# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2011
data_global
_journal_name_full 'Dalton Trans.'
_journal_coden_cambridge 0222
#TrackingRef '- RAL_R43_fin_with_sq_toluene.cif'
#==============================================================================
# 0. AUDIT DETAILS
_audit_creation_date 'Jul 18 00:31:00 2011'
_audit_creation_method 'PLATON
option'
_audit_update_record
;
;
#===============================================================================
# 1. SUBMISSION DETAILS
_publ_contact_author_name # Name of author for correspondence
'Richard Layfield'
_publ_contact_author_address # address of author for correspondence
;
;
_publ_contact_author_email Richard.Layfield@manchester.ac.uk
_publ_contact_author_fax ?
_publ_contact_author_phone ?
# Publication choise FI, CI or EI for Inorganic
# FM, CM or EM for Metal-organic
# FO, CO or EO for Organic
_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 in Acta Crystallographica C.
;
#===============================================================================
# 2. PROCESSING SUMMARY (JOURNAL OFFICE ONLY)
_journal_date_recd_electronic ?
_journal_date_to_coeditor ?
_journal_date_from_coeditor ?
_journal_date_accepted ?
_journal_date_printers_first ?
_journal_date_printers_final ?
_journal_date_proofs_out ?
_journal_date_proofs_in ?
_journal_coeditor_name ?
_journal_coeditor_code ?
_journal_coeditor_notes
;
;
_journal_techeditor_code ?
_journal_techeditor_notes
;
;
_journal_coden_ASTM ?
_journal_year ?
_journal_volume ?
_journal_issue ?
_journal_page_first ?
_journal_page_last ?
_journal_suppl_publ_number ?
_journal_suppl_publ_pages ?
#===============================================================================
# 3. TITLE AND AUTHOR LIST
_publ_section_title
;
;
_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.
loop_
_publ_author_name
_publ_author_footnote
_publ_author_address
# author name
'Daniel Woodruff'
; # author related footnote
;
; # Address of this author
;
'Michael Bodensteiner' '' ''
'Daniel Sells' '' ''
R.Winpenny '' ''
'Richard Layfield' '' ''
#===============================================================================
# 4. TEXT
_publ_section_synopsis
;
?
;
_publ_section_abstract
;
?
;
# Insert blank lines between paragraphs
_publ_section_comment
;
;
_publ_section_exptl_prep
;
?
;
_publ_section_exptl_refinement
;
The structure was solved by chargeflipping methods (SUPERFLIP) and refined by
full-matrix anisotropic least squares (SHELXL97). Cobalt is disordered over
four positions with 0.25 occupancy. Hence, Lithium occupies those positions
with 0.75. EADP and EXYZ constraints were used for the refinement of these
atoms. The H-atoms were calculated geometrically and a riding model was used
during refinement process. The solvent toluene molecules were treated with
SQUEEZE, for disorder at the symmetry reason. Details are given below.
;
# Insert blank lines between references
_publ_section_references
;
Clark, R. C.; Reid, J. S. (1995) Acta Cryst., A51, 887-897.
Cosier, J.; Glazer, A.M. (1986) J. Appl. Cryst., 19, 105-107.
Farrugia, L. J. (1999) J. Appl. Cryst., 32, 837-838.
Palatinus, L., Chapuis G. (2007) J. Appl. Cryst., 40, 786-790.
Sheldrick, G. M. (2008) Acta Cryst., A64, 112-122.
Sluis, P.; Spek, A. L. (1990). Acta Cryst., A46, 194-201.
Spek, A. L. (2003). J. Appl. Cryst. 36, 7-13.
;
_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_RAL_R43
_database_code_depnum_ccdc_archive 'CCDC 815986'
#TrackingRef '- RAL_R43_fin_with_sq_toluene.cif'
#===============================================================================
# 5. CHEMICAL DATA
_chemical_name_systematic
;
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety
'C42 H72 Co Li7 N18 O, C30 H90 Cl Li5 N5 Si10, 2(C7 H8)'
_chemical_formula_structural ?
_chemical_formula_sum 'C86 H178 Cl Co Li12 N23 O Si10'
_chemical_formula_iupac ?
_chemical_formula_weight 2009.07
_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
C C 0.0181 0.0091 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co -2.3653 3.6143 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Li Li 0.0008 0.0003 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 ' 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 '-C 2yc'
_symmetry_space_group_name_H-M 'C 2/c'
_symmetry_Int_Tables_number 15
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 -x,y,1/2-z
3 -x,-y,-z
4 x,-y,1/2+z
5 1/2+x,1/2+y,z
6 1/2-x,1/2+y,1/2-z
7 1/2-x,1/2-y,-z
8 1/2+x,1/2-y,1/2+z
_cell_length_a 20.1006(4)
_cell_length_b 24.5598(4)
_cell_length_c 24.9957(5)
_cell_angle_alpha 90
_cell_angle_beta 105.786(2)
_cell_angle_gamma 90
_cell_volume 11874.2(4)
_cell_formula_units_Z 4
_cell_measurement_temperature 123(1)
_cell_measurement_reflns_used 25312
_cell_measurement_theta_min 3.0876
_cell_measurement_theta_max 76.3759
_cell_special_details
;
;
_exptl_crystal_description block
_exptl_crystal_colour blue
_exptl_crystal_size_max 0.44
_exptl_crystal_size_mid 0.22
_exptl_crystal_size_min 0.14
_exptl_crystal_size_rad ?
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.124
_exptl_crystal_density_method 'Not Measured'
_exptl_crystal_F_000 4332
_exptl_absorpt_coefficient_mu 2.679
_exptl_crystal_density_meas_temp ?
_exptl_absorpt_correction_T_min 0.414
_exptl_absorpt_correction_T_max 0.783
_exptl_absorpt_correction_type analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
;
#===============================================================================
# 7. EXPERIMENTAL DATA
_exptl_special_details
;
;
_diffrn_ambient_temperature 123(1)
_diffrn_radiation_wavelength 1.54178
_diffrn_radiation_probe x-ray
_diffrn_radiation_type CuK\a
_diffrn_radiation_source 'SuperNova (Cu) X-ray Source'
_diffrn_radiation_monochromator mirrors
_diffrn_measurement_device_type 'SuperNova,Single source at offset,Atlas'
_diffrn_measurement_method '\w scans'
_diffrn_detector_area_resol_mean 10.3546
# number of measured reflections (redundant set)
_diffrn_reflns_number 43649
_diffrn_reflns_av_R_equivalents 0.0275
_diffrn_reflns_av_sigmaI/netI 0.0293
_diffrn_reflns_limit_h_min -24
_diffrn_reflns_limit_h_max 25
_diffrn_reflns_limit_k_min -30
_diffrn_reflns_limit_k_max 29
_diffrn_reflns_limit_l_min -31
_diffrn_reflns_limit_l_max 29
_diffrn_reflns_theta_min 3.09
_diffrn_reflns_theta_max 76.56
_diffrn_reflns_theta_full 76.56
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measured_fraction_theta_full 0.988
_diffrn_reflns_reduction_process
;
;
# number of unique reflections
_reflns_number_total 12325
# number of observed reflections (> n sig(I))
_reflns_number_gt 11569
_reflns_threshold_expression >2\s(i)
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_structure_solution 'SUPERFLIP (Palatinus,2007)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics 'SXGRAPH (Farrugia, 1999)'
_computing_publication_material 'PLATON (Spek, 2003)'
#===============================================================================
# 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.
;
_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^)+(0.0755P)^2^+17.0756P] 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_abs_structure_details ?
_refine_ls_abs_structure_Flack .
_refine_ls_number_reflns 12325
_refine_ls_number_parameters 598
_refine_ls_number_restraints 0
_refine_ls_number_constraints ?
_refine_ls_R_factor_all 0.0654
_refine_ls_R_factor_gt 0.0630
_refine_ls_wR_factor_ref 0.1764
_refine_ls_wR_factor_gt 0.1748
_refine_ls_goodness_of_fit_ref 1.088
_refine_ls_restrained_S_all 1.088
_refine_ls_shift/su_max 0.006
_refine_ls_shift/su_mean 0.001
_refine_diff_density_max 0.642
_refine_diff_density_min -0.481
_refine_diff_density_rms 0.054
#===============================================================================
# 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
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co Uani 0.98001(6) 0.01575(6) 0.07413(6) 0.250 0.0481(4) d P A 2
Co2 Co Uani 0.92118(7) -0.05010(6) 0.00402(6) 0.250 0.0569(5) d P . 2
O1 O Uani 1.00000 0.00000 0.00000 1.000 0.0453(7) d S . .
N1 N Uani 0.89807(11) 0.06711(10) 0.04422(11) 1.000 0.0600(8) d . . .
N2 N Uani 0.77577(10) 0.06403(10) 0.01772(10) 1.000 0.0525(7) d . . .
N3 N Uani 0.84174(11) 0.00376(11) -0.02083(11) 1.000 0.0607(8) d . . .
N4 N Uani 1.07067(12) 0.04672(10) 0.11620(11) 1.000 0.0585(8) d . A .
N5 N Uani 1.10608(12) 0.13730(11) 0.14092(13) 1.000 0.0664(9) d . . .
N6 N Uani 1.06384(15) 0.10999(10) 0.04683(13) 1.000 0.0696(10) d . . .
N7 N Uani 0.95460(16) -0.06293(12) 0.08992(13) 1.000 0.0729(10) d . A .
N8 N Uani 1.0155(3) -0.1145(3) 0.1591(2) 0.600 0.081(2) d P A 1
N9 N Uani 1.06152(15) -0.09103(12) 0.08444(13) 1.000 0.0709(9) d . . .
C1 C Uani 0.83821(12) 0.04517(11) 0.01370(12) 1.000 0.0521(8) d . . .
C2 C Uani 0.89207(15) 0.11549(13) 0.07660(14) 1.000 0.0626(10) d . . .
C3 C Uani 0.83550(16) 0.10885(14) 0.10543(14) 1.000 0.0648(10) d . . .
C4 C Uani 0.76826(14) 0.10178(13) 0.06051(14) 1.000 0.0622(10) d . . .
C5 C Uani 0.71044(13) 0.05179(14) -0.02369(12) 1.000 0.0604(9) d . . .
C6 C Uani 0.72128(15) 0.01999(16) -0.07152(14) 1.000 0.0682(10) d . . .
C7 C Uani 0.77551(14) -0.02255(15) -0.04886(16) 1.000 0.0701(11) d . . .
C8 C Uani 1.08066(13) 0.09836(12) 0.10162(14) 1.000 0.0576(9) d . A .
C9 C Uani 1.09659(16) 0.03339(15) 0.17538(14) 1.000 0.0701(11) d . . .
C10 C Uani 1.07737(18) 0.07790(16) 0.21055(15) 1.000 0.0766(13) d . . .
C11 C Uani 1.11158(18) 0.12972(16) 0.19980(16) 1.000 0.0790(11) d . . .
C12 C Uani 1.1305(2) 0.18985(14) 0.1275(2) 1.000 0.0900(16) d . . .
C13 C Uani 1.1324(3) 0.19292(18) 0.0688(2) 1.000 0.114(2) d . . .
C14 C Uani 1.0683(3) 0.16745(15) 0.0329(2) 1.000 0.0957(18) d . . .
C15 C Uani 1.01108(18) -0.09335(14) 0.10898(13) 1.000 0.0666(10) d . . .
C16 C Uani 0.9014(2) -0.06987(18) 0.11887(16) 1.000 0.1013(18) d . . .
C17 C Uani 0.9240(2) -0.05535(18) 0.17580(16) 0.600 0.093(3) d RP A 1
C18 C Uani 0.9727(5) -0.1002(4) 0.1979(3) 0.600 0.113(4) d P A 1
C19 C Uani 1.0780(6) -0.1710(3) 0.1718(4) 0.600 0.097(4) d P A 1
C20 C Uani 1.1388(5) -0.1496(4) 0.1586(4) 0.600 0.106(3) d P A 1
C21 C Uani 1.12289(12) -0.12373(11) 0.10438(11) 1.000 0.1004(16) d . . .
Li1 Li Uani 0.98001(6) 0.01575(6) 0.07413(6) 0.750 0.0481(4) d P . 1
Li2 Li Uani 0.92118(7) -0.05010(6) 0.00402(6) 0.750 0.0569(5) d P . 1
Li3 Li Uani 1.08646(15) -0.01462(11) 0.06516(14) 1.000 0.0263(8) d . . .
Li4 Li Uani 0.97026(14) 0.07772(13) 0.00021(13) 1.000 0.0288(9) d . . .
C18A C Uani 0.9511(6) -0.1618(3) 0.1532(4) 0.400 0.083(4) d P A 2
C19A C Uani 1.0741(7) -0.1455(5) 0.1843(5) 0.400 0.081(4) d P A 2
C20A C Uani 1.1075(6) -0.1675(4) 0.1406(5) 0.400 0.075(4) d P A 2
C17A C Uani 0.8904(6) -0.1326(5) 0.1226(5) 0.400 0.098(4) d P A 2
N8A N Uani 1.0172(5) -0.1419(2) 0.1440(3) 0.400 0.061(3) d P A 2
Cl1 Cl Uani 0.00000 0.48622(3) 0.25000 1.000 0.0504(3) d S . .
Si1 Si Uani 0.13799(4) 0.63603(3) 0.23817(4) 1.000 0.0592(3) d . . .
Si2 Si Uani 0.02355(4) 0.61921(4) 0.13602(4) 1.000 0.0641(3) d . . .
Si3 Si Uani 0.07216(4) 0.42324(4) 0.10353(3) 1.000 0.0530(2) d . . .
Si4 Si Uani 0.19357(3) 0.44054(3) 0.20040(3) 1.000 0.0525(2) d . . .
Si5 Si Uani 0.06601(3) 0.31165(2) 0.29524(3) 1.000 0.0441(2) d . . .
N10 N Uani 0.06701(11) 0.59998(9) 0.20193(10) 1.000 0.0527(7) d . . .
N11 N Uani 0.10627(10) 0.44249(9) 0.17131(8) 1.000 0.0447(6) d . . .
N12 N Uani 0.00000 0.34555(10) 0.25000 1.000 0.0402(7) d S . .
C22 C Uani 0.19491(12) 0.59326(11) 0.29451(11) 1.000 0.0643(10) d R . .
C23 C Uani 0.1133(2) 0.69813(13) 0.27248(18) 1.000 0.0810(13) d . . .
C24 C Uani 0.19597(17) 0.66234(16) 0.19556(17) 1.000 0.0809(13) d . . .
C25 C Uani 0.06734(17) 0.59616(19) 0.08240(15) 1.000 0.0835(13) d . . .
C26 C Uani 0.0102(2) 0.69424(17) 0.1227(2) 1.000 0.1038(18) d . . .
C27 C Uani -0.06535(15) 0.58809(16) 0.11866(15) 1.000 0.0714(11) d . . .
C28 C Uani -0.01670(14) 0.45328(15) 0.07584(13) 1.000 0.0645(10) d . . .
C29 C Uani 0.12312(18) 0.44492(19) 0.05416(13) 1.000 0.0805(13) d . . .
C30 C Uani 0.06310(18) 0.34777(15) 0.09562(14) 1.000 0.0720(11) d . . .
C31 C Uani 0.23935(16) 0.50076(17) 0.17944(15) 1.000 0.0751(13) d . . .
C32 C Uani 0.21166(15) 0.44289(13) 0.27826(12) 1.000 0.0585(9) d . . .
C33 C Uani 0.23945(17) 0.37874(18) 0.18369(15) 1.000 0.0798(13) d . . .
C34 C Uani 0.04096(16) 0.24778(11) 0.32690(14) 1.000 0.0652(9) d . . .
C35 C Uani 0.13524(15) 0.28973(12) 0.26232(13) 1.000 0.0627(9) d . . .
C36 C Uani 0.10868(14) 0.35854(11) 0.35412(10) 1.000 0.0505(7) d . . .
Li5 Li Uani 0.00000 0.5863(3) 0.25000 1.000 0.0505(19) d S . .
Li6 Li Uani 0.0768(2) 0.51681(17) 0.19502(19) 1.000 0.0482(12) d . . .
Li7 Li Uani 0.0459(2) 0.40561(16) 0.21497(16) 1.000 0.0418(11) d . . .
H4A H Uiso 0.73300 0.08830 0.07710 1.000 0.0750 c R . .
H3B H Uiso 0.84450 0.07720 0.12960 1.000 0.0780 c R . .
H2A H Uiso 0.88210 0.14690 0.05220 1.000 0.0750 c R . .
H2B H Uiso 0.93570 0.12200 0.10410 1.000 0.0750 c R . .
H3A H Uiso 0.83320 0.14070 0.12780 1.000 0.0780 c R . .
H7A H Uiso 0.76080 -0.04560 -0.02270 1.000 0.0840 c R . .
H7B H Uiso 0.78140 -0.04530 -0.07900 1.000 0.0840 c R . .
H9A H Uiso 1.14650 0.02940 0.18510 1.000 0.0840 c R . .
H9B H Uiso 1.07700 -0.00090 0.18280 1.000 0.0840 c R . .
H10A H Uiso 1.02760 0.08260 0.20060 1.000 0.0920 c R . .
H10B H Uiso 1.09310 0.06840 0.24960 1.000 0.0920 c R . .
H11A H Uiso 1.09020 0.16040 0.21310 1.000 0.0950 c R . .
H11B H Uiso 1.16000 0.12890 0.22040 1.000 0.0950 c R . .
H12A H Uiso 1.17650 0.19640 0.15150 1.000 0.1080 c R . .
H12B H Uiso 1.10030 0.21820 0.13450 1.000 0.1080 c R . .
H13A H Uiso 1.17280 0.17390 0.06420 1.000 0.1370 c R . .
H13B H Uiso 1.13520 0.23060 0.05810 1.000 0.1370 c R . .
H14A H Uiso 1.02820 0.18660 0.03780 1.000 0.1150 c R . .
H14B H Uiso 1.06820 0.17070 -0.00580 1.000 0.1150 c R . .
H16A H Uiso 0.86170 -0.04770 0.10080 0.600 0.1220 c RP A 1
H16B H Uiso 0.88670 -0.10760 0.11590 0.600 0.1220 c RP A 1
H17A H Uiso 0.88600 -0.05460 0.19280 0.600 0.1120 d RP A 1
H17B H Uiso 0.94730 -0.02040 0.18110 0.600 0.1120 d RP A 1
H18A H Uiso 0.94700 -0.13200 0.20370 0.600 0.1350 c RP A 1
H18B H Uiso 1.00310 -0.08950 0.23360 0.600 0.1350 c RP A 1
H19A H Uiso 1.08910 -0.18250 0.21040 0.600 0.1170 c RP A 1
H19B H Uiso 1.05960 -0.20180 0.14830 0.600 0.1170 c RP A 1
H20A H Uiso 1.17130 -0.17900 0.15970 0.600 0.1270 c RP A 1
H20B H Uiso 1.16090 -0.12320 0.18680 0.600 0.1270 c RP A 1
H21A H Uiso 1.16200 -0.10090 0.10380 0.600 0.1210 c RP A 1
H21B H Uiso 1.12090 -0.15230 0.07720 0.600 0.1210 c RP A 1
H4B H Uiso 0.75320 0.13680 0.04370 1.000 0.0750 c R . .
H5A H Uiso 0.68700 0.08560 -0.03730 1.000 0.0720 c R . .
H5B H Uiso 0.68090 0.03120 -0.00620 1.000 0.0720 c R . .
H6A H Uiso 0.73640 0.04400 -0.09680 1.000 0.0820 c R . .
H6B H Uiso 0.67840 0.00280 -0.09180 1.000 0.0820 c R . .
H16C H Uiso 0.85870 -0.05260 0.09840 0.400 0.1220 d RP A 2
H16D H Uiso 0.91600 -0.05380 0.15570 0.400 0.1220 d RP A 2
H17C H Uiso 0.85360 -0.13890 0.14020 0.400 0.1170 c RP A 2
H17D H Uiso 0.87540 -0.14730 0.08530 0.400 0.1170 c RP A 2
H18C H Uiso 0.94550 -0.19990 0.14290 0.400 0.1000 c RP A 2
H18D H Uiso 0.95430 -0.15920 0.19250 0.400 0.1000 c RP A 2
H19C H Uiso 1.07210 -0.17160 0.21300 0.400 0.0960 c RP A 2
H19D H Uiso 1.09250 -0.11080 0.20010 0.400 0.0960 c RP A 2
H20C H Uiso 1.15010 -0.18610 0.15910 0.400 0.0900 c RP A 2
H20D H Uiso 1.07670 -0.19400 0.11760 0.400 0.0900 c RP A 2
H21C H Uiso 1.16070 -0.10140 0.12560 0.400 0.1210 d RP A 2
H21D H Uiso 1.13640 -0.13950 0.07330 0.400 0.1210 d RP A 2
H22A H Uiso 0.16670 0.57090 0.31110 1.000 0.0960 c R . .
H22B H Uiso 0.22350 0.61650 0.32230 1.000 0.0960 c R . .
H22C H Uiso 0.22370 0.57050 0.27890 1.000 0.0960 c R . .
H23A H Uiso 0.08500 0.72150 0.24470 1.000 0.1210 c R . .
H23B H Uiso 0.15440 0.71730 0.29200 1.000 0.1210 c R . .
H23C H Uiso 0.08800 0.68730 0.29820 1.000 0.1210 c R . .
H24A H Uiso 0.21420 0.63220 0.17960 1.000 0.1210 c R . .
H24B H Uiso 0.23340 0.68270 0.21910 1.000 0.1210 c R . .
H24C H Uiso 0.16970 0.68540 0.16640 1.000 0.1210 c R . .
H25A H Uiso 0.10680 0.61880 0.08420 1.000 0.1260 c R . .
H25B H Uiso 0.03560 0.59890 0.04610 1.000 0.1260 c R . .
H25C H Uiso 0.08200 0.55900 0.08950 1.000 0.1260 c R . .
H26A H Uiso -0.01110 0.70960 0.14930 1.000 0.1550 c R . .
H26B H Uiso -0.01910 0.69990 0.08590 1.000 0.1550 c R . .
H26C H Uiso 0.05410 0.71150 0.12630 1.000 0.1550 c R . .
H27A H Uiso -0.06180 0.55050 0.12950 1.000 0.1070 c R . .
H27B H Uiso -0.08630 0.59080 0.07940 1.000 0.1070 c R . .
H27C H Uiso -0.09320 0.60710 0.13830 1.000 0.1070 c R . .
H28A H Uiso -0.03830 0.45660 0.10550 1.000 0.0970 c R . .
H28B H Uiso -0.04410 0.43000 0.04750 1.000 0.0970 c R . .
H28C H Uiso -0.01300 0.48860 0.06040 1.000 0.0970 c R . .
H29A H Uiso 0.13030 0.48360 0.05680 1.000 0.1210 c R . .
H29B H Uiso 0.09800 0.43550 0.01680 1.000 0.1210 c R . .
H29C H Uiso 0.16700 0.42670 0.06370 1.000 0.1210 c R . .
H30A H Uiso 0.10800 0.33160 0.10180 1.000 0.1080 c R . .
H30B H Uiso 0.03570 0.33920 0.05870 1.000 0.1080 c R . .
H30C H Uiso 0.04090 0.33370 0.12220 1.000 0.1080 c R . .
H31A H Uiso 0.24080 0.49640 0.14160 1.000 0.1130 c R . .
H31B H Uiso 0.28560 0.50290 0.20330 1.000 0.1130 c R . .
H31C H Uiso 0.21490 0.53360 0.18280 1.000 0.1130 c R . .
H32A H Uiso 0.17990 0.46750 0.28830 1.000 0.0880 c R . .
H32B H Uiso 0.25820 0.45520 0.29430 1.000 0.0880 c R . .
H32C H Uiso 0.20610 0.40710 0.29200 1.000 0.0880 c R . .
H33A H Uiso 0.21740 0.34650 0.19220 1.000 0.1190 c R . .
H33B H Uiso 0.28690 0.37930 0.20540 1.000 0.1190 c R . .
H33C H Uiso 0.23750 0.37890 0.14490 1.000 0.1190 c R . .
H34A H Uiso 0.00880 0.25670 0.34770 1.000 0.0980 c R . .
H34B H Uiso 0.08150 0.23150 0.35120 1.000 0.0980 c R . .
H34C H Uiso 0.01990 0.22250 0.29790 1.000 0.0980 c R . .
H35A H Uiso 0.11530 0.26690 0.23090 1.000 0.0940 c R . .
H35B H Uiso 0.17030 0.26980 0.28890 1.000 0.0940 c R . .
H35C H Uiso 0.15550 0.32130 0.25030 1.000 0.0940 c R . .
H36A H Uiso 0.11140 0.39450 0.33990 1.000 0.0760 c R . .
H36B H Uiso 0.15440 0.34560 0.37190 1.000 0.0760 c R . .
H36C H Uiso 0.08200 0.35950 0.38070 1.000 0.0760 c 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
Co1 0.0369(6) 0.0510(7) 0.0568(7) -0.0036(6) 0.0132(5) 0.0005(5)
Co2 0.0418(7) 0.0634(9) 0.0637(8) -0.0005(7) 0.0114(6) -0.0071(6)
O1 0.0326(10) 0.0486(12) 0.0562(13) -0.0012(10) 0.0147(9) -0.0015(9)
N1 0.0369(10) 0.0637(14) 0.0801(16) -0.0128(12) 0.0170(10) 0.0033(10)
N2 0.0335(10) 0.0645(13) 0.0634(13) 0.0077(10) 0.0199(9) 0.0065(9)
N3 0.0351(10) 0.0693(15) 0.0795(16) -0.0106(12) 0.0185(10) -0.0023(10)
N4 0.0435(11) 0.0598(14) 0.0695(15) -0.0087(11) 0.0107(10) -0.0070(10)
N5 0.0479(12) 0.0604(14) 0.097(2) -0.0283(13) 0.0299(12) -0.0036(10)
N6 0.0790(17) 0.0503(13) 0.0902(19) -0.0125(13) 0.0411(15) -0.0136(12)
N7 0.0749(18) 0.0743(17) 0.0788(18) 0.0082(14) 0.0370(15) -0.0094(14)
N8 0.070(3) 0.102(5) 0.071(3) 0.023(3) 0.018(3) 0.001(3)
N9 0.0708(16) 0.0631(15) 0.0802(18) 0.0113(13) 0.0231(14) 0.0099(13)
C1 0.0334(11) 0.0587(15) 0.0669(16) 0.0029(12) 0.0183(11) 0.0024(10)
C2 0.0446(14) 0.0637(17) 0.082(2) -0.0121(14) 0.0215(13) 0.0037(12)
C3 0.0629(17) 0.0664(18) 0.0711(18) -0.0057(14) 0.0283(15) 0.0008(14)
C4 0.0474(14) 0.0661(17) 0.082(2) 0.0029(15) 0.0327(14) 0.0065(12)
C5 0.0353(12) 0.082(2) 0.0650(16) 0.0159(14) 0.0153(11) 0.0053(12)
C6 0.0414(14) 0.097(2) 0.0644(17) 0.0057(16) 0.0112(12) -0.0053(14)
C7 0.0395(14) 0.082(2) 0.087(2) -0.0149(17) 0.0140(14) -0.0056(13)
C8 0.0381(12) 0.0574(15) 0.082(2) -0.0178(14) 0.0243(12) -0.0038(11)
C9 0.0516(16) 0.0728(19) 0.076(2) -0.0089(16) 0.0006(14) 0.0013(14)
C10 0.0616(18) 0.094(3) 0.071(2) -0.0081(18) 0.0127(15) 0.0115(17)
C11 0.0634(19) 0.080(2) 0.087(2) -0.0315(19) 0.0093(17) 0.0147(16)
C12 0.083(2) 0.0587(19) 0.142(4) -0.041(2) 0.054(2) -0.0168(17)
C13 0.143(4) 0.070(2) 0.169(5) -0.038(3) 0.111(4) -0.038(3)
C14 0.141(4) 0.0564(19) 0.108(3) -0.0102(19) 0.065(3) -0.020(2)
C15 0.0704(19) 0.0719(19) 0.0546(15) 0.0020(14) 0.0122(14) -0.0291(16)
C16 0.095(3) 0.148(4) 0.077(2) -0.017(2) 0.051(2) -0.055(3)
C17 0.077(4) 0.108(5) 0.102(5) -0.001(4) 0.038(4) -0.004(4)
C18 0.100(6) 0.163(9) 0.081(4) 0.006(5) 0.034(4) -0.002(6)
C19 0.142(8) 0.060(5) 0.079(5) 0.013(4) 0.011(5) 0.012(5)
C20 0.099(6) 0.078(5) 0.116(7) 0.019(5) -0.012(5) 0.018(5)
C21 0.063(2) 0.109(3) 0.115(3) 0.043(3) 0.000(2) -0.003(2)
Li1 0.0369(6) 0.0510(7) 0.0568(7) -0.0036(6) 0.0132(5) 0.0005(5)
Li2 0.0418(7) 0.0634(9) 0.0637(8) -0.0005(7) 0.0114(6) -0.0071(6)
Li3 0.0215(13) 0.0214(13) 0.0422(16) -0.0049(11) 0.0191(12) -0.0014(10)
Li4 0.0131(12) 0.0376(16) 0.0368(16) 0.0025(13) 0.0087(11) -0.0006(11)
C18A 0.139(9) 0.041(4) 0.098(6) -0.011(4) 0.080(7) -0.029(5)
C19A 0.097(7) 0.071(7) 0.073(7) 0.014(6) 0.022(5) 0.023(7)
C20A 0.065(6) 0.062(6) 0.090(8) 0.019(5) 0.009(5) 0.009(4)
C17A 0.098(7) 0.104(8) 0.123(8) -0.042(7) 0.084(7) -0.042(6)
N8A 0.102(6) 0.031(3) 0.051(4) -0.009(2) 0.023(3) -0.005(3)
Cl1 0.0588(5) 0.0351(4) 0.0711(5) 0.0000 0.0413(4) 0.0000
Si1 0.0452(4) 0.0520(4) 0.0814(5) 0.0135(4) 0.0188(3) -0.0091(3)
Si2 0.0427(4) 0.0676(5) 0.0831(6) 0.0300(4) 0.0188(4) -0.0006(3)
Si3 0.0422(3) 0.0763(5) 0.0420(3) 0.0075(3) 0.0142(3) 0.0108(3)
Si4 0.0345(3) 0.0748(5) 0.0503(4) 0.0081(3) 0.0151(3) 0.0078(3)
Si5 0.0429(3) 0.0356(3) 0.0467(3) 0.0006(2) 0.0000(3) -0.0007(2)
N10 0.0396(10) 0.0472(11) 0.0738(14) 0.0139(10) 0.0198(10) -0.0020(8)
N11 0.0353(9) 0.0568(12) 0.0444(10) 0.0084(8) 0.0152(8) 0.0067(8)
N12 0.0408(13) 0.0345(12) 0.0418(13) 0.0000 0.0053(10) 0.0000
C22 0.0495(14) 0.0646(17) 0.079(2) 0.0084(15) 0.0180(13) -0.0033(13)
C23 0.082(2) 0.0497(16) 0.110(3) 0.0034(17) 0.024(2) -0.0100(15)
C24 0.0536(17) 0.088(2) 0.101(3) 0.027(2) 0.0209(17) -0.0230(16)
C25 0.0543(17) 0.125(3) 0.074(2) 0.030(2) 0.0222(15) -0.0097(19)
C26 0.068(2) 0.083(3) 0.161(4) 0.066(3) 0.032(2) 0.0055(18)
C27 0.0424(14) 0.091(2) 0.080(2) 0.0177(17) 0.0155(14) -0.0041(14)
C28 0.0442(14) 0.090(2) 0.0567(15) 0.0212(15) 0.0094(12) 0.0116(14)
C29 0.0605(18) 0.135(3) 0.0523(16) 0.0222(18) 0.0263(14) 0.0176(19)
C30 0.0648(18) 0.085(2) 0.0644(18) -0.0149(16) 0.0147(14) 0.0094(16)
C31 0.0498(16) 0.109(3) 0.0713(19) 0.0159(18) 0.0246(14) -0.0126(16)
C32 0.0481(14) 0.0736(18) 0.0514(14) 0.0043(13) 0.0096(11) -0.0031(12)
C33 0.0557(17) 0.118(3) 0.0696(19) 0.0064(19) 0.0239(15) 0.0359(18)
C34 0.0619(17) 0.0460(14) 0.0712(18) 0.0151(13) -0.0102(14) -0.0069(12)
C35 0.0516(14) 0.0558(15) 0.0731(18) -0.0178(14) 0.0043(13) 0.0095(12)
C36 0.0514(13) 0.0488(13) 0.0454(12) -0.0023(10) 0.0031(10) -0.0078(10)
Li5 0.040(3) 0.047(3) 0.067(4) 0.0000 0.019(3) 0.0000
Li6 0.042(2) 0.046(2) 0.060(2) 0.0047(18) 0.0196(18) 0.0043(16)
Li7 0.0427(19) 0.0419(19) 0.0430(19) 0.0021(15) 0.0156(15) 0.0026(15)
#===============================================================================
# 10. MOLECULAR GEOMETRY
_geom_special_details
;
Bond distances, angles etc. have been calculated using the
rounded fractional coordinates. All su's 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
Co1 O1 2.0370(14) . . yes
Co1 N1 2.048(3) . . yes
Co1 N4 1.991(3) . . yes
Co1 N7 2.064(3) . . yes
Co2 O1 2.0300(15) . . yes
Co2 N3 2.036(3) . . yes
Co2 N7 2.092(3) . . yes
Co2 N6 2.019(3) . 3_755 yes
Cl1 Li7 2.445(4) . 2_555 yes
Cl1 Li6 2.448(4) . . yes
Cl1 Li7 2.445(4) . . yes
Cl1 Li5 2.458(7) . . yes
Cl1 Li6 2.448(4) . 2_555 yes
Si1 C22 1.876(3) . . yes
Si1 C23 1.881(4) . . yes
Si1 N10 1.714(2) . . yes
Si1 C24 1.894(4) . . yes
Si2 N10 1.708(3) . . yes
Si2 C25 1.880(4) . . yes
Si2 C27 1.883(3) . . yes
Si2 C26 1.879(4) . . yes
Si3 C28 1.882(3) . . yes
Si3 N11 1.712(2) . . yes
Si3 C29 1.882(4) . . yes
Si3 C30 1.868(4) . . yes
Si4 N11 1.708(2) . . yes
Si4 C33 1.881(4) . . yes
Si4 C32 1.881(3) . . yes
Si4 C31 1.890(4) . . yes
Si5 C34 1.886(3) . . yes
Si5 C36 1.882(3) . . yes
Si5 C35 1.878(3) . . yes
Si5 N12 1.7077(14) . . yes
O1 Li4 2.001(3) . . yes
O1 Li3 2.064(3) . 3_755 yes
O1 Li4 2.001(3) . 3_755 yes
O1 Li2 2.0300(15) . . yes
O1 Li3 2.064(3) . . yes
O1 Li1 2.0370(14) . . yes
N1 C1 1.349(4) . . yes
N1 C2 1.461(4) . . yes
N1 Li1 2.048(3) . . yes
N1 Li4 2.062(4) . . yes
N2 C4 1.454(4) . . yes
N2 C5 1.465(4) . . yes
N2 C1 1.367(3) . . yes
N3 C1 1.348(4) . . yes
N3 Li2 2.036(3) . . yes
N3 Li3 2.062(4) . 3_755 yes
N3 C7 1.474(4) . . yes
N4 Li1 1.991(3) . . yes
N4 Li3 2.054(4) . . yes
N4 C8 1.350(4) . . yes
N4 C9 1.465(4) . . yes
N5 C8 1.367(4) . . yes
N5 C11 1.458(5) . . yes
N5 C12 1.452(5) . . yes
N6 C8 1.349(5) . . yes
N6 Li4 2.081(4) . . yes
N6 C14 1.462(5) . . yes
N7 C15 1.334(5) . . yes
N7 C16 1.455(5) . . yes
N7 Li2 2.092(3) . . yes
N7 Li1 2.064(3) . . yes
N8 C15 1.337(6) . . yes
N8 C18 1.503(11) . . yes
N8A C19A 1.305(16) . . yes
N8A C15 1.464(7) . . yes
N8A C18A 1.491(15) . . yes
N9 Li4 2.063(4) . 3_755 yes
N9 C21 1.442(4) . . yes
N9 Li3 2.034(4) . . yes
N9 C15 1.321(5) . . yes
N10 Li5 2.062(3) . . yes
N10 Li6 2.064(5) . . yes
N11 Li7 2.051(5) . . yes
N11 Li6 2.055(5) . . yes
N12 Li7 2.058(4) . 2_555 yes
N12 Li7 2.058(4) . . yes
C2 C3 1.512(5) . . no
C3 C4 1.514(5) . . no
C5 C6 1.493(5) . . no
C6 C7 1.505(5) . . no
C9 C10 1.517(5) . . no
C10 C11 1.505(5) . . no
C12 C13 1.480(7) . . no
C13 C14 1.493(8) . . no
C16 C17A 1.563(13) . . no
C16 C17 1.417(5) . . no
C17 C18 1.477(11) . . no
C17A C18A 1.442(16) . . no
C19 C20 1.449(16) . . no
C19A C20A 1.528(18) . . no
C20 C21 1.452(10) . . no
C20A C21 1.491(11) . . no
C2 H2A 0.9700 . . no
C2 H2B 0.9700 . . no
C3 H3A 0.9700 . . no
C3 H3B 0.9700 . . no
C4 H4B 0.9700 . . no
C4 H4A 0.9700 . . no
C5 H5A 0.9700 . . no
C5 H5B 0.9700 . . no
C6 H6B 0.9700 . . no
C6 H6A 0.9700 . . no
C7 H7A 0.9700 . . no
C7 H7B 0.9700 . . no
C9 H9B 0.9700 . . no
C9 H9A 0.9700 . . no
C10 H10B 0.9700 . . no
C10 H10A 0.9700 . . no
C11 H11A 0.9700 . . no
C11 H11B 0.9700 . . no
C12 H12A 0.9700 . . no
C12 H12B 0.9700 . . no
C13 H13A 0.9700 . . no
C13 H13B 0.9700 . . no
C14 H14A 0.9700 . . no
C14 H14B 0.9700 . . no
C16 H16A 0.9700 . . no
C16 H16B 0.9700 . . no
C16 H16C 0.9700 . . no
C16 H16D 0.9700 . . no
C17 H17A 0.9700 . . no
C17 H17B 0.9700 . . no
C17A H17C 0.9700 . . no
C17A H17D 0.9700 . . no
C18 H18A 0.9700 . . no
C18 H18B 0.9700 . . no
C18A H18C 0.9700 . . no
C18A H18D 0.9700 . . no
C19 H19A 0.9700 . . no
C19 H19B 0.9700 . . no
C19A H19D 0.9700 . . no
C19A H19C 0.9700 . . no
C20 H20B 0.9700 . . no
C20 H20A 0.9700 . . no
C20A H20C 0.9700 . . no
C20A H20D 0.9700 . . no
C21 H21A 0.9700 . . no
C21 H21C 0.9700 . . no
C21 H21D 0.9700 . . no
C21 H21B 0.9700 . . no
C22 H22A 0.9600 . . no
C22 H22B 0.9600 . . no
C22 H22C 0.9600 . . no
C23 H23A 0.9600 . . no
C23 H23B 0.9600 . . no
C23 H23C 0.9600 . . no
C24 H24A 0.9600 . . no
C24 H24B 0.9600 . . no
C24 H24C 0.9600 . . no
C25 H25A 0.9600 . . no
C25 H25B 0.9600 . . no
C25 H25C 0.9600 . . no
C26 H26A 0.9600 . . no
C26 H26B 0.9600 . . no
C26 H26C 0.9600 . . no
C27 H27A 0.9600 . . no
C27 H27B 0.9600 . . no
C27 H27C 0.9600 . . no
C28 H28A 0.9600 . . no
C28 H28B 0.9600 . . no
C28 H28C 0.9600 . . no
C29 H29A 0.9600 . . no
C29 H29B 0.9600 . . no
C29 H29C 0.9600 . . no
C30 H30A 0.9600 . . no
C30 H30B 0.9600 . . no
C30 H30C 0.9600 . . no
C31 H31A 0.9600 . . no
C31 H31B 0.9600 . . no
C31 H31C 0.9600 . . no
C32 H32A 0.9600 . . no
C32 H32B 0.9600 . . no
C32 H32C 0.9600 . . no
C33 H33A 0.9600 . . no
C33 H33B 0.9600 . . no
C33 H33C 0.9600 . . no
C34 H34A 0.9600 . . no
C34 H34B 0.9600 . . no
C34 H34C 0.9600 . . no
C35 H35A 0.9600 . . no
C35 H35B 0.9600 . . no
C35 H35C 0.9600 . . no
C36 H36A 0.9600 . . no
C36 H36B 0.9600 . . no
C36 H36C 0.9600 . . 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
O1 Co1 N1 97.06(9) . . . yes
O1 Co1 N4 100.04(9) . . . yes
O1 Co1 N7 96.69(11) . . . yes
N1 Co1 N4 119.17(12) . . . yes
N1 Co1 N7 115.48(13) . . . yes
N4 Co1 N7 119.69(13) . . . yes
O1 Co2 N3 98.57(9) . . . yes
O1 Co2 N7 96.03(11) . . . yes
O1 Co2 N6 99.11(11) . . 3_755 yes
N3 Co2 N7 114.66(13) . . . yes
N3 Co2 N6 121.34(14) . . 3_755 yes
N6 Co2 N7 118.37(14) 3_755 . . yes
Li6 Cl1 Li7 71.96(14) . . . yes
Li6 Cl1 Li6 144.25(14) . . 2_555 yes
Li6 Cl1 Li7 143.78(14) . . 2_555 yes
Li5 Cl1 Li6 72.12(10) . . . yes
Li5 Cl1 Li7 144.08(9) . . . yes
Li5 Cl1 Li6 72.12(10) . . 2_555 yes
Li5 Cl1 Li7 144.08(9) . . 2_555 yes
Li6 Cl1 Li7 143.78(14) 2_555 . . yes
Li7 Cl1 Li7 71.85(13) . . 2_555 yes
Li6 Cl1 Li7 71.96(14) 2_555 . 2_555 yes
C22 Si1 C23 107.12(16) . . . yes
C22 Si1 C24 105.68(15) . . . yes
C23 Si1 C24 105.00(17) . . . yes
N10 Si1 C22 110.95(12) . . . yes
N10 Si1 C23 112.02(15) . . . yes
N10 Si1 C24 115.49(15) . . . yes
C26 Si2 C27 106.05(18) . . . yes
N10 Si2 C27 108.33(14) . . . yes
N10 Si2 C25 112.87(15) . . . yes
N10 Si2 C26 116.94(17) . . . yes
C25 Si2 C26 104.0(2) . . . yes
C25 Si2 C27 108.22(17) . . . yes
N11 Si3 C28 109.89(13) . . . yes
N11 Si3 C30 112.34(13) . . . yes
C28 Si3 C29 106.22(16) . . . yes
N11 Si3 C29 115.32(14) . . . yes
C29 Si3 C30 105.43(18) . . . yes
C28 Si3 C30 107.14(16) . . . yes
N11 Si4 C33 115.92(14) . . . yes
N11 Si4 C32 109.07(12) . . . yes
N11 Si4 C31 112.43(14) . . . yes
C31 Si4 C32 106.93(15) . . . yes
C31 Si4 C33 105.36(17) . . . yes
C32 Si4 C33 106.62(15) . . . yes
N12 Si5 C35 112.61(10) . . . yes
N12 Si5 C36 109.04(11) . . . yes
C34 Si5 C35 105.05(14) . . . yes
N12 Si5 C34 115.81(12) . . . yes
C34 Si5 C36 107.32(13) . . . yes
C35 Si5 C36 106.48(13) . . . yes
Co1 O1 Li4 71.54(10) . . . yes
Co1 O1 Co2 73.76(6) . . . yes
Co1 O1 Li3 69.36(10) . . . yes
Co2 O1 Li4 70.10(9) . . 3_755 yes
Li1 O1 Li2 73.76(6) . . . yes
Li1 O1 Li3 69.36(10) . . . yes
Li1 O1 Li4 71.54(10) . . . yes
Li1 O1 Li3 110.65(10) . . 3_755 yes
Li1 O1 Li4 108.46(10) . . 3_755 yes
Co1 O1 Co1 180.00 . . 3_755 yes
Co1 O1 Co2 106.24(6) . . 3_755 yes
Co1 O1 Li3 110.65(10) . . 3_755 yes
Co1 O1 Li4 108.46(10) . . 3_755 yes
Co2 O1 Li3 110.88(9) . . . yes
Co2 O1 Li4 109.90(9) . . . yes
Co1 O1 Co2 106.24(6) 3_755 . . yes
Co2 O1 Co2 180.00 . . 3_755 yes
Co2 O1 Li3 69.12(9) . . 3_755 yes
Co2 O1 Li3 69.12(9) 3_755 . . yes
Li3 O1 Li3 180.00 . . 3_755 yes
Li3 O1 Li4 69.40(12) . . 3_755 yes
Co1 O1 Li4 108.46(10) 3_755 . . yes
Co2 O1 Li4 70.10(9) 3_755 . . yes
Li3 O1 Li4 69.40(12) 3_755 . . yes
Li4 O1 Li4 180.00 . . 3_755 yes
Co1 O1 Co2 73.76(6) 3_755 . 3_755 yes
Co1 O1 Li3 69.36(10) 3_755 . 3_755 yes
Co1 O1 Li4 71.54(10) 3_755 . 3_755 yes
Co2 O1 Li3 110.88(9) 3_755 . 3_755 yes
Co2 O1 Li4 109.90(9) 3_755 . 3_755 yes
Li3 O1 Li4 110.60(12) 3_755 . 3_755 yes
Li2 O1 Li4 70.10(9) . . 3_755 yes
Li3 O1 Li4 110.60(12) . . . yes
Co1 O1 Li3 110.65(10) 3_755 . . yes
Li2 O1 Li4 109.90(9) . . . yes
Li2 O1 Li3 69.12(9) . . 3_755 yes
Li2 O1 Li3 110.88(9) . . . yes
C1 N1 C2 116.3(2) . . . yes
C1 N1 Li1 117.74(19) . . . yes
Li1 N1 Li4 70.11(12) . . . yes
Co1 N1 C2 118.6(2) . . . yes
Co1 N1 Li4 70.11(12) . . . yes
C2 N1 Li4 111.7(2) . . . yes
C1 N1 Li4 113.4(2) . . . yes
C2 N1 Li1 118.6(2) . . . yes
Co1 N1 C1 117.74(19) . . . yes
C4 N2 C5 113.5(2) . . . yes
C1 N2 C4 123.5(2) . . . yes
C1 N2 C5 122.9(2) . . . yes
Li2 N3 Li3 69.05(12) . . 3_755 yes
C7 N3 Li3 118.4(2) . . 3_755 yes
C7 N3 Li2 113.1(2) . . . yes
Co2 N3 C1 117.9(2) . . . yes
Co2 N3 C7 113.1(2) . . . yes
Co2 N3 Li3 69.05(12) . . 3_755 yes
C1 N3 C7 115.9(2) . . . yes
C1 N3 Li2 117.9(2) . . . yes
C1 N3 Li3 114.4(2) . . 3_755 yes
Co1 N4 Li3 70.46(13) . . . yes
C8 N4 C9 116.4(3) . . . yes
C8 N4 Li1 113.5(2) . . . yes
C8 N4 Li3 117.5(2) . . . yes
C9 N4 Li1 118.1(2) . . . yes
C9 N4 Li3 113.0(2) . . . yes
Li1 N4 Li3 70.46(13) . . . yes
Co1 N4 C9 118.1(2) . . . yes
Co1 N4 C8 113.5(2) . . . yes
C8 N5 C11 123.2(3) . . . yes
C11 N5 C12 114.2(3) . . . yes
C8 N5 C12 122.7(3) . . . yes
C8 N6 C14 115.6(3) . . . yes
C8 N6 Li4 115.3(2) . . . yes
C14 N6 Li4 109.8(3) . . . yes
Co2 N6 C14 121.6(3) 3_755 . . yes
Co2 N6 C8 116.5(2) 3_755 . . yes
Co2 N6 Li4 68.72(13) 3_755 . . yes
Co1 N7 C16 117.3(3) . . . yes
Co2 N7 C15 117.1(2) . . . yes
Co1 N7 C15 111.2(2) . . . yes
C15 N7 C16 115.2(3) . . . yes
C15 N7 Li1 111.2(2) . . . yes
Co2 N7 C16 117.0(2) . . . yes
Co1 N7 Co2 71.93(11) . . . yes
C16 N7 Li2 117.0(2) . . . yes
C15 N7 Li2 117.1(2) . . . yes
C16 N7 Li1 117.3(3) . . . yes
Li1 N7 Li2 71.93(11) . . . yes
C15 N8 C18 127.6(6) . . . yes
C15 N8A C19A 115.5(8) . . . yes
C18A N8A C19A 119.3(9) . . . yes
C15 N8A C18A 115.2(7) . . . yes
C21 N9 Li4 116.1(2) . . 3_755 yes
Li3 N9 Li4 68.80(16) . . 3_755 yes
C15 N9 C21 120.5(3) . . . yes
C21 N9 Li3 110.7(2) . . . yes
C15 N9 Li4 114.9(3) . . 3_755 yes
C15 N9 Li3 114.8(3) . . . yes
Si2 N10 Li6 103.20(17) . . . yes
Li5 N10 Li6 88.8(3) . . . yes
Si2 N10 Li5 111.31(13) . . . yes
Si1 N10 Li5 110.98(16) . . . yes
Si1 N10 Li6 118.10(17) . . . yes
Si1 N10 Si2 120.05(14) . . . yes
Si3 N11 Si4 120.14(12) . . . yes
Si3 N11 Li6 117.47(17) . . . yes
Li6 N11 Li7 88.86(18) . . . yes
Si4 N11 Li6 104.21(16) . . . yes
Si4 N11 Li7 116.70(15) . . . yes
Si3 N11 Li7 105.60(15) . . . yes
Si5 N12 Li7 105.89(12) . . . yes
Si5 N12 Si5 121.64(15) . . 2_555 yes
Li7 N12 Li7 88.40(18) . . 2_555 yes
Si5 N12 Li7 105.89(12) 2_555 . 2_555 yes
Si5 N12 Li7 115.17(12) . . 2_555 yes
Si5 N12 Li7 115.17(12) 2_555 . . yes
N1 C1 N3 118.0(2) . . . yes
N2 C1 N3 120.8(2) . . . yes
N1 C1 N2 121.2(2) . . . yes
N1 C2 C3 111.3(3) . . . yes
C2 C3 C4 107.1(3) . . . no
N2 C4 C3 111.6(2) . . . yes
N2 C5 C6 112.0(2) . . . yes
C5 C6 C7 108.1(3) . . . no
N3 C7 C6 110.0(3) . . . yes
N5 C8 N6 121.5(3) . . . yes
N4 C8 N5 121.2(3) . . . yes
N4 C8 N6 117.3(3) . . . yes
N4 C9 C10 110.3(3) . . . yes
C9 C10 C11 107.8(3) . . . no
N5 C11 C10 112.1(3) . . . yes
N5 C12 C13 112.1(3) . . . yes
C12 C13 C14 108.9(4) . . . no
N6 C14 C13 111.1(4) . . . yes
N7 C15 N8 112.7(4) . . . yes
N7 C15 N9 119.7(3) . . . yes
N8A C15 N9 111.2(5) . . . yes
N7 C15 N8A 126.5(5) . . . yes
N8 C15 N9 126.0(4) . . . yes
N7 C16 C17 113.1(3) . . . yes
N7 C16 C17A 106.3(5) . . . yes
C16 C17 C18 100.8(4) . . . no
C16 C17A C18A 114.1(9) . . . no
N8 C18 C17 111.7(6) . . . yes
N8A C18A C17A 114.6(8) . . . yes
N8A C19A C20A 86.3(9) . . . yes
C19 C20 C21 112.7(8) . . . no
C19A C20A C21 112.5(8) . . . no
N9 C21 C20 121.1(5) . . . yes
N9 C21 C20A 108.2(5) . . . yes
C3 C2 H2A 109.00 . . . no
N1 C2 H2B 109.00 . . . no
N1 C2 H2A 109.00 . . . no
C3 C2 H2B 109.00 . . . no
H2A C2 H2B 108.00 . . . no
C4 C3 H3B 110.00 . . . no
C4 C3 H3A 110.00 . . . no
H3A C3 H3B 108.00 . . . no
C2 C3 H3A 110.00 . . . no
C2 C3 H3B 110.00 . . . no
C3 C4 H4B 109.00 . . . no
N2 C4 H4A 109.00 . . . no
H4A C4 H4B 108.00 . . . no
C3 C4 H4A 109.00 . . . no
N2 C4 H4B 109.00 . . . no
C6 C5 H5B 109.00 . . . no
C6 C5 H5A 109.00 . . . no
N2 C5 H5A 109.00 . . . no
H5A C5 H5B 108.00 . . . no
N2 C5 H5B 109.00 . . . no
C7 C6 H6B 110.00 . . . no
C7 C6 H6A 110.00 . . . no
H6A C6 H6B 108.00 . . . no
C5 C6 H6A 110.00 . . . no
C5 C6 H6B 110.00 . . . no
C6 C7 H7B 110.00 . . . no
C6 C7 H7A 110.00 . . . no
N3 C7 H7A 110.00 . . . no
H7A C7 H7B 108.00 . . . no
N3 C7 H7B 110.00 . . . no
C10 C9 H9B 110.00 . . . no
H9A C9 H9B 108.00 . . . no
C10 C9 H9A 110.00 . . . no
N4 C9 H9A 110.00 . . . no
N4 C9 H9B 110.00 . . . no
H10A C10 H10B 109.00 . . . no
C9 C10 H10A 110.00 . . . no
C11 C10 H10B 110.00 . . . no
C9 C10 H10B 110.00 . . . no
C11 C10 H10A 110.00 . . . no
N5 C11 H11A 109.00 . . . no
H11A C11 H11B 108.00 . . . no
C10 C11 H11A 109.00 . . . no
N5 C11 H11B 109.00 . . . no
C10 C11 H11B 109.00 . . . no
C13 C12 H12B 109.00 . . . no
C13 C12 H12A 109.00 . . . no
H12A C12 H12B 108.00 . . . no
N5 C12 H12B 109.00 . . . no
N5 C12 H12A 109.00 . . . no
C14 C13 H13A 110.00 . . . no
C14 C13 H13B 110.00 . . . no
C12 C13 H13B 110.00 . . . no
C12 C13 H13A 110.00 . . . no
H13A C13 H13B 108.00 . . . no
C13 C14 H14A 109.00 . . . no
N6 C14 H14A 109.00 . . . no
N6 C14 H14B 109.00 . . . no
C13 C14 H14B 109.00 . . . no
H14A C14 H14B 108.00 . . . no
C17 C16 H16B 109.00 . . . no
N7 C16 H16D 111.00 . . . no
H16A C16 H16B 108.00 . . . no
C17 C16 H16A 109.00 . . . no
C17A C16 H16C 110.00 . . . no
N7 C16 H16C 111.00 . . . no
H16C C16 H16D 109.00 . . . no
N7 C16 H16B 109.00 . . . no
C17A C16 H16D 111.00 . . . no
N7 C16 H16A 109.00 . . . no
C18 C17 H17A 112.00 . . . no
C16 C17 H17B 112.00 . . . no
C18 C17 H17B 111.00 . . . no
H17A C17 H17B 109.00 . . . no
C16 C17 H17A 112.00 . . . no
H17C C17A H17D 108.00 . . . no
C16 C17A H17D 109.00 . . . no
C16 C17A H17C 109.00 . . . no
C18A C17A H17C 109.00 . . . no
C18A C17A H17D 109.00 . . . no
H18A C18 H18B 108.00 . . . no
C17 C18 H18A 109.00 . . . no
C17 C18 H18B 109.00 . . . no
N8 C18 H18B 109.00 . . . no
N8 C18 H18A 109.00 . . . no
N8A C18A H18D 109.00 . . . no
N8A C18A H18C 109.00 . . . no
C17A C18A H18C 109.00 . . . no
C17A C18A H18D 109.00 . . . no
H18C C18A H18D 108.00 . . . no
C20 C19 H19A 111.00 . . . no
H19A C19 H19B 109.00 . . . no
C20 C19 H19B 111.00 . . . no
H19C C19A H19D 112.00 . . . no
N8A C19A H19C 114.00 . . . no
C20A C19A H19D 114.00 . . . no
C20A C19A H19C 114.00 . . . no
N8A C19A H19D 114.00 . . . no
C19 C20 H20A 109.00 . . . no
H20A C20 H20B 108.00 . . . no
C21 C20 H20B 109.00 . . . no
C19 C20 H20B 109.00 . . . no
C21 C20 H20A 109.00 . . . no
C21 C20A H20D 109.00 . . . no
C19A C20A H20C 109.00 . . . no
C19A C20A H20D 109.00 . . . no
H20C C20A H20D 108.00 . . . no
C21 C20A H20C 109.00 . . . no
C20A C21 H21D 110.00 . . . no
H21C C21 H21D 108.00 . . . no
N9 C21 H21A 107.00 . . . no
N9 C21 H21B 107.00 . . . no
N9 C21 H21C 110.00 . . . no
N9 C21 H21D 110.00 . . . no
C20 C21 H21A 107.00 . . . no
C20 C21 H21B 107.00 . . . no
H21A C21 H21B 107.00 . . . no
C20A C21 H21C 110.00 . . . no
H22A C22 H22C 110.00 . . . no
Si1 C22 H22A 109.00 . . . no
Si1 C22 H22B 109.00 . . . no
H22B C22 H22C 109.00 . . . no
H22A C22 H22B 110.00 . . . no
Si1 C22 H22C 109.00 . . . no
Si1 C23 H23C 110.00 . . . no
H23A C23 H23B 109.00 . . . no
H23A C23 H23C 109.00 . . . no
H23B C23 H23C 110.00 . . . no
Si1 C23 H23B 109.00 . . . no
Si1 C23 H23A 109.00 . . . no
Si1 C24 H24C 109.00 . . . no
H24A C24 H24B 109.00 . . . no
Si1 C24 H24B 109.00 . . . no
Si1 C24 H24A 109.00 . . . no
H24A C24 H24C 109.00 . . . no
H24B C24 H24C 110.00 . . . no
H25A C25 H25C 109.00 . . . no
H25B C25 H25C 109.00 . . . no
Si2 C25 H25C 110.00 . . . no
H25A C25 H25B 109.00 . . . no
Si2 C25 H25B 109.00 . . . no
Si2 C25 H25A 109.00 . . . no
Si2 C26 H26B 109.00 . . . no
H26B C26 H26C 110.00 . . . no
Si2 C26 H26A 109.00 . . . no
H26A C26 H26B 110.00 . . . no
Si2 C26 H26C 109.00 . . . no
H26A C26 H26C 109.00 . . . no
Si2 C27 H27A 109.00 . . . no
H27A C27 H27C 109.00 . . . no
Si2 C27 H27B 109.00 . . . no
Si2 C27 H27C 109.00 . . . no
H27B C27 H27C 110.00 . . . no
H27A C27 H27B 110.00 . . . no
Si3 C28 H28C 109.00 . . . no
Si3 C28 H28B 110.00 . . . no
H28B C28 H28C 109.00 . . . no
Si3 C28 H28A 109.00 . . . no
H28A C28 H28C 110.00 . . . no
H28A C28 H28B 109.00 . . . no
Si3 C29 H29B 109.00 . . . no
H29A C29 H29B 110.00 . . . no
Si3 C29 H29A 109.00 . . . no
Si3 C29 H29C 109.00 . . . no
H29B C29 H29C 109.00 . . . no
H29A C29 H29C 109.00 . . . no
Si3 C30 H30A 109.00 . . . no
Si3 C30 H30B 109.00 . . . no
Si3 C30 H30C 110.00 . . . no
H30A C30 H30B 109.00 . . . no
H30B C30 H30C 109.00 . . . no
H30A C30 H30C 109.00 . . . no
H31B C31 H31C 109.00 . . . no
H31A C31 H31B 110.00 . . . no
H31A C31 H31C 109.00 . . . no
Si4 C31 H31C 110.00 . . . no
Si4 C31 H31A 109.00 . . . no
Si4 C31 H31B 109.00 . . . no
Si4 C32 H32B 109.00 . . . no
Si4 C32 H32C 109.00 . . . no
Si4 C32 H32A 110.00 . . . no
H32B C32 H32C 109.00 . . . no
H32A C32 H32B 109.00 . . . no
H32A C32 H32C 109.00 . . . no
Si4 C33 H33B 110.00 . . . no
H33A C33 H33C 109.00 . . . no
H33B C33 H33C 109.00 . . . no
H33A C33 H33B 110.00 . . . no
Si4 C33 H33A 109.00 . . . no
Si4 C33 H33C 109.00 . . . no
Si5 C34 H34A 110.00 . . . no
H34A C34 H34B 109.00 . . . no
Si5 C34 H34B 110.00 . . . no
Si5 C34 H34C 110.00 . . . no
H34B C34 H34C 109.00 . . . no
H34A C34 H34C 109.00 . . . no
H35B C35 H35C 109.00 . . . no
Si5 C35 H35A 109.00 . . . no
Si5 C35 H35C 109.00 . . . no
H35A C35 H35B 109.00 . . . no
Si5 C35 H35B 110.00 . . . no
H35A C35 H35C 109.00 . . . no
H36A C36 H36B 109.00 . . . no
H36A C36 H36C 109.00 . . . no
Si5 C36 H36B 110.00 . . . no
Si5 C36 H36C 110.00 . . . no
H36B C36 H36C 109.00 . . . no
Si5 C36 H36A 109.00 . . . no
O1 Li1 N1 97.06(9) . . . yes
N1 Li1 N7 115.48(13) . . . yes
N4 Li1 N7 119.69(13) . . . yes
N1 Li1 N4 119.17(12) . . . yes
O1 Li1 N7 96.69(11) . . . yes
O1 Li1 N4 100.04(9) . . . yes
O1 Li2 N7 96.03(11) . . . yes
O1 Li2 N3 98.57(9) . . . yes
N3 Li2 N7 114.66(13) . . . yes
N3 Li2 N6 121.34(14) . . 3_755 yes
N6 Li2 N7 118.37(14) 3_755 . . yes
O1 Li2 N6 99.11(11) . . 3_755 yes
N3 Li3 N4 119.21(17) 3_755 . . yes
N3 Li3 N9 120.02(18) 3_755 . . yes
N4 Li3 N9 116.10(19) . . . yes
O1 Li3 N4 97.08(14) . . . yes
O1 Li3 N9 97.97(16) . . . yes
O1 Li3 N3 96.64(16) . . 3_755 yes
N1 Li4 N6 114.17(18) . . . yes
N1 Li4 N9 120.04(18) . . 3_755 yes
N6 Li4 N9 119.63(19) . . 3_755 yes
O1 Li4 N1 97.76(15) . . . yes
O1 Li4 N6 98.03(15) . . . yes
O1 Li4 N9 99.08(16) . . 3_755 yes
N10 Li5 N10 161.2(4) . . 2_555 yes
Cl1 Li5 N10 99.4(2) . . . yes
Cl1 Li5 N10 99.4(2) . . 2_555 yes
N10 Li6 N11 160.8(3) . . . yes
Cl1 Li6 N11 99.47(18) . . . yes
Cl1 Li6 N10 99.66(18) . . . yes
Cl1 Li7 N12 99.88(17) . . . yes
N11 Li7 N12 160.4(2) . . . yes
Cl1 Li7 N11 99.70(17) . . . 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
Li7 Cl1 Li6 N11 2.6(3) 2_555 . . . no
Li7 Cl1 Li5 N10 -1.34(17) . . . . no
Li6 Cl1 Li5 N10 -179.96(12) 2_555 . . . no
Li7 Cl1 Li5 N10 178.66(17) 2_555 . . . no
Li6 Cl1 Li5 N10 -179.96(13) . . . 2_555 no
Li7 Cl1 Li5 N10 178.66(17) . . . 2_555 no
Li6 Cl1 Li7 N12 -2.2(3) 2_555 . . . no
Li5 Cl1 Li7 N11 1.1(3) . . . . no
Li6 Cl1 Li7 N11 -0.33(16) . . . . no
Li6 Cl1 Li7 N11 178.83(19) 2_555 . . . no
Li7 Cl1 Li7 N11 -178.94(19) 2_555 . . . no
Li5 Cl1 Li7 N12 180.00(3) . . . . no
Li6 Cl1 Li7 N12 178.62(19) . . . . no
Li7 Cl1 Li6 N10 -178.67(17) 2_555 . . . no
Li7 Cl1 Li7 N12 0.00(14) 2_555 . . . no
Li6 Cl1 Li5 N10 0.04(13) . . . . no
Li6 Cl1 Li6 N11 -178.82(19) 2_555 . . . no
Li5 Cl1 Li6 N10 -0.04(13) . . . . no
Li7 Cl1 Li6 N10 179.1(2) . . . . no
Li6 Cl1 Li6 N10 0.0(3) 2_555 . . . no
Li5 Cl1 Li6 N11 -178.82(19) . . . . no
Li7 Cl1 Li6 N11 0.32(16) . . . . no
C24 Si1 N10 Si2 -37.4(2) . . . . no
C24 Si1 N10 Li6 90.1(2) . . . . no
C23 Si1 N10 Si2 82.8(2) . . . . no
C22 Si1 N10 Li5 70.2(2) . . . . no
C22 Si1 N10 Si2 -157.60(14) . . . . no
C23 Si1 N10 Li5 -49.4(3) . . . . no
C22 Si1 N10 Li6 -30.2(2) . . . . no
C23 Si1 N10 Li6 -149.8(2) . . . . no
C24 Si1 N10 Li5 -169.6(2) . . . . no
C25 Si2 N10 Li5 -148.5(3) . . . . no
C26 Si2 N10 Li5 91.0(3) . . . . no
C27 Si2 N10 Si1 -160.75(17) . . . . no
C25 Si2 N10 Si1 79.4(2) . . . . no
C27 Si2 N10 Li6 65.3(2) . . . . no
C26 Si2 N10 Li6 -175.1(2) . . . . no
C27 Si2 N10 Li5 -28.7(3) . . . . no
C26 Si2 N10 Si1 -41.1(2) . . . . no
C25 Si2 N10 Li6 -54.6(2) . . . . no
C29 Si3 N11 Si4 -39.1(2) . . . . no
C28 Si3 N11 Si4 -159.04(16) . . . . no
C30 Si3 N11 Li7 -52.8(2) . . . . no
C29 Si3 N11 Li7 -173.6(2) . . . . no
C30 Si3 N11 Li6 -149.8(2) . . . . no
C28 Si3 N11 Li7 66.41(19) . . . . no
C28 Si3 N11 Li6 -30.6(2) . . . . no
C29 Si3 N11 Li6 89.4(2) . . . . no
C30 Si3 N11 Si4 81.79(19) . . . . no
C31 Si4 N11 Li7 -151.42(19) . . . . no
C33 Si4 N11 Li6 -176.70(19) . . . . no
C33 Si4 N11 Li7 87.3(2) . . . . no
C33 Si4 N11 Si3 -42.5(2) . . . . no
C32 Si4 N11 Li6 62.99(19) . . . . no
C31 Si4 N11 Li6 -55.4(2) . . . . no
C31 Si4 N11 Si3 78.77(19) . . . . no
C32 Si4 N11 Li7 -33.0(2) . . . . no
C32 Si4 N11 Si3 -162.80(15) . . . . no
C35 Si5 N12 Li7 -51.08(18) . . . . no
C34 Si5 N12 Li7 -172.00(16) . . . . no
C34 Si5 N12 Li7 92.16(19) . . . 2_555 no
C35 Si5 N12 Li7 -146.92(17) . . . 2_555 no
C36 Si5 N12 Si5 -159.11(9) . . . 2_555 no
C36 Si5 N12 Li7 66.88(16) . . . . no
C34 Si5 N12 Si5 -37.99(12) . . . 2_555 no
C35 Si5 N12 Si5 82.93(11) . . . 2_555 no
C36 Si5 N12 Li7 -28.95(18) . . . 2_555 no
Li4 O1 Li1 N1 -143.74(12) 3_755 . . . no
Li2 O1 Li1 N4 156.79(10) . . . . no
Li3 O1 Li1 N1 -22.27(12) 3_755 . . . no
Li2 O1 Li3 N4 -97.15(12) . . . . no
Li1 O1 Li3 N4 -34.76(11) . . . . no
Li1 O1 Li2 N7 -34.39(10) . . . . no
Li1 O1 Li4 N1 -36.03(11) . . . . no
Li2 O1 Li4 N1 28.23(15) . . . . no
Li3 O1 Li4 N1 -94.53(16) . . . . no
Li3 O1 Li4 N1 85.48(16) 3_755 . . . no
Li4 O1 Li1 N7 -26.93(14) 3_755 . . . no
Li4 O1 Li1 N7 153.07(14) . . . . no
Li3 O1 Li1 N7 94.54(13) 3_755 . . . no
Li4 O1 Li2 N3 18.87(14) . . . . no
Li2 O1 Li1 N1 -81.84(9) . . . . no
Li3 O1 Li1 N1 157.74(12) . . . . no
Li4 O1 Li1 N1 36.26(12) . . . . no
Li4 O1 Li3 N4 -154.97(17) 3_755 . . . no
Li1 O1 Li3 N9 82.95(14) . . . . no
Li1 O1 Li4 N6 79.85(14) . . . . no
Li3 O1 Li1 N4 36.36(12) . . . . no
Li4 O1 Li1 N4 -85.12(13) . . . . no
Li3 O1 Li1 N4 -143.64(12) 3_755 . . . no
Li4 O1 Li1 N4 94.88(13) 3_755 . . . no
Li2 O1 Li1 N7 34.97(11) . . . . no
Li3 O1 Li1 N7 -85.46(13) . . . . no
Li4 O1 Li3 N3 -95.59(15) . . . 3_755 no
Li1 O1 Li2 N3 81.73(10) . . . . no
Li3 O1 Li2 N3 141.45(12) . . . . no
Li3 O1 Li2 N3 -38.55(12) 3_755 . . . no
Li4 O1 Li2 N3 -161.14(14) 3_755 . . . no
Li4 O1 Li3 N4 25.04(17) . . . . no
Li3 O1 Li2 N7 25.34(14) . . . . no
Li4 O1 Li2 N7 -97.25(14) . . . . no
Li3 O1 Li2 N7 -154.66(14) 3_755 . . . no
Li2 O1 Li4 N6 144.10(12) . . . . no
Li3 O1 Li4 N6 21.35(18) . . . . no
Li3 O1 Li4 N6 -158.65(18) 3_755 . . . no
Li1 O1 Li4 N9 -158.27(16) . . . 3_755 no
Li2 O1 Li4 N9 -94.02(14) . . . 3_755 no
Li3 O1 Li4 N9 143.24(15) . . . 3_755 no
Li2 O1 Li3 N3 142.23(11) . . . 3_755 no
Li3 O1 Li2 N6 -94.71(13) . . . 3_755 no
Li4 O1 Li2 N7 82.75(14) 3_755 . . . no
Li1 O1 Li2 N6 -154.44(11) . . . 3_755 no
Li1 O1 Li3 N3 -155.39(14) . . . 3_755 no
Li4 O1 Li2 N6 142.70(13) . . . 3_755 no
Li4 O1 Li3 N9 -37.26(15) 3_755 . . . no
Li2 O1 Li3 N9 20.56(17) . . . . no
Li4 O1 Li3 N9 142.74(15) . . . . no
C1 N1 Li4 N6 -178.8(2) . . . . no
Li1 N1 Li4 O1 36.18(11) . . . . no
Li1 N1 Li4 N9 141.4(2) . . . 3_755 no
C1 N1 C2 C3 43.6(4) . . . . no
Li4 N1 Li1 O1 -35.37(11) . . . . no
C1 N1 Li1 O1 71.3(2) . . . . no
C2 N1 Li4 O1 150.0(2) . . . . no
C1 N1 Li4 O1 -76.3(2) . . . . no
Li4 N1 Li1 N7 -136.27(16) . . . . no
C1 N1 Li1 N4 177.0(2) . . . . no
C2 N1 Li1 N4 -34.1(3) . . . . no
C1 N1 Li4 N9 28.9(3) . . . 3_755 no
C2 N1 Li4 N9 -104.8(3) . . . 3_755 no
Li4 N1 C2 C3 175.9(2) . . . . no
Li1 N1 Li4 N6 -66.27(17) . . . . no
C2 N1 Li4 N6 47.5(3) . . . . no
C2 N1 C1 N2 -6.6(4) . . . . no
Li1 N1 C1 N2 143.0(2) . . . . no
C2 N1 Li1 O1 -139.8(2) . . . . no
Li1 N1 C2 C3 -105.7(3) . . . . no
C1 N1 Li1 N7 -29.6(3) . . . . no
C2 N1 Li1 N7 119.3(2) . . . . no
Li4 N1 Li1 N4 70.32(16) . . . . no
C2 N1 C1 N3 173.7(3) . . . . no
Li1 N1 C1 N3 -36.7(3) . . . . no
Li4 N1 C1 N2 -138.1(2) . . . . no
Li4 N1 C1 N3 42.3(3) . . . . no
C5 N2 C4 C3 174.3(3) . . . . no
C1 N2 C4 C3 -10.8(4) . . . . no
C5 N2 C1 N1 163.9(3) . . . . no
C5 N2 C1 N3 -16.4(4) . . . . no
C4 N2 C1 N1 -10.6(4) . . . . no
C1 N2 C5 C6 -3.8(4) . . . . no
C4 N2 C1 N3 169.1(3) . . . . no
C4 N2 C5 C6 171.2(3) . . . . no
C7 N3 C1 N2 -5.8(4) . . . . no
C1 N3 Li2 N6 -174.9(2) . . . 3_755 no
Li2 N3 C1 N2 -144.5(2) . . . . no
C7 N3 Li2 N6 45.3(3) . . . 3_755 no
Li3 N3 C1 N1 -43.0(3) 3_755 . . . no
C1 N3 Li3 N4 -176.5(2) 3_755 3_755 . . no
C7 N3 Li3 N4 41.4(3) 3_755 3_755 . . no
Li3 N3 C1 N2 137.3(2) 3_755 . . . no
C7 N3 Li3 N9 -113.4(3) 3_755 3_755 . . no
Li3 N3 C7 C6 -96.0(3) 3_755 . . . no
Li2 N3 C1 N1 35.2(3) . . . . no
Li2 N3 C7 C6 -173.8(2) . . . . no
C7 N3 Li2 O1 151.6(2) . . . . no
C1 N3 Li2 O1 -68.7(2) . . . . no
C1 N3 Li3 N9 28.7(3) 3_755 3_755 . . no
C1 N3 C7 C6 45.6(4) . . . . no
Li3 N3 Li2 N7 139.35(16) 3_755 . . . no
C7 N3 C1 N1 173.9(3) . . . . no
Li3 N3 Li2 N6 -67.59(17) 3_755 . . 3_755 no
Li3 N3 Li2 O1 38.62(12) 3_755 . . . no
C7 N3 Li2 N7 -107.7(2) . . . . no
C1 N3 Li2 N7 32.0(3) . . . . no
Li1 N4 Li3 N9 -67.09(19) . . . . no
C9 N4 Li3 N9 46.0(3) . . . . no
C9 N4 Li3 N3 -109.8(3) . . . 3_755 no
Li3 N4 C8 N5 -146.1(2) . . . . no
C8 N4 Li3 N3 30.1(3) . . . 3_755 no
Li3 N4 C8 N6 34.6(4) . . . . no
C8 N4 Li3 O1 -71.6(2) . . . . no
C8 N4 Li1 O1 76.1(2) . . . . no
C9 N4 C8 N5 -7.5(4) . . . . no
Li1 N4 C8 N5 134.5(2) . . . . no
Li1 N4 Li3 N3 137.1(2) . . . 3_755 no
Li1 N4 C8 N6 -44.8(3) . . . . no
C8 N4 Li3 N9 -174.1(2) . . . . no
Li3 N4 C9 C10 -174.7(2) . . . . no
C9 N4 C8 N6 173.2(3) . . . . no
C9 N4 Li3 O1 148.5(2) . . . . no
Li1 N4 Li3 O1 35.41(10) . . . . no
C8 N4 C9 C10 44.9(4) . . . . no
C8 N4 Li1 N7 179.8(2) . . . . no
Li3 N4 Li1 N7 67.43(17) . . . . no
C9 N4 Li1 O1 -142.6(2) . . . . no
Li3 N4 Li1 N1 -140.27(15) . . . . no
C8 N4 Li1 N1 -27.9(3) . . . . no
C9 N4 Li1 N7 -38.9(3) . . . . no
Li1 N4 C9 C10 -95.3(3) . . . . no
Li3 N4 Li1 O1 -36.28(12) . . . . no
C9 N4 Li1 N1 113.4(2) . . . . no
C12 N5 C8 N4 167.3(3) . . . . no
C12 N5 C11 C10 172.6(3) . . . . no
C11 N5 C8 N6 167.1(3) . . . . no
C11 N5 C8 N4 -12.2(4) . . . . no
C8 N5 C12 C13 -7.0(5) . . . . no
C11 N5 C12 C13 172.6(4) . . . . no
C8 N5 C11 C10 -7.8(4) . . . . no
C12 N5 C8 N6 -13.4(5) . . . . no
C8 N6 Li2 N3 33.4(3) 3_755 3_755 . . no
C14 N6 Li4 N1 -104.0(3) . . . . no
C14 N6 Li4 O1 153.7(3) . . . . no
C8 N6 C14 C13 43.2(5) . . . . no
C14 N6 Li2 N3 -117.3(3) 3_755 3_755 . . no
C14 N6 Li4 N9 48.4(4) . . . 3_755 no
Li4 N6 C14 C13 175.6(3) . . . . no
C8 N6 Li4 N9 -179.0(2) . . . 3_755 no
C8 N6 Li4 O1 -73.7(2) . . . . no
Li4 N6 Li2 N3 141.92(16) 3_755 3_755 . . no
C8 N6 Li4 N1 28.6(3) . . . . no
Li4 N6 Li2 N7 -65.97(17) 3_755 3_755 . . no
Li4 N6 C8 N5 -135.5(3) . . . . no
C8 N6 Li2 N7 -174.5(2) 3_755 3_755 . . no
Li4 N6 C8 N4 43.8(3) . . . . no
C14 N6 Li2 N7 34.8(4) 3_755 3_755 . . no
C14 N6 C8 N4 173.6(3) . . . . no
C14 N6 C8 N5 -5.7(5) . . . . no
C16 N7 C15 N9 178.2(3) . . . . no
Li1 N7 C15 N8 121.3(4) . . . . no
C16 N7 Li1 N1 -44.7(3) . . . . no
Li2 N7 Li1 N1 66.96(14) . . . . no
C16 N7 C15 N8 -15.3(5) . . . . no
C15 N7 Li2 N3 -173.2(2) . . . . no
C15 N7 Li1 N1 179.7(2) . . . . no
C16 N7 Li1 O1 -145.8(2) . . . . no
Li2 N7 C15 N8 -158.8(4) . . . . no
C16 N7 Li1 N4 108.6(3) . . . . no
C16 N7 Li2 N3 44.0(3) . . . . no
Li1 N7 Li2 N6 138.03(14) . . . 3_755 no
C15 N7 C16 C17 61.8(5) . . . . no
Li1 N7 Li2 O1 34.26(9) . . . . no
C16 N7 Li2 O1 146.3(3) . . . . no
Li1 N7 Li2 N3 -68.06(14) . . . . no
C15 N7 Li2 N6 32.9(3) . . . 3_755 no
C15 N7 Li1 N4 -27.0(3) . . . . no
Li2 N7 Li1 O1 -34.17(9) . . . . no
Li2 N7 C15 N9 34.6(4) . . . . no
Li2 N7 Li1 N4 -139.77(13) . . . . no
Li1 N7 C15 N9 -45.3(4) . . . . no
C15 N7 Li2 O1 -70.8(3) . . . . no
Li2 N7 C16 C17 -154.7(3) . . . . no
Li1 N7 C16 C17 -72.1(4) . . . . no
C15 N7 Li1 O1 78.6(2) . . . . no
C16 N7 Li2 N6 -110.0(3) . . . 3_755 no
C18 N8 C15 N9 154.2(6) . . . . no
C15 N8 C18 C17 -3.3(11) . . . . no
C18 N8 C15 N7 -11.3(9) . . . . no
Li4 N9 Li3 O1 36.11(14) 3_755 . . . no
C21 N9 C15 N7 -179.8(3) . . . . no
C15 N9 Li3 O1 -72.4(3) . . . . no
Li4 N9 Li3 N3 -66.3(2) 3_755 . . 3_755 no
Li3 N9 Li4 N6 142.3(2) 3_755 3_755 . . no
C21 N9 Li3 N4 -111.0(2) . . . . no
Li3 N9 C15 N8 -120.8(5) . . . . no
C21 N9 C15 N8 15.5(6) . . . . no
C21 N9 Li3 N3 44.6(3) . . . 3_755 no
Li4 N9 Li3 N4 138.1(2) 3_755 . . . no
Li4 N9 C15 N8 162.2(4) 3_755 . . . no
C15 N9 Li3 N4 29.6(3) . . . . no
Li3 N9 Li4 N1 -66.9(2) 3_755 3_755 . . no
Li4 N9 C21 C20 -161.2(5) 3_755 . . . no
C21 N9 Li3 O1 147.1(2) . . . . no
Li4 N9 C15 N7 -33.2(4) 3_755 . . . no
C21 N9 Li4 N1 36.5(3) 3_755 3_755 . . no
C15 N9 C21 C20 -14.9(6) . . . . no
Li3 N9 C21 C20 123.1(5) . . . . no
C15 N9 Li3 N3 -174.9(3) . . . 3_755 no
C15 N9 Li4 N1 -175.3(3) 3_755 3_755 . . no
Li3 N9 C15 N7 43.8(4) . . . . no
C15 N9 Li4 N6 33.8(3) 3_755 3_755 . . no
C21 N9 Li4 N6 -114.3(3) 3_755 3_755 . . no
Si2 N10 Li5 Cl1 103.68(13) . . . . no
Li5 N10 Li6 Cl1 0.05(15) . . . . no
Si2 N10 Li6 Cl1 -111.58(15) . . . . no
Si1 N10 Li6 Cl1 113.33(17) . . . . no
Si1 N10 Li5 Cl1 -119.83(12) . . . . no
Li6 N10 Li5 Cl1 -0.05(14) . . . . no
Si3 N11 Li6 Cl1 106.66(17) . . . . no
Li7 N11 Li6 Cl1 -0.37(18) . . . . no
Si4 N11 Li6 Cl1 -117.66(14) . . . . no
Si3 N11 Li7 Cl1 -117.89(14) . . . . no
Li6 N11 Li7 Cl1 0.37(18) . . . . no
Si4 N11 Li7 Cl1 105.73(16) . . . . no
Si5 N12 Li7 Cl1 106.83(14) 2_555 . . . no
Si5 N12 Li7 Cl1 -115.75(13) . . . . no
Li7 N12 Li7 Cl1 0.00(16) 2_555 . . . no
N1 C2 C3 C4 -61.9(3) . . . . no
C2 C3 C4 N2 44.6(3) . . . . no
N2 C5 C6 C7 41.7(4) . . . . no
C5 C6 C7 N3 -62.9(3) . . . . no
N4 C9 C10 C11 -61.9(4) . . . . no
C9 C10 C11 N5 42.9(4) . . . . no
N5 C12 C13 C14 42.5(5) . . . . no
C12 C13 C14 N6 -61.5(5) . . . . no
N7 C16 C17 C18 -70.5(6) . . . . no
C16 C17 C18 N8 40.6(7) . . . . no
C19 C20 C21 N9 38.9(9) . . . . no
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.250 0.250 0.500 223 52 toluene
2 0.250 0.750 0.000 223 52 toluene
3 0.250 0.250 0.000 199 51 toluene
4 0.250 0.750 0.500 199 51 toluene
5 0.750 0.250 0.000 223 52 toluene
6 0.750 0.750 0.500 223 52 toluene
7 0.750 0.250 0.500 199 51 toluene
8 0.750 0.750 0.000 199 51 toluene
_platon_squeeze_details
;
;
_vrf_CHEMW03_RAL_R43
;
PROBLEM: The ratio of given/expected molecular weight as calculated from the
_atom_site* data lies outside the range 0.90 <> 1.10
RESPONSE: This value considers the squeezed toluene molecules.
;
_vrf_PLAT043_RAL_R43
;
PROBLEM: Check Reported Molecular Weight ................ 2009.07
RESPONSE: This value considers the squeezed toluene molecules.
;
#===END
# Attachment '- Li3hpp compound 1.cif'
# CIF-file generated for Richard Layfield ORAL111 R = 0.04
#===============================================================================
data_ORAL111
_database_code_depnum_ccdc_archive 'CCDC 815987'
#TrackingRef '- Li3hpp compound 1.cif'
#===============================================================================
_audit_creation_date 'Jan 18 00:05:49 2011'
_audit_creation_method 'PLATON option'
# 5. CHEMICAL DATA
_chemical_name_systematic
;
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C19 H48 Li3 N5 Si4'
_chemical_formula_structural ?
_chemical_formula_sum 'C19 H48 Li3 N5 Si4'
_chemical_formula_iupac ?
_chemical_formula_weight 479.80
_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 Tetragonal
_symmetry_space_group_name_Hall 'P 4c -2ab'
_symmetry_space_group_name_H-M 'P 42 b c'
_symmetry_Int_Tables_number 106
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 -y,x,1/2+z
3 -x,-y,z
4 y,-x,1/2+z
5 1/2-x,1/2+y,z
6 1/2-y,1/2-x,1/2+z
7 1/2+x,1/2-y,z
8 1/2+y,1/2+x,1/2+z
_cell_length_a 16.4053(3)
_cell_length_b 16.4053(3)
_cell_length_c 21.4837(10)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_volume 5781.99(31)
_cell_formula_units_Z 8
_cell_measurement_temperature 100
_cell_measurement_reflns_used 5106
_cell_measurement_theta_min 3.0977
_cell_measurement_theta_max 28.5775
_cell_special_details
;
;
_exptl_crystal_description cube
_exptl_crystal_colour colourless
_exptl_crystal_size_max 0.3
_exptl_crystal_size_mid 0.2
_exptl_crystal_size_min 0.1
_exptl_crystal_size_rad ?
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.102
_exptl_crystal_density_method 'Not Measured'
_exptl_crystal_F_000 2096
_exptl_absorpt_coefficient_mu 0.220
_exptl_crystal_density_meas_temp ?
_exptl_absorpt_correction_T_min 0.89186
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov 6 2009,16:24:50)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
#===============================================================================
# 7. EXPERIMENTAL DATA
_exptl_special_details
;
;
_diffrn_ambient_temperature 100
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_probe x-ray
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method '\w scans'
_diffrn_detector_area_resol_mean 8.3367
# number of measured reflections (redundant set)
_diffrn_reflns_number 12200
_diffrn_reflns_av_R_equivalents 0.0397
_diffrn_reflns_av_sigmaI/netI 0.0486
_diffrn_reflns_limit_h_min -18
_diffrn_reflns_limit_h_max 21
_diffrn_reflns_limit_k_min -16
_diffrn_reflns_limit_k_max 21
_diffrn_reflns_limit_l_min -28
_diffrn_reflns_limit_l_max 10
_diffrn_reflns_theta_min 3.12
_diffrn_reflns_theta_max 28.66
_diffrn_reflns_theta_full 28.66
_diffrn_measured_fraction_theta_max 0.896
_diffrn_measured_fraction_theta_full 0.896
_diffrn_reflns_reduction_process
;
;
# number of unique reflections
_reflns_number_total 4177
# number of observed reflections (> n sig(I))
_reflns_number_gt 3128
_reflns_threshold_expression >2\s(i)
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov 6 2009,16:24:50)
;
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov 6 2009,16:24:50)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov 6 2009,16:24:50)
;
_computing_structure_solution 'SUPERFLIP (Palatinus, Chapuis, 2007)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics 'SXGRAPH (Farrugia, 1999)'
_computing_publication_material 'PLATON (Spek, 2003)'
#===============================================================================
# 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.
;
_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^)+(0.0641P)^2^] 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_abs_structure_details 'Flack H.D. (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack 0.3(3)
_chemical_absolute_configuration unk
_refine_ls_number_reflns 4177
_refine_ls_number_parameters 297
_refine_ls_number_restraints 19
_refine_ls_number_constraints ?
_refine_ls_R_factor_all 0.0551
_refine_ls_R_factor_gt 0.0393
_refine_ls_wR_factor_ref 0.1060
_refine_ls_wR_factor_gt 0.0989
_refine_ls_goodness_of_fit_ref 0.995
_refine_ls_restrained_S_all 0.993
_refine_ls_shift/su_max 0.003
_refine_ls_shift/su_mean 0.000
_refine_diff_density_max 0.539
_refine_diff_density_min -0.221
_refine_diff_density_rms 0.063
#===============================================================================
# 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
_atom_site_calc_flag
_atom_site_refinement_flags
Si1 Si Uani 0.13718(6) 1.10019(6) 0.39452(7) 1.000 0.0136(3) . .
Si2 Si Uani 0.18475(6) 0.92668(6) 0.36945(7) 1.000 0.0149(3) . .
N1 N Uani 0.1172(3) 1.00512(18) 0.3651(4) 1.000 0.0120(14) . .
N3 N Uani 0.00272(17) 0.9323(3) 0.2256(3) 1.000 0.0123(19) . .
N4 N Uani 0.00000 1.00000 0.1274(5) 1.000 0.018(3) . .
C1 C Uani 0.1681(4) 1.1743(3) 0.3329(3) 1.000 0.0273(16) . .
C2 C Uani 0.0409(2) 1.1439(2) 0.4281(2) 1.000 0.0217(12) . .
C3 C Uani 0.2135(3) 1.1038(4) 0.4584(3) 1.000 0.0273(16) . .
C4 C Uani 0.1950(3) 0.8793(3) 0.4478(3) 1.000 0.0290(17) . .
C5 C Uani 0.2906(2) 0.9567(3) 0.3442(3) 1.000 0.0272(14) . .
C6 C Uani 0.1536(3) 0.8436(3) 0.3144(3) 1.000 0.0213(14) . .
C13 C Uani 0.00000 1.00000 0.1927(6) 1.000 0.016(2) . .
C14 C Uani 0.0156(4) 0.9251(4) 0.0930(4) 1.000 0.0377(19) . .
C15 C Uani 0.0504(3) 0.8589(2) 0.1335(2) 1.000 0.0283(12) . .
C16 C Uani 0.0010(2) 0.8541(4) 0.1925(4) 1.000 0.0163(19) . .
Li1 Li Uani 0.0832(8) 1.0038(4) 0.2777(7) 1.000 0.020(3) . .
Li2 Li Uani 0.00000 1.00000 0.3900(10) 1.000 0.017(3) . .
Si3 Si Uani 0.36516(6) 0.89648(6) 0.12774(7) 1.000 0.0136(3) . .
Si4 Si Uani 0.31443(6) 1.06925(6) 0.15186(7) 1.000 0.0148(3) . .
N2 N Uani 0.3842(3) 0.99261(19) 0.1548(4) 1.000 0.0117(14) . .
N5 N Uani 0.50000 1.00000 0.3941(5) 1.000 0.018(3) . .
N6 N Uani 0.49550(19) 1.0684(3) 0.2965(3) 1.000 0.0147(17) . .
C7 C Uani 0.4609(2) 0.8571(3) 0.0884(2) 1.000 0.0237(12) . .
C8 C Uani 0.2837(3) 0.8891(3) 0.0663(3) 1.000 0.0213(14) . .
C9 C Uani 0.3395(4) 0.8232(3) 0.1915(3) 1.000 0.0257(16) . .
C10 C Uani 0.2975(3) 1.1120(4) 0.0717(3) 1.000 0.0273(16) . .
C11 C Uani 0.2103(2) 1.0381(3) 0.1806(2) 1.000 0.0267(14) . .
C12 C Uani 0.3467(3) 1.1556(3) 0.2024(3) 1.000 0.0227(14) . .
C17 C Uani 0.50000 1.00000 0.3322(5) 1.000 0.0087(19) . .
C18 C Uani 0.4828(4) 1.0733(4) 0.4310(4) 1.000 0.0293(17) . .
C19 C Uani 0.4469(2) 1.1390(2) 0.3901(2) 1.000 0.0234(11) . .
C20 C Uani 0.4956(2) 1.1453(4) 0.3304(5) 1.000 0.019(2) . .
Li3 Li Uani 0.4204(7) 0.9928(5) 0.2466(7) 1.000 0.020(3) . .
Li4 Li Uani 0.50000 1.00000 0.1283(11) 1.000 0.023(4) . .
H1A H Uiso 0.22080 1.15980 0.31710 1.000 0.0410 calc R
H1B H Uiso 0.17020 1.22820 0.35030 1.000 0.0410 calc R
H1C H Uiso 0.12900 1.17310 0.29960 1.000 0.0410 calc R
H2A H Uiso 0.00140 1.15090 0.39550 1.000 0.0320 calc R
H2B H Uiso 0.05240 1.19560 0.44690 1.000 0.0320 calc R
H2C H Uiso 0.01950 1.10730 0.45890 1.000 0.0320 calc R
H3A H Uiso 0.19560 1.06990 0.49220 1.000 0.0410 calc R
H3B H Uiso 0.21930 1.15890 0.47280 1.000 0.0410 calc R
H3C H Uiso 0.26510 1.08440 0.44330 1.000 0.0410 calc R
H4A H Uiso 0.21020 0.92020 0.47760 1.000 0.0440 calc R
H4B H Uiso 0.23610 0.83770 0.44650 1.000 0.0440 calc R
H4C H Uiso 0.14390 0.85550 0.45980 1.000 0.0440 calc R
H5A H Uiso 0.28740 1.00160 0.31560 1.000 0.0410 calc R
H5B H Uiso 0.31650 0.91120 0.32410 1.000 0.0410 calc R
H5C H Uiso 0.32200 0.97250 0.37990 1.000 0.0410 calc R
H6A H Uiso 0.09900 0.82660 0.32370 1.000 0.0320 calc R
H6B H Uiso 0.19000 0.79810 0.31880 1.000 0.0320 calc R
H6C H Uiso 0.15600 0.86360 0.27240 1.000 0.0320 calc R
H14A H Uiso 0.05340 0.93660 0.05940 1.000 0.0450 calc R
H14B H Uiso -0.03490 0.90610 0.07470 1.000 0.0450 calc R
H15A H Uiso 0.10680 0.87090 0.14330 1.000 0.0340 calc R
H15B H Uiso 0.04840 0.80720 0.11170 1.000 0.0340 calc R
H16A H Uiso -0.05490 0.84000 0.18240 1.000 0.0200 calc R
H16B H Uiso 0.02290 0.81160 0.21910 1.000 0.0200 calc R
H7A H Uiso 0.47350 0.89080 0.05320 1.000 0.0350 calc R
H7B H Uiso 0.45220 0.80210 0.07480 1.000 0.0350 calc R
H7C H Uiso 0.50540 0.85850 0.11740 1.000 0.0350 calc R
H8A H Uiso 0.23220 0.90490 0.08380 1.000 0.0320 calc R
H8B H Uiso 0.28030 0.83400 0.05160 1.000 0.0320 calc R
H8C H Uiso 0.29700 0.92460 0.03230 1.000 0.0320 calc R
H9A H Uiso 0.38290 0.82240 0.22140 1.000 0.0390 calc R
H9B H Uiso 0.33250 0.76970 0.17430 1.000 0.0390 calc R
H9C H Uiso 0.28990 0.84000 0.21140 1.000 0.0390 calc R
H10A H Uiso 0.34790 1.13350 0.05590 1.000 0.0420 calc R
H10B H Uiso 0.25760 1.15480 0.07370 1.000 0.0420 calc R
H10C H Uiso 0.27830 1.06960 0.04460 1.000 0.0420 calc R
H11A H Uiso 0.18580 1.00160 0.15120 1.000 0.0400 calc R
H11B H Uiso 0.17670 1.08560 0.18520 1.000 0.0400 calc R
H11C H Uiso 0.21550 1.01120 0.22010 1.000 0.0400 calc R
H12A H Uiso 0.34410 1.13920 0.24520 1.000 0.0340 calc R
H12B H Uiso 0.31110 1.20120 0.19570 1.000 0.0340 calc R
H12C H Uiso 0.40160 1.17090 0.19220 1.000 0.0340 calc R
H18A H Uiso 0.53280 1.09300 0.44980 1.000 0.0350 calc R
H18B H Uiso 0.44480 1.06010 0.46410 1.000 0.0350 calc R
H19A H Uiso 0.44800 1.19080 0.41180 1.000 0.0280 calc R
H19B H Uiso 0.39060 1.12600 0.38050 1.000 0.0280 calc R
H20A H Uiso 0.47250 1.18770 0.30440 1.000 0.0230 calc R
H20B H Uiso 0.55130 1.16050 0.34020 1.000 0.0230 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
Si1 0.0139(5) 0.0143(5) 0.0127(5) -0.0023(5) -0.0013(5) -0.0015(4)
Si2 0.0118(5) 0.0149(5) 0.0180(6) 0.0004(5) -0.0020(5) 0.0010(4)
N1 0.010(2) 0.014(2) 0.012(3) 0.0004(15) -0.005(2) 0.0002(11)
N3 0.011(3) 0.011(3) 0.015(4) -0.002(3) 0.0004(12) 0.0009(11)
N4 0.023(5) 0.025(5) 0.006(5) 0.0000 0.0000 -0.0062(18)
C1 0.038(3) 0.017(2) 0.027(3) 0.002(2) 0.004(3) -0.004(2)
C2 0.022(2) 0.019(2) 0.024(2) -0.0087(19) -0.0023(19) 0.0041(16)
C3 0.016(2) 0.040(3) 0.026(3) -0.012(3) 0.001(2) -0.005(2)
C4 0.026(3) 0.032(3) 0.029(3) 0.006(3) -0.011(3) 0.001(2)
C5 0.0106(19) 0.027(2) 0.044(3) -0.011(2) 0.001(2) -0.0014(16)
C6 0.017(2) 0.021(2) 0.026(3) -0.006(2) 0.001(2) 0.0029(17)
C13 0.009(3) 0.026(4) 0.013(4) 0.0000 0.0000 -0.0029(18)
C14 0.076(4) 0.025(3) 0.012(3) -0.006(3) 0.008(3) -0.006(3)
C15 0.039(2) 0.020(2) 0.026(2) -0.008(2) 0.014(2) -0.0041(19)
C16 0.020(3) 0.015(3) 0.014(4) -0.003(4) -0.0014(15) -0.0012(14)
Li1 0.028(6) 0.019(5) 0.014(6) -0.005(3) 0.001(5) 0.002(3)
Li2 0.014(5) 0.020(5) 0.016(6) 0.0000 0.0000 -0.001(3)
Si3 0.0129(5) 0.0149(5) 0.0130(5) -0.0021(5) -0.0008(5) -0.0012(4)
Si4 0.0121(5) 0.0155(5) 0.0167(5) 0.0014(5) -0.0007(5) 0.0022(4)
N2 0.010(2) 0.0112(19) 0.014(3) -0.0021(16) 0.002(2) -0.0005(11)
N5 0.028(5) 0.009(4) 0.018(6) 0.0000 0.0000 -0.0024(15)
N6 0.018(3) 0.014(3) 0.012(3) 0.001(3) -0.0001(13) 0.0017(12)
C7 0.018(2) 0.025(2) 0.028(2) -0.007(2) -0.0016(19) 0.0012(16)
C8 0.018(2) 0.025(2) 0.021(3) -0.008(2) -0.009(2) 0.0000(19)
C9 0.033(3) 0.018(2) 0.026(3) 0.001(2) 0.005(2) -0.005(2)
C10 0.037(3) 0.022(2) 0.023(3) 0.009(2) -0.001(2) 0.009(2)
C11 0.017(2) 0.025(2) 0.038(3) 0.000(2) 0.005(2) 0.0022(17)
C12 0.022(2) 0.017(2) 0.029(3) -0.001(2) 0.002(2) 0.0025(18)
C17 0.006(3) 0.009(3) 0.011(4) 0.0000 0.0000 -0.0014(15)
C18 0.053(3) 0.016(3) 0.019(3) -0.006(2) 0.006(3) -0.007(3)
C19 0.029(2) 0.0172(19) 0.024(2) -0.0068(19) 0.005(2) -0.0016(16)
C20 0.017(3) 0.014(3) 0.026(5) -0.002(4) -0.0018(17) -0.0011(14)
Li3 0.011(5) 0.031(5) 0.019(6) -0.002(3) -0.009(5) 0.007(3)
Li4 0.020(6) 0.027(7) 0.022(8) 0.0000 0.0000 -0.001(3)
#===============================================================================
# 10. MOLECULAR GEOMETRY
_geom_special_details
;
Bond distances, angles etc. have been calculated using the
rounded fractional coordinates. All su's 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 N1 1.715(4) . . yes
Si1 C1 1.868(6) . . yes
Si1 C2 1.879(4) . . yes
Si1 C3 1.859(6) . . yes
Si2 N1 1.701(4) . . yes
Si2 C4 1.862(6) . . yes
Si2 C5 1.885(4) . . yes
Si2 C6 1.876(6) . . yes
Si3 C7 1.897(4) . . yes
Si3 C8 1.882(6) . . yes
Si3 C9 1.871(6) . . yes
Si3 N2 1.710(4) . . yes
Si4 C10 1.880(7) . . yes
Si4 C11 1.887(4) . . yes
Si4 N2 1.701(4) . . yes
Si4 C12 1.862(6) . . yes
N1 Li2 1.998(8) . . yes
N1 Li1 1.959(17) . . yes
N3 C13 1.317(9) . . yes
N3 Li1 2.091(13) . . yes
N3 Li1 2.083(13) . 3_575 yes
N3 C16 1.467(9) . . yes
N4 C14 1.457(9) . 3_575 yes
N4 C13 1.403(17) . . yes
N4 C14 1.457(9) . . yes
N2 Li3 2.060(17) . . yes
N2 Li4 1.987(9) . . yes
N5 C18 1.468(9) . 3_675 yes
N5 C17 1.330(15) . . yes
N5 C18 1.468(9) . . yes
N6 C17 1.361(8) . . yes
N6 C20 1.457(9) . . yes
N6 Li3 2.051(13) . . yes
N6 Li3 2.015(13) . 3_675 yes
C13 Li1 2.281(18) . . yes
C13 Li1 2.281(18) . 3_575 yes
C14 C15 1.504(8) . . no
C15 C16 1.507(9) . . no
C1 H1A 0.9600 . . no
C1 H1C 0.9600 . . no
C1 H1B 0.9600 . . no
C2 H2A 0.9600 . . no
C2 H2B 0.9600 . . no
C2 H2C 0.9600 . . no
C3 H3A 0.9600 . . no
C3 H3B 0.9600 . . no
C3 H3C 0.9600 . . no
C4 H4C 0.9600 . . no
C4 H4A 0.9600 . . no
C4 H4B 0.9600 . . no
C5 H5B 0.9600 . . no
C5 H5A 0.9600 . . no
C5 H5C 0.9600 . . no
C6 H6B 0.9600 . . no
C6 H6A 0.9600 . . no
C6 H6C 0.9600 . . no
C14 H14B 0.9700 . . no
C14 H14A 0.9700 . . no
C15 H15A 0.9700 . . no
C15 H15B 0.9700 . . no
C16 H16B 0.9700 . . no
C16 H16A 0.9700 . . no
C17 Li3 2.259(16) . . yes
C17 Li3 2.259(16) . 3_675 yes
C18 C19 1.510(8) . . no
C19 C20 1.515(10) . . no
C7 H7A 0.9600 . . no
C7 H7B 0.9600 . . no
C7 H7C 0.9600 . . no
C8 H8A 0.9600 . . no
C8 H8B 0.9600 . . no
C8 H8C 0.9600 . . no
C9 H9A 0.9600 . . no
C9 H9B 0.9600 . . no
C9 H9C 0.9600 . . no
C10 H10A 0.9600 . . no
C10 H10B 0.9600 . . no
C10 H10C 0.9600 . . no
C11 H11A 0.9600 . . no
C11 H11B 0.9600 . . no
C11 H11C 0.9600 . . no
C12 H12A 0.9600 . . no
C12 H12B 0.9600 . . no
C12 H12C 0.9600 . . no
C18 H18A 0.9700 . . no
C18 H18B 0.9700 . . no
C19 H19A 0.9700 . . no
C19 H19B 0.9700 . . no
C20 H20A 0.9700 . . no
C20 H20B 0.9700 . . 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
N1 Si1 C1 112.5(3) . . . yes
N1 Si1 C2 109.2(2) . . . yes
N1 Si1 C3 115.5(3) . . . yes
C1 Si1 C2 104.6(2) . . . yes
C1 Si1 C3 108.6(3) . . . yes
C2 Si1 C3 105.7(2) . . . yes
N1 Si2 C4 115.1(3) . . . yes
N1 Si2 C5 112.8(2) . . . yes
N1 Si2 C6 109.7(3) . . . yes
C4 Si2 C5 106.6(2) . . . yes
C4 Si2 C6 106.9(2) . . . yes
C5 Si2 C6 105.0(2) . . . yes
N2 Si3 C9 112.6(3) . . . yes
N2 Si3 C7 108.3(2) . . . yes
N2 Si3 C8 115.3(3) . . . yes
C8 Si3 C9 108.2(3) . . . yes
C7 Si3 C8 104.7(2) . . . yes
C7 Si3 C9 107.1(2) . . . yes
N2 Si4 C12 110.5(3) . . . yes
N2 Si4 C10 114.1(3) . . . yes
C10 Si4 C11 105.5(2) . . . yes
C10 Si4 C12 107.0(3) . . . yes
C11 Si4 C12 105.8(2) . . . yes
N2 Si4 C11 113.4(2) . . . yes
Si2 N1 Li2 125.5(3) . . . yes
Si1 N1 Si2 122.9(3) . . . yes
Si1 N1 Li1 114.7(4) . . . yes
Li1 N1 Li2 89.0(7) . . . yes
Si2 N1 Li1 103.3(4) . . . yes
Si1 N1 Li2 97.1(4) . . . yes
C13 N3 Li1 80.5(5) . . . yes
C13 N3 C16 118.5(7) . . . yes
C13 N3 Li1 80.9(5) . . 3_575 yes
C16 N3 Li1 139.7(4) . . . yes
C16 N3 Li1 133.4(4) . . 3_575 yes
Li1 N3 Li1 81.8(5) . . 3_575 yes
C13 N4 C14 120.5(5) . . 3_575 yes
C14 N4 C14 119.0(9) . . 3_575 yes
C13 N4 C14 120.5(5) . . . yes
Si3 N2 Si4 123.1(3) . . . yes
Si3 N2 Li3 112.3(4) . . . yes
Si3 N2 Li4 97.7(4) . . . yes
Li3 N2 Li4 89.9(8) . . . yes
Si4 N2 Li3 103.2(4) . . . yes
Si4 N2 Li4 126.0(3) . . . yes
C18 N5 C18 114.6(8) . . 3_675 yes
C17 N5 C18 122.7(5) . . . yes
C17 N5 C18 122.7(5) . . 3_675 yes
C17 N6 Li3 81.5(5) . . 3_675 yes
C17 N6 C20 115.6(7) . . . yes
C20 N6 Li3 141.8(4) . . . yes
C20 N6 Li3 134.2(4) . . 3_675 yes
Li3 N6 Li3 80.3(5) . . 3_675 yes
C17 N6 Li3 80.1(5) . . . yes
N4 C13 Li1 143.2(4) . . . yes
N4 C13 Li1 143.2(4) . . 3_575 yes
N3 C13 Li1 64.4(5) 3_575 . . yes
N3 C13 N4 122.5(5) 3_575 . . yes
N3 C13 N4 122.5(5) . . . yes
N3 C13 Li1 64.7(5) . . . yes
N3 C13 N3 115.1(10) . . 3_575 yes
N3 C13 Li1 64.4(5) . . 3_575 yes
N3 C13 Li1 64.7(5) 3_575 . 3_575 yes
Li1 C13 Li1 73.6(6) . . 3_575 yes
N4 C14 C15 112.5(7) . . . yes
C14 C15 C16 108.7(5) . . . no
N3 C16 C15 110.6(5) . . . yes
Si1 C1 H1C 109.00 . . . no
Si1 C1 H1B 109.00 . . . no
H1A C1 H1C 109.00 . . . no
H1B C1 H1C 109.00 . . . no
Si1 C1 H1A 110.00 . . . no
H1A C1 H1B 109.00 . . . no
H2A C2 H2B 110.00 . . . no
H2A C2 H2C 109.00 . . . no
Si1 C2 H2C 109.00 . . . no
Si1 C2 H2B 110.00 . . . no
Si1 C2 H2A 109.00 . . . no
H2B C2 H2C 110.00 . . . no
H3A C3 H3C 109.00 . . . no
Si1 C3 H3A 109.00 . . . no
Si1 C3 H3B 110.00 . . . no
H3A C3 H3B 109.00 . . . no
H3B C3 H3C 109.00 . . . no
Si1 C3 H3C 109.00 . . . no
Si2 C4 H4B 110.00 . . . no
Si2 C4 H4A 110.00 . . . no
H4B C4 H4C 109.00 . . . no
Si2 C4 H4C 109.00 . . . no
H4A C4 H4B 109.00 . . . no
H4A C4 H4C 109.00 . . . no
Si2 C5 H5C 110.00 . . . no
H5A C5 H5B 109.00 . . . no
H5A C5 H5C 109.00 . . . no
Si2 C5 H5B 109.00 . . . no
Si2 C5 H5A 110.00 . . . no
H5B C5 H5C 109.00 . . . no
H6A C6 H6B 110.00 . . . no
H6A C6 H6C 109.00 . . . no
Si2 C6 H6A 110.00 . . . no
Si2 C6 H6B 109.00 . . . no
Si2 C6 H6C 109.00 . . . no
H6B C6 H6C 109.00 . . . no
N4 C14 H14B 109.00 . . . no
N4 C14 H14A 109.00 . . . no
H14A C14 H14B 108.00 . . . no
C15 C14 H14B 109.00 . . . no
C15 C14 H14A 109.00 . . . no
C14 C15 H15B 110.00 . . . no
H15A C15 H15B 108.00 . . . no
C14 C15 H15A 110.00 . . . no
C16 C15 H15B 110.00 . . . no
C16 C15 H15A 110.00 . . . no
H16A C16 H16B 108.00 . . . no
C15 C16 H16B 110.00 . . . no
N3 C16 H16B 110.00 . . . no
N3 C16 H16A 110.00 . . . no
C15 C16 H16A 109.00 . . . no
N6 C17 Li3 63.5(5) 3_675 . 3_675 yes
N5 C17 Li3 144.5(4) . . . yes
N5 C17 N6 124.3(4) . . 3_675 yes
N5 C17 Li3 144.5(4) . . 3_675 yes
N6 C17 Li3 63.5(5) . . . yes
N6 C17 N6 111.4(8) . . 3_675 yes
N6 C17 Li3 61.9(5) . . 3_675 yes
N5 C17 N6 124.3(4) . . . yes
Li3 C17 Li3 71.0(6) . . 3_675 yes
N6 C17 Li3 61.9(5) 3_675 . . yes
N5 C18 C19 110.2(7) . . . yes
C18 C19 C20 109.6(4) . . . no
N6 C20 C19 111.3(5) . . . yes
Si3 C7 H7A 109.00 . . . no
H7B C7 H7C 109.00 . . . no
Si3 C7 H7B 109.00 . . . no
H7A C7 H7C 110.00 . . . no
H7A C7 H7B 110.00 . . . no
Si3 C7 H7C 109.00 . . . no
Si3 C8 H8C 109.00 . . . no
Si3 C8 H8B 109.00 . . . no
Si3 C8 H8A 109.00 . . . no
H8A C8 H8B 109.00 . . . no
H8B C8 H8C 110.00 . . . no
H8A C8 H8C 110.00 . . . no
Si3 C9 H9C 109.00 . . . no
Si3 C9 H9B 109.00 . . . no
Si3 C9 H9A 109.00 . . . no
H9A C9 H9B 110.00 . . . no
H9A C9 H9C 110.00 . . . no
H9B C9 H9C 109.00 . . . no
H10A C10 H10B 109.00 . . . no
H10B C10 H10C 109.00 . . . no
Si4 C10 H10C 109.00 . . . no
H10A C10 H10C 110.00 . . . no
Si4 C10 H10A 109.00 . . . no
Si4 C10 H10B 109.00 . . . no
Si4 C11 H11B 110.00 . . . no
H11A C11 H11C 109.00 . . . no
H11A C11 H11B 110.00 . . . no
Si4 C11 H11C 109.00 . . . no
Si4 C11 H11A 109.00 . . . no
H11B C11 H11C 109.00 . . . no
Si4 C12 H12C 109.00 . . . no
H12A C12 H12B 110.00 . . . no
Si4 C12 H12A 109.00 . . . no
H12B C12 H12C 109.00 . . . no
Si4 C12 H12B 109.00 . . . no
H12A C12 H12C 110.00 . . . no
C19 C18 H18B 110.00 . . . no
N5 C18 H18A 110.00 . . . no
C19 C18 H18A 110.00 . . . no
N5 C18 H18B 110.00 . . . no
H18A C18 H18B 108.00 . . . no
H19A C19 H19B 108.00 . . . no
C18 C19 H19A 110.00 . . . no
C18 C19 H19B 110.00 . . . no
C20 C19 H19B 110.00 . . . no
C20 C19 H19A 110.00 . . . no
C19 C20 H20A 109.00 . . . no
N6 C20 H20B 109.00 . . . no
H20A C20 H20B 108.00 . . . no
N6 C20 H20A 109.00 . . . no
C19 C20 H20B 109.00 . . . no
N3 Li1 C13 34.7(3) . . . yes
N1 Li1 C13 159.8(8) . . . yes
N1 Li1 N3 134.6(6) . . 3_575 yes
N1 Li1 N3 134.4(6) . . . yes
N3 Li1 N3 64.4(4) . . 3_575 yes
N3 Li1 C13 34.8(3) 3_575 . . yes
N1 Li2 N1 148.9(12) . . 3_575 yes
N6 Li3 C17 36.6(3) 3_675 . . yes
N2 Li3 N6 134.9(6) . . 3_675 yes
N2 Li3 N6 132.4(6) . . . yes
N2 Li3 C17 161.2(7) . . . yes
N6 Li3 C17 36.4(3) . . . yes
N6 Li3 N6 67.2(4) . . 3_675 yes
N2 Li4 N2 146.7(14) . . 3_675 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
C1 Si1 N1 Si2 100.9(5) . . . . no
C2 Si1 N1 Si2 -143.5(4) . . . . no
C3 Si1 N1 Si2 -24.6(6) . . . . no
C1 Si1 N1 Li1 -25.9(6) . . . . no
C2 Si1 N1 Li1 89.7(5) . . . . no
C3 Si1 N1 Li1 -151.4(5) . . . . no
C1 Si1 N1 Li2 -118.1(6) . . . . no
C2 Si1 N1 Li2 -2.4(7) . . . . no
C3 Si1 N1 Li2 116.4(6) . . . . no
C4 Si2 N1 Si1 74.6(5) . . . . no
C5 Si2 N1 Si1 -48.0(6) . . . . no
C6 Si2 N1 Si1 -164.7(4) . . . . no
C4 Si2 N1 Li1 -153.7(4) . . . . no
C5 Si2 N1 Li1 83.6(4) . . . . no
C6 Si2 N1 Li1 -33.1(5) . . . . no
C4 Si2 N1 Li2 -55.3(9) . . . . no
C5 Si2 N1 Li2 -178.0(8) . . . . no
C6 Si2 N1 Li2 65.3(9) . . . . no
C9 Si3 N2 Si4 -100.5(5) . . . . no
C7 Si3 N2 Li3 -94.5(5) . . . . no
C8 Si3 N2 Li3 148.6(4) . . . . no
C9 Si3 N2 Li3 23.8(5) . . . . no
C7 Si3 N2 Li4 -1.4(7) . . . . no
C8 Si3 N2 Li4 -118.3(7) . . . . no
C9 Si3 N2 Li4 116.8(7) . . . . no
C7 Si3 N2 Si4 141.3(4) . . . . no
C8 Si3 N2 Si4 24.4(6) . . . . no
C10 Si4 N2 Si3 -73.5(5) . . . . no
C10 Si4 N2 Li3 158.3(4) . . . . no
C11 Si4 N2 Li3 -80.8(4) . . . . no
C12 Si4 N2 Li3 37.7(4) . . . . no
C10 Si4 N2 Li4 58.6(10) . . . . no
C11 Si4 N2 Li4 179.5(9) . . . . no
C11 Si4 N2 Si3 47.4(6) . . . . no
C12 Si4 N2 Si3 166.0(5) . . . . no
C12 Si4 N2 Li4 -62.0(10) . . . . no
Si1 N1 Li1 C13 -97.8(10) . . . . no
Si1 N1 Li1 N3 -49.1(10) . . . 3_575 no
Si1 N1 Li1 N3 -145.6(6) . . . . no
Si2 N1 Li1 C13 125.9(10) . . . . no
Si2 N1 Li1 N3 174.6(7) . . . 3_575 no
Si2 N1 Li1 N3 78.0(9) . . . . no
Li2 N1 Li1 C13 -0.4(10) . . . . no
Li2 N1 Li1 N3 48.3(7) . . . 3_575 no
Si1 N1 Li2 N1 114.9(4) . . . 3_575 no
Si2 N1 Li2 N1 -105.6(7) . . . 3_575 no
Li1 N1 Li2 N1 0.1(3) . . . 3_575 no
Li2 N1 Li1 N3 -48.3(8) . . . . no
C16 N3 C13 Li1 -142.1(5) . . . . no
C16 N3 Li1 N3 148.3(8) . . . 3_575 no
Li1 N3 Li1 N1 71.2(9) 3_575 . . . no
Li1 N3 Li1 C13 -82.0(5) 3_575 . . . no
Li1 N3 Li1 N3 -57.1(4) 3_575 . . 3_575 no
C16 N3 Li1 C13 -120.8(9) . . 3_575 . no
C16 N3 Li1 N1 86.3(12) . . 3_575 3_575 no
C16 N3 Li1 N3 -145.7(7) . . 3_575 3_575 no
Li1 N3 Li1 C13 81.7(5) . . 3_575 . no
Li1 N3 Li1 N1 -71.2(8) . . 3_575 3_575 no
Li1 N3 Li1 N3 56.8(4) . . 3_575 3_575 no
C16 N3 C13 N4 -3.5(3) . . . . no
Li1 N3 C13 N4 138.5(4) . . . . no
Li1 N3 C13 N4 -138.4(4) 3_575 . . . no
C13 N3 Li1 N1 153.2(9) . . . . no
C13 N3 Li1 N3 24.9(4) . . . 3_575 no
C16 N3 Li1 N1 -83.4(13) . . . . no
C16 N3 Li1 C13 123.4(10) . . . . no
Li1 N3 C13 N3 -41.5(4) . . . 3_575 no
C16 N3 C13 Li1 134.8(5) . . . 3_575 no
Li1 N3 C13 N3 41.6(4) . 3_575 . . no
Li1 N3 C13 N4 -138.4(4) . 3_575 . . no
Li1 N3 C16 C15 -72.1(10) . . . . no
Li1 N3 C16 C15 143.7(7) 3_575 . . . no
Li1 N3 C13 Li1 83.1(6) 3_575 . . . no
C16 N3 C13 N3 176.5(2) . . . 3_575 no
Li1 N3 C13 Li1 -83.1(6) . . . 3_575 no
C13 N3 C16 C15 38.4(4) . . . . no
C14 N4 C13 Li1 80.9(4) . . . . no
C14 N4 C13 Li1 -99.2(4) . . . 3_575 no
C14 N4 C13 N3 170.5(3) . . . 3_575 no
C13 N4 C14 C15 -14.1(6) . . . . no
C14 N4 C13 N3 170.5(3) 3_575 . . . no
C14 N4 C13 N3 -9.5(3) . . . . no
C14 N4 C14 C15 166.0(4) 3_575 . . . no
C14 N4 C13 Li1 -99.2(4) 3_575 . . . no
Li3 N2 Li4 N2 -1.0(4) . . . 3_675 no
Li4 N2 Li3 N6 51.4(7) . . . . no
Li4 N2 Li3 N6 -48.3(7) . . . 3_675 no
Si3 N2 Li3 N6 49.9(9) . . . 3_675 no
Si3 N2 Li3 N6 149.7(6) . . . . no
Si3 N2 Li4 N2 -113.5(4) . . . 3_675 no
Si4 N2 Li4 N2 105.4(7) . . . 3_675 no
Si4 N2 Li3 N6 -75.7(8) . . . . no
Si4 N2 Li3 N6 -175.4(7) . . . 3_675 no
C18 N5 C17 Li3 98.0(5) 3_675 . . . no
C18 N5 C17 N6 9.4(3) . . . . no
C17 N5 C18 C19 13.4(5) . . . . no
C18 N5 C17 Li3 -82.0(5) . . . . no
C18 N5 C17 Li3 98.0(5) . . . 3_675 no
C18 N5 C18 C19 -166.7(4) 3_675 . . . no
C18 N5 C17 N6 -170.6(3) . . . 3_675 no
C18 N5 C17 N6 -170.6(3) 3_675 . . . no
Li3 N6 C17 N5 -139.6(4) . . . . no
Li3 N6 C17 Li3 81.6(5) . . . 3_675 no
C20 N6 C17 N5 3.7(3) . . . . no
C20 N6 C17 Li3 -135.2(5) . . . 3_675 no
C17 N6 Li3 N2 -157.0(8) . . . . no
Li3 N6 C17 N5 138.9(4) 3_675 . . . no
C20 N6 C17 Li3 143.2(5) . . . . no
C20 N6 Li3 N2 83.7(13) . . . . no
C20 N6 Li3 C17 -119.2(11) . . . . no
C20 N6 Li3 N6 -145.5(9) . . . 3_675 no
Li3 N6 Li3 N2 -74.1(8) 3_675 . . . no
Li3 N6 Li3 C17 82.9(5) 3_675 . . . no
Li3 N6 C17 Li3 -81.6(5) 3_675 . . . no
C17 N6 Li3 N6 -26.3(4) . . . 3_675 no
C20 N6 Li3 N2 -88.3(11) . . 3_675 3_675 no
C20 N6 Li3 N6 143.8(8) . . 3_675 3_675 no
Li3 N6 Li3 C17 -81.4(5) . . 3_675 . no
Li3 N6 Li3 N2 72.7(8) . . 3_675 3_675 no
Li3 N6 Li3 N6 -55.2(4) . . 3_675 3_675 no
Li3 N6 C20 C19 -141.7(7) 3_675 . . . no
C20 N6 C17 N6 -176.3(3) . . . 3_675 no
Li3 N6 Li3 N6 56.7(5) 3_675 . . 3_675 no
C20 N6 Li3 C17 117.6(9) . . 3_675 . no
Li3 N6 C20 C19 69.6(12) . . . . no
Li3 N6 C17 N5 138.9(4) . 3_675 . . no
Li3 N6 C17 N6 -41.1(4) . 3_675 . . no
C17 N6 C20 C19 -38.0(5) . . . . no
Li3 N6 C17 N6 40.5(4) . . . 3_675 no
Li1 C13 Li1 N3 -69.4(4) . . 3_575 . no
N3 C13 Li1 N3 138.3(7) 3_575 . . . no
N4 C13 Li1 N1 -179.7(8) . . . . no
N3 C13 Li1 N1 -68.6(11) . . . . no
N3 C13 Li1 N3 -138.3(7) . . . 3_575 no
N3 C13 Li1 N1 69.7(11) 3_575 . . . no
Li1 C13 Li1 N3 68.9(4) 3_575 . . . no
N4 C13 Li1 N3 110.6(4) . . 3_575 . no
Li1 C13 Li1 N1 0.3(10) 3_575 . . . no
N4 C13 Li1 N3 110.6(4) . . . 3_575 no
N4 C13 Li1 N3 -111.1(4) . . . . no
N4 C14 C15 C16 46.8(6) . . . . no
C14 C15 C16 N3 -59.0(5) . . . . no
N5 C17 Li3 N6 -110.6(4) . . . 3_675 no
Li3 C17 Li3 N6 69.4(4) . . 3_675 . no
N6 C17 Li3 N6 136.8(6) . . . 3_675 no
Li3 C17 Li3 N6 -67.4(4) 3_675 . . . no
N5 C17 Li3 N6 -110.6(4) . . 3_675 . no
N5 C17 Li3 N6 112.6(4) . . . . no
N6 C17 Li3 N6 -136.8(6) 3_675 . . . no
N5 C18 C19 C20 -45.6(6) . . . . no
C18 C19 C20 N6 59.2(6) . . . . 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 H5A 3.4000 . . no
Si2 H3C 3.3100 . . no
Si2 H2A 3.3600 . 3_575 no
Si3 H11A 3.4500 . . no
Si4 H7C 3.2700 . 3_675 no
Si4 H8A 3.3500 . . no
N3 C6 3.447(7) . . no
N3 H6C 2.9300 . . no
C5 C17 3.517(3) . . no
C5 C17 3.517(3) . . no
C5 Li3 3.047(14) . . no
C6 N3 3.447(7) . . no
C11 Li1 3.003(14) . . no
C11 C13 3.516(3) . . no
C11 C13 3.516(3) . . no
C13 C11 3.516(3) . . no
C13 C11 3.516(3) . 3_575 no
C17 C5 3.517(3) . . no
C17 C5 3.517(3) . 3_675 no
C3 H4A 3.0400 . . no
C5 H3C 3.0200 . . no
C5 H11C 3.0700 . . no
C6 H16B 3.0100 . . no
C6 H2A 3.0800 . 3_575 no
C7 H15B 3.0900 . 7_565 no
C8 H11A 3.0500 . . no
C8 H10C 3.0000 . . no
C8 H2B 3.1000 . 4_464 no
C11 H8A 3.0400 . . no
C12 H7C 3.0500 . 3_675 no
C12 H20A 3.0600 . . no
C13 H15A 2.9500 . . no
C13 H15A 2.9500 . 3_575 no
C14 H3A 3.0700 . 4_464 no
C16 H11B 3.0800 . 3_575 no
C16 H6C 3.0700 . . no
C17 H19B 2.9300 . . no
C17 H19B 2.9300 . 3_675 no
C20 H12A 3.0900 . . no
Li1 C11 3.003(14) . . no
Li3 C5 3.047(14) . . no
Li1 H1C 2.9200 . . no
Li1 H11A 3.2000 . . no
Li1 H11B 2.8500 . . no
Li1 H11C 2.5000 . . no
Li1 H6C 2.5900 . . no
Li1 H6A 3.0800 . . no
Li2 H2C 2.3200 . . no
Li2 H2A 2.4800 . . no
Li2 H2C 2.3200 . 3_575 no
Li2 H2A 2.4800 . 3_575 no
Li3 H5B 2.7300 . . no
Li3 H9A 2.9100 . . no
Li3 H12C 3.1600 . . no
Li3 H12A 2.7100 . . no
Li3 H5A 2.6400 . . no
Li4 H7A 2.4500 . . no
Li4 H7C 2.3300 . 3_675 no
Li4 H7C 2.3300 . . no
Li4 H7A 2.4500 . 3_675 no
H1A H12A 2.5700 . . no
H1C Li1 2.9200 . . no
H2A Li2 2.4800 . . no
H2A Si2 3.3600 . 3_575 no
H2A C6 3.0800 . 3_575 no
H2A H6A 2.2900 . 3_575 no
H2B H8C 2.5100 . 2_665 no
H2B C8 3.1000 . 2_665 no
H2C H14A 2.4400 . 2_665 no
H2C Li2 2.3200 . . no
H3A H4A 2.4900 . . no
H3A H15B 2.5900 . 2_665 no
H3A C14 3.0700 . 2_665 no
H3C C5 3.0200 . . no
H3C Si2 3.3100 . . no
H3C H5C 2.4700 . . no
H3C H19B 2.5500 . . no
H4A C3 3.0400 . . no
H4A H3A 2.4900 . . no
H5A Li3 2.6400 . . no
H5A H11C 2.3700 . . no
H5A Si1 3.4000 . . no
H5B Li3 2.7300 . . no
H5B H20B 2.4900 . 3_675 no
H5C H3C 2.4700 . . no
H6A H2A 2.2900 . 3_575 no
H6A H20A 2.6000 . 5_545 no
H6A Li1 3.0800 . . no
H6A H16B 2.5800 . . no
H6C N3 2.9300 . . no
H6C C16 3.0700 . . no
H6C Li1 2.5900 . . no
H6C H9C 2.5900 . . no
H7A Li4 2.4500 . . no
H7A H18B 2.5400 . 8_454 no
H7B H15B 2.5200 . 7_565 no
H7C C12 3.0500 . 3_675 no
H7C H12C 2.2700 . 3_675 no
H7C Li4 2.3300 . . no
H7C Si4 3.2700 . 3_675 no
H8A Si4 3.3500 . . no
H8A H15A 2.4900 . . no
H8A C11 3.0400 . . no
H8A H11A 2.2800 . . no
H8C H2B 2.5100 . 4_464 no
H8C H10C 2.4100 . . no
H9A Li3 2.9100 . . no
H9B H16A 2.5800 . 7_565 no
H9C H6C 2.5900 . . no
H10C H8C 2.4100 . . no
H10C C8 3.0000 . . no
H11A H15A 2.5100 . . no
H11A H8A 2.2800 . . no
H11A Li1 3.2000 . . no
H11A Si3 3.4500 . . no
H11A C8 3.0500 . . no
H11B C16 3.0800 . 3_575 no
H11B H16A 2.3400 . 3_575 no
H11B Li1 2.8500 . . no
H11C C5 3.0700 . . no
H11C Li1 2.5000 . . no
H11C H5A 2.3700 . . no
H12A C20 3.0900 . . no
H12A Li3 2.7100 . . no
H12A H20A 2.5900 . . no
H12A H1A 2.5700 . . no
H12C Li3 3.1600 . . no
H12C H7C 2.2700 . 3_675 no
H14A H2C 2.4400 . 4_464 no
H14B H16A 2.5800 . . no
H15A C13 2.9500 . . no
H15A H8A 2.4900 . . no
H15A H11A 2.5100 . . no
H15B H3A 2.5900 . 4_464 no
H15B C7 3.0900 . 7_465 no
H15B H7B 2.5200 . 7_465 no
H16A H14B 2.5800 . . no
H16A H11B 2.3400 . 3_575 no
H16A H9B 2.5800 . 7_465 no
H16B C6 3.0100 . . no
H16B H6A 2.5800 . . no
H18A H18B 2.5600 . 3_675 no
H18B H18A 2.5600 . 3_675 no
H18B H7A 2.5400 . 8_455 no
H19B C17 2.9300 . . no
H19B H3C 2.5500 . . no
H20A C12 3.0600 . . no
H20A H12A 2.5900 . . no
H20A H6A 2.6000 . 5_555 no
H20B H5B 2.4900 . 3_675 no
_vrf_PLAT029_ORAL111
;
PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.90
RESPONSE: The crystal was erroneously processed in the centric Laue class.
;
#===END
# Attachment '- MnLi.cif'
# CIF-file generated for D. Woodruff/ R. A. Layfield oral145 R = 0.09
#===============================================================================
data_oral145
_database_code_depnum_ccdc_archive 'CCDC 827193'
#TrackingRef '- MnLi.cif'
_audit_creation_date 'May 13 10:57:32 2011'
_audit_creation_method 'PLATON option'
#===============================================================================
# 5. CHEMICAL DATA
_chemical_name_systematic
;
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety
'C42 H72 Li7 Mn N18 O, C30 H90 Cl Li5 N5 Si10, 2(C7 H8)'
_chemical_formula_structural ?
_chemical_formula_sum 'C86 H178 Cl Li12 Mn N23 O Si10'
_chemical_formula_iupac ?
_chemical_formula_weight 1988.96
_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'
O O 0.0106 0.0060 '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'
Mn Mn 0.3368 0.7283 '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'
Cl Cl 0.1484 0.1585 '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 '-C 2yc'
_symmetry_space_group_name_H-M 'C 2/c'
_symmetry_Int_Tables_number 15
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 -x,y,1/2-z
3 -x,-y,-z
4 x,-y,1/2+z
5 1/2+x,1/2+y,z
6 1/2-x,1/2+y,1/2-z
7 1/2-x,1/2-y,-z
8 1/2+x,1/2-y,1/2+z
_cell_length_a 20.1096(12)
_cell_length_b 24.4769(15)
_cell_length_c 24.9736(17)
_cell_angle_alpha 90
_cell_angle_beta 105.769(6)
_cell_angle_gamma 90
_cell_volume 11829.9(13)
_cell_formula_units_Z 4
_cell_measurement_temperature 100(1)
_cell_measurement_reflns_used 6420
_cell_measurement_theta_min 2.9161
_cell_measurement_theta_max 23.9788
_cell_special_details
;
;
_exptl_crystal_description platelet
_exptl_crystal_colour brown
_exptl_crystal_size_max 0.200
_exptl_crystal_size_mid 0.100
_exptl_crystal_size_min 0.100
_exptl_crystal_size_rad ?
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.117
_exptl_crystal_density_method 'Not Measured'
_exptl_crystal_F_000 4260
_exptl_absorpt_coefficient_mu 0.284
_exptl_crystal_density_meas_temp ?
_exptl_absorpt_correction_T_min 0.66492
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov 6 2009,16:24:50)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
#===============================================================================
# 7. EXPERIMENTAL DATA
_exptl_special_details
;
;
_diffrn_ambient_temperature 100(1)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_probe x-ray
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method '\w scans'
_diffrn_detector_area_resol_mean 8.3367
# number of measured reflections (redundant set)
_diffrn_reflns_number 21119
_diffrn_reflns_av_R_equivalents 0.0906
_diffrn_reflns_av_sigmaI/netI 0.1765
_diffrn_reflns_limit_h_min -22
_diffrn_reflns_limit_h_max 21
_diffrn_reflns_limit_k_min -26
_diffrn_reflns_limit_k_max 27
_diffrn_reflns_limit_l_min -25
_diffrn_reflns_limit_l_max 18
_diffrn_reflns_theta_min 2.92
_diffrn_reflns_theta_max 24.04
_diffrn_reflns_theta_full 21.00
_diffrn_measured_fraction_theta_max 0.813
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_reduction_process
;
;
# number of unique reflections
_reflns_number_total 7584
# number of observed reflections (> n sig(I))
_reflns_number_gt 3705
_reflns_threshold_expression >2\s(i)
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov 6 2009,16:24:50)
;
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov 6 2009,16:24:50)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov 6 2009,16:24:50)
;
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics 'SXGRAPH (Farrugia, 1999)'
_computing_publication_material 'PLATON (Spek, 2003)'
#===============================================================================
# 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.
;
_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^)+(0.0952P)^2^+17.5420P] 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_abs_structure_details ?
_refine_ls_abs_structure_Flack .
_refine_ls_number_reflns 7584
_refine_ls_number_parameters 617
_refine_ls_number_restraints 0
_refine_ls_number_constraints ?
_refine_ls_R_factor_all 0.1783
_refine_ls_R_factor_gt 0.0857
_refine_ls_wR_factor_ref 0.2215
_refine_ls_wR_factor_gt 0.1979
_refine_ls_goodness_of_fit_ref 1.040
_refine_ls_restrained_S_all 1.040
_refine_ls_shift/su_max 0.020
_refine_ls_shift/su_mean 0.001
_refine_diff_density_max 0.491
_refine_diff_density_min -0.273
_refine_diff_density_rms 0.059
#===============================================================================
# 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
_atom_site_calc_flag
_atom_site_refinement_flags
Mn1 Mn Uani 0.08153(18) -0.05525(15) 0.49437(16) 0.220 0.0470(14) . .
Mn2 Mn Uani 0.0216(2) 0.01498(17) 0.42107(17) 0.160 0.0354(16) . .
Mn3 Mn Uani 0.0918(3) 0.0161(2) 0.5690(3) 0.090 0.046(3) . .
Mn4 Mn Uani -0.0294(4) -0.0810(4) 0.5013(4) 0.030 0.042(3) . .
O1 O Uani 0.00000 0.00000 0.50000 1.000 0.052(3) . .
N1 N Uani 0.1033(3) 0.0664(3) 0.4555(3) 1.000 0.057(3) . .
N2 N Uani 0.2254(3) 0.0629(2) 0.4829(2) 1.000 0.046(2) . .
N3 N Uani 0.1588(3) 0.0025(3) 0.5206(3) 1.000 0.060(3) . .
N4 N Uani -0.0715(3) 0.0469(3) 0.3836(3) 1.000 0.050(3) . .
N5 N Uani -0.1066(3) 0.1377(3) 0.3587(3) 1.000 0.057(3) . .
N6 N Uani -0.0639(3) 0.1109(3) 0.4525(3) 1.000 0.061(3) . .
N7 N Uani 0.0445(4) -0.0643(3) 0.4096(3) 1.000 0.068(3) . .
N8 N Uani -0.0182(5) -0.1275(5) 0.3481(4) 1.000 0.145(6) . .
N9 N Uani -0.0614(4) -0.0922(3) 0.4160(3) 1.000 0.071(3) . .
C1 C Uani 0.1634(4) 0.0446(3) 0.4855(3) 1.000 0.051(3) . .
C2 C Uani 0.2330(4) 0.1013(3) 0.4409(3) 1.000 0.055(3) . .
C3 C Uani 0.1659(4) 0.1091(3) 0.3950(3) 1.000 0.059(3) . .
C4 C Uani 0.1096(4) 0.1144(3) 0.4239(3) 1.000 0.058(3) . .
C5 C Uani 0.2908(3) 0.0508(3) 0.5248(3) 1.000 0.054(3) . .
C6 C Uani 0.2786(4) 0.0186(4) 0.5721(3) 1.000 0.064(3) . .
C7 C Uani 0.2258(4) -0.0231(4) 0.5491(4) 1.000 0.077(4) . .
C8 C Uani -0.0817(4) 0.0986(3) 0.3976(4) 1.000 0.051(3) . .
C9 C Uani -0.1312(4) 0.1901(3) 0.3718(4) 1.000 0.077(4) . .
C10 C Uani -0.1323(6) 0.1937(4) 0.4314(5) 1.000 0.105(5) . .
C11 C Uani -0.0676(5) 0.1676(4) 0.4655(4) 1.000 0.091(5) . .
C12 C Uani -0.1127(4) 0.1296(4) 0.2998(4) 1.000 0.073(4) . .
C13 C Uani -0.0793(4) 0.0779(4) 0.2893(4) 1.000 0.072(4) . .
C14 C Uani -0.0978(4) 0.0343(3) 0.3241(4) 1.000 0.069(4) . .
C15 C Uani -0.0126(7) -0.0952(5) 0.3918(4) 1.000 0.083(4) . .
C16 C Uani 0.0468(13) -0.1619(7) 0.3444(8) 0.500 0.085(9) . .
C17 C Uani 0.1072(12) -0.1343(13) 0.3741(12) 0.500 0.146(15) . .
C18 C Uani 0.0744(8) -0.0541(7) 0.3232(9) 0.500 0.081(9) . .
C19 C Uani 0.0269(12) -0.1023(11) 0.3026(8) 0.500 0.133(13) . .
C20 C Uani 0.0944(5) -0.0748(5) 0.3789(4) 1.000 0.081(5) . .
C21 C Uani -0.0798(7) -0.1580(6) 0.3223(6) 1.000 0.146(7) . .
C22 C Uani -0.1274(9) -0.1567(6) 0.3496(7) 1.000 0.166(9) . .
C23 C Uani -0.1215(5) -0.1240(5) 0.3984(5) 1.000 0.115(6) . .
Li1 Li Uani 0.08153(18) -0.05525(15) 0.49437(16) 0.780 0.0470(14) . .
Li2 Li Uani 0.0216(2) 0.01498(17) 0.42107(17) 0.840 0.0354(16) . .
Li3 Li Uani 0.0918(3) 0.0161(2) 0.5690(3) 0.910 0.046(3) . .
Li4 Li Uani -0.0294(4) -0.0810(4) 0.5013(4) 0.970 0.042(3) . .
Cl1 Cl Uani 0.00000 0.48580(9) 0.25000 1.000 0.0442(10) . .
Si1 Si Uani 0.06608(10) 0.31098(8) 0.29525(8) 1.000 0.0416(7) . .
Si2 Si Uani 0.07176(10) 0.42318(9) 0.10353(9) 1.000 0.0491(8) . .
Si3 Si Uani 0.19322(10) 0.43997(9) 0.20021(9) 1.000 0.0475(8) . .
Si4 Si Uani -0.13796(11) 0.63605(9) 0.26171(10) 1.000 0.0554(9) . .
Si5 Si Uani -0.02296(11) 0.61937(9) 0.36363(10) 1.000 0.0617(9) . .
N10 N Uani 0.00000 0.3449(3) 0.25000 1.000 0.035(3) . .
N11 N Uani 0.1060(3) 0.4421(2) 0.1714(2) 1.000 0.039(2) . .
N12 N Uani -0.0666(3) 0.6006(2) 0.2981(2) 1.000 0.045(2) . .
C24 C Uani 0.1084(3) 0.3581(2) 0.3545(3) 1.000 0.040(3) . .
C25 C Uani 0.1352(3) 0.2896(3) 0.2627(3) 1.000 0.056(3) . .
C26 C Uani 0.0412(4) 0.2475(3) 0.3269(3) 1.000 0.064(3) . .
C27 C Uani 0.1227(4) 0.4446(4) 0.0541(3) 1.000 0.073(4) . .
C28 C Uani 0.0636(4) 0.3477(3) 0.0956(3) 1.000 0.065(3) . .
C29 C Uani -0.0169(3) 0.4536(3) 0.0758(3) 1.000 0.056(3) . .
C30 C Uani 0.2393(4) 0.5003(4) 0.1787(3) 1.000 0.074(4) . .
C31 C Uani 0.2379(4) 0.3778(3) 0.1835(3) 1.000 0.068(3) . .
C32 C Uani 0.2114(3) 0.4426(3) 0.2775(3) 1.000 0.050(3) . .
C33 C Uani -0.1133(4) 0.6977(3) 0.2276(4) 1.000 0.077(4) . .
C34 C Uani -0.1951(3) 0.5937(3) 0.2061(3) 1.000 0.056(3) . .
C35 C Uani -0.1947(4) 0.6626(3) 0.3041(4) 1.000 0.075(3) . .
C36 C Uani 0.0652(3) 0.5879(3) 0.3811(3) 1.000 0.066(3) . .
C37 C Uani -0.0668(4) 0.5967(4) 0.4176(3) 1.000 0.075(3) . .
C38 C Uani -0.0090(4) 0.6938(3) 0.3763(4) 1.000 0.101(5) . .
Li5 Li Uani 0.0458(5) 0.4047(4) 0.2154(5) 1.000 0.038(4) . .
Li6 Li Uani 0.0760(6) 0.5157(5) 0.1954(5) 1.000 0.047(4) . .
Li7 Li Uani 0.00000 0.5864(6) 0.25000 1.000 0.044(6) . .
C39 C Uiso 0.2800(8) 0.2464(7) 0.4958(8) 0.500 0.068(5) . .
C40 C Uiso 0.3417(8) 0.2335(6) 0.5212(7) 0.500 0.064(5) . .
C41 C Uiso 0.2851(5) 0.2420(3) 0.5464(4) 1.000 0.077(3) . .
C42 C Uiso 0.3406(5) 0.2373(4) 0.4696(5) 1.000 0.112(4) . .
C43 C Uiso 0.2704(9) 0.2509(7) 0.4301(7) 0.500 0.074(5) . .
C44 C Uiso 0.2288(10) 0.2765(8) -0.0057(10) 0.500 0.086(6) . .
C45 C Uiso 0.2522(11) 0.3048(9) 0.0348(9) 0.500 0.083(6) . .
C46 C Uiso 0.2089(11) 0.3239(9) -0.0049(10) 1.000 0.230(8) . .
C47 C Uiso 0.1893(10) 0.2931(10) -0.0508(9) 0.500 0.098(7) . .
C48 C Uiso 0.2887(7) 0.2616(7) 0.0513(6) 1.000 0.149(5) . .
H2A H Uiso 0.26930 0.08800 0.42420 1.000 0.0660 calc R
H2B H Uiso 0.24810 0.13700 0.45870 1.000 0.0660 calc R
H3A H Uiso 0.16840 0.14250 0.37320 1.000 0.0710 calc R
H3B H Uiso 0.15720 0.07740 0.36960 1.000 0.0710 calc R
H4A H Uiso 0.11940 0.14640 0.44910 1.000 0.0690 calc R
H4B H Uiso 0.06510 0.12110 0.39570 1.000 0.0690 calc R
H5A H Uiso 0.31440 0.08540 0.53900 1.000 0.0640 calc R
H5B H Uiso 0.32130 0.02980 0.50720 1.000 0.0640 calc R
H6A H Uiso 0.32210 0.00090 0.59340 1.000 0.0760 calc R
H6B H Uiso 0.26250 0.04300 0.59760 1.000 0.0760 calc R
H7A H Uiso 0.21990 -0.04690 0.57950 1.000 0.0920 calc R
H7B H Uiso 0.24150 -0.04620 0.52230 1.000 0.0920 calc R
H9A H Uiso -0.17840 0.19640 0.34760 1.000 0.0930 calc R
H9B H Uiso -0.10090 0.21920 0.36410 1.000 0.0930 calc R
H10A H Uiso -0.13440 0.23240 0.44240 1.000 0.1260 calc R
H10B H Uiso -0.17320 0.17450 0.43680 1.000 0.1260 calc R
H11A H Uiso -0.02730 0.18690 0.45900 1.000 0.1090 calc R
H11B H Uiso -0.06550 0.17140 0.50540 1.000 0.1090 calc R
H12A H Uiso -0.09100 0.16080 0.28570 1.000 0.0870 calc R
H12B H Uiso -0.16220 0.12880 0.27900 1.000 0.0870 calc R
H13A H Uiso -0.09570 0.06790 0.24940 1.000 0.0870 calc R
H13B H Uiso -0.02850 0.08250 0.29910 1.000 0.0870 calc R
H14A H Uiso -0.14870 0.03050 0.31440 1.000 0.0830 calc R
H14B H Uiso -0.07830 -0.00090 0.31610 1.000 0.0830 calc R
H16A H Uiso 0.04520 -0.19870 0.36050 0.500 0.1030 calc .
H16B H Uiso 0.04690 -0.16620 0.30500 0.500 0.1030 calc .
H17A H Uiso 0.14380 -0.13950 0.35490 0.500 0.1730 calc .
H17B H Uiso 0.12380 -0.15030 0.41180 0.500 0.1730 calc .
H18A H Uiso 0.11320 -0.05170 0.30600 0.500 0.0980 calc .
H18B H Uiso 0.04950 -0.01880 0.31990 0.500 0.0980 calc .
H19A H Uiso 0.05490 -0.13240 0.29360 0.500 0.1570 calc .
H19B H Uiso -0.00710 -0.09140 0.26750 0.500 0.1570 calc .
H20A H Uiso 0.13850 -0.05650 0.39780 0.500 0.0970 calc .
H20B H Uiso 0.07760 -0.05900 0.34120 0.500 0.0970 calc .
H20C H Uiso 0.13800 -0.05820 0.39870 0.500 0.0970 . .
H20D H Uiso 0.10180 -0.11390 0.37780 0.500 0.0970 . .
H21A H Uiso -0.09990 -0.14340 0.28440 1.000 0.1750 calc R
H21B H Uiso -0.06680 -0.19650 0.31840 1.000 0.1750 calc R
H22A H Uiso -0.13380 -0.19490 0.36040 1.000 0.1990 calc R
H22B H Uiso -0.17100 -0.14580 0.32240 1.000 0.1990 calc R
H23A H Uiso -0.16200 -0.09930 0.39110 1.000 0.1380 calc R
H23B H Uiso -0.12410 -0.14850 0.42930 1.000 0.1380 calc R
H24A H Uiso 0.15480 0.34460 0.37310 1.000 0.0600 calc R
H24B H Uiso 0.08060 0.35930 0.38120 1.000 0.0600 calc R
H24C H Uiso 0.11170 0.39490 0.34000 1.000 0.0600 calc R
H25A H Uiso 0.17100 0.26930 0.28990 1.000 0.0840 calc R
H25B H Uiso 0.15570 0.32200 0.25060 1.000 0.0840 calc R
H25C H Uiso 0.11520 0.26620 0.23050 1.000 0.0840 calc R
H26A H Uiso 0.08240 0.23140 0.35240 1.000 0.0960 calc R
H26B H Uiso 0.02070 0.22120 0.29750 1.000 0.0960 calc R
H26C H Uiso 0.00760 0.25670 0.34750 1.000 0.0960 calc R
H27A H Uiso 0.09720 0.43490 0.01600 1.000 0.1090 calc R
H27B H Uiso 0.16750 0.42600 0.06390 1.000 0.1090 calc R
H27C H Uiso 0.13010 0.48430 0.05670 1.000 0.1090 calc R
H28A H Uiso 0.03630 0.33870 0.05780 1.000 0.0980 calc R
H28B H Uiso 0.04050 0.33310 0.12250 1.000 0.0980 calc R
H28C H Uiso 0.10970 0.33140 0.10250 1.000 0.0980 calc R
H29A H Uiso -0.01270 0.49110 0.06340 1.000 0.0850 calc R
H29B H Uiso -0.04070 0.45380 0.10520 1.000 0.0850 calc R
H29C H Uiso -0.04340 0.43170 0.04430 1.000 0.0850 calc R
H30A H Uiso 0.28760 0.50070 0.20100 1.000 0.1110 calc R
H30B H Uiso 0.21670 0.53420 0.18480 1.000 0.1110 calc R
H30C H Uiso 0.23750 0.49700 0.13930 1.000 0.1110 calc R
H31A H Uiso 0.28610 0.37770 0.20620 1.000 0.1030 calc R
H31B H Uiso 0.23660 0.37820 0.14400 1.000 0.1030 calc R
H31C H Uiso 0.21440 0.34500 0.19160 1.000 0.1030 calc R
H32A H Uiso 0.26060 0.45020 0.29400 1.000 0.0750 calc R
H32B H Uiso 0.19960 0.40740 0.29120 1.000 0.0750 calc R
H32C H Uiso 0.18370 0.47160 0.28790 1.000 0.0750 calc R
H33A H Uiso -0.15460 0.71950 0.21100 1.000 0.1160 calc R
H33B H Uiso -0.09200 0.68640 0.19840 1.000 0.1160 calc R
H33C H Uiso -0.08030 0.71970 0.25530 1.000 0.1160 calc R
H34A H Uiso -0.22840 0.61730 0.18040 1.000 0.0840 calc R
H34B H Uiso -0.21990 0.56720 0.22290 1.000 0.0840 calc R
H34C H Uiso -0.16700 0.57430 0.18570 1.000 0.0840 calc R
H35A H Uiso -0.23630 0.67900 0.27940 1.000 0.1120 calc R
H35B H Uiso -0.16950 0.69030 0.33020 1.000 0.1120 calc R
H35C H Uiso -0.20790 0.63250 0.32490 1.000 0.1120 calc R
H36A H Uiso 0.08700 0.59150 0.42110 1.000 0.0980 calc R
H36B H Uiso 0.09350 0.60660 0.36040 1.000 0.0980 calc R
H36C H Uiso 0.06130 0.54920 0.37090 1.000 0.0980 calc R
H37A H Uiso -0.03420 0.59920 0.45470 1.000 0.1130 calc R
H37B H Uiso -0.08240 0.55880 0.41030 1.000 0.1130 calc R
H37C H Uiso -0.10670 0.62020 0.41600 1.000 0.1130 calc R
H38A H Uiso 0.02200 0.69960 0.41360 1.000 0.1510 calc R
H38B H Uiso -0.05340 0.71160 0.37360 1.000 0.1510 calc R
H38C H Uiso 0.01180 0.70930 0.34840 1.000 0.1510 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
Mn1 0.043(2) 0.051(2) 0.041(3) 0.001(2) 0.001(2) 0.011(2)
Mn2 0.024(2) 0.046(3) 0.035(3) 0.002(2) 0.006(2) -0.001(2)
Mn3 0.040(4) 0.044(4) 0.065(5) 0.016(4) 0.031(4) 0.006(3)
Mn4 0.025(5) 0.059(6) 0.044(6) -0.005(5) 0.012(4) -0.001(5)
O1 0.041(4) 0.059(5) 0.056(5) 0.009(4) 0.014(4) 0.000(4)
N1 0.037(4) 0.065(5) 0.066(5) 0.026(4) 0.007(4) -0.003(4)
N2 0.034(4) 0.064(4) 0.043(4) 0.000(3) 0.017(3) -0.006(3)
N3 0.039(4) 0.067(5) 0.072(5) 0.019(4) 0.012(4) 0.001(4)
N4 0.041(4) 0.044(4) 0.062(5) 0.005(4) 0.008(3) 0.004(3)
N5 0.047(4) 0.043(4) 0.088(6) 0.026(5) 0.029(4) 0.007(3)
N6 0.078(5) 0.044(5) 0.074(6) -0.009(4) 0.042(4) 0.004(4)
N7 0.070(5) 0.082(5) 0.051(5) 0.000(4) 0.014(4) 0.015(4)
N8 0.076(7) 0.235(12) 0.112(9) -0.090(9) 0.004(6) 0.029(8)
N9 0.048(5) 0.088(6) 0.071(6) 0.003(4) 0.006(5) -0.012(5)
C1 0.038(5) 0.063(6) 0.048(6) 0.012(5) 0.006(4) 0.001(5)
C2 0.042(5) 0.065(5) 0.067(6) 0.004(5) 0.031(5) -0.001(4)
C3 0.059(5) 0.068(6) 0.054(6) 0.014(5) 0.021(5) 0.004(5)
C4 0.044(5) 0.066(6) 0.062(6) 0.008(5) 0.012(4) 0.001(4)
C5 0.031(5) 0.075(6) 0.050(6) -0.003(5) 0.002(4) 0.003(4)
C6 0.045(5) 0.095(7) 0.049(6) 0.007(5) 0.010(4) 0.007(5)
C7 0.068(6) 0.081(7) 0.078(7) 0.040(6) 0.013(5) 0.008(6)
C8 0.035(5) 0.045(6) 0.080(7) 0.009(6) 0.026(5) 0.000(4)
C9 0.075(6) 0.047(6) 0.119(9) 0.018(6) 0.042(6) 0.007(5)
C10 0.137(10) 0.076(7) 0.141(11) 0.018(7) 0.105(9) 0.027(7)
C11 0.127(9) 0.072(7) 0.095(8) -0.002(6) 0.067(7) 0.017(7)
C12 0.060(6) 0.070(7) 0.083(8) 0.027(6) 0.011(5) -0.020(5)
C13 0.055(5) 0.078(7) 0.080(7) 0.017(6) 0.013(5) -0.011(5)
C14 0.055(6) 0.068(6) 0.079(8) 0.001(6) 0.008(5) 0.000(5)
C15 0.100(9) 0.100(8) 0.034(6) -0.011(6) -0.005(6) 0.081(8)
C16 0.15(2) 0.047(12) 0.075(15) 0.014(11) 0.060(15) 0.013(14)
C17 0.094(18) 0.18(3) 0.21(3) 0.07(2) 0.12(2) 0.04(2)
C18 0.044(11) 0.065(12) 0.13(2) -0.039(14) 0.017(12) -0.018(10)
C19 0.14(2) 0.21(3) 0.069(16) -0.015(18) 0.064(15) 0.02(2)
C20 0.071(7) 0.129(10) 0.053(7) 0.022(6) 0.033(5) 0.050(6)
C21 0.093(10) 0.218(16) 0.113(12) -0.078(11) 0.006(9) 0.003(10)
C22 0.210(17) 0.133(12) 0.174(16) -0.056(11) 0.085(13) -0.101(12)
C23 0.071(8) 0.151(11) 0.115(10) -0.032(9) 0.011(7) 0.016(8)
Li1 0.043(2) 0.051(2) 0.041(3) 0.001(2) 0.001(2) 0.011(2)
Li2 0.024(2) 0.046(3) 0.035(3) 0.002(2) 0.006(2) -0.001(2)
Li3 0.040(4) 0.044(4) 0.065(5) 0.016(4) 0.031(4) 0.006(3)
Li4 0.025(5) 0.059(6) 0.044(6) -0.005(5) 0.012(4) -0.001(5)
Cl1 0.0541(16) 0.0333(14) 0.0580(19) 0.0000 0.0373(15) 0.0000
Si1 0.0412(12) 0.0336(12) 0.0406(13) 0.0025(10) -0.0051(10) -0.0024(10)
Si2 0.0398(13) 0.0746(16) 0.0343(14) 0.0062(12) 0.0126(10) 0.0136(12)
Si3 0.0357(12) 0.0694(15) 0.0396(14) 0.0083(12) 0.0140(11) 0.0089(11)
Si4 0.0471(14) 0.0499(14) 0.0720(18) -0.0163(13) 0.0212(13) 0.0060(12)
Si5 0.0413(13) 0.0670(16) 0.0806(19) -0.0337(14) 0.0231(13) -0.0023(12)
N10 0.035(5) 0.037(5) 0.026(5) 0.0000 -0.005(4) 0.0000
N11 0.038(3) 0.056(4) 0.029(4) 0.005(3) 0.019(3) 0.004(3)
N12 0.035(3) 0.042(4) 0.060(4) -0.019(3) 0.018(3) 0.001(3)
C24 0.041(4) 0.035(4) 0.036(5) 0.013(3) -0.003(4) -0.005(3)
C25 0.050(5) 0.036(4) 0.070(6) -0.018(4) -0.002(4) 0.004(4)
C26 0.052(5) 0.040(5) 0.079(6) 0.012(4) -0.018(5) 0.006(4)
C27 0.051(5) 0.129(8) 0.044(5) 0.008(5) 0.024(4) 0.012(5)
C28 0.059(5) 0.094(7) 0.038(5) -0.017(5) 0.007(4) 0.026(5)
C29 0.049(5) 0.076(6) 0.042(5) 0.025(4) 0.010(4) 0.011(4)
C30 0.039(5) 0.131(8) 0.057(6) 0.021(5) 0.021(4) -0.010(5)
C31 0.044(5) 0.109(7) 0.055(6) -0.003(5) 0.018(4) 0.023(5)
C32 0.043(4) 0.069(5) 0.039(5) 0.007(4) 0.012(4) 0.008(4)
C33 0.071(6) 0.046(5) 0.112(8) -0.005(5) 0.021(6) 0.006(5)
C34 0.039(4) 0.065(5) 0.068(6) 0.000(4) 0.021(4) 0.010(4)
C35 0.054(5) 0.074(6) 0.097(7) -0.024(5) 0.021(5) 0.015(5)
C36 0.049(5) 0.088(6) 0.063(6) -0.022(5) 0.020(4) -0.007(5)
C37 0.041(5) 0.115(7) 0.068(6) -0.034(5) 0.014(4) 0.010(5)
C38 0.060(6) 0.078(7) 0.165(11) -0.067(7) 0.031(6) -0.009(5)
Li5 0.043(7) 0.038(7) 0.040(7) -0.012(6) 0.026(6) 0.008(6)
Li6 0.040(7) 0.063(8) 0.045(8) 0.016(7) 0.022(6) 0.004(6)
Li7 0.030(9) 0.052(11) 0.048(11) 0.0000 0.009(8) 0.0000
#===============================================================================
# 10. MOLECULAR GEOMETRY
_geom_special_details
;
Bond distances, angles etc. have been calculated using the
rounded fractional coordinates. All su's 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
Mn1 O1 2.159(4) . . yes
Mn1 N3 2.071(8) . . yes
Mn1 N7 2.056(8) . . yes
Mn1 N6 1.999(8) . 3_556 yes
Mn2 O1 2.162(4) . . yes
Mn2 N1 2.063(8) . . yes
Mn2 N4 2.010(8) . . yes
Mn2 N7 2.033(9) . . yes
Mn3 O1 2.192(7) . . yes
Mn3 N3 2.067(9) . . yes
Mn3 N4 2.052(9) . 3_556 yes
Mn3 N9 2.027(9) . 3_556 yes
Mn4 O1 2.072(10) . . yes
Mn4 N9 2.069(12) . . yes
Mn4 N1 2.091(11) . 3_556 yes
Mn4 N6 2.052(11) . 3_556 yes
Cl1 Li5 2.443(10) . 2_555 yes
Cl1 Li6 2.421(12) . 2_555 yes
Cl1 Li7 2.462(15) . . yes
Cl1 Li5 2.443(10) . . yes
Cl1 Li6 2.421(12) . . yes
Si1 N10 1.708(4) . . yes
Si1 C24 1.887(7) . . yes
Si1 C25 1.866(7) . . yes
Si1 C26 1.872(8) . . yes
Si2 C29 1.882(7) . . yes
Si2 N11 1.711(5) . . yes
Si2 C27 1.880(8) . . yes
Si2 C28 1.861(8) . . yes
Si3 N11 1.706(6) . . yes
Si3 C30 1.897(9) . . yes
Si3 C31 1.871(8) . . yes
Si3 C32 1.866(8) . . yes
Si4 C34 1.859(7) . . yes
Si4 C35 1.871(9) . . yes
Si4 N12 1.712(6) . . yes
Si4 C33 1.865(8) . . yes
Si5 N12 1.697(5) . . yes
Si5 C36 1.873(7) . . yes
Si5 C37 1.884(8) . . yes
Si5 C38 1.857(8) . . yes
O1 Li1 2.159(4) . . yes
O1 Li3 2.192(7) . . yes
O1 Li4 2.072(10) . . yes
O1 Li2 2.162(4) . . yes
N1 Li2 2.063(8) . . yes
N1 C4 1.440(10) . . yes
N1 C1 1.347(10) . . yes
N2 C2 1.447(9) . . yes
N2 C1 1.343(10) . . yes
N2 C5 1.471(9) . . yes
N3 C7 1.481(11) . . yes
N3 C1 1.372(10) . . yes
N3 Li3 2.067(9) . . yes
N3 Li1 2.071(8) . . yes
N4 C8 1.343(11) . . yes
N4 C14 1.468(12) . . yes
N4 Li2 2.010(8) . . yes
N5 C8 1.359(11) . . yes
N5 C9 1.444(11) . . yes
N5 C12 1.456(12) . . yes
N6 C8 1.353(12) . . yes
N6 C11 1.432(12) . . yes
N7 Li1 2.056(8) . . yes
N7 C20 1.442(13) . . yes
N7 C15 1.346(15) . . yes
N7 Li2 2.033(9) . . yes
N8 C15 1.327(15) . . yes
N8 C16 1.58(3) . . yes
N8 C19 1.75(3) . . yes
N8 C21 1.440(18) . . yes
N9 C15 1.287(16) . . yes
N9 C23 1.404(14) . . yes
N9 Li4 2.069(12) . . yes
N10 Li5 2.042(12) . 2_555 yes
N10 Li5 2.042(12) . . yes
N11 Li5 2.058(12) . . yes
N11 Li6 2.041(13) . . yes
N12 Li6 2.097(13) . 2_555 yes
N12 Li7 2.057(6) . . yes
C2 C3 1.527(11) . . no
C3 C4 1.505(11) . . no
C5 C6 1.495(11) . . no
C6 C7 1.472(13) . . no
C9 C10 1.497(15) . . no
C10 C11 1.491(16) . . no
C12 C13 1.489(13) . . no
C13 C14 1.486(13) . . no
C16 C17 1.41(4) . . no
C17 C20 1.49(3) . . no
C18 C19 1.52(3) . . no
C18 C20 1.43(2) . . no
C21 C22 1.32(2) . . no
C22 C23 1.44(2) . . no
C2 H2B 0.9900 . . no
C2 H2A 0.9900 . . no
C3 H3A 0.9900 . . no
C3 H3B 0.9900 . . no
C4 H4B 0.9900 . . no
C4 H4A 0.9900 . . no
C5 H5A 0.9900 . . no
C5 H5B 0.9900 . . no
C6 H6B 0.9900 . . no
C6 H6A 0.9900 . . no
C7 H7B 0.9900 . . no
C7 H7A 0.9900 . . no
C9 H9A 0.9900 . . no
C9 H9B 0.9900 . . no
C10 H10A 0.9900 . . no
C10 H10B 0.9900 . . no
C11 H11A 0.9900 . . no
C11 H11B 0.9900 . . no
C12 H12A 0.9900 . . no
C12 H12B 0.9900 . . no
C13 H13A 0.9900 . . no
C13 H13B 0.9900 . . no
C14 H14A 0.9900 . . no
C14 H14B 0.9900 . . no
C16 H16A 0.9900 . . no
C16 H16B 0.9900 . . no
C17 H17A 0.9900 . . no
C17 H17B 0.9900 . . no
C17 H20D 0.5200 . . no
C18 H18A 0.9900 . . no
C18 H18B 0.9900 . . no
C18 H20B 0.4500 . . no
C19 H19A 0.9900 . . no
C19 H19B 0.9900 . . no
C20 H20A 0.9900 . . no
C20 H20B 0.9900 . . no
C20 H20C 0.9700 . . no
C20 H20D 0.9700 . . no
C21 H21A 0.9900 . . no
C21 H21B 0.9900 . . no
C22 H22A 0.9900 . . no
C22 H22B 0.9900 . . no
C23 H23A 0.9900 . . no
C23 H23B 0.9900 . . no
C24 H24A 0.9800 . . no
C24 H24B 0.9800 . . no
C24 H24C 0.9800 . . no
C25 H25A 0.9800 . . no
C25 H25B 0.9800 . . no
C25 H25C 0.9800 . . no
C26 H26A 0.9800 . . no
C26 H26B 0.9800 . . no
C26 H26C 0.9800 . . no
C27 H27A 0.9800 . . no
C27 H27B 0.9800 . . no
C27 H27C 0.9800 . . no
C28 H28A 0.9800 . . no
C28 H28B 0.9800 . . no
C28 H28C 0.9800 . . no
C29 H29A 0.9800 . . no
C29 H29B 0.9800 . . no
C29 H29C 0.9800 . . no
C30 H30A 0.9800 . . no
C30 H30B 0.9800 . . no
C30 H30C 0.9800 . . no
C31 H31A 0.9800 . . no
C31 H31B 0.9800 . . no
C31 H31C 0.9800 . . no
C32 H32A 0.9800 . . no
C32 H32B 0.9800 . . no
C32 H32C 0.9800 . . no
C33 H33A 0.9800 . . no
C33 H33B 0.9800 . . no
C33 H33C 0.9800 . . no
C34 H34A 0.9800 . . no
C34 H34B 0.9800 . . no
C34 H34C 0.9800 . . no
C35 H35A 0.9800 . . no
C35 H35B 0.9800 . . no
C35 H35C 0.9800 . . no
C36 H36A 0.9800 . . no
C36 H36B 0.9800 . . no
C36 H36C 0.9800 . . no
C37 H37A 0.9800 . . no
C37 H37B 0.9800 . . no
C37 H37C 0.9800 . . no
C38 H38A 0.9800 . . no
C38 H38B 0.9800 . . no
C38 H38C 0.9800 . . no
C39 C40 1.27(2) . . no
C39 C41 1.24(2) . . no
C39 C42 1.55(2) . . no
C39 C43 1.60(3) . . no
C39 C41 1.47(2) . 7_556 no
C40 C41 1.46(2) . . no
C40 C42 1.29(2) . . no
C41 C43 1.41(2) . 7_556 no
C42 C43 1.52(2) . . no
C44 C45 1.21(3) . . no
C44 C46 1.23(3) . . no
C44 C47 1.26(3) . . no
C44 C48 1.64(3) . . no
C44 C48 1.44(3) . 7_555 no
C45 C46 1.22(3) . . no
C45 C48 1.29(3) . . no
C46 C47 1.34(3) . . no
C47 C48 1.41(3) . 7_555 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
O1 Mn1 N3 94.0(2) . . . yes
O1 Mn1 N7 93.8(3) . . . yes
O1 Mn1 N6 96.2(2) . . 3_556 yes
N3 Mn1 N7 115.5(3) . . . yes
N3 Mn1 N6 120.6(3) . . 3_556 yes
N6 Mn1 N7 122.0(3) 3_556 . . yes
O1 Mn2 N1 93.3(3) . . . yes
O1 Mn2 N4 95.6(3) . . . yes
O1 Mn2 N7 94.4(3) . . . yes
N1 Mn2 N4 119.5(3) . . . yes
N1 Mn2 N7 117.1(4) . . . yes
N4 Mn2 N7 121.6(4) . . . yes
O1 Mn3 N3 93.2(3) . . . yes
O1 Mn3 N4 93.5(3) . . 3_556 yes
O1 Mn3 N9 94.5(3) . . 3_556 yes
N3 Mn3 N4 118.7(4) . . 3_556 yes
N3 Mn3 N9 122.2(4) . . 3_556 yes
N4 Mn3 N9 117.8(4) 3_556 . 3_556 yes
O1 Mn4 N9 96.9(4) . . . yes
O1 Mn4 N1 95.2(4) . . 3_556 yes
O1 Mn4 N6 97.4(4) . . 3_556 yes
N1 Mn4 N9 119.2(5) 3_556 . . yes
N6 Mn4 N9 120.8(5) 3_556 . . yes
N1 Mn4 N6 116.1(5) 3_556 . 3_556 yes
Li5 Cl1 Li6 72.0(4) . . . yes
Li5 Cl1 Li7 144.4(3) . . . yes
Li5 Cl1 Li5 71.3(4) . . 2_555 yes
Li5 Cl1 Li6 143.2(4) . . 2_555 yes
Li6 Cl1 Li7 72.4(3) . . . yes
Li5 Cl1 Li6 143.2(4) 2_555 . . yes
Li6 Cl1 Li6 144.8(4) . . 2_555 yes
Li5 Cl1 Li7 144.4(3) 2_555 . . yes
Li6 Cl1 Li7 72.4(3) 2_555 . . yes
Li5 Cl1 Li6 72.0(4) 2_555 . 2_555 yes
N10 Si1 C24 109.0(3) . . . yes
N10 Si1 C25 112.7(2) . . . yes
N10 Si1 C26 115.7(3) . . . yes
C24 Si1 C25 106.4(3) . . . yes
C24 Si1 C26 107.0(3) . . . yes
C25 Si1 C26 105.5(3) . . . yes
C27 Si2 C29 106.2(3) . . . yes
C28 Si2 C29 107.8(3) . . . yes
N11 Si2 C29 110.1(3) . . . yes
N11 Si2 C28 112.0(3) . . . yes
C27 Si2 C28 104.8(4) . . . yes
N11 Si2 C27 115.5(3) . . . yes
N11 Si3 C31 115.6(3) . . . yes
N11 Si3 C32 109.0(3) . . . yes
C30 Si3 C31 105.6(4) . . . yes
C30 Si3 C32 107.0(3) . . . yes
N11 Si3 C30 112.5(3) . . . yes
C31 Si3 C32 106.7(3) . . . yes
C33 Si4 C35 104.8(4) . . . yes
C34 Si4 C35 105.6(4) . . . yes
C33 Si4 C34 107.3(4) . . . yes
N12 Si4 C33 111.4(3) . . . yes
N12 Si4 C34 111.9(3) . . . yes
N12 Si4 C35 115.3(4) . . . yes
C36 Si5 C37 108.0(4) . . . yes
C36 Si5 C38 105.9(4) . . . yes
C37 Si5 C38 104.2(4) . . . yes
N12 Si5 C37 113.0(3) . . . yes
N12 Si5 C38 116.4(4) . . . yes
N12 Si5 C36 108.8(3) . . . yes
Mn4 O1 Mn4 180.00 . . 3_556 yes
Mn3 O1 Mn3 180.00 . . 3_556 yes
Mn1 O1 Mn1 180.00 . . 3_556 yes
Mn2 O1 Mn2 180.00 . . 3_556 yes
Mn2 N1 C1 118.9(6) . . . yes
C1 N1 Li2 118.9(6) . . . yes
Mn2 N1 C4 116.6(5) . . . yes
C1 N1 C4 115.4(6) . . . yes
Mn4 N1 C4 108.9(6) 3_556 . . yes
Mn4 N1 C1 115.9(6) 3_556 . . yes
C4 N1 Li2 116.6(5) . . . yes
C1 N2 C2 122.3(6) . . . yes
C1 N2 C5 124.1(5) . . . yes
C2 N2 C5 113.3(6) . . . yes
C1 N3 Li3 114.9(6) . . . yes
C7 N3 Li1 111.7(6) . . . yes
C7 N3 Li3 116.1(6) . . . yes
Mn1 N3 C1 119.1(5) . . . yes
Mn1 N3 C7 111.7(6) . . . yes
Mn3 N3 C1 114.9(6) . . . yes
Mn3 N3 C7 116.1(6) . . . yes
C1 N3 C7 114.5(7) . . . yes
C1 N3 Li1 119.1(5) . . . yes
C8 N4 C14 115.0(7) . . . yes
C8 N4 Li2 115.7(6) . . . yes
Mn3 N4 C8 119.3(6) 3_556 . . yes
C14 N4 Li2 115.1(5) . . . yes
Mn3 N4 C14 110.7(5) 3_556 . . yes
Mn2 N4 C14 115.1(5) . . . yes
Mn2 N4 C8 115.7(6) . . . yes
C8 N5 C9 123.1(7) . . . yes
C9 N5 C12 114.2(7) . . . yes
C8 N5 C12 122.7(7) . . . yes
C8 N6 C11 115.4(7) . . . yes
Mn1 N6 C8 118.4(6) 3_556 . . yes
Mn1 N6 C11 118.7(6) 3_556 . . yes
Mn4 N6 C11 108.3(6) 3_556 . . yes
Mn4 N6 C8 116.1(6) 3_556 . . yes
Mn2 N7 C15 112.2(7) . . . yes
Mn2 N7 C20 117.5(7) . . . yes
C15 N7 C20 112.3(8) . . . yes
C15 N7 Li1 116.0(6) . . . yes
C15 N7 Li2 112.2(7) . . . yes
C20 N7 Li1 117.2(6) . . . yes
Mn1 N7 C15 116.0(6) . . . yes
Mn1 N7 C20 117.2(6) . . . yes
C20 N7 Li2 117.5(7) . . . yes
C19 N8 C21 115.3(11) . . . yes
C15 N8 C16 118.6(12) . . . yes
C15 N8 C19 112.4(12) . . . yes
C15 N8 C21 123.2(11) . . . yes
C16 N8 C19 64.3(12) . . . yes
C16 N8 C21 108.8(12) . . . yes
Mn4 N9 C23 113.3(7) . . . yes
C15 N9 C23 121.5(9) . . . yes
C15 N9 Li4 115.3(7) . . . yes
Mn3 N9 C15 116.5(7) 3_556 . . yes
C23 N9 Li4 113.3(7) . . . yes
Mn3 N9 C23 106.9(7) 3_556 . . yes
Mn4 N9 C15 115.3(7) . . . yes
Si1 N10 Li5 105.6(3) 2_555 . 2_555 yes
Si1 N10 Si1 121.8(4) . . 2_555 yes
Si1 N10 Li5 105.6(3) . . . yes
Li5 N10 Li5 88.4(5) . . 2_555 yes
Si1 N10 Li5 115.3(3) . . 2_555 yes
Si1 N10 Li5 115.3(3) 2_555 . . yes
Si2 N11 Li5 105.8(4) . . . yes
Si2 N11 Si3 120.0(3) . . . yes
Si3 N11 Li6 104.8(4) . . . yes
Si2 N11 Li6 117.3(4) . . . yes
Si3 N11 Li5 116.6(4) . . . yes
Li5 N11 Li6 88.4(5) . . . yes
Si4 N12 Li6 117.6(5) . . 2_555 yes
Si4 N12 Si5 120.9(3) . . . yes
Si4 N12 Li7 111.1(3) . . . yes
Li6 N12 Li7 88.0(6) 2_555 . . yes
Si5 N12 Li7 111.2(3) . . . yes
Si5 N12 Li6 103.2(4) . . 2_555 yes
N1 C1 N2 123.1(7) . . . yes
N2 C1 N3 120.4(7) . . . yes
N1 C1 N3 116.5(7) . . . yes
N2 C2 C3 112.3(6) . . . yes
C2 C3 C4 106.1(6) . . . no
N1 C4 C3 112.5(6) . . . yes
N2 C5 C6 111.2(6) . . . yes
C5 C6 C7 108.3(6) . . . no
N3 C7 C6 111.1(8) . . . yes
N5 C8 N6 120.8(7) . . . yes
N4 C8 N6 117.1(8) . . . yes
N4 C8 N5 122.0(8) . . . yes
N5 C9 C10 112.1(7) . . . yes
C9 C10 C11 107.2(9) . . . no
N6 C11 C10 112.1(8) . . . yes
N5 C12 C13 112.1(8) . . . yes
C12 C13 C14 108.1(7) . . . no
N4 C14 C13 111.3(7) . . . yes
N7 C15 N9 120.3(9) . . . yes
N8 C15 N9 121.0(12) . . . yes
N7 C15 N8 118.7(11) . . . yes
N8 C16 C17 108.8(17) . . . yes
C16 C17 C20 112(2) . . . no
C19 C18 C20 92.2(14) . . . no
N8 C19 C18 116.4(15) . . . yes
C17 C20 C18 106.1(15) . . . no
N7 C20 C18 113.7(10) . . . yes
N7 C20 C17 112.2(13) . . . yes
N8 C21 C22 114.4(13) . . . yes
C21 C22 C23 123.3(15) . . . no
N9 C23 C22 116.1(11) . . . yes
C40 C39 C43 111.0(16) . . . no
C40 C39 C41 70.8(13) . . . no
C42 C39 C43 57.8(10) . . . no
C40 C39 C42 53.2(11) . . . no
C41 C39 C42 112.0(13) 7_556 . . no
C40 C39 C41 165.0(18) . . 7_556 no
C41 C39 C42 124.0(15) . . . no
C41 C39 C43 177.7(17) . . . no
C41 C39 C41 123.9(14) . . 7_556 no
C41 C39 C43 54.3(10) 7_556 . . no
C39 C40 C41 53.8(11) . . . no
C39 C40 C42 74.5(13) . . . no
C41 C40 C42 128.3(14) . . . no
C40 C41 C43 178.6(11) . . 7_556 no
C39 C41 C43 67.8(11) 7_556 . 7_556 no
C39 C41 C40 111.5(12) 7_556 . . no
C39 C41 C40 55.4(11) . . . no
C39 C41 C39 56.2(11) . . 7_556 no
C39 C41 C43 123.9(13) . . 7_556 no
C40 C42 C43 115.2(12) . . . no
C39 C42 C40 52.3(11) . . . no
C39 C42 C43 62.9(10) . . . no
C41 C43 C42 117.3(13) 7_556 . . no
C39 C43 C42 59.3(10) . . . no
C39 C43 C41 58.0(10) . . 7_556 no
C45 C44 C48 171(2) . . 7_555 no
C46 C44 C48 128(2) . . 7_555 no
C46 C44 C47 65.2(19) . . . no
C46 C44 C48 111(2) . . . no
C48 C44 C48 120.5(15) . . 7_555 no
C47 C44 C48 171(2) . . . no
C47 C44 C48 62.7(16) . . 7_555 no
C45 C44 C47 125(2) . . . no
C45 C44 C48 51.2(15) . . . no
C45 C44 C46 60.1(18) . . . no
C44 C45 C48 81.7(18) . . . no
C44 C45 C46 60.7(18) . . . no
C46 C45 C48 142(2) . . . no
C45 C46 C47 117(2) . . . no
C44 C46 C45 59.2(18) . . . no
C44 C46 C47 58.4(18) . . . no
C44 C47 C46 56.4(16) . . . no
C44 C47 C48 65.0(15) . . 7_555 no
C46 C47 C48 122(2) . . 7_555 no
C44 C48 C45 106.4(16) 7_555 . . no
C45 C48 C47 158.1(18) . . 7_555 no
C44 C48 C47 52.3(14) 7_555 . 7_555 no
C44 C48 C45 47.1(13) . . . no
C44 C48 C44 59.5(12) . . 7_555 no
C44 C48 C47 111.2(15) . . 7_555 no
O1 Li1 N3 94.0(2) . . . yes
N3 Li1 N7 115.5(3) . . . yes
O1 Li1 N6 96.2(2) . . 3_556 yes
N3 Li1 N6 120.6(3) . . 3_556 yes
N6 Li1 N7 122.0(3) 3_556 . . yes
O1 Li1 N7 93.8(3) . . . yes
O1 Li2 N4 95.6(3) . . . yes
O1 Li2 N7 94.4(3) . . . yes
O1 Li2 N1 93.3(3) . . . yes
N4 Li2 N7 121.6(4) . . . yes
N1 Li2 N7 117.1(4) . . . yes
N1 Li2 N4 119.5(3) . . . yes
O1 Li3 N9 94.5(3) . . 3_556 yes
N3 Li3 N4 118.7(4) . . 3_556 yes
N4 Li3 N9 117.8(4) 3_556 . 3_556 yes
O1 Li3 N3 93.2(3) . . . yes
N3 Li3 N9 122.2(4) . . 3_556 yes
O1 Li3 N4 93.5(3) . . 3_556 yes
O1 Li4 N9 96.9(4) . . . yes
N1 Li4 N6 116.1(5) 3_556 . 3_556 yes
N1 Li4 N9 119.2(5) 3_556 . . yes
N6 Li4 N9 120.8(5) 3_556 . . yes
O1 Li4 N1 95.2(4) . . 3_556 yes
O1 Li4 N6 97.4(4) . . 3_556 yes
Cl1 Li5 N10 100.1(5) . . . yes
N10 Li5 N11 160.6(6) . . . yes
Cl1 Li5 N11 99.2(4) . . . yes
Cl1 Li6 N11 100.4(5) . . . yes
N11 Li6 N12 159.7(7) . . 2_555 yes
Cl1 Li6 N12 99.9(5) . . 2_555 yes
N12 Li7 N12 160.6(8) . . 2_555 yes
Cl1 Li7 N12 99.7(4) . . 2_555 yes
Cl1 Li7 N12 99.7(4) . . . 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
Li7 Cl1 Li6 N12 -0.1(3) . . 2_555 . no
Li5 Cl1 Li6 N12 179.2(6) . . . 2_555 no
Li7 Cl1 Li6 N11 -178.9(5) . . . . no
Li7 Cl1 Li6 N12 -0.1(3) . . . 2_555 no
Li5 Cl1 Li6 N11 2.2(9) 2_555 . . . no
Li6 Cl1 Li6 N11 -178.9(5) 2_555 . . . no
Li5 Cl1 Li7 N12 179.0(5) . . . . no
Li6 Cl1 Li5 N10 178.9(6) . . . . no
Li6 Cl1 Li5 N11 -0.4(4) . . . . no
Li7 Cl1 Li5 N10 180.00(1) . . . . no
Li7 Cl1 Li5 N11 0.7(8) . . . . no
Li5 Cl1 Li5 N10 0.0(4) 2_555 . . . no
Li5 Cl1 Li5 N11 -179.4(6) 2_555 . . . no
Li6 Cl1 Li5 N10 -1.7(9) 2_555 . . . no
Li6 Cl1 Li5 N11 178.9(5) 2_555 . . . no
Li5 Cl1 Li6 N11 0.5(4) . . . . no
Li6 Cl1 Li7 N12 -179.9(3) . . . . no
Li6 Cl1 Li7 N12 0.1(3) . . . 2_555 no
Li5 Cl1 Li7 N12 -1.0(5) 2_555 . . . no
Li6 Cl1 Li7 N12 0.1(3) 2_555 . . . no
Li5 Cl1 Li5 N10 0.0(4) . . 2_555 . no
Li6 Cl1 Li5 N10 -1.7(9) . . 2_555 . no
Li5 Cl1 Li7 N12 -1.0(5) . . . 2_555 no
Li6 Cl1 Li6 N12 -0.1(10) . . 2_555 . no
Li5 Cl1 Li6 N12 -179.1(5) . . 2_555 . no
C25 Si1 N10 Li5 -50.7(5) . . . . no
C26 Si1 N10 Li5 -172.3(4) . . . . no
C25 Si1 N10 Si1 83.4(3) . . . 2_555 no
C26 Si1 N10 Si1 -38.2(3) . . . 2_555 no
C24 Si1 N10 Si1 -158.7(2) . . . 2_555 no
C24 Si1 N10 Li5 67.2(4) . . . . no
C24 Si1 N10 Li5 -28.6(5) . . . 2_555 no
C25 Si1 N10 Li5 -146.5(4) . . . 2_555 no
C26 Si1 N10 Li5 92.0(5) . . . 2_555 no
C29 Si2 N11 Li6 -29.8(6) . . . . no
C28 Si2 N11 Si3 81.3(4) . . . . no
C29 Si2 N11 Si3 -158.8(3) . . . . no
C27 Si2 N11 Li5 -173.0(5) . . . . no
C29 Si2 N11 Li5 66.7(4) . . . . no
C27 Si2 N11 Li6 90.5(6) . . . . no
C28 Si2 N11 Li6 -149.7(5) . . . . no
C27 Si2 N11 Si3 -38.6(5) . . . . no
C28 Si2 N11 Li5 -53.2(5) . . . . no
C31 Si3 N11 Si2 -43.3(5) . . . . no
C32 Si3 N11 Si2 -163.4(3) . . . . no
C30 Si3 N11 Si2 78.1(4) . . . . no
C30 Si3 N11 Li5 -152.1(5) . . . . no
C31 Si3 N11 Li5 86.6(5) . . . . no
C32 Si3 N11 Li5 -33.6(5) . . . . no
C30 Si3 N11 Li6 -56.3(5) . . . . no
C31 Si3 N11 Li6 -177.7(5) . . . . no
C32 Si3 N11 Li6 62.2(5) . . . . no
C33 Si4 N12 Si5 83.0(5) . . . . no
C33 Si4 N12 Li6 -149.2(5) . . . 2_555 no
C34 Si4 N12 Li6 -29.2(6) . . . 2_555 no
C35 Si4 N12 Li6 91.5(5) . . . 2_555 no
C35 Si4 N12 Li7 -169.4(5) . . . . no
C34 Si4 N12 Si5 -157.0(4) . . . . no
C35 Si4 N12 Si5 -36.3(5) . . . . no
C33 Si4 N12 Li7 -50.1(6) . . . . no
C34 Si4 N12 Li7 70.0(5) . . . . no
C38 Si5 N12 Si4 -42.2(5) . . . . no
C36 Si5 N12 Li7 -28.6(6) . . . . no
C37 Si5 N12 Si4 78.4(5) . . . . no
C36 Si5 N12 Si4 -161.7(4) . . . . no
C36 Si5 N12 Li6 64.3(5) . . . 2_555 no
C37 Si5 N12 Li6 -55.7(6) . . . 2_555 no
C38 Si5 N12 Li6 -176.2(5) . . . 2_555 no
C38 Si5 N12 Li7 90.9(6) . . . . no
C37 Si5 N12 Li7 -148.6(6) . . . . no
Li2 O1 Li4 N1 -143.4(3) . . . 3_556 no
Li4 O1 Li2 N7 -25.3(4) . . . . no
Li4 O1 Li2 N4 97.0(4) . . . . no
Li1 O1 Li2 N7 34.0(3) . . . . no
Li3 O1 Li2 N7 95.0(3) . . . . no
Li2 O1 Li3 N3 -24.7(3) . . . . no
Li4 O1 Li3 N3 94.3(4) . . . . no
Li1 O1 Li3 N4 -81.5(3) . . . 3_556 no
Li2 O1 Li3 N4 -143.7(3) . . . 3_556 no
Li4 O1 Li3 N4 -24.7(4) . . . 3_556 no
Li1 O1 Li4 N9 -85.3(4) . . . . no
Li2 O1 Li4 N9 -23.1(4) . . . . no
Li3 O1 Li4 N9 -143.7(4) . . . . no
Li1 O1 Li4 N1 154.4(4) . . . 3_556 no
Li3 O1 Li1 N6 83.9(3) . . . 3_556 no
Li3 O1 Li4 N1 96.0(4) . . . 3_556 no
Li1 O1 Li4 N6 37.2(3) . . . 3_556 no
Li2 O1 Li4 N6 99.4(4) . . . 3_556 no
Li3 O1 Li4 N6 -21.3(5) . . . 3_556 no
Li1 O1 Li3 N3 37.5(3) . . . . no
Li4 O1 Li3 N9 -143.0(4) . . . 3_556 no
Li4 O1 Li1 N6 -38.2(4) . . . 3_556 no
Li2 O1 Li1 N3 82.4(3) . . . . no
Li3 O1 Li1 N3 -37.5(3) . . . . no
Li1 O1 Li2 N1 -83.6(3) . . . . no
Li1 O1 Li3 N9 160.2(4) . . . 3_556 no
Li2 O1 Li3 N9 98.0(3) . . . 3_556 no
Li4 O1 Li2 N1 -142.9(3) . . . . no
Li1 O1 Li2 N4 156.3(3) . . . . no
Li2 O1 Li1 N6 -156.3(3) . . . 3_556 no
Li4 O1 Li1 N7 84.6(4) . . . . no
Li4 O1 Li1 N3 -159.6(4) . . . . no
Li2 O1 Li1 N7 -33.5(3) . . . . no
Li3 O1 Li2 N1 -22.6(3) . . . . no
Li3 O1 Li1 N7 -153.3(3) . . . . no
Li3 O1 Li2 N4 -142.7(3) . . . . no
C4 N1 Li2 O1 -139.8(5) . . . . no
Li2 N1 C1 N3 -40.9(9) . . . . no
C4 N1 C1 N2 -5.6(11) . . . . no
C4 N1 Li4 N9 107.5(7) 3_556 3_556 . . no
C4 N1 C1 N3 173.2(7) . . . . no
C4 N1 Li2 N7 123.6(6) . . . . no
C1 N1 Li2 N7 -21.9(7) . . . . no
C1 N1 Li2 N4 173.1(6) . . . . no
C1 N1 Li2 O1 74.7(6) . . . . no
Li2 N1 C1 N2 140.3(6) . . . . no
C1 N1 Li4 N9 -24.5(9) 3_556 3_556 . . no
C4 N1 Li2 N4 -41.4(7) . . . . no
Li2 N1 C4 C3 -103.6(6) . . . . no
C1 N1 C4 C3 43.1(9) . . . . no
C2 N2 C5 C6 170.5(6) . . . . no
C2 N2 C1 N3 170.5(6) . . . . no
C5 N2 C1 N3 -15.9(10) . . . . no
C2 N2 C1 N1 -10.8(10) . . . . no
C1 N2 C5 C6 -3.6(9) . . . . no
C1 N2 C2 C3 -11.1(9) . . . . no
C5 N2 C2 C3 174.7(6) . . . . no
C5 N2 C1 N1 162.8(7) . . . . no
C1 N3 C7 C6 46.3(10) . . . . no
Li1 N3 C1 N1 39.3(9) . . . . no
Li1 N3 Li3 O1 -38.4(2) . . . . no
C1 N3 Li3 N4 172.9(6) . . . 3_556 no
C1 N3 Li1 O1 -71.4(6) . . . . no
C7 N3 Li3 N4 -49.8(8) . . . 3_556 no
Li1 N3 C7 C6 -174.7(6) . . . . no
Li3 N3 C1 N2 132.0(6) . . . . no
Li3 N3 Li1 N6 -60.6(4) . . . 3_556 no
C7 N3 C1 N2 -6.1(10) . . . . no
Li3 N3 C7 C6 -91.2(7) . . . . no
C7 N3 Li1 N6 52.0(7) . . . 3_556 no
C7 N3 C1 N1 175.2(7) . . . . no
C7 N3 Li1 O1 151.6(5) . . . . no
Li1 N3 Li3 N4 57.4(4) . . . 3_556 no
C1 N3 Li3 N9 -20.2(8) . . . 3_556 no
Li1 N3 C1 N2 -141.9(6) . . . . no
C1 N3 Li3 O1 77.1(6) . . . . no
Li1 N3 Li3 N9 -135.7(5) . . . 3_556 no
C1 N3 Li1 N6 -171.1(6) . . . 3_556 no
C1 N3 Li1 N7 24.7(7) . . . . no
Li3 N3 Li1 O1 39.1(3) . . . . no
C7 N3 Li3 O1 -145.6(6) . . . . no
Li3 N3 Li1 N7 135.2(4) . . . . no
Li3 N3 C1 N1 -46.8(9) . . . . no
C7 N3 Li3 N9 117.1(7) . . . 3_556 no
C7 N3 Li1 N7 -112.3(6) . . . . no
Li2 N4 C14 C13 -93.3(7) . . . . no
C14 N4 Li2 O1 -145.1(5) . . . . no
C8 N4 Li2 N7 175.6(6) . . . . no
C14 N4 C8 N6 174.3(7) . . . . no
C14 N4 Li2 N1 117.9(6) . . . . no
C8 N4 Li2 O1 76.9(6) . . . . no
Li2 N4 C8 N6 -47.7(9) . . . . no
C14 N4 Li2 N7 -46.5(7) . . . . no
C8 N4 Li2 N1 -20.1(8) . . . . no
C14 N4 Li3 N3 114.8(6) 3_556 3_556 . . no
Li2 N4 C8 N5 130.1(7) . . . . no
C8 N4 Li3 N3 -22.1(8) 3_556 3_556 . . no
C8 N4 C14 C13 45.0(9) . . . . no
C14 N4 C8 N5 -7.9(11) . . . . no
C9 N5 C8 N6 -15.2(12) . . . . no
C12 N5 C8 N4 -11.0(12) . . . . no
C8 N5 C12 C13 -8.4(11) . . . . no
C12 N5 C9 C10 172.7(8) . . . . no
C9 N5 C12 C13 173.3(7) . . . . no
C12 N5 C8 N6 166.7(7) . . . . no
C9 N5 C8 N4 167.0(7) . . . . no
C8 N5 C9 C10 -5.6(11) . . . . no
C11 N6 Li1 N3 -122.7(7) 3_556 3_556 . . no
Li4 N6 Li1 O1 37.6(3) . 3_556 . . no
Li1 N6 Li4 O1 -39.6(3) . 3_556 . . no
Li4 N6 Li1 N7 -60.8(5) . 3_556 . . no
C8 N6 Li1 N3 25.7(7) 3_556 3_556 . . no
Li4 N6 Li1 N3 136.0(4) . 3_556 . . no
C11 N6 Li4 N9 -52.0(8) 3_556 3_556 . . no
C8 N6 Li1 N7 -171.1(6) 3_556 3_556 . . no
Li1 N6 Li4 N9 63.1(6) . 3_556 . . no
C11 N6 C8 N5 -5.2(11) . . . . no
Li1 N6 Li4 N1 -139.2(6) . 3_556 . 3_556 no
C11 N6 C8 N4 172.7(7) . . . . no
C8 N6 C11 C10 44.7(11) . . . . no
C11 N6 Li1 N7 40.5(8) 3_556 3_556 . . no
C8 N6 Li4 N9 176.3(6) 3_556 3_556 . . no
Li1 N7 Li2 N1 61.0(4) . . . . no
C20 N7 Li2 O1 -149.4(6) . . . . no
C15 N7 Li2 N4 -21.1(8) . . . . no
C15 N7 Li2 N1 174.3(6) . . . . no
C15 N7 Li1 N3 -170.0(8) . . . . no
Li1 N7 Li2 N4 -134.3(4) . . . . no
Li1 N7 Li2 O1 -35.0(2) . . . . no
Li1 N7 C15 N8 -142.6(9) . . . . no
C20 N7 Li2 N1 -53.4(7) . . . . no
C15 N7 C20 C18 71.9(13) . . . . no
Li1 N7 C20 C18 -150.1(10) . . . . no
C20 N7 Li1 O1 149.8(7) . . . . no
Li1 N7 C20 C17 89.6(14) . . . . no
C20 N7 C15 N8 -4.1(14) . . . . no
Li2 N7 C20 C17 179.2(13) . . . . no
Li2 N7 C15 N8 130.9(10) . . . . no
C20 N7 C15 N9 177.7(10) . . . . no
Li2 N7 Li1 O1 35.0(2) . . . . no
Li2 N7 Li1 N6 134.8(4) . . . 3_556 no
Li2 N7 C15 N9 -47.4(12) . . . . no
C20 N7 Li2 N4 111.3(7) . . . . no
Li1 N7 C15 N9 39.2(13) . . . . no
C15 N7 C20 C17 -48.4(15) . . . . no
C20 N7 Li1 N3 53.5(8) . . . . no
C20 N7 Li1 N6 -110.5(7) . . . 3_556 no
C15 N7 Li2 O1 78.3(6) . . . . no
C15 N7 Li1 O1 -73.8(8) . . . . no
Li2 N7 C20 C18 -60.4(12) . . . . no
C15 N7 Li1 N6 26.0(9) . . . 3_556 no
Li2 N7 Li1 N3 -61.2(4) . . . . no
C19 N8 C15 N9 149.9(12) . . . . no
C21 N8 C19 C18 158.0(16) . . . . no
C19 N8 C15 N7 -28.3(16) . . . . no
C21 N8 C15 N7 -173.6(11) . . . . no
C16 N8 C15 N9 -138.2(13) . . . . no
C16 N8 C19 C18 -102.3(19) . . . . no
C16 N8 C15 N7 43.7(17) . . . . no
C19 N8 C21 C22 -152.4(15) . . . . no
C15 N8 C19 C18 10(2) . . . . no
C21 N8 C15 N9 4.6(18) . . . . no
C21 N8 C16 C17 -174.7(17) . . . . no
C16 N8 C21 C22 137.9(14) . . . . no
C19 N8 C16 C17 75.6(19) . . . . no
C15 N8 C21 C22 -8(2) . . . . no
C15 N8 C16 C17 -27(2) . . . . no
C15 N9 C23 C22 -4.5(16) . . . . no
C23 N9 Li4 N1 -40.5(9) . . . 3_556 no
C23 N9 C15 N7 -179.9(10) . . . . no
C23 N9 Li4 N6 116.6(8) . . . 3_556 no
C15 N9 Li3 N3 170.8(7) 3_556 3_556 . . no
C23 N9 Li3 N3 -49.6(8) 3_556 3_556 . . no
C15 N9 Li4 N1 173.0(8) . . . 3_556 no
Li4 N9 C15 N8 145.5(10) . . . . no
Li4 N9 C15 N7 -36.4(13) . . . . no
Li4 N9 C23 C22 -148.7(10) . . . . no
C15 N9 Li4 N6 -29.9(10) . . . 3_556 no
C15 N9 Li4 O1 73.0(8) . . . . no
C23 N9 C15 N8 1.9(16) . . . . no
C23 N9 Li4 O1 -140.5(7) . . . . no
Li5 N10 Li5 Cl1 0.0(4) 2_555 . . . no
Si1 N10 Li5 Cl1 106.6(4) 2_555 . . . no
Si1 N10 Li5 Cl1 -115.9(4) . . . . no
Li5 N11 Li6 N12 -177(2) . . . 2_555 no
Si2 N11 Li6 Cl1 106.5(5) . . . . no
Si2 N11 Li6 N12 -70(2) . . . 2_555 no
Si3 N11 Li6 Cl1 -117.6(4) . . . . no
Li6 N11 Li5 Cl1 0.5(5) . . . . no
Si3 N11 Li5 Cl1 106.3(4) . . . . no
Li5 N11 Li6 Cl1 -0.5(5) . . . . no
Si2 N11 Li5 Cl1 -117.5(4) . . . . no
Si3 N11 Li6 N12 66(2) . . . 2_555 no
Li7 N12 Li6 N11 177(2) . 2_555 . . no
Si4 N12 Li6 N11 -71(2) 2_555 2_555 . . no
Si5 N12 Li6 N11 65(2) 2_555 2_555 . . no
Si4 N12 Li7 Cl1 -119.0(3) . . . . no
Li6 N12 Li7 Cl1 -0.1(4) . 2_555 . . no
Li6 N12 Li7 Cl1 -0.1(4) 2_555 . . . no
Li7 N12 Li6 Cl1 0.1(4) . 2_555 . . no
Si5 N12 Li7 Cl1 103.2(3) . . . . no
N2 C2 C3 C4 44.1(8) . . . . no
C2 C3 C4 N1 -61.2(8) . . . . no
N2 C5 C6 C7 41.7(9) . . . . no
C5 C6 C7 N3 -63.7(9) . . . . no
N5 C9 C10 C11 41.6(10) . . . . no
C9 C10 C11 N6 -62.4(10) . . . . no
N5 C12 C13 C14 43.0(10) . . . . no
C12 C13 C14 N4 -62.2(9) . . . . no
N8 C16 C17 C20 -23(2) . . . . no
C16 C17 C20 C18 -62(2) . . . . no
C16 C17 C20 N7 63(2) . . . . no
C19 C18 C20 N7 -79.8(15) . . . . no
C20 C18 C19 N8 36.9(18) . . . . no
C19 C18 C20 C17 43.9(17) . . . . no
N8 C21 C22 C23 5(2) . . . . no
C21 C22 C23 N9 1(2) . . . . no
C41 C39 C40 C42 -179.9(12) . . . . no
C42 C39 C40 C41 179.9(12) . . . . no
C43 C39 C40 C41 -178.4(17) . . . . no
C43 C39 C40 C42 1.7(13) . . . . no
C40 C39 C41 C39 -176.6(15) . . . 7_556 no
C40 C39 C41 C43 -178.5(13) . . . 7_556 no
C42 C39 C41 C40 -0.1(12) . . . . no
C42 C39 C41 C39 -177(2) . . . 7_556 no
C42 C39 C41 C43 -178.5(13) . . . 7_556 no
C41 C39 C41 C40 177(2) 7_556 . . . no
C41 C39 C41 C39 0.0(12) 7_556 . . 7_556 no
C41 C39 C41 C43 -2(2) 7_556 . . 7_556 no
C40 C39 C42 C43 178.2(15) . . . . no
C41 C39 C42 C40 0.1(14) . . . . no
C41 C39 C42 C43 178.3(19) . . . . no
C43 C39 C42 C40 -178.2(15) . . . . no
C41 C39 C42 C40 -176.9(17) 7_556 . . . no
C41 C39 C42 C43 1.3(11) 7_556 . . . no
C40 C39 C43 C42 -1.6(13) . . . . no
C40 C39 C43 C41 177.0(17) . . . 7_556 no
C42 C39 C43 C41 178.6(12) . . . 7_556 no
C41 C39 C43 C42 -178.6(12) 7_556 . . . no
C41 C39 C41 C43 -178.3(19) . . 7_556 . no
C41 C39 C41 C39 0.0(15) . . 7_556 7_556 no
C41 C39 C41 C40 3.0(19) . . 7_556 7_556 no
C42 C39 C41 C43 -1.3(11) . . 7_556 . no
C42 C39 C41 C39 177.0(17) . . 7_556 7_556 no
C42 C39 C41 C40 -180.0(11) . . 7_556 7_556 no
C43 C39 C41 C39 178.3(15) . . 7_556 7_556 no
C43 C39 C41 C40 -178.7(12) . . 7_556 7_556 no
C39 C40 C41 C39 3.1(14) . . . 7_556 no
C42 C40 C41 C39 0.1(15) . . . . no
C42 C40 C41 C39 3.1(19) . . . 7_556 no
C39 C40 C42 C43 -1.8(14) . . . . no
C41 C40 C42 C39 -0.1(13) . . . . no
C41 C40 C42 C43 -2(2) . . . . no
C39 C41 C43 C39 1.7(15) . . 7_556 7_556 no
C39 C41 C43 C42 0(2) . . 7_556 7_556 no
C39 C42 C43 C41 -1.4(12) . . . 7_556 no
C40 C42 C43 C39 1.6(13) . . . . no
C40 C42 C43 C41 0.2(18) . . . 7_556 no
C46 C44 C45 C48 -178(2) . . . . no
C47 C44 C45 C46 7(3) . . . . no
C47 C44 C45 C48 -170(2) . . . . no
C48 C44 C45 C46 178(2) . . . . no
C45 C44 C46 C47 173(2) . . . . no
C47 C44 C46 C45 -173(2) . . . . no
C48 C44 C46 C45 -2.1(18) . . . . no
C48 C44 C46 C47 171(2) . . . . no
C48 C44 C46 C45 -175(3) 7_555 . . . no
C48 C44 C46 C47 -1(2) 7_555 . . . no
C45 C44 C47 C46 -7(2) . . . . no
C45 C44 C47 C48 174(3) . . . 7_555 no
C46 C44 C47 C48 -179(2) . . . 7_555 no
C48 C44 C47 C46 179(2) 7_555 . . . no
C45 C44 C48 C44 -176(2) . . . 7_555 no
C45 C44 C48 C47 177(2) . . . 7_555 no
C46 C44 C48 C45 2(2) . . . . no
C46 C44 C48 C44 -173(2) . . . 7_555 no
C46 C44 C48 C47 179(2) . . . 7_555 no
C48 C44 C48 C45 176(3) 7_555 . . . no
C48 C44 C48 C44 0.0(17) 7_555 . . 7_555 no
C48 C44 C48 C47 -8(2) 7_555 . . 7_555 no
C46 C44 C48 C47 1(2) . . 7_555 . no
C46 C44 C48 C44 172(3) . . 7_555 7_555 no
C46 C44 C48 C45 175(2) . . 7_555 7_555 no
C47 C44 C48 C44 170.7(19) . . 7_555 7_555 no
C47 C44 C48 C45 174(2) . . 7_555 7_555 no
C48 C44 C48 C47 -171(2) . . 7_555 . no
C48 C44 C48 C44 0.0(15) . . 7_555 7_555 no
C48 C44 C48 C45 4(2) . . 7_555 7_555 no
C44 C45 C46 C47 -6(2) . . . . no
C48 C45 C46 C44 4(4) . . . . no
C48 C45 C46 C47 -2(5) . . . . no
C44 C45 C48 C44 4(2) . . . 7_555 no
C44 C45 C48 C47 -8(5) . . . 7_555 no
C46 C45 C48 C44 -4(3) . . . . no
C46 C45 C48 C44 1(4) . . . 7_555 no
C46 C45 C48 C47 -12(7) . . . 7_555 no
C44 C46 C47 C48 1(2) . . . 7_555 no
C45 C46 C47 C44 6(2) . . . . no
C45 C46 C47 C48 7(3) . . . 7_555 no
C44 C47 C48 C44 -8.6(18) . . 7_555 7_555 no
C44 C47 C48 C45 -15(5) . . 7_555 7_555 no
C46 C47 C48 C44 -1.0(19) . . 7_555 . no
C46 C47 C48 C44 -10(3) . . 7_555 7_555 no
C46 C47 C48 C45 -16(6) . . 7_555 7_555 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
Mn1 H17B 3.3700 . . no
Mn2 H13B 3.3700 . . no
Mn2 H18B 2.8600 . . no
Mn3 H6B 3.3800 . . no
Cl1 N12 3.465(6) . . no
Cl1 N11 3.437(6) . 2_555 no
Cl1 N12 3.465(6) . 2_555 no
Cl1 N10 3.449(8) . . no
Cl1 N11 3.437(6) . . no
Si1 H26B 3.3200 . 2_555 no
Si1 H28B 3.3900 . 2_555 no
Si2 H31B 3.3800 . . no
Si2 H37B 3.3500 . 2_555 no
Si3 H27B 3.3200 . . no
Si3 H25B 3.3200 . . no
Si4 H38B 3.4000 . . no
Si4 H30B 3.4100 . 2_555 no
Si4 H36B 3.4800 . 2_555 no
Si5 H35B 3.3300 . . no
O1 N1 3.074(7) . . no
O1 N3 3.094(6) . . no
O1 N4 3.093(7) . . no
O1 N6 3.098(7) . . no
O1 N7 3.078(8) . . no
O1 N9 3.100(7) . . no
O1 Mn2 2.162(4) . . no
O1 Mn3 2.192(7) . . no
O1 Mn4 2.072(10) . . no
O1 N1 3.074(7) . 3_556 no
O1 N3 3.094(6) . 3_556 no
O1 N4 3.093(7) . 3_556 no
O1 N6 3.098(7) . 3_556 no
O1 Mn3 2.192(7) . 3_556 no
O1 Mn4 2.072(10) . 3_556 no
O1 Mn1 2.159(4) . 3_556 no
O1 N7 3.078(8) . 3_556 no
O1 N9 3.100(7) . 3_556 no
O1 Mn2 2.162(4) . 3_556 no
N1 Mn1 3.199(8) . . no
N1 Mn4 2.091(11) . 3_556 no
N1 O1 3.074(7) . . no
N1 Mn1 3.199(8) . . no
N1 Mn3 3.156(10) . . no
N1 Mn3 3.156(10) . . no
N3 Mn2 3.187(8) . . no
N3 Mn3 2.067(9) . . no
N3 O1 3.094(6) . . no
N3 Mn4 3.161(11) . 3_556 no
N3 Mn4 3.161(11) . 3_556 no
N3 Mn2 3.187(8) . . no
N4 Mn4 3.147(12) . 3_556 no
N4 Mn1 3.115(8) . 3_556 no
N4 O1 3.093(7) . . no
N4 Mn1 3.115(8) . 3_556 no
N4 Mn4 3.147(12) . 3_556 no
N4 Mn3 2.052(9) . 3_556 no
N6 O1 3.098(7) . . no
N7 Mn2 2.033(9) . . no
N7 Mn4 3.077(12) . . no
N7 Mn3 3.160(10) . 3_556 no
N7 O1 3.078(8) . . no
N7 Mn4 3.077(12) . . no
N7 Mn3 3.160(10) . 3_556 no
N9 Mn2 3.094(9) . . no
N9 O1 3.100(7) . . no
N9 Mn2 3.094(9) . . no
N9 Mn3 2.027(9) . 3_556 no
N9 Mn1 3.139(9) . . no
N9 Mn1 3.139(9) . . no
N10 Cl1 3.449(8) . . no
N11 Cl1 3.437(6) . . no
N12 Cl1 3.465(6) . . no
N2 H7B 2.8300 . . no
N2 H4A 2.9100 . . no
N5 H11A 2.8500 . . no
N5 H14A 2.8800 . . no
C17 C48 3.50(3) . 6_545 no
C48 C17 3.50(3) . 6_555 no
C1 H6B 2.9600 . . no
C1 H3B 2.9700 . . no
C8 H10B 2.9600 . . no
C8 H13B 2.9600 . . no
C8 H4B 3.0200 . . no
C15 H17B 2.9700 . . no
C15 H14B 3.0500 . . no
C15 H18B 3.0800 . . no
C19 H17A 2.5300 . . no
C24 H5A 3.0300 . 7_556 no
C24 H32B 2.9800 . . no
C24 H29B 3.0200 . 2_555 no
C25 H31C 3.0100 . . no
C26 H26B 3.0800 . 2_555 no
C27 H5B 2.9800 . 6_555 no
C27 H30C 2.9700 . . no
C29 H36C 2.9500 . 2_555 no
C29 H24B 2.9800 . 2_555 no
C30 H34B 3.0600 . 2_555 no
C31 H25B 2.9900 . . no
C31 H17A 2.8300 . 6_555 no
C31 H28C 3.0300 . . no
C32 H34B 3.0500 . 2_555 no
C32 H6B 3.0400 . 7_556 no
C32 H24C 3.0900 . . no
C34 H36B 2.9800 . 2_555 no
C34 H32C 3.0000 . 2_555 no
C35 H37C 3.0500 . . no
C36 H34C 2.9900 . 2_555 no
C36 H29A 3.0700 . 2_555 no
C36 H6A 3.0800 . 7_556 no
C37 H29A 3.0100 . 2_555 no
C38 H33C 3.0400 . . no
C38 H16A 2.9200 . 1_565 no
C39 H2B 2.8500 . . no
C40 H4A 3.0800 . 7_556 no
C41 H24A 2.9500 . 7_556 no
C41 H2B 3.0300 . 7_556 no
C42 H2B 3.0500 . . no
C43 H2B 2.9400 . . no
C44 H10B 2.9900 . 8_554 no
C44 H10A 2.9800 . 2_555 no
C47 H10B 2.9700 . 8_554 no
C48 H17B 2.7800 . 6_555 no
Li5 H24C 3.1000 . 2_555 no
Li5 H28B 2.8900 . . no
Li5 H29B 3.0700 . . no
Li5 H24B 3.1900 . 2_555 no
Li5 H25B 2.9500 . . no
Li5 H32B 3.1600 . . no
Li5 H24C 3.0400 . . no
Li6 H37B 2.8800 . 2_555 no
Li6 H30B 2.9500 . . no
Li6 H29B 3.1600 . . no
Li6 H36C 2.9200 . 2_555 no
Li6 H32C 2.9100 . . no
Li7 H36B 2.9300 . . no
Li7 H36C 3.0700 . 2_555 no
Li7 H33B 3.1300 . . no
Li7 H36B 2.9300 . 2_555 no
Li7 H36C 3.0700 . . no
Li7 H33B 3.1300 . 2_555 no
H2A H5B 2.5000 . . no
H2B C39 2.8500 . . no
H2B C41 3.0300 . 7_556 no
H2B C42 3.0500 . . no
H2B H4A 2.5400 . . no
H2B H5A 2.4400 . . no
H2B C43 2.9400 . . no
H3B C1 2.9700 . . no
H4A N2 2.9100 . . no
H4A H2B 2.5400 . . no
H4A C40 3.0800 . 7_556 no
H4B C8 3.0200 . . no
H5A C24 3.0300 . 7_556 no
H5A H2B 2.4400 . . no
H5B C27 2.9800 . 6_545 no
H5B H2A 2.5000 . . no
H5B H7B 2.5500 . . no
H5B H27C 2.3600 . 6_545 no
H6A C36 3.0800 . 7_556 no
H6A H36C 2.5800 . 7_556 no
H6B Mn3 3.3800 . . no
H6B C1 2.9600 . . no
H6B H23A 2.5200 . 3_556 no
H6B C32 3.0400 . 7_556 no
H7B H5B 2.5500 . . no
H7B N2 2.8300 . . no
H9A H12B 2.4700 . . no
H9B H12A 2.4800 . . no
H9B H26C 2.5000 . . no
H9B H25C 2.5700 . 2_555 no
H9B H11A 2.5500 . . no
H10A C44 2.9800 . 2_555 no
H10B C8 2.9600 . . no
H10B C44 2.9900 . 8_455 no
H10B C47 2.9700 . 8_455 no
H11A H9B 2.5500 . . no
H11A N5 2.8500 . . no
H12A H9B 2.4800 . . no
H12B H9A 2.4700 . . no
H12B H35A 2.4900 . 6_445 no
H12B H14A 2.5500 . . no
H13B Mn2 3.3700 . . no
H13B C8 2.9600 . . no
H14A H12B 2.5500 . . no
H14A N5 2.8800 . . no
H14B C15 3.0500 . . no
H14B H18B 2.5800 . . no
H16A C38 2.9200 . 1_545 no
H16A H21B 2.2100 . . no
H16A H38C 2.3500 . 1_545 no
H16B H21B 2.5100 . . no
H17A H31A 2.3800 . 6_545 no
H17A C19 2.5300 . . no
H17A H18A 2.4700 . . no
H17A H19A 2.0200 . . no
H17A C31 2.8300 . 6_545 no
H17A H31B 2.4400 . 6_545 no
H17B C48 2.7800 . 6_545 no
H17B C15 2.9700 . . no
H17B Mn1 3.3700 . . no
H18A H17A 2.4700 . . no
H18A H30A 2.4200 . 6_545 no
H18B C15 3.0800 . . no
H18B Mn2 2.8600 . . no
H18B H14B 2.5800 . . no
H19A H17A 2.0200 . . no
H19A H20D 2.1100 . . no
H19A H21A 2.3800 . 2_555 no
H19B H21A 2.3900 . . no
H20D H19A 2.1100 . . no
H21A H19A 2.3800 . 2_555 no
H21A H19B 2.3900 . . no
H21B H16B 2.5100 . . no
H21B H33C 2.5600 . 1_545 no
H21B H16A 2.2100 . . no
H23A H6B 2.5200 . 3_556 no
H24A C41 2.9500 . 7_556 no
H24B Li5 3.1900 . 2_555 no
H24B H28B 2.5000 . 2_555 no
H24B H29B 2.5000 . 2_555 no
H24B C29 2.9800 . 2_555 no
H24C C32 3.0900 . . no
H24C Li5 3.1000 . 2_555 no
H24C Li5 3.0400 . . no
H24C H32B 2.4200 . . no
H25B Si3 3.3200 . . no
H25B H31C 2.2000 . . no
H25B C31 2.9900 . . no
H25B Li5 2.9500 . . no
H25B H32B 2.3900 . . no
H25C H9B 2.5700 . 2_555 no
H26B C26 3.0800 . 2_555 no
H26B H26B 2.2900 . 2_555 no
H26B Si1 3.3200 . 2_555 no
H26C H28B 2.3200 . 2_555 no
H26C H9B 2.5000 . . no
H27A H36A 2.4100 . 4_564 no
H27B Si3 3.3200 . . no
H27B H31B 2.4100 . . no
H27C H5B 2.3600 . 6_555 no
H27C H30C 2.5700 . . no
H27C H37B 2.3100 . 2_555 no
H28B Li5 2.8900 . . no
H28B Si1 3.3900 . 2_555 no
H28B H24B 2.5000 . 2_555 no
H28B H26C 2.3200 . 2_555 no
H28C C31 3.0300 . . no
H29A H36C 2.5600 . 2_555 no
H29A C36 3.0700 . 2_555 no
H29A H37B 2.4800 . 2_555 no
H29A C37 3.0100 . 2_555 no
H29B Li5 3.0700 . . no
H29B Li6 3.1600 . . no
H29B H24B 2.5000 . 2_555 no
H29B H36C 2.4700 . 2_555 no
H29B C24 3.0200 . 2_555 no
H29C H37A 2.4200 . 4_564 no
H30A H18A 2.4200 . 6_555 no
H30B Li6 2.9500 . . no
H30B Si4 3.4100 . 2_555 no
H30B H35C 2.4200 . 2_555 no
H30B H34B 2.4300 . 2_555 no
H30C C27 2.9700 . . no
H30C H27C 2.5700 . . no
H31A H17A 2.3800 . 6_555 no
H31B H27B 2.4100 . . no
H31B H17A 2.4400 . 6_555 no
H31B Si2 3.3800 . . no
H31C C25 3.0100 . . no
H31C H25B 2.2000 . . no
H32B H25B 2.3900 . . no
H32B C24 2.9800 . . no
H32B Li5 3.1600 . . no
H32B H24C 2.4200 . . no
H32C Li6 2.9100 . . no
H32C C34 3.0000 . 2_555 no
H32C H34B 2.4900 . 2_555 no
H33B H38C 2.3000 . 2_555 no
H33B Li7 3.1300 . . no
H33B H36B 2.4400 . 2_555 no
H33C H21B 2.5600 . 1_565 no
H33C H38C 2.5600 . . no
H33C C38 3.0400 . . no
H34B C30 3.0600 . 2_555 no
H34B C32 3.0500 . 2_555 no
H34B H32C 2.4900 . 2_555 no
H34B H30B 2.4300 . 2_555 no
H34C H36B 2.2500 . 2_555 no
H34C C36 2.9900 . 2_555 no
H35A H12B 2.4900 . 6_455 no
H35B H38B 2.3500 . . no
H35B Si5 3.3300 . . no
H35C H30B 2.4200 . 2_555 no
H36A H27A 2.4100 . 4_565 no
H36B H33B 2.4400 . 2_555 no
H36B C34 2.9800 . 2_555 no
H36B Li7 2.9300 . . no
H36B H34C 2.2500 . 2_555 no
H36B Si4 3.4800 . 2_555 no
H36C Li7 3.0700 . . no
H36C C29 2.9500 . 2_555 no
H36C H6A 2.5800 . 7_556 no
H36C Li6 2.9200 . 2_555 no
H36C H29A 2.5600 . 2_555 no
H36C H29B 2.4700 . 2_555 no
H37A H29C 2.4200 . 4_565 no
H37B Si2 3.3500 . 2_555 no
H37B Li6 2.8800 . 2_555 no
H37B H27C 2.3100 . 2_555 no
H37B H29A 2.4800 . 2_555 no
H37C C35 3.0500 . . no
H38B H35B 2.3500 . . no
H38B Si4 3.4000 . . no
H38C H33C 2.5600 . . no
H38C H33B 2.3000 . 2_555 no
H38C H16A 2.3500 . 1_565 no
_vrf_PLAT022_oral145
;
PROBLEM: Ratio Unique / Expected Reflections (too) Low .. 0.81
RESPONSE: The crystals were only poorly diffracting, hence reflections could
only be observed to a resolution of 1 Angstrom.
;
_vrf_PLAT027_oral145
;
PROBLEM: _diffrn_reflns_theta_full (too) Low ............ 21.00 Deg.
RESPONSE: The crystals were only poorly diffracting, hence reflections could
only be observed to a resolution of 1 Angstrom.
;
#===END
# Attachment '- oral149_mb.cif'
data_oral149
_database_code_depnum_ccdc_archive 'CCDC 827194'
#TrackingRef '- oral149_mb.cif'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_publ_section_exptl_refinement
;
Several constraints and restraints have been applied to the disordered
positions.
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C42 H72 Li7 N18 O Zn, C18 H54 N3 Si6 Zn '
_chemical_formula_sum 'C60 H126 Li7 N21 O Si6 Zn2'
_chemical_formula_weight 1505.68
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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting Orthorhombic
_symmetry_space_group_name_Hall 'P 2 -2ab'
_symmetry_space_group_name_H-M 'P b a 2'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z'
_cell_length_a 27.7860(13)
_cell_length_b 24.4230(11)
_cell_length_c 12.1310(7)
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_volume 8232.3(7)
_cell_formula_units_Z 4
_cell_measurement_temperature 100(2)
_cell_measurement_reflns_used 5732
_cell_measurement_theta_min 2.8829
_cell_measurement_theta_max 23.8998
_exptl_crystal_description block
_exptl_crystal_colour colourless
_exptl_crystal_size_max 0.1
_exptl_crystal_size_mid 0.1
_exptl_crystal_size_min 0.05
_exptl_crystal_density_diffrn 1.215
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 3224
_exptl_absorpt_coefficient_mu 0.720
_exptl_absorpt_correction_T_min 0.78454
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov 6 2009,16:24:50)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 100
_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 'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method '\w scans'
_diffrn_detector_area_resol_mean 8.3367
_diffrn_reflns_number 33772
_diffrn_reflns_av_R_equivalents 0.1008
_diffrn_reflns_av_sigmaI/netI 0.2480
_diffrn_reflns_limit_h_min -30
_diffrn_reflns_limit_h_max 22
_diffrn_reflns_limit_k_min -25
_diffrn_reflns_limit_k_max 27
_diffrn_reflns_limit_l_min -12
_diffrn_reflns_limit_l_max 13
_diffrn_reflns_theta_min 2.89
_diffrn_reflns_theta_max 23.25
_reflns_number_total 10107
_reflns_number_gt 4346
_reflns_threshold_expression >2\s(I)
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov 6 2009,16:24:50)
;
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov 6 2009,16:24:50)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov 6 2009,16:24:50)
;
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics ?
_computing_publication_material ?
_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^ > 2\s(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^)+(0.0485P)^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 constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack 0.013(19)
_refine_ls_number_reflns 10107
_refine_ls_number_parameters 937
_refine_ls_number_restraints 199
_refine_ls_R_factor_all 0.1317
_refine_ls_R_factor_gt 0.0481
_refine_ls_wR_factor_ref 0.1268
_refine_ls_wR_factor_gt 0.1150
_refine_ls_goodness_of_fit_ref 0.876
_refine_ls_restrained_S_all 0.877
_refine_ls_shift/su_max 0.002
_refine_ls_shift/su_mean 0.000
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
Zn9 Zn 0.50229(3) 0.23201(3) 0.47257(8) 0.0460(2) Uani 1 1 d . . .
Si1 Si 0.47794(7) 0.35823(8) 0.44183(18) 0.0464(7) Uani 1 1 d . . .
Zn1 Zn 0.32702(7) 0.50689(8) 0.09360(17) 0.0216(6) Uani 0.31 1 d P A 1
Zn2 Zn 0.3077(2) 0.5953(2) 0.0383(5) 0.0209(19) Uani 0.05 1 d P A 1
Zn3 Zn 0.23028(8) 0.57647(10) 0.0960(2) 0.0269(8) Uani 0.25 1 d P A 1
Zn4 Zn 0.24890(14) 0.48408(17) 0.1400(3) 0.0181(12) Uani 0.11 1 d PU A 1
Zn5 Zn 0.30882(12) 0.47365(14) -0.0954(3) 0.0205(11) Uani 0.14 1 d P A 1
Zn6 Zn 0.29063(17) 0.5627(2) -0.1416(5) 0.0178(16) Uani 0.07 1 d P A 1
Zn7 Zn 0.2114(3) 0.5468(3) -0.0814(7) 0.014(2) Uani 0.01 1 d PU A 1
Zn8 Zn 0.22998(18) 0.4600(2) -0.0324(6) 0.0260(18) Uani 0.06 1 d P A 1
Li1 Li 0.32702(7) 0.50689(8) 0.09360(17) 0.0216(6) Uani 0.69 1 d P A 2
Li2 Li 0.3077(2) 0.5953(2) 0.0383(5) 0.0209(19) Uani 0.95 1 d P A 2
Li3 Li 0.23028(8) 0.57647(10) 0.0960(2) 0.0269(8) Uani 0.75 1 d P A 2
Li4 Li 0.24890(14) 0.48408(17) 0.1400(3) 0.0181(12) Uani 0.89 1 d PU A 2
Li5 Li 0.30882(12) 0.47365(14) -0.0954(3) 0.0205(11) Uani 0.86 1 d P A 2
Li6 Li 0.29063(17) 0.5627(2) -0.1416(5) 0.0178(16) Uani 0.93 1 d P A 2
Li7 Li 0.2114(3) 0.5468(3) -0.0814(7) 0.014(2) Uani 0.99 1 d PU A 2
Li8 Li 0.22998(18) 0.4600(2) -0.0324(6) 0.0260(18) Uani 0.94 1 d P A 2
C38 C 0.2617(3) 0.3798(3) -0.3406(7) 0.084(3) Uani 1 1 d . . .
H38A H 0.2586 0.3410 -0.3556 0.101 Uiso 1 1 calc R . .
H38B H 0.2940 0.3909 -0.3609 0.101 Uiso 1 1 calc R . .
Si2 Si 0.40359(8) 0.28643(9) 0.5439(2) 0.0521(7) Uani 1 1 d . . .
Si4 Si 0.51162(8) 0.11640(8) 0.5909(2) 0.0533(7) Uani 1 1 d . . .
Si5 Si 0.59059(8) 0.20152(10) 0.3182(3) 0.0789(10) Uani 1 1 d . . .
Si6 Si 0.49399(8) 0.21176(9) 0.21681(19) 0.0538(7) Uani 1 1 d . . .
Si3 Si 0.53544(11) 0.21659(10) 0.7176(2) 0.0879(10) Uani 1 1 d . . .
N19 N 0.53018(17) 0.2143(2) 0.3281(5) 0.0431(19) Uani 1 1 d . E .
N3 N 0.32126(19) 0.3390(2) 0.0988(5) 0.0471(19) Uani 1 1 d . . .
N18 N 0.3050(2) 0.5875(2) 0.3804(5) 0.0434(19) Uani 1 1 d . . .
O1 O 0.26957(15) 0.52546(16) 0.0042(4) 0.0388(15) Uani 1 1 d . . .
C40 C 0.1908(3) 0.4998(3) -0.4406(6) 0.065(3) Uani 1 1 d . A .
H40A H 0.1619 0.4799 -0.4607 0.078 Uiso 1 1 calc R . .
H40B H 0.2083 0.5082 -0.5077 0.078 Uiso 1 1 calc R . .
N6 N 0.43617(18) 0.5621(2) -0.1056(5) 0.0418(19) Uani 1 1 d . . .
N21 N 0.5182(2) 0.1855(2) 0.6017(5) 0.0507(19) Uani 1 1 d . . .
N13 N 0.16381(17) 0.4886(2) -0.0113(5) 0.0505(19) Uani 1 1 d . . .
N5 N 0.37381(19) 0.5633(2) 0.0308(5) 0.0451(19) Uani 1 1 d . . .
N7 N 0.2565(2) 0.4490(2) -0.1933(5) 0.049(2) Uani 1 1 d . . .
N2 N 0.33720(18) 0.4282(2) 0.0353(5) 0.052(2) Uani 1 1 d . . .
C4 C 0.2928(3) 0.3000(3) 0.1589(7) 0.068(3) Uani 1 1 d . A .
H4A H 0.3123 0.2828 0.2153 0.082 Uiso 1 1 calc R . .
H4B H 0.2815 0.2717 0.1091 0.082 Uiso 1 1 calc R . .
C2 C 0.2263(2) 0.3654(3) 0.1274(6) 0.056(3) Uani 1 1 d . A .
H2A H 0.2159 0.3438 0.0646 0.068 Uiso 1 1 calc R . .
H2B H 0.1981 0.3828 0.1592 0.068 Uiso 1 1 calc R . .
N4 N 0.35826(19) 0.5327(2) -0.1466(5) 0.0421(19) Uani 1 1 d . . .
N20 N 0.45931(18) 0.2963(2) 0.4847(5) 0.0460(19) Uani 1 1 d . . .
N9 N 0.2205(2) 0.4660(2) -0.3693(5) 0.046(2) Uani 1 1 d . . .
N15 N 0.1836(2) 0.5205(2) 0.1603(5) 0.054(2) Uani 1 1 d . . .
N17 N 0.3034(2) 0.5176(2) 0.2488(5) 0.047(2) Uani 1 1 d . . .
C41 C 0.1769(3) 0.5530(3) -0.3824(7) 0.080(3) Uani 1 1 d . . .
H41A H 0.1666 0.5799 -0.4363 0.096 Uiso 1 1 calc R A .
H41B H 0.1503 0.5463 -0.3322 0.096 Uiso 1 1 calc R . .
C10 C 0.4113(3) 0.5575(3) -0.2979(7) 0.063(3) Uani 1 1 d . . .
H10A H 0.4232 0.5461 -0.3696 0.076 Uiso 1 1 calc R A .
H10B H 0.3947 0.5921 -0.3065 0.076 Uiso 1 1 calc R . .
N1 N 0.26049(18) 0.4075(2) 0.0909(6) 0.052(2) Uani 1 1 d . . .
N16 N 0.2799(2) 0.6047(2) 0.1992(5) 0.058(2) Uani 1 1 d . . .
N8 N 0.2353(2) 0.5355(2) -0.2400(5) 0.055(2) Uani 1 1 d . . .
C11 C 0.4523(3) 0.5638(3) -0.2199(6) 0.056(3) Uani 1 1 d . A .
H11A H 0.4755 0.5347 -0.2323 0.067 Uiso 1 1 calc R . .
H11B H 0.4683 0.5985 -0.2337 0.067 Uiso 1 1 calc R . .
C56 C 0.4461(2) 0.3848(3) 0.3145(6) 0.050(2) Uani 1 1 d . . .
H56A H 0.4120 0.3831 0.3256 0.075 Uiso 1 1 calc R . .
H56B H 0.4548 0.3627 0.2522 0.075 Uiso 1 1 calc R . .
H56C H 0.4556 0.4221 0.3014 0.075 Uiso 1 1 calc R . .
C47 C 0.6054(3) 0.1270(3) 0.3021(7) 0.080(3) Uani 1 1 d U E .
H47A H 0.5950 0.1146 0.2309 0.120 Uiso 1 1 calc R . .
H47B H 0.5893 0.1063 0.3584 0.120 Uiso 1 1 calc R . .
H47C H 0.6396 0.1219 0.3088 0.120 Uiso 1 1 calc R . .
C21 C 0.3185(2) 0.4802(3) 0.3316(6) 0.047(3) Uani 1 1 d . A .
H21A H 0.3326 0.4482 0.2970 0.057 Uiso 1 1 calc R . .
H21B H 0.2908 0.4683 0.3738 0.057 Uiso 1 1 calc R . .
C1 C 0.3059(3) 0.3915(3) 0.0767(6) 0.043(2) Uani 1 1 d . A .
C43 C 0.4291(2) 0.2091(3) 0.2562(6) 0.048(3) Uani 1 1 d . E .
H43A H 0.4210 0.2412 0.2980 0.072 Uiso 1 1 calc R . .
H43B H 0.4233 0.1771 0.3001 0.072 Uiso 1 1 calc R . .
H43C H 0.4097 0.2077 0.1909 0.072 Uiso 1 1 calc R . .
C44 C 0.5050(3) 0.1497(3) 0.1299(6) 0.067(3) Uani 1 1 d . E .
H44A H 0.5373 0.1508 0.1017 0.100 Uiso 1 1 calc R . .
H44B H 0.4826 0.1492 0.0696 0.100 Uiso 1 1 calc R . .
H44C H 0.5008 0.1174 0.1738 0.100 Uiso 1 1 calc R . .
C12 C 0.4736(2) 0.5767(3) -0.0268(8) 0.071(3) Uani 1 1 d . A .
H12A H 0.4817 0.6151 -0.0361 0.085 Uiso 1 1 calc R . .
H12B H 0.5022 0.5553 -0.0420 0.085 Uiso 1 1 calc R . .
C8 C 0.3893(3) 0.5533(3) -0.0718(7) 0.039(2) Uani 1 1 d . A .
C57 C 0.4678(3) 0.4144(3) 0.5427(6) 0.068(3) Uani 1 1 d . . .
H57A H 0.4339 0.4219 0.5478 0.101 Uiso 1 1 calc R . .
H57B H 0.4844 0.4467 0.5187 0.101 Uiso 1 1 calc R . .
H57C H 0.4797 0.4035 0.6137 0.101 Uiso 1 1 calc R . .
C15 C 0.2966(2) 0.5701(3) 0.2774(6) 0.038(2) Uani 1 1 d . A .
C5 C 0.3700(3) 0.3203(3) 0.0757(7) 0.067(3) Uani 1 1 d . A .
H5A H 0.3691 0.2827 0.0498 0.080 Uiso 1 1 calc R B 2
H5B H 0.3890 0.3213 0.1428 0.080 Uiso 1 1 calc R B 2
C51 C 0.4801(2) 0.0953(3) 0.4607(7) 0.064(3) Uani 1 1 d . . .
H51A H 0.4467 0.1051 0.4654 0.097 Uiso 1 1 calc R . .
H51B H 0.4830 0.0565 0.4511 0.097 Uiso 1 1 calc R . .
H51C H 0.4945 0.1137 0.3990 0.097 Uiso 1 1 calc R . .
C17 C 0.2570(3) 0.6698(3) 0.3458(7) 0.079(3) Uani 1 1 d . . .
H17A H 0.2253 0.6536 0.3541 0.095 Uiso 1 1 calc R A .
H17B H 0.2549 0.7084 0.3638 0.095 Uiso 1 1 calc R . .
C9 C 0.3773(3) 0.5148(3) -0.2526(6) 0.070(3) Uani 1 1 d . A .
H9A H 0.3510 0.5091 -0.3040 0.084 Uiso 1 1 calc R . .
H9B H 0.3941 0.4803 -0.2437 0.084 Uiso 1 1 calc R . .
C7 C 0.3880(2) 0.4124(3) 0.0215(7) 0.060(3) Uani 1 1 d . A .
H7A H 0.4027 0.4356 -0.0341 0.072 Uiso 1 1 calc R . .
H7B H 0.4050 0.4184 0.0904 0.072 Uiso 1 1 calc R . .
C33 C 0.0639(3) 0.4927(3) 0.0407(7) 0.075(3) Uani 1 1 d U . .
H33A H 0.0514 0.5264 0.0095 0.090 Uiso 0.50 1 calc PR C 1
H33B H 0.0378 0.4745 0.0791 0.090 Uiso 0.50 1 calc PR C 1
H33C H 0.0384 0.5196 0.0468 0.090 Uiso 0.50 1 d PR C 2
H33D H 0.0504 0.4571 0.0583 0.090 Uiso 0.50 1 d PR C 2
C6 C 0.3932(2) 0.3561(3) -0.0105(7) 0.062(3) Uani 1 1 d . . .
H6A H 0.4271 0.3470 -0.0172 0.075 Uiso 1 1 calc R A .
H6B H 0.3780 0.3501 -0.0814 0.075 Uiso 1 1 calc R . .
C50 C 0.4753(2) 0.0869(3) 0.7082(6) 0.057(3) Uani 1 1 d . . .
H50A H 0.4915 0.0938 0.7767 0.086 Uiso 1 1 calc R . .
H50B H 0.4718 0.0481 0.6980 0.086 Uiso 1 1 calc R . .
H50C H 0.4441 0.1037 0.7096 0.086 Uiso 1 1 calc R . .
C37 C 0.2546(3) 0.3895(3) -0.2223(7) 0.069(3) Uani 1 1 d . A .
H37A H 0.2793 0.3701 -0.1813 0.083 Uiso 1 1 calc R . .
H37B H 0.2236 0.3747 -0.2004 0.083 Uiso 1 1 calc R . .
C3 C 0.2497(3) 0.3284(4) 0.2124(7) 0.082(3) Uani 1 1 d . . .
H3A H 0.2267 0.3013 0.2379 0.098 Uiso 1 1 calc R A .
H3B H 0.2602 0.3498 0.2753 0.098 Uiso 1 1 calc R . .
C39 C 0.2261(3) 0.4107(3) -0.4095(7) 0.067(3) Uani 1 1 d . A .
H39A H 0.2371 0.4116 -0.4854 0.081 Uiso 1 1 calc R . .
H39B H 0.1953 0.3922 -0.4076 0.081 Uiso 1 1 calc R . .
C18 C 0.2924(3) 0.6417(3) 0.4209(7) 0.087(3) Uani 1 1 d . A .
H18A H 0.3213 0.6638 0.4265 0.104 Uiso 1 1 calc R . .
H18B H 0.2786 0.6386 0.4940 0.104 Uiso 1 1 calc R . .
C16 C 0.2747(3) 0.6625(3) 0.2295(8) 0.082(3) Uani 1 1 d . A .
H16A H 0.2522 0.6799 0.1792 0.099 Uiso 1 1 calc R . .
H16B H 0.3056 0.6806 0.2215 0.099 Uiso 1 1 calc R . .
C36 C 0.2377(3) 0.4820(3) -0.2682(7) 0.040(2) Uani 1 1 d . A .
C49 C 0.5705(2) 0.0772(3) 0.5937(7) 0.059(3) Uani 1 1 d . . .
H49A H 0.5894 0.0891 0.6553 0.088 Uiso 1 1 calc R . .
H49B H 0.5879 0.0838 0.5266 0.088 Uiso 1 1 calc R . .
H49C H 0.5640 0.0387 0.6006 0.088 Uiso 1 1 calc R . .
C46 C 0.6234(3) 0.2253(3) 0.4449(9) 0.111(4) Uani 1 1 d U E .
H46A H 0.6205 0.2643 0.4514 0.167 Uiso 1 1 calc R . .
H46B H 0.6568 0.2155 0.4393 0.167 Uiso 1 1 calc R . .
H46C H 0.6096 0.2082 0.5088 0.167 Uiso 1 1 calc R . .
C59 C 0.3955(3) 0.3210(3) 0.6820(6) 0.068(3) Uani 1 1 d . . .
H59A H 0.4234 0.3145 0.7270 0.103 Uiso 1 1 calc R . .
H59B H 0.3675 0.3065 0.7180 0.103 Uiso 1 1 calc R . .
H59C H 0.3915 0.3597 0.6713 0.103 Uiso 1 1 calc R . .
C58 C 0.3532(2) 0.3141(3) 0.4556(7) 0.070(3) Uani 1 1 d . . .
H58A H 0.3522 0.3532 0.4619 0.104 Uiso 1 1 calc R . .
H58B H 0.3231 0.2990 0.4800 0.104 Uiso 1 1 calc R . .
H58C H 0.3586 0.3041 0.3801 0.104 Uiso 1 1 calc R . .
C42 C 0.2190(3) 0.5739(3) -0.3203(7) 0.062(3) Uani 1 1 d . A .
H42A H 0.2450 0.5816 -0.3715 0.074 Uiso 1 1 calc R . .
H42B H 0.2104 0.6078 -0.2839 0.074 Uiso 1 1 calc R . .
C20 C 0.3543(3) 0.5054(3) 0.4071(7) 0.073(3) Uani 1 1 d . . .
H20A H 0.3831 0.5149 0.3663 0.088 Uiso 1 1 calc R A .
H20B H 0.3630 0.4794 0.4641 0.088 Uiso 1 1 calc R . .
C19 C 0.3334(3) 0.5558(3) 0.4587(8) 0.074(3) Uani 1 1 d . A .
H19A H 0.3132 0.5453 0.5204 0.088 Uiso 1 1 calc R . .
H19B H 0.3593 0.5785 0.4869 0.088 Uiso 1 1 calc R . .
N14 N 0.10155(19) 0.5056(3) 0.1184(5) 0.052(2) Uani 1 1 d . A .
C29 C 0.1491(3) 0.5043(3) 0.0872(8) 0.048(2) Uani 1 1 d . A .
C14 C 0.4077(2) 0.5899(3) 0.1037(7) 0.063(3) Uani 1 1 d . A .
H14A H 0.3969 0.5856 0.1793 0.076 Uiso 1 1 calc R . .
H14B H 0.4085 0.6287 0.0873 0.076 Uiso 1 1 calc R . .
C13 C 0.4579(3) 0.5668(4) 0.0930(8) 0.075(3) Uani 1 1 d . . .
H13A H 0.4579 0.5280 0.1095 0.090 Uiso 1 1 calc R A .
H13B H 0.4796 0.5851 0.1436 0.090 Uiso 1 1 calc R . .
C32 C 0.0840(3) 0.5220(4) 0.2252(8) 0.095(4) Uani 1 1 d . . .
H32A H 0.0570 0.4988 0.2454 0.114 Uiso 0.50 1 calc PR D 1
H32B H 0.0724 0.5594 0.2210 0.114 Uiso 0.50 1 calc PR D 1
H32C H 0.0788 0.4901 0.2716 0.114 Uiso 0.50 1 d PR D 2
H32D H 0.0538 0.5417 0.2182 0.114 Uiso 0.50 1 d PR D 2
C45 C 0.5016(3) 0.2722(3) 0.1239(6) 0.061(3) Uani 1 1 d . E .
H45A H 0.5337 0.2724 0.0945 0.091 Uiso 1 1 calc R . .
H45B H 0.4963 0.3053 0.1650 0.091 Uiso 1 1 calc R . .
H45C H 0.4789 0.2700 0.0646 0.091 Uiso 1 1 calc R . .
C60 C 0.3889(3) 0.2114(3) 0.5604(7) 0.073(3) Uani 1 1 d . . .
H60A H 0.4098 0.1956 0.6148 0.109 Uiso 1 1 calc R . .
H60B H 0.3934 0.1930 0.4913 0.109 Uiso 1 1 calc R . .
H60C H 0.3561 0.2075 0.5836 0.109 Uiso 1 1 calc R . .
C55 C 0.5431(2) 0.3578(3) 0.4049(7) 0.072(3) Uani 1 1 d . . .
H55A H 0.5497 0.3270 0.3581 0.108 Uiso 1 1 calc R . .
H55B H 0.5620 0.3552 0.4708 0.108 Uiso 1 1 calc R . .
H55C H 0.5510 0.3911 0.3667 0.108 Uiso 1 1 calc R . .
C54 C 0.4856(3) 0.2194(4) 0.8234(7) 0.122(4) Uani 1 1 d U . .
H54A H 0.4970 0.2376 0.8885 0.183 Uiso 1 1 calc R . .
H54B H 0.4757 0.1828 0.8418 0.183 Uiso 1 1 calc R . .
H54C H 0.4587 0.2392 0.7936 0.183 Uiso 1 1 calc R . .
C35A C 0.0834(5) 0.4921(7) -0.0800(13) 0.055(5) Uani 0.50 1 d PU A 2
H35A H 0.0601 0.4754 -0.1293 0.066 Uiso 0.50 1 calc PR A 2
H35B H 0.0899 0.5291 -0.1051 0.066 Uiso 0.50 1 calc PR A 2
C35B C 0.0811(5) 0.4576(7) -0.0476(14) 0.054(5) Uani 0.50 1 d PU A 1
H35C H 0.0553 0.4512 -0.0999 0.065 Uiso 0.50 1 calc PR A 1
H35D H 0.0908 0.4225 -0.0174 0.065 Uiso 0.50 1 calc PR A 1
C48 C 0.6177(3) 0.2362(3) 0.1946(9) 0.113(4) Uani 1 1 d U E 1
H48A H 0.6043 0.2207 0.1286 0.169 Uiso 1 1 calc R E 1
H48B H 0.6519 0.2309 0.1949 0.169 Uiso 1 1 calc R E 1
H48C H 0.6106 0.2747 0.1971 0.169 Uiso 1 1 calc R E 1
C31A C 0.1261(6) 0.5620(8) 0.2787(16) 0.083(6) Uani 0.50 1 d PU A 2
H31A H 0.1303 0.5954 0.2365 0.099 Uiso 0.50 1 calc PR A 2
H31B H 0.1195 0.5710 0.3551 0.099 Uiso 0.50 1 calc PR A 2
C34A C 0.1242(7) 0.4842(8) -0.1073(16) 0.083(7) Uani 0.50 1 d PU A 1
H34A H 0.1159 0.5200 -0.1358 0.100 Uiso 0.50 1 calc PR A 1
H34B H 0.1355 0.4613 -0.1674 0.100 Uiso 0.50 1 calc PR A 1
C30A C 0.1616(6) 0.5487(7) 0.2684(14) 0.045(5) Uani 0.50 1 d PU A 1
H30A H 0.1866 0.5518 0.3237 0.054 Uiso 0.50 1 calc PR A 1
H30B H 0.1508 0.5853 0.2500 0.054 Uiso 0.50 1 calc PR A 1
C53 C 0.5555(3) 0.2894(3) 0.6931(8) 0.109(4) Uani 1 1 d U . .
H53A H 0.5849 0.2894 0.6514 0.163 Uiso 1 1 calc R . .
H53B H 0.5608 0.3072 0.7627 0.163 Uiso 1 1 calc R . .
H53C H 0.5311 0.3087 0.6529 0.163 Uiso 1 1 calc R . .
C31B C 0.1219(5) 0.5183(6) 0.3136(13) 0.049(5) Uani 0.50 1 d PU A 1
H31C H 0.1108 0.5347 0.3818 0.059 Uiso 0.50 1 calc PR A 1
H31D H 0.1309 0.4806 0.3274 0.059 Uiso 0.50 1 calc PR A 1
C34B C 0.1296(5) 0.4585(6) -0.0767(12) 0.030(4) Uani 0.50 1 d PU A 2
H34C H 0.1235 0.4229 -0.0439 0.036 Uiso 0.50 1 calc PR A 2
H34D H 0.1419 0.4531 -0.1507 0.036 Uiso 0.50 1 calc PR A 2
C30B C 0.1708(6) 0.5225(7) 0.2670(16) 0.056(6) Uani 0.50 1 d PU A 2
H30C H 0.1974 0.5360 0.3111 0.067 Uiso 0.50 1 calc PR A 2
H30D H 0.1625 0.4861 0.2929 0.067 Uiso 0.50 1 calc PR A 2
C52 C 0.5859(3) 0.1815(4) 0.7933(9) 0.137(4) Uani 1 1 d U . .
H52A H 0.5760 0.1453 0.8138 0.205 Uiso 1 1 calc R . .
H52B H 0.5937 0.2020 0.8584 0.205 Uiso 1 1 calc R . .
H52C H 0.6137 0.1794 0.7464 0.205 Uiso 1 1 calc R . .
C61 C 0.1560(3) 0.6458(4) -0.0165(9) 0.135(4) Uani 1 1 d DU . .
H61A H 0.1346 0.6145 -0.0107 0.162 Uiso 1 1 calc R F 2
H61B H 0.1532 0.6666 0.0513 0.162 Uiso 1 1 calc R F 2
C62 C 0.1405(4) 0.6789(5) -0.1050(11) 0.183(5) Uani 1 1 d DU G 2
H62A H 0.1101 0.6957 -0.0852 0.220 Uiso 1 1 calc R G 2
H62B H 0.1348 0.6557 -0.1686 0.220 Uiso 1 1 calc R G 2
N64 N 0.2207(3) 0.7058(3) -0.1227(7) 0.099(3) Uani 1 1 d DU G .
C68 C 0.2986(7) 0.7396(8) -0.1158(19) 0.122(7) Uani 0.50 1 d PU H 2
H68A H 0.2929 0.7456 -0.0379 0.147 Uiso 0.50 1 calc PR H 2
H68B H 0.3215 0.7665 -0.1425 0.147 Uiso 0.50 1 calc PR H 2
C67 C 0.3163(3) 0.6805(4) -0.1385(8) 0.094(3) Uani 1 1 d U . .
H67A H 0.3303 0.7051 -0.0846 0.113 Uiso 0.50 1 calc PR H 1
H67B H 0.3422 0.6586 -0.1687 0.113 Uiso 0.50 1 calc PR H 1
H67C H 0.3160 0.6731 -0.2171 0.113 Uiso 0.50 1 d PR H 2
H67D H 0.3488 0.6755 -0.1112 0.113 Uiso 0.50 1 d PR H 2
C69 C 0.2515(4) 0.7411(5) -0.1822(11) 0.147(4) Uani 1 1 d U . .
H69A H 0.2612 0.7710 -0.1344 0.176 Uiso 0.50 1 calc PR H 1
H69B H 0.2338 0.7567 -0.2435 0.176 Uiso 0.50 1 calc PR H 1
H69C H 0.2386 0.7780 -0.1852 0.176 Uiso 0.50 1 d PR H 2
H69D H 0.2565 0.7279 -0.2567 0.176 Uiso 0.50 1 d PR H 2
N65 N 0.2053(2) 0.6260(3) -0.0266(7) 0.076(2) Uani 1 1 d U A .
C63 C 0.1738(4) 0.7209(5) -0.1351(11) 0.155(4) Uani 1 1 d DU . .
H63A H 0.1683 0.7309 -0.2114 0.185 Uiso 1 1 calc R G 2
H63B H 0.1677 0.7530 -0.0901 0.185 Uiso 1 1 calc R G 2
N66 N 0.2828(2) 0.6437(3) -0.0810(6) 0.067(2) Uani 1 1 d U A .
C70 C 0.2376(3) 0.6572(3) -0.0764(7) 0.056(3) Uani 1 1 d U . .
C68A C 0.2962(7) 0.7130(8) -0.2262(18) 0.105(7) Uani 0.50 1 d PU H 1
H68C H 0.2880 0.6898 -0.2884 0.126 Uiso 0.50 1 calc PR H 1
H68D H 0.3195 0.7400 -0.2507 0.126 Uiso 0.50 1 calc PR H 1
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
Zn9 0.0447(5) 0.0324(4) 0.0608(6) -0.0010(6) -0.0144(6) 0.0007(5)
Si1 0.0519(14) 0.0356(14) 0.0516(18) 0.0021(13) -0.0151(12) 0.0044(11)
Zn1 0.0173(11) 0.0251(13) 0.0224(12) 0.0074(14) -0.0054(10) -0.0063(11)
Zn2 0.010(4) 0.026(4) 0.026(4) 0.010(4) 0.000(3) 0.004(3)
Zn3 0.0226(15) 0.0204(15) 0.0377(18) 0.0076(16) -0.0114(15) 0.0033(13)
Zn4 0.006(2) 0.014(3) 0.034(3) 0.012(2) -0.005(2) 0.0020(18)
Zn5 0.017(2) 0.026(2) 0.019(2) 0.002(2) 0.007(2) -0.0063(19)
Zn6 0.019(3) 0.011(3) 0.023(4) 0.008(3) -0.007(3) -0.003(3)
Zn7 0.011(4) 0.018(4) 0.014(5) 0.008(4) -0.003(4) 0.001(4)
Zn8 0.007(3) 0.025(4) 0.046(5) 0.002(4) 0.004(4) -0.005(3)
Li1 0.0173(11) 0.0251(13) 0.0224(12) 0.0074(14) -0.0054(10) -0.0063(11)
Li2 0.010(4) 0.026(4) 0.026(4) 0.010(4) 0.000(3) 0.004(3)
Li3 0.0226(15) 0.0204(15) 0.0377(18) 0.0076(16) -0.0114(15) 0.0033(13)
Li4 0.006(2) 0.014(3) 0.034(3) 0.012(2) -0.005(2) 0.0020(18)
Li5 0.017(2) 0.026(2) 0.019(2) 0.002(2) 0.007(2) -0.0063(19)
Li6 0.019(3) 0.011(3) 0.023(4) 0.008(3) -0.007(3) -0.003(3)
Li7 0.011(4) 0.018(4) 0.014(5) 0.008(4) -0.003(4) 0.001(4)
Li8 0.007(3) 0.025(4) 0.046(5) 0.002(4) 0.004(4) -0.005(3)
C38 0.126(8) 0.046(6) 0.080(7) -0.025(6) 0.036(7) -0.003(6)
Si2 0.0648(16) 0.0412(14) 0.0501(16) 0.0013(14) 0.0010(14) 0.0078(13)
Si4 0.0537(16) 0.0416(14) 0.0645(16) 0.0055(15) -0.0147(14) 0.0038(12)
Si5 0.0433(15) 0.0572(18) 0.136(3) 0.0239(19) 0.0085(18) 0.0093(13)
Si6 0.0501(15) 0.0463(15) 0.0651(17) -0.0067(14) 0.0134(15) 0.0045(13)
Si3 0.130(2) 0.0500(18) 0.084(2) -0.0022(17) -0.067(2) 0.0070(17)
N19 0.026(3) 0.049(4) 0.054(4) -0.015(4) 0.003(3) 0.009(3)
N3 0.043(4) 0.028(4) 0.070(5) 0.019(4) 0.002(4) -0.005(3)
N18 0.063(4) 0.035(4) 0.033(4) 0.000(4) 0.003(3) -0.005(3)
O1 0.043(3) 0.038(3) 0.036(4) 0.009(3) -0.003(2) -0.009(2)
C40 0.082(6) 0.073(6) 0.040(6) 0.027(6) -0.025(5) -0.019(5)
N6 0.021(4) 0.044(4) 0.060(5) 0.012(4) -0.010(3) -0.012(3)
N21 0.063(4) 0.037(4) 0.053(4) 0.002(4) -0.021(4) 0.003(3)
N13 0.034(3) 0.066(5) 0.051(4) 0.005(4) -0.012(4) -0.008(3)
N5 0.051(4) 0.056(4) 0.028(4) -0.005(4) -0.004(4) -0.019(3)
N7 0.062(4) 0.021(4) 0.064(5) 0.003(4) -0.023(4) 0.001(3)
N2 0.028(4) 0.051(4) 0.077(5) 0.024(4) -0.011(4) 0.001(3)
C4 0.055(6) 0.070(6) 0.080(7) 0.029(6) 0.003(5) -0.021(5)
C2 0.047(5) 0.061(6) 0.061(6) 0.031(5) 0.026(5) -0.005(5)
N4 0.042(4) 0.053(4) 0.032(4) 0.011(4) 0.014(4) -0.011(3)
N20 0.045(4) 0.032(3) 0.061(5) -0.001(4) 0.001(4) -0.001(3)
N9 0.046(4) 0.042(4) 0.051(5) -0.004(4) -0.003(4) 0.002(3)
N15 0.037(4) 0.063(5) 0.061(5) 0.003(4) -0.005(4) -0.009(3)
N17 0.061(4) 0.036(4) 0.045(4) 0.010(4) -0.022(3) 0.008(3)
C41 0.084(7) 0.075(7) 0.080(8) 0.023(6) -0.021(6) 0.013(6)
C10 0.077(6) 0.057(6) 0.056(6) 0.010(5) 0.022(5) -0.011(5)
N1 0.016(3) 0.049(4) 0.092(5) 0.011(5) 0.006(4) -0.006(3)
N16 0.082(5) 0.031(4) 0.061(5) -0.007(4) -0.018(4) 0.013(4)
N8 0.065(5) 0.042(4) 0.058(5) 0.010(4) -0.033(4) 0.007(4)
C11 0.038(5) 0.065(6) 0.064(7) 0.016(5) 0.015(5) 0.000(5)
C56 0.053(5) 0.049(5) 0.049(6) 0.000(5) -0.005(5) 0.019(4)
C47 0.068(6) 0.053(6) 0.119(8) 0.017(6) 0.028(6) 0.027(5)
C21 0.045(5) 0.054(6) 0.044(6) 0.012(5) -0.012(5) 0.002(4)
C1 0.044(5) 0.033(5) 0.053(6) 0.014(5) -0.012(5) -0.018(4)
C43 0.060(5) 0.038(5) 0.047(6) -0.005(5) -0.005(4) 0.006(4)
C44 0.081(6) 0.039(5) 0.081(7) -0.004(5) 0.021(6) 0.017(5)
C12 0.037(5) 0.081(6) 0.095(7) 0.024(7) 0.010(6) -0.015(4)
C8 0.029(5) 0.032(5) 0.055(6) 0.012(5) -0.014(5) -0.015(4)
C57 0.118(7) 0.042(6) 0.043(5) -0.005(5) -0.025(5) -0.001(5)
C15 0.037(5) 0.043(6) 0.033(6) 0.004(5) 0.004(4) -0.005(4)
C5 0.072(6) 0.031(5) 0.097(8) 0.005(6) -0.017(6) 0.012(5)
C51 0.059(5) 0.041(5) 0.093(7) 0.010(6) -0.009(6) 0.002(4)
C17 0.090(7) 0.042(6) 0.106(8) -0.010(6) 0.035(7) -0.003(5)
C9 0.077(6) 0.073(7) 0.059(7) 0.022(6) 0.002(5) -0.023(5)
C7 0.041(5) 0.049(5) 0.091(8) 0.028(5) -0.005(5) 0.005(4)
C33 0.052(5) 0.075(5) 0.098(6) 0.004(5) -0.001(5) 0.005(4)
C6 0.047(5) 0.071(6) 0.069(7) 0.009(6) 0.004(5) 0.022(5)
C50 0.052(5) 0.047(5) 0.072(6) 0.008(5) -0.004(5) 0.011(4)
C37 0.076(7) 0.067(7) 0.065(7) 0.010(6) -0.016(5) -0.010(5)
C3 0.083(7) 0.086(7) 0.077(7) 0.017(7) 0.014(6) -0.058(5)
C39 0.078(6) 0.071(7) 0.052(6) 0.007(6) -0.013(5) -0.004(5)
C18 0.167(9) 0.052(6) 0.042(7) -0.003(5) -0.005(6) 0.015(6)
C16 0.112(7) 0.047(6) 0.088(8) -0.006(6) -0.027(7) 0.003(6)
C36 0.043(5) 0.041(6) 0.035(6) 0.007(5) 0.005(4) -0.008(4)
C49 0.058(5) 0.045(5) 0.073(6) 0.023(5) -0.009(5) -0.003(4)
C46 0.048(5) 0.086(7) 0.200(13) -0.001(8) -0.017(8) 0.014(5)
C59 0.089(7) 0.065(6) 0.051(6) 0.004(5) 0.012(5) 0.001(5)
C58 0.052(5) 0.080(6) 0.077(7) 0.008(6) 0.001(6) 0.015(4)
C42 0.076(6) 0.039(6) 0.070(7) 0.003(5) -0.024(5) 0.010(5)
C20 0.071(6) 0.067(6) 0.082(7) 0.017(6) -0.039(5) 0.015(5)
C19 0.098(6) 0.065(6) 0.058(6) 0.002(6) -0.026(6) 0.007(5)
N14 0.023(4) 0.068(5) 0.065(5) 0.003(5) -0.005(4) 0.007(4)
C29 0.033(5) 0.034(5) 0.078(7) 0.007(6) -0.003(5) 0.000(4)
C14 0.047(5) 0.078(6) 0.065(6) -0.006(6) -0.006(5) -0.018(5)
C13 0.055(6) 0.087(7) 0.083(7) 0.003(6) -0.021(6) -0.025(5)
C32 0.039(6) 0.161(11) 0.086(8) -0.008(8) 0.006(6) 0.031(6)
C45 0.078(6) 0.046(5) 0.058(6) -0.001(5) 0.002(5) 0.020(5)
C60 0.076(6) 0.053(6) 0.090(8) 0.009(6) 0.013(6) 0.005(5)
C55 0.061(6) 0.044(5) 0.111(8) 0.019(6) -0.028(5) -0.018(5)
C54 0.194(11) 0.119(9) 0.053(7) -0.016(7) -0.035(8) 0.009(8)
C35A 0.061(8) 0.048(8) 0.058(8) -0.013(7) -0.012(6) 0.000(7)
C35B 0.052(7) 0.062(8) 0.050(8) 0.003(7) -0.019(7) -0.016(6)
C48 0.032(5) 0.079(7) 0.227(12) 0.070(8) 0.035(7) 0.015(5)
C31A 0.083(9) 0.088(9) 0.077(9) 0.003(7) 0.005(7) 0.006(7)
C34A 0.078(9) 0.085(9) 0.086(9) 0.002(7) -0.001(7) -0.011(7)
C30A 0.048(8) 0.045(8) 0.043(8) -0.004(7) -0.001(6) -0.002(7)
C53 0.175(9) 0.043(6) 0.108(8) -0.015(6) -0.085(8) 0.000(6)
C31B 0.047(7) 0.047(8) 0.055(8) 0.000(7) 0.012(6) 0.001(6)
C34B 0.028(7) 0.036(7) 0.026(8) -0.008(6) -0.003(6) 0.002(6)
C30B 0.055(8) 0.054(9) 0.058(9) 0.002(7) 0.007(7) 0.001(7)
C52 0.175(9) 0.070(7) 0.166(10) -0.007(7) -0.150(8) 0.017(7)
C61 0.106(6) 0.155(6) 0.143(7) 0.011(5) -0.007(6) 0.020(5)
C62 0.170(7) 0.190(7) 0.190(8) 0.023(6) -0.005(6) 0.037(6)
N64 0.108(5) 0.089(5) 0.100(6) 0.000(5) -0.002(5) 0.020(4)
C68 0.137(9) 0.107(9) 0.124(10) 0.001(8) 0.019(8) -0.017(7)
C67 0.112(6) 0.080(6) 0.091(6) 0.005(5) 0.001(6) -0.012(5)
C69 0.170(7) 0.113(7) 0.158(8) 0.029(7) 0.014(7) 0.023(6)
N65 0.066(4) 0.072(4) 0.090(5) 0.015(5) -0.010(4) 0.016(4)
C63 0.158(7) 0.156(7) 0.150(7) 0.015(6) 0.008(6) 0.048(6)
N66 0.069(4) 0.060(4) 0.073(5) 0.011(4) -0.006(4) -0.017(4)
C70 0.074(6) 0.040(5) 0.053(6) -0.001(4) -0.012(5) 0.003(5)
C68A 0.105(9) 0.110(9) 0.101(10) 0.012(8) -0.002(7) -0.011(7)
_geom_special_details
;
All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell s.u.'s are taken
into account individually in the estimation of s.u.'s in distances, angles
and torsion angles; correlations between s.u.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.
;
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
Zn9 N19 1.964(6) . ?
Zn9 N20 1.978(5) . ?
Zn9 N21 1.984(6) . ?
Si1 N20 1.682(5) . ?
Si1 C57 1.860(7) . ?
Si1 C55 1.864(7) . ?
Si1 C56 1.894(7) . ?
Zn1 O1 1.983(5) . ?
Zn1 N17 2.011(6) . ?
Zn1 N5 2.042(6) . ?
Zn1 N2 2.066(6) . ?
Zn1 Zn4 2.311(4) . ?
Zn1 Zn2 2.323(6) . ?
Zn1 Zn5 2.485(4) . ?
Zn2 N66 1.993(9) . ?
Zn2 N5 1.997(8) . ?
Zn2 O1 2.050(7) . ?
Zn2 N16 2.112(9) . ?
Zn2 Zn3 2.309(6) . ?
Zn2 Zn6 2.371(8) . ?
Zn3 N16 1.986(7) . ?
Zn3 O1 1.996(5) . ?
Zn3 N65 2.039(8) . ?
Zn3 N15 2.040(6) . ?
Zn3 Zn7 2.330(9) . ?
Zn3 Zn4 2.376(5) . ?
Zn4 N1 1.990(7) . ?
Zn4 O1 2.017(6) . ?
Zn4 N15 2.035(7) . ?
Zn4 N17 2.169(7) . ?
Zn4 Zn8 2.235(8) . ?
Zn5 N7 1.970(7) . ?
Zn5 O1 2.062(5) . ?
Zn5 N4 2.086(6) . ?
Zn5 N2 2.090(7) . ?
Zn5 Zn6 2.301(6) . ?
Zn5 Zn8 2.344(6) . ?
Zn6 N4 2.017(7) . ?
Zn6 N8 2.057(8) . ?
Zn6 O1 2.072(7) . ?
Zn6 N66 2.122(8) . ?
Zn6 Zn7 2.350(9) . ?
Zn7 O1 1.989(9) . ?
Zn7 N65 2.052(11) . ?
Zn7 N8 2.053(11) . ?
Zn7 N13 2.121(10) . ?
Zn7 Zn8 2.261(10) . ?
Zn8 N13 1.983(7) . ?
Zn8 O1 1.990(7) . ?
Zn8 N7 2.104(9) . ?
Zn8 N1 2.146(9) . ?
C38 C37 1.467(11) . ?
C38 C39 1.499(10) . ?
Si2 N20 1.723(6) . ?
Si2 C60 1.888(7) . ?
Si2 C58 1.888(7) . ?
Si2 C59 1.891(8) . ?
Si4 N21 1.703(6) . ?
Si4 C51 1.878(8) . ?
Si4 C50 1.889(7) . ?
Si4 C49 1.896(6) . ?
Si5 N19 1.711(5) . ?
Si5 C47 1.876(7) . ?
Si5 C46 1.879(10) . ?
Si5 C48 1.880(9) . ?
Si6 N19 1.684(6) . ?
Si6 C43 1.866(7) . ?
Si6 C45 1.870(7) . ?
Si6 C44 1.871(7) . ?
Si3 N21 1.668(6) . ?
Si3 C52 1.882(8) . ?
Si3 C53 1.888(8) . ?
Si3 C54 1.890(10) . ?
N3 C1 1.376(8) . ?
N3 C4 1.438(8) . ?
N3 C5 1.457(8) . ?
N18 C15 1.341(9) . ?
N18 C18 1.455(9) . ?
N18 C19 1.457(9) . ?
C40 N9 1.454(8) . ?
C40 C41 1.528(10) . ?
N6 C8 1.382(8) . ?
N6 C12 1.457(9) . ?
N6 C11 1.458(9) . ?
N13 C29 1.320(10) . ?
N13 C34B 1.440(15) . ?
N13 C34A 1.605(19) . ?
N5 C8 1.340(9) . ?
N5 C14 1.446(9) . ?
N7 C36 1.323(9) . ?
N7 C37 1.497(9) . ?
N2 C1 1.347(8) . ?
N2 C7 1.474(8) . ?
C4 C3 1.528(10) . ?
C2 N1 1.467(8) . ?
C2 C3 1.518(10) . ?
N4 C8 1.349(8) . ?
N4 C9 1.458(9) . ?
N9 C36 1.373(9) . ?
N9 C39 1.444(9) . ?
N15 C30B 1.343(19) . ?
N15 C29 1.365(9) . ?
N15 C30A 1.602(17) . ?
N17 C15 1.343(8) . ?
N17 C21 1.421(8) . ?
C41 C42 1.483(10) . ?
C10 C11 1.489(10) . ?
C10 C9 1.511(10) . ?
N1 C1 1.332(8) . ?
N16 C15 1.351(9) . ?
N16 C16 1.467(9) . ?
N8 C36 1.351(9) . ?
N8 C42 1.426(9) . ?
C21 C20 1.484(9) . ?
C12 C13 1.537(12) . ?
C5 C6 1.508(10) . ?
C17 C16 1.504(11) . ?
C17 C18 1.505(10) . ?
C7 C6 1.436(9) . ?
C33 N14 1.442(9) . ?
C33 C35B 1.453(17) . ?
C33 C35A 1.561(16) . ?
C20 C19 1.499(10) . ?
N14 C29 1.373(8) . ?
N14 C32 1.442(10) . ?
C14 C13 1.509(9) . ?
C32 C31B 1.506(16) . ?
C32 C31A 1.658(19) . ?
C35A C34B 1.52(2) . ?
C35B C34A 1.54(2) . ?
C31A C30B 1.58(2) . ?
C30A C31B 1.44(2) . ?
C61 C62 1.410(12) . ?
C61 N65 1.458(10) . ?
C62 C63 1.429(12) . ?
N64 C63 1.364(10) . ?
N64 C70 1.395(10) . ?
N64 C69 1.412(12) . ?
C68 C69 1.54(2) . ?
C68 C67 1.55(2) . ?
C67 C68A 1.44(2) . ?
C67 N66 1.470(10) . ?
C69 C68A 1.52(2) . ?
N65 C70 1.324(9) . ?
N66 C70 1.299(9) . ?
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
N19 Zn9 N20 118.6(2) . . ?
N19 Zn9 N21 119.3(2) . . ?
N20 Zn9 N21 122.0(2) . . ?
N20 Si1 C57 114.4(3) . . ?
N20 Si1 C55 111.6(3) . . ?
C57 Si1 C55 108.1(4) . . ?
N20 Si1 C56 114.7(3) . . ?
C57 Si1 C56 102.3(3) . . ?
C55 Si1 C56 105.0(4) . . ?
O1 Zn1 N17 102.7(2) . . ?
O1 Zn1 N5 98.9(2) . . ?
N17 Zn1 N5 118.0(3) . . ?
O1 Zn1 N2 97.8(2) . . ?
N17 Zn1 N2 119.1(3) . . ?
N5 Zn1 N2 114.4(2) . . ?
O1 Zn1 Zn4 55.40(16) . . ?
N17 Zn1 Zn4 59.8(2) . . ?
N5 Zn1 Zn4 148.4(2) . . ?
N2 Zn1 Zn4 89.30(19) . . ?
O1 Zn1 Zn2 56.18(19) . . ?
N17 Zn1 Zn2 94.3(2) . . ?
N5 Zn1 Zn2 54.0(2) . . ?
N2 Zn1 Zn2 142.8(2) . . ?
Zn4 Zn1 Zn2 94.44(19) . . ?
O1 Zn1 Zn5 53.55(16) . . ?
N17 Zn1 Zn5 147.2(2) . . ?
N5 Zn1 Zn5 90.3(2) . . ?
N2 Zn1 Zn5 53.73(18) . . ?
Zn4 Zn1 Zn5 87.41(14) . . ?
Zn2 Zn1 Zn5 89.4(2) . . ?
N66 Zn2 N5 121.2(4) . . ?
N66 Zn2 O1 99.6(3) . . ?
N5 Zn2 O1 98.1(3) . . ?
N66 Zn2 N16 118.6(4) . . ?
N5 Zn2 N16 114.9(4) . . ?
O1 Zn2 N16 95.1(3) . . ?
N66 Zn2 Zn3 90.8(3) . . ?
N5 Zn2 Zn3 142.5(3) . . ?
O1 Zn2 Zn3 54.13(19) . . ?
N16 Zn2 Zn3 53.1(2) . . ?
N66 Zn2 Zn1 147.3(4) . . ?
N5 Zn2 Zn1 55.8(2) . . ?
O1 Zn2 Zn1 53.48(19) . . ?
N16 Zn2 Zn1 85.3(3) . . ?
Zn3 Zn2 Zn1 86.7(2) . . ?
N66 Zn2 Zn6 57.4(3) . . ?
N5 Zn2 Zn6 90.6(3) . . ?
O1 Zn2 Zn6 55.3(2) . . ?
N16 Zn2 Zn6 144.5(3) . . ?
Zn3 Zn2 Zn6 91.5(2) . . ?
Zn1 Zn2 Zn6 90.0(3) . . ?
N16 Zn3 O1 100.9(2) . . ?
N16 Zn3 N65 119.4(3) . . ?
O1 Zn3 N65 98.6(3) . . ?
N16 Zn3 N15 115.7(3) . . ?
O1 Zn3 N15 98.2(2) . . ?
N65 Zn3 N15 117.4(3) . . ?
N16 Zn3 Zn2 58.3(3) . . ?
O1 Zn3 Zn2 56.3(2) . . ?
N65 Zn3 Zn2 88.8(3) . . ?
N15 Zn3 Zn2 147.3(2) . . ?
N16 Zn3 Zn7 147.8(3) . . ?
O1 Zn3 Zn7 54.1(2) . . ?
N65 Zn3 Zn7 55.5(3) . . ?
N15 Zn3 Zn7 90.1(3) . . ?
Zn2 Zn3 Zn7 89.5(3) . . ?
N16 Zn3 Zn4 92.1(2) . . ?
O1 Zn3 Zn4 54.10(17) . . ?
N65 Zn3 Zn4 143.3(3) . . ?
N15 Zn3 Zn4 54.2(2) . . ?
Zn2 Zn3 Zn4 93.09(19) . . ?
Zn7 Zn3 Zn4 87.8(2) . . ?
N1 Zn4 O1 100.4(3) . . ?
N1 Zn4 N15 126.2(3) . . ?
O1 Zn4 N15 97.7(3) . . ?
N1 Zn4 N17 115.1(3) . . ?
O1 Zn4 N17 96.3(3) . . ?
N15 Zn4 N17 112.6(3) . . ?
N1 Zn4 Zn8 60.7(3) . . ?
O1 Zn4 Zn8 55.5(2) . . ?
N15 Zn4 Zn8 91.1(3) . . ?
N17 Zn4 Zn8 146.4(3) . . ?
N1 Zn4 Zn1 90.1(2) . . ?
O1 Zn4 Zn1 54.02(16) . . ?
N15 Zn4 Zn1 139.6(3) . . ?
N17 Zn4 Zn1 53.22(19) . . ?
Zn8 Zn4 Zn1 93.2(2) . . ?
N1 Zn4 Zn3 149.5(3) . . ?
O1 Zn4 Zn3 53.31(16) . . ?
N15 Zn4 Zn3 54.4(2) . . ?
N17 Zn4 Zn3 86.0(2) . . ?
Zn8 Zn4 Zn3 89.3(2) . . ?
Zn1 Zn4 Zn3 85.46(15) . . ?
N7 Zn5 O1 98.6(3) . . ?
N7 Zn5 N4 121.2(3) . . ?
O1 Zn5 N4 95.6(2) . . ?
N7 Zn5 N2 125.0(3) . . ?
O1 Zn5 N2 94.6(2) . . ?
N4 Zn5 N2 110.1(3) . . ?
N7 Zn5 Zn6 88.9(2) . . ?
O1 Zn5 Zn6 56.4(2) . . ?
N4 Zn5 Zn6 54.5(2) . . ?
N2 Zn5 Zn6 140.2(3) . . ?
N7 Zn5 Zn8 57.6(3) . . ?
O1 Zn5 Zn8 53.2(2) . . ?
N4 Zn5 Zn8 144.1(3) . . ?
N2 Zn5 Zn8 91.7(3) . . ?
Zn6 Zn5 Zn8 90.5(2) . . ?
N7 Zn5 Zn1 143.7(3) . . ?
O1 Zn5 Zn1 50.67(15) . . ?
N4 Zn5 Zn1 85.1(2) . . ?
N2 Zn5 Zn1 52.85(19) . . ?
Zn6 Zn5 Zn1 87.73(19) . . ?
Zn8 Zn5 Zn1 86.3(2) . . ?
N4 Zn6 N8 124.2(4) . . ?
N4 Zn6 O1 97.5(3) . . ?
N8 Zn6 O1 98.2(3) . . ?
N4 Zn6 N66 116.4(3) . . ?
N8 Zn6 N66 115.2(3) . . ?
O1 Zn6 N66 94.8(3) . . ?
N4 Zn6 Zn5 57.3(2) . . ?
N8 Zn6 Zn5 90.0(3) . . ?
O1 Zn6 Zn5 55.96(19) . . ?
N66 Zn6 Zn5 145.0(3) . . ?
N4 Zn6 Zn7 145.2(4) . . ?
N8 Zn6 Zn7 55.0(3) . . ?
O1 Zn6 Zn7 53.0(3) . . ?
N66 Zn6 Zn7 87.1(3) . . ?
Zn5 Zn6 Zn7 88.5(3) . . ?
N4 Zn6 Zn2 87.9(3) . . ?
N8 Zn6 Zn2 142.4(3) . . ?
O1 Zn6 Zn2 54.4(2) . . ?
N66 Zn6 Zn2 52.3(3) . . ?
Zn5 Zn6 Zn2 92.8(3) . . ?
Zn7 Zn6 Zn2 87.5(3) . . ?
O1 Zn7 N65 98.4(4) . . ?
O1 Zn7 N8 101.0(4) . . ?
N65 Zn7 N8 117.2(5) . . ?
O1 Zn7 N13 97.0(4) . . ?
N65 Zn7 N13 116.7(5) . . ?
N8 Zn7 N13 119.1(5) . . ?
O1 Zn7 Zn8 55.4(3) . . ?
N65 Zn7 Zn8 144.8(5) . . ?
N8 Zn7 Zn8 92.6(4) . . ?
N13 Zn7 Zn8 53.7(3) . . ?
O1 Zn7 Zn3 54.4(2) . . ?
N65 Zn7 Zn3 55.0(3) . . ?
N8 Zn7 Zn3 146.6(4) . . ?
N13 Zn7 Zn3 88.8(4) . . ?
Zn8 Zn7 Zn3 89.8(4) . . ?
O1 Zn7 Zn6 56.3(3) . . ?
N65 Zn7 Zn6 91.4(4) . . ?
N8 Zn7 Zn6 55.2(3) . . ?
N13 Zn7 Zn6 145.0(4) . . ?
Zn8 Zn7 Zn6 91.3(3) . . ?
Zn3 Zn7 Zn6 91.5(3) . . ?
N13 Zn8 O1 101.6(3) . . ?
N13 Zn8 N7 119.3(4) . . ?
O1 Zn8 N7 96.7(3) . . ?
N13 Zn8 N1 119.1(4) . . ?
O1 Zn8 N1 96.1(3) . . ?
N7 Zn8 N1 115.6(3) . . ?
N13 Zn8 Zn4 90.3(3) . . ?
O1 Zn8 Zn4 56.7(2) . . ?
N7 Zn8 Zn4 145.0(3) . . ?
N1 Zn8 Zn4 54.0(3) . . ?
N13 Zn8 Zn7 59.6(3) . . ?
O1 Zn8 Zn7 55.4(3) . . ?
N7 Zn8 Zn7 87.5(4) . . ?
N1 Zn8 Zn7 146.5(4) . . ?
Zn4 Zn8 Zn7 93.1(3) . . ?
N13 Zn8 Zn5 149.2(3) . . ?
O1 Zn8 Zn5 56.11(19) . . ?
N7 Zn8 Zn5 52.3(2) . . ?
N1 Zn8 Zn5 86.7(2) . . ?
Zn4 Zn8 Zn5 92.8(2) . . ?
Zn7 Zn8 Zn5 89.7(3) . . ?
C37 C38 C39 112.0(7) . . ?
N20 Si2 C60 112.0(3) . . ?
N20 Si2 C58 112.4(3) . . ?
C60 Si2 C58 104.3(3) . . ?
N20 Si2 C59 114.4(3) . . ?
C60 Si2 C59 108.3(4) . . ?
C58 Si2 C59 104.7(4) . . ?
N21 Si4 C51 112.7(3) . . ?
N21 Si4 C50 112.2(3) . . ?
C51 Si4 C50 106.2(3) . . ?
N21 Si4 C49 114.0(3) . . ?
C51 Si4 C49 106.2(3) . . ?
C50 Si4 C49 104.7(3) . . ?
N19 Si5 C47 113.6(3) . . ?
N19 Si5 C46 111.2(3) . . ?
C47 Si5 C46 106.2(4) . . ?
N19 Si5 C48 111.5(3) . . ?
C47 Si5 C48 105.4(4) . . ?
C46 Si5 C48 108.6(4) . . ?
N19 Si6 C43 111.9(3) . . ?
N19 Si6 C45 112.7(3) . . ?
C43 Si6 C45 106.9(3) . . ?
N19 Si6 C44 112.6(3) . . ?
C43 Si6 C44 106.0(3) . . ?
C45 Si6 C44 106.3(3) . . ?
N21 Si3 C52 114.7(4) . . ?
N21 Si3 C53 112.4(4) . . ?
C52 Si3 C53 106.6(4) . . ?
N21 Si3 C54 112.3(4) . . ?
C52 Si3 C54 103.3(5) . . ?
C53 Si3 C54 106.8(4) . . ?
Si6 N19 Si5 121.5(4) . . ?
Si6 N19 Zn9 119.2(3) . . ?
Si5 N19 Zn9 119.3(3) . . ?
C1 N3 C4 123.0(6) . . ?
C1 N3 C5 122.9(6) . . ?
C4 N3 C5 113.7(6) . . ?
C15 N18 C18 124.1(6) . . ?
C15 N18 C19 122.3(6) . . ?
C18 N18 C19 113.2(6) . . ?
Zn1 O1 Zn7 177.6(4) . . ?
Zn1 O1 Zn8 112.5(3) . . ?
Zn7 O1 Zn8 69.2(3) . . ?
Zn1 O1 Zn3 106.1(2) . . ?
Zn7 O1 Zn3 71.6(3) . . ?
Zn8 O1 Zn3 108.9(3) . . ?
Zn1 O1 Zn4 70.58(19) . . ?
Zn7 O1 Zn4 109.1(3) . . ?
Zn8 O1 Zn4 67.8(3) . . ?
Zn3 O1 Zn4 72.6(2) . . ?
Zn1 O1 Zn2 70.3(2) . . ?
Zn7 O1 Zn2 107.9(3) . . ?
Zn8 O1 Zn2 177.1(3) . . ?
Zn3 O1 Zn2 69.6(2) . . ?
Zn4 O1 Zn2 113.5(3) . . ?
N9 C40 C41 110.6(6) . . ?
C8 N6 C12 121.1(6) . . ?
C8 N6 C11 125.2(6) . . ?
C12 N6 C11 113.4(6) . . ?
Si3 N21 Si4 123.1(4) . . ?
Si3 N21 Zn9 118.0(3) . . ?
Si4 N21 Zn9 118.8(3) . . ?
C29 N13 C34B 116.2(8) . . ?
C29 N13 C34A 117.6(9) . . ?
C29 N13 Zn8 120.5(5) . . ?
C34B N13 Zn8 111.2(7) . . ?
C34A N13 Zn8 121.2(8) . . ?
C29 N13 Zn7 111.2(6) . . ?
C34B N13 Zn7 122.2(8) . . ?
C34A N13 Zn7 100.5(8) . . ?
Zn8 N13 Zn7 66.7(3) . . ?
C8 N5 C14 116.2(6) . . ?
C8 N5 Zn2 114.1(5) . . ?
C14 N5 Zn2 113.4(5) . . ?
C8 N5 Zn1 115.3(5) . . ?
C14 N5 Zn1 119.3(5) . . ?
Zn2 N5 Zn1 70.2(3) . . ?
C36 N7 C37 114.6(6) . . ?
C36 N7 Zn5 121.3(5) . . ?
C37 N7 Zn5 117.7(5) . . ?
C36 N7 Zn8 114.9(5) . . ?
C37 N7 Zn8 109.3(5) . . ?
Zn5 N7 Zn8 70.2(3) . . ?
C1 N2 C7 119.1(6) . . ?
C1 N2 Zn1 113.8(5) . . ?
C7 N2 Zn1 114.5(4) . . ?
C1 N2 Zn5 113.1(5) . . ?
C7 N2 Zn5 114.5(5) . . ?
Zn1 N2 Zn5 73.4(2) . . ?
N3 C4 C3 110.3(6) . . ?
N1 C2 C3 110.1(6) . . ?
C8 N4 C9 118.3(6) . . ?
C8 N4 Zn6 116.1(5) . . ?
C9 N4 Zn6 118.2(5) . . ?
C8 N4 Zn5 118.6(5) . . ?
C9 N4 Zn5 107.1(5) . . ?
Zn6 N4 Zn5 68.2(2) . . ?
Si1 N20 Si2 122.1(3) . . ?
Si1 N20 Zn9 120.3(3) . . ?
Si2 N20 Zn9 117.6(3) . . ?
C36 N9 C39 122.0(7) . . ?
C36 N9 C40 124.6(6) . . ?
C39 N9 C40 113.1(6) . . ?
C30B N15 C29 116.8(10) . . ?
C29 N15 C30A 112.8(8) . . ?
C30B N15 Zn4 111.6(9) . . ?
C29 N15 Zn4 114.9(5) . . ?
C30A N15 Zn4 128.9(7) . . ?
C30B N15 Zn3 120.8(9) . . ?
C29 N15 Zn3 113.1(5) . . ?
C30A N15 Zn3 105.5(7) . . ?
Zn4 N15 Zn3 71.3(2) . . ?
C15 N17 C21 118.3(6) . . ?
C15 N17 Zn1 114.3(5) . . ?
C21 N17 Zn1 118.8(5) . . ?
C15 N17 Zn4 114.8(5) . . ?
C21 N17 Zn4 113.2(4) . . ?
Zn1 N17 Zn4 67.0(2) . . ?
C42 C41 C40 109.1(7) . . ?
C11 C10 C9 108.7(6) . . ?
C1 N1 C2 116.6(6) . . ?
C1 N1 Zn4 117.9(5) . . ?
C2 N1 Zn4 117.6(5) . . ?
C1 N1 Zn8 117.3(5) . . ?
C2 N1 Zn8 111.9(4) . . ?
Zn4 N1 Zn8 65.3(3) . . ?
C15 N16 C16 117.4(7) . . ?
C15 N16 Zn3 117.7(5) . . ?
C16 N16 Zn3 115.1(5) . . ?
C15 N16 Zn2 117.0(5) . . ?
C16 N16 Zn2 111.9(6) . . ?
Zn3 N16 Zn2 68.5(3) . . ?
C36 N8 C42 118.5(7) . . ?
C36 N8 Zn7 112.6(6) . . ?
C42 N8 Zn7 116.7(5) . . ?
C36 N8 Zn6 115.0(5) . . ?
C42 N8 Zn6 114.9(5) . . ?
Zn7 N8 Zn6 69.8(3) . . ?
N6 C11 C10 111.5(6) . . ?
N17 C21 C20 111.5(6) . . ?
N1 C1 N2 117.7(6) . . ?
N1 C1 N3 122.8(6) . . ?
N2 C1 N3 119.5(6) . . ?
N6 C12 C13 112.3(6) . . ?
N5 C8 N4 119.2(6) . . ?
N5 C8 N6 123.3(7) . . ?
N4 C8 N6 117.4(7) . . ?
N18 C15 N17 121.2(7) . . ?
N18 C15 N16 121.1(7) . . ?
N17 C15 N16 117.6(7) . . ?
N3 C5 C6 110.4(6) . . ?
C16 C17 C18 107.5(7) . . ?
N4 C9 C10 109.9(6) . . ?
C6 C7 N2 112.3(6) . . ?
N14 C33 C35B 111.8(8) . . ?
N14 C33 C35A 111.3(8) . . ?
C7 C6 C5 108.9(7) . . ?
C38 C37 N7 112.4(7) . . ?
C2 C3 C4 108.5(7) . . ?
N9 C39 C38 110.7(7) . . ?
N18 C18 C17 111.5(7) . . ?
N16 C16 C17 112.4(7) . . ?
N7 C36 N8 115.7(7) . . ?
N7 C36 N9 125.3(7) . . ?
N8 C36 N9 119.0(7) . . ?
N8 C42 C41 111.8(6) . . ?
C21 C20 C19 109.8(6) . . ?
N18 C19 C20 112.0(7) . . ?
C29 N14 C32 125.4(7) . . ?
C29 N14 C33 120.8(7) . . ?
C32 N14 C33 113.7(6) . . ?
N13 C29 N15 117.0(7) . . ?
N13 C29 N14 123.7(7) . . ?
N15 C29 N14 119.4(8) . . ?
N5 C14 C13 112.5(7) . . ?
C14 C13 C12 106.5(7) . . ?
N14 C32 C31B 112.7(8) . . ?
N14 C32 C31A 106.1(9) . . ?
C34B C35A C33 105.8(11) . . ?
C33 C35B C34A 110.7(13) . . ?
C30B C31A C32 99.1(12) . . ?
C35B C34A N13 102.7(13) . . ?
C31B C30A N15 112.6(12) . . ?
C30A C31B C32 103.6(12) . . ?
N13 C34B C35A 107.2(11) . . ?
N15 C30B C31A 108.5(14) . . ?
C62 C61 N65 114.4(9) . . ?
C61 C62 C63 114.2(11) . . ?
C63 N64 C70 126.5(9) . . ?
C63 N64 C69 111.0(9) . . ?
C70 N64 C69 121.4(8) . . ?
C69 C68 C67 101.4(14) . . ?
C68A C67 N66 116.4(11) . . ?
C68A C67 C68 59.7(11) . . ?
N66 C67 C68 106.6(10) . . ?
N64 C69 C68A 113.5(11) . . ?
N64 C69 C68 103.5(11) . . ?
C68A C69 C68 58.4(11) . . ?
C70 N65 C61 119.0(7) . . ?
C70 N65 Zn3 116.3(6) . . ?
C61 N65 Zn3 117.1(6) . . ?
C70 N65 Zn7 109.8(6) . . ?
C61 N65 Zn7 114.7(6) . . ?
Zn3 N65 Zn7 69.4(3) . . ?
N64 C63 C62 113.4(10) . . ?
C70 N66 C67 118.4(7) . . ?
C70 N66 Zn2 117.1(6) . . ?
C67 N66 Zn2 119.2(6) . . ?
C70 N66 Zn6 110.6(5) . . ?
C67 N66 Zn6 109.9(5) . . ?
Zn2 N66 Zn6 70.3(3) . . ?
N66 C70 N65 121.9(8) . . ?
N66 C70 N64 121.6(8) . . ?
N65 C70 N64 116.4(8) . . ?
C67 C68A C69 107.8(15) . . ?
_diffrn_measured_fraction_theta_max 0.945
_diffrn_reflns_theta_full 23.25
_diffrn_measured_fraction_theta_full 0.945
_refine_diff_density_max 0.380
_refine_diff_density_min -0.232
_refine_diff_density_rms 0.049