
C(7) SI(2) Z C(7) C(1) Y
C(11) N Z C(11) C(12) Y
C(12) C(11) X C(12) C(13) Y
C(13) C(12) X C(13) C(14) Y
C(14) C(13) X C(14) C(15) Y
C(15) C(14) X C(15) N Y
LI C(1) X LI SI(2) Y
H(2A) C(2) Z H(2A) SI(1) Y
H(2B) C(2) Z H(2B) SI(1) Y
H(2C) C(2) Z H(2C) SI(1) Y
H(3A) C(3) Z H(3A) SI(1) Y
H(3B) C(3) Z H(3B) SI(1) Y
H(3C) C(3) Z H(3C) SI(1) Y
H(4A) C(4) Z H(4A) SI(1) Y
H(4B) C(4) Z H(4B) SI(1) Y
H(4C) C(4) Z H(4C) SI(1) Y
H(5A) C(5) Z H(5A) SI(2) Y
H(5B) C(5) Z H(5B) SI(2) Y
H(5C) C(5) Z H(5C) SI(2) Y
H(6A) C(6) Z H(6A) SI(2) Y
H(6B) C(6) Z H(6B) SI(2) Y
H(6C) C(6) Z H(6C) SI(2) Y
H(7A) C(7) Z H(7A) SI(2) Y
H(7B) C(7) Z H(7B) SI(2) Y
H(7C) C(7) Z H(7C) SI(2) Y
H(12) C(12) Z H(12) C(13) Y
H(13) C(13) Z H(13) C(12) Y
H(14) C(14) Z H(14) C(15) Y
H(15) C(15) Z H(15) N Y
# End of Crystallographic Information File
# CIF-file generated for li_n_100 / compound 1 / 100 K neutron measurement
#==============================================================================
data_li_n_100 # compound 1 /100 K neutron measurement
_database_code_CSD 169891
#===============================================================================
# 5. CHEMICAL DATA
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety
'C24 H44 Li2 N2 Si4'
_chemical_formula_structural ?
# Ex: 'C12 H16 N2 O6, H2 O' and '(Cd 2+)3, (C6 N6 Cr 3-)2, 2(H2 O)'
_chemical_formula_sum
'C24 H44 Li2 N2 Si4'
_chemical_formula_weight 486.85
_chemical_compound_source 'see text'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_length_neutron
_atom_type_scat_source
Si Si 4.1491
'Sears, V. F. (1992) Neutron News 3, 26-37.'
N N 9.36
'Sears, V. F. (1992) Neutron News 3, 26-37.'
Li Li -1.90
'Sears, V. F. (1992) Neutron News 3, 26-37.'
H H -3.7390
'Sears, V. F. (1992) Neutron News 3, 26-37.'
C C 6.6460
'Sears, V. F. (1992) Neutron News 3, 26-37.'
#===============================================================================
# 6. CRYSTAL DATA
_symmetry_cell_setting Monoclinic
_symmetry_space_group_name_Hall '-P 2yn'
_symmetry_space_group_name_H-M 'P 21/n'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
1/2-x,1/2+y,1/2-z
-x,-y,-z
1/2+x,1/2-y,1/2+z
_cell_length_a 11.7220(13)
_cell_length_b 9.8640(12)
_cell_length_c 12.7517(15)
_cell_angle_alpha 90
_cell_angle_beta 93.479(4)
_cell_angle_gamma 90
_cell_volume 1471.7(3)
_cell_formula_units_Z 2
_cell_measurement_temperature 100(1)
_cell_measurement_reflns_used 4132
_cell_measurement_theta_min 3.93
_cell_measurement_theta_max 39.97
_cell_special_details
; ?
;
_exptl_crystal_description 'plate'
_exptl_crystal_colour 'yellow'
_exptl_crystal_size_max 4.5
_exptl_crystal_size_mid 2.2
_exptl_crystal_size_min 1.7
_exptl_crystal_size_rad ?
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.099
_exptl_crystal_density_method 'Not Measured'
_exptl_crystal_F_000 528
_exptl_absorpt_coefficient_mu 0.231
_exptl_crystal_density_meas_temp ?
# Permitted for _exptl_absorpt_correction_type :
# analytical 'analytical from crystal shape'
# cylinder 'cylindrical'
# empirical 'empirical from intensities'
# gaussian 'Gaussian from crystal shape'
# integration 'integration from crystal shape'
# multi-scan 'symmetry-related measurements'
# none 'no absorption corr. applied'
# numerical 'numerical from crystal shape'
# psi-scan 'psi-scan corrections'
# refdelf 'refined from delta-F'
# sphere 'spherical'
_exptl_absorpt_correction_type none
# Example: '(North, Phillips & Mathews, 1968)'
_exptl_absorpt_process_details ?
_exptl_absorpt_correction_T_min 0.422
_exptl_absorpt_correction_T_max 0.694
#===============================================================================
# 7. EXPERIMENTAL DATA
_exptl_special_details
; ?
;
_diffrn_ambient_temperature 100(1)
_diffrn_radiation_wavelength 0.82306
_diffrn_radiation_type neutron
_diffrn_radiation_monochromator 'Cu 220'
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_details
;
hot neutron four-circle diffractometer D9 at the ILL (Grenoble, France)
;
_diffrn_measurement_method 'profile data from coupled \wx\q scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number 3
_diffrn_standards_interval_count 200
_diffrn_standards_decay_% 0
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
9 0 3 -1 8 2 -2 0 8
# number of measured reflections (redundant set)
_diffrn_reflns_number 4132
_diffrn_reflns_av_R_equivalents 0.0216
_diffrn_reflns_av_sigmaI/netI 0.0508
_diffrn_reflns_limit_h_min -18
_diffrn_reflns_limit_h_max 18
_diffrn_reflns_limit_k_min 0
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_l_min -15
_diffrn_reflns_limit_l_max 15
_diffrn_reflns_theta_min 3.03
_diffrn_reflns_theta_max 39.97
_diffrn_reflns_theta_full 39.97
_diffrn_measured_fraction_theta_max 0.62
_diffrn_measured_fraction_theta_full 0.62
_diffrn_reflns_reduction_process
;
?
;
# number of unique reflections
_reflns_number_total 3811
# number of observed reflections (> n sig(I))
_reflns_number_gt 3145
_reflns_threshold_expression 'I>2\s(I)'
_computing_data_collection 'MAD, HKLGEN (ILL)'
_computing_cell_refinement 'RAFD9 (ILL)'
_computing_data_reduction 'RACER (ILL)'
_computing_structure_solution 'SIR-92 (C. Giacovazzo, 1992)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics 'PLATON (Spek, 1990)'
_computing_publication_material 'PLATON (Spek, 1990)'
#===============================================================================
# 8. REFINEMENT DATA
_refine_special_details
;
Refinement on F^2 for ALL reflections except those
flagged by the user for potential systematic errors.
Weighted R-factors wR and all goodnesses 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
observed criterion of F^2 > 2sigma(F^2) is used only
for calculating -R-factor-obs 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.
Density synthesis with coefficients Fo-Fc
Highest peak 0.57 at 0.2620 0.6585 0.0383 [ 0.78 A from N ]
Deepest hole -0.64 at 0.3720 0.6397 0.0462 [ 0.71 A from N ]
All hydrogen atoms could be located with difference Fourier maps and
were refined anisotropically.
Unit cell contains no residual solvent accessible area.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0226P)^2^+3.057P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens difmap
_refine_ls_hydrogen_treatment refall
_refine_ls_extinction_method 'shelxl'
_refine_ls_extinction_coef 0.0285(8)
_refine_ls_extinction_expression
'FC^*^=KFC[1+0.001XFC^2^\L^3^/SIN(2\Q)]^-1/4^'
_refine_ls_abs_structure_details none
_refine_ls_number_reflns 3811
_refine_ls_number_parameters 344
_refine_ls_number_restraints 0
_refine_ls_number_constraints ?
_refine_ls_R_factor_all 0.0519
_refine_ls_R_factor_gt 0.0330
_refine_ls_wR_factor_ref 0.0776
_refine_ls_wR_factor_gt 0.0670
_refine_ls_goodness_of_fit_ref 1.083
_refine_ls_restrained_S_all 1.083
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_diff_density_max 0.575
_refine_diff_density_min -0.639
_refine_diff_density_rms 0.135
#===============================================================================
# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_thermal_displace_type
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_U_iso_or_equiv
Si1 Si Uani 0.35970(11) 0.36448(15) 0.14255(11) 1.000 0.0147(3)
Si2 Si Uani 0.30233(11) 0.26314(15) -0.08654(12) 1.000 0.0150(3)
N N Uani 0.32145(5) 0.65239(7) 0.01388(5) 1.000 0.0144(1)
C1 C Uani 0.34450(7) 0.40762(9) 0.00074(7) 1.000 0.0123(2)
C2 C Uani 0.21789(9) 0.35774(15) 0.20407(9) 1.000 0.0279(3)
C3 C Uani 0.44730(10) 0.49276(12) 0.22394(9) 1.000 0.0257(3)
C4 C Uani 0.43425(10) 0.19848(12) 0.16972(10) 1.000 0.0270(3)
C5 C Uani 0.25182(10) 0.31850(13) -0.22274(9) 1.000 0.0266(3)
C6 C Uani 0.18767(9) 0.14504(11) -0.04199(9) 1.000 0.0242(3)
C7 C Uani 0.43098(8) 0.15144(12) -0.10682(10) 1.000 0.0253(3)
C11 C Uani 0.27249(7) 0.53084(9) -0.01296(7) 1.000 0.0122(2)
C12 C Uani 0.15549(7) 0.52956(10) -0.04801(8) 1.000 0.0176(2)
C13 C Uani 0.09198(7) 0.64811(11) -0.05324(9) 1.000 0.0206(2)
C14 C Uani 0.14394(8) 0.77074(10) -0.02332(8) 1.000 0.0190(3)
C15 C Uani 0.25900(8) 0.76697(10) 0.00859(8) 1.000 0.0164(2)
Li Li Uani 0.5192(3) 0.3930(4) -0.0528(3) 1.000 0.0218(9)
H2A H Uani 0.2290(3) 0.3352(5) 0.2873(2) 1.000 0.0683(15)
H2B H Uani 0.1637(3) 0.2786(4) 0.1684(3) 1.000 0.0530(10)
H2C H Uani 0.1717(3) 0.4520(4) 0.1943(3) 1.000 0.0571(11)
H3A H Uani 0.4503(3) 0.4618(4) 0.3061(2) 1.000 0.0539(10)
H3B H Uani 0.4114(3) 0.5943(3) 0.2208(2) 1.000 0.0503(9)
H3C H Uani 0.5368(2) 0.4980(4) 0.2028(3) 1.000 0.0505(9)
H4A H Uani 0.4423(3) 0.1822(4) 0.2550(3) 1.000 0.0565(10)
H4B H Uani 0.5204(2) 0.1970(4) 0.1419(3) 1.000 0.0525(10)
H4C H Uani 0.3882(3) 0.1119(3) 0.1353(3) 1.000 0.0527(10)
H5A H Uani 0.2397(4) 0.2307(4) -0.2729(3) 1.000 0.0637(13)
H5B H Uani 0.3112(4) 0.3833(5) -0.2581(3) 1.000 0.0775(15)
H5C H Uani 0.1704(3) 0.3707(5) -0.2263(3) 1.000 0.0739(13)
H6A H Uani 0.1737(3) 0.0630(3) -0.0990(3) 1.000 0.0516(9)
H6B H Uani 0.1064(2) 0.1968(3) -0.0367(3) 1.000 0.0533(9)
H6C H Uani 0.2100(3) 0.0990(3) 0.0344(3) 1.000 0.0522(10)
H7A H Uani 0.4025(3) 0.0622(3) -0.1507(3) 1.000 0.0603(12)
H7B H Uani 0.4751(3) 0.1179(4) -0.0345(3) 1.000 0.0558(10)
H7C H Uani 0.4947(3) 0.1990(3) -0.1546(3) 1.000 0.0512(9)
H12 H Uani 0.1145(2) 0.4338(2) -0.0680(3) 1.000 0.0397(7)
H13 H Uani 0.00191(18) 0.6446(3) -0.0801(3) 1.000 0.0434(8)
H14 H Uani 0.0973(2) 0.8657(2) -0.0267(2) 1.000 0.0384(7)
H15 H Uani 0.3045(2) 0.8593(2) 0.0311(2) 1.000 0.0361(6)
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
Si1 0.0125(5) 0.0183(6) 0.0131(6) 0.0031(5) -0.0006(4) 0.0005(5)
Si2 0.0120(5) 0.0159(6) 0.0170(7) -0.0030(5) 0.0004(5) -0.0001(4)
N 0.0122(2) 0.0143(2) 0.0164(3) -0.0012(2) -0.0010(2) 0.0007(2)
C1 0.0110(3) 0.0133(3) 0.0124(4) 0.0000(3) 0.0000(3) 0.0003(3)
C2 0.0193(4) 0.0456(7) 0.0195(5) 0.0068(5) 0.0061(3) 0.0012(5)
C3 0.0313(5) 0.0282(5) 0.0167(5) -0.0008(4) -0.0056(4) -0.0064(4)
C4 0.0280(5) 0.0228(5) 0.0293(6) 0.0087(4) -0.0059(4) 0.0054(4)
C5 0.0241(5) 0.0372(6) 0.0177(5) -0.0036(4) -0.0046(4) -0.0036(4)
C6 0.0193(4) 0.0180(4) 0.0354(6) -0.0034(4) 0.0028(4) -0.0054(4)
C7 0.0175(4) 0.0222(4) 0.0362(6) -0.0105(4) 0.0019(4) 0.0035(4)
C11 0.0099(3) 0.0136(3) 0.0131(4) 0.0003(3) -0.0001(3) 0.0001(3)
C12 0.0105(3) 0.0159(4) 0.0260(5) 0.0010(3) -0.0022(3) 0.0001(3)
C13 0.0112(3) 0.0180(4) 0.0322(5) 0.0030(4) -0.0019(3) 0.0022(3)
C14 0.0148(4) 0.0165(4) 0.0259(5) 0.0029(3) 0.0018(3) 0.0039(3)
C15 0.0150(3) 0.0143(4) 0.0197(4) -0.0014(3) 0.0004(3) 0.0010(3)
Li 0.0118(12) 0.0314(17) 0.0223(17) -0.0015(14) 0.0008(11) 0.0015(12)
H2A 0.0516(17) 0.127(4) 0.0268(14) 0.0164(18) 0.0074(12) -0.003(2)
H2B 0.0362(13) 0.0625(19) 0.0609(19) 0.0027(15) 0.0080(12) -0.0127(13)
H2C 0.0428(15) 0.062(2) 0.068(2) -0.0005(16) 0.0169(14) 0.0166(14)
H3A 0.073(2) 0.0625(19) 0.0243(13) 0.0061(12) -0.0119(12) -0.0129(16)
H3B 0.074(2) 0.0341(13) 0.0421(15) -0.0086(11) -0.0010(13) -0.0002(13)
H3C 0.0342(12) 0.0664(19) 0.0501(16) 0.0010(14) -0.0039(11) -0.0158(13)
H4A 0.076(2) 0.0534(18) 0.0385(16) 0.0180(13) -0.0106(14) 0.0100(15)
H4B 0.0352(13) 0.0541(17) 0.068(2) 0.0066(15) 0.0003(12) 0.0157(12)
H4C 0.0632(18) 0.0270(12) 0.0660(19) 0.0009(12) -0.0129(15) 0.0005(12)
H5A 0.090(3) 0.061(2) 0.0388(17) -0.0213(15) -0.0057(16) -0.0057(19)
H5B 0.082(3) 0.104(3) 0.0441(17) 0.0275(19) -0.0153(17) -0.051(2)
H5C 0.064(2) 0.113(3) 0.0427(17) -0.0005(19) -0.0134(15) 0.042(2)
H6A 0.0567(17) 0.0389(14) 0.0595(18) -0.0201(13) 0.0048(14) -0.0176(12)
H6B 0.0282(11) 0.0421(14) 0.091(2) 0.0021(15) 0.0149(13) 0.0008(10)
H6C 0.0570(17) 0.0482(16) 0.0509(17) 0.0126(13) 0.0000(13) -0.0135(13)
H7A 0.0445(15) 0.0421(15) 0.094(3) -0.0399(16) 0.0023(16) -0.0006(12)
H7B 0.0512(16) 0.0612(19) 0.0541(17) 0.0014(15) -0.0054(13) 0.0275(14)
H7C 0.0389(13) 0.0488(15) 0.068(2) -0.0085(14) 0.0211(13) 0.0023(12)
H12 0.0240(9) 0.0246(10) 0.0692(18) -0.0038(10) -0.0082(10) -0.0042(8)
H13 0.0188(9) 0.0395(12) 0.0704(18) 0.0031(12) -0.0089(10) 0.0035(9)
H14 0.0327(10) 0.0255(10) 0.0569(15) 0.0030(10) 0.0024(10) 0.0119(8)
H15 0.0316(10) 0.0223(9) 0.0536(14) -0.0065(9) -0.0049(9) -0.0026(8)
#===============================================================================
# 10. MOLECULAR GEOMETRY
_geom_special_details
;
Bond distances, angles etc. have been calculated using the
rounded fractional coordinates. All esds are estimated
from the variances of the (full) variance-covariance matrix.
The cell esds are taken into account in the estimation of
distances, angles and torsion angles
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Si1 C1 1.8557(17) . . yes
Si1 C2 1.8818(17) . . yes
Si1 C3 1.8982(18) . . yes
Si1 C4 1.8783(19) . . yes
Si2 C1 1.8567(17) . . yes
Si2 C5 1.8816(19) . . yes
Si2 C6 1.8918(18) . . yes
Si2 C7 1.8980(17) . . yes
Si2 Li 2.856(4) . . yes
N C11 1.3639(11) . . yes
N C15 1.3460(12) . . yes
N Li 1.955(4) . 3_665 yes
C1 C11 1.4841(12) . . no
C1 Li 2.202(4) . . yes
C11 C12 1.4165(12) . . no
C12 C13 1.3857(14) . . no
C13 C14 1.3970(14) . . no
C14 C15 1.3854(13) . . no
C2 H2A 1.084(3) . . no
C2 H2B 1.088(4) . . no
C2 H2C 1.079(4) . . no
C3 H3A 1.090(3) . . no
C3 H3B 1.086(3) . . no
C3 H3C 1.100(3) . . no
C4 H4A 1.098(4) . . no
C4 H4B 1.091(3) . . no
C4 H4C 1.088(3) . . no
C5 H5A 1.081(4) . . no
C5 H5B 1.065(5) . . no
C5 H5C 1.083(4) . . no
C6 H6A 1.093(4) . . no
C6 H6B 1.087(3) . . no
C6 H6C 1.092(4) . . no
C7 H7A 1.085(3) . . no
C7 H7B 1.081(4) . . no
C7 H7C 1.097(4) . . no
C12 H12 1.083(2) . . no
C13 H13 1.091(2) . . no
C14 H14 1.084(2) . . no
C15 H15 1.085(2) . . no
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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Si1 C2 112.29(8) . . . yes
C1 Si1 C3 113.37(9) . . . yes
C1 Si1 C4 113.31(9) . . . yes
C2 Si1 C3 104.94(9) . . . yes
C2 Si1 C4 107.77(9) . . . yes
C3 Si1 C4 104.48(8) . . . yes
C1 Si2 C5 112.83(9) . . . yes
C1 Si2 C6 117.44(9) . . . yes
C1 Si2 C7 110.02(8) . . . yes
C1 Si2 Li 50.45(9) . . . yes
C5 Si2 C6 105.45(8) . . . yes
C5 Si2 C7 104.53(9) . . . yes
C5 Si2 Li 103.67(10) . . . yes
C6 Si2 C7 105.56(9) . . . yes
C6 Si2 Li 150.82(11) . . . yes
C7 Si2 Li 64.76(9) . . . yes
C11 N C15 120.42(7) . . . yes
C11 N Li 104.08(13) . . 3_665 yes
C15 N Li 135.50(13) . . 3_665 yes
Si1 C1 Si2 114.48(8) . . . yes
Si1 C1 C11 108.83(7) . . . yes
Si1 C1 Li 104.53(11) . . . yes
Si2 C1 C11 115.42(7) . . . yes
Si2 C1 Li 89.01(11) . . . yes
C11 C1 Li 123.37(12) . . . yes
N C11 C1 117.57(7) . . . yes
N C11 C12 118.14(8) . . . yes
C1 C11 C12 124.25(8) . . . no
C11 C12 C13 120.98(9) . . . no
C12 C13 C14 119.57(8) . . . no
C13 C14 C15 117.23(9) . . . no
N C15 C14 123.64(9) . . . yes
H2A C2 H2C 108.6(3) . . . no
H2B C2 H2C 107.1(3) . . . no
Si1 C2 H2C 111.8(2) . . . no
Si1 C2 H2A 111.0(2) . . . no
Si1 C2 H2B 111.0(2) . . . no
H2A C2 H2B 107.1(3) . . . no
Si1 C3 H3A 108.9(2) . . . no
H3B C3 H3C 108.7(3) . . . no
Si1 C3 H3C 112.9(2) . . . no
H3A C3 H3B 106.5(3) . . . no
Si1 C3 H3B 113.52(19) . . . no
H3A C3 H3C 105.8(3) . . . no
Si1 C4 H4B 112.4(2) . . . no
Si1 C4 H4C 113.3(2) . . . no
Si1 C4 H4A 108.7(2) . . . no
H4A C4 H4B 107.1(3) . . . no
H4A C4 H4C 107.2(3) . . . no
H4B C4 H4C 107.7(3) . . . no
Si2 C5 H5B 112.8(2) . . . no
Si2 C5 H5C 113.8(2) . . . no
H5A C5 H5B 107.2(3) . . . no
Si2 C5 H5A 109.7(2) . . . no
H5A C5 H5C 105.8(4) . . . no
H5B C5 H5C 107.1(4) . . . no
Si2 C6 H6A 109.7(2) . . . no
H6A C6 H6C 107.7(3) . . . no
H6B C6 H6C 107.7(3) . . . no
H6A C6 H6B 107.0(3) . . . no
Si2 C6 H6B 111.77(18) . . . no
Si2 C6 H6C 112.8(2) . . . no
Si2 C7 H7A 108.6(2) . . . no
H7B C7 H7C 107.3(3) . . . no
Si2 C7 H7C 113.62(19) . . . no
H7A C7 H7B 107.9(3) . . . no
Si2 C7 H7B 113.8(2) . . . no
H7A C7 H7C 105.0(3) . . . no
C11 C12 H12 119.29(15) . . . no
C13 C12 H12 119.69(15) . . . no
C12 C13 H13 119.70(18) . . . no
C14 C13 H13 120.73(18) . . . no
C13 C14 H14 121.79(15) . . . no
C15 C14 H14 120.96(15) . . . no
N C15 H15 115.74(14) . . . no
C14 C15 H15 120.61(15) . . . no
N Li C1 145.9(2) 3_665 . . yes
Si2 Li N 139.77(19) . . 3_665 yes
Si2 Li C1 40.55(7) . . . yes
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
C2 Si1 C1 Si2 -80.14(11) . . . . no
C3 Si1 C1 Si2 161.13(8) . . . . no
C4 Si1 C1 Si2 42.26(11) . . . . no
C2 Si1 C1 C11 50.68(11) . . . . no
C3 Si1 C1 C11 -68.06(10) . . . . no
C4 Si1 C1 C11 173.07(8) . . . . no
C2 Si1 C1 Li -175.78(13) . . . . no
C3 Si1 C1 Li 65.48(14) . . . . no
C4 Si1 C1 Li -53.39(14) . . . . no
C5 Si2 C1 Si1 165.33(8) . . . . no
C6 Si2 C1 Si1 42.36(11) . . . . no
C7 Si2 C1 Si1 -78.37(10) . . . . no
Li Si2 C1 Si1 -105.54(12) . . . . no
C5 Si2 C1 C11 37.80(11) . . . . no
C6 Si2 C1 C11 -85.17(11) . . . . no
C7 Si2 C1 C11 154.10(8) . . . . no
Li Si2 C1 C11 126.93(13) . . . . no
C5 Si2 C1 Li -89.13(13) . . . . no
C6 Si2 C1 Li 147.90(13) . . . . no
C7 Si2 C1 Li 27.17(13) . . . . no
C6 Si2 Li N 50.9(4) . . . 3_665 no
C7 Si2 Li N -25.5(2) . . . 3_665 no
C5 Si2 Li C1 108.48(11) . . . . no
C6 Si2 Li C1 -75.3(2) . . . . no
C7 Si2 Li C1 -151.69(13) . . . . no
C1 Si2 Li N 126.2(3) . . . 3_665 no
C5 Si2 Li N -125.3(3) . . . 3_665 no
C11 N Li C1 -95.1(4) 3_665 3_665 . . no
C15 N Li C1 84.4(4) 3_665 3_665 . . no
Li N C11 C12 -178.49(13) 3_665 . . . no
Li N C15 C14 179.50(17) 3_665 . . . no
C11 N Li Si2 -164.4(2) 3_665 3_665 . . no
C11 N C15 C14 0.05(15) . . . . no
Li N C11 C1 3.96(14) 3_665 . . . no
C15 N C11 C12 1.10(12) . . . . no
C15 N C11 C1 -176.45(8) . . . . no
C15 N Li Si2 15.1(4) 3_665 3_665 . . no
C11 N C15 H15 -179.84(18) . . . . no
Li N C15 H15 -0.4(3) 3_665 . . . no
C11 C1 Li Si2 -120.17(12) . . . . no
Si1 C1 Li N 3.5(4) . . . 3_665 no
Si2 C1 Li N -111.6(4) . . . 3_665 no
Li C1 C11 N -47.07(16) . . . . no
Si2 C1 C11 N -153.93(8) . . . . no
Si2 C1 C11 C12 28.68(13) . . . . no
Si1 C1 C11 C12 -101.62(10) . . . . no
Li C1 C11 C12 135.54(14) . . . . no
Si1 C1 Li Si2 115.07(9) . . . . no
C11 C1 Li N 128.2(3) . . . 3_665 no
Si1 C1 C11 N 75.76(9) . . . . no
C1 C11 C12 C13 176.31(9) . . . . no
N C11 C12 C13 -1.06(14) . . . . no
C11 C12 C13 C14 -0.13(16) . . . . no
C12 C13 C14 C15 1.25(15) . . . . no
C13 C14 C15 N -1.26(15) . . . . no
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
Si1 Li 3.041(4) . 3_665 no
Si2 Li 4.311(4) . 3_665 no
Si1 H6C 3.398(4) . . no
Si2 H4C 3.301(4) . . no
Si2 H12 2.793(3) . . no
Si2 H3C 3.412(4) . 3_665 no
N C3 3.3691(14) . . no
N H3B 2.840(3) . . no
C3 N 3.3691(14) . . no
C3 Li 2.508(4) . 3_665 no
C4 C7 3.5547(18) . . no
C5 C12 3.2984(16) . . no
C5 C14 3.5610(16) . 2_544 no
C7 C4 3.5547(18) . . no
C12 C5 3.2984(16) . . no
C14 C5 3.5610(16) . 2_554 no
C2 H13 2.940(3) . 3_565 no
C3 H5B 3.090(5) . 3_665 no
C4 H5C 3.073(4) . 4_555 no
C4 H7B 2.792(4) . . no
C5 H12 2.857(3) . . no
C5 H3C 3.067(3) . 3_665 no
C6 H2B 3.017(4) . . no
C6 H12 2.987(2) . . no
C6 H14 2.963(2) . 1_545 no
C11 H2C 3.060(4) . . no
C12 H5C 2.775(4) . . no
C12 H13 3.064(3) . 3_565 no
C13 H12 3.059(3) . 3_565 no
C13 H6B 3.064(3) . 3_565 no
C14 H6A 3.067(3) . 1_565 no
C14 H5A 3.033(4) . 2_554 no
C14 H5B 3.075(4) . 2_554 no
C14 H6B 3.094(3) . 3_565 no
C15 H2A 2.684(3) . 2_555 no
C15 H5A 3.028(4) . 2_554 no
Li Si2 4.311(4) . 3_665 no
Li C3 2.508(4) . 3_665 no
Li Si1 3.041(4) . 3_665 no
Li Li 2.558(6) . 3_665 no
Li H3C 3.414(5) . . no
Li H4B 3.146(5) . . no
Li H3B 2.341(5) . 3_665 no
Li H3C 2.257(5) . 3_665 no
H2A C15 2.684(3) . 2_545 no
H2A H15 2.384(4) . 2_545 no
H2B C6 3.017(4) . . no
H2B H6C 2.543(5) . . no
H2B H3B 2.495(5) . 2_545 no
H2B H13 2.312(5) . 3_565 no
H2C C11 3.060(4) . . no
H3B N 2.840(3) . . no
H3B H2B 2.495(5) . 2_555 no
H3B Li 2.341(5) . 3_665 no
H3B H7C 2.489(4) . 3_665 no
H3C Li 3.414(5) . . no
H3C Si2 3.412(4) . 3_665 no
H3C C5 3.067(3) . 3_665 no
H3C Li 2.257(5) . 3_665 no
H3C H5B 2.211(6) . 3_665 no
H4B Li 3.146(5) . . no
H4B H7B 2.409(5) . . no
H4B H5C 2.450(5) . 4_555 no
H4C Si2 3.301(4) . . no
H4C H6C 2.389(5) . . no
H4C H7B 2.449(5) . . no
H5A C14 3.033(4) . 2_544 no
H5A C15 3.028(4) . 2_544 no
H5B C14 3.075(4) . 2_544 no
H5B H6A 2.556(6) . 2_554 no
H5B C3 3.090(5) . 3_665 no
H5B H3C 2.211(6) . 3_665 no
H5C C12 2.775(4) . . no
H5C H12 2.248(5) . . no
H5C H7A 2.568(6) . 2_554 no
H5C C4 3.073(4) . 4_454 no
H5C H4B 2.450(5) . 4_454 no
H6A C14 3.067(3) . 1_545 no
H6A H14 2.354(4) . 1_545 no
H6A H5B 2.556(6) . 2_544 no
H6B H12 2.374(4) . . no
H6B C13 3.064(3) . 3_565 no
H6B C14 3.094(3) . 3_565 no
H6B H13 2.551(4) . 3_565 no
H6C Si1 3.398(4) . . no
H6C H2B 2.543(5) . . no
H6C H4C 2.389(5) . . no
H7A H5C 2.568(6) . 2_544 no
H7B C4 2.792(4) . . no
H7B H4B 2.409(5) . . no
H7B H4C 2.449(5) . . no
H7B H7B 2.542(6) . 3_655 no
H7B H15 2.591(4) . 3_665 no
H7C H3B 2.489(4) . 3_665 no
H12 Si2 2.793(3) . . no
H12 C5 2.857(3) . . no
H12 C6 2.987(2) . . no
H12 H5C 2.248(5) . . no
H12 H6B 2.374(4) . . no
H12 C13 3.059(3) . 3_565 no
H12 H13 2.518(5) . 3_565 no
H13 C2 2.940(3) . 3_565 no
H13 C12 3.064(3) . 3_565 no
H13 H2B 2.312(5) . 3_565 no
H13 H6B 2.551(4) . 3_565 no
H13 H12 2.518(5) . 3_565 no
H14 C6 2.963(2) . 1_565 no
H14 H6A 2.354(4) . 1_565 no
H15 H2A 2.384(4) . 2_555 no
H15 H7B 2.591(4) . 3_665 no
# End of Crystallographic Information File
# CIF-file generated for li_n_20 / compound 1 /20 K neutron measurement
#==============================================================================
data_li_n_20 # compound 1 / 20 K neutron measurement
_database_code_CSD 169892
#===============================================================================
# 5. CHEMICAL DATA
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety
'C24 H44 Li2 N2 Si4'
_chemical_formula_structural ?
# Ex: 'C12 H16 N2 O6, H2 O' and '(Cd 2+)3, (C6 N6 Cr 3-)2, 2(H2 O)'
_chemical_formula_sum
'C24 H44 Li2 N2 Si4'
_chemical_formula_weight 486.85
_chemical_compound_source 'see text'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_length_neutron
_atom_type_scat_source
Si Si 4.1491
'Sears, V. F. (1992) Neutron News 3, 26-37.'
N N 9.36
'Sears, V. F. (1992) Neutron News 3, 26-37.'
Li Li -1.90
'Sears, V. F. (1992) Neutron News 3, 26-37.'
H H -3.7390
'Sears, V. F. (1992) Neutron News 3, 26-37.'
C C 6.6460
'Sears, V. F. (1992) Neutron News 3, 26-37.'
#===============================================================================
# 6. CRYSTAL DATA
_symmetry_cell_setting Monoclinic
_symmetry_space_group_name_Hall '-P 2yn'
_symmetry_space_group_name_H-M 'P 21/n'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
1/2-x,1/2+y,1/2-z
-x,-y,-z
1/2+x,1/2-y,1/2+z
_cell_length_a 11.6982(5)
_cell_length_b 9.8218(5)
_cell_length_c 12.6895(6)
_cell_angle_alpha 90
_cell_angle_beta 93.5114(19)
_cell_angle_gamma 90
_cell_volume 1455.25(12)
_cell_formula_units_Z 2
_cell_measurement_temperature 20(1)
_cell_measurement_reflns_used 4077
_cell_measurement_theta_min 3.08
_cell_measurement_theta_max 33.78
_cell_special_details
; ?
;
_exptl_crystal_description 'plate'
_exptl_crystal_colour 'yellow'
_exptl_crystal_size_max 4.5
_exptl_crystal_size_mid 2.2
_exptl_crystal_size_min 1.7
_exptl_crystal_size_rad ?
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.111
_exptl_crystal_density_method 'Not Measured'
_exptl_crystal_F_000 528
_exptl_absorpt_coefficient_mu 0.231
_exptl_crystal_density_meas_temp ?
# Permitted for _exptl_absorpt_correction_type :
# analytical 'analytical from crystal shape'
# cylinder 'cylindrical'
# empirical 'empirical from intensities'
# gaussian 'Gaussian from crystal shape'
# integration 'integration from crystal shape'
# multi-scan 'symmetry-related measurements'
# none 'no absorption corr. applied'
# numerical 'numerical from crystal shape'
# psi-scan 'psi-scan corrections'
# refdelf 'refined from delta-F'
# sphere 'spherical'
_exptl_absorpt_correction_type none
# Example: '(North, Phillips & Mathews, 1968)'
_exptl_absorpt_process_details ?
_exptl_absorpt_correction_T_min 0.422
_exptl_absorpt_correction_T_max 0.694
#===============================================================================
# 7. EXPERIMENTAL DATA
_exptl_special_details
; ?
;
_diffrn_ambient_temperature 20(1)
_diffrn_radiation_wavelength 0.95070
_diffrn_radiation_type neutron
_diffrn_radiation_monochromator 'Cu 220'
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_details
;
thermal neutron four-circle diffractometer D19 at the ILL (Grenoble, France)
;
_diffrn_measurement_method 'profile data from \w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number 3
_diffrn_standards_interval_count 200
_diffrn_standards_decay_% 0
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
9 0 3 -1 8 2 -2 0 8
# number of measured reflections (redundant set)
_diffrn_reflns_number 4077
_diffrn_reflns_av_R_equivalents 0.0407
_diffrn_reflns_av_sigmaI/netI 0.0429
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_k_min -5
_diffrn_reflns_limit_k_max 11
_diffrn_reflns_limit_l_min -5
_diffrn_reflns_limit_l_max 14
_diffrn_reflns_theta_min 3.08
_diffrn_reflns_theta_max 33.78
_diffrn_reflns_theta_full 33.78
_diffrn_measured_fraction_theta_max 0.83
_diffrn_measured_fraction_theta_full 0.83
_diffrn_reflns_reduction_process
;
?
;
# number of unique reflections
_reflns_number_total 2161
# number of observed reflections (> n sig(I))
_reflns_number_gt 1844
_reflns_threshold_expression 'I>2\s(I)'
_computing_data_collection 'MAD, HKLGEN (ILL)'
_computing_cell_refinement 'RAFD19 (ILL)'
_computing_data_reduction 'RETREAT (ILL)'
_computing_structure_solution 'SIR-92 (C. Giacovazzo, 1992)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics 'PLATON (Spek, 1990)'
_computing_publication_material 'PLATON (Spek, 1990)'
#===============================================================================
# 8. REFINEMENT DATA
_refine_special_details
;
Refinement on F^2 for ALL reflections except those
flagged by the user for potential systematic errors.
Weighted R-factors wR and all goodnesses 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
observed criterion of F^2 > 2sigma(F^2) is used only
for calculating -R-factor-obs 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.
Density synthesis with coefficients Fo-Fc
Highest peak 0.40 at 0.0434 0.0170 0.4231 [ 0.98 A from LI ]
Deepest hole -0.38 at 0.1651 0.0371 0.5636 [ 1.00 A from C11 ]
All hydrogen atoms could be located with difference Fourier maps and
were refined anisotropically.
Unit cell contains no residual solvent accessible area.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0314P)^2^+1.3674P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens difmap
_refine_ls_hydrogen_treatment refall
_refine_ls_extinction_method shelxl
_refine_ls_extinction_coef 0.0203(7)
_refine_ls_extinction_expression
'FC^*^=KFC[1+0.001XFC^2^\L^3^/SIN(2\Q)]^-1/4^'
_refine_ls_abs_structure_details none
_refine_ls_number_reflns 2161
_refine_ls_number_parameters 344
_refine_ls_number_restraints 0
_refine_ls_number_constraints ?
_refine_ls_R_factor_all 0.0425
_refine_ls_R_factor_gt 0.0311
_refine_ls_wR_factor_ref 0.0687
_refine_ls_wR_factor_gt 0.0652
_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 0.403
_refine_diff_density_min -0.377
_refine_diff_density_rms 0.096
#===============================================================================
# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_thermal_displace_type
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_U_iso_or_equiv
Si1 Si Uani 0.35926(15) 0.36443(19) 0.14273(14) 1.000 0.0049(5)
Si2 Si Uani 0.30227(15) 0.26266(19) -0.08745(14) 1.000 0.0054(5)
N N Uani 0.32122(7) 0.65396(9) 0.01344(6) 1.000 0.0063(2)
C1 C Uani 0.34450(10) 0.40827(12) 0.00011(9) 1.000 0.0053(3)
C2 C Uani 0.21661(11) 0.35694(14) 0.20372(10) 1.000 0.0097(4)
C3 C Uani 0.44635(11) 0.49360(14) 0.22454(10) 1.000 0.0100(4)
C4 C Uani 0.43409(11) 0.19746(13) 0.17012(11) 1.000 0.0098(4)
C5 C Uani 0.25123(11) 0.31810(14) -0.22433(10) 1.000 0.0102(4)
C6 C Uani 0.18755(10) 0.14406(13) -0.04250(10) 1.000 0.0086(4)
C7 C Uani 0.43153(11) 0.15108(14) -0.10778(11) 1.000 0.0098(4)
C11 C Uani 0.27203(10) 0.53179(12) -0.01337(9) 1.000 0.0046(3)
C12 C Uani 0.15487(10) 0.53024(13) -0.04835(9) 1.000 0.0068(4)
C13 C Uani 0.09083(10) 0.64931(13) -0.05307(9) 1.000 0.0082(4)
C14 C Uani 0.14303(10) 0.77224(13) -0.02320(10) 1.000 0.0076(4)
C15 C Uani 0.25822(10) 0.76880(13) 0.00838(9) 1.000 0.0064(4)
Li Li Uani 0.5193(4) 0.3925(5) -0.0535(3) 1.000 0.0113(12)
H2A H Uani 0.2276(3) 0.3342(4) 0.2874(2) 1.000 0.0372(10)
H2B H Uani 0.1634(2) 0.2774(3) 0.1672(3) 1.000 0.0323(9)
H2C H Uani 0.1707(3) 0.4535(3) 0.1949(3) 1.000 0.0348(10)
H3A H Uani 0.4487(3) 0.4632(3) 0.3080(2) 1.000 0.0328(10)
H3B H Uani 0.4100(3) 0.5952(3) 0.2209(2) 1.000 0.0296(9)
H3C H Uani 0.5358(3) 0.4982(3) 0.2035(2) 1.000 0.0319(10)
H4A H Uani 0.4422(3) 0.1814(3) 0.2550(2) 1.000 0.0329(10)
H4B H Uani 0.5206(2) 0.1970(3) 0.1419(2) 1.000 0.0313(10)
H4C H Uani 0.3882(3) 0.1100(3) 0.1355(3) 1.000 0.0312(9)
H5A H Uani 0.2399(3) 0.2290(3) -0.2748(2) 1.000 0.0349(10)
H5B H Uani 0.3128(3) 0.3820(4) -0.2606(3) 1.000 0.0405(10)
H5C H Uani 0.1712(3) 0.3722(4) -0.2273(2) 1.000 0.0407(11)
H6A H Uani 0.1735(3) 0.0620(3) -0.0997(3) 1.000 0.0321(9)
H6B H Uani 0.1060(3) 0.1966(3) -0.0371(3) 1.000 0.0329(10)
H6C H Uani 0.2096(3) 0.0981(3) 0.0346(2) 1.000 0.0318(9)
H7A H Uani 0.4026(3) 0.0606(3) -0.1513(3) 1.000 0.0355(10)
H7B H Uani 0.4757(3) 0.1167(3) -0.0348(3) 1.000 0.0352(10)
H7C H Uani 0.4945(3) 0.1978(3) -0.1559(3) 1.000 0.0326(9)
H12 H Uani 0.1137(2) 0.4341(3) -0.0687(2) 1.000 0.0217(8)
H13 H Uani 0.0010(2) 0.6457(3) -0.0800(2) 1.000 0.0257(9)
H14 H Uani 0.0962(2) 0.8680(3) -0.0260(2) 1.000 0.0230(8)
H15 H Uani 0.3042(2) 0.8619(3) 0.0302(2) 1.000 0.0223(8)
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
Si1 0.0074(9) 0.0038(9) 0.0036(9) 0.0017(7) 0.0012(7) -0.0015(7)
Si2 0.0071(9) 0.0036(9) 0.0054(9) 0.0005(7) -0.0004(7) -0.0015(7)
N 0.0070(4) 0.0038(4) 0.0079(4) -0.0004(3) -0.0001(3) 0.0004(3)
C1 0.0065(5) 0.0040(6) 0.0052(6) 0.0006(4) -0.0002(4) 0.0010(4)
C2 0.0085(6) 0.0134(8) 0.0076(8) 0.0024(6) 0.0026(5) 0.0001(6)
C3 0.0140(8) 0.0096(8) 0.0062(7) -0.0004(5) -0.0013(5) -0.0031(6)
C4 0.0124(7) 0.0063(7) 0.0106(8) 0.0016(5) -0.0008(5) 0.0015(6)
C5 0.0130(7) 0.0121(7) 0.0052(6) 0.0004(6) -0.0015(5) -0.0015(7)
C6 0.0093(7) 0.0058(6) 0.0109(7) -0.0008(6) 0.0021(5) -0.0025(5)
C7 0.0093(6) 0.0082(7) 0.0122(7) -0.0026(6) 0.0028(6) 0.0025(5)
C11 0.0059(6) 0.0033(6) 0.0047(6) -0.0001(5) 0.0002(4) 0.0004(5)
C12 0.0052(6) 0.0044(7) 0.0106(6) 0.0007(5) -0.0003(4) -0.0001(5)
C13 0.0078(7) 0.0057(6) 0.0109(6) 0.0001(5) -0.0005(5) 0.0015(5)
C14 0.0073(6) 0.0050(7) 0.0106(6) 0.0003(5) 0.0012(5) 0.0008(5)
C15 0.0071(6) 0.0039(7) 0.0082(6) 0.0007(5) 0.0005(4) 0.0005(5)
Li 0.010(2) 0.011(2) 0.013(2) -0.0017(19) 0.0009(17) -0.0005(18)
H2A 0.0353(16) 0.065(2) 0.0118(16) 0.0082(14) 0.0054(11) -0.0014(15)
H2B 0.0248(14) 0.0324(17) 0.0396(17) -0.0057(14) 0.0011(13) -0.0102(14)
H2C 0.0317(16) 0.0257(17) 0.0482(19) 0.0025(14) 0.0128(13) 0.0103(14)
H3A 0.0478(18) 0.0362(17) 0.0138(16) 0.0051(13) -0.0023(12) -0.0087(14)
H3B 0.0381(16) 0.0179(16) 0.0323(16) -0.0035(12) -0.0012(12) 0.0042(13)
H3C 0.0213(17) 0.0388(18) 0.0353(17) -0.0011(14) 0.0005(13) -0.0071(13)
H4A 0.0465(18) 0.0321(16) 0.0198(18) 0.0067(13) -0.0010(12) 0.0071(14)
H4B 0.0235(16) 0.0331(17) 0.0380(17) 0.0028(13) 0.0085(13) 0.0056(12)
H4C 0.0361(16) 0.0150(14) 0.0414(17) -0.0031(13) -0.0066(13) -0.0066(13)
H5A 0.055(2) 0.0270(18) 0.0219(16) -0.0096(14) -0.0050(14) -0.0010(14)
H5B 0.0421(18) 0.051(2) 0.0279(16) 0.0169(16) -0.0021(14) -0.0234(17)
H5C 0.0379(19) 0.059(2) 0.0247(16) 0.0015(15) -0.0026(13) 0.0249(18)
H6A 0.0401(17) 0.0229(16) 0.0336(16) -0.0121(15) 0.0052(13) -0.0097(13)
H6B 0.0204(15) 0.0273(15) 0.052(2) 0.0046(14) 0.0112(13) 0.0057(13)
H6C 0.0379(16) 0.0341(16) 0.0231(17) 0.0136(14) -0.0006(12) -0.0047(13)
H7A 0.0346(16) 0.0231(16) 0.0485(19) -0.0194(15) 0.0009(14) -0.0007(13)
H7B 0.0379(16) 0.0404(18) 0.0264(17) 0.0023(14) -0.0043(14) 0.0174(14)
H7C 0.0291(15) 0.0306(16) 0.0403(18) 0.0020(14) 0.0192(15) 0.0003(14)
H12 0.0196(12) 0.0104(14) 0.0348(15) -0.0041(11) -0.0014(11) -0.0033(11)
H13 0.0160(15) 0.0232(14) 0.0370(16) -0.0031(12) -0.0051(12) 0.0016(11)
H14 0.0218(13) 0.0119(14) 0.0353(15) 0.0007(11) 0.0010(11) 0.0062(12)
H15 0.0226(13) 0.0122(14) 0.0317(15) -0.0053(11) -0.0005(11) -0.0025(12)
#===============================================================================
# 10. MOLECULAR GEOMETRY
_geom_special_details
;
Bond distances, angles etc. have been calculated using the
rounded fractional coordinates. All esds are estimated
from the variances of the (full) variance-covariance matrix.
The cell esds are taken into account in the estimation of
distances, angles and torsion angles
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Si1 C1 1.858(2) . . yes
Si1 C2 1.883(2) . . yes
Si1 C3 1.896(2) . . yes
Si1 C4 1.881(2) . . yes
Si2 C1 1.859(2) . . yes
Si2 C5 1.882(2) . . yes
Si2 C6 1.891(2) . . yes
Si2 C7 1.898(2) . . yes
Si2 Li 2.850(5) . . yes
N C11 1.3648(15) . . yes
N C15 1.3467(15) . . yes
N Li 1.957(5) . 3_665 yes
C1 C11 1.4839(17) . . no
C1 Li 2.200(5) . . yes
C11 C12 1.4146(17) . . no
C12 C13 1.3882(18) . . no
C13 C14 1.3950(18) . . no
C14 C15 1.3825(17) . . no
C2 H2A 1.085(3) . . no
C2 H2B 1.085(3) . . no
C2 H2C 1.092(3) . . no
C3 H3A 1.099(3) . . no
C3 H3B 1.085(3) . . no
C3 H3C 1.097(4) . . no
C4 H4A 1.087(3) . . no
C4 H4B 1.094(3) . . no
C4 H4C 1.091(3) . . no
C5 H5A 1.088(3) . . no
C5 H5B 1.079(4) . . no
C5 H5C 1.075(4) . . no
C6 H6A 1.090(4) . . no
C6 H6B 1.090(4) . . no
C6 H6C 1.094(3) . . no
C7 H7A 1.089(4) . . no
C7 H7B 1.086(4) . . no
C7 H7C 1.087(4) . . no
C12 H12 1.084(3) . . no
C13 H13 1.086(3) . . no
C14 H14 1.088(3) . . no
C15 H15 1.088(3) . . no
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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Si1 C2 112.18(10) . . . yes
C1 Si1 C3 113.14(11) . . . yes
C1 Si1 C4 113.35(11) . . . yes
C2 Si1 C3 105.13(10) . . . yes
C2 Si1 C4 107.70(11) . . . yes
C3 Si1 C4 104.70(10) . . . yes
C1 Si2 C5 112.74(11) . . . yes
C1 Si2 C6 117.45(11) . . . yes
C1 Si2 C7 109.92(10) . . . yes
C1 Si2 Li 50.50(10) . . . yes
C5 Si2 C6 105.40(10) . . . yes
C5 Si2 C7 104.59(10) . . . yes
C5 Si2 Li 103.85(12) . . . yes
C6 Si2 C7 105.74(11) . . . yes
C6 Si2 Li 150.68(13) . . . yes
C7 Si2 Li 64.48(12) . . . yes
C11 N C15 120.22(9) . . . yes
C11 N Li 103.91(16) . . 3_665 yes
C15 N Li 135.87(16) . . 3_665 yes
Si1 C1 Si2 114.16(10) . . . yes
Si1 C1 C11 108.67(10) . . . yes
Si1 C1 Li 104.61(13) . . . yes
Si2 C1 C11 115.53(10) . . . yes
Si2 C1 Li 88.80(14) . . . yes
C11 C1 Li 123.87(15) . . . yes
N C11 C1 117.44(10) . . . yes
N C11 C12 118.25(10) . . . yes
C1 C11 C12 124.27(11) . . . no
C11 C12 C13 120.96(11) . . . no
C12 C13 C14 119.43(11) . . . no
C13 C14 C15 117.40(11) . . . no
N C15 C14 123.72(11) . . . yes
H2A C2 H2C 107.9(3) . . . no
H2B C2 H2C 108.4(3) . . . no
Si1 C2 H2C 111.5(2) . . . no
Si1 C2 H2A 110.8(2) . . . no
Si1 C2 H2B 110.62(19) . . . no
H2A C2 H2B 107.5(3) . . . no
Si1 C3 H3A 109.07(19) . . . no
H3B C3 H3C 109.2(3) . . . no
Si1 C3 H3C 112.52(18) . . . no
H3A C3 H3B 106.1(2) . . . no
Si1 C3 H3B 113.3(2) . . . no
H3A C3 H3C 106.1(3) . . . no
Si1 C4 H4B 111.87(18) . . . no
Si1 C4 H4C 113.6(2) . . . no
Si1 C4 H4A 108.72(19) . . . no
H4A C4 H4B 107.3(3) . . . no
H4A C4 H4C 107.2(3) . . . no
H4B C4 H4C 107.9(3) . . . no
Si2 C5 H5B 112.3(2) . . . no
Si2 C5 H5C 113.68(17) . . . no
H5A C5 H5B 106.1(3) . . . no
Si2 C5 H5A 109.32(18) . . . no
H5A C5 H5C 107.6(3) . . . no
H5B C5 H5C 107.5(3) . . . no
Si2 C6 H6A 109.6(2) . . . no
H6A C6 H6C 107.9(3) . . . no
H6B C6 H6C 107.4(3) . . . no
H6A C6 H6B 107.1(3) . . . no
Si2 C6 H6B 111.5(2) . . . no
Si2 C6 H6C 113.0(2) . . . no
Si2 C7 H7A 108.3(2) . . . no
H7B C7 H7C 107.9(3) . . . no
Si2 C7 H7C 113.9(2) . . . no
H7A C7 H7B 107.2(3) . . . no
Si2 C7 H7B 113.9(2) . . . no
H7A C7 H7C 105.1(3) . . . no
C11 C12 H12 119.47(17) . . . no
C13 C12 H12 119.53(17) . . . no
C12 C13 H13 119.71(19) . . . no
C14 C13 H13 120.87(19) . . . no
C13 C14 H14 121.88(17) . . . no
C15 C14 H14 120.70(18) . . . no
N C15 H15 115.54(17) . . . no
C14 C15 H15 120.74(18) . . . no
N Li C1 145.6(2) 3_665 . . yes
Si2 Li N 139.6(2) . . 3_665 yes
Si2 Li C1 40.70(9) . . . yes
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
C2 Si1 C1 Si2 -79.87(13) . . . . no
C3 Si1 C1 Si2 161.40(10) . . . . no
C4 Si1 C1 Si2 42.38(14) . . . . no
C2 Si1 C1 C11 50.69(14) . . . . no
C3 Si1 C1 C11 -68.05(13) . . . . no
C4 Si1 C1 C11 172.93(10) . . . . no
C2 Si1 C1 Li -175.21(16) . . . . no
C3 Si1 C1 Li 66.05(17) . . . . no
C4 Si1 C1 Li -52.97(17) . . . . no
C5 Si2 C1 Si1 165.04(10) . . . . no
C6 Si2 C1 Si1 42.20(15) . . . . no
C7 Si2 C1 Si1 -78.70(13) . . . . no
Li Si2 C1 Si1 -105.49(15) . . . . no
C5 Si2 C1 C11 37.95(14) . . . . no
C6 Si2 C1 C11 -84.89(14) . . . . no
C7 Si2 C1 C11 154.22(10) . . . . no
Li Si2 C1 C11 127.42(15) . . . . no
C5 Si2 C1 Li -89.47(15) . . . . no
C6 Si2 C1 Li 147.69(15) . . . . no
C7 Si2 C1 Li 26.79(15) . . . . no
C6 Si2 Li N 50.3(5) . . . 3_665 no
C7 Si2 Li N -26.0(3) . . . 3_665 no
C5 Si2 Li C1 108.23(13) . . . . no
C6 Si2 Li C1 -75.6(3) . . . . no
C7 Si2 Li C1 -151.99(15) . . . . no
C1 Si2 Li N 126.0(3) . . . 3_665 no
C5 Si2 Li N -125.8(3) . . . 3_665 no
C11 N Li C1 -95.1(4) 3_665 3_665 . . no
C15 N Li C1 85.3(5) 3_665 3_665 . . no
Li N C11 C12 -179.00(15) 3_665 . . . no
Li N C15 C14 -179.57(19) 3_665 . . . no
C11 N Li Si2 -164.3(2) 3_665 3_665 . . no
C11 N C15 C14 -0.03(16) . . . . no
Li N C11 C1 3.25(16) 3_665 . . . no
C15 N C11 C12 1.33(15) . . . . no
C15 N C11 C1 -176.42(10) . . . . no
C15 N Li Si2 16.1(4) 3_665 3_665 . . no
C11 N C15 H15 -179.31(17) . . . . no
Li N C15 H15 1.1(3) 3_665 . . . no
C11 C1 Li Si2 -120.34(14) . . . . no
Si1 C1 Li N 3.1(5) . . . 3_665 no
Si2 C1 Li N -111.6(4) . . . 3_665 no
Li C1 C11 N -46.89(18) . . . . no
Si2 C1 C11 N -153.90(10) . . . . no
Si2 C1 C11 C12 28.51(16) . . . . no
Si1 C1 C11 C12 -101.30(13) . . . . no
Li C1 C11 C12 135.52(16) . . . . no
Si1 C1 Li Si2 114.68(11) . . . . no
C11 C1 Li N 128.1(4) . . . 3_665 no
Si1 C1 C11 N 76.30(12) . . . . no
C1 C11 C12 C13 176.15(11) . . . . no
N C11 C12 C13 -1.43(17) . . . . no
C11 C12 C13 C14 0.23(17) . . . . no
C12 C13 C14 C15 1.04(17) . . . . no
C13 C14 C15 N -1.19(18) . . . . no
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
Si1 Li 3.033(5) . 3_665 no
Si2 Li 4.309(5) . 3_665 no
Si1 H6C 3.391(4) . . no
Si2 H4C 3.304(4) . . no
Si2 H12 2.797(3) . . no
Si2 H3C 3.408(4) . 3_665 no
N C3 3.3643(15) . . no
N H3B 2.830(3) . . no
C3 N 3.3643(15) . . no
C3 Li 2.496(4) . 3_665 no
C4 C7 3.554(2) . . no
C5 C12 3.3026(18) . . no
C5 C14 3.5330(18) . 2_544 no
C7 C4 3.554(2) . . no
C12 C5 3.3026(18) . . no
C14 C5 3.5330(18) . 2_554 no
C2 H13 2.908(3) . 3_565 no
C3 H5B 3.079(4) . 3_665 no
C4 H5C 3.068(4) . 4_555 no
C4 H7B 2.790(4) . . no
C5 H12 2.859(3) . . no
C5 H3C 3.074(4) . 3_665 no
C6 H2B 2.995(4) . . no
C6 H12 2.989(3) . . no
C6 H14 2.927(3) . 1_545 no
C11 H2C 3.060(4) . . no
C12 H5C 2.767(3) . . no
C12 H13 3.054(3) . 3_565 no
C13 H12 3.039(3) . 3_565 no
C13 H6B 3.037(4) . 3_565 no
C14 H6A 3.035(3) . 1_565 no
C14 H5A 3.009(3) . 2_554 no
C14 H5B 3.021(4) . 2_554 no
C14 H6B 3.072(4) . 3_565 no
C15 H2A 2.665(3) . 2_555 no
C15 H5A 2.991(3) . 2_554 no
Li Si2 4.309(5) . 3_665 no
Li C3 2.496(4) . 3_665 no
Li Si1 3.033(5) . 3_665 no
Li Li 2.565(7) . 3_665 no
Li H3C 3.417(5) . . no
Li H4B 3.135(5) . . no
Li H3B 2.329(5) . 3_665 no
Li H3C 2.245(5) . 3_665 no
H2A C15 2.665(3) . 2_545 no
H2A H15 2.382(4) . 2_545 no
H2B C6 2.995(4) . . no
H2B H6C 2.517(4) . . no
H2B H3B 2.471(4) . 2_545 no
H2B H13 2.288(4) . 3_565 no
H2C C11 3.060(4) . . no
H2C H13 2.598(4) . 3_565 no
H3B N 2.830(3) . . no
H3B H2B 2.471(4) . 2_555 no
H3B Li 2.329(5) . 3_665 no
H3B H7C 2.485(4) . 3_665 no
H3C Li 3.417(5) . . no
H3C Si2 3.408(4) . 3_665 no
H3C C5 3.074(4) . 3_665 no
H3C Li 2.245(5) . 3_665 no
H3C H5B 2.211(5) . 3_665 no
H4B Li 3.135(5) . . no
H4B H7B 2.404(5) . . no
H4B H5C 2.442(4) . 4_555 no
H4C Si2 3.304(4) . . no
H4C H6C 2.385(5) . . no
H4C H7B 2.448(5) . . no
H5A C14 3.009(3) . 2_544 no
H5A C15 2.991(3) . 2_544 no
H5B C14 3.021(4) . 2_544 no
H5B H6A 2.516(5) . 2_554 no
H5B C3 3.079(4) . 3_665 no
H5B H3C 2.211(5) . 3_665 no
H5C C12 2.767(3) . . no
H5C H12 2.245(4) . . no
H5C H7A 2.526(5) . 2_554 no
H5C C4 3.068(4) . 4_454 no
H5C H4B 2.442(4) . 4_454 no
H6A C14 3.035(3) . 1_545 no
H6A H14 2.330(4) . 1_545 no
H6A H5B 2.516(5) . 2_544 no
H6B H12 2.370(4) . . no
H6B C13 3.037(4) . 3_565 no
H6B C14 3.072(4) . 3_565 no
H6B H13 2.530(4) . 3_565 no
H6C Si1 3.391(4) . . no
H6C H2B 2.517(4) . . no
H6C H4C 2.385(5) . . no
H6C H15 2.572(4) . 1_545 no
H7A H5C 2.526(5) . 2_544 no
H7B C4 2.790(4) . . no
H7B H4B 2.404(5) . . no
H7B H4C 2.448(5) . . no
H7B H7B 2.509(4) . 3_655 no
H7B H15 2.580(4) . 3_665 no
H7C H3B 2.485(4) . 3_665 no
H12 Si2 2.797(3) . . no
H12 C5 2.859(3) . . no
H12 C6 2.989(3) . . no
H12 H5C 2.245(4) . . no
H12 H6B 2.370(4) . . no
H12 C13 3.039(3) . 3_565 no
H12 H13 2.507(4) . 3_565 no
H13 C2 2.908(3) . 3_565 no
H13 C12 3.054(3) . 3_565 no
H13 H2B 2.288(4) . 3_565 no
H13 H2C 2.598(4) . 3_565 no
H13 H6B 2.530(4) . 3_565 no
H13 H12 2.507(4) . 3_565 no
H14 C6 2.927(3) . 1_565 no
H14 H6A 2.330(4) . 1_565 no
H15 H6C 2.572(4) . 1_565 no
H15 H2A 2.382(4) . 2_555 no
H15 H7B 2.580(4) . 3_665 no
# End of Crystallographic Information File