 
data_nha59_sq

_publ_contact_author_name     'Fanwick, Phillip E.'
_publ_contact_author_address
;       Department of Chemistry
        Purdue University
        560 Oval Dr.
        W. Lafayette
        IN 47907-2084
        USA
;
_publ_contact_author_email      'pfanwick@purdue.edu'
_publ_contact_author_fax        '1(765)4940239'
_publ_contact_author_phone      '1(765)4944572'
 

loop_
_publ_author_name
_publ_author_address
_publ_author_footnote

        'Anderson, Nickolas'
;       Department of Chemistry
        Purdue University
        560 Oval Dr.
        W. Lafayette
        IN 47907-2084
        USA
;
;?
;

        'Bart, Suzanne C.'
;       Department of Chemistry
        Purdue University
        560 Oval Dr.
        W. Lafayette
        IN 47907-2084
        USA
;
;?
;

        'Fanwick, Phillip E.'
;       Department of Chemistry
        Purdue University
        560 Oval Dr.
        W. Lafayette
        IN 47907-2084
        USA
;
;?
;

_publ_section_references
;
Nonius(1998), Collect Users Manual, Nonius Delft, The Netherlands.

Otwinowski Z. & Minor, W. (1997). Methods Enzymol., 276, 307-327.

Prince, E. and Nicholson, W. L. (1983). Acta Cryst. A39, 407-410.

Sheldrick, G.M. (2015). Acta Cryst., A71, 3-8 

Sheldrick, G.M. (2015). Acta Cryst., C71, 3-8.

Spek A.L.(2003). J. Appl. Cryst.,36, 7-13.

Spek A.L.(2015). Acta Cryst., C71, 9-18.
;

# start Validation Reply Form
_vrf_PLAT971_nha59_sq
;
PROBLEM: Check Calcd Resid. Dens.  0.94Ang From U1              3.13 eA-3  
RESPONSE: All large Q peaks nearby uranium. Data collected on vintage 
instrument (produced 1997) with limited data processing and absorption 
correction options. 
;
# end Validation Reply Form

 
_audit_creation_method            'SHELXL-2019/3'
_shelx_SHELXL_version_number      '2019/3'
_chemical_name_systematic         ?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          
 'C68 H103 Li2 N5 O2 U [+ solvent]'
_chemical_formula_sum
 'C68 H103 Li2 N5 O2 U' 
_chemical_formula_weight          1274.46

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'
 
_space_group_crystal_system       monoclinic
_space_group_IT_number            14
_space_group_name_H-M_alt         'P 21/c'
_space_group_name_Hall            '-P 2ybc'
 
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
 
loop_
 _space_group_symop_operation_xyz
 'x, y, z'
 '-x, y+1/2, -z+1/2'
 '-x, -y, -z'
 'x, -y-1/2, z-1/2'
 
_cell_length_a                    19.1169(2)
_cell_length_b                    16.8263(2)
_cell_length_c                    23.7598(3)
_cell_angle_alpha                 90
_cell_angle_beta                  96.5600(10)
_cell_angle_gamma                 90
_cell_volume                      7592.70(15)
_cell_formula_units_Z             4
_cell_measurement_temperature     150(2)
_cell_measurement_reflns_used     59181
_cell_measurement_theta_min       1.072
_cell_measurement_theta_max       27.485
 
_exptl_crystal_description        block
_exptl_crystal_colour             brown
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     1.115          
_exptl_crystal_F_000              2640
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           0.480
_exptl_crystal_size_mid           0.420
_exptl_crystal_size_min           0.300
_exptl_absorpt_coefficient_mu     2.177
_shelx_estimated_absorpt_T_min    0.421
_shelx_estimated_absorpt_T_max    0.561
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.034 
_exptl_absorpt_correction_T_max   0.520 
_exptl_absorpt_process_details    'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_absorpt_special_details    ?
_diffrn_ambient_temperature       150(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_source                    'fine focus tube'
_diffrn_measurement_device_type   'Nonius KappaCCD'
_diffrn_measurement_method        'ω and φ'
_diffrn_detector_area_resol_mean  ?
_diffrn_reflns_number             17390
_diffrn_reflns_av_unetI/netI      0.0565
_diffrn_reflns_av_R_equivalents   0.036
_diffrn_reflns_limit_h_min        0
_diffrn_reflns_limit_h_max        26
_diffrn_reflns_limit_k_min        0
_diffrn_reflns_limit_k_max        23
_diffrn_reflns_limit_l_min        -32
_diffrn_reflns_limit_l_max        32
_diffrn_reflns_theta_min          1.072
_diffrn_reflns_theta_max          27.485
_diffrn_reflns_theta_full         25.242
_diffrn_measured_fraction_theta_max   0.998
_diffrn_measured_fraction_theta_full  0.998
_diffrn_reflns_Laue_measured_fraction_max    0.998
_diffrn_reflns_Laue_measured_fraction_full   0.998
_diffrn_reflns_point_group_measured_fraction_max   0.998
_diffrn_reflns_point_group_measured_fraction_full  0.998
_reflns_number_total              17390
_reflns_number_gt                 12434
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_max      .
_reflns_Friedel_fraction_full     .
 
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
 
_computing_data_collection        'Nonius Collect (Nonius, 1998)'
_computing_cell_refinement        'HKL3000 (Otwinowski & Minor, 1997)'
_computing_data_reduction         'HKL3000 (Otwinowski & Minor, 1997)'
_computing_structure_solution     'SHELXT (Sheldrick)'
_computing_structure_refinement 
;  
SHELXL-2019/2 (Sheldrick, 2015a, 2019), 
SHELXLE Rev1737 (Hübschle et al., 2011)
;
_computing_molecular_graphics     ?
_computing_publication_material   ?
_refine_special_details           
;
N-bound H atoms were assigned based on electron density as well 
as N-U bond lengths of the associated N atoms. N-H diatnces were 
restrained to a target value of 0.88(2) Angstrom and a mild 
anti-bumping restraint was applied.

The structure contains additional 1609 Ang3 of solvent accessible 
pores. No substantial electron density peaks were found in the 
solvent accessible pores (less than 2.2 electron per cubic Angstrom) 
and the residual electron density peaks were only partially arranged 
in an interpretable pattern (vaguely resembling pentane or ether). 
The structure factors were instead augmented via reverse Fourier 
transform methods using the SQUEEZE routine (P. van der Sluis & A.L. 
Spek (1990). Acta Cryst. A46, 194-201) as implemented in the program 
Platon. The resultant FAB file containing the structure factor 
contribution from the electron content of the pore space was used in 
together with the original hkl file in the further refinement. (The 
FAB file with details of the Squeeze results is appended to this cif 
file). The Squeeze procedure corrected for 364 electrons within the 
solvent accessible pores.
;
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0351P)²+24.7491P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      dual
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    mixed
_refine_ls_hydrogen_treatment     mixed
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        .
_refine_ls_number_reflns          17390
_refine_ls_number_parameters      729
_refine_ls_number_restraints      5
_refine_ls_R_factor_all           0.0802
_refine_ls_R_factor_gt            0.0496
_refine_ls_wR_factor_ref          0.1209
_refine_ls_wR_factor_gt           0.1092
_refine_ls_goodness_of_fit_ref    1.110
_refine_ls_restrained_S_all       1.109
_refine_ls_shift/su_max           0.002
_refine_ls_shift/su_mean          0.000
 
loop_
 _atom_site_label
 _atom_site_type_symbol
 _atom_site_fract_x
 _atom_site_fract_y
 _atom_site_fract_z
 _atom_site_U_iso_or_equiv
 _atom_site_adp_type
 _atom_site_occupancy
 _atom_site_site_symmetry_order  
 _atom_site_calc_flag
 _atom_site_refinement_flags_posn
 _atom_site_refinement_flags_adp
 _atom_site_refinement_flags_occupancy
 _atom_site_disorder_assembly
 _atom_site_disorder_group
U1 U 0.74772(2) 0.66423(2) 0.74033(2) 0.02899(6) Uani 1 1 d . . . . .
O1 O 0.5709(2) 0.8341(3) 0.63272(18) 0.0614(12) Uani 1 1 d . . . . .
O2 O 0.9975(2) 0.6317(3) 0.7478(2) 0.0594(12) Uani 1 1 d . . . . .
N1 N 0.8268(2) 0.6759(3) 0.80294(18) 0.0394(11) Uani 1 1 d . . . . .
N2 N 0.6621(2) 0.6558(2) 0.68289(17) 0.0331(9) Uani 1 1 d . . . . .
N3 N 0.8210(3) 0.6280(3) 0.6859(2) 0.0525(13) Uani 1 1 d . . . . .
N4 N 0.6998(2) 0.5595(2) 0.78326(18) 0.0336(10) Uani 1 1 d D . . . .
H4N H 0.686(2) 0.5301(13) 0.7529(14) 0.050 Uiso 1 1 d D U . . .
N5 N 0.7340(3) 0.8041(3) 0.7159(3) 0.0573(14) Uani 1 1 d D . . . .
H5N H 0.758(3) 0.7858(13) 0.690(2) 0.086 Uiso 1 1 d D U . . .
C1 C 0.5186(5) 0.8152(6) 0.5866(4) 0.103(3) Uani 1 1 d . . . . .
H1A H 0.473335 0.801743 0.600868 0.123 Uiso 1 1 calc R U . . .
H1B H 0.533805 0.769324 0.564928 0.123 Uiso 1 1 calc R U . . .
C2 C 0.5109(6) 0.8866(8) 0.5508(4) 0.122(4) Uani 1 1 d . . . . .
H2A H 0.462318 0.891151 0.531610 0.146 Uiso 1 1 calc R U . . .
H2B H 0.544178 0.885361 0.521808 0.146 Uiso 1 1 calc R U . . .
C3 C 0.5276(5) 0.9540(6) 0.5913(4) 0.108(3) Uani 1 1 d . . . . .
H3A H 0.484635 0.985084 0.596027 0.129 Uiso 1 1 calc R U . . .
H3B H 0.563026 0.989904 0.577649 0.129 Uiso 1 1 calc R U . . .
C4 C 0.5561(4) 0.9155(4) 0.6462(3) 0.071(2) Uani 1 1 d . . . . .
H4A H 0.599616 0.942651 0.662764 0.085 Uiso 1 1 calc R U . . .
H4B H 0.521060 0.917841 0.673788 0.085 Uiso 1 1 calc R U . . .
C5 C 1.0507(3) 0.6734(6) 0.7839(4) 0.084(3) Uani 1 1 d . . . . .
H5A H 1.060590 0.645867 0.820770 0.100 Uiso 1 1 calc R U . . .
H5B H 1.035177 0.728297 0.790808 0.100 Uiso 1 1 calc R U . . .
C6 C 1.1126(4) 0.6742(6) 0.7544(6) 0.120(4) Uani 1 1 d . . . . .
H6A H 1.118246 0.726908 0.736984 0.144 Uiso 1 1 calc R U . . .
H6B H 1.155109 0.662984 0.781082 0.144 Uiso 1 1 calc R U . . .
C7 C 1.1034(4) 0.6137(7) 0.7112(4) 0.104(3) Uani 1 1 d . . . . .
H7A H 1.139479 0.571669 0.718971 0.125 Uiso 1 1 calc R U . . .
H7B H 1.108137 0.637007 0.673598 0.125 Uiso 1 1 calc R U . . .
C8 C 1.0335(4) 0.5804(5) 0.7121(4) 0.074(2) Uani 1 1 d . . . . .
H8A H 1.008195 0.578789 0.673356 0.089 Uiso 1 1 calc R U . . .
H8B H 1.036450 0.525706 0.727525 0.089 Uiso 1 1 calc R U . . .
C10 C 0.8817(3) 0.6853(4) 0.8471(2) 0.0450(14) Uani 1 1 d . . . . .
C11 C 0.9076(3) 0.7625(4) 0.8621(3) 0.0533(16) Uani 1 1 d . . . . .
C12 C 0.9647(4) 0.7707(5) 0.9033(3) 0.076(2) Uani 1 1 d . . . . .
H12 H 0.982338 0.822223 0.913274 0.091 Uiso 1 1 calc R U . . .
C13 C 0.9961(5) 0.7049(6) 0.9298(4) 0.093(3) Uani 1 1 d . . . . .
H13 H 1.036324 0.711327 0.956872 0.112 Uiso 1 1 calc R U . . .
C14 C 0.9700(4) 0.6302(5) 0.9176(3) 0.078(2) Uani 1 1 d . . . . .
H14 H 0.991871 0.585588 0.936769 0.094 Uiso 1 1 calc R U . . .
C15 C 0.9115(3) 0.6186(4) 0.8771(3) 0.0559(16) Uani 1 1 d . . . . .
C16 C 0.8828(4) 0.5361(5) 0.8665(3) 0.072(2) Uani 1 1 d . . . . .
H16 H 0.836678 0.541702 0.842353 0.086 Uiso 1 1 calc R U . . .
C17 C 0.8738(3) 0.8349(4) 0.8323(3) 0.0556(16) Uani 1 1 d . . . . .
H17 H 0.823277 0.821453 0.820714 0.067 Uiso 1 1 calc R U . . .
C20 C 0.6098(3) 0.6070(3) 0.6525(2) 0.0347(11) Uani 1 1 d . . . . .
C21 C 0.6204(3) 0.5784(4) 0.5979(2) 0.0420(13) Uani 1 1 d . . . . .
C22 C 0.5702(4) 0.5270(4) 0.5706(3) 0.0627(19) Uani 1 1 d . . . . .
H22 H 0.577505 0.505963 0.534590 0.075 Uiso 1 1 calc R U . . .
C23 C 0.5113(4) 0.5063(5) 0.5940(3) 0.069(2) Uani 1 1 d . . . . .
H23 H 0.478535 0.470183 0.574878 0.083 Uiso 1 1 calc R U . . .
C24 C 0.4989(3) 0.5378(4) 0.6462(3) 0.0606(18) Uani 1 1 d . . . . .
H24 H 0.456738 0.524672 0.661718 0.073 Uiso 1 1 calc R U . . .
C25 C 0.5477(3) 0.5886(3) 0.6757(2) 0.0397(13) Uani 1 1 d . . . . .
C26 C 0.5290(3) 0.6248(4) 0.7309(2) 0.0432(13) Uani 1 1 d . . . . .
H26 H 0.571794 0.652603 0.749475 0.052 Uiso 1 1 calc R U . . .
C27 C 0.6833(4) 0.6054(4) 0.5700(3) 0.0563(17) Uani 1 1 d . . . . .
H27 H 0.724191 0.609897 0.600116 0.068 Uiso 1 1 calc R U . . .
C30 C 0.8565(3) 0.5947(4) 0.6434(2) 0.0467(14) Uani 1 1 d . . . . .
C31 C 0.8614(3) 0.5103(4) 0.6397(3) 0.0490(15) Uani 1 1 d . . . . .
C32 C 0.8984(4) 0.4771(4) 0.5981(3) 0.0626(19) Uani 1 1 d . . . . .
H32 H 0.901762 0.420879 0.595740 0.075 Uiso 1 1 calc R U . . .
C33 C 0.9299(4) 0.5229(5) 0.5607(3) 0.077(2) Uani 1 1 d . . . . .
H33 H 0.955463 0.498717 0.533232 0.092 Uiso 1 1 calc R U . . .
C34 C 0.9241(4) 0.6043(5) 0.5631(3) 0.068(2) Uani 1 1 d . . . . .
H34 H 0.944806 0.636005 0.536356 0.081 Uiso 1 1 calc R U . . .
C35 C 0.8886(3) 0.6413(4) 0.6039(3) 0.0551(16) Uani 1 1 d . . . . .
C36 C 0.8847(4) 0.7304(4) 0.6058(3) 0.0666(19) Uani 1 1 d . . . . .
H36 H 0.846320 0.745869 0.629003 0.080 Uiso 1 1 calc R U . . .
C37 C 0.8261(3) 0.4559(4) 0.6782(3) 0.0568(17) Uani 1 1 d . . . . .
H37 H 0.813660 0.487345 0.711300 0.068 Uiso 1 1 calc R U . . .
C40 C 0.6916(3) 0.5147(3) 0.8328(2) 0.0390(12) Uani 1 1 d . . . . .
C41 C 0.6898(3) 0.4317(4) 0.8324(3) 0.0477(15) Uani 1 1 d . . . . .
C42 C 0.6824(4) 0.3904(4) 0.8829(3) 0.0639(19) Uani 1 1 d . . . . .
H42 H 0.681156 0.333960 0.882624 0.077 Uiso 1 1 calc R U . . .
C43 C 0.6770(4) 0.4307(5) 0.9326(3) 0.074(2) Uani 1 1 d . . . . .
H43 H 0.673380 0.402369 0.966744 0.088 Uiso 1 1 calc R U . . .
C44 C 0.6769(4) 0.5116(5) 0.9325(3) 0.0640(19) Uani 1 1 d . . . . .
H44 H 0.672395 0.538795 0.966922 0.077 Uiso 1 1 calc R U . . .
C45 C 0.6830(3) 0.5566(4) 0.8836(2) 0.0444(14) Uani 1 1 d . . . . .
C46 C 0.6786(3) 0.6457(4) 0.8867(2) 0.0467(15) Uani 1 1 d . . . . .
H46 H 0.680820 0.667284 0.847722 0.056 Uiso 1 1 calc R U . . .
C47 C 0.6950(3) 0.3845(4) 0.7781(3) 0.0543(16) Uani 1 1 d . . . . .
H47 H 0.727438 0.414480 0.755625 0.065 Uiso 1 1 calc R U . . .
C50 C 0.7301(3) 0.8852(3) 0.7260(3) 0.0463(15) Uani 1 1 d . . . . .
C51 C 0.6974(3) 0.9114(3) 0.7739(3) 0.0445(14) Uani 1 1 d . . . . .
C52 C 0.6891(3) 0.9919(4) 0.7825(3) 0.0478(14) Uani 1 1 d . . . . .
H52 H 0.667509 1.009403 0.814438 0.057 Uiso 1 1 calc R U . . .
C53 C 0.7113(4) 1.0474(4) 0.7458(3) 0.0607(18) Uani 1 1 d . . . . .
H53 H 0.703493 1.102386 0.751654 0.073 Uiso 1 1 calc R U . . .
C54 C 0.7451(4) 1.0230(4) 0.7004(3) 0.0651(19) Uani 1 1 d . . . . .
H54 H 0.761609 1.061455 0.675796 0.078 Uiso 1 1 calc R U . . .
C55 C 0.7548(3) 0.9439(4) 0.6907(3) 0.0539(16) Uani 1 1 d . . . . .
C56 C 0.7909(4) 0.9230(5) 0.6378(3) 0.0657(19) Uani 1 1 d . . . . .
H56 H 0.810069 0.867894 0.643560 0.079 Uiso 1 1 calc R U . . .
C57 C 0.6680(3) 0.8525(4) 0.8131(3) 0.0515(15) Uani 1 1 d . . . . .
H57 H 0.696976 0.802970 0.813547 0.062 Uiso 1 1 calc R U . . .
C161 C 0.9286(6) 0.4836(6) 0.8346(5) 0.127(4) Uani 1 1 d . . . . .
H16A H 0.928564 0.503580 0.795836 0.191 Uiso 1 1 calc R U . . .
H16B H 0.910185 0.429211 0.833479 0.191 Uiso 1 1 calc R U . . .
H16C H 0.976828 0.483909 0.853698 0.191 Uiso 1 1 calc R U . . .
C162 C 0.8675(4) 0.4941(6) 0.9218(4) 0.099(3) Uani 1 1 d . . . . .
H16D H 0.911797 0.486053 0.946246 0.148 Uiso 1 1 calc R U . . .
H16E H 0.845288 0.442580 0.912517 0.148 Uiso 1 1 calc R U . . .
H16F H 0.835868 0.527178 0.941496 0.148 Uiso 1 1 calc R U . . .
C171 C 0.8750(4) 0.9082(5) 0.8712(4) 0.088(3) Uani 1 1 d . . . . .
H17A H 0.922741 0.930359 0.876680 0.132 Uiso 1 1 calc R U . . .
H17B H 0.860801 0.892601 0.908005 0.132 Uiso 1 1 calc R U . . .
H17C H 0.842306 0.948384 0.853793 0.132 Uiso 1 1 calc R U . . .
C172 C 0.9069(4) 0.8526(4) 0.7786(3) 0.068(2) Uani 1 1 d . . . . .
H17D H 0.956646 0.866188 0.788290 0.102 Uiso 1 1 calc R U . . .
H17E H 0.882310 0.897385 0.758697 0.102 Uiso 1 1 calc R U . . .
H17F H 0.903040 0.805677 0.753964 0.102 Uiso 1 1 calc R U . . .
C261 C 0.4707(3) 0.6871(4) 0.7186(3) 0.0607(18) Uani 1 1 d . . . . .
H26A H 0.487137 0.729468 0.695009 0.091 Uiso 1 1 calc R U . . .
H26B H 0.458949 0.709710 0.754331 0.091 Uiso 1 1 calc R U . . .
H26C H 0.428834 0.661952 0.698522 0.091 Uiso 1 1 calc R U . . .
C262 C 0.5064(3) 0.5637(4) 0.7728(3) 0.0536(16) Uani 1 1 d . . . . .
H26D H 0.466574 0.532842 0.754630 0.080 Uiso 1 1 calc R U . . .
H26E H 0.492307 0.591101 0.806100 0.080 Uiso 1 1 calc R U . . .
H26F H 0.545842 0.527919 0.784498 0.080 Uiso 1 1 calc R U . . .
C271 C 0.6695(6) 0.6875(5) 0.5440(3) 0.096(3) Uani 1 1 d . . . . .
H27A H 0.630192 0.684512 0.513830 0.144 Uiso 1 1 calc R U . . .
H27B H 0.711791 0.706126 0.528277 0.144 Uiso 1 1 calc R U . . .
H27C H 0.657778 0.724595 0.573328 0.144 Uiso 1 1 calc R U . . .
C272 C 0.7047(4) 0.5487(5) 0.5239(3) 0.074(2) Uani 1 1 d . . . . .
H27D H 0.709055 0.494490 0.539066 0.110 Uiso 1 1 calc R U . . .
H27E H 0.749971 0.565630 0.512349 0.110 Uiso 1 1 calc R U . . .
H27F H 0.668681 0.549847 0.491102 0.110 Uiso 1 1 calc R U . . .
C361 C 0.9545(5) 0.7657(5) 0.6337(4) 0.093(3) Uani 1 1 d . . . . .
H36A H 0.964958 0.744239 0.672093 0.139 Uiso 1 1 calc R U . . .
H36B H 0.950454 0.823641 0.635542 0.139 Uiso 1 1 calc R U . . .
H36C H 0.992558 0.751527 0.611200 0.139 Uiso 1 1 calc R U . . .
C362 C 0.8689(7) 0.7674(6) 0.5470(4) 0.127(4) Uani 1 1 d . . . . .
H36D H 0.910080 0.761534 0.526267 0.190 Uiso 1 1 calc R U . . .
H36E H 0.858048 0.823907 0.550738 0.190 Uiso 1 1 calc R U . . .
H36F H 0.828473 0.740324 0.526247 0.190 Uiso 1 1 calc R U . . .
C371 C 0.8720(5) 0.3857(6) 0.7002(4) 0.101(3) Uani 1 1 d . . . . .
H37A H 0.877229 0.348894 0.668994 0.151 Uiso 1 1 calc R U . . .
H37B H 0.849850 0.358127 0.729841 0.151 Uiso 1 1 calc R U . . .
H37C H 0.918543 0.405189 0.715881 0.151 Uiso 1 1 calc R U . . .
C372 C 0.7577(4) 0.4215(5) 0.6463(3) 0.079(2) Uani 1 1 d . . . . .
H37D H 0.722436 0.463812 0.639990 0.118 Uiso 1 1 calc R U . . .
H37E H 0.739695 0.379199 0.669066 0.118 Uiso 1 1 calc R U . . .
H37F H 0.767675 0.399874 0.609815 0.118 Uiso 1 1 calc R U . . .
C461 C 0.7390(3) 0.6816(4) 0.9255(3) 0.0564(17) Uani 1 1 d . . . . .
H46A H 0.737392 0.662199 0.964183 0.085 Uiso 1 1 calc R U . . .
H46B H 0.734786 0.739697 0.924954 0.085 Uiso 1 1 calc R U . . .
H46C H 0.783813 0.666232 0.912310 0.085 Uiso 1 1 calc R U . . .
C462 C 0.6075(4) 0.6703(5) 0.9056(3) 0.0655(19) Uani 1 1 d . . . . .
H46D H 0.569219 0.650085 0.878478 0.098 Uiso 1 1 calc R U . . .
H46E H 0.604808 0.728383 0.907300 0.098 Uiso 1 1 calc R U . . .
H46F H 0.603244 0.648065 0.943209 0.098 Uiso 1 1 calc R U . . .
C471 C 0.7249(4) 0.3010(4) 0.7868(4) 0.081(2) Uani 1 1 d . . . . .
H47A H 0.771505 0.303777 0.808740 0.122 Uiso 1 1 calc R U . . .
H47B H 0.729096 0.276570 0.749921 0.122 Uiso 1 1 calc R U . . .
H47C H 0.693432 0.268966 0.807429 0.122 Uiso 1 1 calc R U . . .
C472 C 0.6232(4) 0.3802(4) 0.7419(3) 0.0618(18) Uani 1 1 d . . . . .
H47D H 0.588795 0.355077 0.763742 0.093 Uiso 1 1 calc R U . . .
H47E H 0.627603 0.348865 0.707685 0.093 Uiso 1 1 calc R U . . .
H47F H 0.607394 0.434074 0.731014 0.093 Uiso 1 1 calc R U . . .
C561 C 0.7362(5) 0.9205(6) 0.5857(3) 0.089(3) Uani 1 1 d . . . . .
H56A H 0.702546 0.877619 0.589906 0.133 Uiso 1 1 calc R U . . .
H56B H 0.759883 0.910900 0.551809 0.133 Uiso 1 1 calc R U . . .
H56C H 0.711220 0.971387 0.581814 0.133 Uiso 1 1 calc R U . . .
C562 C 0.8535(5) 0.9774(6) 0.6283(4) 0.094(3) Uani 1 1 d . . . . .
H56D H 0.836261 1.031366 0.619689 0.140 Uiso 1 1 calc R U . . .
H56E H 0.876673 0.957066 0.596485 0.140 Uiso 1 1 calc R U . . .
H56F H 0.887186 0.978172 0.662587 0.140 Uiso 1 1 calc R U . . .
C571 C 0.5917(3) 0.8307(4) 0.7920(3) 0.0592(17) Uani 1 1 d . . . . .
H57A H 0.561607 0.877539 0.793901 0.089 Uiso 1 1 calc R U . . .
H57B H 0.575650 0.788445 0.815920 0.089 Uiso 1 1 calc R U . . .
H57C H 0.588915 0.812004 0.752751 0.089 Uiso 1 1 calc R U . . .
C572 C 0.6716(4) 0.8838(4) 0.8745(3) 0.0630(18) Uani 1 1 d . . . . .
H57D H 0.719886 0.900579 0.887476 0.095 Uiso 1 1 calc R U . . .
H57E H 0.657600 0.841496 0.899279 0.095 Uiso 1 1 calc R U . . .
H57F H 0.639699 0.929167 0.875792 0.095 Uiso 1 1 calc R U . . .
Li1 Li 0.6437(6) 0.7717(6) 0.6703(4) 0.052(3) Uani 1 1 d . . . . .
Li2 Li 0.8994(5) 0.6396(7) 0.7492(5) 0.056(3) Uani 1 1 d . . . . .
 
 
_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 N1 2.006(4) . ?
U1 N2 2.013(4) . ?
U1 N3 2.102(5) . ?
U1 N4 2.280(4) . ?
U1 N5 2.432(6) . ?
U1 Li2 2.912(10) . ?
U1 Li1 3.039(10) . ?
U1 H4N 2.58(4) . ?
U1 H5N 2.38(3) . ?
O1 C1 1.432(9) . ?
O1 C4 1.441(8) . ?
O1 Li1 1.885(11) . ?
O2 C5 1.436(8) . ?
O2 C8 1.440(8) . ?
O2 Li2 1.884(11) . ?
N1 C10 1.406(7) . ?
N1 Li2 2.083(11) . ?
N2 C20 1.425(6) . ?
N2 Li1 1.998(12) . ?
N3 C30 1.397(7) . ?
N3 Li2 2.007(12) . ?
N4 C40 1.420(6) . ?
N4 H4N 0.890(19) . ?
N5 C50 1.389(7) . ?
N5 Li1 2.005(12) . ?
N5 H5N 0.86(2) . ?
C1 C2 1.470(13) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.499(14) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.502(11) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.443(11) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 C7 1.442(13) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.451(11) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C10 C15 1.413(9) . ?
C10 C11 1.421(9) . ?
C10 Li2 2.510(12) . ?
C11 C12 1.387(9) . ?
C11 C17 1.516(9) . ?
C12 C13 1.378(11) . ?
C12 H12 0.9500 . ?
C13 C14 1.372(12) . ?
C13 H13 0.9500 . ?
C14 C15 1.403(10) . ?
C14 H14 0.9500 . ?
C15 C16 1.502(10) . ?
C16 C161 1.509(12) . ?
C16 C162 1.548(10) . ?
C16 H16 1.0000 . ?
C17 C172 1.518(10) . ?
C17 C171 1.541(9) . ?
C17 H17 1.0000 . ?
C20 C25 1.400(7) . ?
C20 C21 1.419(7) . ?
C21 C22 1.396(8) . ?
C21 C27 1.509(8) . ?
C22 C23 1.359(9) . ?
C22 H22 0.9500 . ?
C23 C24 1.393(9) . ?
C23 H23 0.9500 . ?
C24 C25 1.394(8) . ?
C24 H24 0.9500 . ?
C25 C26 1.525(7) . ?
C26 C262 1.527(8) . ?
C26 C261 1.533(8) . ?
C26 H26 1.0000 . ?
C27 C271 1.523(10) . ?
C27 C272 1.543(9) . ?
C27 H27 1.0000 . ?
C30 C35 1.416(9) . ?
C30 C31 1.426(9) . ?
C30 Li2 2.662(12) . ?
C31 C32 1.396(8) . ?
C31 C37 1.507(9) . ?
C32 C33 1.368(10) . ?
C32 H32 0.9500 . ?
C33 C34 1.377(10) . ?
C33 H33 0.9500 . ?
C34 C35 1.392(9) . ?
C34 H34 0.9500 . ?
C35 C36 1.503(9) . ?
C36 C362 1.528(11) . ?
C36 C361 1.539(11) . ?
C36 H36 1.0000 . ?
C37 C371 1.527(10) . ?
C37 C372 1.545(9) . ?
C37 H37 1.0000 . ?
C40 C41 1.397(8) . ?
C40 C45 1.424(8) . ?
C41 C42 1.406(9) . ?
C41 C47 1.529(9) . ?
C42 C43 1.377(10) . ?
C42 H42 0.9500 . ?
C43 C44 1.361(10) . ?
C43 H43 0.9500 . ?
C44 C45 1.402(8) . ?
C44 H44 0.9500 . ?
C45 C46 1.505(8) . ?
C46 C461 1.519(8) . ?
C46 C462 1.535(9) . ?
C46 H46 1.0000 . ?
C47 C471 1.521(9) . ?
C47 C472 1.537(9) . ?
C47 H47 1.0000 . ?
C50 C55 1.412(9) . ?
C50 C51 1.429(8) . ?
C50 Li1 2.762(12) . ?
C51 C52 1.383(8) . ?
C51 C57 1.511(9) . ?
C52 C53 1.379(9) . ?
C52 H52 0.9500 . ?
C53 C54 1.379(9) . ?
C53 H53 0.9500 . ?
C54 C55 1.368(9) . ?
C54 H54 0.9500 . ?
C55 C56 1.542(9) . ?
C56 C561 1.528(10) . ?
C56 C562 1.543(10) . ?
C56 H56 1.0000 . ?
C57 C571 1.533(8) . ?
C57 C572 1.546(9) . ?
C57 H57 1.0000 . ?
C161 H16A 0.9800 . ?
C161 H16B 0.9800 . ?
C161 H16C 0.9800 . ?
C162 H16D 0.9800 . ?
C162 H16E 0.9800 . ?
C162 H16F 0.9800 . ?
C171 H17A 0.9800 . ?
C171 H17B 0.9800 . ?
C171 H17C 0.9800 . ?
C172 H17D 0.9800 . ?
C172 H17E 0.9800 . ?
C172 H17F 0.9800 . ?
C261 H26A 0.9800 . ?
C261 H26B 0.9800 . ?
C261 H26C 0.9800 . ?
C262 H26D 0.9800 . ?
C262 H26E 0.9800 . ?
C262 H26F 0.9800 . ?
C271 H27A 0.9800 . ?
C271 H27B 0.9800 . ?
C271 H27C 0.9800 . ?
C272 H27D 0.9800 . ?
C272 H27E 0.9800 . ?
C272 H27F 0.9800 . ?
C361 H36A 0.9800 . ?
C361 H36B 0.9800 . ?
C361 H36C 0.9800 . ?
C362 H36D 0.9800 . ?
C362 H36E 0.9800 . ?
C362 H36F 0.9800 . ?
C371 H37A 0.9800 . ?
C371 H37B 0.9800 . ?
C371 H37C 0.9800 . ?
C372 H37D 0.9800 . ?
C372 H37E 0.9800 . ?
C372 H37F 0.9800 . ?
C461 H46A 0.9800 . ?
C461 H46B 0.9800 . ?
C461 H46C 0.9800 . ?
C462 H46D 0.9800 . ?
C462 H46E 0.9800 . ?
C462 H46F 0.9800 . ?
C471 H47A 0.9800 . ?
C471 H47B 0.9800 . ?
C471 H47C 0.9800 . ?
C472 H47D 0.9800 . ?
C472 H47E 0.9800 . ?
C472 H47F 0.9800 . ?
C561 H56A 0.9800 . ?
C561 H56B 0.9800 . ?
C561 H56C 0.9800 . ?
C562 H56D 0.9800 . ?
C562 H56E 0.9800 . ?
C562 H56F 0.9800 . ?
C571 H57A 0.9800 . ?
C571 H57B 0.9800 . ?
C571 H57C 0.9800 . ?
C572 H57D 0.9800 . ?
C572 H57E 0.9800 . ?
C572 H57F 0.9800 . ?
Li1 H5N 2.20(7) . ?
 
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_atom_site_label_2
 _geom_angle_atom_site_label_3
 _geom_angle
 _geom_angle_site_symmetry_1
 _geom_angle_site_symmetry_3
 _geom_angle_publ_flag
N1 U1 N2 174.48(17) . . ?
N1 U1 N3 89.20(19) . . ?
N2 U1 N3 96.32(18) . . ?
N1 U1 N4 92.93(17) . . ?
N2 U1 N4 84.94(16) . . ?
N3 U1 N4 112.38(18) . . ?
N1 U1 N5 97.70(19) . . ?
N2 U1 N5 81.30(17) . . ?
N3 U1 N5 101.2(2) . . ?
N4 U1 N5 144.83(17) . . ?
N1 U1 Li2 45.6(2) . . ?
N2 U1 Li2 139.9(2) . . ?
N3 U1 Li2 43.6(3) . . ?
N4 U1 Li2 107.7(3) . . ?
N5 U1 Li2 103.6(3) . . ?
N1 U1 Li1 137.6(2) . . ?
N2 U1 Li1 40.6(2) . . ?
N3 U1 Li1 106.0(2) . . ?
N4 U1 Li1 115.7(2) . . ?
N5 U1 Li1 41.2(2) . . ?
Li2 U1 Li1 135.1(3) . . ?
N1 U1 H4N 108.4(5) . . ?
N2 U1 H4N 70.7(5) . . ?
N3 U1 H4N 99.4(9) . . ?
N4 U1 H4N 19.9(7) . . ?
N5 U1 H4N 146.7(7) . . ?
Li2 U1 H4N 109.4(8) . . ?
Li1 U1 H4N 107.7(6) . . ?
N1 U1 H5N 100.8(18) . . ?
N2 U1 H5N 80.2(18) . . ?
N3 U1 H5N 81.0(6) . . ?
N4 U1 H5N 161.1(15) . . ?
N5 U1 H5N 20.5(5) . . ?
Li2 U1 H5N 91.2(15) . . ?
Li1 U1 H5N 45.8(17) . . ?
H4N U1 H5N 150.8(19) . . ?
C1 O1 C4 104.2(6) . . ?
C1 O1 Li1 130.6(6) . . ?
C4 O1 Li1 125.2(5) . . ?
C5 O2 C8 106.9(5) . . ?
C5 O2 Li2 126.5(5) . . ?
C8 O2 Li2 126.6(5) . . ?
C10 N1 U1 179.1(4) . . ?
C10 N1 Li2 89.9(4) . . ?
U1 N1 Li2 90.8(3) . . ?
C20 N2 Li1 112.7(4) . . ?
C20 N2 U1 148.6(3) . . ?
Li1 N2 U1 98.5(3) . . ?
C30 N3 Li2 101.4(5) . . ?
C30 N3 U1 166.8(5) . . ?
Li2 N3 U1 90.2(3) . . ?
C40 N4 U1 150.3(4) . . ?
C40 N4 H4N 109(3) . . ?
U1 N4 H4N 100(3) . . ?
C50 N5 Li1 107.6(5) . . ?
C50 N5 U1 156.3(5) . . ?
Li1 N5 U1 85.9(4) . . ?
C50 N5 H5N 121.3(14) . . ?
Li1 N5 H5N 91(5) . . ?
U1 N5 H5N 76.7(19) . . ?
O1 C1 C2 106.0(8) . . ?
O1 C1 H1A 110.5 . . ?
C2 C1 H1A 110.5 . . ?
O1 C1 H1B 110.5 . . ?
C2 C1 H1B 110.5 . . ?
H1A C1 H1B 108.7 . . ?
C1 C2 C3 104.3(7) . . ?
C1 C2 H2A 110.9 . . ?
C3 C2 H2A 110.9 . . ?
C1 C2 H2B 110.9 . . ?
C3 C2 H2B 110.9 . . ?
H2A C2 H2B 108.9 . . ?
C2 C3 C4 105.1(8) . . ?
C2 C3 H3A 110.7 . . ?
C4 C3 H3A 110.7 . . ?
C2 C3 H3B 110.7 . . ?
C4 C3 H3B 110.7 . . ?
H3A C3 H3B 108.8 . . ?
O1 C4 C3 106.1(7) . . ?
O1 C4 H4A 110.5 . . ?
C3 C4 H4A 110.5 . . ?
O1 C4 H4B 110.5 . . ?
C3 C4 H4B 110.5 . . ?
H4A C4 H4B 108.7 . . ?
O2 C5 C6 106.2(7) . . ?
O2 C5 H5A 110.5 . . ?
C6 C5 H5A 110.5 . . ?
O2 C5 H5B 110.5 . . ?
C6 C5 H5B 110.5 . . ?
H5A C5 H5B 108.7 . . ?
C7 C6 C5 107.4(7) . . ?
C7 C6 H6A 110.2 . . ?
C5 C6 H6A 110.2 . . ?
C7 C6 H6B 110.2 . . ?
C5 C6 H6B 110.2 . . ?
H6A C6 H6B 108.5 . . ?
C6 C7 C8 107.4(7) . . ?
C6 C7 H7A 110.2 . . ?
C8 C7 H7A 110.2 . . ?
C6 C7 H7B 110.2 . . ?
C8 C7 H7B 110.2 . . ?
H7A C7 H7B 108.5 . . ?
O2 C8 C7 106.3(7) . . ?
O2 C8 H8A 110.5 . . ?
C7 C8 H8A 110.5 . . ?
O2 C8 H8B 110.5 . . ?
C7 C8 H8B 110.5 . . ?
H8A C8 H8B 108.7 . . ?
N1 C10 C15 120.7(6) . . ?
N1 C10 C11 119.9(5) . . ?
C15 C10 C11 119.4(6) . . ?
N1 C10 Li2 56.1(4) . . ?
C15 C10 Li2 97.7(5) . . ?
C11 C10 Li2 115.6(5) . . ?
C12 C11 C10 119.5(7) . . ?
C12 C11 C17 120.6(6) . . ?
C10 C11 C17 120.0(5) . . ?
C13 C12 C11 120.6(8) . . ?
C13 C12 H12 119.7 . . ?
C11 C12 H12 119.7 . . ?
C14 C13 C12 120.7(7) . . ?
C14 C13 H13 119.7 . . ?
C12 C13 H13 119.7 . . ?
C13 C14 C15 121.0(7) . . ?
C13 C14 H14 119.5 . . ?
C15 C14 H14 119.5 . . ?
C14 C15 C10 118.6(7) . . ?
C14 C15 C16 119.3(7) . . ?
C10 C15 C16 122.1(6) . . ?
C15 C16 C161 113.8(7) . . ?
C15 C16 C162 112.4(7) . . ?
C161 C16 C162 109.6(7) . . ?
C15 C16 H16 106.9 . . ?
C161 C16 H16 106.9 . . ?
C162 C16 H16 106.9 . . ?
C11 C17 C172 110.8(5) . . ?
C11 C17 C171 112.8(6) . . ?
C172 C17 C171 111.6(6) . . ?
C11 C17 H17 107.1 . . ?
C172 C17 H17 107.1 . . ?
C171 C17 H17 107.1 . . ?
C25 C20 C21 120.1(5) . . ?
C25 C20 N2 120.4(5) . . ?
C21 C20 N2 119.6(5) . . ?
C22 C21 C20 118.3(5) . . ?
C22 C21 C27 121.4(5) . . ?
C20 C21 C27 120.3(5) . . ?
C23 C22 C21 121.7(6) . . ?
C23 C22 H22 119.1 . . ?
C21 C22 H22 119.1 . . ?
C22 C23 C24 120.0(6) . . ?
C22 C23 H23 120.0 . . ?
C24 C23 H23 120.0 . . ?
C23 C24 C25 120.6(6) . . ?
C23 C24 H24 119.7 . . ?
C25 C24 H24 119.7 . . ?
C24 C25 C20 119.1(5) . . ?
C24 C25 C26 118.0(5) . . ?
C20 C25 C26 122.9(5) . . ?
C25 C26 C262 113.7(5) . . ?
C25 C26 C261 110.2(5) . . ?
C262 C26 C261 109.4(5) . . ?
C25 C26 H26 107.8 . . ?
C262 C26 H26 107.8 . . ?
C261 C26 H26 107.8 . . ?
C21 C27 C271 109.9(6) . . ?
C21 C27 C272 114.6(6) . . ?
C271 C27 C272 108.7(6) . . ?
C21 C27 H27 107.8 . . ?
C271 C27 H27 107.8 . . ?
C272 C27 H27 107.8 . . ?
N3 C30 C35 122.7(6) . . ?
N3 C30 C31 119.0(6) . . ?
C35 C30 C31 118.3(5) . . ?
N3 C30 Li2 47.6(4) . . ?
C35 C30 Li2 111.0(5) . . ?
C31 C30 Li2 109.0(5) . . ?
C32 C31 C30 119.0(6) . . ?
C32 C31 C37 119.0(6) . . ?
C30 C31 C37 122.0(5) . . ?
C33 C32 C31 122.1(7) . . ?
C33 C32 H32 119.0 . . ?
C31 C32 H32 119.0 . . ?
C32 C33 C34 119.4(6) . . ?
C32 C33 H33 120.3 . . ?
C34 C33 H33 120.3 . . ?
C33 C34 C35 121.5(7) . . ?
C33 C34 H34 119.3 . . ?
C35 C34 H34 119.3 . . ?
C34 C35 C30 119.8(6) . . ?
C34 C35 C36 119.8(6) . . ?
C30 C35 C36 120.4(6) . . ?
C35 C36 C362 112.5(7) . . ?
C35 C36 C361 110.7(6) . . ?
C362 C36 C361 107.9(8) . . ?
C35 C36 H36 108.5 . . ?
C362 C36 H36 108.5 . . ?
C361 C36 H36 108.5 . . ?
C31 C37 C371 113.5(6) . . ?
C31 C37 C372 110.0(6) . . ?
C371 C37 C372 107.5(7) . . ?
C31 C37 H37 108.6 . . ?
C371 C37 H37 108.6 . . ?
C372 C37 H37 108.6 . . ?
C41 C40 N4 122.0(5) . . ?
C41 C40 C45 119.6(5) . . ?
N4 C40 C45 118.3(5) . . ?
C40 C41 C42 119.6(6) . . ?
C40 C41 C47 121.4(5) . . ?
C42 C41 C47 119.1(6) . . ?
C43 C42 C41 120.9(7) . . ?
C43 C42 H42 119.6 . . ?
C41 C42 H42 119.6 . . ?
C44 C43 C42 119.4(6) . . ?
C44 C43 H43 120.3 . . ?
C42 C43 H43 120.3 . . ?
C43 C44 C45 122.8(7) . . ?
C43 C44 H44 118.6 . . ?
C45 C44 H44 118.6 . . ?
C44 C45 C40 117.7(6) . . ?
C44 C45 C46 119.1(6) . . ?
C40 C45 C46 123.2(5) . . ?
C45 C46 C461 112.5(5) . . ?
C45 C46 C462 109.9(5) . . ?
C461 C46 C462 110.6(5) . . ?
C45 C46 H46 107.9 . . ?
C461 C46 H46 107.9 . . ?
C462 C46 H46 107.9 . . ?
C471 C47 C41 115.1(6) . . ?
C471 C47 C472 109.4(6) . . ?
C41 C47 C472 110.9(5) . . ?
C471 C47 H47 107.0 . . ?
C41 C47 H47 107.0 . . ?
C472 C47 H47 107.0 . . ?
N5 C50 C55 123.8(6) . . ?
N5 C50 C51 118.6(6) . . ?
C55 C50 C51 117.6(5) . . ?
N5 C50 Li1 43.8(4) . . ?
C55 C50 Li1 114.9(5) . . ?
C51 C50 Li1 107.6(4) . . ?
C52 C51 C50 119.2(6) . . ?
C52 C51 C57 119.6(5) . . ?
C50 C51 C57 121.0(5) . . ?
C53 C52 C51 121.4(6) . . ?
C53 C52 H52 119.3 . . ?
C51 C52 H52 119.3 . . ?
C52 C53 C54 119.9(7) . . ?
C52 C53 H53 120.0 . . ?
C54 C53 H53 120.0 . . ?
C55 C54 C53 120.4(7) . . ?
C55 C54 H54 119.8 . . ?
C53 C54 H54 119.8 . . ?
C54 C55 C50 121.3(6) . . ?
C54 C55 C56 116.3(6) . . ?
C50 C55 C56 122.4(6) . . ?
C561 C56 C55 109.8(6) . . ?
C561 C56 C562 111.5(7) . . ?
C55 C56 C562 114.2(6) . . ?
C561 C56 H56 107.0 . . ?
C55 C56 H56 107.0 . . ?
C562 C56 H56 107.0 . . ?
C51 C57 C571 111.3(5) . . ?
C51 C57 C572 112.3(5) . . ?
C571 C57 C572 109.2(5) . . ?
C51 C57 H57 108.0 . . ?
C571 C57 H57 108.0 . . ?
C572 C57 H57 108.0 . . ?
C16 C161 H16A 109.5 . . ?
C16 C161 H16B 109.5 . . ?
H16A C161 H16B 109.5 . . ?
C16 C161 H16C 109.5 . . ?
H16A C161 H16C 109.5 . . ?
H16B C161 H16C 109.5 . . ?
C16 C162 H16D 109.5 . . ?
C16 C162 H16E 109.5 . . ?
H16D C162 H16E 109.5 . . ?
C16 C162 H16F 109.5 . . ?
H16D C162 H16F 109.5 . . ?
H16E C162 H16F 109.5 . . ?
C17 C171 H17A 109.5 . . ?
C17 C171 H17B 109.5 . . ?
H17A C171 H17B 109.5 . . ?
C17 C171 H17C 109.5 . . ?
H17A C171 H17C 109.5 . . ?
H17B C171 H17C 109.5 . . ?
C17 C172 H17D 109.5 . . ?
C17 C172 H17E 109.5 . . ?
H17D C172 H17E 109.5 . . ?
C17 C172 H17F 109.5 . . ?
H17D C172 H17F 109.5 . . ?
H17E C172 H17F 109.5 . . ?
C26 C261 H26A 109.5 . . ?
C26 C261 H26B 109.5 . . ?
H26A C261 H26B 109.5 . . ?
C26 C261 H26C 109.5 . . ?
H26A C261 H26C 109.5 . . ?
H26B C261 H26C 109.5 . . ?
C26 C262 H26D 109.5 . . ?
C26 C262 H26E 109.5 . . ?
H26D C262 H26E 109.5 . . ?
C26 C262 H26F 109.5 . . ?
H26D C262 H26F 109.5 . . ?
H26E C262 H26F 109.5 . . ?
C27 C271 H27A 109.5 . . ?
C27 C271 H27B 109.5 . . ?
H27A C271 H27B 109.5 . . ?
C27 C271 H27C 109.5 . . ?
H27A C271 H27C 109.5 . . ?
H27B C271 H27C 109.5 . . ?
C27 C272 H27D 109.5 . . ?
C27 C272 H27E 109.5 . . ?
H27D C272 H27E 109.5 . . ?
C27 C272 H27F 109.5 . . ?
H27D C272 H27F 109.5 . . ?
H27E C272 H27F 109.5 . . ?
C36 C361 H36A 109.5 . . ?
C36 C361 H36B 109.5 . . ?
H36A C361 H36B 109.5 . . ?
C36 C361 H36C 109.5 . . ?
H36A C361 H36C 109.5 . . ?
H36B C361 H36C 109.5 . . ?
C36 C362 H36D 109.5 . . ?
C36 C362 H36E 109.5 . . ?
H36D C362 H36E 109.5 . . ?
C36 C362 H36F 109.5 . . ?
H36D C362 H36F 109.5 . . ?
H36E C362 H36F 109.5 . . ?
C37 C371 H37A 109.5 . . ?
C37 C371 H37B 109.5 . . ?
H37A C371 H37B 109.5 . . ?
C37 C371 H37C 109.5 . . ?
H37A C371 H37C 109.5 . . ?
H37B C371 H37C 109.5 . . ?
C37 C372 H37D 109.5 . . ?
C37 C372 H37E 109.5 . . ?
H37D C372 H37E 109.5 . . ?
C37 C372 H37F 109.5 . . ?
H37D C372 H37F 109.5 . . ?
H37E C372 H37F 109.5 . . ?
C46 C461 H46A 109.5 . . ?
C46 C461 H46B 109.5 . . ?
H46A C461 H46B 109.5 . . ?
C46 C461 H46C 109.5 . . ?
H46A C461 H46C 109.5 . . ?
H46B C461 H46C 109.5 . . ?
C46 C462 H46D 109.5 . . ?
C46 C462 H46E 109.5 . . ?
H46D C462 H46E 109.5 . . ?
C46 C462 H46F 109.5 . . ?
H46D C462 H46F 109.5 . . ?
H46E C462 H46F 109.5 . . ?
C47 C471 H47A 109.5 . . ?
C47 C471 H47B 109.5 . . ?
H47A C471 H47B 109.5 . . ?
C47 C471 H47C 109.5 . . ?
H47A C471 H47C 109.5 . . ?
H47B C471 H47C 109.5 . . ?
C47 C472 H47D 109.5 . . ?
C47 C472 H47E 109.5 . . ?
H47D C472 H47E 109.5 . . ?
C47 C472 H47F 109.5 . . ?
H47D C472 H47F 109.5 . . ?
H47E C472 H47F 109.5 . . ?
C56 C561 H56A 109.5 . . ?
C56 C561 H56B 109.5 . . ?
H56A C561 H56B 109.5 . . ?
C56 C561 H56C 109.5 . . ?
H56A C561 H56C 109.5 . . ?
H56B C561 H56C 109.5 . . ?
C56 C562 H56D 109.5 . . ?
C56 C562 H56E 109.5 . . ?
H56D C562 H56E 109.5 . . ?
C56 C562 H56F 109.5 . . ?
H56D C562 H56F 109.5 . . ?
H56E C562 H56F 109.5 . . ?
C57 C571 H57A 109.5 . . ?
C57 C571 H57B 109.5 . . ?
H57A C571 H57B 109.5 . . ?
C57 C571 H57C 109.5 . . ?
H57A C571 H57C 109.5 . . ?
H57B C571 H57C 109.5 . . ?
C57 C572 H57D 109.5 . . ?
C57 C572 H57E 109.5 . . ?
H57D C572 H57E 109.5 . . ?
C57 C572 H57F 109.5 . . ?
H57D C572 H57F 109.5 . . ?
H57E C572 H57F 109.5 . . ?
O1 Li1 N2 136.2(6) . . ?
O1 Li1 N5 130.3(6) . . ?
N2 Li1 N5 93.4(5) . . ?
O1 Li1 C50 102.2(5) . . ?
N2 Li1 C50 121.2(5) . . ?
N5 Li1 C50 28.6(2) . . ?
O1 Li1 U1 172.9(6) . . ?
N2 Li1 U1 40.9(2) . . ?
N5 Li1 U1 53.0(3) . . ?
C50 Li1 U1 80.3(3) . . ?
O1 Li1 H5N 134.8(10) . . ?
N2 Li1 H5N 85.4(8) . . ?
N5 Li1 H5N 23.0(9) . . ?
C50 Li1 H5N 45.2(7) . . ?
U1 Li1 H5N 51.2(9) . . ?
O2 Li2 N3 129.8(6) . . ?
O2 Li2 N1 139.9(6) . . ?
N3 Li2 N1 89.7(4) . . ?
O2 Li2 C10 106.1(5) . . ?
N3 Li2 C10 123.8(5) . . ?
N1 Li2 C10 34.1(2) . . ?
O2 Li2 C30 99.4(5) . . ?
N3 Li2 C30 31.0(2) . . ?
N1 Li2 C30 120.5(5) . . ?
C10 Li2 C30 154.5(5) . . ?
O2 Li2 U1 173.4(6) . . ?
N3 Li2 U1 46.2(3) . . ?
N1 Li2 U1 43.5(2) . . ?
C10 Li2 U1 77.6(3) . . ?
C30 Li2 U1 77.0(3) . . ?
 
loop_
 _geom_torsion_atom_site_label_1
 _geom_torsion_atom_site_label_2
 _geom_torsion_atom_site_label_3
 _geom_torsion_atom_site_label_4
 _geom_torsion
 _geom_torsion_site_symmetry_1
 _geom_torsion_site_symmetry_2
 _geom_torsion_site_symmetry_3
 _geom_torsion_site_symmetry_4
 _geom_torsion_publ_flag
C4 O1 C1 C2 39.1(9) . . . . ?
Li1 O1 C1 C2 -141.3(8) . . . . ?
O1 C1 C2 C3 -30.0(11) . . . . ?
C1 C2 C3 C4 9.7(11) . . . . ?
C1 O1 C4 C3 -32.2(9) . . . . ?
Li1 O1 C4 C3 148.2(7) . . . . ?
C2 C3 C4 O1 13.5(10) . . . . ?
C8 O2 C5 C6 24.4(10) . . . . ?
Li2 O2 C5 C6 -157.8(8) . . . . ?
O2 C5 C6 C7 -17.6(12) . . . . ?
C5 C6 C7 C8 4.1(13) . . . . ?
C5 O2 C8 C7 -21.8(9) . . . . ?
Li2 O2 C8 C7 160.4(7) . . . . ?
C6 C7 C8 O2 10.9(11) . . . . ?
Li2 N1 C10 C15 -77.8(6) . . . . ?
Li2 N1 C10 C11 102.4(6) . . . . ?
N1 C10 C11 C12 -175.9(6) . . . . ?
C15 C10 C11 C12 4.2(9) . . . . ?
Li2 C10 C11 C12 -111.9(7) . . . . ?
N1 C10 C11 C17 2.8(9) . . . . ?
C15 C10 C11 C17 -177.0(6) . . . . ?
Li2 C10 C11 C17 66.8(7) . . . . ?
C10 C11 C12 C13 -0.3(12) . . . . ?
C17 C11 C12 C13 -179.1(8) . . . . ?
C11 C12 C13 C14 -2.4(14) . . . . ?
C12 C13 C14 C15 1.1(14) . . . . ?
C13 C14 C15 C10 2.8(12) . . . . ?
C13 C14 C15 C16 -177.7(8) . . . . ?
N1 C10 C15 C14 174.7(6) . . . . ?
C11 C10 C15 C14 -5.5(9) . . . . ?
Li2 C10 C15 C14 119.8(7) . . . . ?
N1 C10 C15 C16 -4.8(9) . . . . ?
C11 C10 C15 C16 175.1(6) . . . . ?
Li2 C10 C15 C16 -59.7(7) . . . . ?
C14 C15 C16 C161 -72.9(10) . . . . ?
C10 C15 C16 C161 106.6(9) . . . . ?
C14 C15 C16 C162 52.4(9) . . . . ?
C10 C15 C16 C162 -128.1(7) . . . . ?
C12 C11 C17 C172 91.7(8) . . . . ?
C10 C11 C17 C172 -87.1(7) . . . . ?
C12 C11 C17 C171 -34.2(9) . . . . ?
C10 C11 C17 C171 147.0(6) . . . . ?
Li1 N2 C20 C25 -85.5(6) . . . . ?
U1 N2 C20 C25 87.2(8) . . . . ?
Li1 N2 C20 C21 93.2(6) . . . . ?
U1 N2 C20 C21 -94.1(7) . . . . ?
C25 C20 C21 C22 -5.0(9) . . . . ?
N2 C20 C21 C22 176.3(5) . . . . ?
C25 C20 C21 C27 173.2(5) . . . . ?
N2 C20 C21 C27 -5.4(8) . . . . ?
C20 C21 C22 C23 2.2(11) . . . . ?
C27 C21 C22 C23 -176.0(7) . . . . ?
C21 C22 C23 C24 1.4(12) . . . . ?
C22 C23 C24 C25 -2.3(12) . . . . ?
C23 C24 C25 C20 -0.5(10) . . . . ?
C23 C24 C25 C26 176.6(7) . . . . ?
C21 C20 C25 C24 4.2(9) . . . . ?
N2 C20 C25 C24 -177.2(5) . . . . ?
C21 C20 C25 C26 -172.8(5) . . . . ?
N2 C20 C25 C26 5.9(8) . . . . ?
C24 C25 C26 C262 52.2(8) . . . . ?
C20 C25 C26 C262 -130.8(6) . . . . ?
C24 C25 C26 C261 -71.0(7) . . . . ?
C20 C25 C26 C261 106.0(6) . . . . ?
C22 C21 C27 C271 98.4(8) . . . . ?
C20 C21 C27 C271 -79.7(7) . . . . ?
C22 C21 C27 C272 -24.3(9) . . . . ?
C20 C21 C27 C272 157.5(6) . . . . ?
Li2 N3 C30 C35 -89.5(7) . . . . ?
U1 N3 C30 C35 118.5(19) . . . . ?
Li2 N3 C30 C31 89.9(7) . . . . ?
U1 N3 C30 C31 -62(2) . . . . ?
U1 N3 C30 Li2 -152(2) . . . . ?
N3 C30 C31 C32 -178.4(6) . . . . ?
C35 C30 C31 C32 1.0(9) . . . . ?
Li2 C30 C31 C32 -127.0(6) . . . . ?
N3 C30 C31 C37 3.4(9) . . . . ?
C35 C30 C31 C37 -177.2(6) . . . . ?
Li2 C30 C31 C37 54.8(7) . . . . ?
C30 C31 C32 C33 -0.2(11) . . . . ?
C37 C31 C32 C33 178.0(7) . . . . ?
C31 C32 C33 C34 -1.2(12) . . . . ?
C32 C33 C34 C35 1.8(13) . . . . ?
C33 C34 C35 C30 -1.1(11) . . . . ?
C33 C34 C35 C36 178.8(7) . . . . ?
N3 C30 C35 C34 179.0(6) . . . . ?
C31 C30 C35 C34 -0.4(10) . . . . ?
Li2 C30 C35 C34 126.7(6) . . . . ?
N3 C30 C35 C36 -0.9(10) . . . . ?
C31 C30 C35 C36 179.7(6) . . . . ?
Li2 C30 C35 C36 -53.2(8) . . . . ?
C34 C35 C36 C362 43.1(10) . . . . ?
C30 C35 C36 C362 -137.0(8) . . . . ?
C34 C35 C36 C361 -77.7(9) . . . . ?
C30 C35 C36 C361 102.1(8) . . . . ?
C32 C31 C37 C371 44.0(9) . . . . ?
C30 C31 C37 C371 -137.8(7) . . . . ?
C32 C31 C37 C372 -76.4(8) . . . . ?
C30 C31 C37 C372 101.8(7) . . . . ?
U1 N4 C40 C41 -139.8(6) . . . . ?
U1 N4 C40 C45 42.0(9) . . . . ?
N4 C40 C41 C42 179.2(5) . . . . ?
C45 C40 C41 C42 -2.6(9) . . . . ?
N4 C40 C41 C47 -1.3(9) . . . . ?
C45 C40 C41 C47 176.9(5) . . . . ?
C40 C41 C42 C43 0.0(10) . . . . ?
C47 C41 C42 C43 -179.5(7) . . . . ?
C41 C42 C43 C44 1.8(12) . . . . ?
C42 C43 C44 C45 -0.9(12) . . . . ?
C43 C44 C45 C40 -1.7(10) . . . . ?
C43 C44 C45 C46 176.8(7) . . . . ?
C41 C40 C45 C44 3.4(8) . . . . ?
N4 C40 C45 C44 -178.3(5) . . . . ?
C41 C40 C45 C46 -175.0(5) . . . . ?
N4 C40 C45 C46 3.2(8) . . . . ?
C44 C45 C46 C461 64.8(7) . . . . ?
C40 C45 C46 C461 -116.8(6) . . . . ?
C44 C45 C46 C462 -58.9(7) . . . . ?
C40 C45 C46 C462 119.5(6) . . . . ?
C40 C41 C47 C471 153.5(6) . . . . ?
C42 C41 C47 C471 -27.0(9) . . . . ?
C40 C41 C47 C472 -81.6(7) . . . . ?
C42 C41 C47 C472 97.8(7) . . . . ?
Li1 N5 C50 C55 -92.0(7) . . . . ?
U1 N5 C50 C55 145.7(9) . . . . ?
Li1 N5 C50 C51 86.0(7) . . . . ?
U1 N5 C50 C51 -36.4(13) . . . . ?
U1 N5 C50 Li1 -122.3(12) . . . . ?
N5 C50 C51 C52 -175.8(5) . . . . ?
C55 C50 C51 C52 2.2(8) . . . . ?
Li1 C50 C51 C52 -129.4(5) . . . . ?
N5 C50 C51 C57 0.5(8) . . . . ?
C55 C50 C51 C57 178.6(5) . . . . ?
Li1 C50 C51 C57 46.9(6) . . . . ?
C50 C51 C52 C53 0.3(9) . . . . ?
C57 C51 C52 C53 -176.1(6) . . . . ?
C51 C52 C53 C54 -2.4(10) . . . . ?
C52 C53 C54 C55 1.8(11) . . . . ?
C53 C54 C55 C50 0.8(11) . . . . ?
C53 C54 C55 C56 178.1(6) . . . . ?
N5 C50 C55 C54 175.1(6) . . . . ?
C51 C50 C55 C54 -2.8(9) . . . . ?
Li1 C50 C55 C54 125.5(6) . . . . ?
N5 C50 C55 C56 -2.0(10) . . . . ?
C51 C50 C55 C56 -179.9(6) . . . . ?
Li1 C50 C55 C56 -51.6(8) . . . . ?
C54 C55 C56 C561 -84.5(8) . . . . ?
C50 C55 C56 C561 92.7(8) . . . . ?
C54 C55 C56 C562 41.6(10) . . . . ?
C50 C55 C56 C562 -141.2(7) . . . . ?
C52 C51 C57 C571 88.8(7) . . . . ?
C50 C51 C57 C571 -87.6(7) . . . . ?
C52 C51 C57 C572 -33.9(8) . . . . ?
C50 C51 C57 C572 149.7(6) . . . . ?
C1 O1 Li1 N2 -24.3(13) . . . . ?
C4 O1 Li1 N2 155.2(8) . . . . ?
C1 O1 Li1 N5 157.6(8) . . . . ?
C4 O1 Li1 N5 -22.9(11) . . . . ?
C1 O1 Li1 C50 163.3(7) . . . . ?
C4 O1 Li1 C50 -17.2(8) . . . . ?
C5 O2 Li2 N3 149.2(8) . . . . ?
C8 O2 Li2 N3 -33.4(12) . . . . ?
C5 O2 Li2 N1 -19.5(14) . . . . ?
C8 O2 Li2 N1 157.9(9) . . . . ?
C5 O2 Li2 C10 -24.0(9) . . . . ?
C8 O2 Li2 C10 153.4(6) . . . . ?
C5 O2 Li2 C30 156.0(6) . . . . ?
C8 O2 Li2 C30 -26.6(8) . . . . ?
 
_refine_diff_density_max    3.079
_refine_diff_density_min   -1.928
_refine_diff_density_rms    0.108




