# Supplementary Material (ESI) for Dalton Transactions
# This journal is (c) The Royal Society of Chemistry 2010

data_global

_journal_coden_Cambridge         222

_publ_requested_journal          'Dalton Transactions'

loop_
_publ_author_name
'Trevor Hayton'
'David D. Schnaars'
'Lani A Seaman'
'Guang Wu.'

_publ_contact_author_name        'Trevor Hayton'
_publ_contact_author_address     
;
Department of Chemistry and Biochemistry
University of California Santa Barbara
Santa Barbara
CA
CA 93106 - 9510
UNITED STATES OF AMERICA
;

_publ_contact_author_email       HAYTON@CHEM.UCSB.EDU

_publ_section_title              
;
Isolation of a uranyl amide by "ate" complex formation
;

# Attachment 'dalton_comm_merge.CIF'

data_g:\lani\ls_3_5\work\ls_3_51m
_database_code_depnum_ccdc_archive 'CCDC 763967'
#TrackingRef 'dalton_comm_merge.CIF'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
Complex 1
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C45 H97 Cl Li3 N6 O10 U2'
_chemical_formula_weight         1414.62

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'
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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   12.5313(12)
_cell_length_b                   12.7238(13)
_cell_length_c                   19.6221(19)
_cell_angle_alpha                83.505(2)
_cell_angle_beta                 73.948(2)
_cell_angle_gamma                77.607(2)
_cell_volume                     2931.8(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       irregular
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.602
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1398
_exptl_absorpt_coefficient_mu    5.615
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.309
_exptl_absorpt_correction_T_max  0.402
_exptl_absorpt_process_details   'psi scan'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(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  'CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            25453
_diffrn_reflns_av_R_equivalents  0.0819
_diffrn_reflns_av_sigmaI/netI    0.0791
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.08
_diffrn_reflns_theta_max         26.37
_reflns_number_total             11708
_reflns_number_gt                8776
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_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^ > 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^)+(0.0664P)^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_number_reflns         11708
_refine_ls_number_parameters     611
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0635
_refine_ls_R_factor_gt           0.0441
_refine_ls_wR_factor_ref         0.1234
_refine_ls_wR_factor_gt          0.1106
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_restrained_S_all      1.046
_refine_ls_shift/su_max          0.100
_refine_ls_shift/su_mean         0.002

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
O2 O 0.7930(4) 0.7328(4) 0.6457(2) 0.0278(11) Uani 1 1 d . . .
U2 U 0.708400(19) 0.63499(2) 0.695016(13) 0.02216(9) Uani 1 1 d . . .
U1 U 0.449126(19) 0.836040(19) 0.791522(13) 0.02122(9) Uani 1 1 d . . .
Cl1 Cl 0.74825(16) 1.03075(16) 0.61278(12) 0.0426(5) Uani 1 1 d . . .
O1 O 0.6194(4) 0.5423(4) 0.7499(2) 0.0273(11) Uani 1 1 d . . .
O4 O 0.4940(4) 0.9600(4) 0.7466(2) 0.0294(11) Uani 1 1 d . . .
O3 O 0.4126(4) 0.7065(4) 0.8333(3) 0.0311(12) Uani 1 1 d . . .
N6 N 0.4233(5) 0.9008(5) 0.8980(3) 0.0338(15) Uani 1 1 d . . .
N1 N 0.7332(5) 0.5538(5) 0.5945(3) 0.0289(14) Uani 1 1 d . . .
O5 O 0.3620(4) 0.4714(4) 0.8343(3) 0.0396(13) Uani 1 1 d . . .
N3 N 0.5260(5) 0.7525(5) 0.6763(3) 0.0236(13) Uani 1 1 d . . .
N4 N 0.6518(5) 0.7512(5) 0.7982(3) 0.0279(14) Uani 1 1 d . . .
O7 O 0.4933(4) 1.2025(4) 0.6776(3) 0.0441(14) Uani 1 1 d . . .
O6 O 0.5171(5) 0.4532(4) 0.9063(3) 0.0411(14) Uani 1 1 d . . .
O10 O 1.0048(4) 0.8520(5) 0.5724(3) 0.0395(13) Uani 1 1 d . . .
O8 O 0.6240(5) 1.1565(4) 0.7700(3) 0.0403(14) Uani 1 1 d . . .
O9 O 0.8809(5) 0.8364(5) 0.4851(3) 0.0410(14) Uani 1 1 d . . .
N5 N 0.2717(5) 0.8945(5) 0.7804(3) 0.0314(15) Uani 1 1 d . . .
N2 N 0.8623(5) 0.5197(5) 0.7138(4) 0.0339(15) Uani 1 1 d . . .
C15 C 0.4563(6) 0.6817(6) 0.6604(4) 0.0304(17) Uani 1 1 d . . .
H15A H 0.4283 0.6394 0.7035 0.036 Uiso 1 1 calc R . .
H15B H 0.5051 0.6318 0.6258 0.036 Uiso 1 1 calc R . .
C11 C 0.5622(6) 0.8221(6) 0.6120(4) 0.0274(16) Uani 1 1 d . . .
H11A H 0.6161 0.7778 0.5758 0.033 Uiso 1 1 calc R . .
H11B H 0.6006 0.8737 0.6233 0.033 Uiso 1 1 calc R . .
C20 C 0.6483(6) 0.6969(6) 0.8692(4) 0.0307(17) Uani 1 1 d . . .
H20A H 0.6037 0.6410 0.8764 0.037 Uiso 1 1 calc R . .
H20B H 0.6103 0.7489 0.9049 0.037 Uiso 1 1 calc R . .
C16 C 0.7155(6) 0.8383(6) 0.7923(4) 0.0303(17) Uani 1 1 d . . .
H16A H 0.6753 0.8884 0.8289 0.036 Uiso 1 1 calc R . .
H16B H 0.7190 0.8774 0.7466 0.036 Uiso 1 1 calc R . .
C14 C 0.3572(6) 0.7384(6) 0.6327(4) 0.0323(17) Uani 1 1 d . . .
H14A H 0.3035 0.7838 0.6684 0.039 Uiso 1 1 calc R . .
H14B H 0.3192 0.6859 0.6220 0.039 Uiso 1 1 calc R . .
C19 C 0.7641(6) 0.6465(6) 0.8803(4) 0.0342(18) Uani 1 1 d . . .
H19A H 0.7558 0.6130 0.9279 0.041 Uiso 1 1 calc R . .
H19B H 0.8014 0.5912 0.8467 0.041 Uiso 1 1 calc R . .
C30 C 0.3810(7) 0.8456(7) 0.9659(4) 0.041(2) Uani 1 1 d . . .
H30A H 0.4333 0.8421 0.9948 0.049 Uiso 1 1 calc R . .
H30B H 0.3793 0.7722 0.9578 0.049 Uiso 1 1 calc R . .
C25 C 0.1724(7) 0.8450(8) 0.8132(4) 0.045(2) Uani 1 1 d . . .
H25A H 0.1483 0.8214 0.7755 0.053 Uiso 1 1 calc R . .
H25B H 0.1959 0.7811 0.8415 0.053 Uiso 1 1 calc R . .
C1 C 0.8080(7) 0.5789(7) 0.5265(4) 0.040(2) Uani 1 1 d . . .
H1A H 0.8744 0.5219 0.5167 0.048 Uiso 1 1 calc R . .
H1B H 0.8327 0.6453 0.5288 0.048 Uiso 1 1 calc R . .
C17 C 0.8348(6) 0.7968(6) 0.7997(4) 0.0363(18) Uani 1 1 d . . .
H17A H 0.8719 0.8573 0.7967 0.044 Uiso 1 1 calc R . .
H17B H 0.8772 0.7515 0.7608 0.044 Uiso 1 1 calc R . .
C13 C 0.3994(6) 0.8075(7) 0.5655(4) 0.042(2) Uani 1 1 d . . .
H13A H 0.4474 0.7615 0.5282 0.051 Uiso 1 1 calc R . .
H13B H 0.3356 0.8484 0.5490 0.051 Uiso 1 1 calc R . .
C18 C 0.8355(7) 0.7325(7) 0.8697(4) 0.041(2) Uani 1 1 d . . .
H18A H 0.8056 0.7805 0.9085 0.049 Uiso 1 1 calc R . .
H18B H 0.9126 0.6988 0.8699 0.049 Uiso 1 1 calc R . .
C26 C 0.4288(7) 1.0106(7) 0.9101(4) 0.041(2) Uani 1 1 d . . .
H26A H 0.4557 1.0479 0.8647 0.050 Uiso 1 1 calc R . .
H26B H 0.4831 1.0075 0.9375 0.050 Uiso 1 1 calc R . .
C5 C 0.6995(9) 0.4526(7) 0.5900(5) 0.052(2) Uani 1 1 d . . .
H5A H 0.6490 0.4355 0.6353 0.062 Uiso 1 1 calc R . .
H5B H 0.7664 0.3959 0.5826 0.062 Uiso 1 1 calc R . .
C12 C 0.4651(6) 0.8831(7) 0.5818(4) 0.040(2) Uani 1 1 d . . .
H12A H 0.4148 0.9332 0.6159 0.048 Uiso 1 1 calc R . .
H12B H 0.4951 0.9244 0.5388 0.048 Uiso 1 1 calc R . .
C22 C 0.1364(7) 1.0703(7) 0.7835(5) 0.046(2) Uani 1 1 d . . .
H22A H 0.1136 1.1313 0.7528 0.055 Uiso 1 1 calc R . .
H22B H 0.1603 1.0973 0.8201 0.055 Uiso 1 1 calc R . .
C21 C 0.2345(6) 0.9945(7) 0.7406(4) 0.039(2) Uani 1 1 d . . .
H21A H 0.2135 0.9759 0.7001 0.047 Uiso 1 1 calc R . .
H21B H 0.2976 1.0315 0.7225 0.047 Uiso 1 1 calc R . .
C23 C 0.0351(6) 1.0171(7) 0.8184(5) 0.048(2) Uani 1 1 d . . .
H23A H 0.0009 1.0027 0.7825 0.058 Uiso 1 1 calc R . .
H23B H -0.0212 1.0647 0.8516 0.058 Uiso 1 1 calc R . .
C2 C 0.7506(8) 0.5915(7) 0.4657(4) 0.047(2) Uani 1 1 d . . .
H2A H 0.6858 0.6504 0.4742 0.056 Uiso 1 1 calc R . .
H2B H 0.8032 0.6085 0.4214 0.056 Uiso 1 1 calc R . .
C7 C 1.0579(7) 0.4980(8) 0.7218(5) 0.052(2) Uani 1 1 d . . .
H7A H 1.0356 0.5421 0.7625 0.062 Uiso 1 1 calc R . .
H7B H 1.1331 0.5073 0.6946 0.062 Uiso 1 1 calc R . .
C29 C 0.2646(7) 0.8984(8) 1.0064(5) 0.050(2) Uani 1 1 d . . .
H29A H 0.2426 0.8591 1.0517 0.059 Uiso 1 1 calc R . .
H29B H 0.2103 0.8971 0.9798 0.059 Uiso 1 1 calc R . .
C24 C 0.0755(7) 0.9110(7) 0.8577(5) 0.047(2) Uani 1 1 d . . .
H24A H 0.0952 0.9270 0.8994 0.056 Uiso 1 1 calc R . .
H24B H 0.0143 0.8712 0.8736 0.056 Uiso 1 1 calc R . .
C6 C 0.9784(6) 0.5343(7) 0.6774(5) 0.046(2) Uani 1 1 d . . .
H6A H 1.0050 0.4946 0.6346 0.055 Uiso 1 1 calc R . .
H6B H 0.9773 0.6101 0.6633 0.055 Uiso 1 1 calc R . .
C33 C 0.4448(7) 0.3769(8) 0.9236(5) 0.054(3) Uani 1 1 d . . .
H33A H 0.4315 0.3542 0.9736 0.064 Uiso 1 1 calc R . .
H33B H 0.4793 0.3139 0.8961 0.064 Uiso 1 1 calc R . .
C34 C 0.6204(7) 0.4117(7) 0.9234(5) 0.054(2) Uani 1 1 d . . .
H34A H 0.6075 0.4023 0.9741 0.081 Uiso 1 1 calc R . .
H34B H 0.6711 0.4611 0.9051 0.081 Uiso 1 1 calc R . .
H34C H 0.6531 0.3435 0.9027 0.081 Uiso 1 1 calc R . .
C28 C 0.2646(7) 1.0149(8) 1.0186(5) 0.049(2) Uani 1 1 d . . .
H28A H 0.3078 1.0157 1.0525 0.058 Uiso 1 1 calc R . .
H28B H 0.1876 1.0517 1.0383 0.058 Uiso 1 1 calc R . .
C8 C 1.0612(7) 0.3798(8) 0.7477(6) 0.059(3) Uani 1 1 d . . .
H8A H 1.1074 0.3605 0.7812 0.071 Uiso 1 1 calc R . .
H8B H 1.0946 0.3342 0.7079 0.071 Uiso 1 1 calc R . .
C10 C 0.8640(6) 0.4081(7) 0.7370(5) 0.048(2) Uani 1 1 d . . .
H10A H 0.8874 0.3660 0.6953 0.058 Uiso 1 1 calc R . .
H10B H 0.7874 0.3999 0.7617 0.058 Uiso 1 1 calc R . .
C37 C 0.6086(8) 1.2613(7) 0.7360(5) 0.047(2) Uani 1 1 d . . .
H37A H 0.6666 1.2647 0.6917 0.056 Uiso 1 1 calc R . .
H37B H 0.6129 1.3145 0.7664 0.056 Uiso 1 1 calc R . .
C27 C 0.3161(8) 1.0746(7) 0.9489(5) 0.054(2) Uani 1 1 d . . .
H27A H 0.2645 1.0872 0.9187 0.065 Uiso 1 1 calc R . .
H27B H 0.3264 1.1441 0.9590 0.065 Uiso 1 1 calc R . .
C38 C 0.7322(8) 1.1283(8) 0.7845(5) 0.057(3) Uani 1 1 d . . .
H38A H 0.7902 1.1269 0.7406 0.086 Uiso 1 1 calc R . .
H38B H 0.7397 1.0584 0.8089 0.086 Uiso 1 1 calc R . .
H38C H 0.7395 1.1806 0.8137 0.086 Uiso 1 1 calc R . .
C31 C 0.2639(7) 0.5144(8) 0.8098(5) 0.055(3) Uani 1 1 d . . .
H31A H 0.2138 0.4637 0.8217 0.082 Uiso 1 1 calc R . .
H31B H 0.2856 0.5278 0.7592 0.082 Uiso 1 1 calc R . .
H31C H 0.2260 0.5807 0.8319 0.082 Uiso 1 1 calc R . .
C36 C 0.4933(8) 1.2827(7) 0.7221(6) 0.051(2) Uani 1 1 d . . .
H36A H 0.4354 1.2792 0.7664 0.061 Uiso 1 1 calc R . .
H36B H 0.4781 1.3538 0.6990 0.061 Uiso 1 1 calc R . .
C32 C 0.3363(7) 0.4296(8) 0.9068(5) 0.053(3) Uani 1 1 d . . .
H32A H 0.2873 0.3776 0.9133 0.063 Uiso 1 1 calc R . .
H32B H 0.2977 0.4875 0.9381 0.063 Uiso 1 1 calc R . .
C9 C 0.9387(7) 0.3620(8) 0.7842(6) 0.059(3) Uani 1 1 d . . .
H9A H 0.9388 0.2855 0.7938 0.070 Uiso 1 1 calc R . .
H9B H 0.9107 0.3966 0.8290 0.070 Uiso 1 1 calc R . .
C3 C 0.7124(8) 0.4875(8) 0.4605(5) 0.058(3) Uani 1 1 d . . .
H3A H 0.6676 0.4989 0.4261 0.070 Uiso 1 1 calc R . .
H3B H 0.7780 0.4315 0.4442 0.070 Uiso 1 1 calc R . .
C4 C 0.6421(8) 0.4518(9) 0.5326(6) 0.066(3) Uani 1 1 d . . .
H4A H 0.5689 0.4997 0.5437 0.079 Uiso 1 1 calc R . .
H4B H 0.6298 0.3797 0.5305 0.079 Uiso 1 1 calc R . .
Li2 Li 0.5867(9) 1.0654(10) 0.7032(7) 0.030(3) Uani 1 1 d . . .
Li1 Li 0.4837(10) 0.5557(10) 0.8234(7) 0.029(3) Uani 1 1 d . . .
C41 C 1.0614(7) 0.8010(7) 0.5081(5) 0.049(2) Uani 1 1 d . . .
H41A H 1.0636 0.7240 0.5152 0.059 Uiso 1 1 calc R . .
H41B H 1.1385 0.8131 0.4920 0.059 Uiso 1 1 calc R . .
C40 C 0.9970(7) 0.8489(8) 0.4546(5) 0.050(2) Uani 1 1 d . . .
H40A H 1.0008 0.9246 0.4442 0.060 Uiso 1 1 calc R . .
H40B H 1.0286 0.8119 0.4107 0.060 Uiso 1 1 calc R . .
C42 C 1.0678(7) 0.8283(9) 0.6242(5) 0.058(3) Uani 1 1 d . . .
H42A H 1.0809 0.7521 0.6358 0.087 Uiso 1 1 calc R . .
H42B H 1.0260 0.8656 0.6662 0.087 Uiso 1 1 calc R . .
H42C H 1.1390 0.8512 0.6056 0.087 Uiso 1 1 calc R . .
C39 C 0.8089(9) 0.8819(9) 0.4409(5) 0.063(3) Uani 1 1 d . . .
H39A H 0.8144 0.9562 0.4288 0.094 Uiso 1 1 calc R . .
H39B H 0.7323 0.8772 0.4654 0.094 Uiso 1 1 calc R . .
H39C H 0.8313 0.8433 0.3983 0.094 Uiso 1 1 calc R . .
C35 C 0.3954(9) 1.2223(8) 0.6516(7) 0.075(3) Uani 1 1 d . . .
H35A H 0.3290 1.2311 0.6907 0.113 Uiso 1 1 calc R . .
H35B H 0.3967 1.1624 0.6254 0.113 Uiso 1 1 calc R . .
H35C H 0.3944 1.2867 0.6209 0.113 Uiso 1 1 calc R . .
Li3 Li 0.8402(9) 0.8562(11) 0.5896(6) 0.031(3) Uani 1 1 d . . .
C43 C 1.0034(18) 0.2660(11) 0.9625(10) 0.184(9) Uani 1 1 d D . .
H43A H 1.0705 0.2850 0.9304 0.276 Uiso 1 1 calc R . .
H43B H 0.9625 0.2376 0.9364 0.276 Uiso 1 1 calc R . .
H43C H 1.0240 0.2125 0.9976 0.276 Uiso 1 1 calc R . .
C44 C 0.9198(12) 0.3783(15) 1.0035(9) 0.188(12) Uani 1 1 d D . .
H44A H 0.8565 0.4091 0.9836 0.226 Uiso 1 1 calc R . .
H44B H 0.8939 0.3665 1.0546 0.226 Uiso 1 1 calc R . .
C45 C 1.0105(15) 0.4390(11) 0.9819(9) 0.133(7) Uani 1 1 d D . .
H45A H 1.0275 0.4515 0.9307 0.160 Uiso 1 1 calc R . .
H45B H 1.0772 0.3938 0.9929 0.160 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
O2 0.026(2) 0.025(3) 0.027(3) 0.004(2) -0.002(2) -0.002(2)
U2 0.02112(14) 0.01779(15) 0.02477(15) 0.00398(11) -0.00521(11) -0.00144(10)
U1 0.02103(14) 0.01874(15) 0.02181(15) 0.00301(11) -0.00513(11) -0.00212(10)
Cl1 0.0345(10) 0.0280(10) 0.0530(13) 0.0035(9) 0.0066(9) -0.0058(8)
O1 0.028(2) 0.026(3) 0.023(3) 0.005(2) -0.006(2) -0.001(2)
O4 0.033(3) 0.030(3) 0.024(3) 0.006(2) -0.008(2) -0.004(2)
O3 0.034(3) 0.028(3) 0.031(3) 0.009(2) -0.010(2) -0.007(2)
N6 0.038(3) 0.037(4) 0.024(3) 0.003(3) -0.007(3) -0.008(3)
N1 0.031(3) 0.024(3) 0.030(3) 0.003(3) -0.005(3) -0.008(3)
O5 0.043(3) 0.034(3) 0.042(3) 0.008(3) -0.010(3) -0.014(3)
N3 0.022(3) 0.025(3) 0.020(3) 0.004(2) -0.007(2) 0.000(2)
N4 0.030(3) 0.028(3) 0.028(3) 0.005(3) -0.014(3) -0.006(3)
O7 0.043(3) 0.030(3) 0.059(4) 0.008(3) -0.022(3) -0.001(3)
O6 0.046(3) 0.031(3) 0.046(3) 0.013(3) -0.015(3) -0.012(3)
O10 0.028(3) 0.046(3) 0.042(3) 0.006(3) -0.007(2) -0.007(2)
O8 0.051(3) 0.028(3) 0.046(3) 0.010(3) -0.018(3) -0.018(3)
O9 0.048(3) 0.040(3) 0.032(3) 0.007(3) -0.008(3) -0.010(3)
N5 0.025(3) 0.036(4) 0.028(3) 0.009(3) -0.005(3) -0.003(3)
N2 0.025(3) 0.019(3) 0.051(4) 0.005(3) -0.008(3) 0.006(3)
C15 0.033(4) 0.022(4) 0.037(4) 0.001(3) -0.011(3) -0.008(3)
C11 0.027(4) 0.022(4) 0.029(4) 0.001(3) -0.007(3) 0.003(3)
C20 0.032(4) 0.035(4) 0.024(4) 0.011(3) -0.011(3) -0.005(3)
C16 0.031(4) 0.025(4) 0.032(4) 0.001(3) -0.005(3) -0.006(3)
C14 0.032(4) 0.035(4) 0.029(4) -0.001(3) -0.010(3) -0.001(3)
C19 0.033(4) 0.034(5) 0.034(4) 0.009(4) -0.013(3) -0.003(3)
C30 0.054(5) 0.037(5) 0.029(4) -0.002(4) -0.016(4) 0.002(4)
C25 0.050(5) 0.072(7) 0.026(4) 0.021(4) -0.018(4) -0.045(5)
C1 0.041(4) 0.041(5) 0.032(4) -0.004(4) -0.001(4) -0.007(4)
C17 0.039(4) 0.033(4) 0.043(5) 0.000(4) -0.014(4) -0.015(4)
C13 0.035(4) 0.052(6) 0.039(5) 0.001(4) -0.021(4) 0.005(4)
C18 0.038(4) 0.044(5) 0.045(5) 0.001(4) -0.023(4) -0.005(4)
C26 0.060(5) 0.036(5) 0.029(4) -0.006(4) -0.005(4) -0.017(4)
C5 0.071(6) 0.033(5) 0.041(5) -0.010(4) 0.005(5) -0.009(5)
C12 0.040(4) 0.045(5) 0.031(4) 0.013(4) -0.016(4) 0.001(4)
C22 0.040(5) 0.037(5) 0.052(5) 0.001(4) -0.011(4) 0.006(4)
C21 0.031(4) 0.036(5) 0.046(5) 0.016(4) -0.012(4) -0.002(4)
C23 0.023(4) 0.054(6) 0.057(6) 0.002(5) -0.005(4) 0.004(4)
C2 0.066(6) 0.038(5) 0.029(4) -0.005(4) -0.010(4) 0.005(4)
C7 0.035(4) 0.057(6) 0.066(6) 0.004(5) -0.018(4) -0.011(4)
C29 0.044(5) 0.069(7) 0.033(5) -0.005(5) 0.001(4) -0.019(5)
C24 0.033(4) 0.048(6) 0.053(6) 0.008(4) -0.005(4) -0.009(4)
C6 0.034(4) 0.038(5) 0.063(6) 0.013(4) -0.010(4) -0.014(4)
C33 0.040(5) 0.052(6) 0.060(6) 0.031(5) -0.006(4) -0.015(4)
C34 0.056(6) 0.041(5) 0.068(6) 0.018(5) -0.028(5) -0.012(4)
C28 0.039(5) 0.059(6) 0.040(5) -0.016(5) 0.003(4) -0.004(4)
C8 0.040(5) 0.045(6) 0.089(8) 0.012(5) -0.024(5) 0.003(4)
C10 0.028(4) 0.034(5) 0.080(7) 0.016(5) -0.018(4) -0.005(4)
C37 0.058(5) 0.023(4) 0.065(6) 0.005(4) -0.022(5) -0.013(4)
C27 0.077(7) 0.035(5) 0.042(5) -0.013(4) -0.006(5) 0.002(5)
C38 0.069(6) 0.051(6) 0.074(7) 0.013(5) -0.050(6) -0.026(5)
C31 0.039(5) 0.056(6) 0.070(7) 0.011(5) -0.017(5) -0.015(4)
C36 0.050(5) 0.025(5) 0.070(7) 0.000(4) -0.014(5) 0.004(4)
C32 0.043(5) 0.057(6) 0.053(6) 0.027(5) -0.006(4) -0.023(4)
C9 0.044(5) 0.044(6) 0.079(7) 0.017(5) -0.014(5) -0.001(4)
C3 0.069(6) 0.045(6) 0.068(7) -0.025(5) -0.033(6) 0.005(5)
C4 0.049(6) 0.067(7) 0.080(8) -0.041(6) 0.006(5) -0.020(5)
Li2 0.023(6) 0.026(7) 0.036(7) 0.008(5) -0.001(5) -0.006(5)
Li1 0.029(6) 0.021(6) 0.034(7) 0.003(5) 0.002(5) -0.010(5)
C41 0.044(5) 0.037(5) 0.057(6) 0.002(4) 0.001(4) -0.009(4)
C40 0.059(6) 0.048(6) 0.037(5) 0.002(4) 0.001(4) -0.017(5)
C42 0.040(5) 0.073(7) 0.066(6) 0.022(6) -0.026(5) -0.021(5)
C39 0.077(7) 0.078(8) 0.044(6) 0.016(5) -0.029(5) -0.032(6)
C35 0.082(7) 0.044(6) 0.114(10) 0.010(6) -0.063(8) -0.001(5)
Li3 0.021(6) 0.040(8) 0.025(6) -0.006(6) 0.003(5) -0.004(5)
C43 0.19(2) 0.21(2) 0.136(17) 0.052(17) -0.065(16) 0.003(18)
C44 0.093(12) 0.33(3) 0.085(12) 0.042(17) 0.000(10) 0.017(17)
C45 0.119(12) 0.165(18) 0.125(15) 0.086(14) -0.046(11) -0.075(15)

_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
O2 U2 1.827(5) . ?
O2 Li3 1.917(14) . ?
U2 O1 1.846(5) . ?
U2 N1 2.245(6) . ?
U2 N2 2.251(5) . ?
U2 N4 2.494(6) . ?
U2 N3 2.543(5) . ?
U1 O4 1.836(5) . ?
U1 O3 1.847(5) . ?
U1 N6 2.248(6) . ?
U1 N5 2.251(6) . ?
U1 N3 2.463(6) . ?
U1 N4 2.571(6) . ?
Cl1 Li2 2.291(12) . ?
Cl1 Li3 2.304(13) . ?
O1 Li1 1.892(12) . ?
O4 Li2 1.934(13) . ?
O3 Li1 1.941(13) . ?
N6 C30 1.451(10) . ?
N6 C26 1.463(10) . ?
N1 C1 1.450(9) . ?
N1 C5 1.458(10) . ?
O5 C31 1.422(9) . ?
O5 C32 1.435(10) . ?
O5 Li1 1.998(13) . ?
N3 C11 1.479(9) . ?
N3 C15 1.491(9) . ?
N4 C16 1.476(9) . ?
N4 C20 1.478(8) . ?
O7 C36 1.416(10) . ?
O7 C35 1.419(10) . ?
O7 Li2 1.979(13) . ?
O6 C34 1.405(9) . ?
O6 C33 1.418(10) . ?
O6 Li1 2.045(13) . ?
O10 C41 1.416(10) . ?
O10 C42 1.421(9) . ?
O10 Li3 1.986(12) . ?
O8 C37 1.421(9) . ?
O8 C38 1.425(9) . ?
O8 Li2 2.047(15) . ?
O9 C39 1.413(10) . ?
O9 C40 1.448(10) . ?
O9 Li3 2.001(13) . ?
N5 C25 1.469(9) . ?
N5 C21 1.473(9) . ?
N2 C10 1.438(10) . ?
N2 C6 1.474(9) . ?
C15 C14 1.504(9) . ?
C11 C12 1.524(9) . ?
C20 C19 1.519(9) . ?
C16 C17 1.516(10) . ?
C14 C13 1.531(11) . ?
C19 C18 1.519(11) . ?
C30 C29 1.507(11) . ?
C25 C24 1.444(12) . ?
C1 C2 1.531(11) . ?
C17 C18 1.518(11) . ?
C13 C12 1.504(11) . ?
C26 C27 1.512(12) . ?
C5 C4 1.498(14) . ?
C22 C21 1.501(11) . ?
C22 C23 1.523(11) . ?
C23 C24 1.536(11) . ?
C2 C3 1.524(12) . ?
C7 C6 1.469(11) . ?
C7 C8 1.527(12) . ?
C29 C28 1.528(13) . ?
C33 C32 1.488(11) . ?
C28 C27 1.533(12) . ?
C8 C9 1.557(12) . ?
C10 C9 1.483(11) . ?
C37 C36 1.505(12) . ?
C3 C4 1.523(13) . ?
C41 C40 1.497(12) . ?
C43 C44 1.715(10) . ?
C44 C45 1.450(10) . ?
C45 C45 1.72(3) 2_767 ?

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
U2 O2 Li3 163.3(4) . . ?
O2 U2 O1 176.2(2) . . ?
O2 U2 N1 90.3(2) . . ?
O1 U2 N1 93.4(2) . . ?
O2 U2 N2 92.1(2) . . ?
O1 U2 N2 89.0(2) . . ?
N1 U2 N2 88.6(2) . . ?
O2 U2 N4 87.7(2) . . ?
O1 U2 N4 88.5(2) . . ?
N1 U2 N4 168.7(2) . . ?
N2 U2 N4 102.6(2) . . ?
O2 U2 N3 92.34(19) . . ?
O1 U2 N3 86.63(19) . . ?
N1 U2 N3 90.0(2) . . ?
N2 U2 N3 175.3(2) . . ?
N4 U2 N3 79.00(18) . . ?
O4 U1 O3 176.3(2) . . ?
O4 U1 N6 90.6(2) . . ?
O3 U1 N6 91.6(2) . . ?
O4 U1 N5 92.1(2) . . ?
O3 U1 N5 90.5(2) . . ?
N6 U1 N5 97.7(2) . . ?
O4 U1 N3 87.8(2) . . ?
O3 U1 N3 89.4(2) . . ?
N6 U1 N3 165.9(2) . . ?
N5 U1 N3 96.3(2) . . ?
O4 U1 N4 91.6(2) . . ?
O3 U1 N4 85.6(2) . . ?
N6 U1 N4 87.0(2) . . ?
N5 U1 N4 174.0(2) . . ?
N3 U1 N4 79.04(18) . . ?
Li2 Cl1 Li3 120.7(5) . . ?
U2 O1 Li1 136.1(5) . . ?
U1 O4 Li2 161.8(4) . . ?
U1 O3 Li1 135.4(4) . . ?
C30 N6 C26 108.9(6) . . ?
C30 N6 U1 124.8(5) . . ?
C26 N6 U1 125.6(5) . . ?
C1 N1 C5 108.0(6) . . ?
C1 N1 U2 125.0(5) . . ?
C5 N1 U2 125.5(5) . . ?
C31 O5 C32 113.1(6) . . ?
C31 O5 Li1 121.7(6) . . ?
C32 O5 Li1 106.4(6) . . ?
C11 N3 C15 108.2(5) . . ?
C11 N3 U1 118.5(4) . . ?
C15 N3 U1 115.2(4) . . ?
C11 N3 U2 104.8(4) . . ?
C15 N3 U2 108.4(4) . . ?
U1 N3 U2 100.48(19) . . ?
C16 N4 C20 105.9(6) . . ?
C16 N4 U2 116.3(4) . . ?
C20 N4 U2 117.4(5) . . ?
C16 N4 U1 108.7(4) . . ?
C20 N4 U1 109.1(4) . . ?
U2 N4 U1 98.9(2) . . ?
C36 O7 C35 113.2(7) . . ?
C36 O7 Li2 109.1(6) . . ?
C35 O7 Li2 130.6(7) . . ?
C34 O6 C33 111.6(6) . . ?
C34 O6 Li1 129.8(6) . . ?
C33 O6 Li1 110.3(6) . . ?
C41 O10 C42 113.1(7) . . ?
C41 O10 Li3 108.1(6) . . ?
C42 O10 Li3 126.3(6) . . ?
C37 O8 C38 110.9(6) . . ?
C37 O8 Li2 102.4(6) . . ?
C38 O8 Li2 118.8(6) . . ?
C39 O9 C40 113.1(6) . . ?
C39 O9 Li3 123.6(7) . . ?
C40 O9 Li3 108.9(6) . . ?
C25 N5 C21 107.9(6) . . ?
C25 N5 U1 127.4(5) . . ?
C21 N5 U1 124.6(5) . . ?
C10 N2 C6 109.2(6) . . ?
C10 N2 U2 123.9(5) . . ?
C6 N2 U2 122.4(5) . . ?
N3 C15 C14 115.8(6) . . ?
N3 C11 C12 113.8(6) . . ?
N4 C20 C19 113.9(6) . . ?
N4 C16 C17 112.8(6) . . ?
C15 C14 C13 109.1(6) . . ?
C18 C19 C20 109.8(6) . . ?
N6 C30 C29 114.0(7) . . ?
C24 C25 N5 117.0(8) . . ?
N1 C1 C2 112.3(7) . . ?
C16 C17 C18 111.8(6) . . ?
C12 C13 C14 109.1(6) . . ?
C17 C18 C19 110.3(6) . . ?
N6 C26 C27 113.3(7) . . ?
N1 C5 C4 115.1(8) . . ?
C13 C12 C11 111.4(7) . . ?
C21 C22 C23 112.7(7) . . ?
N5 C21 C22 114.1(7) . . ?
C22 C23 C24 108.8(6) . . ?
C3 C2 C1 110.0(7) . . ?
C6 C7 C8 111.7(8) . . ?
C30 C29 C28 109.7(7) . . ?
C25 C24 C23 111.9(7) . . ?
C7 C6 N2 113.0(7) . . ?
O6 C33 C32 107.6(7) . . ?
C29 C28 C27 111.0(7) . . ?
C7 C8 C9 109.4(7) . . ?
N2 C10 C9 115.8(7) . . ?
O8 C37 C36 106.8(7) . . ?
C26 C27 C28 111.3(7) . . ?
O7 C36 C37 107.2(7) . . ?
O5 C32 C33 107.9(7) . . ?
C10 C9 C8 109.6(8) . . ?
C4 C3 C2 110.3(8) . . ?
C5 C4 C3 111.5(8) . . ?
O4 Li2 O7 111.1(6) . . ?
O4 Li2 O8 117.1(6) . . ?
O7 Li2 O8 84.3(5) . . ?
O4 Li2 Cl1 123.9(6) . . ?
O7 Li2 Cl1 108.1(6) . . ?
O8 Li2 Cl1 105.1(5) . . ?
O1 Li1 O3 110.1(6) . . ?
O1 Li1 O5 125.1(7) . . ?
O3 Li1 O5 107.9(6) . . ?
O1 Li1 O6 106.9(6) . . ?
O3 Li1 O6 123.5(7) . . ?
O5 Li1 O6 82.3(5) . . ?
O10 C41 C40 107.2(7) . . ?
O9 C40 C41 107.0(7) . . ?
O2 Li3 O10 112.5(6) . . ?
O2 Li3 O9 112.7(7) . . ?
O10 Li3 O9 83.6(5) . . ?
O2 Li3 Cl1 123.3(6) . . ?
O10 Li3 Cl1 107.5(6) . . ?
O9 Li3 Cl1 110.1(6) . . ?
C45 C44 C43 92.9(7) . . ?
C44 C45 C45 118.1(18) . 2_767 ?

_diffrn_measured_fraction_theta_max 0.976
_diffrn_reflns_theta_full        26.37
_diffrn_measured_fraction_theta_full 0.976
_refine_diff_density_max         3.568
_refine_diff_density_min         -1.460
_refine_diff_density_rms         0.191

#===END===

data_ls_4_14m
_database_code_depnum_ccdc_archive 'CCDC 763968'
#TrackingRef 'dalton_comm_merge.CIF'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
Complex 2
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C48 H76 Li2 N4 O6 U'
_chemical_formula_weight         1057.04

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'
U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   9.001(3)
_cell_length_b                   11.766(4)
_cell_length_c                   12.875(4)
_cell_angle_alpha                115.047(4)
_cell_angle_beta                 92.432(4)
_cell_angle_gamma                96.819(4)
_cell_volume                     1220.0(6)
_cell_formula_units_Z            1
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       sheet
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.439
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             538
_exptl_absorpt_coefficient_mu    3.375
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.374
_exptl_absorpt_correction_T_max  0.542
_exptl_absorpt_process_details   'psi scan'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(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  'CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10192
_diffrn_reflns_av_R_equivalents  0.0430
_diffrn_reflns_av_sigmaI/netI    0.0464
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.93
_diffrn_reflns_theta_max         26.37
_reflns_number_total             4843
_reflns_number_gt                4838
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_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^ > 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^)+(0.0438P)^2^+0.9791P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4843
_refine_ls_number_parameters     289
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0303
_refine_ls_R_factor_gt           0.0303
_refine_ls_wR_factor_ref         0.0753
_refine_ls_wR_factor_gt          0.0752
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_restrained_S_all      1.047
_refine_ls_shift/su_max          0.100
_refine_ls_shift/su_mean         0.007

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
O1 O 0.6579(3) 0.4151(2) 0.4782(2) 0.0218(5) Uani 1 1 d . . .
U1 U 0.5000 0.5000 0.5000 0.01732(7) Uani 1 2 d S . .
O3 O 0.7105(3) 0.6759(2) 0.2313(2) 0.0223(5) Uani 1 1 d . . .
O2 O 0.4249(3) 0.7416(3) 0.3389(2) 0.0285(6) Uani 1 1 d . . .
N1 N 0.3543(3) 0.3053(3) 0.4804(3) 0.0190(6) Uani 1 1 d . . .
H1 H 0.420(5) 0.250(4) 0.448(4) 0.023 Uiso 1 1 calc . . .
N2 N 0.4573(4) 0.4658(3) 0.3020(3) 0.0220(7) Uani 1 1 d . . .
H2 H 0.364(5) 0.488(4) 0.302(4) 0.026 Uiso 1 1 calc . . .
C9 C 0.4381(4) 0.3558(3) 0.1968(3) 0.0191(7) Uani 1 1 d . . .
C1 C 0.2216(4) 0.2387(3) 0.4076(3) 0.0200(7) Uani 1 1 d . . .
C6 C 0.0817(4) 0.2772(4) 0.4395(3) 0.0216(8) Uani 1 1 d . . .
C10 C 0.5614(4) 0.2966(4) 0.1477(3) 0.0234(8) Uani 1 1 d . . .
C14 C 0.2926(4) 0.3019(4) 0.1374(3) 0.0226(8) Uani 1 1 d . . .
C2 C 0.2260(4) 0.1329(4) 0.3019(3) 0.0232(8) Uani 1 1 d . . .
C5 C -0.0477(4) 0.2128(4) 0.3642(4) 0.0274(9) Uani 1 1 d . . .
H5 H -0.1397 0.2394 0.3850 0.033 Uiso 1 1 calc R . .
C21 C 0.7874(5) 0.7987(4) 0.2521(3) 0.0293(9) Uani 1 1 d . . .
H21A H 0.7362 0.8311 0.2049 0.035 Uiso 1 1 calc R . .
H21B H 0.8894 0.7921 0.2313 0.035 Uiso 1 1 calc R . .
C11 C 0.5392(5) 0.1882(4) 0.0454(3) 0.0291(9) Uani 1 1 d . . .
H11 H 0.6218 0.1507 0.0138 0.035 Uiso 1 1 calc R . .
C23 C 0.6861(5) 0.5897(4) 0.1107(3) 0.0269(8) Uani 1 1 d . . .
H23A H 0.6394 0.6304 0.0690 0.032 Uiso 1 1 calc R . .
H23B H 0.6171 0.5151 0.1007 0.032 Uiso 1 1 calc R . .
C15 C 0.1564(5) 0.3595(4) 0.1866(4) 0.0297(9) Uani 1 1 d . . .
H15A H 0.0676 0.3091 0.1370 0.045 Uiso 1 1 calc R . .
H15B H 0.1648 0.4442 0.1925 0.045 Uiso 1 1 calc R . .
H15C H 0.1498 0.3620 0.2618 0.045 Uiso 1 1 calc R . .
C16 C 0.7180(5) 0.3498(4) 0.2091(4) 0.0302(9) Uani 1 1 d . . .
H16A H 0.7275 0.3326 0.2754 0.045 Uiso 1 1 calc R . .
H16B H 0.7358 0.4399 0.2331 0.045 Uiso 1 1 calc R . .
H16C H 0.7904 0.3108 0.1578 0.045 Uiso 1 1 calc R . .
C13 C 0.2752(5) 0.1908(4) 0.0349(3) 0.0301(9) Uani 1 1 d . . .
H13 H 0.1794 0.1543 -0.0028 0.036 Uiso 1 1 calc R . .
C3 C 0.0942(5) 0.0707(4) 0.2296(4) 0.0325(10) Uani 1 1 d . . .
H3 H 0.0983 0.0012 0.1598 0.039 Uiso 1 1 calc R . .
C18 C 0.2075(5) 0.8430(4) 0.3664(4) 0.0311(9) Uani 1 1 d . . .
H18A H 0.2217 0.9311 0.3789 0.037 Uiso 1 1 calc R . .
H18B H 0.1135 0.8246 0.3943 0.037 Uiso 1 1 calc R . .
C8 C 0.3736(5) 0.0886(4) 0.2658(4) 0.0313(9) Uani 1 1 d . . .
H8A H 0.3582 0.0217 0.1889 0.047 Uiso 1 1 calc R . .
H8B H 0.4135 0.0577 0.3176 0.047 Uiso 1 1 calc R . .
H8C H 0.4432 0.1582 0.2679 0.047 Uiso 1 1 calc R . .
C12 C 0.3974(5) 0.1340(4) -0.0115(4) 0.0324(9) Uani 1 1 d . . .
H12 H 0.3843 0.0603 -0.0801 0.039 Uiso 1 1 calc R . .
C4 C -0.0430(5) 0.1102(4) 0.2595(4) 0.0341(10) Uani 1 1 d . . .
H4 H -0.1304 0.0686 0.2102 0.041 Uiso 1 1 calc R . .
C20 C 0.3723(5) 0.7362(5) 0.2303(4) 0.0338(10) Uani 1 1 d . . .
H20A H 0.3811 0.6548 0.1680 0.041 Uiso 1 1 calc R . .
H20B H 0.4294 0.8028 0.2164 0.041 Uiso 1 1 calc R . .
C17 C 0.3382(5) 0.8156(5) 0.4256(4) 0.0396(11) Uani 1 1 d . . .
H17A H 0.3995 0.8943 0.4788 0.048 Uiso 1 1 calc R . .
H17B H 0.3014 0.7694 0.4687 0.048 Uiso 1 1 calc R . .
C19 C 0.2090(5) 0.7548(5) 0.2396(4) 0.0396(11) Uani 1 1 d . . .
H19A H 0.1442 0.6748 0.2186 0.048 Uiso 1 1 calc R . .
H19B H 0.1771 0.7934 0.1908 0.048 Uiso 1 1 calc R . .
Li1 Li 0.5910(7) 0.6443(6) 0.3438(5) 0.0239(13) Uani 1 1 d . . .
C7 C 0.0690(4) 0.3866(4) 0.5527(3) 0.0259(8) Uani 1 1 d . . .
H7A H -0.0346 0.3975 0.5600 0.039 Uiso 1 1 calc R . .
H7B H 0.1260 0.4626 0.5559 0.039 Uiso 1 1 calc R . .
H7C H 0.1077 0.3697 0.6145 0.039 Uiso 1 1 calc R . .
C22 C 0.7904(5) 0.8878(4) 0.3768(4) 0.0324(9) Uani 1 1 d . . .
H22A H 0.6894 0.8979 0.3959 0.049 Uiso 1 1 calc R . .
H22B H 0.8460 0.9687 0.3911 0.049 Uiso 1 1 calc R . .
H22C H 0.8378 0.8538 0.4233 0.049 Uiso 1 1 calc R . .
C24 C 0.8298(5) 0.5490(5) 0.0599(4) 0.0380(10) Uani 1 1 d . . .
H24A H 0.8926 0.6205 0.0592 0.057 Uiso 1 1 calc R . .
H24B H 0.8062 0.4839 -0.0174 0.057 Uiso 1 1 calc R . .
H24C H 0.8820 0.5167 0.1058 0.057 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
O1 0.0182(12) 0.0254(14) 0.0258(13) 0.0133(11) 0.0066(10) 0.0073(10)
U1 0.01768(11) 0.01850(11) 0.01774(11) 0.00889(8) 0.00437(7) 0.00489(7)
O3 0.0262(14) 0.0228(14) 0.0192(12) 0.0100(11) 0.0061(10) 0.0040(11)
O2 0.0316(15) 0.0349(16) 0.0247(14) 0.0150(12) 0.0069(11) 0.0162(12)
N1 0.0158(15) 0.0200(16) 0.0212(15) 0.0086(13) 0.0031(12) 0.0031(12)
N2 0.0259(17) 0.0228(17) 0.0188(15) 0.0095(13) 0.0038(13) 0.0073(13)
C9 0.0280(19) 0.0175(18) 0.0149(16) 0.0103(14) 0.0029(14) 0.0017(14)
C1 0.0230(18) 0.0194(18) 0.0220(18) 0.0145(15) -0.0007(14) -0.0010(14)
C6 0.0236(18) 0.0242(19) 0.0222(18) 0.0155(16) 0.0029(14) 0.0024(15)
C10 0.029(2) 0.026(2) 0.0202(18) 0.0136(16) 0.0069(15) 0.0100(16)
C14 0.0253(19) 0.026(2) 0.0230(18) 0.0157(16) 0.0054(15) 0.0063(15)
C2 0.031(2) 0.0209(19) 0.0212(18) 0.0119(16) 0.0051(15) 0.0044(15)
C5 0.0216(19) 0.034(2) 0.033(2) 0.0210(19) 0.0005(16) 0.0009(16)
C21 0.034(2) 0.029(2) 0.028(2) 0.0167(18) 0.0059(17) -0.0019(17)
C11 0.039(2) 0.027(2) 0.0244(19) 0.0118(17) 0.0080(17) 0.0117(17)
C23 0.029(2) 0.031(2) 0.0185(18) 0.0093(16) 0.0019(15) 0.0026(16)
C15 0.028(2) 0.035(2) 0.030(2) 0.0184(18) 0.0035(16) 0.0044(17)
C16 0.028(2) 0.035(2) 0.026(2) 0.0096(18) 0.0058(16) 0.0118(17)
C13 0.032(2) 0.032(2) 0.027(2) 0.0162(18) -0.0053(17) -0.0040(17)
C3 0.048(3) 0.022(2) 0.024(2) 0.0095(17) -0.0045(18) -0.0034(18)
C18 0.030(2) 0.032(2) 0.035(2) 0.0159(19) 0.0077(17) 0.0117(17)
C8 0.046(3) 0.020(2) 0.025(2) 0.0063(17) 0.0084(18) 0.0065(18)
C12 0.048(3) 0.024(2) 0.0222(19) 0.0071(17) 0.0023(18) 0.0062(18)
C4 0.034(2) 0.033(2) 0.034(2) 0.0187(19) -0.0111(18) -0.0099(18)
C20 0.033(2) 0.047(3) 0.024(2) 0.0143(19) 0.0036(17) 0.020(2)
C17 0.039(3) 0.054(3) 0.029(2) 0.015(2) 0.0098(19) 0.028(2)
C19 0.032(2) 0.043(3) 0.038(2) 0.010(2) -0.0006(19) 0.016(2)
Li1 0.026(3) 0.024(3) 0.023(3) 0.010(3) 0.004(2) 0.006(3)
C7 0.0231(19) 0.028(2) 0.029(2) 0.0131(17) 0.0071(15) 0.0066(15)
C22 0.040(2) 0.025(2) 0.032(2) 0.0127(18) 0.0098(18) 0.0039(18)
C24 0.037(2) 0.042(3) 0.028(2) 0.007(2) 0.0126(18) 0.007(2)

_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
O1 U1 1.797(3) . ?
U1 O1 1.797(3) 2_666 ?
U1 N1 2.408(3) . ?
U1 N1 2.408(3) 2_666 ?
U1 N2 2.413(3) . ?
U1 N2 2.413(3) 2_666 ?
U1 Li1 3.210(7) . ?
U1 Li1 3.210(7) 2_666 ?
O3 C21 1.435(5) . ?
O3 C23 1.439(4) . ?
O3 Li1 1.970(7) . ?
O2 C17 1.423(5) . ?
O2 C20 1.431(5) . ?
O2 Li1 2.002(7) . ?
N1 C1 1.407(4) . ?
N1 Li1 2.102(7) 2_666 ?
N2 C9 1.407(5) . ?
N2 Li1 2.131(7) . ?
C9 C10 1.409(5) . ?
C9 C14 1.418(5) . ?
C1 C6 1.408(5) . ?
C1 C2 1.409(5) . ?
C6 C5 1.394(5) . ?
C6 C7 1.501(5) . ?
C10 C11 1.377(6) . ?
C10 C16 1.510(5) . ?
C14 C13 1.396(6) . ?
C14 C15 1.505(6) . ?
C2 C3 1.390(6) . ?
C2 C8 1.505(6) . ?
C5 C4 1.384(6) . ?
C21 C22 1.497(6) . ?
C11 C12 1.380(6) . ?
C23 C24 1.511(6) . ?
C13 C12 1.380(6) . ?
C3 C4 1.384(7) . ?
C18 C17 1.514(6) . ?
C18 C19 1.520(6) . ?
C20 C19 1.513(6) . ?
Li1 N1 2.102(7) 2_666 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 U1 O1 180.000(1) 2_666 . ?
O1 U1 N1 94.62(12) 2_666 . ?
O1 U1 N1 85.38(12) . . ?
O1 U1 N1 85.38(12) 2_666 2_666 ?
O1 U1 N1 94.62(12) . 2_666 ?
N1 U1 N1 180.0 . 2_666 ?
O1 U1 N2 84.90(11) 2_666 . ?
O1 U1 N2 95.10(11) . . ?
N1 U1 N2 97.51(11) . . ?
N1 U1 N2 82.49(11) 2_666 . ?
O1 U1 N2 95.10(11) 2_666 2_666 ?
O1 U1 N2 84.90(11) . 2_666 ?
N1 U1 N2 82.49(11) . 2_666 ?
N1 U1 N2 97.51(11) 2_666 2_666 ?
N2 U1 N2 180.000(1) . 2_666 ?
O1 U1 Li1 83.26(15) 2_666 . ?
O1 U1 Li1 96.74(15) . . ?
N1 U1 Li1 139.09(13) . . ?
N1 U1 Li1 40.91(13) 2_666 . ?
N2 U1 Li1 41.58(14) . . ?
N2 U1 Li1 138.42(14) 2_666 . ?
O1 U1 Li1 96.74(15) 2_666 2_666 ?
O1 U1 Li1 83.26(15) . 2_666 ?
N1 U1 Li1 40.91(13) . 2_666 ?
N1 U1 Li1 139.09(13) 2_666 2_666 ?
N2 U1 Li1 138.42(14) . 2_666 ?
N2 U1 Li1 41.58(14) 2_666 2_666 ?
Li1 U1 Li1 180.00(17) . 2_666 ?
C21 O3 C23 112.7(3) . . ?
C21 O3 Li1 123.3(3) . . ?
C23 O3 Li1 120.9(3) . . ?
C17 O2 C20 109.6(3) . . ?
C17 O2 Li1 132.0(3) . . ?
C20 O2 Li1 118.4(3) . . ?
C1 N1 Li1 130.6(3) . 2_666 ?
C1 N1 U1 128.2(2) . . ?
Li1 N1 U1 90.5(2) 2_666 . ?
C9 N2 Li1 128.2(3) . . ?
C9 N2 U1 132.7(2) . . ?
Li1 N2 U1 89.7(2) . . ?
N2 C9 C10 121.5(3) . . ?
N2 C9 C14 120.2(3) . . ?
C10 C9 C14 118.3(3) . . ?
N1 C1 C6 120.2(3) . . ?
N1 C1 C2 120.9(3) . . ?
C6 C1 C2 118.8(3) . . ?
C5 C6 C1 119.3(4) . . ?
C5 C6 C7 119.3(4) . . ?
C1 C6 C7 121.4(3) . . ?
C11 C10 C9 120.3(4) . . ?
C11 C10 C16 119.7(4) . . ?
C9 C10 C16 120.0(3) . . ?
C13 C14 C9 119.4(4) . . ?
C13 C14 C15 119.8(4) . . ?
C9 C14 C15 120.7(3) . . ?
C3 C2 C1 120.0(4) . . ?
C3 C2 C8 119.8(4) . . ?
C1 C2 C8 120.1(3) . . ?
C4 C5 C6 121.8(4) . . ?
O3 C21 C22 109.7(3) . . ?
C10 C11 C12 121.6(4) . . ?
O3 C23 C24 112.8(3) . . ?
C12 C13 C14 121.3(4) . . ?
C4 C3 C2 121.2(4) . . ?
C17 C18 C19 103.9(3) . . ?
C13 C12 C11 119.0(4) . . ?
C5 C4 C3 118.8(4) . . ?
O2 C20 C19 105.1(3) . . ?
O2 C17 C18 107.8(3) . . ?
C20 C19 C18 103.1(3) . . ?
O3 Li1 O2 98.0(3) . . ?
O3 Li1 N1 130.5(3) . 2_666 ?
O2 Li1 N1 105.1(3) . 2_666 ?
O3 Li1 N2 122.0(3) . . ?
O2 Li1 N2 98.2(3) . . ?
N1 Li1 N2 97.3(3) 2_666 . ?
O3 Li1 U1 153.7(3) . . ?
O2 Li1 U1 107.5(3) . . ?
N1 Li1 U1 48.60(16) 2_666 . ?
N2 Li1 U1 48.73(16) . . ?

_diffrn_measured_fraction_theta_max 0.969
_diffrn_reflns_theta_full        26.37
_diffrn_measured_fraction_theta_full 0.969
_refine_diff_density_max         2.255
_refine_diff_density_min         -1.516
_refine_diff_density_rms         0.121