# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_ponebar
_database_code_depnum_ccdc_archive 'CCDC 1836170'
loop_
_audit_author_name
_audit_author_address
'Nickolas Anderson'
;Los Alamos National Laboratory
United States of America
;
_audit_update_record             
;
2019-03-06 deposited with the CCDC.	2019-04-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H38 N4 S2 U'
_chemical_formula_weight         756.79

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'
S S 0.1246 0.1234 '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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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, -z'

_cell_length_a                   8.1655(8)
_cell_length_b                   9.6294(10)
_cell_length_c                   11.0077(11)
_cell_angle_alpha                89.562(2)
_cell_angle_beta                 73.0830(10)
_cell_angle_gamma                70.7190(10)
_cell_volume                     777.87(14)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9906
_cell_measurement_theta_max      28.33
_cell_measurement_theta_min      2.25

_exptl_crystal_description       block
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.616
_exptl_crystal_F_000             370
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_exptl_absorpt_coefficient_mu    5.375
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.4666
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/3 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.1325 before and 0.0399 after correction.
The Ratio of minimum to maximum transmission is 0.6257.
The λ/2 correction factor is 0.00150.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            11445
_diffrn_reflns_av_unetI/netI     0.0297
_diffrn_reflns_av_R_equivalents  0.0291
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.251
_diffrn_reflns_theta_max         28.334
_diffrn_reflns_theta_full        26.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             3865
_reflns_number_gt                3865
_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.
 
 _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_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 V.2014.7-1 (Bruker AXS, 2014)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2008)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0118P)²+0.3421P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3865
_refine_ls_number_parameters     172
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0159
_refine_ls_R_factor_gt           0.0159
_refine_ls_wR_factor_ref         0.0382
_refine_ls_wR_factor_gt          0.0381
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_restrained_S_all      1.085
_refine_ls_shift/su_max          0.001
_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 0.500000 0.500000 0.500000 0.00984(4) Uani 1 2 d S . P . .
S1 S 0.33869(6) 0.31839(6) 0.43269(5) 0.01581(9) Uani 1 1 d . . . . .
N1 N 0.3204(2) 0.52925(19) 0.65659(15) 0.0132(3) Uani 1 1 d . . . . .
N2 N 0.7070(2) 0.27623(19) 0.57348(16) 0.0141(3) Uani 1 1 d . . . . .
C6 C 0.6152(3) 0.0794(2) 0.2816(2) 0.0180(4) Uani 1 1 d . . . . .
H6 H 0.634028 0.044798 0.359239 0.022 Uiso 1 1 calc R U . . .
C5 C 0.4802(3) 0.2150(2) 0.28443(19) 0.0157(4) Uani 1 1 d . . . . .
C15 C 0.6460(3) 0.1730(2) 0.63590(19) 0.0160(4) Uani 1 1 d . . . . .
H15 H 0.524772 0.178305 0.644625 0.019 Uiso 1 1 calc R U . . .
C1 C 0.1843(3) 0.5325(2) 0.77925(18) 0.0156(4) Uani 1 1 d . . . . .
C7 C 0.7224(3) -0.0058(2) 0.1667(2) 0.0225(4) Uani 1 1 d . . . . .
H7 H 0.813669 -0.097730 0.166386 0.027 Uiso 1 1 calc R U . . .
C11 C 0.8802(3) 0.2656(2) 0.5593(2) 0.0165(4) Uani 1 1 d . . . . .
H11 H 0.925289 0.336721 0.514628 0.020 Uiso 1 1 calc R U . . .
C10 C 0.4547(3) 0.2627(3) 0.1693(2) 0.0252(5) Uani 1 1 d . . . . .
H10 H 0.362986 0.354267 0.169124 0.030 Uiso 1 1 calc R U . . .
C8 C 0.6966(4) 0.0430(3) 0.0524(2) 0.0300(5) Uani 1 1 d . . . . .
H8 H 0.769799 -0.014880 -0.026127 0.036 Uiso 1 1 calc R U . . .
C2 C 0.0617(3) 0.6925(2) 0.8260(2) 0.0240(5) Uani 1 1 d . . . . .
H2A H 0.136287 0.751128 0.834555 0.036 Uiso 1 1 calc R U . . .
H2B H -0.026814 0.695551 0.909062 0.036 Uiso 1 1 calc R U . . .
H2C H -0.003056 0.733302 0.764471 0.036 Uiso 1 1 calc R U . . .
C14 C 0.7516(3) 0.0605(2) 0.6875(2) 0.0191(4) Uani 1 1 d . . . . .
H14 H 0.703569 -0.009410 0.731817 0.023 Uiso 1 1 calc R U . . .
C13 C 0.9300(3) 0.0513(2) 0.6733(2) 0.0214(4) Uani 1 1 d . . . . .
H13 H 1.005729 -0.024671 0.708339 0.026 Uiso 1 1 calc R U . . .
C12 C 0.9953(3) 0.1548(2) 0.6073(2) 0.0192(4) Uani 1 1 d . . . . .
H12 H 1.117207 0.149818 0.595078 0.023 Uiso 1 1 calc R U . . .
C9 C 0.5624(4) 0.1773(3) 0.0545(2) 0.0346(6) Uani 1 1 d . . . . .
H9 H 0.543783 0.211456 -0.023283 0.041 Uiso 1 1 calc R U . . .
C3 C 0.0722(3) 0.4406(3) 0.7570(2) 0.0237(5) Uani 1 1 d . . . . .
H3A H 0.006127 0.486760 0.697481 0.036 Uiso 1 1 calc R U . . .
H3B H -0.014996 0.435866 0.838292 0.036 Uiso 1 1 calc R U . . .
H3C H 0.153894 0.340386 0.720882 0.036 Uiso 1 1 calc R U . . .
C4 C 0.2849(3) 0.4643(3) 0.8742(2) 0.0271(5) Uani 1 1 d . . . . .
H4A H 0.364055 0.362478 0.841549 0.041 Uiso 1 1 calc R U . . .
H4B H 0.196248 0.464452 0.956334 0.041 Uiso 1 1 calc R U . . .
H4C H 0.358909 0.522284 0.885533 0.041 Uiso 1 1 calc R U . . .


_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 1.8615(16) . ?
U1 N1 1.8615(16) 2_666 ?
U1 N2 2.5531(17) 2_666 ?
U1 N2 2.5531(17) . ?
U1 S1 2.7296(5) . ?
U1 S1 2.7297(5) 2_666 ?
S1 C5 1.777(2) . ?
N1 C1 1.471(2) . ?
N2 C11 1.346(3) . ?
N2 C15 1.351(3) . ?
C6 C7 1.392(3) . ?
C6 C5 1.397(3) . ?
C6 H6 0.9500 . ?
C5 C10 1.394(3) . ?
C15 C14 1.378(3) . ?
C15 H15 0.9500 . ?
C1 C4 1.527(3) . ?
C1 C2 1.527(3) . ?
C1 C3 1.533(3) . ?
C7 C8 1.388(3) . ?
C7 H7 0.9500 . ?
C11 C12 1.385(3) . ?
C11 H11 0.9500 . ?
C10 C9 1.392(3) . ?
C10 H10 0.9500 . ?
C8 C9 1.387(4) . ?
C8 H8 0.9500 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C14 C13 1.392(3) . ?
C14 H14 0.9500 . ?
C13 C12 1.386(3) . ?
C13 H13 0.9500 . ?
C12 H12 0.9500 . ?
C9 H9 0.9500 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?

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 N1 180.0 . 2_666 ?
N1 U1 N2 89.82(6) . 2_666 ?
N1 U1 N2 90.18(6) 2_666 2_666 ?
N1 U1 N2 90.18(6) . . ?
N1 U1 N2 89.82(6) 2_666 . ?
N2 U1 N2 180.0 2_666 . ?
N1 U1 S1 84.15(5) . . ?
N1 U1 S1 95.85(5) 2_666 . ?
N2 U1 S1 91.90(4) 2_666 . ?
N2 U1 S1 88.10(4) . . ?
N1 U1 S1 95.85(5) . 2_666 ?
N1 U1 S1 84.15(5) 2_666 2_666 ?
N2 U1 S1 88.10(4) 2_666 2_666 ?
N2 U1 S1 91.90(4) . 2_666 ?
S1 U1 S1 180.000(14) . 2_666 ?
C5 S1 U1 109.22(7) . . ?
C1 N1 U1 172.96(14) . . ?
C11 N2 C15 117.93(18) . . ?
C11 N2 U1 119.27(13) . . ?
C15 N2 U1 122.58(13) . . ?
C7 C6 C5 120.9(2) . . ?
C7 C6 H6 119.6 . . ?
C5 C6 H6 119.6 . . ?
C10 C5 C6 118.39(19) . . ?
C10 C5 S1 121.41(16) . . ?
C6 C5 S1 120.13(16) . . ?
N2 C15 C14 122.95(18) . . ?
N2 C15 H15 118.5 . . ?
C14 C15 H15 118.5 . . ?
N1 C1 C4 108.30(17) . . ?
N1 C1 C2 109.15(16) . . ?
C4 C1 C2 110.92(18) . . ?
N1 C1 C3 107.65(16) . . ?
C4 C1 C3 110.27(19) . . ?
C2 C1 C3 110.46(18) . . ?
C8 C7 C6 120.3(2) . . ?
C8 C7 H7 119.8 . . ?
C6 C7 H7 119.8 . . ?
N2 C11 C12 122.49(19) . . ?
N2 C11 H11 118.8 . . ?
C12 C11 H11 118.8 . . ?
C9 C10 C5 120.6(2) . . ?
C9 C10 H10 119.7 . . ?
C5 C10 H10 119.7 . . ?
C9 C8 C7 119.1(2) . . ?
C9 C8 H8 120.4 . . ?
C7 C8 H8 120.4 . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C15 C14 C13 118.6(2) . . ?
C15 C14 H14 120.7 . . ?
C13 C14 H14 120.7 . . ?
C12 C13 C14 118.9(2) . . ?
C12 C13 H13 120.5 . . ?
C14 C13 H13 120.5 . . ?
C11 C12 C13 119.04(19) . . ?
C11 C12 H12 120.5 . . ?
C13 C12 H12 120.5 . . ?
C8 C9 C10 120.7(2) . . ?
C8 C9 H9 119.6 . . ?
C10 C9 H9 119.6 . . ?
C1 C3 H3A 109.5 . . ?
C1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C1 C4 H4A 109.5 . . ?
C1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?

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
C7 C6 C5 C10 0.4(3) . . . . ?
C7 C6 C5 S1 177.41(17) . . . . ?
U1 S1 C5 C10 -94.19(18) . . . . ?
U1 S1 C5 C6 88.89(17) . . . . ?
C11 N2 C15 C14 1.5(3) . . . . ?
U1 N2 C15 C14 -173.06(15) . . . . ?
C5 C6 C7 C8 -0.1(3) . . . . ?
C15 N2 C11 C12 -0.8(3) . . . . ?
U1 N2 C11 C12 173.95(16) . . . . ?
C6 C5 C10 C9 -0.5(4) . . . . ?
S1 C5 C10 C9 -177.5(2) . . . . ?
C6 C7 C8 C9 -0.2(4) . . . . ?
N2 C15 C14 C13 -0.9(3) . . . . ?
C15 C14 C13 C12 -0.4(3) . . . . ?
N2 C11 C12 C13 -0.5(3) . . . . ?
C14 C13 C12 C11 1.1(3) . . . . ?
C7 C8 C9 C10 0.1(4) . . . . ?
C5 C10 C9 C8 0.3(4) . . . . ?

_refine_diff_density_max         1.269
_refine_diff_density_min         -1.227
_refine_diff_density_rms         0.091

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_untbu2teph2py2
_database_code_depnum_ccdc_archive 'CCDC 1836176'
loop_
_audit_author_name
_audit_author_address
'Nickolas Anderson'
;Los Alamos National Laboratory
United States of America
;
_audit_update_record             
;
2019-03-06 deposited with the CCDC.	2019-04-23 downloaded from the CCDC.
;
_audit_creation_date             2018-08-23
_audit_creation_method           
;
Olex2 1.2
(compiled Aug 10 2017 17:28:52 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C30 H38 N4 Te2 U'
_chemical_formula_sum            'C30 H38 N4 Te2 U'
_chemical_formula_weight         947.87
_chemical_melting_point          ?
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'
Te Te -0.5308 1.6751 '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'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.3876(11)
_cell_length_b                   9.8459(13)
_cell_length_c                   11.1701(14)
_cell_angle_alpha                87.084(6)
_cell_angle_beta                 73.083(6)
_cell_angle_gamma                69.599(6)
_cell_volume                     825.88(19)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    7229
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.560
_cell_measurement_theta_min      2.709
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    6.668
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5353
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/2 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.0982 before and 0.0391 after correction.
The Ratio of minimum to maximum transmission is 0.7181.
The λ/2 correction factor is 0.00150.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark orange'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.906
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             442
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0280
_diffrn_reflns_av_unetI/netI     0.0259
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            11462
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.574
_diffrn_reflns_theta_min         2.709
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3274
_reflns_number_total             3400
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 V.2014.7-1 (Bruker AXS, 2014)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.900
_refine_diff_density_min         -0.481
_refine_diff_density_rms         0.089
_refine_ls_extinction_coef       0.0016(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     173
_refine_ls_number_reflns         3400
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0188
_refine_ls_R_factor_gt           0.0178
_refine_ls_restrained_S_all      1.054
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0187P)²+0.2970P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0421
_refine_ls_wR_factor_ref         0.0427
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C11(H11), C12(H12), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C13(H13),
 C14(H14), C15(H15)
2.b Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C3(H3A,H3B,H3C), C2(H2A,H2B,H2C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_special_details      
;
The structure was solved using Patterson Methods, followed by a Tangent Expansion (ShelXS). RE = 0.1, Nqual =   0, Ralpha = 0.029
;
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 0.500000 0.500000 0.500000 0.01229(6) Uani 1 2 d S T P . .
Te1 Te 0.32978(2) 0.30957(2) 0.41386(2) 0.02065(7) Uani 1 1 d . . . . .
N2 N 0.3003(3) 0.7283(3) 0.4247(2) 0.0177(5) Uani 1 1 d . . . . .
N1 N 0.6784(3) 0.4817(2) 0.3504(2) 0.0165(5) Uani 1 1 d . . . . .
C11 C 0.6475(4) 0.0661(3) 0.2486(3) 0.0243(7) Uani 1 1 d . . . . .
H11 H 0.659353 0.031007 0.327497 0.029 Uiso 1 1 calc R . . . .
C12 C 0.7647(5) -0.0127(4) 0.1400(3) 0.0311(8) Uani 1 1 d . . . . .
H12 H 0.855896 -0.101187 0.144987 0.037 Uiso 1 1 calc R . . . .
C5 C 0.3581(4) 0.8324(3) 0.3657(3) 0.0195(6) Uani 1 1 d . . . . .
H5 H 0.476080 0.826280 0.358553 0.023 Uiso 1 1 calc R . . . .
C6 C 0.2537(4) 0.9476(3) 0.3153(3) 0.0207(6) Uani 1 1 d . . . . .
H6 H 0.299625 1.018214 0.273046 0.025 Uiso 1 1 calc R . . . .
C7 C 0.0808(4) 0.9582(3) 0.3273(3) 0.0219(7) Uani 1 1 d . . . . .
H7 H 0.005641 1.036432 0.293652 0.026 Uiso 1 1 calc R . . . .
C8 C 0.0193(4) 0.8523(3) 0.3897(3) 0.0219(7) Uani 1 1 d . . . . .
H8 H -0.099055 0.857262 0.399787 0.026 Uiso 1 1 calc R . . . .
C9 C 0.1329(4) 0.7398(3) 0.4368(3) 0.0194(6) Uani 1 1 d . . . . .
H9 H 0.090194 0.667686 0.479425 0.023 Uiso 1 1 calc R . . . .
C1 C 0.8084(4) 0.4798(3) 0.2274(3) 0.0175(6) Uani 1 1 d . . . . .
C4 C 0.9318(4) 0.3234(3) 0.1884(3) 0.0260(7) Uani 1 1 d . . . . .
H4A H 0.993922 0.284902 0.251440 0.039 Uiso 1 1 calc GR . . . .
H4B H 1.018896 0.320542 0.107175 0.039 Uiso 1 1 calc GR . . . .
H4C H 0.861668 0.264238 0.181462 0.039 Uiso 1 1 calc GR . . . .
C3 C 0.7057(5) 0.5412(4) 0.1322(3) 0.0303(8) Uani 1 1 d . . . . .
H3A H 0.635227 0.481865 0.126741 0.045 Uiso 1 1 calc GR . . . .
H3B H 0.789815 0.539765 0.049873 0.045 Uiso 1 1 calc GR . . . .
H3C H 0.626460 0.641271 0.159091 0.045 Uiso 1 1 calc GR . . . .
C2 C 0.9146(4) 0.5735(3) 0.2410(3) 0.0271(7) Uani 1 1 d . . . . .
H2A H 0.833286 0.672770 0.269098 0.041 Uiso 1 1 calc GR . . . .
H2B H 0.999998 0.574694 0.159918 0.041 Uiso 1 1 calc GR . . . .
H2C H 0.978721 0.533296 0.302714 0.041 Uiso 1 1 calc GR . . . .
C10 C 0.5127(4) 0.1957(3) 0.2444(3) 0.0211(6) Uani 1 1 d . . . . .
C13 C 0.7500(5) 0.0364(4) 0.0242(4) 0.0438(10) Uani 1 1 d . . . . .
H13 H 0.830245 -0.017738 -0.050601 0.053 Uiso 1 1 calc R . . . .
C14 C 0.6157(6) 0.1663(5) 0.0189(4) 0.0510(12) Uani 1 1 d . . . . .
H14 H 0.604675 0.201826 -0.060111 0.061 Uiso 1 1 calc R . . . .
C15 C 0.4980(5) 0.2442(4) 0.1282(3) 0.0370(9) Uani 1 1 d . . . . .
H15 H 0.405816 0.332075 0.123330 0.044 Uiso 1 1 calc R . . . .


_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 Te1 3.0544(3) 2_666 ?
U1 Te1 3.0544(3) . ?
U1 N2 2.562(2) . ?
U1 N2 2.562(2) 2_666 ?
U1 N1 1.858(3) 2_666 ?
U1 N1 1.858(3) . ?
Te1 C10 2.126(3) . ?
N2 C5 1.346(4) . ?
N2 C9 1.336(4) . ?
N1 C1 1.481(4) . ?
C11 H11 0.9500 . ?
C11 C12 1.382(5) . ?
C11 C10 1.389(4) . ?
C12 H12 0.9500 . ?
C12 C13 1.382(5) . ?
C5 H5 0.9500 . ?
C5 C6 1.378(4) . ?
C6 H6 0.9500 . ?
C6 C7 1.383(4) . ?
C7 H7 0.9500 . ?
C7 C8 1.389(4) . ?
C8 H8 0.9500 . ?
C8 C9 1.382(4) . ?
C9 H9 0.9500 . ?
C1 C4 1.525(4) . ?
C1 C3 1.531(4) . ?
C1 C2 1.528(4) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C10 C15 1.384(5) . ?
C13 H13 0.9500 . ?
C13 C14 1.391(5) . ?
C14 H14 0.9500 . ?
C14 C15 1.386(5) . ?
C15 H15 0.9500 . ?

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
Te1 U1 Te1 180.0 . 2_666 ?
N2 U1 Te1 91.83(6) 2_666 2_666 ?
N2 U1 Te1 88.17(6) . 2_666 ?
N2 U1 Te1 88.17(6) 2_666 . ?
N2 U1 Te1 91.83(6) . . ?
N2 U1 N2 180.0 2_666 . ?
N1 U1 Te1 83.58(7) 2_666 . ?
N1 U1 Te1 96.42(7) . . ?
N1 U1 Te1 83.58(7) . 2_666 ?
N1 U1 Te1 96.42(7) 2_666 2_666 ?
N1 U1 N2 89.57(9) . . ?
N1 U1 N2 90.43(9) 2_666 . ?
N1 U1 N2 90.43(9) . 2_666 ?
N1 U1 N2 89.57(9) 2_666 2_666 ?
N1 U1 N1 180.00(12) 2_666 . ?
C10 Te1 U1 106.83(8) . . ?
C5 N2 U1 123.67(19) . . ?
C9 N2 U1 118.17(18) . . ?
C9 N2 C5 118.0(2) . . ?
C1 N1 U1 174.41(19) . . ?
C12 C11 H11 119.4 . . ?
C12 C11 C10 121.2(3) . . ?
C10 C11 H11 119.4 . . ?
C11 C12 H12 119.8 . . ?
C11 C12 C13 120.4(3) . . ?
C13 C12 H12 119.8 . . ?
N2 C5 H5 118.5 . . ?
N2 C5 C6 123.0(3) . . ?
C6 C5 H5 118.5 . . ?
C5 C6 H6 120.6 . . ?
C5 C6 C7 118.7(3) . . ?
C7 C6 H6 120.6 . . ?
C6 C7 H7 120.6 . . ?
C6 C7 C8 118.7(3) . . ?
C8 C7 H7 120.6 . . ?
C7 C8 H8 120.5 . . ?
C9 C8 C7 119.0(3) . . ?
C9 C8 H8 120.5 . . ?
N2 C9 C8 122.6(3) . . ?
N2 C9 H9 118.7 . . ?
C8 C9 H9 118.7 . . ?
N1 C1 C4 108.6(2) . . ?
N1 C1 C3 108.3(2) . . ?
N1 C1 C2 108.5(2) . . ?
C4 C1 C3 110.5(3) . . ?
C4 C1 C2 110.4(3) . . ?
C2 C1 C3 110.5(3) . . ?
C1 C4 H4A 109.5 . . ?
C1 C4 H4B 109.5 . . ?
C1 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C1 C3 H3A 109.5 . . ?
C1 C3 H3B 109.5 . . ?
C1 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C11 C10 Te1 119.9(2) . . ?
C15 C10 Te1 121.8(2) . . ?
C15 C10 C11 118.3(3) . . ?
C12 C13 H13 120.5 . . ?
C12 C13 C14 118.9(3) . . ?
C14 C13 H13 120.5 . . ?
C13 C14 H14 119.8 . . ?
C15 C14 C13 120.3(4) . . ?
C15 C14 H14 119.8 . . ?
C10 C15 C14 120.9(3) . . ?
C10 C15 H15 119.5 . . ?
C14 C15 H15 119.5 . . ?

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
U1 N2 C5 C6 173.6(2) . . . . ?
U1 N2 C9 C8 -174.4(2) . . . . ?
Te1 C10 C15 C14 -178.2(3) . . . . ?
N2 C5 C6 C7 1.1(5) . . . . ?
C11 C12 C13 C14 0.1(6) . . . . ?
C11 C10 C15 C14 -0.7(6) . . . . ?
C12 C11 C10 Te1 177.8(2) . . . . ?
C12 C11 C10 C15 0.2(5) . . . . ?
C12 C13 C14 C15 -0.6(7) . . . . ?
C5 N2 C9 C8 1.0(4) . . . . ?
C5 C6 C7 C8 -0.1(4) . . . . ?
C6 C7 C8 C9 -0.4(5) . . . . ?
C7 C8 C9 N2 -0.1(5) . . . . ?
C9 N2 C5 C6 -1.5(4) . . . . ?
C10 C11 C12 C13 0.1(5) . . . . ?
C13 C14 C15 C10 0.9(7) . . . . ?

_olex2_exptl_crystal_mounting_method loop
_olex2_submission_special_instructions 'No special instructions were received'

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_apx2054
_database_code_depnum_ccdc_archive 'CCDC 1836172'
loop_
_audit_author_name
_audit_author_address
'Nickolas Anderson'
;Los Alamos National Laboratory
United States of America
;
_audit_update_record             
;
2019-03-06 deposited with the CCDC.	2019-04-23 downloaded from the CCDC.
;
_audit_creation_date             2018-08-24
_audit_creation_method           
;
Olex2 1.2
(compiled Nov 22 2016 11:51:51 for OlexSys, GUI svn.r5269)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C72 H99 N7 U, 2.5(C7 H8)'
_chemical_formula_sum            'C89.50 H119 N7 U'
_chemical_formula_weight         1530.94
_chemical_absolute_configuration ?
_chemical_melting_point          ?
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'
U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   15.8483(16)
_cell_length_b                   20.707(2)
_cell_length_c                   26.010(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     8536.0(15)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3083
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      21.26
_cell_measurement_theta_min      2.28
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.947
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  .836
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   
'SADABS-2014/2 - Bruker AXS area detector scaling and absorption correction'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.191
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             3188
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.22
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0737
_diffrn_reflns_av_unetI/netI     0.0656
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            87023
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.718
_diffrn_reflns_theta_max         25.718
_diffrn_reflns_theta_min         1.798
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.834
_reflns_Friedel_fraction_full    0.994
_reflns_Friedel_fraction_max     0.994
_reflns_number_gt                14349
_reflns_number_total             16182
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 V.2014.7-1 (Bruker AXS, 2014)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.258
_refine_diff_density_min         -0.821
_refine_diff_density_rms         0.098
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.017(8)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     866
_refine_ls_number_reflns         16182
_refine_ls_number_restraints     132
_refine_ls_R_factor_all          0.0538
_refine_ls_R_factor_gt           0.0433
_refine_ls_restrained_S_all      1.028
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0542P)²+7.8120P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1024
_refine_ls_wR_factor_ref         0.1080
_refine_special_details          
'A small percentage of a racemic twin was accounted for with a TWIN law and BASF 0.017. A highly diordered toluene molecule in the lattice with partial occupancy was modeled and constrained.'
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.983(8) 0.017(8)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C3AA-C0AA
 2.5 with sigma of 0.01
 C4AA-C3AA
 2.5 with sigma of 0.01
 C1AA-C3AA
 1.53 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
C4AA \\sim C1AA \\sim C0AA \\sim C6AA \\sim C5AA \\sim C2AA \\sim C3AA: within
2A with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C4AA) \\sim Ueq, Uanis(C3AA) \\sim Ueq, Uanis(C1AA) \\sim Ueq,
Uanis(C0AA) \\sim Ueq, Uanis(C2AA) \\sim Ueq, Uanis(C6AA) \\sim Ueq,
Uanis(C5AA) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C81) = Uanis(C82) = Uanis(C83) = Uanis(C84) = Uanis(C85) = Uanis(C86) =
Uanis(C80) = Uanis(C73) = Uanis(C71) = Uanis(C72) = Uanis(C70)
5. Rigid body (RIGU) restrains
 C5AA, C0AA, C1AA, C6AA, C3AA, C4AA, C2AA
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
6. Others
 Fixed Sof: C3AA(0.5) H3AA(0.5) H3AB(0.5) H3AC(0.5) C4AA(0.5) H4AA(0.5)
 C2AA(0.5) H2AA(0.5) C5AA(0.5) H5AA(0.5) C6AA(0.5) H6AA(0.5) C0AA(0.5)
 H0AA(0.5) C1AA(0.5)
7.a Ternary CH refined with riding coordinates:
 C7(H7), C10(H10), C19(H19), C22(H22), C31(H31), C34(H34)
7.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C15(H15), C16(H16), C17(H17), C27(H27), C28(H28),
 C29(H29), C37(H37), C38(H38), C40(H40), C47(H47), C49(H49), C50(H50), C55(H55),
  C56(H56), C58(H58), C65(H65), C67(H67), C68(H68), C82(H82), C83(H83),
 C84(H84), C85(H85), C86(H86), C75(H75), C76(H76), C77(H77), C78(H78), C79(H79),
  C4AA(H4AA), C2AA(H2AA), C5AA(H5AA), C6AA(H6AA), C0AA(H0AA)
7.c Fitted hexagon refined as free rotating group:
 C4AA(C2AA,C5AA,C6AA,C0AA,C1AA)
7.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C),
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C35(H35A,H35B,H35C), C36(H36A,
 H36B,H36C), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C),
 C52(H52A,H52B,H52C), C53(H53A,H53B,H53C), C54(H54A,H54B,H54C), C61(H61A,H61B,
 H61C), C62(H62A,H62B,H62C), C63(H63A,H63B,H63C), C70(H70A,H70B,H70C), C71(H71A,
 H71B,H71C), C72(H72A,H72B,H72C), C80(H80A,H80B,H80C), C73(H73A,H73B,H73C),
 C3AA(H3AA,H3AB,H3AC)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 0.26349(2) 0.62106(2) 0.69065(2) 0.02277(9) Uani 1 1 d . . . . .
N1 N 0.3376(4) 0.5379(3) 0.6822(3) 0.0324(17) Uani 1 1 d . . . . .
N2 N 0.2635(5) 0.6759(3) 0.6104(2) 0.0305(15) Uani 1 1 d . . . . .
N3 N 0.1732(5) 0.6911(3) 0.7181(3) 0.0349(18) Uani 1 1 d . . . . .
N4 N 0.4076(4) 0.6846(3) 0.6994(2) 0.0242(15) Uani 1 1 d . . . . .
N5 N 0.3262(4) 0.6465(3) 0.7838(3) 0.0258(15) Uani 1 1 d . . . . .
N6 N 0.1254(4) 0.5718(3) 0.6465(2) 0.0236(15) Uani 1 1 d . . . . .
N7 N 0.1721(4) 0.5358(3) 0.7399(2) 0.0222(15) Uani 1 1 d . . . . .
C1 C 0.3754(6) 0.4790(4) 0.6698(3) 0.033(2) Uani 1 1 d . . . . .
C2 C 0.4626(6) 0.4701(5) 0.6756(4) 0.041(2) Uani 1 1 d . . . . .
C3 C 0.4992(7) 0.4128(6) 0.6612(5) 0.057(3) Uani 1 1 d . . . . .
H3 H 0.558751 0.408356 0.663548 0.068 Uiso 1 1 calc R . . . .
C4 C 0.4530(7) 0.3625(5) 0.6437(5) 0.057(3) Uani 1 1 d . . . . .
H4 H 0.479793 0.323141 0.634447 0.068 Uiso 1 1 calc R . . . .
C5 C 0.3682(6) 0.3685(5) 0.6396(4) 0.043(2) Uani 1 1 d . . . . .
H5 H 0.335638 0.332796 0.628083 0.051 Uiso 1 1 calc R . . . .
C6 C 0.3281(6) 0.4262(5) 0.6519(3) 0.036(2) Uani 1 1 d . . . . .
C7 C 0.2312(6) 0.4291(4) 0.6471(3) 0.034(2) Uani 1 1 d . . . . .
H7 H 0.214293 0.474682 0.654537 0.041 Uiso 1 1 calc R . . . .
C8 C 0.1991(7) 0.4136(5) 0.5934(4) 0.048(3) Uani 1 1 d . . . . .
H8A H 0.230191 0.439293 0.568095 0.072 Uiso 1 1 calc GR . . . .
H8B H 0.138838 0.423820 0.591236 0.072 Uiso 1 1 calc GR . . . .
H8C H 0.207559 0.367534 0.586308 0.072 Uiso 1 1 calc GR . . . .
C9 C 0.1873(6) 0.3867(4) 0.6869(4) 0.041(2) Uani 1 1 d . . . . .
H9A H 0.197263 0.341154 0.678788 0.062 Uiso 1 1 calc GR . . . .
H9B H 0.126539 0.395465 0.686470 0.062 Uiso 1 1 calc GR . . . .
H9C H 0.209930 0.396346 0.721159 0.062 Uiso 1 1 calc GR . . . .
C10 C 0.5152(7) 0.5245(5) 0.6993(5) 0.055(3) Uani 1 1 d . . . . .
H10 H 0.488523 0.566368 0.688990 0.066 Uiso 1 1 calc R . . . .
C11 C 0.6068(7) 0.5270(6) 0.6830(6) 0.076(4) Uani 1 1 d . . . . .
H11A H 0.635813 0.488011 0.694842 0.113 Uiso 1 1 calc GR . . . .
H11B H 0.633759 0.565172 0.698062 0.113 Uiso 1 1 calc GR . . . .
H11C H 0.610143 0.529570 0.645382 0.113 Uiso 1 1 calc GR . . . .
C12 C 0.5091(9) 0.5194(6) 0.7581(5) 0.063(3) Uani 1 1 d . . . . .
H12A H 0.449664 0.517378 0.768295 0.095 Uiso 1 1 calc GR . . . .
H12B H 0.535678 0.557268 0.773799 0.095 Uiso 1 1 calc GR . . . .
H12C H 0.538155 0.480188 0.769602 0.095 Uiso 1 1 calc GR . . . .
C13 C 0.2922(5) 0.6923(4) 0.5619(3) 0.0276(19) Uani 1 1 d . . . . .
C14 C 0.3573(6) 0.6570(4) 0.5375(3) 0.033(2) Uani 1 1 d . . . . .
C15 C 0.3840(6) 0.6751(5) 0.4889(3) 0.040(2) Uani 1 1 d . . . . .
H15 H 0.427722 0.650858 0.473080 0.048 Uiso 1 1 calc R . . . .
C16 C 0.3502(7) 0.7268(5) 0.4621(4) 0.051(3) Uani 1 1 d . . . . .
H16 H 0.368904 0.737671 0.428520 0.061 Uiso 1 1 calc R . . . .
C17 C 0.2879(6) 0.7618(4) 0.4867(3) 0.037(2) Uani 1 1 d . . . . .
H17 H 0.264411 0.797994 0.469415 0.044 Uiso 1 1 calc R . . . .
C18 C 0.2580(5) 0.7467(4) 0.5353(3) 0.0307(18) Uani 1 1 d . . . . .
C19 C 0.1917(6) 0.7886(5) 0.5607(4) 0.044(3) Uani 1 1 d . . . . .
H19 H 0.206175 0.790633 0.598097 0.052 Uiso 1 1 calc R . . . .
C20 C 0.1053(8) 0.7624(7) 0.5572(6) 0.083(4) Uani 1 1 d . . . . .
H20A H 0.086868 0.762712 0.521197 0.124 Uiso 1 1 calc GR . . . .
H20B H 0.066967 0.789108 0.577739 0.124 Uiso 1 1 calc GR . . . .
H20C H 0.104582 0.718012 0.570214 0.124 Uiso 1 1 calc GR . . . .
C21 C 0.1896(9) 0.8597(6) 0.5407(5) 0.086(5) Uani 1 1 d . . . . .
H21A H 0.247071 0.877135 0.539960 0.129 Uiso 1 1 calc GR . . . .
H21B H 0.154612 0.886041 0.563655 0.129 Uiso 1 1 calc GR . . . .
H21C H 0.165737 0.860624 0.505948 0.129 Uiso 1 1 calc GR . . . .
C22 C 0.3950(6) 0.5971(5) 0.5631(3) 0.037(2) Uani 1 1 d . . . . .
H22 H 0.383758 0.600525 0.600842 0.045 Uiso 1 1 calc R . . . .
C23 C 0.4896(7) 0.5904(6) 0.5562(4) 0.058(3) Uani 1 1 d . . . . .
H23A H 0.502061 0.579450 0.520333 0.087 Uiso 1 1 calc GR . . . .
H23B H 0.510728 0.556040 0.578731 0.087 Uiso 1 1 calc GR . . . .
H23C H 0.517142 0.631234 0.565071 0.087 Uiso 1 1 calc GR . . . .
C24 C 0.3523(8) 0.5368(5) 0.5442(4) 0.055(3) Uani 1 1 d . . . . .
H24A H 0.362360 0.531887 0.507259 0.082 Uiso 1 1 calc GR . . . .
H24B H 0.291448 0.539946 0.550589 0.082 Uiso 1 1 calc GR . . . .
H24C H 0.375060 0.499280 0.562503 0.082 Uiso 1 1 calc GR . . . .
C25 C 0.1329(6) 0.7390(4) 0.7467(3) 0.030(2) Uani 1 1 d . . . . .
C26 C 0.0451(6) 0.7345(4) 0.7596(4) 0.039(2) Uani 1 1 d . . . . .
C27 C 0.0082(6) 0.7828(5) 0.7876(4) 0.047(3) Uani 1 1 d . . . . .
H27 H -0.050048 0.779482 0.795898 0.057 Uiso 1 1 calc R . . . .
C28 C 0.0528(6) 0.8364(4) 0.8044(4) 0.044(2) Uani 1 1 d . . . . .
H28 H 0.025766 0.869426 0.823606 0.052 Uiso 1 1 calc R . . . .
C29 C 0.1373(5) 0.8405(4) 0.7924(3) 0.032(2) Uani 1 1 d . . . . .
H29 H 0.168174 0.876994 0.804051 0.038 Uiso 1 1 calc R . . . .
C30 C 0.1790(5) 0.7938(4) 0.7642(3) 0.0263(18) Uani 1 1 d . . . . .
C31 C -0.0043(7) 0.6771(5) 0.7408(6) 0.064(4) Uani 1 1 d . . . . .
H31 H 0.036930 0.640881 0.737055 0.077 Uiso 1 1 calc R . . . .
C32 C -0.0719(8) 0.6541(6) 0.7798(7) 0.096(6) Uani 1 1 d . . . . .
H32A H -0.044220 0.639417 0.811356 0.144 Uiso 1 1 calc GR . . . .
H32B H -0.104178 0.618373 0.764770 0.144 Uiso 1 1 calc GR . . . .
H32C H -0.110142 0.689908 0.787768 0.144 Uiso 1 1 calc GR . . . .
C33 C -0.0416(8) 0.6887(6) 0.6883(6) 0.087(5) Uani 1 1 d . . . . .
H33A H -0.084896 0.722333 0.690495 0.131 Uiso 1 1 calc GR . . . .
H33B H -0.067110 0.648606 0.675566 0.131 Uiso 1 1 calc GR . . . .
H33C H 0.002965 0.702518 0.664596 0.131 Uiso 1 1 calc GR . . . .
C34 C 0.2705(6) 0.8017(4) 0.7519(3) 0.035(2) Uani 1 1 d . . . . .
H34 H 0.290082 0.760884 0.735209 0.042 Uiso 1 1 calc R . . . .
C35 C 0.2869(8) 0.8571(6) 0.7140(5) 0.080(4) Uani 1 1 d . . . . .
H35A H 0.259561 0.847450 0.681096 0.120 Uiso 1 1 calc GR . . . .
H35B H 0.347774 0.861990 0.708711 0.120 Uiso 1 1 calc GR . . . .
H35C H 0.263757 0.897352 0.728008 0.120 Uiso 1 1 calc GR . . . .
C36 C 0.3236(6) 0.8114(5) 0.8010(5) 0.053(3) Uani 1 1 d . . . . .
H36A H 0.307309 0.852041 0.817592 0.079 Uiso 1 1 calc GR . . . .
H36B H 0.383562 0.813030 0.791856 0.079 Uiso 1 1 calc GR . . . .
H36C H 0.313673 0.775423 0.824655 0.079 Uiso 1 1 calc GR . . . .
C37 C 0.4436(6) 0.7106(5) 0.6576(3) 0.033(2) Uani 1 1 d . . . . .
H37 H 0.411907 0.712425 0.626659 0.040 Uiso 1 1 calc R . . . .
C38 C 0.5249(6) 0.7349(5) 0.6575(3) 0.036(2) Uani 1 1 d . . . . .
H38 H 0.547832 0.752114 0.626693 0.043 Uiso 1 1 calc R . . . .
C39 C 0.5727(5) 0.7345(4) 0.7015(3) 0.0284(19) Uani 1 1 d . . . . .
C40 C 0.5351(6) 0.7083(5) 0.7452(3) 0.034(2) Uani 1 1 d . . . . .
H40 H 0.565971 0.706120 0.776439 0.041 Uiso 1 1 calc R . . . .
C41 C 0.4534(5) 0.6854(4) 0.7435(3) 0.0252(19) Uani 1 1 d . . . . .
C42 C 0.6614(6) 0.7640(6) 0.7023(4) 0.048(3) Uani 1 1 d . . . . .
C43 C 0.7122(6) 0.7414(5) 0.7483(4) 0.046(3) Uani 1 1 d . . . . .
H43A H 0.686095 0.757579 0.779945 0.070 Uiso 1 1 calc GR . . . .
H43B H 0.769968 0.757959 0.745684 0.070 Uiso 1 1 calc GR . . . .
H43C H 0.713345 0.694106 0.749019 0.070 Uiso 1 1 calc GR . . . .
C44 C 0.6510(7) 0.8376(6) 0.7046(5) 0.073(4) Uani 1 1 d . . . . .
H44A H 0.618385 0.852221 0.674735 0.109 Uiso 1 1 calc GR . . . .
H44B H 0.706692 0.858110 0.704205 0.109 Uiso 1 1 calc GR . . . .
H44C H 0.621185 0.849460 0.736200 0.109 Uiso 1 1 calc GR . . . .
C45 C 0.7090(7) 0.7432(9) 0.6528(5) 0.093(6) Uani 1 1 d . . . . .
H45A H 0.713209 0.696034 0.651642 0.139 Uiso 1 1 calc GR . . . .
H45B H 0.765801 0.761989 0.652883 0.139 Uiso 1 1 calc GR . . . .
H45C H 0.678117 0.758568 0.622490 0.139 Uiso 1 1 calc GR . . . .
C46 C 0.4076(6) 0.6638(4) 0.7898(3) 0.029(2) Uani 1 1 d . . . . .
C47 C 0.4444(6) 0.6672(4) 0.8384(3) 0.033(2) Uani 1 1 d . . . . .
H47 H 0.502751 0.677193 0.841298 0.040 Uiso 1 1 calc R . . . .
C48 C 0.3976(6) 0.6562(5) 0.8827(3) 0.036(2) Uani 1 1 d . . . . .
C49 C 0.3115(5) 0.6437(4) 0.8751(3) 0.033(2) Uani 1 1 d . . . . .
H49 H 0.275021 0.638624 0.903816 0.039 Uiso 1 1 calc R . . . .
C50 C 0.2804(5) 0.6390(4) 0.8262(3) 0.0264(18) Uani 1 1 d . . . . .
H50 H 0.222105 0.629662 0.822309 0.032 Uiso 1 1 calc R . . . .
C51 C 0.4352(7) 0.6630(6) 0.9366(4) 0.054(3) Uani 1 1 d . . . . .
C52 C 0.4114(10) 0.7297(8) 0.9568(5) 0.090(5) Uani 1 1 d . . . . .
H52A H 0.435706 0.762877 0.934377 0.135 Uiso 1 1 calc GR . . . .
H52B H 0.433430 0.735014 0.991749 0.135 Uiso 1 1 calc GR . . . .
H52C H 0.349847 0.734060 0.957233 0.135 Uiso 1 1 calc GR . . . .
C53 C 0.5320(7) 0.6542(7) 0.9352(4) 0.074(4) Uani 1 1 d . . . . .
H53A H 0.546030 0.615583 0.915181 0.111 Uiso 1 1 calc GR . . . .
H53B H 0.553426 0.649427 0.970311 0.111 Uiso 1 1 calc GR . . . .
H53C H 0.557961 0.692165 0.919122 0.111 Uiso 1 1 calc GR . . . .
C54 C 0.4001(7) 0.6091(9) 0.9711(4) 0.083(5) Uani 1 1 d . . . . .
H54A H 0.340852 0.618087 0.979105 0.125 Uiso 1 1 calc GR . . . .
H54B H 0.432797 0.607138 1.003001 0.125 Uiso 1 1 calc GR . . . .
H54C H 0.404274 0.567624 0.953062 0.125 Uiso 1 1 calc GR . . . .
C55 C 0.1070(6) 0.5845(4) 0.5967(3) 0.032(2) Uani 1 1 d . . . . .
H55 H 0.147783 0.606153 0.576250 0.038 Uiso 1 1 calc R . . . .
C56 C 0.0313(5) 0.5671(4) 0.5746(3) 0.0294(19) Uani 1 1 d . . . . .
H56 H 0.021462 0.576753 0.539392 0.035 Uiso 1 1 calc R . . . .
C57 C -0.0302(5) 0.5361(4) 0.6026(3) 0.0253(18) Uani 1 1 d . . . . .
C58 C -0.0096(5) 0.5216(4) 0.6532(3) 0.0250(18) Uani 1 1 d . . . . .
H58 H -0.049177 0.499006 0.673911 0.030 Uiso 1 1 calc R . . . .
C59 C 0.0677(5) 0.5396(4) 0.6743(3) 0.0228(18) Uani 1 1 d . . . . .
C60 C -0.1151(6) 0.5189(4) 0.5786(3) 0.035(2) Uani 1 1 d . . . . .
C61 C -0.0995(9) 0.4805(7) 0.5307(5) 0.078(4) Uani 1 1 d . . . . .
H61A H -0.055239 0.501400 0.510283 0.117 Uiso 1 1 calc GR . . . .
H61B H -0.151548 0.478172 0.510449 0.117 Uiso 1 1 calc GR . . . .
H61C H -0.081421 0.436756 0.539989 0.117 Uiso 1 1 calc GR . . . .
C62 C -0.1720(7) 0.4822(6) 0.6148(4) 0.057(3) Uani 1 1 d . . . . .
H62A H -0.148184 0.439271 0.621234 0.086 Uiso 1 1 calc GR . . . .
H62B H -0.228072 0.477714 0.599337 0.086 Uiso 1 1 calc GR . . . .
H62C H -0.176691 0.505743 0.647374 0.086 Uiso 1 1 calc GR . . . .
C63 C -0.1591(8) 0.5830(6) 0.5646(6) 0.077(4) Uani 1 1 d . . . . .
H63A H -0.169411 0.607976 0.595965 0.115 Uiso 1 1 calc GR . . . .
H63B H -0.212887 0.573765 0.547570 0.115 Uiso 1 1 calc GR . . . .
H63C H -0.122837 0.607858 0.541373 0.115 Uiso 1 1 calc GR . . . .
C64 C 0.0922(5) 0.5221(4) 0.7273(3) 0.0227(18) Uani 1 1 d . . . . .
C65 C 0.0396(6) 0.4878(4) 0.7598(3) 0.028(2) Uani 1 1 d . . . . .
H65 H -0.016827 0.478693 0.749787 0.034 Uiso 1 1 calc R . . . .
C66 C 0.0697(6) 0.4665(4) 0.8076(4) 0.037(2) Uani 1 1 d . . . . .
C67 C 0.1529(6) 0.4771(4) 0.8181(3) 0.032(2) Uani 1 1 d . . . . .
H67 H 0.176865 0.460585 0.848931 0.039 Uiso 1 1 calc R . . . .
C68 C 0.2022(6) 0.5114(4) 0.7846(3) 0.0283(19) Uani 1 1 d . . . . .
H68 H 0.259793 0.518411 0.792971 0.034 Uiso 1 1 calc R . . . .
C69 C 0.0126(8) 0.4295(6) 0.8446(4) 0.059(3) Uani 1 1 d . . . . .
C70 C -0.0763(10) 0.4261(8) 0.8266(5) 0.0911(16) Uani 1 1 d . . . . .
H70A H -0.102299 0.468890 0.829202 0.137 Uiso 1 1 calc GR . . . .
H70B H -0.107768 0.395383 0.847906 0.137 Uiso 1 1 calc GR . . . .
H70C H -0.077471 0.411711 0.790672 0.137 Uiso 1 1 calc GR . . . .
C71 C 0.0517(10) 0.3587(7) 0.8467(5) 0.0911(16) Uani 1 1 d . . . . .
H71A H 0.050347 0.339515 0.812294 0.137 Uiso 1 1 calc GR . . . .
H71B H 0.018738 0.331955 0.870418 0.137 Uiso 1 1 calc GR . . . .
H71C H 0.110272 0.361104 0.858737 0.137 Uiso 1 1 calc GR . . . .
C72 C 0.0187(10) 0.4621(8) 0.8978(5) 0.0911(16) Uani 1 1 d . . . . .
H72A H 0.077994 0.470520 0.906068 0.137 Uiso 1 1 calc GR . . . .
H72B H -0.005690 0.433591 0.923993 0.137 Uiso 1 1 calc GR . . . .
H72C H -0.012483 0.503007 0.897265 0.137 Uiso 1 1 calc GR . . . .
C80 C 0.1881(10) 0.5683(7) 0.4333(5) 0.0911(16) Uani 1 1 d . . . . .
H80A H 0.194172 0.546793 0.466682 0.137 Uiso 1 1 calc GR . . . .
H80B H 0.227469 0.604730 0.431377 0.137 Uiso 1 1 calc GR . . . .
H80C H 0.200463 0.537601 0.405712 0.137 Uiso 1 1 calc GR . . . .
C81 C 0.0961(11) 0.5936(8) 0.4274(6) 0.0911(16) Uani 1 1 d . . . . .
C82 C 0.0420(11) 0.5572(8) 0.3985(5) 0.0911(16) Uani 1 1 d . . . . .
H82 H 0.059581 0.517716 0.383282 0.109 Uiso 1 1 calc R . . . .
C83 C -0.0427(11) 0.5811(8) 0.3920(6) 0.0911(16) Uani 1 1 d . . . . .
H83 H -0.080353 0.559910 0.369047 0.109 Uiso 1 1 calc R . . . .
C84 C -0.0673(10) 0.6310(8) 0.4172(5) 0.0911(16) Uani 1 1 d . . . . .
H84 H -0.124151 0.644849 0.413686 0.109 Uiso 1 1 calc R . . . .
C85 C -0.0109(11) 0.6672(8) 0.4511(5) 0.0911(16) Uani 1 1 d . . . . .
H85 H -0.029449 0.703505 0.470398 0.109 Uiso 1 1 calc R . . . .
C86 C 0.0758(11) 0.6435(8) 0.4533(6) 0.0911(16) Uani 1 1 d . . . . .
H86 H 0.116699 0.665154 0.473723 0.109 Uiso 1 1 calc R . . . .
C73 C 0.1798(10) 0.8070(7) 0.9373(5) 0.0911(16) Uani 1 1 d . . . . .
H73A H 0.195913 0.823584 0.971175 0.137 Uiso 1 1 calc GR . . . .
H73B H 0.135453 0.834409 0.922655 0.137 Uiso 1 1 calc GR . . . .
H73C H 0.229054 0.807269 0.914526 0.137 Uiso 1 1 calc GR . . . .
C74 C 0.1480(9) 0.7402(5) 0.9426(5) 0.066(4) Uani 1 1 d . . . . .
C75 C 0.1606(9) 0.7091(6) 0.9907(4) 0.064(3) Uani 1 1 d . . . . .
H75 H 0.187588 0.730542 1.018473 0.077 Uiso 1 1 calc R . . . .
C76 C 0.1321(8) 0.6463(6) 0.9955(5) 0.066(3) Uani 1 1 d . . . . .
H76 H 0.137064 0.624852 1.027628 0.079 Uiso 1 1 calc R . . . .
C77 C 0.0975(7) 0.6150(8) 0.9555(5) 0.068(3) Uani 1 1 d . . . . .
H77 H 0.081295 0.571118 0.959350 0.082 Uiso 1 1 calc R . . . .
C78 C 0.0851(8) 0.6456(6) 0.9091(5) 0.064(3) Uani 1 1 d . . . . .
H78 H 0.058385 0.623393 0.881540 0.076 Uiso 1 1 calc R . . . .
C79 C 0.1111(8) 0.7069(7) 0.9028(5) 0.062(3) Uani 1 1 d . . . . .
H79 H 0.103735 0.727465 0.870504 0.074 Uiso 1 1 calc R . . . .
C3AA C -0.1262(17) 0.5694(13) 0.9999(8) 0.106(7) Uani 0.5 1 d D U P . .
H3AA H -0.066102 0.564768 0.991808 0.159 Uiso 0.5 1 calc GR . P . .
H3AB H -0.147543 0.528751 1.014191 0.159 Uiso 0.5 1 calc GR . P . .
H3AC H -0.133748 0.604077 1.025085 0.159 Uiso 0.5 1 calc GR . P . .
C4AA C -0.1753(12) 0.6484(8) 0.9335(8) 0.102(6) Uani 0.5 1 d D U P . .
H4AA H -0.145078 0.681367 0.950938 0.122 Uiso 0.5 1 calc R . P . .
C2AA C -0.2211(13) 0.6632(8) 0.8894(8) 0.102(6) Uani 0.5 1 d G U P . .
H2AA H -0.222092 0.706201 0.876771 0.123 Uiso 0.5 1 calc R . P . .
C5AA C -0.2653(12) 0.6149(11) 0.8638(6) 0.110(6) Uani 0.5 1 d G U P . .
H5AA H -0.296590 0.625013 0.833697 0.133 Uiso 0.5 1 calc R . P . .
C6AA C -0.2638(12) 0.5520(10) 0.8823(7) 0.109(6) Uani 0.5 1 d G U P . .
H6AA H -0.294073 0.518991 0.864789 0.131 Uiso 0.5 1 calc R . P . .
C0AA C -0.2181(12) 0.5372(7) 0.9263(7) 0.091(6) Uani 0.5 1 d DG U P . .
H0AA H -0.217060 0.494156 0.938956 0.110 Uiso 0.5 1 calc R . P . .
C1AA C -0.1738(11) 0.5854(9) 0.9519(6) 0.096(5) Uani 0.5 1 d DG U P . .


_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 2.097(7) . ?
U1 N2 2.376(6) . ?
U1 N3 2.159(8) . ?
U1 N4 2.646(6) . ?
U1 N5 2.670(7) . ?
U1 N6 2.674(7) . ?
U1 N7 2.618(6) . ?
N1 C1 1.395(11) . ?
N2 C13 1.384(10) . ?
N3 C25 1.395(11) . ?
N4 C37 1.341(10) . ?
N4 C41 1.356(10) . ?
N5 C46 1.348(11) . ?
N5 C50 1.331(9) . ?
N6 C55 1.354(10) . ?
N6 C59 1.343(10) . ?
N7 C64 1.338(11) . ?
N7 C68 1.353(10) . ?
C1 C2 1.403(13) . ?
C1 C6 1.405(13) . ?
C2 C3 1.374(14) . ?
C2 C10 1.531(15) . ?
C3 H3 0.9500 . ?
C3 C4 1.352(16) . ?
C4 H4 0.9500 . ?
C4 C5 1.353(14) . ?
C5 H5 0.9500 . ?
C5 C6 1.390(12) . ?
C6 C7 1.542(14) . ?
C7 H7 1.0000 . ?
C7 C8 1.520(12) . ?
C7 C9 1.526(12) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10 1.0000 . ?
C10 C11 1.514(16) . ?
C10 C12 1.536(17) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C14 1.415(12) . ?
C13 C18 1.428(11) . ?
C14 C15 1.384(12) . ?
C14 C22 1.531(12) . ?
C15 H15 0.9500 . ?
C15 C16 1.384(13) . ?
C16 H16 0.9500 . ?
C16 C17 1.381(13) . ?
C17 H17 0.9500 . ?
C17 C18 1.387(11) . ?
C18 C19 1.514(12) . ?
C19 H19 1.0000 . ?
C19 C20 1.476(16) . ?
C19 C21 1.562(15) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22 1.0000 . ?
C22 C23 1.516(13) . ?
C22 C24 1.503(14) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 C26 1.435(14) . ?
C25 C30 1.423(12) . ?
C26 C27 1.368(14) . ?
C26 C31 1.504(13) . ?
C27 H27 0.9500 . ?
C27 C28 1.385(13) . ?
C28 H28 0.9500 . ?
C28 C29 1.377(13) . ?
C29 H29 0.9500 . ?
C29 C30 1.383(11) . ?
C30 C34 1.495(13) . ?
C31 H31 1.0000 . ?
C31 C32 1.55(2) . ?
C31 C33 1.509(18) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 H34 1.0000 . ?
C34 C35 1.535(13) . ?
C34 C36 1.542(13) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37 0.9500 . ?
C37 C38 1.382(13) . ?
C38 H38 0.9500 . ?
C38 C39 1.373(11) . ?
C39 C40 1.393(12) . ?
C39 C42 1.532(12) . ?
C40 H40 0.9500 . ?
C40 C41 1.380(12) . ?
C41 C46 1.477(11) . ?
C42 C43 1.516(12) . ?
C42 C44 1.534(16) . ?
C42 C45 1.554(15) . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C46 C47 1.393(12) . ?
C47 H47 0.9500 . ?
C47 C48 1.390(12) . ?
C48 C49 1.402(12) . ?
C48 C51 1.530(13) . ?
C49 H49 0.9500 . ?
C49 C50 1.368(11) . ?
C50 H50 0.9500 . ?
C51 C52 1.526(18) . ?
C51 C53 1.546(15) . ?
C51 C54 1.535(16) . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
C55 H55 0.9500 . ?
C55 C56 1.378(12) . ?
C56 H56 0.9500 . ?
C56 C57 1.375(12) . ?
C57 C58 1.390(11) . ?
C57 C60 1.525(12) . ?
C58 H58 0.9500 . ?
C58 C59 1.393(12) . ?
C59 C64 1.479(11) . ?
C60 C61 1.500(15) . ?
C60 C62 1.510(14) . ?
C60 C63 1.541(14) . ?
C61 H61A 0.9800 . ?
C61 H61B 0.9800 . ?
C61 H61C 0.9800 . ?
C62 H62A 0.9800 . ?
C62 H62B 0.9800 . ?
C62 H62C 0.9800 . ?
C63 H63A 0.9800 . ?
C63 H63B 0.9800 . ?
C63 H63C 0.9800 . ?
C64 C65 1.384(12) . ?
C65 H65 0.9500 . ?
C65 C66 1.402(12) . ?
C66 C67 1.366(13) . ?
C66 C69 1.528(13) . ?
C67 H67 0.9500 . ?
C67 C68 1.370(12) . ?
C68 H68 0.9500 . ?
C69 C70 1.487(18) . ?
C69 C71 1.592(19) . ?
C69 C72 1.543(18) . ?
C70 H70A 0.9800 . ?
C70 H70B 0.9800 . ?
C70 H70C 0.9800 . ?
C71 H71A 0.9800 . ?
C71 H71B 0.9800 . ?
C71 H71C 0.9800 . ?
C72 H72A 0.9800 . ?
C72 H72B 0.9800 . ?
C72 H72C 0.9800 . ?
C80 H80A 0.9800 . ?
C80 H80B 0.9800 . ?
C80 H80C 0.9800 . ?
C80 C81 1.56(2) . ?
C81 C82 1.37(2) . ?
C81 C86 1.28(2) . ?
C82 H82 0.9500 . ?
C82 C83 1.44(2) . ?
C83 H83 0.9500 . ?
C83 C84 1.28(2) . ?
C84 H84 0.9500 . ?
C84 C85 1.46(2) . ?
C85 H85 0.9500 . ?
C85 C86 1.46(2) . ?
C86 H86 0.9500 . ?
C73 H73A 0.9800 . ?
C73 H73B 0.9800 . ?
C73 H73C 0.9800 . ?
C73 C74 1.478(18) . ?
C74 C75 1.423(16) . ?
C74 C79 1.373(18) . ?
C75 H75 0.9500 . ?
C75 C76 1.382(17) . ?
C76 H76 0.9500 . ?
C76 C77 1.340(17) . ?
C77 H77 0.9500 . ?
C77 C78 1.379(17) . ?
C78 H78 0.9500 . ?
C78 C79 1.344(17) . ?
C79 H79 0.9500 . ?
C3AA H3AA 0.9800 . ?
C3AA H3AB 0.9800 . ?
C3AA H3AC 0.9800 . ?
C3AA C1AA 1.496(9) . ?
C4AA H4AA 0.9500 . ?
C4AA C2AA 1.3900 . ?
C4AA C1AA 1.3900 . ?
C2AA H2AA 0.9500 . ?
C2AA C5AA 1.3900 . ?
C5AA H5AA 0.9500 . ?
C5AA C6AA 1.3900 . ?
C6AA H6AA 0.9500 . ?
C6AA C0AA 1.3900 . ?
C0AA H0AA 0.9500 . ?
C0AA C1AA 1.3900 . ?

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 107.5(3) . . ?
N1 U1 N3 163.3(3) . . ?
N1 U1 N4 86.2(2) . . ?
N1 U1 N5 92.8(2) . . ?
N1 U1 N6 95.7(2) . . ?
N1 U1 N7 78.9(2) . . ?
N2 U1 N4 80.7(2) . . ?
N2 U1 N5 134.6(2) . . ?
N2 U1 N6 78.8(2) . . ?
N2 U1 N7 138.8(2) . . ?
N3 U1 N2 88.3(2) . . ?
N3 U1 N4 102.1(3) . . ?
N3 U1 N5 79.3(2) . . ?
N3 U1 N6 81.7(3) . . ?
N3 U1 N7 85.6(2) . . ?
N4 U1 N5 60.13(19) . . ?
N4 U1 N6 158.99(19) . . ?
N5 U1 N6 140.3(2) . . ?
N7 U1 N4 140.4(2) . . ?
N7 U1 N5 84.0(2) . . ?
N7 U1 N6 60.0(2) . . ?
C1 N1 U1 169.1(6) . . ?
C13 N2 U1 156.7(6) . . ?
C25 N3 U1 163.3(6) . . ?
C37 N4 U1 119.8(5) . . ?
C37 N4 C41 116.9(7) . . ?
C41 N4 U1 122.7(5) . . ?
C46 N5 U1 121.0(5) . . ?
C50 N5 U1 121.8(5) . . ?
C50 N5 C46 117.1(7) . . ?
C55 N6 U1 120.8(6) . . ?
C59 N6 U1 121.1(5) . . ?
C59 N6 C55 117.7(7) . . ?
C64 N7 U1 123.2(5) . . ?
C64 N7 C68 117.6(7) . . ?
C68 N7 U1 118.5(5) . . ?
N1 C1 C2 120.8(9) . . ?
N1 C1 C6 121.9(8) . . ?
C2 C1 C6 117.3(9) . . ?
C1 C2 C10 118.9(9) . . ?
C3 C2 C1 120.1(10) . . ?
C3 C2 C10 121.0(9) . . ?
C2 C3 H3 119.1 . . ?
C4 C3 C2 121.9(10) . . ?
C4 C3 H3 119.1 . . ?
C3 C4 H4 120.2 . . ?
C3 C4 C5 119.6(9) . . ?
C5 C4 H4 120.2 . . ?
C4 C5 H5 119.5 . . ?
C4 C5 C6 121.0(10) . . ?
C6 C5 H5 119.5 . . ?
C1 C6 C7 121.8(8) . . ?
C5 C6 C1 120.1(9) . . ?
C5 C6 C7 118.1(9) . . ?
C6 C7 H7 106.8 . . ?
C8 C7 C6 113.5(8) . . ?
C8 C7 H7 106.8 . . ?
C8 C7 C9 110.4(8) . . ?
C9 C7 C6 112.1(8) . . ?
C9 C7 H7 106.8 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C2 C10 H10 107.5 . . ?
C2 C10 C12 108.4(9) . . ?
C11 C10 C2 115.8(11) . . ?
C11 C10 H10 107.5 . . ?
C11 C10 C12 110.0(10) . . ?
C12 C10 H10 107.5 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N2 C13 C14 121.5(7) . . ?
N2 C13 C18 120.6(7) . . ?
C14 C13 C18 117.8(7) . . ?
C13 C14 C22 120.5(7) . . ?
C15 C14 C13 119.5(8) . . ?
C15 C14 C22 119.9(8) . . ?
C14 C15 H15 118.3 . . ?
C14 C15 C16 123.4(9) . . ?
C16 C15 H15 118.3 . . ?
C15 C16 H16 121.6 . . ?
C17 C16 C15 116.7(9) . . ?
C17 C16 H16 121.6 . . ?
C16 C17 H17 118.4 . . ?
C16 C17 C18 123.2(8) . . ?
C18 C17 H17 118.4 . . ?
C13 C18 C19 120.3(7) . . ?
C17 C18 C13 119.3(8) . . ?
C17 C18 C19 120.4(7) . . ?
C18 C19 H19 106.8 . . ?
C18 C19 C21 114.2(8) . . ?
C20 C19 C18 113.9(10) . . ?
C20 C19 H19 106.8 . . ?
C20 C19 C21 107.8(10) . . ?
C21 C19 H19 106.8 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C14 C22 H22 107.4 . . ?
C23 C22 C14 114.1(8) . . ?
C23 C22 H22 107.4 . . ?
C24 C22 C14 110.8(8) . . ?
C24 C22 H22 107.4 . . ?
C24 C22 C23 109.3(9) . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
N3 C25 C26 121.5(8) . . ?
N3 C25 C30 120.2(8) . . ?
C30 C25 C26 118.3(8) . . ?
C25 C26 C31 118.7(9) . . ?
C27 C26 C25 119.5(8) . . ?
C27 C26 C31 121.9(10) . . ?
C26 C27 H27 118.9 . . ?
C26 C27 C28 122.3(9) . . ?
C28 C27 H27 118.9 . . ?
C27 C28 H28 120.8 . . ?
C29 C28 C27 118.4(9) . . ?
C29 C28 H28 120.8 . . ?
C28 C29 H29 118.6 . . ?
C28 C29 C30 122.7(8) . . ?
C30 C29 H29 118.6 . . ?
C25 C30 C34 121.2(8) . . ?
C29 C30 C25 118.8(8) . . ?
C29 C30 C34 120.0(8) . . ?
C26 C31 H31 106.6 . . ?
C26 C31 C32 113.0(11) . . ?
C26 C31 C33 111.9(10) . . ?
C32 C31 H31 106.6 . . ?
C33 C31 H31 106.6 . . ?
C33 C31 C32 111.7(11) . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C31 C33 H33A 109.5 . . ?
C31 C33 H33B 109.5 . . ?
C31 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C30 C34 H34 107.5 . . ?
C30 C34 C35 112.6(8) . . ?
C30 C34 C36 111.5(8) . . ?
C35 C34 H34 107.5 . . ?
C35 C34 C36 110.0(9) . . ?
C36 C34 H34 107.5 . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C34 C36 H36A 109.5 . . ?
C34 C36 H36B 109.5 . . ?
C34 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
N4 C37 H37 118.5 . . ?
N4 C37 C38 123.0(8) . . ?
C38 C37 H37 118.5 . . ?
C37 C38 H38 119.6 . . ?
C39 C38 C37 120.7(8) . . ?
C39 C38 H38 119.6 . . ?
C38 C39 C40 116.4(8) . . ?
C38 C39 C42 121.0(7) . . ?
C40 C39 C42 122.5(8) . . ?
C39 C40 H40 119.7 . . ?
C41 C40 C39 120.6(8) . . ?
C41 C40 H40 119.7 . . ?
N4 C41 C40 122.3(8) . . ?
N4 C41 C46 115.1(7) . . ?
C40 C41 C46 122.6(8) . . ?
C39 C42 C44 107.3(8) . . ?
C39 C42 C45 108.9(9) . . ?
C43 C42 C39 112.0(7) . . ?
C43 C42 C44 109.5(9) . . ?
C43 C42 C45 108.1(9) . . ?
C44 C42 C45 111.1(10) . . ?
C42 C43 H43A 109.5 . . ?
C42 C43 H43B 109.5 . . ?
C42 C43 H43C 109.5 . . ?
H43A C43 H43B 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C42 C44 H44A 109.5 . . ?
C42 C44 H44B 109.5 . . ?
C42 C44 H44C 109.5 . . ?
H44A C44 H44B 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C42 C45 H45A 109.5 . . ?
C42 C45 H45B 109.5 . . ?
C42 C45 H45C 109.5 . . ?
H45A C45 H45B 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
N5 C46 C41 117.0(7) . . ?
N5 C46 C47 121.4(8) . . ?
C47 C46 C41 121.3(8) . . ?
C46 C47 H47 119.3 . . ?
C48 C47 C46 121.3(8) . . ?
C48 C47 H47 119.3 . . ?
C47 C48 C49 115.7(8) . . ?
C47 C48 C51 122.5(8) . . ?
C49 C48 C51 121.6(8) . . ?
C48 C49 H49 120.2 . . ?
C50 C49 C48 119.6(8) . . ?
C50 C49 H49 120.2 . . ?
N5 C50 C49 124.5(7) . . ?
N5 C50 H50 117.7 . . ?
C49 C50 H50 117.7 . . ?
C48 C51 C53 110.7(9) . . ?
C48 C51 C54 109.1(9) . . ?
C52 C51 C48 107.6(10) . . ?
C52 C51 C53 111.0(11) . . ?
C52 C51 C54 111.6(11) . . ?
C54 C51 C53 106.8(10) . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52B 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C51 C53 H53A 109.5 . . ?
C51 C53 H53B 109.5 . . ?
C51 C53 H53C 109.5 . . ?
H53A C53 H53B 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C51 C54 H54A 109.5 . . ?
C51 C54 H54B 109.5 . . ?
C51 C54 H54C 109.5 . . ?
H54A C54 H54B 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
N6 C55 H55 118.8 . . ?
N6 C55 C56 122.4(8) . . ?
C56 C55 H55 118.8 . . ?
C55 C56 H56 119.4 . . ?
C57 C56 C55 121.2(8) . . ?
C57 C56 H56 119.4 . . ?
C56 C57 C58 115.8(8) . . ?
C56 C57 C60 121.2(7) . . ?
C58 C57 C60 122.9(8) . . ?
C57 C58 H58 119.3 . . ?
C57 C58 C59 121.5(8) . . ?
C59 C58 H58 119.3 . . ?
N6 C59 C58 121.3(7) . . ?
N6 C59 C64 116.4(7) . . ?
C58 C59 C64 122.3(7) . . ?
C57 C60 C63 107.2(7) . . ?
C61 C60 C57 108.5(9) . . ?
C61 C60 C62 110.4(9) . . ?
C61 C60 C63 109.5(10) . . ?
C62 C60 C57 113.0(7) . . ?
C62 C60 C63 108.1(10) . . ?
C60 C61 H61A 109.5 . . ?
C60 C61 H61B 109.5 . . ?
C60 C61 H61C 109.5 . . ?
H61A C61 H61B 109.5 . . ?
H61A C61 H61C 109.5 . . ?
H61B C61 H61C 109.5 . . ?
C60 C62 H62A 109.5 . . ?
C60 C62 H62B 109.5 . . ?
C60 C62 H62C 109.5 . . ?
H62A C62 H62B 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
C60 C63 H63A 109.5 . . ?
C60 C63 H63B 109.5 . . ?
C60 C63 H63C 109.5 . . ?
H63A C63 H63B 109.5 . . ?
H63A C63 H63C 109.5 . . ?
H63B C63 H63C 109.5 . . ?
N7 C64 C59 115.1(7) . . ?
N7 C64 C65 122.1(7) . . ?
C65 C64 C59 122.5(8) . . ?
C64 C65 H65 120.1 . . ?
C64 C65 C66 119.8(8) . . ?
C66 C65 H65 120.1 . . ?
C65 C66 C69 121.0(8) . . ?
C67 C66 C65 117.1(8) . . ?
C67 C66 C69 121.8(8) . . ?
C66 C67 H67 119.8 . . ?
C66 C67 C68 120.4(8) . . ?
C68 C67 H67 119.8 . . ?
N7 C68 C67 122.7(8) . . ?
N7 C68 H68 118.7 . . ?
C67 C68 H68 118.7 . . ?
C66 C69 C71 104.6(10) . . ?
C66 C69 C72 108.0(9) . . ?
C70 C69 C66 112.7(9) . . ?
C70 C69 C71 109.7(11) . . ?
C70 C69 C72 111.3(12) . . ?
C72 C69 C71 110.4(10) . . ?
C69 C70 H70A 109.5 . . ?
C69 C70 H70B 109.5 . . ?
C69 C70 H70C 109.5 . . ?
H70A C70 H70B 109.5 . . ?
H70A C70 H70C 109.5 . . ?
H70B C70 H70C 109.5 . . ?
C69 C71 H71A 109.5 . . ?
C69 C71 H71B 109.5 . . ?
C69 C71 H71C 109.5 . . ?
H71A C71 H71B 109.5 . . ?
H71A C71 H71C 109.5 . . ?
H71B C71 H71C 109.5 . . ?
C69 C72 H72A 109.5 . . ?
C69 C72 H72B 109.5 . . ?
C69 C72 H72C 109.5 . . ?
H72A C72 H72B 109.5 . . ?
H72A C72 H72C 109.5 . . ?
H72B C72 H72C 109.5 . . ?
H80A C80 H80B 109.5 . . ?
H80A C80 H80C 109.5 . . ?
H80B C80 H80C 109.5 . . ?
C81 C80 H80A 109.5 . . ?
C81 C80 H80B 109.5 . . ?
C81 C80 H80C 109.5 . . ?
C82 C81 C80 117.2(17) . . ?
C86 C81 C80 117.2(17) . . ?
C86 C81 C82 125(2) . . ?
C81 C82 H82 121.3 . . ?
C81 C82 C83 117.4(18) . . ?
C83 C82 H82 121.3 . . ?
C82 C83 H83 120.1 . . ?
C84 C83 C82 119.9(17) . . ?
C84 C83 H83 120.1 . . ?
C83 C84 H84 118.8 . . ?
C83 C84 C85 122.4(18) . . ?
C85 C84 H84 118.8 . . ?
C84 C85 H85 122.4 . . ?
C86 C85 C84 115.2(16) . . ?
C86 C85 H85 122.4 . . ?
C81 C86 C85 119.3(18) . . ?
C81 C86 H86 120.4 . . ?
C85 C86 H86 120.4 . . ?
H73A C73 H73B 109.5 . . ?
H73A C73 H73C 109.5 . . ?
H73B C73 H73C 109.5 . . ?
C74 C73 H73A 109.5 . . ?
C74 C73 H73B 109.5 . . ?
C74 C73 H73C 109.5 . . ?
C75 C74 C73 117.3(14) . . ?
C79 C74 C73 123.1(12) . . ?
C79 C74 C75 119.6(12) . . ?
C74 C75 H75 121.3 . . ?
C76 C75 C74 117.4(12) . . ?
C76 C75 H75 121.3 . . ?
C75 C76 H76 119.4 . . ?
C77 C76 C75 121.2(12) . . ?
C77 C76 H76 119.4 . . ?
C76 C77 H77 119.5 . . ?
C76 C77 C78 121.1(14) . . ?
C78 C77 H77 119.5 . . ?
C77 C78 H78 120.2 . . ?
C79 C78 C77 119.7(13) . . ?
C79 C78 H78 120.2 . . ?
C74 C79 H79 119.5 . . ?
C78 C79 C74 121.0(12) . . ?
C78 C79 H79 119.5 . . ?
H3AA C3AA H3AB 109.5 . . ?
H3AA C3AA H3AC 109.5 . . ?
H3AB C3AA H3AC 109.5 . . ?
C1AA C3AA H3AA 109.5 . . ?
C1AA C3AA H3AB 109.5 . . ?
C1AA C3AA H3AC 109.5 . . ?
C2AA C4AA H4AA 120.0 . . ?
C2AA C4AA C1AA 120.0 . . ?
C1AA C4AA H4AA 120.0 . . ?
C4AA C2AA H2AA 120.0 . . ?
C4AA C2AA C5AA 120.0 . . ?
C5AA C2AA H2AA 120.0 . . ?
C2AA C5AA H5AA 120.0 . . ?
C6AA C5AA C2AA 120.0 . . ?
C6AA C5AA H5AA 120.0 . . ?
C5AA C6AA H6AA 120.0 . . ?
C0AA C6AA C5AA 120.0 . . ?
C0AA C6AA H6AA 120.0 . . ?
C6AA C0AA H0AA 120.0 . . ?
C1AA C0AA C6AA 120.0 . . ?
C1AA C0AA H0AA 120.0 . . ?
C4AA C1AA C3AA 120.4(8) . . ?
C0AA C1AA C3AA 119.6(8) . . ?
C0AA C1AA C4AA 120.0 . . ?

_shelx_SHELXL_version_number     2018/3
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.983(8)
2 0.017(8)


####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_apx1763
_database_code_depnum_ccdc_archive 'CCDC 1836174'
loop_
_audit_author_name
_audit_author_address
'Nickolas Anderson'
;Los Alamos National Laboratory
United States of America
;
_audit_update_record             
;
2019-03-06 deposited with the CCDC.	2019-04-23 downloaded from the CCDC.
;
_audit_creation_date             2018-08-24
_audit_creation_method           
;
Olex2 1.2
(compiled Nov 22 2016 11:51:51 for OlexSys, GUI svn.r5269)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C47.99 H69 Li2 N2 O4 S4 U'
_chemical_formula_sum            'C47.98 H69 Li2 N2 O4 S4 U'
_chemical_formula_weight         1118.02
_chemical_melting_point          ?
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'
S S 0.1246 0.1234 '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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   10.790(2)
_cell_length_b                   22.803(5)
_cell_length_c                   21.399(5)
_cell_angle_alpha                90
_cell_angle_beta                 99.345(2)
_cell_angle_gamma                90
_cell_volume                     5195.0(19)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3083
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      21.26
_cell_measurement_theta_min      2.28
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    3.326
_exptl_absorpt_correction_T_max  .865
_exptl_absorpt_correction_T_min  .788
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   
'SADABS-2014/2 - Bruker AXS area detector scaling and absorption correction'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.429
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2260
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.06
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1206
_diffrn_reflns_av_unetI/netI     0.0917
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            47137
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.709
_diffrn_reflns_theta_max         24.709
_diffrn_reflns_theta_min         1.929
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5929
_reflns_number_total             8850
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_data_collection       'APEX2 V.2014.7-1 (Bruker AXS, 2014)'
_computing_cell_refinement       'APEX2 V.2014.7-1 (Bruker AXS, 2014)'
_computing_data_reduction        'SAINT, v. 8.34A (Bruker AXS, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.036
_refine_diff_density_min         -1.380
_refine_diff_density_rms         0.147
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     603
_refine_ls_number_reflns         8850
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0918
_refine_ls_R_factor_gt           0.0486
_refine_ls_restrained_S_all      0.999
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0515P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0971
_refine_ls_wR_factor_ref         0.1124
_refine_special_details          
'This molecule is disordered over two positions in the coordinated THF molecules and in two of the four phenyl rings. The disorder is roughly 50:50.'
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(Li1) = Uanis(Li2) = Uanis(C45) = Uanis(C45A)
Uanis(C53) = Uanis(C54) = Uanis(C1C)
Uanis(C65) = Uanis(C65A) = Uanis(C71A) = Uanis(C71) = Uanis(C73A) = Uanis(C73)
= Uanis(C72A) = Uanis(C72) = Uanis(C46) = Uanis(C46A) = Uanis(C1D)
Uanis(C1J) = Uanis(C1K) = Uanis(C1I) = Uanis(C1H)
Uanis(C2) = Uanis(C1) = Uanis(C11) = Uanis(C3)
3. Others
 Sof(C58)=Sof(H58A)=Sof(H58B)=Sof(C1C)=Sof(H1CA)=Sof(H1CB)=Sof(C1D)=Sof(H1DA)=
 Sof(H1DB)=Sof(C65A)=Sof(C70A)=Sof(H70A)=Sof(C69A)=Sof(H69A)=Sof(C68A)=
 Sof(H68A)=Sof(C67A)=Sof(H67A)=Sof(C66A)=Sof(H66A)=1-FVAR(1)
 Sof(C65)=Sof(C66)=Sof(H66)=Sof(C69)=Sof(H69)=Sof(C68)=Sof(H68)=Sof(C59)=
 Sof(H59A)=Sof(H59B)=Sof(C67)=Sof(H67)=Sof(C70)=Sof(H70)=Sof(C54)=Sof(H54A)=
 Sof(H54B)=Sof(C1E)=Sof(H1EA)=Sof(H1EB)=FVAR(1)
 Sof(C45A)=Sof(C46A)=Sof(H46A)=Sof(C72A)=Sof(H72A)=Sof(C73A)=Sof(H73A)=
 Sof(C71A)=Sof(H71A)=Sof(C44A)=Sof(H44A)=1-FVAR(2)
 Sof(C45)=Sof(C44)=Sof(H44)=Sof(C46)=Sof(H46)=Sof(C72)=Sof(H72)=Sof(C71)=
 Sof(H71)=Sof(H73)=FVAR(2)
 Fixed Sof: H49A(0.5) H49B(0.5) H49C(0.5) H49D(0.5) H55C(0.5) H55D(0.5)
 H55A(0.5) H55B(0.5) H53C(0.5) H53D(0.5) H53A(0.5) H53B(0.5) H57A(0.5)
 H57B(0.5) H60A(0.5) H60B(0.5) H60C(0.5) H60D(0.5) C62(0.5) H62A(0.5) H62B(0.5)
 C73(0.5) C4(0.5) H4A(0.5) H4B(0.5) C9(0.5) H9A(0.5) H9B(0.5) C10(0.5)
 H10A(0.5) H10B(0.5) C1A(0.5) H1AA(0.5) H1AB(0.5) C1B(0.5) H1BA(0.5) H1BB(0.5)
 C1F(0.5) H1FA(0.5) H1FB(0.5) C1G(0.5) H1GA(0.5) H1GB(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C51(H51A,H51B), C49(H49A,H49B), C49(H49C,H49D), C50(H50A,H50B), C52(H52A,
 H52B), C55(H55C,H55D), C55(H55A,H55B), C53(H53C,H53D), C53(H53A,H53B),
 C56(H56A,H56B), C57(H57A,H57B), C60(H60A,H60B), C60(H60C,H60D), C59(H59A,H59B),
  C58(H58A,H58B), C62(H62A,H62B), C54(H54A,H54B), C4(H4A,H4B), C9(H9A,H9B),
 C10(H10A,H10B), C1A(H1AA,H1AB), C1B(H1BA,H1BB), C1C(H1CA,H1CB), C1D(H1DA,H1DB),
  C1E(H1EA,H1EB), C1F(H1FA,H1FB), C1G(H1GA,H1GB)
4.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C66(H66), C17(H17), C16(H16), C13(H13), C15(H15), C69(H69),
 C68(H68), C44(H44), C46(H46), C67(H67), C70(H70), C72(H72), C71(H71), C73(H73),
  C46A(H46A), C72A(H72A), C73A(H73A), C71A(H71A), C44A(H44A), C70A(H70A),
 C69A(H69A), C68A(H68A), C67A(H67A), C66A(H66A), C19(H19), C1H(H1H), C1I(H1I),
 C1J(H1J), C1K(H1K)
4.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C11(H11A,H11B,H11C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C),
 C3(H3A,H3B,H3C), C2(H2A,H2B,H2C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 0.04113(3) 0.76053(2) 0.06150(2) 0.02024(10) Uani 1 1 d . . . . .
S4 S 0.12342(19) 0.79126(9) 0.18676(9) 0.0263(5) Uani 1 1 d . . . . .
S1 S 0.27766(19) 0.79450(10) 0.03793(10) 0.0350(5) Uani 1 1 d . . . . .
S2 S -0.19861(18) 0.72808(9) 0.08114(9) 0.0310(5) Uani 1 1 d . . . . .
S3 S -0.0362(2) 0.72709(8) -0.06345(9) 0.0288(5) Uani 1 1 d . . . . .
N2 N 0.1246(5) 0.6917(2) 0.0876(3) 0.0200(14) Uani 1 1 d . . . . .
N1 N -0.0419(5) 0.8292(3) 0.0379(3) 0.0227(15) Uani 1 1 d . . . . .
C14 C -0.3354(11) 0.5894(5) 0.1636(5) 0.075(4) Uani 1 1 d . . . . .
H14 H -0.411114 0.567295 0.157667 0.090 Uiso 1 1 calc R . . . .
C5 C 0.1997(7) 0.6384(3) 0.1056(4) 0.0260(19) Uani 1 1 d . . . . .
C6 C 0.3180(7) 0.6395(4) 0.0755(4) 0.045(2) Uani 1 1 d . . . . .
H6A H 0.295091 0.636322 0.029364 0.068 Uiso 1 1 calc GR . . . .
H6B H 0.372157 0.606492 0.091462 0.068 Uiso 1 1 calc GR . . . .
H6C H 0.363028 0.676413 0.086165 0.068 Uiso 1 1 calc GR . . . .
C1 C -0.1200(9) 0.8827(4) 0.0215(5) 0.0517(13) Uani 1 1 d . . . . .
C11 C -0.2319(8) 0.8819(4) 0.0556(4) 0.0517(13) Uani 1 1 d . . . . .
H11A H -0.284644 0.847843 0.041662 0.078 Uiso 1 1 calc GR . . . .
H11B H -0.280728 0.917898 0.046024 0.078 Uiso 1 1 calc GR . . . .
H11C H -0.202833 0.879306 0.101390 0.078 Uiso 1 1 calc GR . . . .
C7 C 0.1183(7) 0.5847(3) 0.0843(4) 0.036(2) Uani 1 1 d . . . . .
H7A H 0.039016 0.587400 0.100936 0.054 Uiso 1 1 calc GR . . . .
H7B H 0.163004 0.548989 0.100495 0.054 Uiso 1 1 calc GR . . . .
H7C H 0.100774 0.583265 0.037952 0.054 Uiso 1 1 calc GR . . . .
C8 C 0.2368(9) 0.6379(4) 0.1784(4) 0.055(3) Uani 1 1 d . . . . .
H8A H 0.282630 0.673997 0.192227 0.083 Uiso 1 1 calc GR . . . .
H8B H 0.290466 0.603927 0.191282 0.083 Uiso 1 1 calc GR . . . .
H8C H 0.160883 0.635570 0.197975 0.083 Uiso 1 1 calc GR . . . .
C3 C -0.0405(9) 0.9357(4) 0.0430(4) 0.0517(13) Uani 1 1 d . . . . .
H3A H -0.015243 0.934427 0.089069 0.078 Uiso 1 1 calc GR . . . .
H3B H -0.089207 0.971461 0.031231 0.078 Uiso 1 1 calc GR . . . .
H3C H 0.034500 0.935699 0.022582 0.078 Uiso 1 1 calc GR . . . .
C2 C -0.1648(9) 0.8833(4) -0.0504(4) 0.0517(13) Uani 1 1 d . . . . .
H2A H -0.091838 0.884894 -0.072307 0.078 Uiso 1 1 calc GR . . . .
H2B H -0.217993 0.917686 -0.061845 0.078 Uiso 1 1 calc GR . . . .
H2C H -0.213036 0.847556 -0.062898 0.078 Uiso 1 1 calc GR . . . .
C65 C 0.016(2) 0.8464(11) 0.2110(11) 0.0363(17) Uani 0.510(13) 1 d . . P A 1
C66 C -0.0934(14) 0.8287(9) 0.2287(8) 0.024(4) Uani 0.510(13) 1 d . . P A 1
H66 H -0.117133 0.788521 0.225303 0.029 Uiso 0.510(13) 1 calc R . P A 1
C17 C -0.1150(8) 0.6535(3) 0.1804(4) 0.031(2) Uani 1 1 d . . . . .
H17 H -0.038235 0.674791 0.186415 0.038 Uiso 1 1 calc R . . . .
C16 C -0.1336(9) 0.6083(4) 0.2214(4) 0.048(3) Uani 1 1 d . . . . .
H16 H -0.068919 0.599310 0.255728 0.058 Uiso 1 1 calc R . . . .
C12 C -0.2110(8) 0.6675(3) 0.1298(4) 0.034(2) Uani 1 1 d . . . . .
C13 C -0.3200(8) 0.6340(4) 0.1221(4) 0.051(3) Uani 1 1 d . . . . .
H13 H -0.385044 0.641991 0.087646 0.061 Uiso 1 1 calc R . . . .
C15 C -0.2414(11) 0.5765(5) 0.2137(5) 0.077(4) Uani 1 1 d . . . . .
H15 H -0.252061 0.545833 0.242464 0.093 Uiso 1 1 calc R . . . .
C69 C -0.029(6) 0.9489(18) 0.237(3) 0.046(15) Uani 0.510(13) 1 d . . P A 1
H69 H -0.008088 0.989428 0.239353 0.055 Uiso 0.510(13) 1 calc R . P A 1
C68 C -0.139(2) 0.9273(12) 0.2562(10) 0.040(6) Uani 0.510(13) 1 d . . P A 1
H68 H -0.192969 0.954266 0.272526 0.048 Uiso 0.510(13) 1 calc R . P A 1
C45 C 0.067(2) 0.6696(10) -0.0822(10) 0.0274(18) Uani 0.514(10) 1 d . . P B 1
C44 C 0.0235(19) 0.6114(11) -0.0947(11) 0.029(6) Uani 0.514(10) 1 d . . P B 1
H44 H -0.060265 0.602237 -0.089842 0.035 Uiso 0.514(10) 1 calc R . P B 1
C46 C 0.1888(18) 0.6818(9) -0.0952(8) 0.0363(17) Uani 0.514(10) 1 d . . P B 1
H46 H 0.220719 0.720643 -0.089706 0.044 Uiso 0.514(10) 1 calc R . P B 1
O2 O -0.3668(5) 0.7354(2) -0.0794(2) 0.0398(14) Uani 1 1 d . . . . .
O1 O -0.2776(6) 0.6136(3) -0.0422(3) 0.058(2) Uani 1 1 d . . . . .
C51 C -0.2299(8) 0.5633(4) -0.0049(5) 0.051(3) Uani 1 1 d . . . . .
H51A H -0.203422 0.574197 0.040095 0.061 Uiso 1 1 calc R . . . .
H51B H -0.157883 0.545502 -0.021227 0.061 Uiso 1 1 calc R . . . .
C49 C -0.4063(9) 0.5324(4) -0.0794(6) 0.070(4) Uani 1 1 d . . . . .
H49A H -0.498239 0.533276 -0.080171 0.084 Uiso 0.5 1 calc R . P C 1
H49B H -0.386886 0.499890 -0.106874 0.084 Uiso 0.5 1 calc R . P C 1
H49C H -0.357193 0.519361 -0.112113 0.084 Uiso 0.5 1 calc R . P D 2
H49D H -0.492571 0.516309 -0.087704 0.084 Uiso 0.5 1 calc R . P D 2
C50 C -0.3402(11) 0.5224(4) -0.0125(5) 0.064(3) Uani 1 1 d . . . . .
H50A H -0.396318 0.531701 0.018402 0.077 Uiso 1 1 calc R . . . .
H50B H -0.311992 0.481209 -0.006473 0.077 Uiso 1 1 calc R . . . .
C52 C -0.3694(8) 0.7505(4) -0.1445(4) 0.042(2) Uani 1 1 d . . . . .
H52A H -0.380233 0.715032 -0.171559 0.051 Uiso 1 1 calc R . . . .
H52B H -0.290785 0.770517 -0.150504 0.051 Uiso 1 1 calc R . . . .
C55 C -0.4817(9) 0.7538(6) -0.0612(4) 0.080(4) Uani 1 1 d . . . . .
H55C H -0.466409 0.777189 -0.021697 0.096 Uiso 0.5 1 calc R . P A 2
H55D H -0.535348 0.719763 -0.054942 0.096 Uiso 0.5 1 calc R . P A 2
H55A H -0.509479 0.724911 -0.031782 0.096 Uiso 0.5 1 calc R . P A 1
H55B H -0.470723 0.792255 -0.039533 0.096 Uiso 0.5 1 calc R . P A 1
C53 C -0.4773(12) 0.7898(7) -0.1598(5) 0.103(5) Uani 1 1 d . . . . .
H53C H -0.444367 0.829251 -0.167416 0.124 Uiso 0.5 1 calc R . P A 2
H53D H -0.526361 0.776389 -0.200460 0.124 Uiso 0.5 1 calc R . P A 2
H53A H -0.513207 0.788886 -0.205442 0.124 Uiso 0.5 1 calc R . P A 1
H53B H -0.456547 0.830679 -0.146450 0.124 Uiso 0.5 1 calc R . P A 1
Li1 Li -0.2350(12) 0.6958(6) -0.0300(5) 0.0274(18) Uani 1 1 d . . . . .
Li2 Li 0.3205(12) 0.8302(6) 0.1479(6) 0.0274(18) Uani 1 1 d . . . . .
O3 O 0.4528(5) 0.7865(3) 0.2009(3) 0.0575(19) Uani 1 1 d . . . . .
O4 O 0.3666(7) 0.9101(4) 0.1617(3) 0.086(3) Uani 1 1 d . . . . .
C56 C 0.4502(8) 0.7667(4) 0.2645(4) 0.047(2) Uani 1 1 d . . . . .
H56A H 0.367818 0.748750 0.267631 0.056 Uiso 1 1 calc R . . . .
H56B H 0.464505 0.799915 0.294574 0.056 Uiso 1 1 calc R . . . .
C57 C 0.5534(11) 0.7221(6) 0.2793(7) 0.091(5) Uani 1 1 d . . . . .
H57A H 0.532049 0.683425 0.259347 0.109 Uiso 0.5 1 calc R . P A 1
H57B H 0.584816 0.717711 0.325135 0.109 Uiso 0.5 1 calc R . P A 1
C60 C 0.3183(11) 0.9630(6) 0.1335(5) 0.072(3) Uani 1 1 d . . . . .
H60A H 0.233672 0.955108 0.109309 0.086 Uiso 0.5 1 calc R . P E 1
H60B H 0.372389 0.975452 0.102660 0.086 Uiso 0.5 1 calc R . P E 1
H60C H 0.338481 0.967611 0.090215 0.086 Uiso 0.5 1 calc R . P F 2
H60D H 0.226236 0.965763 0.131804 0.086 Uiso 0.5 1 calc R . P F 2
C59 C 0.5672(16) 0.7901(11) 0.1817(9) 0.046(6) Uani 0.510(13) 1 d . . P A 1
H59A H 0.587966 0.831184 0.172540 0.055 Uiso 0.510(13) 1 calc R . P A 1
H59B H 0.569551 0.765930 0.143431 0.055 Uiso 0.510(13) 1 calc R . P A 1
C58 C 0.628(3) 0.7203(14) 0.2479(12) 0.074(9) Uani 0.490(13) 1 d . . P A 2
H58A H 0.648702 0.679078 0.239055 0.089 Uiso 0.490(13) 1 calc R . P A 2
H58B H 0.705709 0.740156 0.268482 0.089 Uiso 0.490(13) 1 calc R . P A 2
C62 C 0.3602(19) 0.9905(8) 0.2482(8) 0.047(5) Uani 0.5 1 d . . P G 1
H62A H 0.424926 1.015477 0.273378 0.057 Uiso 0.5 1 calc R . P G 1
H62B H 0.292606 0.982689 0.273285 0.057 Uiso 0.5 1 calc R . P G 1
C67 C -0.1725(16) 0.8703(8) 0.2525(8) 0.033(5) Uani 0.510(13) 1 d . . P A 1
H67 H -0.248387 0.857948 0.265596 0.040 Uiso 0.510(13) 1 calc R . P A 1
C70 C 0.0496(19) 0.9053(8) 0.2147(8) 0.035(5) Uani 0.510(13) 1 d . . P A 1
H70 H 0.126228 0.917126 0.202093 0.042 Uiso 0.510(13) 1 calc R . P A 1
C72 C 0.2622(17) 0.6386(8) -0.1157(8) 0.0363(17) Uani 0.514(10) 1 d . . P B 1
H72 H 0.343609 0.648332 -0.123937 0.044 Uiso 0.514(10) 1 calc R . P B 1
C71 C 0.0968(19) 0.5675(9) -0.1136(10) 0.0363(17) Uani 0.514(10) 1 d . . P B 1
H71 H 0.065312 0.528624 -0.119111 0.044 Uiso 0.514(10) 1 calc R . P B 1
C73 C 0.2197(18) 0.5807(9) -0.1247(8) 0.0363(17) Uani 0.5 1 d . . P B 1
H73 H 0.271746 0.551139 -0.137950 0.044 Uiso 0.514(10) 1 calc R . P B 1
C54 C -0.548(3) 0.7952(15) -0.1235(12) 0.103(5) Uani 0.510(13) 1 d . . P A 2
H54A H -0.632420 0.780426 -0.141491 0.124 Uiso 0.510(13) 1 calc R . P A 2
H54B H -0.554577 0.836730 -0.111008 0.124 Uiso 0.510(13) 1 calc R . P A 2
C4 C 0.499(2) 0.9825(8) 0.1977(10) 0.058(6) Uani 0.5 1 d . . P H 2
H4A H 0.517290 0.990900 0.243630 0.070 Uiso 0.5 1 calc R . P H 2
H4B H 0.561795 1.003315 0.176802 0.070 Uiso 0.5 1 calc R . P H 2
C9 C 0.5061(19) 0.9188(10) 0.1866(12) 0.072(7) Uani 0.5 1 d . . P H 2
H9A H 0.534479 0.896574 0.226096 0.086 Uiso 0.5 1 calc R . P H 2
H9B H 0.559656 0.909023 0.154580 0.086 Uiso 0.5 1 calc R . P H 2
C10 C 0.415(2) 0.9357(9) 0.2300(10) 0.075(8) Uani 0.5 1 d . . P G 1
H10A H 0.401395 0.905425 0.261285 0.090 Uiso 0.5 1 calc R . P G 1
H10B H 0.506910 0.941597 0.233894 0.090 Uiso 0.5 1 calc R . P G 1
C1A C -0.3603(19) 0.5945(8) -0.1059(9) 0.046(5) Uani 0.5 1 d . . P I 1
H1AA H -0.310514 0.589074 -0.140505 0.055 Uiso 0.5 1 calc R . P I 1
H1AB H -0.430896 0.621773 -0.119530 0.055 Uiso 0.5 1 calc R . P I 1
C1B C -0.4017(16) 0.5974(8) -0.0684(8) 0.034(5) Uani 0.5 1 d . . P I 2
H1BA H -0.428082 0.618271 -0.108906 0.041 Uiso 0.5 1 calc R . P I 2
H1BB H -0.459898 0.608298 -0.038973 0.041 Uiso 0.5 1 calc R . P I 2
C1C C -0.570(3) 0.7580(15) -0.1158(12) 0.103(5) Uani 0.490(13) 1 d . . P A 1
H1CA H -0.641941 0.782998 -0.110075 0.124 Uiso 0.490(13) 1 calc R . P A 1
H1CB H -0.599605 0.719164 -0.132506 0.124 Uiso 0.490(13) 1 calc R . P A 1
C1D C 0.5743(18) 0.7509(9) 0.1882(9) 0.0363(17) Uani 0.490(13) 1 d . . P A 2
H1DA H 0.550644 0.722102 0.153777 0.044 Uiso 0.490(13) 1 calc R . P A 2
H1DB H 0.636939 0.778239 0.175404 0.044 Uiso 0.490(13) 1 calc R . P A 2
C1E C 0.6560(16) 0.7664(13) 0.2378(9) 0.057(7) Uani 0.510(13) 1 d . . P A 1
H1EA H 0.695500 0.798642 0.265018 0.068 Uiso 0.510(13) 1 calc R . P A 1
H1EB H 0.722590 0.742125 0.223977 0.068 Uiso 0.510(13) 1 calc R . P A 1
C45A C 0.0274(19) 0.6628(12) -0.0862(11) 0.0274(18) Uani 0.486(10) 1 d . . P B
2
C46A C 0.157(2) 0.6610(9) -0.0809(9) 0.0363(17) Uani 0.486(10) 1 d . . P B 2
H46A H 0.206492 0.693641 -0.064281 0.044 Uiso 0.486(10) 1 calc R . P B 2
C72A C 0.2168(19) 0.6088(9) -0.1009(9) 0.0363(17) Uani 0.486(10) 1 d . . P B 2
H72A H 0.305350 0.606296 -0.098665 0.044 Uiso 0.486(10) 1 calc R . P B 2
C73A C 0.140(2) 0.5635(10) -0.1232(10) 0.0363(17) Uani 0.486(10) 1 d . . P B 2
H73A H 0.176799 0.527943 -0.134383 0.044 Uiso 0.486(10) 1 calc R . P B 2
C71A C 0.0109(18) 0.5669(8) -0.1301(8) 0.0363(17) Uani 0.486(10) 1 d . . P B 2
H71A H -0.039792 0.535360 -0.148438 0.044 Uiso 0.486(10) 1 calc R . P B 2
C44A C -0.044(2) 0.6168(12) -0.1101(12) 0.039(7) Uani 0.486(10) 1 d . . P B 2
H44A H -0.132651 0.618725 -0.113044 0.047 Uiso 0.486(10) 1 calc R . P B 2
C1F C 0.307(3) 1.0204(11) 0.1838(11) 0.073(8) Uani 0.5 1 d . . P G 1
H1FA H 0.358355 1.054228 0.174790 0.088 Uiso 0.5 1 calc R . P G 1
H1FB H 0.218457 1.033061 0.182320 0.088 Uiso 0.5 1 calc R . P G 1
C1G C 0.378(2) 1.0016(11) 0.1726(14) 0.065(8) Uani 0.5 1 d . . P H 2
H1GA H 0.330154 1.008601 0.207658 0.078 Uiso 0.5 1 calc R . P H 2
H1GB H 0.383448 1.039142 0.150071 0.078 Uiso 0.5 1 calc R . P H 2
C65A C 0.062(2) 0.8538(12) 0.2126(11) 0.0363(17) Uani 0.490(13) 1 d . . P A 2
C70A C 0.143(2) 0.9002(8) 0.2396(8) 0.035(5) Uani 0.490(13) 1 d . . P A 2
H70A H 0.231267 0.896168 0.243621 0.042 Uiso 0.490(13) 1 calc R . P A 2
C69A C 0.090(2) 0.9517(8) 0.2601(8) 0.049(6) Uani 0.490(13) 1 d . . P A 2
H69A H 0.141119 0.983718 0.277293 0.058 Uiso 0.490(13) 1 calc R . P A 2
C68A C -0.037(8) 0.953(3) 0.254(4) 0.08(2) Uani 0.490(13) 1 d . . P A 2
H68A H -0.073675 0.986980 0.269574 0.097 Uiso 0.490(13) 1 calc R . P A 2
C67A C -0.112(3) 0.9121(14) 0.2283(13) 0.062(10) Uani 0.490(13) 1 d . . P A 2
H67A H -0.200298 0.917465 0.222478 0.075 Uiso 0.490(13) 1 calc R . P A 2
C66A C -0.064(3) 0.8628(11) 0.2103(10) 0.050(7) Uani 0.490(13) 1 d . . P A 2
H66A H -0.119770 0.831962 0.194965 0.060 Uiso 0.490(13) 1 calc R . P A 2
C18 C 0.2801(9) 0.8552(4) -0.0124(4) 0.042(2) Uani 1 1 d . . . . .
C19 C 0.1831(10) 0.8672(4) -0.0620(4) 0.046(3) Uani 1 1 d . . . . .
H19 H 0.110864 0.842713 -0.067590 0.055 Uiso 1 1 calc R . . . .
C1H C 0.1878(13) 0.9128(5) -0.1028(5) 0.085(2) Uani 1 1 d . . . . .
H1H H 0.120080 0.919022 -0.136507 0.102 Uiso 1 1 calc R . . . .
C1I C 0.2878(13) 0.9491(5) -0.0958(5) 0.085(2) Uani 1 1 d . . . . .
H1I H 0.289276 0.981230 -0.123886 0.102 Uiso 1 1 calc R . . . .
C1J C 0.3853(13) 0.8925(5) -0.0053(5) 0.085(2) Uani 1 1 d . . . . .
H1J H 0.454201 0.886245 0.027778 0.102 Uiso 1 1 calc R . . . .
C1K C 0.3865(13) 0.9399(5) -0.0485(5) 0.085(2) Uani 1 1 d . . . . .
H1K H 0.457095 0.965365 -0.044345 0.102 Uiso 1 1 calc R . . . .


_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 S4 2.773(2) . ?
U1 S1 2.790(2) . ?
U1 S2 2.787(2) . ?
U1 S3 2.775(2) . ?
U1 N2 1.850(5) . ?
U1 N1 1.834(6) . ?
U1 Li1 3.604(12) . ?
U1 Li2 3.636(12) . ?
S4 C65 1.84(3) . ?
S4 Li2 2.564(13) . ?
S4 C65A 1.70(3) . ?
S1 Li2 2.463(12) . ?
S1 C18 1.758(9) . ?
S2 C12 1.747(8) . ?
S2 Li1 2.458(12) . ?
S3 C45 1.81(3) . ?
S3 Li1 2.475(13) . ?
S3 C45A 1.72(3) . ?
N2 C5 1.477(9) . ?
N1 C1 1.491(10) . ?
C14 C13 1.378(12) . ?
C14 C15 1.384(14) . ?
C5 C6 1.521(11) . ?
C5 C7 1.533(10) . ?
C5 C8 1.545(11) . ?
C1 C11 1.509(12) . ?
C1 C3 1.510(12) . ?
C1 C2 1.536(12) . ?
C65 C66 1.36(3) . ?
C65 C70 1.39(3) . ?
C66 C67 1.42(2) . ?
C17 C16 1.390(11) . ?
C17 C12 1.408(10) . ?
C16 C15 1.358(12) . ?
C12 C13 1.390(11) . ?
C69 C68 1.40(6) . ?
C69 C70 1.44(7) . ?
C68 C67 1.35(3) . ?
C45 C44 1.42(3) . ?
C45 C46 1.41(3) . ?
C44 C71 1.38(3) . ?
C46 C72 1.38(2) . ?
O2 C52 1.431(9) . ?
O2 C55 1.422(11) . ?
O2 Li1 1.862(14) . ?
O1 C51 1.442(10) . ?
O1 Li1 1.939(14) . ?
O1 C1A 1.565(17) . ?
O1 C1B 1.414(17) . ?
C51 C50 1.499(12) . ?
C49 C50 1.509(14) . ?
C49 C1A 1.63(2) . ?
C49 C1B 1.50(2) . ?
C52 C53 1.464(13) . ?
C55 C54 1.69(2) . ?
C55 C1C 1.38(3) . ?
C53 C54 1.18(3) . ?
C53 C1C 1.65(3) . ?
Li2 O3 1.947(14) . ?
Li2 O4 1.899(15) . ?
O3 C56 1.439(9) . ?
O3 C59 1.366(17) . ?
O3 C1D 1.601(19) . ?
O4 C60 1.412(12) . ?
O4 C9 1.526(19) . ?
O4 C10 1.582(19) . ?
C56 C57 1.503(13) . ?
C57 C58 1.13(3) . ?
C57 C1E 1.83(3) . ?
C60 C1F 1.71(2) . ?
C60 C1G 1.31(2) . ?
C59 C1E 1.51(3) . ?
C58 C1D 1.49(3) . ?
C62 C10 1.46(3) . ?
C62 C1F 1.56(3) . ?
C72 C73 1.40(3) . ?
C71 C73 1.42(3) . ?
C4 C9 1.48(3) . ?
C4 C1G 1.40(3) . ?
C45A C46A 1.39(3) . ?
C45A C44A 1.35(3) . ?
C46A C72A 1.45(3) . ?
C72A C73A 1.36(3) . ?
C73A C71A 1.38(3) . ?
C71A C44A 1.38(3) . ?
C65A C70A 1.43(3) . ?
C65A C66A 1.37(3) . ?
C70A C69A 1.40(3) . ?
C69A C68A 1.36(9) . ?
C68A C67A 1.30(7) . ?
C67A C66A 1.32(3) . ?
C18 C19 1.391(12) . ?
C18 C1J 1.407(13) . ?
C19 C1H 1.365(13) . ?
C1H C1I 1.349(14) . ?
C1I C1K 1.361(16) . ?
C1J C1K 1.424(14) . ?

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
S4 U1 S1 86.90(6) . . ?
S4 U1 S2 94.63(6) . . ?
S4 U1 S3 178.32(6) . . ?
S4 U1 Li1 137.3(2) . . ?
S4 U1 Li2 44.7(2) . . ?
S1 U1 Li1 135.7(2) . . ?
S1 U1 Li2 42.6(2) . . ?
S2 U1 S1 178.10(6) . . ?
S2 U1 Li1 42.9(2) . . ?
S2 U1 Li2 138.8(2) . . ?
S3 U1 S1 92.45(6) . . ?
S3 U1 S2 86.05(6) . . ?
S3 U1 Li1 43.3(2) . . ?
S3 U1 Li2 134.8(2) . . ?
N2 U1 S4 81.86(18) . . ?
N2 U1 S1 82.83(18) . . ?
N2 U1 S2 98.49(18) . . ?
N2 U1 S3 96.53(18) . . ?
N2 U1 Li1 97.8(3) . . ?
N2 U1 Li2 83.9(3) . . ?
N1 U1 S4 96.65(18) . . ?
N1 U1 S1 97.66(19) . . ?
N1 U1 S2 81.05(19) . . ?
N1 U1 S3 84.97(18) . . ?
N1 U1 N2 178.4(2) . . ?
N1 U1 Li1 82.9(3) . . ?
N1 U1 Li2 95.4(3) . . ?
Li1 U1 Li2 177.5(3) . . ?
C65 S4 U1 109.1(7) . . ?
C65 S4 Li2 116.6(8) . . ?
Li2 S4 U1 85.8(3) . . ?
C65A S4 U1 116.4(8) . . ?
C65A S4 Li2 101.7(9) . . ?
Li2 S1 U1 87.4(3) . . ?
C18 S1 U1 115.8(3) . . ?
C18 S1 Li2 107.9(4) . . ?
C12 S2 U1 117.5(3) . . ?
C12 S2 Li1 108.9(4) . . ?
Li1 S2 U1 86.6(3) . . ?
C45 S3 U1 108.3(6) . . ?
C45 S3 Li1 116.8(7) . . ?
Li1 S3 U1 86.5(3) . . ?
C45A S3 U1 115.8(7) . . ?
C45A S3 Li1 104.0(7) . . ?
C5 N2 U1 175.2(5) . . ?
C1 N1 U1 174.3(6) . . ?
C13 C14 C15 120.4(9) . . ?
N2 C5 C6 109.8(6) . . ?
N2 C5 C7 108.5(6) . . ?
N2 C5 C8 108.0(6) . . ?
C6 C5 C7 111.6(6) . . ?
C6 C5 C8 109.3(7) . . ?
C7 C5 C8 109.6(7) . . ?
N1 C1 C11 110.0(7) . . ?
N1 C1 C3 108.2(7) . . ?
N1 C1 C2 108.4(7) . . ?
C11 C1 C3 108.8(8) . . ?
C11 C1 C2 109.8(8) . . ?
C3 C1 C2 111.6(8) . . ?
C66 C65 S4 119.3(18) . . ?
C66 C65 C70 120(2) . . ?
C70 C65 S4 120.4(16) . . ?
C65 C66 C67 120(2) . . ?
C16 C17 C12 119.3(8) . . ?
C15 C16 C17 122.0(9) . . ?
C17 C12 S2 121.3(6) . . ?
C13 C12 S2 120.7(7) . . ?
C13 C12 C17 117.9(7) . . ?
C14 C13 C12 121.3(9) . . ?
C16 C15 C14 119.1(9) . . ?
C68 C69 C70 115(3) . . ?
C67 C68 C69 124(3) . . ?
C44 C45 S3 121.6(15) . . ?
C46 C45 S3 121.8(16) . . ?
C46 C45 C44 116(2) . . ?
C71 C44 C45 123(2) . . ?
C72 C46 C45 121.4(19) . . ?
C52 O2 Li1 124.2(6) . . ?
C55 O2 C52 108.5(7) . . ?
C55 O2 Li1 127.3(7) . . ?
C51 O1 Li1 129.6(7) . . ?
C51 O1 C1A 111.3(9) . . ?
C1A O1 Li1 118.4(8) . . ?
C1B O1 C51 104.0(9) . . ?
C1B O1 Li1 119.6(9) . . ?
O1 C51 C50 103.2(8) . . ?
C50 C49 C1A 109.7(9) . . ?
C1B C49 C50 90.1(10) . . ?
C51 C50 C49 104.7(8) . . ?
O2 C52 C53 104.7(8) . . ?
O2 C55 C54 102.9(12) . . ?
C1C C55 O2 107.3(13) . . ?
C52 C53 C1C 97.8(12) . . ?
C54 C53 C52 119.4(15) . . ?
S2 Li1 U1 50.5(2) . . ?
S2 Li1 S3 100.6(4) . . ?
S3 Li1 U1 50.2(2) . . ?
O2 Li1 U1 126.7(6) . . ?
O2 Li1 S2 113.1(6) . . ?
O2 Li1 S3 108.3(6) . . ?
O2 Li1 O1 104.5(6) . . ?
O1 Li1 U1 128.8(6) . . ?
O1 Li1 S2 114.7(6) . . ?
O1 Li1 S3 115.9(6) . . ?
S4 Li2 U1 49.5(2) . . ?
S1 Li2 U1 50.1(2) . . ?
S1 Li2 S4 99.1(4) . . ?
O3 Li2 U1 122.8(5) . . ?
O3 Li2 S4 101.7(5) . . ?
O3 Li2 S1 113.2(6) . . ?
O4 Li2 U1 132.3(6) . . ?
O4 Li2 S4 119.5(7) . . ?
O4 Li2 S1 117.9(6) . . ?
O4 Li2 O3 104.6(6) . . ?
C56 O3 Li2 125.9(6) . . ?
C56 O3 C1D 98.3(9) . . ?
C59 O3 Li2 114.0(11) . . ?
C59 O3 C56 117.5(10) . . ?
C1D O3 Li2 134.7(9) . . ?
C60 O4 Li2 133.2(8) . . ?
C60 O4 C9 108.3(11) . . ?
C60 O4 C10 97.1(10) . . ?
C9 O4 Li2 113.4(11) . . ?
C10 O4 Li2 122.4(10) . . ?
O3 C56 C57 106.4(8) . . ?
C56 C57 C1E 90.6(10) . . ?
C58 C57 C56 118.4(19) . . ?
O4 C60 C1F 116.4(11) . . ?
C1G C60 O4 101.0(14) . . ?
O3 C59 C1E 103.1(14) . . ?
C57 C58 C1D 106(2) . . ?
C10 C62 C1F 104.2(17) . . ?
C68 C67 C66 120(2) . . ?
C65 C70 C69 122(2) . . ?
C46 C72 C73 121.7(18) . . ?
C44 C71 C73 120(2) . . ?
C72 C73 C71 118.2(17) . . ?
C53 C54 C55 103.1(18) . . ?
C1G C4 C9 108.3(18) . . ?
C4 C9 O4 96.3(16) . . ?
C62 C10 O4 118.3(14) . . ?
O1 C1A C49 95.7(11) . . ?
O1 C1B C49 108.9(12) . . ?
C55 C1C C53 97(2) . . ?
C58 C1D O3 108.0(17) . . ?
C59 C1E C57 103.2(13) . . ?
C46A C45A S3 116.5(16) . . ?
C44A C45A S3 122.6(19) . . ?
C44A C45A C46A 121(3) . . ?
C45A C46A C72A 119(2) . . ?
C73A C72A C46A 116.8(19) . . ?
C72A C73A C71A 123(2) . . ?
C73A C71A C44A 119(2) . . ?
C45A C44A C71A 121(2) . . ?
C62 C1F C60 99.7(15) . . ?
C60 C1G C4 111.7(19) . . ?
C70A C65A S4 120.5(16) . . ?
C66A C65A S4 123.5(19) . . ?
C66A C65A C70A 116(2) . . ?
C69A C70A C65A 120(2) . . ?
C68A C69A C70A 116(3) . . ?
C67A C68A C69A 125(6) . . ?
C68A C67A C66A 119(5) . . ?
C67A C66A C65A 124(3) . . ?
C19 C18 S1 122.5(7) . . ?
C19 C18 C1J 117.3(9) . . ?
C1J C18 S1 120.1(9) . . ?
C1H C19 C18 122.4(10) . . ?
C1I C1H C19 120.5(13) . . ?
C1H C1I C1K 120.3(12) . . ?
C18 C1J C1K 118.7(12) . . ?
C1I C1K C1J 120.7(12) . . ?

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
U1 S4 C65 C66 81.5(19) . . . . ?
U1 S4 C65 C70 -102.3(17) . . . . ?
U1 S4 C65A C70A -123.8(16) . . . . ?
U1 S4 C65A C66A 57(2) . . . . ?
U1 S1 C18 C19 -32.7(8) . . . . ?
U1 S1 C18 C1J 150.1(7) . . . . ?
U1 S2 C12 C17 31.1(8) . . . . ?
U1 S2 C12 C13 -153.2(7) . . . . ?
U1 S3 C45 C44 112.8(17) . . . . ?
U1 S3 C45 C46 -77.6(18) . . . . ?
U1 S3 C45A C46A -59.7(18) . . . . ?
U1 S3 C45A C44A 122(2) . . . . ?
U1 Li2 O4 C60 -13.9(15) . . . . ?
U1 Li2 O4 C9 -165.1(12) . . . . ?
U1 Li2 O4 C10 129.0(13) . . . . ?
S4 C65 C66 C67 174.9(13) . . . . ?
S4 C65 C70 C69 -176(3) . . . . ?
S4 Li2 O4 C60 -74.4(12) . . . . ?
S4 Li2 O4 C9 134.4(12) . . . . ?
S4 Li2 O4 C10 68.6(14) . . . . ?
S4 C65A C70A C69A 179.4(15) . . . . ?
S4 C65A C66A C67A -178(2) . . . . ?
S1 Li2 O4 C60 46.1(14) . . . . ?
S1 Li2 O4 C9 -105.1(13) . . . . ?
S1 Li2 O4 C10 -171.0(12) . . . . ?
S1 C18 C19 C1H -176.9(8) . . . . ?
S1 C18 C1J C1K 177.4(8) . . . . ?
S2 C12 C13 C14 -174.2(9) . . . . ?
S3 C45 C44 C71 175.1(17) . . . . ?
S3 C45 C46 C72 -173.3(14) . . . . ?
S3 C45A C46A C72A -178.3(15) . . . . ?
S3 C45A C44A C71A 177.4(17) . . . . ?
C65 C66 C67 C68 1(3) . . . . ?
C66 C65 C70 C69 0(4) . . . . ?
C17 C16 C15 C14 0.2(18) . . . . ?
C17 C12 C13 C14 1.7(15) . . . . ?
C16 C17 C12 S2 174.2(7) . . . . ?
C16 C17 C12 C13 -1.7(13) . . . . ?
C12 C17 C16 C15 0.8(15) . . . . ?
C13 C14 C15 C16 -0.3(19) . . . . ?
C15 C14 C13 C12 -0.7(18) . . . . ?
C69 C68 C67 C66 0(4) . . . . ?
C68 C69 C70 C65 1(6) . . . . ?
C45 C44 C71 C73 -4(3) . . . . ?
C45 C46 C72 C73 0(3) . . . . ?
C44 C45 C46 C72 -3(3) . . . . ?
C44 C71 C73 C72 0(3) . . . . ?
C46 C45 C44 C71 5(3) . . . . ?
C46 C72 C73 C71 1(3) . . . . ?
O2 C52 C53 C54 -10(3) . . . . ?
O2 C52 C53 C1C -35.6(15) . . . . ?
O2 C55 C54 C53 4(3) . . . . ?
O2 C55 C1C C53 -43(2) . . . . ?
O1 C51 C50 C49 34.7(10) . . . . ?
C51 O1 C1A C49 28.3(14) . . . . ?
C51 O1 C1B C49 -32.2(15) . . . . ?
C50 C49 C1A O1 -5.1(15) . . . . ?
C50 C49 C1B O1 50.0(13) . . . . ?
C52 O2 C55 C54 -10.3(16) . . . . ?
C52 O2 C55 C1C 22.7(19) . . . . ?
C52 O2 Li1 U1 88.1(9) . . . . ?
C52 O2 Li1 S2 145.1(6) . . . . ?
C52 O2 Li1 S3 34.6(9) . . . . ?
C52 O2 Li1 O1 -89.5(8) . . . . ?
C52 C53 C54 C55 4(3) . . . . ?
C52 C53 C1C C55 47.9(19) . . . . ?
C55 O2 C52 C53 12.3(11) . . . . ?
C55 O2 Li1 U1 -94.4(10) . . . . ?
C55 O2 Li1 S2 -37.4(11) . . . . ?
C55 O2 Li1 S3 -147.9(8) . . . . ?
C55 O2 Li1 O1 88.0(10) . . . . ?
Li1 S2 C12 C17 127.2(7) . . . . ?
Li1 S2 C12 C13 -57.0(9) . . . . ?
Li1 S3 C45 C44 17(2) . . . . ?
Li1 S3 C45 C46 -173.1(14) . . . . ?
Li1 S3 C45A C46A -152.6(15) . . . . ?
Li1 S3 C45A C44A 29(2) . . . . ?
Li1 O2 C52 C53 -169.9(9) . . . . ?
Li1 O2 C55 C54 171.9(15) . . . . ?
Li1 O2 C55 C1C -155.1(17) . . . . ?
Li1 O1 C51 C50 148.2(8) . . . . ?
Li1 O1 C1A C49 -160.1(8) . . . . ?
Li1 O1 C1B C49 173.9(9) . . . . ?
Li2 S4 C65 C66 176.4(15) . . . . ?
Li2 S4 C65 C70 -7(2) . . . . ?
Li2 S4 C65A C70A -33(2) . . . . ?
Li2 S4 C65A C66A 148.5(19) . . . . ?
Li2 S1 C18 C19 -128.5(8) . . . . ?
Li2 S1 C18 C1J 54.3(9) . . . . ?
Li2 O3 C56 C57 165.1(9) . . . . ?
Li2 O3 C59 C1E 166.4(13) . . . . ?
Li2 O3 C1D C58 -172.3(15) . . . . ?
Li2 O4 C60 C1F 137.6(16) . . . . ?
Li2 O4 C60 C1G 168.8(15) . . . . ?
Li2 O4 C9 C4 -173.6(12) . . . . ?
Li2 O4 C10 C62 -132.2(18) . . . . ?
O3 Li2 O4 C60 172.8(9) . . . . ?
O3 Li2 O4 C9 21.6(14) . . . . ?
O3 Li2 O4 C10 -44.3(15) . . . . ?
O3 C56 C57 C58 16(3) . . . . ?
O3 C56 C57 C1E 39.4(10) . . . . ?
O3 C59 C1E C57 22.2(18) . . . . ?
O4 C60 C1F C62 1(2) . . . . ?
O4 C60 C1G C4 34(2) . . . . ?
C56 O3 C59 C1E 4(2) . . . . ?
C56 O3 C1D C58 -4.5(19) . . . . ?
C56 C57 C58 C1D -19(3) . . . . ?
C56 C57 C1E C59 -38.3(15) . . . . ?
C57 C58 C1D O3 14(3) . . . . ?
C60 O4 C9 C4 28.1(19) . . . . ?
C60 O4 C10 C62 22(2) . . . . ?
C59 O3 C56 C57 -34.4(16) . . . . ?
C70 C65 C66 C67 -1(3) . . . . ?
C70 C69 C68 C67 -2(6) . . . . ?
C9 O4 C60 C1G -38.9(19) . . . . ?
C9 C4 C1G C60 -17(3) . . . . ?
C10 O4 C60 C1F -11.6(19) . . . . ?
C10 C62 C1F C60 12(2) . . . . ?
C1A O1 C51 C50 -41.4(13) . . . . ?
C1A C49 C50 C51 -17.6(14) . . . . ?
C1B O1 C51 C50 -2.0(12) . . . . ?
C1B C49 C50 C51 -48.8(11) . . . . ?
C1D O3 C56 C57 -4.2(12) . . . . ?
C45A C46A C72A C73A -1(3) . . . . ?
C46A C45A C44A C71A 0(4) . . . . ?
C46A C72A C73A C71A 3(3) . . . . ?
C72A C73A C71A C44A -4(3) . . . . ?
C73A C71A C44A C45A 3(3) . . . . ?
C44A C45A C46A C72A 0(3) . . . . ?
C1F C62 C10 O4 -22(3) . . . . ?
C1G C4 C9 O4 -8(2) . . . . ?
C65A C70A C69A C68A 2(4) . . . . ?
C70A C65A C66A C67A 4(3) . . . . ?
C70A C69A C68A C67A -3(8) . . . . ?
C69A C68A C67A C66A 5(9) . . . . ?
C68A C67A C66A C65A -5(6) . . . . ?
C66A C65A C70A C69A -2(3) . . . . ?
C18 C19 C1H C1I -1.1(16) . . . . ?
C18 C1J C1K C1I 0.2(17) . . . . ?
C19 C18 C1J C1K 0.1(15) . . . . ?
C19 C1H C1I C1K 1.4(18) . . . . ?
C1H C1I C1K C1J -1.0(18) . . . . ?
C1J C18 C19 C1H 0.4(14) . . . . ?

_shelx_SHELXL_version_number     2018/3
_olex2_submission_special_instructions 'No special instructions were received'

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_NTUSePh2
_database_code_depnum_ccdc_archive 'CCDC 1836171'
loop_
_audit_author_name
_audit_author_address
'Nickolas Anderson'
;Los Alamos National Laboratory
United States of America
;
_audit_update_record             
;
2019-03-06 deposited with the CCDC.	2019-04-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C46 H54 N4 Se2 U'
_chemical_formula_weight         1058.88

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'
Se Se -0.0929 2.2259 '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/n'
_space_group_name_Hall           '-P 2yn'

_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+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   8.8361(8)
_cell_length_b                   16.7930(14)
_cell_length_c                   14.5778(12)
_cell_angle_alpha                90
_cell_angle_beta                 96.450(3)
_cell_angle_gamma                90
_cell_volume                     2149.4(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9763
_cell_measurement_theta_min      2.57
_cell_measurement_theta_max      30.31

_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.636
_exptl_crystal_F_000             1036
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.11
_exptl_absorpt_coefficient_mu    5.506
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.4286
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_process_details   
' SADABS-2014/2 - Bruker AXS area detector scaling and absorption correction'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            48471
_diffrn_reflns_av_unetI/netI     0.0136
_diffrn_reflns_av_R_equivalents  0.0276
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.857
_diffrn_reflns_theta_max         28.280
_diffrn_reflns_theta_full        26.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             5348
_reflns_number_gt                5071
_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.
 
 _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       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0186P)²+1.0501P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5348
_refine_ls_number_parameters     245
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0145
_refine_ls_R_factor_gt           0.0130
_refine_ls_wR_factor_ref         0.0349
_refine_ls_wR_factor_gt          0.0343
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_restrained_S_all      1.061
_refine_ls_shift/su_max          0.001
_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 0.500000 0.500000 0.500000 0.00770(3) Uani 1 2 d S . P . .
Se1 Se 0.65030(2) 0.59067(2) 0.37392(2) 0.01210(3) Uani 1 1 d . . . . .
N1 N 0.58974(13) 0.57262(7) 0.58868(8) 0.0107(2) Uani 1 1 d . . . . .
N2 N 0.26666(13) 0.59386(7) 0.47045(8) 0.0128(2) Uani 1 1 d . . . . .
C19 C 0.26092(16) 0.65375(9) 0.40902(10) 0.0150(3) Uani 1 1 d . . . . .
H19 H 0.342000 0.658904 0.371798 0.018 Uiso 1 1 calc R U . . .
C7 C 0.79825(18) 0.51189(9) 0.74416(11) 0.0139(3) Uani 1 1 d . . . . .
H7 H 0.716336 0.482400 0.705143 0.017 Uiso 1 1 calc R U . . .
C13 C 0.64449(16) 0.53697(9) 0.25735(10) 0.0141(3) Uani 1 1 d . . . . .
C6 C 0.79882(16) 0.59709(8) 0.71028(9) 0.0120(3) Uani 1 1 d . . . . .
C4 C 0.90609(17) 0.73009(9) 0.72716(10) 0.0177(3) Uani 1 1 d . . . . .
H4 H 0.983170 0.764941 0.754309 0.021 Uiso 1 1 calc R U . . .
C9 C 0.7605(2) 0.51010(10) 0.84460(12) 0.0217(3) Uani 1 1 d . . . . .
H9A H 0.843028 0.535491 0.884739 0.033 Uiso 1 1 calc R U . . .
H9B H 0.749187 0.454748 0.864011 0.033 Uiso 1 1 calc R U . . .
H9C H 0.665138 0.538927 0.849043 0.033 Uiso 1 1 calc R U . . .
C1 C 0.68954(15) 0.62609(8) 0.64037(9) 0.0104(2) Uani 1 1 d . . . . .
C10 C 0.41271(19) 0.75578(10) 0.61089(12) 0.0228(3) Uani 1 1 d . . . . .
H10A H 0.390101 0.707473 0.644516 0.034 Uiso 1 1 calc R U . . .
H10B H 0.322940 0.771106 0.568938 0.034 Uiso 1 1 calc R U . . .
H10C H 0.439509 0.798999 0.654911 0.034 Uiso 1 1 calc R U . . .
C23 C 0.14920(17) 0.58719(9) 0.52148(10) 0.0165(3) Uani 1 1 d . . . . .
H23 H 0.150512 0.544898 0.564838 0.020 Uiso 1 1 calc R U . . .
C2 C 0.68062(16) 0.70837(8) 0.61900(9) 0.0122(3) Uani 1 1 d . . . . .
C22 C 0.02705(18) 0.63896(11) 0.51367(11) 0.0208(3) Uani 1 1 d . . . . .
H22 H -0.053435 0.632224 0.551042 0.025 Uiso 1 1 calc R U . . .
C11 C 0.54687(17) 0.73975(8) 0.55493(10) 0.0151(3) Uani 1 1 d . . . . .
H11 H 0.514726 0.696606 0.509609 0.018 Uiso 1 1 calc R U . . .
C5 C 0.90749(17) 0.65038(9) 0.75153(10) 0.0158(3) Uani 1 1 d . . . . .
H5 H 0.984029 0.631476 0.797333 0.019 Uiso 1 1 calc R U . . .
C18 C 0.64581(18) 0.45406(9) 0.25067(11) 0.0178(3) Uani 1 1 d . . . . .
H18 H 0.641237 0.422489 0.304367 0.021 Uiso 1 1 calc R U . . .
C20 C 0.14258(18) 0.70847(9) 0.39717(11) 0.0193(3) Uani 1 1 d . . . . .
H20 H 0.143397 0.750252 0.353303 0.023 Uiso 1 1 calc R U . . .
C17 C 0.6538(2) 0.41738(11) 0.16565(12) 0.0244(3) Uani 1 1 d . . . . .
H17 H 0.655289 0.360926 0.161727 0.029 Uiso 1 1 calc R U . . .
C3 C 0.79111(17) 0.75879(9) 0.66267(10) 0.0166(3) Uani 1 1 d . . . . .
H3 H 0.787937 0.813956 0.648131 0.020 Uiso 1 1 calc R U . . .
C14 C 0.65053(18) 0.58232(10) 0.17770(11) 0.0206(3) Uani 1 1 d . . . . .
H14 H 0.649997 0.638805 0.181332 0.025 Uiso 1 1 calc R U . . .
C15 C 0.6574(2) 0.54519(12) 0.09289(11) 0.0274(4) Uani 1 1 d . . . . .
H15 H 0.660497 0.576566 0.038910 0.033 Uiso 1 1 calc R U . . .
C21 C 0.02334(18) 0.70091(10) 0.45059(12) 0.0220(3) Uani 1 1 d . . . . .
H21 H -0.059305 0.737422 0.444157 0.026 Uiso 1 1 calc R U . . .
C16 C 0.6596(2) 0.46294(12) 0.08649(12) 0.0282(4) Uani 1 1 d . . . . .
H16 H 0.665039 0.437862 0.028539 0.034 Uiso 1 1 calc R U . . .
C12 C 0.5808(2) 0.81330(11) 0.50000(13) 0.0285(4) Uani 1 1 d . . . . .
H12A H 0.491859 0.826390 0.456268 0.043 Uiso 1 1 calc R U . . .
H12B H 0.668409 0.802789 0.466072 0.043 Uiso 1 1 calc R U . . .
H12C H 0.604184 0.858146 0.542251 0.043 Uiso 1 1 calc R U . . .
C8 C 0.94953(18) 0.46980(10) 0.73618(12) 0.0220(3) Uani 1 1 d . . . . .
H8A H 0.972223 0.471580 0.671936 0.033 Uiso 1 1 calc R U . . .
H8B H 0.942436 0.414218 0.755715 0.033 Uiso 1 1 calc R U . . .
H8C H 1.030960 0.496625 0.775772 0.033 Uiso 1 1 calc R U . . .


_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 1.8861(11) 3_666 ?
U1 N1 1.8861(11) . ?
U1 N2 2.5926(12) . ?
U1 N2 2.5926(12) 3_666 ?
U1 Se1 2.8299(2) 3_666 ?
U1 Se1 2.8299(2) . ?
Se1 C13 1.9193(15) . ?
N1 C1 1.4150(17) . ?
N2 C19 1.3438(19) . ?
N2 C23 1.3478(18) . ?
C19 C20 1.388(2) . ?
C19 H19 0.9500 . ?
C7 C6 1.514(2) . ?
C7 C8 1.528(2) . ?
C7 C9 1.538(2) . ?
C7 H7 1.0000 . ?
C13 C14 1.395(2) . ?
C13 C18 1.396(2) . ?
C6 C5 1.398(2) . ?
C6 C1 1.4097(19) . ?
C4 C5 1.385(2) . ?
C4 C3 1.391(2) . ?
C4 H4 0.9500 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C1 C2 1.4166(19) . ?
C10 C11 1.536(2) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C23 C22 1.381(2) . ?
C23 H23 0.9500 . ?
C2 C3 1.391(2) . ?
C2 C11 1.516(2) . ?
C22 C21 1.386(2) . ?
C22 H22 0.9500 . ?
C11 C12 1.520(2) . ?
C11 H11 1.0000 . ?
C5 H5 0.9500 . ?
C18 C17 1.393(2) . ?
C18 H18 0.9500 . ?
C20 C21 1.385(2) . ?
C20 H20 0.9500 . ?
C17 C16 1.390(3) . ?
C17 H17 0.9500 . ?
C3 H3 0.9500 . ?
C14 C15 1.392(2) . ?
C14 H14 0.9500 . ?
C15 C16 1.385(3) . ?
C15 H15 0.9500 . ?
C21 H21 0.9500 . ?
C16 H16 0.9500 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?

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 N1 180.0 3_666 . ?
N1 U1 N2 90.80(4) 3_666 . ?
N1 U1 N2 89.20(4) . . ?
N1 U1 N2 89.20(4) 3_666 3_666 ?
N1 U1 N2 90.80(4) . 3_666 ?
N2 U1 N2 180.0 . 3_666 ?
N1 U1 Se1 84.57(4) 3_666 3_666 ?
N1 U1 Se1 95.43(4) . 3_666 ?
N2 U1 Se1 90.72(3) . 3_666 ?
N2 U1 Se1 89.28(3) 3_666 3_666 ?
N1 U1 Se1 95.43(4) 3_666 . ?
N1 U1 Se1 84.57(4) . . ?
N2 U1 Se1 89.28(3) . . ?
N2 U1 Se1 90.72(3) 3_666 . ?
Se1 U1 Se1 180.0 3_666 . ?
C13 Se1 U1 110.76(5) . . ?
C1 N1 U1 164.62(10) . . ?
C19 N2 C23 117.14(13) . . ?
C19 N2 U1 122.37(9) . . ?
C23 N2 U1 120.34(10) . . ?
N2 C19 C20 123.35(14) . . ?
N2 C19 H19 118.3 . . ?
C20 C19 H19 118.3 . . ?
C6 C7 C8 112.16(13) . . ?
C6 C7 C9 109.75(12) . . ?
C8 C7 C9 110.41(13) . . ?
C6 C7 H7 108.1 . . ?
C8 C7 H7 108.1 . . ?
C9 C7 H7 108.1 . . ?
C14 C13 C18 119.02(13) . . ?
C14 C13 Se1 118.74(12) . . ?
C18 C13 Se1 122.06(10) . . ?
C5 C6 C1 118.12(13) . . ?
C5 C6 C7 119.47(13) . . ?
C1 C6 C7 122.36(13) . . ?
C5 C4 C3 119.56(14) . . ?
C5 C4 H4 120.2 . . ?
C3 C4 H4 120.2 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C6 C1 N1 120.07(12) . . ?
C6 C1 C2 120.84(13) . . ?
N1 C1 C2 119.07(12) . . ?
C11 C10 H10A 109.5 . . ?
C11 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C11 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N2 C23 C22 123.06(14) . . ?
N2 C23 H23 118.5 . . ?
C22 C23 H23 118.5 . . ?
C3 C2 C1 118.31(13) . . ?
C3 C2 C11 121.91(13) . . ?
C1 C2 C11 119.66(12) . . ?
C23 C22 C21 119.16(14) . . ?
C23 C22 H22 120.4 . . ?
C21 C22 H22 120.4 . . ?
C2 C11 C12 114.87(13) . . ?
C2 C11 C10 109.17(12) . . ?
C12 C11 C10 110.32(13) . . ?
C2 C11 H11 107.4 . . ?
C12 C11 H11 107.4 . . ?
C10 C11 H11 107.4 . . ?
C4 C5 C6 121.50(14) . . ?
C4 C5 H5 119.2 . . ?
C6 C5 H5 119.2 . . ?
C17 C18 C13 120.32(14) . . ?
C17 C18 H18 119.8 . . ?
C13 C18 H18 119.8 . . ?
C21 C20 C19 118.66(14) . . ?
C21 C20 H20 120.7 . . ?
C19 C20 H20 120.7 . . ?
C16 C17 C18 120.37(17) . . ?
C16 C17 H17 119.8 . . ?
C18 C17 H17 119.8 . . ?
C4 C3 C2 121.34(14) . . ?
C4 C3 H3 119.3 . . ?
C2 C3 H3 119.3 . . ?
C15 C14 C13 120.29(16) . . ?
C15 C14 H14 119.9 . . ?
C13 C14 H14 119.9 . . ?
C16 C15 C14 120.60(15) . . ?
C16 C15 H15 119.7 . . ?
C14 C15 H15 119.7 . . ?
C20 C21 C22 118.62(14) . . ?
C20 C21 H21 120.7 . . ?
C22 C21 H21 120.7 . . ?
C15 C16 C17 119.40(15) . . ?
C15 C16 H16 120.3 . . ?
C17 C16 H16 120.3 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?

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
N2 U1 N1 C1 -125.1(4) . . . . ?
N2 U1 N1 C1 54.9(4) 3_666 . . . ?
Se1 U1 N1 C1 144.2(4) 3_666 . . . ?
Se1 U1 N1 C1 -35.8(4) . . . . ?
C23 N2 C19 C20 0.9(2) . . . . ?
U1 N2 C19 C20 -174.83(11) . . . . ?
C8 C7 C6 C5 -58.50(18) . . . . ?
C9 C7 C6 C5 64.61(18) . . . . ?
C8 C7 C6 C1 123.95(15) . . . . ?
C9 C7 C6 C1 -112.93(15) . . . . ?
C5 C6 C1 N1 172.00(12) . . . . ?
C7 C6 C1 N1 -10.4(2) . . . . ?
C5 C6 C1 C2 -6.20(19) . . . . ?
C7 C6 C1 C2 171.38(13) . . . . ?
U1 N1 C1 C6 -87.5(4) . . . . ?
U1 N1 C1 C2 90.7(4) . . . . ?
C19 N2 C23 C22 -0.7(2) . . . . ?
U1 N2 C23 C22 175.16(12) . . . . ?
C6 C1 C2 C3 5.8(2) . . . . ?
N1 C1 C2 C3 -172.37(12) . . . . ?
C6 C1 C2 C11 -170.11(13) . . . . ?
N1 C1 C2 C11 11.68(19) . . . . ?
N2 C23 C22 C21 0.1(3) . . . . ?
C3 C2 C11 C12 33.0(2) . . . . ?
C1 C2 C11 C12 -151.19(14) . . . . ?
C3 C2 C11 C10 -91.47(16) . . . . ?
C1 C2 C11 C10 84.33(16) . . . . ?
C3 C4 C5 C6 2.4(2) . . . . ?
C1 C6 C5 C4 2.1(2) . . . . ?
C7 C6 C5 C4 -175.59(14) . . . . ?
C14 C13 C18 C17 0.3(2) . . . . ?
Se1 C13 C18 C17 -174.84(13) . . . . ?
N2 C19 C20 C21 -0.6(2) . . . . ?
C13 C18 C17 C16 -0.4(2) . . . . ?
C5 C4 C3 C2 -2.8(2) . . . . ?
C1 C2 C3 C4 -1.3(2) . . . . ?
C11 C2 C3 C4 174.55(14) . . . . ?
C18 C13 C14 C15 0.2(2) . . . . ?
Se1 C13 C14 C15 175.48(13) . . . . ?
C13 C14 C15 C16 -0.6(2) . . . . ?
C19 C20 C21 C22 0.0(2) . . . . ?
C23 C22 C21 C20 0.3(3) . . . . ?
C14 C15 C16 C17 0.5(2) . . . . ?
C18 C17 C16 C15 0.0(3) . . . . ?

_refine_diff_density_max         0.680
_refine_diff_density_min         -0.453
_refine_diff_density_rms         0.076

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_dq0142
_database_code_depnum_ccdc_archive 'CCDC 1836175'
loop_
_audit_author_name
_audit_author_address
'Nickolas Anderson'
;Los Alamos National Laboratories
United States of America
;
_audit_update_record             
;
2018-04-10 deposited with the CCDC.	2019-04-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C64 H86 Li2 N2 O4 S4 U'
_chemical_formula_weight         1327.49

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'
S S 0.1246 0.1234 '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'
O O 0.0106 0.0060 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   12.6118(10)
_cell_length_b                   18.0426(15)
_cell_length_c                   13.8368(11)
_cell_angle_alpha                90
_cell_angle_beta                 98.6350(10)
_cell_angle_gamma                90
_cell_volume                     3112.9(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(1)
_cell_measurement_reflns_used    9806
_cell_measurement_theta_min      2.33
_cell_measurement_theta_max      33.71

_exptl_crystal_description       block
_exptl_crystal_colour            dark
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.416
_exptl_crystal_F_000             1356
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    2.788
_shelx_estimated_absorpt_T_min   0.592
_shelx_estimated_absorpt_T_max   0.808
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.592
_exptl_absorpt_correction_T_max  0.808
_exptl_absorpt_process_details   'SADABS v. 2014/3 (Bruker AXS, 2013)'
_exptl_absorpt_special_details   ?

_diffrn_ambient_temperature      100(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker D8 Quest with CMOS detector'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            70503
_diffrn_reflns_av_unetI/netI     0.0281
_diffrn_reflns_av_R_equivalents  0.0380
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.258
_diffrn_reflns_theta_max         33.724
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             12400
_reflns_number_gt                9692
_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.
 
 _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       'APEX2 V.2014.7-1 (Bruker AXS, 2014)'
_computing_cell_refinement       'APEX2 V.2014.7-1 (Bruker AXS, 2014)'
_computing_data_reduction        'SAINT, v. 8.34A (Bruker AXS, 2013)'
_computing_structure_solution    'SHELXS 2013/1 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELXTL, v. 2014/7, (Bruker AXS, 2014)'
_computing_publication_material  'SHELXTL, v. 2014/7, (Bruker AXS, 2014)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0161P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         12400
_refine_ls_number_parameters     353
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0400
_refine_ls_R_factor_gt           0.0236
_refine_ls_wR_factor_ref         0.0495
_refine_ls_wR_factor_gt          0.0467
_refine_ls_goodness_of_fit_ref   1.372
_refine_ls_restrained_S_all      1.372
_refine_ls_shift/su_max          0.000
_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 0.0000 0.0000 0.5000 0.00974(2) Uani 1 2 d S . P . .
S1 S 0.09652(3) 0.10208(2) 0.39477(3) 0.01306(6) Uani 1 1 d . . . . .
S2 S 0.16557(3) 0.05586(2) 0.64124(3) 0.01410(7) Uani 1 1 d . . . . .
N1 N -0.08875(9) 0.07929(6) 0.52517(8) 0.0122(2) Uani 1 1 d . . . . .
O1 O 0.09358(9) 0.26940(6) 0.52121(8) 0.0202(2) Uani 1 1 d . . . . .
O2 O 0.31389(8) 0.19945(6) 0.56407(8) 0.0213(2) Uani 1 1 d . . . . .
Li1 Li 0.1647(2) 0.17413(15) 0.5493(2) 0.0200(6) Uani 1 1 d . . . . .
C1 C 0.21696(11) 0.06901(8) 0.35754(10) 0.0137(3) Uani 1 1 d . . . . .
C2 C 0.24144(12) 0.09112(8) 0.26691(11) 0.0186(3) Uani 1 1 d . . . . .
H2 H 0.1924 0.1214 0.2255 0.022 Uiso 1 1 calc R U . . .
C3 C 0.33683(13) 0.06927(9) 0.23650(12) 0.0236(3) Uani 1 1 d . . . . .
H3 H 0.3526 0.0850 0.1747 0.028 Uiso 1 1 calc R U . . .
C4 C 0.40908(13) 0.02481(10) 0.29557(13) 0.0226(3) Uani 1 1 d . . . . .
H4 H 0.4743 0.0100 0.2747 0.027 Uiso 1 1 calc R U . . .
C5 C 0.38486(13) 0.00215(9) 0.38576(12) 0.0212(3) Uani 1 1 d . . . . .
H5 H 0.4338 -0.0285 0.4267 0.025 Uiso 1 1 calc R U . . .
C6 C 0.28948(12) 0.02400(9) 0.41673(11) 0.0176(3) Uani 1 1 d . . . . .
H6 H 0.2738 0.0081 0.4785 0.021 Uiso 1 1 calc R U . . .
C7 C 0.17107(12) 0.03869(8) 0.76761(10) 0.0134(3) Uani 1 1 d . . . . .
C8 C 0.25169(12) 0.07300(8) 0.83275(11) 0.0165(3) Uani 1 1 d . . . . .
H8 H 0.3024 0.1041 0.8083 0.020 Uiso 1 1 calc R U . . .
C9 C 0.25855(13) 0.06217(9) 0.93289(11) 0.0197(3) Uani 1 1 d . . . . .
H9 H 0.3137 0.0860 0.9762 0.024 Uiso 1 1 calc R U . . .
C10 C 0.18567(15) 0.01693(9) 0.97034(12) 0.0215(3) Uani 1 1 d . . . . .
H10 H 0.1899 0.0101 1.0389 0.026 Uiso 1 1 calc R U . . .
C11 C 0.10624(14) -0.01832(9) 0.90587(12) 0.0207(3) Uani 1 1 d . . . . .
H11 H 0.0562 -0.0498 0.9307 0.025 Uiso 1 1 calc R U . . .
C12 C 0.09921(13) -0.00806(8) 0.80542(11) 0.0169(3) Uani 1 1 d . . . . .
H12 H 0.0451 -0.0330 0.7623 0.020 Uiso 1 1 calc R U . . .
C13 C -0.14679(10) 0.14394(7) 0.53944(10) 0.0113(2) Uani 1 1 d . . . . .
C14 C -0.20473(11) 0.18018(8) 0.45754(10) 0.0123(3) Uani 1 1 d . . . . .
C15 C -0.25739(11) 0.24609(8) 0.47278(11) 0.0154(3) Uani 1 1 d . . . . .
H15 H -0.2954 0.2717 0.4183 0.018 Uiso 1 1 calc R U . . .
C16 C -0.25549(12) 0.27496(8) 0.56572(11) 0.0166(3) Uani 1 1 d . . . . .
H16 H -0.2910 0.3203 0.5746 0.020 Uiso 1 1 calc R U . . .
C17 C -0.20176(11) 0.23752(8) 0.64573(11) 0.0149(3) Uani 1 1 d . . . . .
H17 H -0.2024 0.2570 0.7094 0.018 Uiso 1 1 calc R U . . .
C18 C -0.14662(11) 0.17177(7) 0.63481(10) 0.0119(2) Uani 1 1 d . . . . .
C19 C -0.21737(11) 0.14568(8) 0.35649(10) 0.0148(3) Uani 1 1 d . . . . .
H19 H -0.1640 0.1045 0.3586 0.018 Uiso 1 1 calc R U . . .
C20 C -0.19633(13) 0.19931(9) 0.27613(11) 0.0221(3) Uani 1 1 d . . . . .
H20A H -0.2460 0.2413 0.2739 0.033 Uiso 1 1 calc R U . . .
H20B H -0.2072 0.1736 0.2130 0.033 Uiso 1 1 calc R U . . .
H20C H -0.1223 0.2174 0.2900 0.033 Uiso 1 1 calc R U . . .
C21 C -0.32960(12) 0.11125(8) 0.33279(11) 0.0191(3) Uani 1 1 d . . . . .
H21A H -0.3410 0.0766 0.3848 0.029 Uiso 1 1 calc R U . . .
H21B H -0.3356 0.0847 0.2704 0.029 Uiso 1 1 calc R U . . .
H21C H -0.3838 0.1505 0.3280 0.029 Uiso 1 1 calc R U . . .
C22 C -0.08934(11) 0.13239(8) 0.72458(10) 0.0140(3) Uani 1 1 d . . . . .
H22 H -0.0549 0.0869 0.7021 0.017 Uiso 1 1 calc R U . . .
C23 C -0.00062(12) 0.18060(8) 0.78064(11) 0.0180(3) Uani 1 1 d . . . . .
H23A H 0.0530 0.1920 0.7383 0.027 Uiso 1 1 calc R U . . .
H23B H 0.0337 0.1538 0.8386 0.027 Uiso 1 1 calc R U . . .
H23C H -0.0318 0.2268 0.8008 0.027 Uiso 1 1 calc R U . . .
C24 C -0.16834(13) 0.10786(9) 0.79202(11) 0.0213(3) Uani 1 1 d . . . . .
H24A H -0.2046 0.1514 0.8139 0.032 Uiso 1 1 calc R U . . .
H24B H -0.1294 0.0821 0.8489 0.032 Uiso 1 1 calc R U . . .
H24C H -0.2217 0.0744 0.7565 0.032 Uiso 1 1 calc R U . . .
C25 C 0.04812(13) 0.31955(8) 0.58445(12) 0.0221(3) Uani 1 1 d . . . . .
H25A H 0.0819 0.3129 0.6532 0.026 Uiso 1 1 calc R U . . .
H25B H -0.0301 0.3116 0.5799 0.026 Uiso 1 1 calc R U . . .
C26 C 0.07186(14) 0.39608(9) 0.54754(12) 0.0237(3) Uani 1 1 d . . . . .
H26A H 0.1421 0.4145 0.5803 0.028 Uiso 1 1 calc R U . . .
H26B H 0.0154 0.4319 0.5585 0.028 Uiso 1 1 calc R U . . .
C27 C 0.07320(15) 0.38397(9) 0.43814(12) 0.0256(4) Uani 1 1 d . . . . .
H27A H 0.0114 0.4089 0.3986 0.031 Uiso 1 1 calc R U . . .
H27B H 0.1403 0.4033 0.4186 0.031 Uiso 1 1 calc R U . . .
C28 C 0.06587(18) 0.30050(10) 0.42520(13) 0.0341(4) Uani 1 1 d . . . . .
H28A H -0.0077 0.2858 0.3964 0.041 Uiso 1 1 calc R U . . .
H28B H 0.1163 0.2832 0.3817 0.041 Uiso 1 1 calc R U . . .
C29 C 0.40495(13) 0.15679(9) 0.60941(14) 0.0258(4) Uani 1 1 d . . . . .
H29A H 0.3952 0.1036 0.5929 0.031 Uiso 1 1 calc R U . . .
H29B H 0.4147 0.1623 0.6814 0.031 Uiso 1 1 calc R U . . .
C30 C 0.50006(15) 0.18783(11) 0.56873(19) 0.0438(6) Uani 1 1 d . . . . .
H30A H 0.5098 0.1629 0.5069 0.053 Uiso 1 1 calc R U . . .
H30B H 0.5667 0.1828 0.6162 0.053 Uiso 1 1 calc R U . . .
C31 C 0.46944(15) 0.26896(11) 0.55145(17) 0.0378(5) Uani 1 1 d . . . . .
H31A H 0.4829 0.2980 0.6128 0.045 Uiso 1 1 calc R U . . .
H31B H 0.5086 0.2918 0.5022 0.045 Uiso 1 1 calc R U . . .
C32 C 0.35120(14) 0.26252(11) 0.51426(14) 0.0322(4) Uani 1 1 d . . . . .
H32A H 0.3131 0.3081 0.5292 0.039 Uiso 1 1 calc R U . . .
H32B H 0.3389 0.2546 0.4426 0.039 Uiso 1 1 calc R U . . .


_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 1.8809(12) . ?
U1 N1 1.8809(12) 3_556 ?
U1 S1 2.7434(4) . ?
U1 S1 2.7434(4) 3_556 ?
U1 S2 2.8232(4) . ?
U1 S2 2.8232(4) 3_556 ?
U1 Li1 3.771(3) 3_556 ?
U1 Li1 3.772(3) . ?
S1 C1 1.7788(15) . ?
S1 Li1 2.540(3) . ?
S2 C7 1.7668(14) . ?
S2 Li1 2.483(3) . ?
N1 C13 1.4068(17) . ?
O1 C28 1.436(2) . ?
O1 C25 1.4365(18) . ?
O1 Li1 1.951(3) . ?
O2 C32 1.4452(19) . ?
O2 C29 1.4452(19) . ?
O2 Li1 1.917(3) . ?
C1 C2 1.394(2) . ?
C1 C6 1.393(2) . ?
C2 C3 1.390(2) . ?
C3 C4 1.385(2) . ?
C4 C5 1.390(2) . ?
C5 C6 1.393(2) . ?
C7 C12 1.396(2) . ?
C7 C8 1.398(2) . ?
C8 C9 1.389(2) . ?
C9 C10 1.387(2) . ?
C10 C11 1.391(2) . ?
C11 C12 1.392(2) . ?
C13 C18 1.4116(18) . ?
C13 C14 1.4131(19) . ?
C14 C15 1.3935(19) . ?
C14 C19 1.5168(19) . ?
C15 C16 1.384(2) . ?
C16 C17 1.384(2) . ?
C17 C18 1.3947(19) . ?
C18 C22 1.517(2) . ?
C19 C20 1.527(2) . ?
C19 C21 1.535(2) . ?
C22 C24 1.529(2) . ?
C22 C23 1.533(2) . ?
C25 C26 1.518(2) . ?
C26 C27 1.532(2) . ?
C27 C28 1.518(2) . ?
C29 C30 1.507(2) . ?
C30 C31 1.524(3) . ?
C31 C32 1.507(3) . ?

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 N1 180.0 . 3_556 ?
N1 U1 S1 84.92(4) . . ?
N1 U1 S1 95.08(4) 3_556 . ?
N1 U1 S1 95.08(4) . 3_556 ?
N1 U1 S1 84.92(4) 3_556 3_556 ?
S1 U1 S1 180.000(13) . 3_556 ?
N1 U1 S2 89.95(4) . . ?
N1 U1 S2 90.04(4) 3_556 . ?
S1 U1 S2 77.686(12) . . ?
S1 U1 S2 102.314(11) 3_556 . ?
N1 U1 S2 90.05(4) . 3_556 ?
N1 U1 S2 89.95(4) 3_556 3_556 ?
S1 U1 S2 102.314(12) . 3_556 ?
S1 U1 S2 77.686(12) 3_556 3_556 ?
S2 U1 S2 180.000(13) . 3_556 ?
N1 U1 Li1 109.89(6) . 3_556 ?
N1 U1 Li1 70.11(6) 3_556 3_556 ?
S1 U1 Li1 137.68(4) . 3_556 ?
S1 U1 Li1 42.32(4) 3_556 3_556 ?
S2 U1 Li1 138.82(4) . 3_556 ?
S2 U1 Li1 41.18(4) 3_556 3_556 ?
N1 U1 Li1 70.11(6) . . ?
N1 U1 Li1 109.89(6) 3_556 . ?
S1 U1 Li1 42.32(4) . . ?
S1 U1 Li1 137.68(4) 3_556 . ?
S2 U1 Li1 41.18(4) . . ?
S2 U1 Li1 138.82(4) 3_556 . ?
Li1 U1 Li1 180.0 3_556 . ?
C1 S1 Li1 102.70(8) . . ?
C1 S1 U1 113.25(5) . . ?
Li1 S1 U1 91.02(6) . . ?
C7 S2 Li1 130.84(8) . . ?
C7 S2 U1 122.52(5) . . ?
Li1 S2 U1 90.36(6) . . ?
C13 N1 U1 173.38(10) . . ?
C28 O1 C25 104.68(12) . . ?
C28 O1 Li1 124.72(13) . . ?
C25 O1 Li1 130.32(12) . . ?
C32 O2 C29 109.39(12) . . ?
C32 O2 Li1 121.43(13) . . ?
C29 O2 Li1 128.50(12) . . ?
O2 Li1 O1 103.04(13) . . ?
O2 Li1 S2 102.79(12) . . ?
O1 Li1 S2 145.69(15) . . ?
O2 Li1 S1 114.47(13) . . ?
O1 Li1 S1 101.29(12) . . ?
S2 Li1 S1 88.07(9) . . ?
O2 Li1 U1 136.28(12) . . ?
O1 Li1 U1 118.28(11) . . ?
S2 Li1 U1 48.46(5) . . ?
S1 Li1 U1 46.66(5) . . ?
C2 C1 C6 118.75(14) . . ?
C2 C1 S1 118.60(11) . . ?
C6 C1 S1 122.61(11) . . ?
C3 C2 C1 120.65(15) . . ?
C4 C3 C2 120.56(15) . . ?
C3 C4 C5 119.10(15) . . ?
C4 C5 C6 120.60(15) . . ?
C5 C6 C1 120.33(15) . . ?
C12 C7 C8 118.44(13) . . ?
C12 C7 S2 123.06(11) . . ?
C8 C7 S2 118.50(11) . . ?
C9 C8 C7 120.74(14) . . ?
C10 C9 C8 120.67(15) . . ?
C9 C10 C11 118.91(15) . . ?
C12 C11 C10 120.75(15) . . ?
C11 C12 C7 120.47(14) . . ?
N1 C13 C18 119.89(12) . . ?
N1 C13 C14 119.23(12) . . ?
C18 C13 C14 120.88(12) . . ?
C15 C14 C13 118.31(13) . . ?
C15 C14 C19 120.22(13) . . ?
C13 C14 C19 121.29(12) . . ?
C16 C15 C14 121.30(14) . . ?
C15 C16 C17 119.84(13) . . ?
C16 C17 C18 121.37(13) . . ?
C17 C18 C13 118.23(13) . . ?
C17 C18 C22 119.59(12) . . ?
C13 C18 C22 122.18(12) . . ?
C14 C19 C20 113.91(12) . . ?
C14 C19 C21 109.20(12) . . ?
C20 C19 C21 110.86(12) . . ?
C18 C22 C24 111.19(12) . . ?
C18 C22 C23 111.73(12) . . ?
C24 C22 C23 110.39(12) . . ?
O1 C25 C26 104.55(12) . . ?
C25 C26 C27 103.57(13) . . ?
C28 C27 C26 104.39(13) . . ?
O1 C28 C27 106.05(14) . . ?
O2 C29 C30 105.37(14) . . ?
C29 C30 C31 102.62(15) . . ?
C32 C31 C30 101.19(16) . . ?
O2 C32 C31 105.91(14) . . ?

_refine_diff_density_max         0.857
_refine_diff_density_min         -0.957
_refine_diff_density_rms         0.098

_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  'Bruker Triumph curved graphite'
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_apx1737a_sq
_database_code_depnum_ccdc_archive 'CCDC 1836173'
loop_
_audit_author_name
_audit_author_address
'Nickolas Anderson'
;Los Alamos National Laboratory
United States of America
;
_audit_update_record             
;
2019-03-06 deposited with the CCDC.	2019-04-23 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_CHEMW03_apx1737a_sq         
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as
RESPONSE: molecular formula correct: four disordered solvent 
toluene molecules treated with Platon/Squeeze- results below.
;
_vrf_PLAT934_apx1737a_sq         
;
PROBLEM: Number of (Iobs-Icalc)/SigmaW > 10 Outliers ....         13 Check 
RESPONSE: Do not appear to be from systematic effects so did not omit.
;
# end Validation Reply Form

_audit_creation_date             2019-03-06
_audit_creation_method           
;
Olex2 1.2
(compiled Apr  3 2018 11:26:26 for OlexSys, GUI svn.r5486)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C48 H70 N2 Na2 O4 Te4 U'
_chemical_formula_sum            'C48 H70 N2 Na2 O4 Te4 U'
_chemical_formula_weight         1533.47
_chemical_melting_point          ?
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'
Na Na 0.0362 0.0249 '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'
Te Te -0.5308 1.6751 '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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
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                   12.2409(16)
_cell_length_b                   26.166(3)
_cell_length_c                   10.0543(13)
_cell_angle_alpha                90
_cell_angle_beta                 103.4770(10)
_cell_angle_gamma                90
_cell_volume                     3131.6(7)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9907
_cell_measurement_temperature    100
_cell_measurement_theta_min      2.22
_cell_measurement_theta_max      27.96
_shelx_estimated_absorpt_T_max   0.775
_shelx_estimated_absorpt_T_min   0.440
_exptl_absorpt_coefficient_mu    4.477
_exptl_absorpt_correction_T_min  0.439
_exptl_absorpt_correction_T_max  0.775
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/2 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.0982 before and 0.0391 after correction.
The Ratio of minimum to maximum transmission is 0.7181.
The λ/2 correction factor is 0.00150.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark orange'
_exptl_crystal_density_diffrn    1.626
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1452
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.06
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0296
_diffrn_reflns_av_unetI/netI     0.0232
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            32175
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         1.879
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 Quest with CMOS detector'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5787
_reflns_number_total             6388
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_data_collection       'APEX2 V.2014.7-1 (Bruker AXS, 2014)'
_computing_cell_refinement       'APEX2 V.2014.7-1 (Bruker AXS, 2014)'
_computing_data_reduction        'SAINT, v. 8.34A (Bruker AXS, 2013)'
_computing_structure_solution    'SHELXS 2013/1 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELXTL, v. 2014/7, (Bruker AXS, 2014)'
_computing_publication_material  'SHELXTL, v. 2014/7, (Bruker AXS, 2014)'
_refine_diff_density_max         1.368
_refine_diff_density_min         -1.697
_refine_diff_density_rms         0.133
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.192
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         6388
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0385
_refine_ls_R_factor_gt           0.0333
_refine_ls_restrained_S_all      1.192
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+19.3757P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0640
_refine_ls_wR_factor_ref         0.0651
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,
 H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12)
2.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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 1.000000 0.000000 0.500000 0.01442(6) Uani 1 2 d S T P . .
Te1 Te 0.77263(3) 0.04114(2) 0.33027(3) 0.01877(8) Uani 1 1 d . . . . .
Te2 Te 0.91410(3) 0.01315(2) 0.76655(3) 0.01878(8) Uani 1 1 d . . . . .
Na1 Na 0.86827(16) 0.05055(8) 0.0575(2) 0.0240(4) Uani 1 1 d . . . . .
O1 O 0.6890(3) 0.07606(16) -0.0550(4) 0.0289(9) Uani 1 1 d . . . . .
O2 O 0.9500(3) 0.12973(15) 0.0672(4) 0.0331(9) Uani 1 1 d . . . . .
N1 N 1.0722(3) 0.06090(16) 0.5602(4) 0.0193(9) Uani 1 1 d . . . . .
C1 C 0.7542(4) 0.1199(2) 0.3699(6) 0.0254(12) Uani 1 1 d . . . . .
C2 C 0.7723(5) 0.1372(2) 0.5047(6) 0.0373(15) Uani 1 1 d . . . . .
H2 H 0.793858 0.114025 0.576099 0.045 Uiso 1 1 calc R . . . .
C3 C 0.7588(6) 0.1877(3) 0.5340(8) 0.0534(19) Uani 1 1 d . . . . .
H3 H 0.770848 0.198342 0.624479 0.064 Uiso 1 1 calc R . . . .
C4 C 0.7278(6) 0.2224(3) 0.4307(9) 0.054(2) Uani 1 1 d . . . . .
H4 H 0.719653 0.256653 0.450730 0.065 Uiso 1 1 calc R . . . .
C5 C 0.7088(6) 0.2065(3) 0.2968(9) 0.053(2) Uani 1 1 d . . . . .
H5 H 0.686947 0.230060 0.226304 0.064 Uiso 1 1 calc R . . . .
C6 C 0.7221(5) 0.1553(2) 0.2669(7) 0.0405(16) Uani 1 1 d . . . . .
H6 H 0.709085 0.144784 0.176143 0.049 Uiso 1 1 calc R . . . .
C7 C 0.7691(4) -0.0328(2) 0.7585(5) 0.0200(10) Uani 1 1 d . . . . .
C8 C 0.7670(5) -0.0694(2) 0.8577(5) 0.0255(12) Uani 1 1 d . . . . .
H8 H 0.831649 -0.075627 0.925373 0.031 Uiso 1 1 calc R . . . .
C9 C 0.6710(5) -0.0965(2) 0.8573(6) 0.0328(13) Uani 1 1 d . . . . .
H9 H 0.671321 -0.121043 0.924279 0.039 Uiso 1 1 calc R . . . .
C10 C 0.5735(5) -0.0876(2) 0.7581(6) 0.0334(14) Uani 1 1 d . . . . .
H10 H 0.508356 -0.105904 0.758069 0.040 Uiso 1 1 calc R . . . .
C11 C 0.5745(5) -0.0514(2) 0.6599(6) 0.0327(13) Uani 1 1 d . . . . .
H11 H 0.509320 -0.044964 0.593338 0.039 Uiso 1 1 calc R . . . .
C12 C 0.6711(4) -0.0244(2) 0.6586(5) 0.0260(12) Uani 1 1 d . . . . .
H12 H 0.670657 -0.000395 0.590338 0.031 Uiso 1 1 calc R . . . .
C13 C 1.1393(4) 0.1053(2) 0.6239(5) 0.0229(11) Uani 1 1 d . . . . .
C14 C 1.1760(5) 0.0968(2) 0.7772(5) 0.0290(13) Uani 1 1 d . . . . .
H14A H 1.110985 0.091981 0.813872 0.043 Uiso 1 1 calc GR . . . .
H14B H 1.217255 0.126088 0.819482 0.043 Uiso 1 1 calc GR . . . .
H14C H 1.222947 0.067056 0.795318 0.043 Uiso 1 1 calc GR . . . .
C15 C 1.2418(5) 0.1100(2) 0.5628(6) 0.0365(14) Uani 1 1 d . . . . .
H15A H 1.286235 0.079452 0.582124 0.055 Uiso 1 1 calc GR . . . .
H15B H 1.285936 0.138859 0.602281 0.055 Uiso 1 1 calc GR . . . .
H15C H 1.217696 0.114476 0.465627 0.055 Uiso 1 1 calc GR . . . .
C16 C 1.0673(5) 0.1532(2) 0.5934(6) 0.0354(14) Uani 1 1 d . . . . .
H16A H 1.040970 0.157090 0.496246 0.053 Uiso 1 1 calc GR . . . .
H16B H 1.111306 0.182498 0.630242 0.053 Uiso 1 1 calc GR . . . .
H16C H 1.004220 0.150262 0.634487 0.053 Uiso 1 1 calc GR . . . .
C17 C 0.5897(4) 0.0466(2) -0.0530(6) 0.0294(12) Uani 1 1 d . . . . .
H17A H 0.576627 0.045626 0.038470 0.035 Uiso 1 1 calc R . . . .
H17B H 0.597436 0.011833 -0.083150 0.035 Uiso 1 1 calc R . . . .
C18 C 0.4954(5) 0.0733(3) -0.1493(8) 0.0478(18) Uani 1 1 d . . . . .
H18A H 0.460814 0.098568 -0.101609 0.057 Uiso 1 1 calc R . . . .
H18B H 0.438492 0.049121 -0.194098 0.057 Uiso 1 1 calc R . . . .
C19 C 0.5516(6) 0.0983(3) -0.2510(7) 0.0470(18) Uani 1 1 d . . . . .
H19A H 0.559006 0.074666 -0.322721 0.056 Uiso 1 1 calc R . . . .
H19B H 0.510316 0.128229 -0.291991 0.056 Uiso 1 1 calc R . . . .
C20 C 0.6644(5) 0.1127(3) -0.1633(7) 0.0393(15) Uani 1 1 d . . . . .
H20A H 0.721257 0.111709 -0.216201 0.047 Uiso 1 1 calc R . . . .
H20B H 0.662132 0.146873 -0.126700 0.047 Uiso 1 1 calc R . . . .
C21 C 1.0016(5) 0.1509(2) 0.1991(6) 0.0350(14) Uani 1 1 d . . . . .
H21A H 1.073236 0.134479 0.236652 0.042 Uiso 1 1 calc R . . . .
H21B H 0.953464 0.146173 0.262271 0.042 Uiso 1 1 calc R . . . .
C22 C 1.0177(10) 0.2061(3) 0.1757(8) 0.084(3) Uani 1 1 d . . . . .
H22A H 1.083795 0.219341 0.239139 0.101 Uiso 1 1 calc R . . . .
H22B H 0.952590 0.225896 0.183670 0.101 Uiso 1 1 calc R . . . .
C23 C 1.0327(9) 0.2062(3) 0.0294(8) 0.080(3) Uani 1 1 d . . . . .
H23A H 1.013873 0.239249 -0.013626 0.096 Uiso 1 1 calc R . . . .
H23B H 1.109012 0.197367 0.026371 0.096 Uiso 1 1 calc R . . . .
C24 C 0.9524(6) 0.1665(2) -0.0362(7) 0.0426(16) Uani 1 1 d . . . . .
H24A H 0.878412 0.181145 -0.070617 0.051 Uiso 1 1 calc R . . . .
H24B H 0.976981 0.150926 -0.111796 0.051 Uiso 1 1 calc R . . . .


_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 Te1 3.0989(4) 3_756 ?
U1 Te1 3.0989(4) . ?
U1 Te2 3.1176(5) . ?
U1 Te2 3.1176(5) 3_756 ?
U1 N1 1.854(4) 3_756 ?
U1 N1 1.854(4) . ?
Te1 Na1 3.232(2) . ?
Te1 C1 2.122(5) . ?
Te2 Na1 3.255(2) 1_556 ?
Te2 Na1 3.287(2) 3_756 ?
Te2 C7 2.131(5) . ?
Na1 O1 2.320(4) . ?
Na1 O2 2.293(4) . ?
O1 C17 1.444(6) . ?
O1 C20 1.429(7) . ?
O2 C21 1.440(7) . ?
O2 C24 1.422(7) . ?
N1 C13 1.480(7) . ?
C1 C2 1.397(8) . ?
C1 C6 1.375(8) . ?
C2 H2 0.9300 . ?
C2 C3 1.371(9) . ?
C3 H3 0.9300 . ?
C3 C4 1.365(10) . ?
C4 H4 0.9300 . ?
C4 C5 1.375(11) . ?
C5 H5 0.9300 . ?
C5 C6 1.393(9) . ?
C6 H6 0.9300 . ?
C7 C8 1.385(7) . ?
C7 C12 1.391(7) . ?
C8 H8 0.9300 . ?
C8 C9 1.373(8) . ?
C9 H9 0.9300 . ?
C9 C10 1.385(8) . ?
C10 H10 0.9300 . ?
C10 C11 1.370(8) . ?
C11 H11 0.9300 . ?
C11 C12 1.380(8) . ?
C12 H12 0.9300 . ?
C13 C14 1.519(7) . ?
C13 C15 1.525(8) . ?
C13 C16 1.521(8) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C17 C18 1.495(8) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C18 C19 1.509(9) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C19 C20 1.503(9) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C21 C22 1.484(10) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C22 C23 1.523(12) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C23 C24 1.476(10) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?

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
Te1 U1 Te1 180.0 3_756 . ?
Te1 U1 Te2 90.259(12) . 3_756 ?
Te1 U1 Te2 90.258(12) 3_756 . ?
Te1 U1 Te2 89.742(12) . . ?
Te1 U1 Te2 89.742(12) 3_756 3_756 ?
Te2 U1 Te2 180.0 3_756 . ?
N1 U1 Te1 100.36(13) 3_756 3_756 ?
N1 U1 Te1 100.35(13) . . ?
N1 U1 Te1 79.65(13) . 3_756 ?
N1 U1 Te1 79.65(13) 3_756 . ?
N1 U1 Te2 81.68(12) 3_756 3_756 ?
N1 U1 Te2 98.32(12) 3_756 . ?
N1 U1 Te2 98.33(12) . 3_756 ?
N1 U1 Te2 81.68(12) . . ?
N1 U1 N1 180.0 3_756 . ?
U1 Te1 Na1 92.13(4) . . ?
C1 Te1 U1 110.82(14) . . ?
C1 Te1 Na1 99.24(16) . . ?
U1 Te2 Na1 165.70(4) . 1_556 ?
U1 Te2 Na1 90.75(4) . 3_756 ?
Na1 Te2 Na1 87.52(5) 1_556 3_756 ?
C7 Te2 U1 110.50(13) . . ?
C7 Te2 Na1 107.31(14) . 3_756 ?
C7 Te2 Na1 83.52(13) . 1_556 ?
Te1 Na1 Te2 85.02(5) . 3_756 ?
Te1 Na1 Te2 155.77(8) . 1_554 ?
Te2 Na1 Te2 92.48(5) 1_554 3_756 ?
O1 Na1 Te1 86.98(11) . . ?
O1 Na1 Te2 89.40(11) . 1_554 ?
O1 Na1 Te2 164.56(13) . 3_756 ?
O2 Na1 Te1 105.89(12) . . ?
O2 Na1 Te2 98.32(12) . 1_554 ?
O2 Na1 Te2 98.31(12) . 3_756 ?
O2 Na1 O1 96.57(16) . . ?
C17 O1 Na1 122.9(3) . . ?
C20 O1 Na1 124.9(3) . . ?
C20 O1 C17 109.9(4) . . ?
C21 O2 Na1 118.7(3) . . ?
C24 O2 Na1 131.6(4) . . ?
C24 O2 C21 109.5(5) . . ?
C13 N1 U1 172.1(4) . . ?
C2 C1 Te1 119.8(4) . . ?
C6 C1 Te1 122.4(5) . . ?
C6 C1 C2 117.8(6) . . ?
C1 C2 H2 119.3 . . ?
C3 C2 C1 121.3(6) . . ?
C3 C2 H2 119.3 . . ?
C2 C3 H3 119.9 . . ?
C4 C3 C2 120.2(7) . . ?
C4 C3 H3 119.9 . . ?
C3 C4 H4 120.1 . . ?
C3 C4 C5 119.9(7) . . ?
C5 C4 H4 120.1 . . ?
C4 C5 H5 120.0 . . ?
C4 C5 C6 120.0(7) . . ?
C6 C5 H5 120.0 . . ?
C1 C6 C5 120.8(7) . . ?
C1 C6 H6 119.6 . . ?
C5 C6 H6 119.6 . . ?
C8 C7 Te2 121.1(4) . . ?
C8 C7 C12 118.2(5) . . ?
C12 C7 Te2 120.6(4) . . ?
C7 C8 H8 119.5 . . ?
C9 C8 C7 120.9(5) . . ?
C9 C8 H8 119.5 . . ?
C8 C9 H9 119.7 . . ?
C8 C9 C10 120.6(5) . . ?
C10 C9 H9 119.7 . . ?
C9 C10 H10 120.5 . . ?
C11 C10 C9 118.9(5) . . ?
C11 C10 H10 120.5 . . ?
C10 C11 H11 119.6 . . ?
C10 C11 C12 120.8(5) . . ?
C12 C11 H11 119.6 . . ?
C7 C12 H12 119.7 . . ?
C11 C12 C7 120.6(5) . . ?
C11 C12 H12 119.7 . . ?
N1 C13 C14 109.1(4) . . ?
N1 C13 C15 108.3(4) . . ?
N1 C13 C16 108.8(4) . . ?
C14 C13 C15 110.1(5) . . ?
C14 C13 C16 110.2(5) . . ?
C16 C13 C15 110.2(5) . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C13 C16 H16A 109.5 . . ?
C13 C16 H16B 109.5 . . ?
C13 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
O1 C17 H17A 110.6 . . ?
O1 C17 H17B 110.6 . . ?
O1 C17 C18 105.5(5) . . ?
H17A C17 H17B 108.8 . . ?
C18 C17 H17A 110.6 . . ?
C18 C17 H17B 110.6 . . ?
C17 C18 H18A 111.0 . . ?
C17 C18 H18B 111.0 . . ?
C17 C18 C19 103.6(5) . . ?
H18A C18 H18B 109.0 . . ?
C19 C18 H18A 111.0 . . ?
C19 C18 H18B 111.0 . . ?
C18 C19 H19A 111.3 . . ?
C18 C19 H19B 111.3 . . ?
H19A C19 H19B 109.2 . . ?
C20 C19 C18 102.3(5) . . ?
C20 C19 H19A 111.3 . . ?
C20 C19 H19B 111.3 . . ?
O1 C20 C19 106.3(5) . . ?
O1 C20 H20A 110.5 . . ?
O1 C20 H20B 110.5 . . ?
C19 C20 H20A 110.5 . . ?
C19 C20 H20B 110.5 . . ?
H20A C20 H20B 108.7 . . ?
O2 C21 H21A 110.6 . . ?
O2 C21 H21B 110.6 . . ?
O2 C21 C22 105.9(5) . . ?
H21A C21 H21B 108.7 . . ?
C22 C21 H21A 110.6 . . ?
C22 C21 H21B 110.6 . . ?
C21 C22 H22A 111.4 . . ?
C21 C22 H22B 111.4 . . ?
C21 C22 C23 101.9(7) . . ?
H22A C22 H22B 109.3 . . ?
C23 C22 H22A 111.4 . . ?
C23 C22 H22B 111.4 . . ?
C22 C23 H23A 111.3 . . ?
C22 C23 H23B 111.3 . . ?
H23A C23 H23B 109.2 . . ?
C24 C23 C22 102.3(6) . . ?
C24 C23 H23A 111.3 . . ?
C24 C23 H23B 111.3 . . ?
O2 C24 C23 105.9(5) . . ?
O2 C24 H24A 110.5 . . ?
O2 C24 H24B 110.5 . . ?
C23 C24 H24A 110.5 . . ?
C23 C24 H24B 110.5 . . ?
H24A C24 H24B 108.7 . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.395 0.250 -0.834 289.0 72.1 ?
2 0.605 0.750 -0.049 289.0 76.0 ?

_olex2_submission_special_instructions 'No special instructions were received'
