# Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2006

data_global
_journal_name_full               Chem.Commun.

_journal_coden_Cambridge         0182

_publ_contact_author_name        'M. Ephritikhine'
_publ_contact_author_address     
;
Laboratoire de Chimie de coordinati
Service de Chimie Moleculaire
CEA Saclay, Batiment 125
Gif sur Yvette
Gif sur Yvette
F91191
FRANCE
;

_publ_contact_author_email       MICHEL.EPHRITIKHINE@CEA.FR

_publ_section_title              
;
Reductive coupling of carbodiimides with metallic
lithium: a new route to metal oxalamidino complexes
;
loop_
_publ_author_name
'M. Ephritikhine'
'Pierre Thuery'
'Claude Villiers'

data_1
_database_code_depnum_ccdc_archive 'CCDC 287348'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C50 H48 Li2 N8'
_chemical_formula_weight         774.84

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'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P c a 21'

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

_cell_length_a                   17.7798(8)
_cell_length_b                   15.1565(6)
_cell_length_c                   15.7185(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4235.8(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    130067
_cell_measurement_theta_min      2.19
_cell_measurement_theta_max      25.68

_exptl_crystal_description       parallelepiped
_exptl_crystal_colour            'translucent light yellow'
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.215
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1640
_exptl_absorpt_coefficient_mu    0.072
_exptl_absorpt_correction_type   none
_exptl_special_details           'crystal-to-detector distance 30 mm'
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method       'two \f and four \w scans with 2\% steps'
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        none
_diffrn_reflns_number            130067
_diffrn_reflns_av_R_equivalents  0.0222
_diffrn_reflns_av_sigmaI/netI    0.0227
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.19
_diffrn_reflns_theta_max         25.68
_reflns_number_total             4178
_reflns_number_gt                3810
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'COLLECT (Hooft, 1998)'
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1999)'
_computing_publication_material  
'SHELXTL (Sheldrick, 1999); PLATON (Spek, 2003)'

_refine_special_details          
;
Structure solved by direct methods and subsequent Fourier-difference
synthesis. All non-hydrogen atoms were refined with anisotropic
displacement parameters. The H atoms were introduced at calculated
positions and were treated as riding atoms with an isotropic displacement
parameter equal to 1.2 (CH) or 1.5 (CH~3~) times that of the
parent atom. In the absence of suitable scatterers, the absolute
structure cannot be determined from the value of the Flack parameter.
The Friedel pairs have in consequence been merged.
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0598P)^2^+0.4300P] 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   -1.6(19)
_refine_ls_number_reflns         4178
_refine_ls_number_parameters     545
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0431
_refine_ls_R_factor_gt           0.0374
_refine_ls_wR_factor_ref         0.0950
_refine_ls_wR_factor_gt          0.0920
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_restrained_S_all      1.066
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.68
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.178
_refine_diff_density_min         -0.146
_refine_diff_density_rms         0.034

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
Li1 Li 0.2513(2) 0.1729(3) 0.5244(3) 0.0387(9) Uani 1 1 d . . .
Li2 Li 0.0029(2) 0.3736(3) 0.4794(3) 0.0385(9) Uani 1 1 d . . .
N1 N 0.13954(11) 0.16267(13) 0.54092(14) 0.0333(5) Uani 1 1 d . . .
N2 N 0.22409(11) 0.29209(13) 0.48073(14) 0.0331(4) Uani 1 1 d . . .
N3 N 0.11287(11) 0.38209(13) 0.46150(14) 0.0329(4) Uani 1 1 d . . .
N4 N 0.03045(11) 0.25847(13) 0.53118(14) 0.0343(5) Uani 1 1 d . . .
N5 N 0.32233(12) 0.14795(13) 0.62859(14) 0.0352(5) Uani 1 1 d . . .
N6 N 0.30205(12) 0.08950(14) 0.43154(15) 0.0385(5) Uani 1 1 d . . .
N7 N -0.04123(12) 0.46914(15) 0.55810(15) 0.0400(5) Uani 1 1 d . . .
N8 N -0.06652(12) 0.35565(14) 0.37370(15) 0.0390(5) Uani 1 1 d . . .
C1 C 0.10198(13) 0.23717(15) 0.52353(16) 0.0319(5) Uani 1 1 d . . .
C2 C 0.15160(13) 0.31103(15) 0.48560(16) 0.0311(5) Uani 1 1 d . . .
C3 C 0.10609(13) 0.07895(16) 0.53904(16) 0.0319(5) Uani 1 1 d . . .
C4 C 0.04389(13) 0.05629(16) 0.48841(17) 0.0338(5) Uani 1 1 d . . .
H4 H 0.0157 0.1007 0.4629 0.041 Uiso 1 1 calc R . .
C5 C 0.02379(14) -0.03124(16) 0.47587(17) 0.0353(5) Uani 1 1 d . . .
H5 H -0.0165 -0.0442 0.4403 0.042 Uiso 1 1 calc R . .
C6 C 0.06226(14) -0.10038(16) 0.51509(17) 0.0366(6) Uani 1 1 d . . .
C7 C 0.12153(14) -0.07799(16) 0.56840(17) 0.0365(6) Uani 1 1 d . . .
H7 H 0.1474 -0.1224 0.5968 0.044 Uiso 1 1 calc R . .
C8 C 0.14312(14) 0.00923(16) 0.58028(16) 0.0342(5) Uani 1 1 d . . .
H8 H 0.1831 0.0217 0.6165 0.041 Uiso 1 1 calc R . .
C9 C 0.03897(17) -0.19488(17) 0.5001(2) 0.0484(7) Uani 1 1 d . . .
H9A H 0.0743 -0.2337 0.5270 0.073 Uiso 1 1 calc R . .
H9B H 0.0380 -0.2065 0.4401 0.073 Uiso 1 1 calc R . .
H9C H -0.0102 -0.2045 0.5236 0.073 Uiso 1 1 calc R . .
C10 C 0.27265(13) 0.33179(15) 0.42147(16) 0.0323(5) Uani 1 1 d . . .
C11 C 0.25134(15) 0.35565(15) 0.33909(16) 0.0350(6) Uani 1 1 d . . .
H11 H 0.2005 0.3575 0.3251 0.042 Uiso 1 1 calc R . .
C12 C 0.30430(14) 0.37648(15) 0.27789(18) 0.0370(6) Uani 1 1 d . . .
H12 H 0.2882 0.3900 0.2231 0.044 Uiso 1 1 calc R . .
C13 C 0.38067(15) 0.37784(16) 0.29555(18) 0.0381(6) Uani 1 1 d . . .
C14 C 0.40227(15) 0.35795(17) 0.37826(18) 0.0394(6) Uani 1 1 d . . .
H14 H 0.4530 0.3598 0.3927 0.047 Uiso 1 1 calc R . .
C15 C 0.34952(14) 0.33529(16) 0.44004(18) 0.0359(6) Uani 1 1 d . . .
H15 H 0.3658 0.3222 0.4948 0.043 Uiso 1 1 calc R . .
C16 C 0.43750(16) 0.40163(19) 0.2285(2) 0.0466(7) Uani 1 1 d . . .
H16A H 0.4187 0.3849 0.1735 0.070 Uiso 1 1 calc R . .
H16B H 0.4838 0.3711 0.2395 0.070 Uiso 1 1 calc R . .
H16C H 0.4463 0.4641 0.2295 0.070 Uiso 1 1 calc R . .
C17 C 0.14574(13) 0.46523(15) 0.44923(16) 0.0322(5) Uani 1 1 d . . .
C18 C 0.20195(14) 0.49977(17) 0.50159(18) 0.0373(6) Uani 1 1 d . . .
H18 H 0.2248 0.4641 0.5422 0.045 Uiso 1 1 calc R . .
C19 C 0.22385(15) 0.58785(16) 0.49298(19) 0.0414(6) Uani 1 1 d . . .
H19 H 0.2605 0.6102 0.5293 0.050 Uiso 1 1 calc R . .
C20 C 0.19274(15) 0.64314(16) 0.4321(2) 0.0412(6) Uani 1 1 d . . .
C21 C 0.13725(15) 0.60859(16) 0.37954(18) 0.0377(6) Uani 1 1 d . . .
H21 H 0.1155 0.6441 0.3380 0.045 Uiso 1 1 calc R . .
C22 C 0.11384(14) 0.52146(16) 0.38840(17) 0.0357(6) Uani 1 1 d . . .
H22 H 0.0761 0.5000 0.3531 0.043 Uiso 1 1 calc R . .
C23 C 0.21996(17) 0.73655(17) 0.4221(2) 0.0517(7) Uani 1 1 d . . .
H23A H 0.2664 0.7368 0.3910 0.078 Uiso 1 1 calc R . .
H23B H 0.2278 0.7622 0.4772 0.078 Uiso 1 1 calc R . .
H23C H 0.1830 0.7703 0.3917 0.078 Uiso 1 1 calc R . .
C24 C -0.02027(14) 0.21301(15) 0.58425(17) 0.0343(5) Uani 1 1 d . . .
C25 C -0.00206(15) 0.18475(18) 0.66592(17) 0.0389(6) Uani 1 1 d . . .
H25 H 0.0471 0.1900 0.6854 0.047 Uiso 1 1 calc R . .
C26 C -0.05662(16) 0.14879(18) 0.71861(19) 0.0427(6) Uani 1 1 d . . .
H26 H -0.0429 0.1306 0.7730 0.051 Uiso 1 1 calc R . .
C27 C -0.13077(15) 0.13891(17) 0.69323(18) 0.0396(6) Uani 1 1 d . . .
C28 C -0.14913(15) 0.16873(18) 0.61235(19) 0.0415(6) Uani 1 1 d . . .
H28 H -0.1986 0.1640 0.5936 0.050 Uiso 1 1 calc R . .
C29 C -0.09560(14) 0.20541(17) 0.55893(19) 0.0394(6) Uani 1 1 d . . .
H29 H -0.1099 0.2253 0.5053 0.047 Uiso 1 1 calc R . .
C30 C -0.18920(17) 0.09641(19) 0.7493(2) 0.0499(7) Uani 1 1 d . . .
H30A H -0.2329 0.1335 0.7521 0.075 Uiso 1 1 calc R . .
H30B H -0.1690 0.0886 0.8055 0.075 Uiso 1 1 calc R . .
H30C H -0.2029 0.0401 0.7261 0.075 Uiso 1 1 calc R . .
C31 C 0.30532(17) 0.17564(17) 0.70666(19) 0.0426(6) Uani 1 1 d . . .
H31 H 0.2615 0.2084 0.7139 0.051 Uiso 1 1 calc R . .
C32 C 0.34871(18) 0.15865(19) 0.77730(19) 0.0496(7) Uani 1 1 d . . .
H32 H 0.3348 0.1801 0.8305 0.060 Uiso 1 1 calc R . .
C33 C 0.41380(17) 0.10882(19) 0.76758(19) 0.0484(7) Uani 1 1 d . . .
H33 H 0.4437 0.0951 0.8143 0.058 Uiso 1 1 calc R . .
C34 C 0.43303(16) 0.08029(19) 0.68736(19) 0.0432(6) Uani 1 1 d . . .
H34 H 0.4767 0.0479 0.6784 0.052 Uiso 1 1 calc R . .
C35 C 0.38620(14) 0.10080(18) 0.62087(18) 0.0392(6) Uani 1 1 d . . .
H35 H 0.3994 0.0809 0.5670 0.047 Uiso 1 1 calc R . .
C36 C 0.30538(15) 0.00203(18) 0.44360(18) 0.0411(6) Uani 1 1 d . . .
H36 H 0.2842 -0.0210 0.4929 0.049 Uiso 1 1 calc R . .
C37 C 0.33837(16) -0.05571(18) 0.38709(19) 0.0426(6) Uani 1 1 d . . .
H37 H 0.3406 -0.1157 0.3993 0.051 Uiso 1 1 calc R . .
C38 C 0.36762(15) -0.02386(18) 0.31328(19) 0.0426(6) Uani 1 1 d . . .
H38 H 0.3891 -0.0618 0.2736 0.051 Uiso 1 1 calc R . .
C39 C 0.36474(16) 0.06541(18) 0.29849(18) 0.0435(6) Uani 1 1 d . . .
H39 H 0.3842 0.0890 0.2485 0.052 Uiso 1 1 calc R . .
C40 C 0.33247(16) 0.11958(18) 0.35896(17) 0.0409(6) Uani 1 1 d . . .
H40 H 0.3318 0.1800 0.3489 0.049 Uiso 1 1 calc R . .
C41 C -0.09906(15) 0.44916(19) 0.6091(2) 0.0457(7) Uani 1 1 d . . .
H41 H -0.1201 0.3931 0.6051 0.055 Uiso 1 1 calc R . .
C42 C -0.12917(16) 0.5076(2) 0.6678(2) 0.0498(7) Uani 1 1 d . . .
H42 H -0.1696 0.4914 0.7019 0.060 Uiso 1 1 calc R . .
C43 C -0.09775(19) 0.5901(2) 0.6742(2) 0.0515(7) Uani 1 1 d . . .
H43 H -0.1171 0.6312 0.7123 0.062 Uiso 1 1 calc R . .
C44 C -0.03799(18) 0.61080(18) 0.6241(2) 0.0472(7) Uani 1 1 d . . .
H44 H -0.0151 0.6658 0.6288 0.057 Uiso 1 1 calc R . .
C45 C -0.01146(16) 0.55006(18) 0.56640(19) 0.0427(6) Uani 1 1 d . . .
H45 H 0.0288 0.5657 0.5317 0.051 Uiso 1 1 calc R . .
C46 C -0.12453(15) 0.40462(17) 0.3475(2) 0.0436(6) Uani 1 1 d . . .
H46 H -0.1383 0.4530 0.3804 0.052 Uiso 1 1 calc R . .
C47 C -0.16506(18) 0.38770(19) 0.2749(2) 0.0534(8) Uani 1 1 d . . .
H47 H -0.2049 0.4241 0.2592 0.064 Uiso 1 1 calc R . .
C48 C -0.14566(19) 0.3154(2) 0.2251(2) 0.0544(8) Uani 1 1 d . . .
H48 H -0.1718 0.3026 0.1753 0.065 Uiso 1 1 calc R . .
C49 C -0.08643(18) 0.26304(19) 0.25159(19) 0.0485(7) Uani 1 1 d . . .
H49 H -0.0723 0.2135 0.2205 0.058 Uiso 1 1 calc R . .
C50 C -0.04898(17) 0.28571(18) 0.32475(18) 0.0447(6) Uani 1 1 d . . .
H50 H -0.0089 0.2505 0.3416 0.054 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Li1 0.036(2) 0.034(2) 0.046(3) 0.0011(19) -0.001(2) 0.0013(18)
Li2 0.033(2) 0.037(2) 0.045(2) 0.000(2) 0.001(2) -0.0003(17)
N1 0.0320(10) 0.0290(10) 0.0388(12) 0.0024(9) -0.0001(9) -0.0012(8)
N2 0.0305(10) 0.0303(10) 0.0385(11) 0.0020(9) 0.0015(9) -0.0015(8)
N3 0.0319(10) 0.0271(9) 0.0396(11) 0.0031(9) 0.0011(9) -0.0008(8)
N4 0.0321(10) 0.0322(10) 0.0386(12) 0.0007(9) 0.0040(9) -0.0029(8)
N5 0.0336(11) 0.0346(10) 0.0375(12) 0.0029(9) 0.0032(10) 0.0004(8)
N6 0.0345(11) 0.0415(11) 0.0395(12) -0.0038(10) -0.0047(10) 0.0027(9)
N7 0.0382(12) 0.0412(12) 0.0406(12) -0.0010(10) -0.0043(10) 0.0065(9)
N8 0.0413(12) 0.0307(10) 0.0450(13) 0.0017(10) 0.0014(10) 0.0003(9)
C1 0.0313(12) 0.0298(12) 0.0345(13) 0.0000(10) -0.0011(10) -0.0019(10)
C2 0.0341(12) 0.0282(12) 0.0311(12) -0.0004(10) -0.0011(11) -0.0006(9)
C3 0.0316(12) 0.0312(12) 0.0328(13) 0.0024(10) 0.0052(10) 0.0017(10)
C4 0.0350(12) 0.0309(12) 0.0355(13) 0.0032(11) 0.0041(11) 0.0026(10)
C5 0.0327(12) 0.0380(13) 0.0352(13) 0.0017(11) -0.0004(11) -0.0045(10)
C6 0.0367(13) 0.0314(13) 0.0418(14) 0.0019(11) 0.0048(12) -0.0019(10)
C7 0.0353(13) 0.0336(13) 0.0407(14) 0.0053(11) 0.0041(12) 0.0012(10)
C8 0.0325(12) 0.0337(12) 0.0363(14) 0.0038(11) 0.0005(11) 0.0004(10)
C9 0.0490(16) 0.0309(13) 0.065(2) -0.0002(14) 0.0011(15) -0.0020(12)
C10 0.0342(12) 0.0254(11) 0.0373(13) -0.0006(10) 0.0038(11) -0.0013(9)
C11 0.0336(12) 0.0313(11) 0.0400(14) -0.0004(11) -0.0027(11) -0.0016(10)
C12 0.0411(13) 0.0295(12) 0.0403(14) 0.0006(11) -0.0003(12) 0.0001(10)
C13 0.0416(14) 0.0289(12) 0.0437(15) -0.0028(11) 0.0079(12) -0.0024(10)
C14 0.0335(13) 0.0346(13) 0.0500(16) -0.0004(12) 0.0001(12) -0.0036(10)
C15 0.0342(13) 0.0335(12) 0.0401(14) 0.0006(11) -0.0011(11) -0.0001(10)
C16 0.0474(16) 0.0421(15) 0.0504(16) -0.0004(13) 0.0139(14) -0.0039(12)
C17 0.0291(12) 0.0291(11) 0.0385(13) 0.0007(10) 0.0034(10) 0.0006(9)
C18 0.0363(13) 0.0340(12) 0.0415(15) -0.0003(11) -0.0016(11) 0.0008(10)
C19 0.0386(13) 0.0351(13) 0.0505(16) -0.0042(13) -0.0049(13) -0.0033(10)
C20 0.0388(14) 0.0306(12) 0.0541(16) 0.0022(12) 0.0054(13) -0.0002(11)
C21 0.0382(13) 0.0302(12) 0.0447(14) 0.0040(11) 0.0008(12) 0.0015(10)
C22 0.0337(13) 0.0310(12) 0.0423(14) -0.0005(11) -0.0014(11) -0.0018(10)
C23 0.0487(16) 0.0311(13) 0.075(2) -0.0005(14) 0.0026(16) -0.0031(11)
C24 0.0347(13) 0.0255(11) 0.0425(14) -0.0025(10) 0.0031(11) 0.0007(9)
C25 0.0359(13) 0.0391(14) 0.0416(14) 0.0028(11) -0.0002(12) -0.0014(11)
C26 0.0463(16) 0.0410(14) 0.0409(15) 0.0034(12) 0.0042(13) -0.0012(12)
C27 0.0406(14) 0.0312(12) 0.0469(16) -0.0037(11) 0.0104(12) -0.0026(10)
C28 0.0322(13) 0.0431(14) 0.0493(16) -0.0034(12) 0.0027(12) -0.0032(11)
C29 0.0351(13) 0.0409(14) 0.0422(14) 0.0008(12) -0.0002(12) -0.0018(11)
C30 0.0471(16) 0.0439(15) 0.0588(19) -0.0025(14) 0.0181(15) -0.0068(12)
C31 0.0475(15) 0.0347(13) 0.0457(16) -0.0030(12) 0.0066(13) -0.0004(11)
C32 0.0630(19) 0.0481(16) 0.0378(16) -0.0086(13) 0.0058(14) -0.0097(14)
C33 0.0484(16) 0.0536(17) 0.0434(16) 0.0077(13) -0.0106(13) -0.0087(13)
C34 0.0380(14) 0.0466(15) 0.0450(16) 0.0051(13) -0.0031(12) 0.0028(12)
C35 0.0343(13) 0.0446(14) 0.0386(14) 0.0008(12) 0.0006(12) 0.0012(11)
C36 0.0436(14) 0.0397(13) 0.0400(14) 0.0006(12) 0.0034(12) -0.0049(11)
C37 0.0447(15) 0.0341(13) 0.0490(16) -0.0042(12) -0.0041(13) -0.0025(11)
C38 0.0416(14) 0.0424(15) 0.0439(16) -0.0139(12) -0.0021(12) 0.0001(12)
C39 0.0517(16) 0.0444(15) 0.0342(14) -0.0025(12) 0.0030(13) -0.0107(13)
C40 0.0483(15) 0.0351(13) 0.0392(15) 0.0002(11) -0.0073(12) 0.0008(12)
C41 0.0348(13) 0.0479(15) 0.0543(17) -0.0011(13) -0.0048(13) 0.0007(12)
C42 0.0380(15) 0.0612(19) 0.0502(17) 0.0027(15) 0.0059(13) 0.0037(13)
C43 0.0596(18) 0.0505(17) 0.0443(16) -0.0053(14) 0.0046(15) 0.0129(14)
C44 0.0561(17) 0.0391(14) 0.0465(16) -0.0009(13) -0.0004(14) 0.0019(12)
C45 0.0435(15) 0.0422(14) 0.0424(15) 0.0051(12) 0.0015(13) 0.0050(12)
C46 0.0400(14) 0.0315(13) 0.0593(18) 0.0021(12) -0.0027(13) 0.0027(11)
C47 0.0460(16) 0.0396(15) 0.075(2) 0.0053(15) -0.0165(16) 0.0050(12)
C48 0.0612(19) 0.0479(17) 0.0540(18) 0.0041(15) -0.0134(16) -0.0087(14)
C49 0.0648(19) 0.0371(14) 0.0436(16) -0.0008(12) -0.0010(14) 0.0025(13)
C50 0.0543(16) 0.0359(13) 0.0437(16) 0.0033(12) -0.0002(14) 0.0086(12)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
Li1 N2 1.992(4) . ?
Li1 N1 2.009(5) . ?
Li1 N5 2.103(5) . ?
Li1 N6 2.131(5) . ?
Li2 N3 1.979(5) . ?
Li2 N4 1.987(5) . ?
Li2 N7 2.060(5) . ?
Li2 N8 2.088(5) . ?
N1 C1 1.340(3) . ?
N1 C3 1.402(3) . ?
N2 C2 1.323(3) . ?
N2 C10 1.405(3) . ?
N3 C2 1.333(3) . ?
N3 C17 1.402(3) . ?
N4 C1 1.318(3) . ?
N4 C24 1.408(3) . ?
N5 C31 1.332(4) . ?
N5 C35 1.347(3) . ?
N6 C36 1.340(3) . ?
N6 C40 1.342(4) . ?
N7 C41 1.339(4) . ?
N7 C45 1.342(4) . ?
N8 C46 1.336(3) . ?
N8 C50 1.346(4) . ?
C1 C2 1.545(3) . ?
C3 C4 1.405(4) . ?
C3 C8 1.404(3) . ?
C4 C5 1.388(3) . ?
C4 H4 0.9300 . ?
C5 C6 1.395(4) . ?
C5 H5 0.9300 . ?
C6 C7 1.388(4) . ?
C6 C9 1.510(3) . ?
C7 C8 1.389(4) . ?
C7 H7 0.9300 . ?
C8 H8 0.9300 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 C15 1.399(4) . ?
C10 C11 1.397(4) . ?
C11 C12 1.383(4) . ?
C11 H11 0.9300 . ?
C12 C13 1.386(4) . ?
C12 H12 0.9300 . ?
C13 C14 1.389(4) . ?
C13 C16 1.504(4) . ?
C14 C15 1.393(4) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 C18 1.396(4) . ?
C17 C22 1.401(4) . ?
C18 C19 1.397(4) . ?
C18 H18 0.9300 . ?
C19 C20 1.387(4) . ?
C19 H19 0.9300 . ?
C20 C21 1.389(4) . ?
C20 C23 1.504(4) . ?
C21 C22 1.392(3) . ?
C21 H21 0.9300 . ?
C22 H22 0.9300 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 C25 1.392(4) . ?
C24 C29 1.402(4) . ?
C25 C26 1.387(4) . ?
C25 H25 0.9300 . ?
C26 C27 1.386(4) . ?
C26 H26 0.9300 . ?
C27 C28 1.388(4) . ?
C27 C30 1.507(4) . ?
C28 C29 1.386(4) . ?
C28 H28 0.9300 . ?
C29 H29 0.9300 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C31 C32 1.376(4) . ?
C31 H31 0.9300 . ?
C32 C33 1.390(4) . ?
C32 H32 0.9300 . ?
C33 C34 1.376(4) . ?
C33 H33 0.9300 . ?
C34 C35 1.372(4) . ?
C34 H34 0.9300 . ?
C35 H35 0.9300 . ?
C36 C37 1.378(4) . ?
C36 H36 0.9300 . ?
C37 C38 1.360(4) . ?
C37 H37 0.9300 . ?
C38 C39 1.374(4) . ?
C38 H38 0.9300 . ?
C39 C40 1.381(4) . ?
C39 H39 0.9300 . ?
C40 H40 0.9300 . ?
C41 C42 1.386(4) . ?
C41 H41 0.9300 . ?
C42 C43 1.373(5) . ?
C42 H42 0.9300 . ?
C43 C44 1.360(4) . ?
C43 H43 0.9300 . ?
C44 C45 1.376(4) . ?
C44 H44 0.9300 . ?
C45 H45 0.9300 . ?
C46 C47 1.375(4) . ?
C46 H46 0.9300 . ?
C47 C48 1.390(5) . ?
C47 H47 0.9300 . ?
C48 C49 1.383(4) . ?
C48 H48 0.9300 . ?
C49 C50 1.373(4) . ?
C49 H49 0.9300 . ?
C50 H50 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Li1 N1 82.80(18) . . ?
N2 Li1 N5 125.2(2) . . ?
N1 Li1 N5 118.6(2) . . ?
N2 Li1 N6 113.9(2) . . ?
N1 Li1 N6 117.5(2) . . ?
N5 Li1 N6 99.9(2) . . ?
N3 Li2 N4 82.66(18) . . ?
N3 Li2 N7 114.6(2) . . ?
N4 Li2 N7 117.7(3) . . ?
N3 Li2 N8 118.7(2) . . ?
N4 Li2 N8 110.9(2) . . ?
N7 Li2 N8 110.1(2) . . ?
C1 N1 C3 123.2(2) . . ?
C1 N1 Li1 113.65(19) . . ?
C3 N1 Li1 119.11(19) . . ?
C2 N2 C10 123.0(2) . . ?
C2 N2 Li1 114.4(2) . . ?
C10 N2 Li1 117.9(2) . . ?
C2 N3 C17 123.3(2) . . ?
C2 N3 Li2 114.7(2) . . ?
C17 N3 Li2 119.3(2) . . ?
C1 N4 C24 123.5(2) . . ?
C1 N4 Li2 114.5(2) . . ?
C24 N4 Li2 121.0(2) . . ?
C31 N5 C35 116.2(2) . . ?
C31 N5 Li1 121.6(2) . . ?
C35 N5 Li1 122.1(2) . . ?
C36 N6 C40 116.0(2) . . ?
C36 N6 Li1 120.6(2) . . ?
C40 N6 Li1 123.4(2) . . ?
C41 N7 C45 116.8(2) . . ?
C41 N7 Li2 119.6(2) . . ?
C45 N7 Li2 123.4(2) . . ?
C46 N8 C50 116.1(3) . . ?
C46 N8 Li2 129.0(2) . . ?
C50 N8 Li2 114.8(2) . . ?
N4 C1 N1 132.0(2) . . ?
N4 C1 C2 114.1(2) . . ?
N1 C1 C2 113.9(2) . . ?
N2 C2 N3 131.5(2) . . ?
N2 C2 C1 114.9(2) . . ?
N3 C2 C1 113.6(2) . . ?
C4 C3 C8 116.5(2) . . ?
C4 C3 N1 124.6(2) . . ?
C8 C3 N1 118.2(2) . . ?
C5 C4 C3 121.1(2) . . ?
C5 C4 H4 119.4 . . ?
C3 C4 H4 119.4 . . ?
C4 C5 C6 121.9(2) . . ?
C4 C5 H5 119.0 . . ?
C6 C5 H5 119.0 . . ?
C7 C6 C5 117.1(2) . . ?
C7 C6 C9 122.3(2) . . ?
C5 C6 C9 120.6(2) . . ?
C6 C7 C8 121.6(2) . . ?
C6 C7 H7 119.2 . . ?
C8 C7 H7 119.2 . . ?
C7 C8 C3 121.7(2) . . ?
C7 C8 H8 119.2 . . ?
C3 C8 H8 119.2 . . ?
C6 C9 H9A 109.5 . . ?
C6 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C6 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C15 C10 C11 116.7(2) . . ?
C15 C10 N2 118.6(2) . . ?
C11 C10 N2 124.0(2) . . ?
C12 C11 C10 121.3(2) . . ?
C12 C11 H11 119.4 . . ?
C10 C11 H11 119.4 . . ?
C11 C12 C13 122.1(3) . . ?
C11 C12 H12 119.0 . . ?
C13 C12 H12 119.0 . . ?
C12 C13 C14 117.1(2) . . ?
C12 C13 C16 121.4(3) . . ?
C14 C13 C16 121.5(3) . . ?
C15 C14 C13 121.3(2) . . ?
C15 C14 H14 119.3 . . ?
C13 C14 H14 119.3 . . ?
C14 C15 C10 121.4(3) . . ?
C14 C15 H15 119.3 . . ?
C10 C15 H15 119.3 . . ?
C13 C16 H16A 109.5 . . ?
C13 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C13 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C18 C17 C22 117.7(2) . . ?
C18 C17 N3 123.6(2) . . ?
C22 C17 N3 118.1(2) . . ?
C19 C18 C17 120.0(2) . . ?
C19 C18 H18 120.0 . . ?
C17 C18 H18 120.0 . . ?
C20 C19 C18 122.2(3) . . ?
C20 C19 H19 118.9 . . ?
C18 C19 H19 118.9 . . ?
C19 C20 C21 117.8(2) . . ?
C19 C20 C23 120.8(3) . . ?
C21 C20 C23 121.4(3) . . ?
C20 C21 C22 120.7(3) . . ?
C20 C21 H21 119.6 . . ?
C22 C21 H21 119.6 . . ?
C21 C22 C17 121.6(2) . . ?
C21 C22 H22 119.2 . . ?
C17 C22 H22 119.2 . . ?
C20 C23 H23A 109.5 . . ?
C20 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C20 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C25 C24 C29 117.3(2) . . ?
C25 C24 N4 123.2(2) . . ?
C29 C24 N4 118.9(2) . . ?
C26 C25 C24 120.6(3) . . ?
C26 C25 H25 119.7 . . ?
C24 C25 H25 119.7 . . ?
C27 C26 C25 122.4(3) . . ?
C27 C26 H26 118.8 . . ?
C25 C26 H26 118.8 . . ?
C26 C27 C28 116.9(3) . . ?
C26 C27 C30 122.3(3) . . ?
C28 C27 C30 120.8(3) . . ?
C27 C28 C29 121.6(3) . . ?
C27 C28 H28 119.2 . . ?
C29 C28 H28 119.2 . . ?
C28 C29 C24 121.1(3) . . ?
C28 C29 H29 119.4 . . ?
C24 C29 H29 119.4 . . ?
C27 C30 H30A 109.5 . . ?
C27 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C27 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
N5 C31 C32 123.9(3) . . ?
N5 C31 H31 118.1 . . ?
C32 C31 H31 118.1 . . ?
C31 C32 C33 118.7(3) . . ?
C31 C32 H32 120.7 . . ?
C33 C32 H32 120.7 . . ?
C34 C33 C32 118.6(3) . . ?
C34 C33 H33 120.7 . . ?
C32 C33 H33 120.7 . . ?
C33 C34 C35 118.4(3) . . ?
C33 C34 H34 120.8 . . ?
C35 C34 H34 120.8 . . ?
N5 C35 C34 124.3(3) . . ?
N5 C35 H35 117.9 . . ?
C34 C35 H35 117.9 . . ?
N6 C36 C37 123.8(3) . . ?
N6 C36 H36 118.1 . . ?
C37 C36 H36 118.1 . . ?
C38 C37 C36 119.2(3) . . ?
C38 C37 H37 120.4 . . ?
C36 C37 H37 120.4 . . ?
C37 C38 C39 118.7(3) . . ?
C37 C38 H38 120.7 . . ?
C39 C38 H38 120.7 . . ?
C38 C39 C40 119.0(3) . . ?
C38 C39 H39 120.5 . . ?
C40 C39 H39 120.5 . . ?
N6 C40 C39 123.4(2) . . ?
N6 C40 H40 118.3 . . ?
C39 C40 H40 118.3 . . ?
N7 C41 C42 123.4(3) . . ?
N7 C41 H41 118.3 . . ?
C42 C41 H41 118.3 . . ?
C43 C42 C41 118.3(3) . . ?
C43 C42 H42 120.8 . . ?
C41 C42 H42 120.8 . . ?
C44 C43 C42 119.0(3) . . ?
C44 C43 H43 120.5 . . ?
C42 C43 H43 120.5 . . ?
C43 C44 C45 119.7(3) . . ?
C43 C44 H44 120.1 . . ?
C45 C44 H44 120.1 . . ?
N7 C45 C44 122.7(3) . . ?
N7 C45 H45 118.6 . . ?
C44 C45 H45 118.6 . . ?
N8 C46 C47 123.9(3) . . ?
N8 C46 H46 118.1 . . ?
C47 C46 H46 118.1 . . ?
C46 C47 C48 119.0(3) . . ?
C46 C47 H47 120.5 . . ?
C48 C47 H47 120.5 . . ?
C49 C48 C47 118.2(3) . . ?
C49 C48 H48 120.9 . . ?
C47 C48 H48 120.9 . . ?
C50 C49 C48 118.6(3) . . ?
C50 C49 H49 120.7 . . ?
C48 C49 H49 120.7 . . ?
N8 C50 C49 124.3(3) . . ?
N8 C50 H50 117.9 . . ?
C49 C50 H50 117.9 . . ?

#===END

data_3.2py
_database_code_depnum_ccdc_archive 'CCDC 287349'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C86 H104 Cl8 Li2 N16 U2'
_chemical_formula_weight         2135.39

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 2/n'

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

_cell_length_a                   15.4340(5)
_cell_length_b                   24.5917(5)
_cell_length_c                   25.6952(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 107.322(2)
_cell_angle_gamma                90.00
_cell_volume                     9310.3(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    136445
_cell_measurement_theta_min      2.35
_cell_measurement_theta_max      25.68

_exptl_crystal_description       irregular
_exptl_crystal_colour            'translucent light green'
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.523
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             4232
_exptl_absorpt_coefficient_mu    3.755
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_correction_T_min  0.332
_exptl_absorpt_correction_T_max  0.687
_exptl_absorpt_process_details   'program DELABS from PLATON (Spek, 2003)'
_exptl_special_details           'crystal-to-detector distance 30 mm'
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method       'two \f scans with 2\% steps'
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        none
_diffrn_reflns_number            136445
_diffrn_reflns_av_R_equivalents  0.0836
_diffrn_reflns_av_sigmaI/netI    0.0722
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         2.35
_diffrn_reflns_theta_max         25.68
_reflns_number_total             17403
_reflns_number_gt                10272
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Kappa-CCD software (Nonius B.V., 1998)'
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1999)'
_computing_publication_material  
'SHELXTL (Sheldrick, 1999); PLATON (Spek, 2003)'

_refine_special_details          
;
Structure solved by direct methods and subsequent Fourier-difference
synthesis. All non-hydrogen atoms were refined with anisotropic
displacement parameters. The H atoms were introduced at calculated
positions and were treated as riding atoms with an isotropic displacement
parameter equal to 1.2 times that of the parent atom.
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0136P)^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_extinction_coef       ?
_refine_ls_number_reflns         17403
_refine_ls_number_parameters     1035
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0889
_refine_ls_R_factor_gt           0.0387
_refine_ls_wR_factor_ref         0.0758
_refine_ls_wR_factor_gt          0.0637
_refine_ls_goodness_of_fit_ref   0.975
_refine_ls_restrained_S_all      0.975
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_diffrn_measured_fraction_theta_max 0.984
_diffrn_reflns_theta_full        25.68
_diffrn_measured_fraction_theta_full 0.984
_refine_diff_density_max         0.494
_refine_diff_density_min         -0.878
_refine_diff_density_rms         0.111

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
U1 U 0.2500 0.363345(12) 0.7500 0.02501(10) Uani 1 2 d S . .
U2 U 0.2500 0.070062(12) 0.7500 0.02277(9) Uani 1 2 d S . .
Cl1A Cl 0.40354(13) 0.36229(6) 0.72461(7) 0.0324(4) Uani 1 1 d . . .
Cl2A Cl 0.15784(13) 0.40002(5) 0.65013(6) 0.0340(4) Uani 1 1 d . . .
Cl3A Cl 0.40738(12) 0.03526(5) 0.73830(6) 0.0291(4) Uani 1 1 d . . .
Cl4A Cl 0.18088(13) 0.06494(6) 0.64285(7) 0.0322(4) Uani 1 1 d . . .
N1A N 0.2106(4) 0.27675(16) 0.7052(2) 0.0242(13) Uani 1 1 d . . .
N2A N 0.3161(4) 0.15738(17) 0.7393(2) 0.0259(12) Uani 1 1 d . . .
N3A N 0.2500 0.4709(3) 0.7500 0.031(2) Uani 1 2 d S . .
N4A N 0.2500 -0.0393(3) 0.7500 0.0250(19) Uani 1 2 d S . .
C1A C 0.2500 0.2485(3) 0.7500 0.024(2) Uani 1 2 d S . .
C2A C 0.2500 0.1862(3) 0.7500 0.024(2) Uani 1 2 d S . .
C3A C 0.1640(4) 0.2504(2) 0.6531(2) 0.0245(14) Uani 1 1 d . . .
H3A H 0.1717 0.2110 0.6581 0.029 Uiso 1 1 calc R . .
C4A C 0.2025(5) 0.2673(2) 0.6079(2) 0.0357(16) Uani 1 1 d . . .
H4A1 H 0.2669 0.2591 0.6182 0.043 Uiso 1 1 calc R . .
H4A2 H 0.1952 0.3062 0.6019 0.043 Uiso 1 1 calc R . .
C5A C 0.1534(5) 0.2370(3) 0.5551(3) 0.0456(17) Uani 1 1 d . . .
H5A1 H 0.1766 0.2496 0.5260 0.055 Uiso 1 1 calc R . .
H5A2 H 0.1665 0.1985 0.5602 0.055 Uiso 1 1 calc R . .
C6A C 0.0510(5) 0.2454(3) 0.5383(3) 0.0464(18) Uani 1 1 d . . .
H6A1 H 0.0227 0.2225 0.5071 0.056 Uiso 1 1 calc R . .
H6A2 H 0.0373 0.2830 0.5274 0.056 Uiso 1 1 calc R . .
C7A C 0.0115(5) 0.2318(2) 0.5847(3) 0.0398(16) Uani 1 1 d . . .
H7A1 H 0.0165 0.1930 0.5917 0.048 Uiso 1 1 calc R . .
H7A2 H -0.0523 0.2414 0.5740 0.048 Uiso 1 1 calc R . .
C8A C 0.0624(4) 0.2630(2) 0.6369(2) 0.0290(14) Uani 1 1 d . . .
H8A1 H 0.0530 0.3017 0.6308 0.035 Uiso 1 1 calc R . .
H8A2 H 0.0383 0.2527 0.6663 0.035 Uiso 1 1 calc R . .
C9A C 0.3875(4) 0.1842(2) 0.7217(2) 0.0272(15) Uani 1 1 d . . .
H9A H 0.3779 0.2235 0.7224 0.033 Uiso 1 1 calc R . .
C10A C 0.4816(4) 0.1719(2) 0.7595(2) 0.0288(14) Uani 1 1 d . . .
H10A H 0.4938 0.1333 0.7589 0.035 Uiso 1 1 calc R . .
H10B H 0.4848 0.1820 0.7965 0.035 Uiso 1 1 calc R . .
C11A C 0.5533(4) 0.2043(2) 0.7409(3) 0.0343(15) Uani 1 1 d . . .
H11A H 0.5444 0.2429 0.7451 0.041 Uiso 1 1 calc R . .
H11B H 0.6135 0.1948 0.7640 0.041 Uiso 1 1 calc R . .
C12A C 0.5469(5) 0.1923(2) 0.6812(3) 0.0379(15) Uani 1 1 d . . .
H12A H 0.5879 0.2163 0.6699 0.045 Uiso 1 1 calc R . .
H12B H 0.5660 0.1552 0.6782 0.045 Uiso 1 1 calc R . .
C13A C 0.4510(4) 0.2001(2) 0.6434(3) 0.0364(15) Uani 1 1 d . . .
H13A H 0.4482 0.1879 0.6071 0.044 Uiso 1 1 calc R . .
H13B H 0.4359 0.2385 0.6413 0.044 Uiso 1 1 calc R . .
C14A C 0.3814(4) 0.1685(2) 0.6634(2) 0.0304(14) Uani 1 1 d . . .
H14A H 0.3207 0.1761 0.6398 0.037 Uiso 1 1 calc R . .
H14B H 0.3923 0.1298 0.6617 0.037 Uiso 1 1 calc R . .
C15A C 0.3262(5) 0.4986(2) 0.7536(3) 0.0352(18) Uani 1 1 d . . .
H15A H 0.3797 0.4795 0.7572 0.042 Uiso 1 1 calc R . .
C16A C 0.3279(5) 0.5551(2) 0.7521(3) 0.040(2) Uani 1 1 d . . .
H16A H 0.3808 0.5733 0.7525 0.048 Uiso 1 1 calc R . .
C17A C 0.2500 0.5837(4) 0.7500 0.047(3) Uani 1 2 d S . .
H17A H 0.2500 0.6215 0.7500 0.056 Uiso 1 2 calc SR . .
C18A C 0.1868(5) -0.0683(2) 0.7131(3) 0.0290(17) Uani 1 1 d . . .
H18A H 0.1422 -0.0494 0.6870 0.035 Uiso 1 1 calc R . .
C19A C 0.1839(5) -0.1245(2) 0.7114(3) 0.0352(18) Uani 1 1 d . . .
H19A H 0.1388 -0.1427 0.6850 0.042 Uiso 1 1 calc R . .
C20A C 0.2500 -0.1525(3) 0.7500 0.046(3) Uani 1 2 d S . .
H20A H 0.2500 -0.1904 0.7500 0.056 Uiso 1 2 calc SR . .
U3 U 0.2500 0.129821(12) 0.2500 0.02469(10) Uani 1 2 d S . .
U4 U 0.2500 0.423030(12) 0.2500 0.02249(9) Uani 1 2 d S . .
Cl1B Cl 0.15887(12) 0.09381(5) 0.14971(6) 0.0330(4) Uani 1 1 d . . .
Cl2B Cl 0.40539(13) 0.13072(6) 0.22722(7) 0.0323(4) Uani 1 1 d . . .
Cl3B Cl 0.18009(13) 0.42520(6) 0.14284(7) 0.0325(4) Uani 1 1 d . . .
Cl4B Cl 0.40692(11) 0.45794(5) 0.23822(6) 0.0287(4) Uani 1 1 d . . .
N1B N 0.2221(4) 0.21646(16) 0.2040(2) 0.0265(13) Uani 1 1 d . . .
N2B N 0.3222(4) 0.33611(17) 0.2482(2) 0.0249(12) Uani 1 1 d . . .
N3B N 0.2500 0.0220(3) 0.2500 0.028(2) Uani 1 2 d S . .
N4B N 0.2500 0.5338(3) 0.2500 0.029(2) Uani 1 2 d S . .
C1B C 0.2500 0.2451(3) 0.2500 0.023(2) Uani 1 2 d S . .
C2B C 0.2500 0.3077(3) 0.2500 0.024(2) Uani 1 2 d S . .
C3B C 0.1910(4) 0.2435(2) 0.1510(2) 0.0258(14) Uani 1 1 d . . .
H3B H 0.2030 0.2826 0.1561 0.031 Uiso 1 1 calc R . .
C4B C 0.0885(4) 0.2347(2) 0.1251(2) 0.0252(13) Uani 1 1 d . . .
H4B1 H 0.0759 0.1961 0.1196 0.030 Uiso 1 1 calc R . .
H4B2 H 0.0559 0.2482 0.1495 0.030 Uiso 1 1 calc R . .
C5B C 0.0557(4) 0.2645(2) 0.0703(2) 0.0320(14) Uani 1 1 d . . .
H5B1 H -0.0089 0.2586 0.0543 0.038 Uiso 1 1 calc R . .
H5B2 H 0.0659 0.3032 0.0761 0.038 Uiso 1 1 calc R . .
C6B C 0.1067(5) 0.2438(3) 0.0314(3) 0.0412(16) Uani 1 1 d . . .
H6B1 H 0.0878 0.2644 -0.0024 0.049 Uiso 1 1 calc R . .
H6B2 H 0.0920 0.2059 0.0229 0.049 Uiso 1 1 calc R . .
C7B C 0.2097(5) 0.2500(2) 0.0574(2) 0.0368(15) Uani 1 1 d . . .
H7B1 H 0.2411 0.2347 0.0333 0.044 Uiso 1 1 calc R . .
H7B2 H 0.2250 0.2883 0.0622 0.044 Uiso 1 1 calc R . .
C8B C 0.2413(4) 0.2214(2) 0.1124(2) 0.0293(15) Uani 1 1 d . . .
H8B1 H 0.3060 0.2268 0.1284 0.035 Uiso 1 1 calc R . .
H8B2 H 0.2302 0.1826 0.1073 0.035 Uiso 1 1 calc R . .
C9B C 0.4034(4) 0.3088(2) 0.2427(2) 0.0286(15) Uani 1 1 d . . .
H9B H 0.3962 0.2697 0.2475 0.034 Uiso 1 1 calc R . .
C10B C 0.4896(5) 0.3274(2) 0.2863(3) 0.0368(16) Uani 1 1 d . . .
H10C H 0.4828 0.3220 0.3222 0.044 Uiso 1 1 calc R . .
H10D H 0.4997 0.3658 0.2818 0.044 Uiso 1 1 calc R . .
C11B C 0.5709(5) 0.2943(2) 0.2807(3) 0.0468(18) Uani 1 1 d . . .
H11C H 0.6260 0.3075 0.3068 0.056 Uiso 1 1 calc R . .
H11D H 0.5632 0.2565 0.2891 0.056 Uiso 1 1 calc R . .
C12B C 0.5804(5) 0.2982(3) 0.2236(3) 0.0454(18) Uani 1 1 d . . .
H12C H 0.5968 0.3351 0.2172 0.055 Uiso 1 1 calc R . .
H12D H 0.6290 0.2744 0.2209 0.055 Uiso 1 1 calc R . .
C13B C 0.4933(5) 0.2827(2) 0.1799(3) 0.0420(16) Uani 1 1 d . . .
H13C H 0.4803 0.2445 0.1833 0.050 Uiso 1 1 calc R . .
H13D H 0.5006 0.2884 0.1440 0.050 Uiso 1 1 calc R . .
C14B C 0.4143(4) 0.3174(2) 0.1861(2) 0.0320(15) Uani 1 1 d . . .
H14C H 0.4262 0.3555 0.1812 0.038 Uiso 1 1 calc R . .
H14D H 0.3587 0.3073 0.1584 0.038 Uiso 1 1 calc R . .
C15B C 0.1740(5) -0.0055(2) 0.2470(3) 0.0300(17) Uani 1 1 d . . .
H15B H 0.1211 0.0139 0.2443 0.036 Uiso 1 1 calc R . .
C16B C 0.1710(5) -0.0617(2) 0.2476(3) 0.0369(19) Uani 1 1 d . . .
H16B H 0.1176 -0.0799 0.2464 0.044 Uiso 1 1 calc R . .
C17B C 0.2500 -0.0902(4) 0.2500 0.046(3) Uani 1 2 d S . .
H17B H 0.2500 -0.1280 0.2500 0.055 Uiso 1 2 calc SR . .
C18B C 0.1848(5) 0.5616(2) 0.2138(3) 0.0357(19) Uani 1 1 d . . .
H18B H 0.1394 0.5425 0.1884 0.043 Uiso 1 1 calc R . .
C19B C 0.1826(5) 0.6176(2) 0.2128(3) 0.0386(19) Uani 1 1 d . . .
H19B H 0.1361 0.6359 0.1873 0.046 Uiso 1 1 calc R . .
C20B C 0.2500 0.6464(3) 0.2500 0.037(3) Uani 1 2 d S . .
H20B H 0.2500 0.6842 0.2500 0.045 Uiso 1 2 calc SR . .
Li1 Li 0.1605(9) 0.6022(4) 0.5321(5) 0.034(3) Uani 1 1 d . . .
Li2 Li 0.6714(9) 0.1060(4) 0.5365(5) 0.037(3) Uani 1 1 d . . .
N1 N 0.1774(4) 0.68357(19) 0.5521(2) 0.0354(13) Uani 1 1 d . . .
N2 N 0.0427(5) 0.5773(2) 0.5442(3) 0.0398(17) Uani 1 1 d . . .
N3 N 0.2709(4) 0.5610(2) 0.5788(2) 0.0371(15) Uani 1 1 d . . .
N4 N 0.1606(4) 0.59775(18) 0.4533(2) 0.0339(14) Uani 1 1 d . . .
N5 N 0.6882(4) 0.18358(19) 0.5746(2) 0.0342(13) Uani 1 1 d . . .
N6 N 0.5499(4) 0.07764(19) 0.5435(2) 0.0349(15) Uani 1 1 d . . .
N7 N 0.7790(4) 0.06159(19) 0.5750(2) 0.0349(15) Uani 1 1 d . . .
N8 N 0.6618(4) 0.10812(17) 0.4551(2) 0.0285(13) Uani 1 1 d . . .
N9 N 0.0287(6) 0.8896(3) 0.5920(3) 0.066(2) Uani 1 1 d . . .
N10 N 0.4722(5) 0.6026(3) 0.4070(3) 0.0522(19) Uani 1 1 d . . .
C1 C 0.1520(5) 0.7038(2) 0.5936(3) 0.0499(19) Uani 1 1 d . . .
H1 H 0.1282 0.6800 0.6139 0.060 Uiso 1 1 calc R . .
C2 C 0.1590(6) 0.7582(3) 0.6079(3) 0.055(2) Uani 1 1 d . . .
H2 H 0.1397 0.7706 0.6369 0.065 Uiso 1 1 calc R . .
C3 C 0.1947(5) 0.7932(3) 0.5788(3) 0.048(2) Uani 1 1 d . . .
H3 H 0.2010 0.8300 0.5876 0.058 Uiso 1 1 calc R . .
C4 C 0.2209(5) 0.7731(2) 0.5364(3) 0.0476(19) Uani 1 1 d . . .
H4 H 0.2453 0.7960 0.5156 0.057 Uiso 1 1 calc R . .
C5 C 0.2110(5) 0.7184(2) 0.5246(3) 0.0455(18) Uani 1 1 d . . .
H5 H 0.2290 0.7054 0.4954 0.055 Uiso 1 1 calc R . .
C6 C 0.0414(6) 0.5628(3) 0.5943(3) 0.044(2) Uani 1 1 d . . .
H6 H 0.0967 0.5555 0.6202 0.053 Uiso 1 1 calc R . .
C7 C -0.0346(7) 0.5582(3) 0.6098(3) 0.052(2) Uani 1 1 d . . .
H7 H -0.0312 0.5476 0.6451 0.063 Uiso 1 1 calc R . .
C8 C -0.1185(7) 0.5695(3) 0.5717(4) 0.063(3) Uani 1 1 d . . .
H8 H -0.1724 0.5681 0.5809 0.076 Uiso 1 1 calc R . .
C9 C -0.1172(7) 0.5827(3) 0.5197(4) 0.059(2) Uani 1 1 d . . .
H9 H -0.1717 0.5895 0.4929 0.070 Uiso 1 1 calc R . .
C10 C -0.0381(6) 0.5861(3) 0.5068(4) 0.051(2) Uani 1 1 d . . .
H10 H -0.0399 0.5948 0.4713 0.061 Uiso 1 1 calc R . .
C11 C 0.3527(6) 0.5826(3) 0.5924(3) 0.045(2) Uani 1 1 d . . .
H11 H 0.3587 0.6182 0.5819 0.054 Uiso 1 1 calc R . .
C12 C 0.4301(5) 0.5548(3) 0.6215(3) 0.0438(19) Uani 1 1 d . . .
H12 H 0.4867 0.5714 0.6296 0.053 Uiso 1 1 calc R . .
C13 C 0.4223(6) 0.5028(3) 0.6380(3) 0.047(2) Uani 1 1 d . . .
H13 H 0.4732 0.4836 0.6581 0.056 Uiso 1 1 calc R . .
C14 C 0.3377(5) 0.4791(3) 0.6242(3) 0.0384(19) Uani 1 1 d . . .
H14 H 0.3304 0.4434 0.6340 0.046 Uiso 1 1 calc R . .
C15 C 0.2637(5) 0.5098(2) 0.5955(3) 0.0353(17) Uani 1 1 d . . .
H15 H 0.2063 0.4943 0.5872 0.042 Uiso 1 1 calc R . .
C16 C 0.2103(5) 0.5617(2) 0.4358(3) 0.0365(18) Uani 1 1 d . . .
H16 H 0.2552 0.5430 0.4619 0.044 Uiso 1 1 calc R . .
C17 C 0.1995(6) 0.5503(2) 0.3816(3) 0.045(2) Uani 1 1 d . . .
H17 H 0.2369 0.5256 0.3714 0.053 Uiso 1 1 calc R . .
C18 C 0.1308(6) 0.5772(2) 0.3431(3) 0.040(2) Uani 1 1 d . . .
H18 H 0.1187 0.5690 0.3063 0.048 Uiso 1 1 calc R . .
C19 C 0.0813(5) 0.6155(3) 0.3593(3) 0.0363(17) Uani 1 1 d . . .
H19 H 0.0371 0.6355 0.3341 0.044 Uiso 1 1 calc R . .
C20 C 0.0986(6) 0.6239(3) 0.4144(3) 0.044(2) Uani 1 1 d . . .
H20 H 0.0640 0.6500 0.4252 0.052 Uiso 1 1 calc R . .
C21 C 0.7633(5) 0.2031(2) 0.6107(3) 0.0406(16) Uani 1 1 d . . .
H21 H 0.8107 0.1792 0.6259 0.049 Uiso 1 1 calc R . .
C22 C 0.7738(5) 0.2573(2) 0.6265(3) 0.0407(16) Uani 1 1 d . . .
H22 H 0.8272 0.2692 0.6517 0.049 Uiso 1 1 calc R . .
C23 C 0.7036(5) 0.2935(3) 0.6043(3) 0.0429(17) Uani 1 1 d . . .
H23 H 0.7089 0.3301 0.6139 0.051 Uiso 1 1 calc R . .
C24 C 0.6267(5) 0.2737(2) 0.5680(3) 0.0388(16) Uani 1 1 d . . .
H24 H 0.5782 0.2968 0.5522 0.047 Uiso 1 1 calc R . .
C25 C 0.6212(4) 0.2192(2) 0.5548(2) 0.0362(15) Uani 1 1 d . . .
H25 H 0.5674 0.2064 0.5306 0.043 Uiso 1 1 calc R . .
C26 C 0.5460(6) 0.0615(2) 0.5926(3) 0.040(2) Uani 1 1 d . . .
H26 H 0.6005 0.0576 0.6202 0.048 Uiso 1 1 calc R . .
C27 C 0.4666(6) 0.0504(3) 0.6049(3) 0.043(2) Uani 1 1 d . . .
H27 H 0.4675 0.0384 0.6394 0.052 Uiso 1 1 calc R . .
C28 C 0.3859(6) 0.0578(3) 0.5642(3) 0.047(2) Uani 1 1 d . . .
H28 H 0.3309 0.0527 0.5715 0.057 Uiso 1 1 calc R . .
C29 C 0.3873(6) 0.0728(2) 0.5130(3) 0.047(2) Uani 1 1 d . . .
H29 H 0.3336 0.0766 0.4847 0.056 Uiso 1 1 calc R . .
C30 C 0.4696(6) 0.0820(2) 0.5046(3) 0.041(2) Uani 1 1 d . . .
H30 H 0.4700 0.0919 0.4698 0.049 Uiso 1 1 calc R . .
C31 C 0.7733(6) 0.0125(2) 0.5970(3) 0.0373(19) Uani 1 1 d . . .
H31 H 0.7158 -0.0025 0.5906 0.045 Uiso 1 1 calc R . .
C32 C 0.8441(6) -0.0164(3) 0.6274(3) 0.047(2) Uani 1 1 d . . .
H32 H 0.8352 -0.0498 0.6419 0.056 Uiso 1 1 calc R . .
C33 C 0.9298(7) 0.0043(3) 0.6366(3) 0.058(3) Uani 1 1 d . . .
H33 H 0.9799 -0.0151 0.6575 0.069 Uiso 1 1 calc R . .
C34 C 0.9413(6) 0.0542(3) 0.6146(4) 0.058(2) Uani 1 1 d . . .
H34 H 0.9987 0.0693 0.6206 0.069 Uiso 1 1 calc R . .
C35 C 0.8636(6) 0.0808(3) 0.5832(3) 0.043(2) Uani 1 1 d . . .
H35 H 0.8706 0.1137 0.5670 0.052 Uiso 1 1 calc R . .
C36 C 0.5987(5) 0.1370(2) 0.4174(3) 0.0313(16) Uani 1 1 d . . .
H36 H 0.5681 0.1644 0.4297 0.038 Uiso 1 1 calc R . .
C37 C 0.5769(5) 0.1285(2) 0.3624(3) 0.0357(17) Uani 1 1 d . . .
H37 H 0.5321 0.1492 0.3383 0.043 Uiso 1 1 calc R . .
C38 C 0.6228(5) 0.0885(2) 0.3431(3) 0.0337(17) Uani 1 1 d . . .
H38 H 0.6107 0.0821 0.3059 0.040 Uiso 1 1 calc R . .
C39 C 0.6868(6) 0.0587(2) 0.3808(3) 0.042(2) Uani 1 1 d . . .
H39 H 0.7188 0.0313 0.3695 0.050 Uiso 1 1 calc R . .
C40 C 0.7038(6) 0.0696(2) 0.4361(3) 0.0362(19) Uani 1 1 d . . .
H40 H 0.7469 0.0486 0.4609 0.043 Uiso 1 1 calc R . .
C41 C 0.0311(7) 0.9190(4) 0.5491(4) 0.079(3) Uani 1 1 d . . .
H41 H 0.0856 0.9355 0.5498 0.095 Uiso 1 1 calc R . .
C42 C -0.0435(7) 0.9265(3) 0.5031(4) 0.066(3) Uani 1 1 d . . .
H42 H -0.0383 0.9472 0.4738 0.079 Uiso 1 1 calc R . .
C43 C -0.1230(6) 0.9033(3) 0.5020(3) 0.046(2) Uani 1 1 d . . .
H43 H -0.1743 0.9079 0.4722 0.055 Uiso 1 1 calc R . .
C44 C -0.1263(6) 0.8732(3) 0.5454(3) 0.045(2) Uani 1 1 d . . .
H44 H -0.1801 0.8563 0.5456 0.054 Uiso 1 1 calc R . .
C45 C -0.0506(7) 0.8677(3) 0.5888(3) 0.050(3) Uani 1 1 d . . .
H45 H -0.0551 0.8471 0.6182 0.060 Uiso 1 1 calc R . .
C46 C 0.5470(7) 0.6312(3) 0.4075(3) 0.047(2) Uani 1 1 d . . .
H46 H 0.5475 0.6497 0.3760 0.056 Uiso 1 1 calc R . .
C47 C 0.6224(7) 0.6344(3) 0.4522(3) 0.049(2) Uani 1 1 d . . .
H47 H 0.6732 0.6539 0.4506 0.059 Uiso 1 1 calc R . .
C48 C 0.6215(6) 0.6081(3) 0.4997(3) 0.043(2) Uani 1 1 d . . .
H48 H 0.6710 0.6103 0.5309 0.052 Uiso 1 1 calc R . .
C49 C 0.5459(6) 0.5788(3) 0.4996(3) 0.046(2) Uani 1 1 d . . .
H49 H 0.5426 0.5605 0.5306 0.055 Uiso 1 1 calc R . .
C50 C 0.4752(7) 0.5772(3) 0.4523(4) 0.053(2) Uani 1 1 d . . .
H50 H 0.4250 0.5563 0.4523 0.064 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
U1 0.0263(2) 0.02235(15) 0.0260(2) 0.000 0.00716(18) 0.000
U2 0.0231(2) 0.02256(15) 0.0230(2) 0.000 0.00741(17) 0.000
Cl1A 0.0300(12) 0.0367(8) 0.0325(10) 0.0027(6) 0.0127(8) 0.0000(6)
Cl2A 0.0390(12) 0.0306(7) 0.0285(9) 0.0026(6) 0.0042(8) -0.0022(7)
Cl3A 0.0291(11) 0.0275(7) 0.0317(9) 0.0010(6) 0.0107(8) 0.0036(6)
Cl4A 0.0293(11) 0.0413(8) 0.0245(9) 0.0018(7) 0.0056(8) 0.0022(7)
N1A 0.025(3) 0.025(2) 0.021(3) 0.000(2) 0.006(2) 0.0021(19)
N2A 0.022(3) 0.023(2) 0.034(3) -0.002(2) 0.010(2) -0.003(2)
N3A 0.030(6) 0.036(4) 0.028(5) 0.000 0.012(4) 0.000
N4A 0.029(6) 0.025(3) 0.021(4) 0.000 0.009(4) 0.000
C1A 0.024(6) 0.024(4) 0.031(6) 0.000 0.016(5) 0.000
C2A 0.035(7) 0.021(4) 0.017(5) 0.000 0.009(5) 0.000
C3A 0.029(4) 0.023(3) 0.022(3) -0.002(2) 0.010(3) -0.001(2)
C4A 0.036(5) 0.043(3) 0.029(3) -0.001(3) 0.011(3) 0.006(3)
C5A 0.049(5) 0.058(4) 0.028(4) -0.010(3) 0.010(3) 0.001(4)
C6A 0.043(5) 0.062(4) 0.029(4) -0.008(3) 0.002(3) 0.000(4)
C7A 0.029(4) 0.039(3) 0.042(4) 0.000(3) -0.004(3) 0.001(3)
C8A 0.030(4) 0.026(3) 0.027(3) -0.002(2) 0.003(3) 0.000(2)
C9A 0.028(4) 0.022(3) 0.038(4) 0.003(3) 0.018(3) 0.002(2)
C10A 0.021(4) 0.032(3) 0.035(4) -0.002(3) 0.009(3) 0.001(2)
C11A 0.026(4) 0.038(3) 0.041(4) -0.004(3) 0.013(3) -0.001(3)
C12A 0.034(4) 0.036(3) 0.049(4) 0.000(3) 0.021(3) -0.002(3)
C13A 0.033(4) 0.041(3) 0.041(4) 0.010(3) 0.020(3) 0.005(3)
C14A 0.028(4) 0.036(3) 0.027(3) 0.002(3) 0.008(3) 0.005(3)
C15A 0.029(5) 0.034(3) 0.038(5) 0.005(3) 0.004(4) 0.004(3)
C16A 0.023(5) 0.034(3) 0.064(6) -0.001(3) 0.013(4) -0.006(3)
C17A 0.047(9) 0.029(5) 0.058(8) 0.000 0.007(7) 0.000
C18A 0.024(4) 0.032(3) 0.027(4) 0.001(3) 0.001(3) 0.010(3)
C19A 0.033(5) 0.027(3) 0.042(5) -0.009(3) 0.005(4) -0.004(3)
C20A 0.053(9) 0.020(4) 0.053(7) 0.000 -0.004(6) 0.000
U3 0.0273(3) 0.02233(15) 0.0243(2) 0.000 0.00757(18) 0.000
U4 0.0233(2) 0.02287(15) 0.0214(2) 0.000 0.00681(17) 0.000
Cl1B 0.0371(12) 0.0293(7) 0.0288(9) -0.0020(6) 0.0039(8) -0.0010(7)
Cl2B 0.0291(12) 0.0357(8) 0.0328(10) -0.0007(6) 0.0100(8) -0.0002(6)
Cl3B 0.0332(12) 0.0409(8) 0.0225(9) -0.0018(6) 0.0068(8) -0.0058(7)
Cl4B 0.0253(10) 0.0295(7) 0.0328(9) 0.0001(6) 0.0109(8) -0.0022(6)
N1B 0.028(4) 0.027(2) 0.026(3) -0.002(2) 0.010(3) 0.000(2)
N2B 0.023(3) 0.030(2) 0.024(3) -0.005(2) 0.011(2) -0.002(2)
N3B 0.037(6) 0.024(3) 0.018(4) 0.000 0.001(4) 0.000
N4B 0.030(6) 0.025(4) 0.028(5) 0.000 0.003(4) 0.000
C1B 0.017(6) 0.021(4) 0.032(6) 0.000 0.010(4) 0.000
C2B 0.027(6) 0.030(4) 0.013(5) 0.000 0.004(4) 0.000
C3B 0.029(4) 0.021(3) 0.027(3) 0.004(2) 0.008(3) -0.005(2)
C4B 0.022(4) 0.026(3) 0.027(3) -0.001(2) 0.006(3) -0.002(2)
C5B 0.025(4) 0.034(3) 0.030(3) 0.004(3) -0.001(3) -0.003(3)
C6B 0.047(5) 0.043(3) 0.033(4) 0.006(3) 0.012(3) -0.004(3)
C7B 0.045(5) 0.038(3) 0.029(3) 0.003(3) 0.012(3) 0.000(3)
C8B 0.027(4) 0.033(3) 0.030(3) -0.004(3) 0.012(3) -0.002(3)
C9B 0.029(4) 0.025(3) 0.036(4) -0.002(3) 0.015(3) 0.001(2)
C10B 0.036(4) 0.030(3) 0.040(4) -0.005(3) 0.005(3) 0.001(3)
C11B 0.031(4) 0.035(3) 0.072(5) 0.005(3) 0.011(4) 0.002(3)
C12B 0.041(5) 0.037(3) 0.071(5) -0.013(3) 0.034(4) -0.002(3)
C13B 0.040(4) 0.038(3) 0.058(5) -0.008(3) 0.030(4) -0.005(3)
C14B 0.033(4) 0.034(3) 0.034(4) -0.009(3) 0.017(3) -0.007(3)
C15B 0.026(5) 0.029(3) 0.036(4) -0.004(3) 0.011(3) 0.001(3)
C16B 0.042(6) 0.028(3) 0.044(5) -0.003(3) 0.018(4) -0.009(3)
C17B 0.052(9) 0.026(5) 0.065(8) 0.000 0.024(7) 0.000
C18B 0.046(6) 0.031(3) 0.030(4) 0.001(3) 0.011(4) 0.000(3)
C19B 0.042(5) 0.033(3) 0.034(4) 0.001(3) 0.001(4) 0.004(3)
C20B 0.054(8) 0.023(4) 0.036(6) 0.000 0.015(6) 0.000
Li1 0.037(8) 0.037(5) 0.030(6) 0.003(5) 0.011(6) 0.005(5)
Li2 0.025(7) 0.044(6) 0.042(7) 0.006(5) 0.011(6) 0.004(5)
N1 0.035(4) 0.042(3) 0.033(3) -0.001(2) 0.016(3) -0.004(2)
N2 0.039(5) 0.042(3) 0.041(4) -0.002(3) 0.015(4) -0.004(3)
N3 0.034(4) 0.041(3) 0.033(4) 0.006(3) 0.006(3) -0.001(3)
N4 0.040(4) 0.030(2) 0.033(3) -0.001(2) 0.012(3) 0.008(2)
N5 0.036(4) 0.041(3) 0.029(3) 0.003(2) 0.015(3) 0.003(2)
N6 0.026(4) 0.046(3) 0.032(4) 0.000(2) 0.009(3) -0.003(2)
N7 0.031(4) 0.035(3) 0.039(4) 0.002(2) 0.009(3) 0.000(2)
N8 0.022(3) 0.029(2) 0.036(3) 0.000(2) 0.012(3) -0.004(2)
N9 0.047(6) 0.092(5) 0.045(5) 0.003(4) -0.007(4) 0.014(4)
N10 0.056(6) 0.059(4) 0.038(4) 0.001(3) 0.008(4) 0.017(3)
C1 0.067(6) 0.037(3) 0.063(5) 0.006(3) 0.045(4) 0.001(3)
C2 0.075(6) 0.046(4) 0.064(5) -0.014(4) 0.054(5) -0.015(4)
C3 0.056(6) 0.036(3) 0.057(5) -0.015(3) 0.024(4) -0.016(3)
C4 0.058(5) 0.048(4) 0.041(4) 0.003(3) 0.021(4) -0.025(3)
C5 0.059(5) 0.050(4) 0.038(4) -0.011(3) 0.031(4) -0.018(3)
C6 0.042(6) 0.055(4) 0.038(5) -0.003(4) 0.017(4) -0.008(4)
C7 0.064(7) 0.049(4) 0.048(5) -0.004(4) 0.024(5) -0.006(4)
C8 0.051(7) 0.064(5) 0.092(8) -0.012(5) 0.047(6) -0.008(4)
C9 0.032(6) 0.065(5) 0.078(7) -0.008(5) 0.015(5) -0.006(4)
C10 0.041(6) 0.055(4) 0.050(6) 0.005(4) 0.003(5) 0.000(4)
C11 0.051(6) 0.040(3) 0.044(5) -0.001(3) 0.013(4) -0.006(3)
C12 0.019(4) 0.069(5) 0.046(5) -0.018(4) 0.013(4) -0.008(3)
C13 0.046(6) 0.054(4) 0.036(5) -0.007(3) 0.006(4) 0.015(4)
C14 0.038(5) 0.042(3) 0.031(4) 0.003(3) 0.002(4) 0.009(3)
C15 0.030(5) 0.041(3) 0.036(4) 0.007(3) 0.012(4) 0.004(3)
C16 0.034(5) 0.037(3) 0.039(5) 0.000(3) 0.012(4) 0.009(3)
C17 0.057(6) 0.033(3) 0.052(5) 0.002(3) 0.030(4) 0.015(3)
C18 0.053(6) 0.034(3) 0.035(4) -0.011(3) 0.016(4) -0.010(3)
C19 0.027(5) 0.055(4) 0.027(4) -0.001(3) 0.008(3) 0.005(3)
C20 0.044(6) 0.050(4) 0.041(5) -0.004(3) 0.018(4) 0.019(3)
C21 0.033(4) 0.044(3) 0.041(4) 0.003(3) 0.005(3) 0.002(3)
C22 0.030(4) 0.050(4) 0.038(4) -0.007(3) 0.005(3) -0.009(3)
C23 0.040(5) 0.050(4) 0.044(4) -0.012(3) 0.021(4) -0.004(3)
C24 0.043(4) 0.034(3) 0.043(4) 0.003(3) 0.017(3) 0.011(3)
C25 0.028(4) 0.048(4) 0.031(3) 0.003(3) 0.007(3) 0.003(3)
C26 0.041(6) 0.043(3) 0.038(5) -0.005(3) 0.014(4) 0.003(3)
C27 0.041(6) 0.048(4) 0.053(5) -0.010(4) 0.031(4) -0.004(3)
C28 0.037(5) 0.043(4) 0.067(6) -0.010(4) 0.023(4) -0.007(3)
C29 0.040(6) 0.044(4) 0.053(5) -0.017(3) 0.009(4) -0.004(3)
C30 0.040(6) 0.047(4) 0.035(5) -0.010(3) 0.011(4) 0.000(3)
C31 0.042(5) 0.036(3) 0.033(4) 0.000(3) 0.010(4) 0.000(3)
C32 0.055(7) 0.048(4) 0.041(5) 0.009(3) 0.020(5) 0.023(4)
C33 0.044(6) 0.071(5) 0.045(5) -0.020(4) -0.007(5) 0.020(4)
C34 0.028(5) 0.072(5) 0.072(6) -0.025(5) 0.014(5) -0.001(4)
C35 0.032(5) 0.045(4) 0.054(5) 0.003(3) 0.014(4) -0.005(3)
C36 0.029(5) 0.038(3) 0.027(4) 0.000(3) 0.010(3) 0.012(3)
C37 0.037(5) 0.044(3) 0.030(4) 0.001(3) 0.014(3) 0.003(3)
C38 0.044(5) 0.035(3) 0.022(4) -0.006(3) 0.010(3) -0.010(3)
C39 0.058(6) 0.032(3) 0.046(5) -0.008(3) 0.031(4) 0.001(3)
C40 0.043(5) 0.029(3) 0.041(5) 0.004(3) 0.017(4) 0.000(3)
C41 0.037(7) 0.129(8) 0.063(7) 0.028(6) 0.002(5) -0.002(5)
C42 0.058(8) 0.088(6) 0.052(6) 0.026(5) 0.017(5) 0.000(5)
C43 0.050(6) 0.054(4) 0.033(4) 0.004(3) 0.009(4) -0.006(4)
C44 0.044(6) 0.049(4) 0.045(5) -0.004(4) 0.017(4) -0.008(3)
C45 0.085(9) 0.040(4) 0.029(5) 0.006(3) 0.021(5) 0.013(4)
C46 0.063(7) 0.043(4) 0.038(5) 0.006(3) 0.019(5) 0.016(4)
C47 0.060(7) 0.043(4) 0.051(6) -0.008(4) 0.027(5) -0.008(4)
C48 0.039(5) 0.049(4) 0.036(4) -0.004(3) 0.003(4) 0.000(3)
C49 0.049(7) 0.052(4) 0.034(5) 0.003(3) 0.008(4) -0.004(4)
C50 0.043(7) 0.058(5) 0.057(6) 0.000(4) 0.013(5) -0.005(4)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
U1 N1A 2.411(4) . ?
U1 N1A 2.411(4) 2_556 ?
U1 Cl1A 2.6387(19) . ?
U1 Cl1A 2.6388(19) 2_556 ?
U1 N3A 2.646(7) . ?
U1 Cl2A 2.6923(16) 2_556 ?
U1 Cl2A 2.6923(15) . ?
U1 C1A 2.824(8) . ?
U2 N2A 2.428(4) . ?
U2 N2A 2.428(4) 2_556 ?
U2 Cl4A 2.6428(16) 2_556 ?
U2 Cl4A 2.6429(16) . ?
U2 Cl3A 2.6753(17) 2_556 ?
U2 Cl3A 2.6754(17) . ?
U2 N4A 2.690(6) . ?
U2 C2A 2.855(8) . ?
N1A C1A 1.327(6) . ?
N1A C3A 1.467(7) . ?
N2A C2A 1.337(6) . ?
N2A C9A 1.466(8) . ?
N3A C15A 1.338(7) . ?
N3A C15A 1.338(7) 2_556 ?
N4A C18A 1.345(7) 2_556 ?
N4A C18A 1.345(7) . ?
C1A N1A 1.327(6) 2_556 ?
C1A C2A 1.534(11) . ?
C2A N2A 1.337(6) 2_556 ?
C3A C4A 1.515(8) . ?
C3A C8A 1.529(8) . ?
C4A C5A 1.535(8) . ?
C5A C6A 1.523(10) . ?
C6A C7A 1.529(9) . ?
C7A C8A 1.543(8) . ?
C9A C10A 1.517(8) . ?
C9A C14A 1.521(8) . ?
C10A C11A 1.550(8) . ?
C11A C12A 1.536(8) . ?
C12A C13A 1.522(9) . ?
C13A C14A 1.534(8) . ?
C15A C16A 1.389(8) . ?
C16A C17A 1.380(8) . ?
C17A C16A 1.380(8) 2_556 ?
C18A C19A 1.382(7) . ?
C19A C20A 1.378(7) . ?
C20A C19A 1.378(7) 2_556 ?
U3 N1B 2.412(4) 2 ?
U3 N1B 2.412(4) . ?
U3 Cl2B 2.6326(19) . ?
U3 Cl2B 2.6326(19) 2 ?
U3 N3B 2.651(6) . ?
U3 Cl1B 2.6916(15) 2 ?
U3 Cl1B 2.6917(15) . ?
U3 C1B 2.836(7) . ?
U4 N2B 2.417(5) 2 ?
U4 N2B 2.417(5) . ?
U4 Cl3B 2.6420(16) . ?
U4 Cl3B 2.6420(16) 2 ?
U4 Cl4B 2.6704(17) . ?
U4 Cl4B 2.6705(17) 2 ?
U4 N4B 2.724(6) . ?
U4 C2B 2.837(8) . ?
N1B C1B 1.333(6) . ?
N1B C3B 1.462(7) . ?
N2B C2B 1.328(6) . ?
N2B C9B 1.465(8) . ?
N3B C15B 1.336(7) . ?
N3B C15B 1.336(7) 2 ?
N4B C18B 1.338(7) 2 ?
N4B C18B 1.338(7) . ?
C1B N1B 1.333(6) 2 ?
C1B C2B 1.538(11) . ?
C2B N2B 1.328(6) 2 ?
C3B C8B 1.529(8) . ?
C3B C4B 1.539(8) . ?
C4B C5B 1.534(7) . ?
C5B C6B 1.532(9) . ?
C6B C7B 1.538(9) . ?
C7B C8B 1.523(8) . ?
C9B C14B 1.527(8) . ?
C9B C10B 1.532(8) . ?
C10B C11B 1.538(9) . ?
C11B C12B 1.521(9) . ?
C12B C13B 1.521(9) . ?
C13B C14B 1.536(8) . ?
C15B C16B 1.383(7) . ?
C16B C17B 1.392(8) . ?
C17B C16B 1.392(8) 2 ?
C18B C19B 1.378(8) . ?
C19B C20B 1.380(7) . ?
C20B C19B 1.379(7) 2 ?
Li1 N4 2.028(12) . ?
Li1 N2 2.029(14) . ?
Li1 N3 2.038(13) . ?
Li1 N1 2.063(11) . ?
Li2 N7 1.988(13) . ?
Li2 N8 2.053(13) . ?
Li2 N6 2.057(14) . ?
Li2 N5 2.124(12) . ?
N1 C5 1.311(8) . ?
N1 C1 1.338(8) . ?
N2 C6 1.342(9) . ?
N2 C10 1.346(10) . ?
N3 C11 1.317(10) . ?
N3 C15 1.343(7) . ?
N4 C20 1.325(9) . ?
N4 C16 1.335(8) . ?
N5 C25 1.335(8) . ?
N5 C21 1.340(8) . ?
N6 C26 1.340(9) . ?
N6 C30 1.344(9) . ?
N7 C35 1.345(10) . ?
N7 C31 1.346(8) . ?
N8 C40 1.322(8) . ?
N8 C36 1.352(8) . ?
N9 C45 1.316(12) . ?
N9 C41 1.327(11) . ?
N10 C50 1.308(10) . ?
N10 C46 1.347(11) . ?
C1 C2 1.382(9) . ?
C2 C3 1.361(9) . ?
C3 C4 1.364(9) . ?
C4 C5 1.378(8) . ?
C6 C7 1.350(12) . ?
C7 C8 1.399(12) . ?
C8 C9 1.381(12) . ?
C9 C10 1.359(12) . ?
C11 C12 1.386(11) . ?
C12 C13 1.364(10) . ?
C13 C14 1.376(11) . ?
C14 C15 1.385(9) . ?
C16 C17 1.381(10) . ?
C17 C18 1.384(10) . ?
C18 C19 1.354(10) . ?
C19 C20 1.374(9) . ?
C21 C22 1.389(8) . ?
C22 C23 1.387(9) . ?
C23 C24 1.363(9) . ?
C24 C25 1.379(7) . ?
C26 C27 1.382(11) . ?
C27 C28 1.378(11) . ?
C28 C29 1.374(11) . ?
C29 C30 1.369(11) . ?
C31 C32 1.342(10) . ?
C32 C33 1.370(12) . ?
C33 C34 1.385(11) . ?
C34 C35 1.394(11) . ?
C36 C37 1.369(9) . ?
C37 C38 1.389(9) . ?
C38 C39 1.372(10) . ?
C39 C40 1.390(9) . ?
C41 C42 1.395(13) . ?
C42 C43 1.347(12) . ?
C43 C44 1.353(10) . ?
C44 C45 1.360(11) . ?
C46 C47 1.372(11) . ?
C47 C48 1.385(10) . ?
C48 C49 1.371(11) . ?
C49 C50 1.372(11) . ?

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
N1A U1 N1A 55.9(2) . 2_556 ?
N1A U1 Cl1A 89.44(15) . . ?
N1A U1 Cl1A 89.56(15) 2_556 . ?
N1A U1 Cl1A 89.56(15) . 2_556 ?
N1A U1 Cl1A 89.45(15) 2_556 2_556 ?
Cl1A U1 Cl1A 178.87(6) . 2_556 ?
N1A U1 N3A 152.03(11) . . ?
N1A U1 N3A 152.03(11) 2_556 . ?
Cl1A U1 N3A 90.56(3) . . ?
Cl1A U1 N3A 90.56(3) 2_556 . ?
N1A U1 Cl2A 137.52(12) . 2_556 ?
N1A U1 Cl2A 81.61(12) 2_556 2_556 ?
Cl1A U1 Cl2A 88.88(6) . 2_556 ?
Cl1A U1 Cl2A 91.49(6) 2_556 2_556 ?
N3A U1 Cl2A 70.43(3) . 2_556 ?
N1A U1 Cl2A 81.61(12) . . ?
N1A U1 Cl2A 137.52(12) 2_556 . ?
Cl1A U1 Cl2A 91.50(6) . . ?
Cl1A U1 Cl2A 88.88(6) 2_556 . ?
N3A U1 Cl2A 70.43(3) . . ?
Cl2A U1 Cl2A 140.86(6) 2_556 . ?
N2A U2 N2A 55.7(3) . 2_556 ?
N2A U2 Cl4A 96.17(13) . 2_556 ?
N2A U2 Cl4A 88.67(13) 2_556 2_556 ?
N2A U2 Cl4A 88.67(13) . . ?
N2A U2 Cl4A 96.17(13) 2_556 . ?
Cl4A U2 Cl4A 174.54(6) 2_556 . ?
N2A U2 Cl3A 136.23(13) . 2_556 ?
N2A U2 Cl3A 81.01(13) 2_556 2_556 ?
Cl4A U2 Cl3A 88.06(5) 2_556 2_556 ?
Cl4A U2 Cl3A 90.19(5) . 2_556 ?
N2A U2 Cl3A 81.01(13) . . ?
N2A U2 Cl3A 136.23(13) 2_556 . ?
Cl4A U2 Cl3A 90.19(5) 2_556 . ?
Cl4A U2 Cl3A 88.06(5) . . ?
Cl3A U2 Cl3A 142.68(6) 2_556 . ?
N2A U2 N4A 152.16(13) . . ?
N2A U2 N4A 152.16(13) 2_556 . ?
Cl4A U2 N4A 87.27(3) 2_556 . ?
Cl4A U2 N4A 87.27(3) . . ?
Cl3A U2 N4A 71.34(3) 2_556 . ?
Cl3A U2 N4A 71.34(3) . . ?
C1A N1A C3A 122.2(4) . . ?
C1A N1A U1 93.6(4) . . ?
C3A N1A U1 144.2(3) . . ?
C2A N2A C9A 121.1(5) . . ?
C2A N2A U2 94.1(4) . . ?
C9A N2A U2 144.3(4) . . ?
C15A N3A C15A 118.9(8) . 2_556 ?
C15A N3A U1 120.6(4) . . ?
C15A N3A U1 120.6(4) 2_556 . ?
C18A N4A C18A 116.0(7) 2_556 . ?
C18A N4A U2 122.0(3) 2_556 . ?
C18A N4A U2 122.0(3) . . ?
N1A C1A N1A 116.9(7) 2_556 . ?
N1A C1A C2A 121.5(3) 2_556 . ?
N1A C1A C2A 121.5(3) . . ?
N2A C2A N2A 116.1(7) 2_556 . ?
N2A C2A C1A 122.0(3) 2_556 . ?
N2A C2A C1A 122.0(4) . . ?
N1A C3A C4A 112.3(5) . . ?
N1A C3A C8A 110.1(5) . . ?
C4A C3A C8A 109.9(5) . . ?
C3A C4A C5A 110.0(5) . . ?
C6A C5A C4A 112.5(6) . . ?
C5A C6A C7A 111.7(6) . . ?
C6A C7A C8A 110.6(5) . . ?
C3A C8A C7A 110.6(5) . . ?
N2A C9A C10A 112.2(5) . . ?
N2A C9A C14A 110.9(5) . . ?
C10A C9A C14A 110.3(5) . . ?
C9A C10A C11A 109.7(5) . . ?
C12A C11A C10A 111.7(5) . . ?
C13A C12A C11A 112.0(6) . . ?
C12A C13A C14A 111.6(5) . . ?
C9A C14A C13A 110.9(5) . . ?
N3A C15A C16A 122.0(7) . . ?
C17A C16A C15A 119.1(7) . . ?
C16A C17A C16A 118.7(9) 2_556 . ?
N4A C18A C19A 124.1(6) . . ?
C20A C19A C18A 117.9(6) . . ?
C19A C20A C19A 119.8(8) 2_556 . ?
N1B U3 N1B 55.9(2) 2 . ?
N1B U3 Cl2B 93.44(15) 2 . ?
N1B U3 Cl2B 85.72(15) . . ?
N1B U3 Cl2B 85.71(15) 2 2 ?
N1B U3 Cl2B 93.43(15) . 2 ?
Cl2B U3 Cl2B 179.04(6) . 2 ?
N1B U3 N3B 152.04(12) 2 . ?
N1B U3 N3B 152.04(12) . . ?
Cl2B U3 N3B 90.48(3) . . ?
Cl2B U3 N3B 90.48(3) 2 . ?
N1B U3 Cl1B 81.68(12) 2 2 ?
N1B U3 Cl1B 136.54(12) . 2 ?
Cl2B U3 Cl1B 87.98(5) . 2 ?
Cl2B U3 Cl1B 92.34(5) 2 2 ?
N3B U3 Cl1B 70.79(3) . 2 ?
N1B U3 Cl1B 136.54(12) 2 . ?
N1B U3 Cl1B 81.69(12) . . ?
Cl2B U3 Cl1B 92.34(5) . . ?
Cl2B U3 Cl1B 87.98(5) 2 . ?
N3B U3 Cl1B 70.79(3) . . ?
Cl1B U3 Cl1B 141.58(6) 2 . ?
N2B U4 N2B 55.7(3) 2 . ?
N2B U4 Cl3B 89.43(12) 2 . ?
N2B U4 Cl3B 92.62(12) . . ?
N2B U4 Cl3B 92.62(12) 2 2 ?
N2B U4 Cl3B 89.43(12) . 2 ?
Cl3B U4 Cl3B 177.68(6) . 2 ?
N2B U4 Cl4B 136.49(13) 2 . ?
N2B U4 Cl4B 80.98(13) . . ?
Cl3B U4 Cl4B 88.74(5) . . ?
Cl3B U4 Cl4B 90.51(5) 2 . ?
N2B U4 Cl4B 80.98(13) 2 2 ?
N2B U4 Cl4B 136.49(13) . 2 ?
Cl3B U4 Cl4B 90.51(5) . 2 ?
Cl3B U4 Cl4B 88.74(5) 2 2 ?
Cl4B U4 Cl4B 142.50(6) . 2 ?
N2B U4 N4B 152.16(13) 2 . ?
N2B U4 N4B 152.16(13) . . ?
Cl3B U4 N4B 88.84(3) . . ?
Cl3B U4 N4B 88.84(3) 2 . ?
Cl4B U4 N4B 71.25(3) . . ?
Cl4B U4 N4B 71.25(3) 2 . ?
C1B N1B C3B 121.0(4) . . ?
C1B N1B U3 94.0(4) . . ?
C3B N1B U3 145.0(3) . . ?
C2B N2B C9B 120.8(5) . . ?
C2B N2B U4 93.9(4) . . ?
C9B N2B U4 145.0(4) . . ?
C15B N3B C15B 119.1(7) . 2 ?
C15B N3B U3 120.4(4) . . ?
C15B N3B U3 120.4(4) 2 . ?
C18B N4B C18B 118.5(7) 2 . ?
C18B N4B U4 120.7(4) 2 . ?
C18B N4B U4 120.7(4) . . ?
N1B C1B N1B 116.1(7) . 2 ?
N1B C1B C2B 122.0(3) . . ?
N1B C1B C2B 122.0(3) 2 . ?
N2B C2B N2B 116.5(7) . 2 ?
N2B C2B C1B 121.8(4) . . ?
N2B C2B C1B 121.8(4) 2 . ?
N1B C3B C8B 110.7(5) . . ?
N1B C3B C4B 110.4(5) . . ?
C8B C3B C4B 109.0(5) . . ?
C5B C4B C3B 110.1(5) . . ?
C6B C5B C4B 110.4(5) . . ?
C5B C6B C7B 110.4(5) . . ?
C8B C7B C6B 111.2(5) . . ?
C7B C8B C3B 110.7(5) . . ?
N2B C9B C14B 111.7(5) . . ?
N2B C9B C10B 111.9(5) . . ?
C14B C9B C10B 109.6(6) . . ?
C9B C10B C11B 109.2(5) . . ?
C12B C11B C10B 111.9(6) . . ?
C13B C12B C11B 112.3(6) . . ?
C12B C13B C14B 109.7(5) . . ?
C9B C14B C13B 109.8(5) . . ?
N3B C15B C16B 122.5(7) . . ?
C15B C16B C17B 118.2(7) . . ?
C16B C17B C16B 119.5(9) 2 . ?
N4B C18B C19B 122.2(7) . . ?
C18B C19B C20B 119.4(7) . . ?
C19B C20B C19B 118.4(8) 2 . ?
N4 Li1 N2 113.8(6) . . ?
N4 Li1 N3 108.2(6) . . ?
N2 Li1 N3 112.9(6) . . ?
N4 Li1 N1 105.3(5) . . ?
N2 Li1 N1 107.9(6) . . ?
N3 Li1 N1 108.3(6) . . ?
N7 Li2 N8 108.4(6) . . ?
N7 Li2 N6 114.8(6) . . ?
N8 Li2 N6 107.8(6) . . ?
N7 Li2 N5 107.1(6) . . ?
N8 Li2 N5 114.1(5) . . ?
N6 Li2 N5 104.7(6) . . ?
C5 N1 C1 116.4(5) . . ?
C5 N1 Li1 122.7(5) . . ?
C1 N1 Li1 121.0(5) . . ?
C6 N2 C10 116.9(8) . . ?
C6 N2 Li1 119.8(7) . . ?
C10 N2 Li1 121.6(7) . . ?
C11 N3 C15 117.2(6) . . ?
C11 N3 Li1 121.5(6) . . ?
C15 N3 Li1 121.3(6) . . ?
C20 N4 C16 115.2(6) . . ?
C20 N4 Li1 120.8(6) . . ?
C16 N4 Li1 122.9(5) . . ?
C25 N5 C21 116.2(5) . . ?
C25 N5 Li2 116.0(5) . . ?
C21 N5 Li2 127.1(6) . . ?
C26 N6 C30 115.6(7) . . ?
C26 N6 Li2 118.6(6) . . ?
C30 N6 Li2 124.8(6) . . ?
C35 N7 C31 115.6(6) . . ?
C35 N7 Li2 120.9(6) . . ?
C31 N7 Li2 123.5(6) . . ?
C40 N8 C36 116.1(6) . . ?
C40 N8 Li2 117.7(5) . . ?
C36 N8 Li2 124.1(6) . . ?
C45 N9 C41 115.2(8) . . ?
C50 N10 C46 115.9(8) . . ?
N1 C1 C2 123.7(6) . . ?
C3 C2 C1 118.6(7) . . ?
C2 C3 C4 118.3(6) . . ?
C3 C4 C5 119.4(6) . . ?
N1 C5 C4 123.7(6) . . ?
N2 C6 C7 124.5(9) . . ?
C6 C7 C8 118.8(9) . . ?
C9 C8 C7 116.5(9) . . ?
C10 C9 C8 121.5(9) . . ?
N2 C10 C9 121.6(9) . . ?
N3 C11 C12 123.3(6) . . ?
C13 C12 C11 119.2(8) . . ?
C12 C13 C14 118.8(7) . . ?
C13 C14 C15 118.4(6) . . ?
N3 C15 C14 123.2(7) . . ?
N4 C16 C17 124.4(7) . . ?
C16 C17 C18 117.5(7) . . ?
C19 C18 C17 119.6(7) . . ?
C18 C19 C20 117.8(7) . . ?
N4 C20 C19 125.5(7) . . ?
N5 C21 C22 123.2(6) . . ?
C23 C22 C21 119.1(6) . . ?
C24 C23 C22 117.9(6) . . ?
C23 C24 C25 119.5(6) . . ?
N5 C25 C24 124.1(6) . . ?
N6 C26 C27 124.4(8) . . ?
C28 C27 C26 117.6(8) . . ?
C29 C28 C27 119.5(8) . . ?
C30 C29 C28 118.4(8) . . ?
N6 C30 C29 124.3(8) . . ?
C32 C31 N7 125.1(8) . . ?
C31 C32 C33 118.7(7) . . ?
C32 C33 C34 119.5(8) . . ?
C33 C34 C35 117.4(8) . . ?
N7 C35 C34 123.5(7) . . ?
N8 C36 C37 124.3(6) . . ?
C36 C37 C38 118.8(7) . . ?
C39 C38 C37 117.6(6) . . ?
C38 C39 C40 119.8(7) . . ?
N8 C40 C39 123.5(7) . . ?
N9 C41 C42 123.8(10) . . ?
C43 C42 C41 118.5(8) . . ?
C42 C43 C44 118.2(8) . . ?
C43 C44 C45 119.8(8) . . ?
N9 C45 C44 124.5(8) . . ?
N10 C46 C47 123.2(8) . . ?
C46 C47 C48 118.8(8) . . ?
C49 C48 C47 118.4(8) . . ?
C48 C49 C50 117.9(8) . . ?
N10 C50 C49 125.6(9) . . ?