# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 1510088'
_audit_update_record             
;
2016-10-16 deposited with the CCDC.
2017-08-14 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            'C42 H48 Cl2 N14 Th2'
_chemical_formula_weight         1283.92

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Th Th -7.2400 8.8979 '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                   13.3667(4)
_cell_length_b                   9.8584(3)
_cell_length_c                   16.0849(5)
_cell_angle_alpha                90
_cell_angle_beta                 95.5180(10)
_cell_angle_gamma                90
_cell_volume                     2109.75(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3920
_cell_measurement_theta_min      1.89
_cell_measurement_theta_max      26.39

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.021
_exptl_crystal_F_000             1224
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    7.218
_shelx_estimated_absorpt_T_min   0.326
_shelx_estimated_absorpt_T_max   0.714
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.472
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_process_details   'Blessing, 1995'
_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 Kappa Quazar'
_diffrn_measurement_method       'omega phi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            16056
_diffrn_reflns_av_unetI/netI     0.0387
_diffrn_reflns_av_R_equivalents  0.0437
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.894
_diffrn_reflns_theta_max         26.396
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             4272
_reflns_number_gt                3920
_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 ApexII suite, 2015'
_computing_cell_refinement       'Bruker ApexII suite, 2015'
_computing_data_reduction        'Bruker ApexII suite, 2015'
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0172P)²+1.8275P] 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         4272
_refine_ls_number_parameters     271
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0249
_refine_ls_R_factor_gt           0.0222
_refine_ls_wR_factor_ref         0.0547
_refine_ls_wR_factor_gt          0.0532
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_restrained_S_all      1.078
_refine_ls_shift/su_max          0.004
_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
Th1 Th 0.34618(2) 0.45665(2) 0.54823(2) 0.01266(5) Uani 1 1 d . . . . .
Cl1 Cl 0.44114(6) 0.62672(8) 0.43032(4) 0.01647(16) Uani 1 1 d . . . . .
N11 N 0.4310(2) 0.6674(3) 0.63143(17) 0.0191(6) Uani 1 1 d . . . . .
N1 N 0.2923(2) 0.2481(3) 0.65165(16) 0.0199(6) Uani 1 1 d . . . . .
N21 N 0.2662(2) 0.3772(3) 0.39760(16) 0.0170(6) Uani 1 1 d . . . . .
N31 N 0.20670(19) 0.6401(3) 0.51268(16) 0.0169(6) Uani 1 1 d . . . . .
N20 N 0.3328(2) 0.2298(3) 0.49273(17) 0.0181(6) Uani 1 1 d . . . . .
N10 N 0.3919(2) 0.4769(3) 0.69529(17) 0.0191(6) Uani 1 1 d . . . . .
N30 N 0.1752(2) 0.4460(3) 0.57622(18) 0.0205(7) Uani 1 1 d . . . . .
C23 C 0.2298(2) 0.1429(4) 0.3664(2) 0.0205(7) Uani 1 1 d . . . . .
H23 H 0.2337 0.0500 0.3821 0.025 Uiso 1 1 calc R U . . .
C16 C 0.4765(3) 0.7874(4) 0.6282(2) 0.0220(8) Uani 1 1 d . . . . .
H16 H 0.4631 0.8409 0.5793 0.026 Uiso 1 1 calc R U . . .
C20 C 0.3526(3) 0.1299(4) 0.6299(2) 0.0252(8) Uani 1 1 d . . . . .
H20A H 0.3323 0.0492 0.6608 0.030 Uiso 1 1 calc R U . . .
H20B H 0.4246 0.1478 0.6469 0.030 Uiso 1 1 calc R U . . .
C31 C 0.1245(3) 0.3547(4) 0.6286(2) 0.0235(8) Uani 1 1 d . . . . .
H31A H 0.0543 0.3393 0.6047 0.028 Uiso 1 1 calc R U . . .
H31B H 0.1234 0.3930 0.6854 0.028 Uiso 1 1 calc R U . . .
C32 C 0.1386(3) 0.5690(4) 0.5548(2) 0.0174(7) Uani 1 1 d . . . . .
C22 C 0.2766(2) 0.2440(3) 0.4188(2) 0.0176(7) Uani 1 1 d . . . . .
C35 C 0.0962(3) 0.8306(4) 0.5014(2) 0.0273(9) Uani 1 1 d . . . . .
H35 H 0.0827 0.9204 0.4821 0.033 Uiso 1 1 calc R U . . .
C15 C 0.5419(3) 0.8376(4) 0.6919(2) 0.0244(8) Uani 1 1 d . . . . .
H15 H 0.5697 0.9259 0.6890 0.029 Uiso 1 1 calc R U . . .
C12 C 0.4492(3) 0.5892(4) 0.7008(2) 0.0200(7) Uani 1 1 d . . . . .
C33 C 0.0469(2) 0.6297(4) 0.5716(2) 0.0228(8) Uani 1 1 d . . . . .
H33 H 0.0000 0.5817 0.6013 0.027 Uiso 1 1 calc R U . . .
C21 C 0.3380(3) 0.1011(4) 0.5353(2) 0.0251(8) Uani 1 1 d . . . . .
H21A H 0.3950 0.0471 0.5182 0.030 Uiso 1 1 calc R U . . .
H21B H 0.2752 0.0492 0.5212 0.030 Uiso 1 1 calc R U . . .
C26 C 0.2147(3) 0.4113(4) 0.3254(2) 0.0194(7) Uani 1 1 d . . . . .
H26 H 0.2080 0.5047 0.3117 0.023 Uiso 1 1 calc R U . . .
C14 C 0.5661(3) 0.7541(4) 0.7610(2) 0.0267(8) Uani 1 1 d . . . . .
H14 H 0.6138 0.7842 0.8048 0.032 Uiso 1 1 calc R U . . .
C13 C 0.5222(3) 0.6299(4) 0.7667(2) 0.0217(7) Uani 1 1 d . . . . .
H13 H 0.5397 0.5722 0.8131 0.026 Uiso 1 1 calc R U . . .
C10 C 0.3129(3) 0.2802(4) 0.7423(2) 0.0251(8) Uani 1 1 d . . . . .
H10A H 0.3249 0.1951 0.7744 0.030 Uiso 1 1 calc R U . . .
H10B H 0.2535 0.3256 0.7622 0.030 Uiso 1 1 calc R U . . .
C30 C 0.1832(3) 0.2229(4) 0.6317(2) 0.0235(8) Uani 1 1 d . . . . .
H30A H 0.1588 0.1626 0.6747 0.028 Uiso 1 1 calc R U . . .
H30B H 0.1719 0.1764 0.5770 0.028 Uiso 1 1 calc R U . . .
C25 C 0.1708(3) 0.3179(4) 0.2701(2) 0.0222(8) Uani 1 1 d . . . . .
H25 H 0.1365 0.3454 0.2184 0.027 Uiso 1 1 calc R U . . .
C36 C 0.1850(3) 0.7662(4) 0.4882(2) 0.0233(8) Uani 1 1 d . . . . .
H36 H 0.2330 0.8146 0.4600 0.028 Uiso 1 1 calc R U . . .
C11 C 0.4032(3) 0.3713(4) 0.7575(2) 0.0224(8) Uani 1 1 d . . . . .
H11A H 0.4065 0.4109 0.8143 0.027 Uiso 1 1 calc R U . . .
H11B H 0.4657 0.3194 0.7523 0.027 Uiso 1 1 calc R U . . .
C34 C 0.0274(3) 0.7593(4) 0.5440(2) 0.0283(9) Uani 1 1 d . . . . .
H34 H -0.0343 0.8012 0.5542 0.034 Uiso 1 1 calc R U . . .
C24 C 0.1783(2) 0.1819(4) 0.2921(2) 0.0226(8) Uani 1 1 d . . . . .
H24 H 0.1476 0.1151 0.2555 0.027 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
Th1 N30 2.373(3) . ?
Th1 N10 2.394(3) . ?
Th1 N20 2.408(3) . ?
Th1 N31 2.621(3) . ?
Th1 N11 2.665(3) . ?
Th1 N21 2.670(3) . ?
Th1 N1 2.783(3) . ?
Th1 Cl1 2.9124(8) . ?
Th1 Cl1 2.9475(8) 3_666 ?
Th1 C12 2.996(3) . ?
Th1 C32 2.999(3) . ?
Th1 C22 3.037(3) . ?
Cl1 Th1 2.9475(8) 3_666 ?
N11 C16 1.333(4) . ?
N11 C12 1.359(4) . ?
N1 C20 1.478(5) . ?
N1 C30 1.483(4) . ?
N1 C10 1.492(4) . ?
N21 C26 1.334(4) . ?
N21 C22 1.361(4) . ?
N31 C36 1.328(4) . ?
N31 C32 1.377(4) . ?
N20 C22 1.351(4) . ?
N20 C21 1.441(5) . ?
N10 C12 1.344(5) . ?
N10 C11 1.442(4) . ?
N30 C32 1.340(4) . ?
N30 C31 1.446(4) . ?
C23 C24 1.375(5) . ?
C23 C22 1.412(5) . ?
C23 H23 0.9500 . ?
C16 C15 1.374(5) . ?
C16 H16 0.9500 . ?
C20 C21 1.541(5) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C31 C30 1.517(5) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 C33 1.413(5) . ?
C35 C36 1.380(5) . ?
C35 C34 1.389(6) . ?
C35 H35 0.9500 . ?
C15 C14 1.396(5) . ?
C15 H15 0.9500 . ?
C12 C13 1.428(5) . ?
C33 C34 1.370(5) . ?
C33 H33 0.9500 . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C26 C25 1.372(5) . ?
C26 H26 0.9500 . ?
C14 C13 1.365(5) . ?
C14 H14 0.9500 . ?
C13 H13 0.9500 . ?
C10 C11 1.506(5) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C25 C24 1.388(5) . ?
C25 H25 0.9500 . ?
C36 H36 0.9500 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C34 H34 0.9500 . ?
C24 H24 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
N30 Th1 N10 88.57(10) . . ?
N30 Th1 N20 89.48(10) . . ?
N10 Th1 N20 116.53(9) . . ?
N30 Th1 N31 52.71(9) . . ?
N10 Th1 N31 105.46(9) . . ?
N20 Th1 N31 122.27(9) . . ?
N30 Th1 N11 108.05(9) . . ?
N10 Th1 N11 51.90(9) . . ?
N20 Th1 N11 157.38(9) . . ?
N31 Th1 N11 80.26(8) . . ?
N30 Th1 N21 81.40(9) . . ?
N10 Th1 N21 164.38(9) . . ?
N20 Th1 N21 51.85(9) . . ?
N31 Th1 N21 77.88(8) . . ?
N11 Th1 N21 142.96(8) . . ?
N30 Th1 N1 62.92(9) . . ?
N10 Th1 N1 61.77(9) . . ?
N20 Th1 N1 61.39(9) . . ?
N31 Th1 N1 114.88(8) . . ?
N11 Th1 N1 113.46(8) . . ?
N21 Th1 N1 102.81(8) . . ?
N30 Th1 Cl1 129.55(7) . . ?
N10 Th1 Cl1 120.65(7) . . ?
N20 Th1 Cl1 108.34(7) . . ?
N31 Th1 Cl1 78.82(6) . . ?
N11 Th1 Cl1 71.77(6) . . ?
N21 Th1 Cl1 74.89(6) . . ?
N1 Th1 Cl1 165.62(6) . . ?
N30 Th1 Cl1 154.27(7) . 3_666 ?
N10 Th1 Cl1 75.88(8) . 3_666 ?
N20 Th1 Cl1 79.68(7) . 3_666 ?
N31 Th1 Cl1 151.14(6) . 3_666 ?
N11 Th1 Cl1 78.45(6) . 3_666 ?
N21 Th1 Cl1 108.78(6) . 3_666 ?
N1 Th1 Cl1 91.50(6) . 3_666 ?
Cl1 Th1 Cl1 76.17(2) . 3_666 ?
N30 Th1 C12 103.81(10) . . ?
N10 Th1 C12 25.93(10) . . ?
N20 Th1 C12 136.11(9) . . ?
N31 Th1 C12 97.99(9) . . ?
N11 Th1 C12 26.98(9) . . ?
N21 Th1 C12 169.62(9) . . ?
N1 Th1 C12 87.57(9) . . ?
Cl1 Th1 C12 95.03(7) . . ?
Cl1 Th1 C12 70.35(7) 3_666 . ?
N30 Th1 C32 25.67(9) . . ?
N10 Th1 C32 94.79(10) . . ?
N20 Th1 C32 108.66(9) . . ?
N31 Th1 C32 27.32(9) . . ?
N11 Th1 C32 92.56(9) . . ?
N21 Th1 C32 81.32(8) . . ?
N1 Th1 C32 87.62(9) . . ?
Cl1 Th1 C32 105.83(7) . . ?
Cl1 Th1 C32 169.78(6) 3_666 . ?
C12 Th1 C32 99.44(9) . . ?
N30 Th1 C22 82.10(9) . . ?
N10 Th1 C22 140.10(9) . . ?
N20 Th1 C22 25.55(9) . . ?
N31 Th1 C22 99.34(8) . . ?
N11 Th1 C22 165.93(9) . . ?
N21 Th1 C22 26.61(9) . . ?
N1 Th1 C22 79.62(8) . . ?
Cl1 Th1 C22 94.30(6) . . ?
Cl1 Th1 C22 96.67(6) 3_666 . ?
C12 Th1 C22 161.62(9) . . ?
C32 Th1 C22 93.18(9) . . ?
Th1 Cl1 Th1 103.83(2) . 3_666 ?
C16 N11 C12 119.3(3) . . ?
C16 N11 Th1 147.7(2) . . ?
C12 N11 Th1 90.2(2) . . ?
C20 N1 C30 111.4(3) . . ?
C20 N1 C10 110.2(3) . . ?
C30 N1 C10 109.4(3) . . ?
C20 N1 Th1 105.2(2) . . ?
C30 N1 Th1 107.45(19) . . ?
C10 N1 Th1 113.2(2) . . ?
C26 N21 C22 119.5(3) . . ?
C26 N21 Th1 147.6(2) . . ?
C22 N21 Th1 91.92(18) . . ?
C36 N31 C32 119.1(3) . . ?
C36 N31 Th1 147.3(2) . . ?
C32 N31 Th1 91.79(19) . . ?
C22 N20 C21 120.4(3) . . ?
C22 N20 Th1 104.2(2) . . ?
C21 N20 Th1 130.0(2) . . ?
C12 N10 C11 121.8(3) . . ?
C12 N10 Th1 102.9(2) . . ?
C11 N10 Th1 128.7(2) . . ?
C32 N30 C31 122.2(3) . . ?
C32 N30 Th1 104.2(2) . . ?
C31 N30 Th1 130.7(2) . . ?
C24 C23 C22 118.6(3) . . ?
C24 C23 H23 120.7 . . ?
C22 C23 H23 120.7 . . ?
N11 C16 C15 123.4(3) . . ?
N11 C16 H16 118.3 . . ?
C15 C16 H16 118.3 . . ?
N1 C20 C21 111.0(3) . . ?
N1 C20 H20A 109.4 . . ?
C21 C20 H20A 109.4 . . ?
N1 C20 H20B 109.4 . . ?
C21 C20 H20B 109.4 . . ?
H20A C20 H20B 108.0 . . ?
N30 C31 C30 106.4(3) . . ?
N30 C31 H31A 110.4 . . ?
C30 C31 H31A 110.4 . . ?
N30 C31 H31B 110.4 . . ?
C30 C31 H31B 110.4 . . ?
H31A C31 H31B 108.6 . . ?
N30 C32 N31 110.2(3) . . ?
N30 C32 C33 129.5(3) . . ?
N31 C32 C33 120.3(3) . . ?
N30 C32 Th1 50.11(18) . . ?
N31 C32 Th1 60.89(17) . . ?
C33 C32 Th1 170.2(2) . . ?
N20 C22 N21 110.8(3) . . ?
N20 C22 C23 129.1(3) . . ?
N21 C22 C23 120.2(3) . . ?
N20 C22 Th1 50.22(16) . . ?
N21 C22 Th1 61.47(16) . . ?
C23 C22 Th1 170.2(2) . . ?
C36 C35 C34 117.6(3) . . ?
C36 C35 H35 121.2 . . ?
C34 C35 H35 121.2 . . ?
C16 C15 C14 117.7(3) . . ?
C16 C15 H15 121.2 . . ?
C14 C15 H15 121.2 . . ?
N10 C12 N11 111.0(3) . . ?
N10 C12 C13 128.7(3) . . ?
N11 C12 C13 120.3(3) . . ?
N10 C12 Th1 51.16(16) . . ?
N11 C12 Th1 62.83(17) . . ?
C13 C12 Th1 163.4(2) . . ?
C34 C33 C32 118.3(4) . . ?
C34 C33 H33 120.8 . . ?
C32 C33 H33 120.8 . . ?
N20 C21 C20 107.6(3) . . ?
N20 C21 H21A 110.2 . . ?
C20 C21 H21A 110.2 . . ?
N20 C21 H21B 110.2 . . ?
C20 C21 H21B 110.2 . . ?
H21A C21 H21B 108.5 . . ?
N21 C26 C25 123.2(3) . . ?
N21 C26 H26 118.4 . . ?
C25 C26 H26 118.4 . . ?
C13 C14 C15 120.9(3) . . ?
C13 C14 H14 119.6 . . ?
C15 C14 H14 119.6 . . ?
C14 C13 C12 118.1(3) . . ?
C14 C13 H13 120.9 . . ?
C12 C13 H13 120.9 . . ?
N1 C10 C11 110.8(3) . . ?
N1 C10 H10A 109.5 . . ?
C11 C10 H10A 109.5 . . ?
N1 C10 H10B 109.5 . . ?
C11 C10 H10B 109.5 . . ?
H10A C10 H10B 108.1 . . ?
N1 C30 C31 111.0(3) . . ?
N1 C30 H30A 109.4 . . ?
C31 C30 H30A 109.4 . . ?
N1 C30 H30B 109.4 . . ?
C31 C30 H30B 109.4 . . ?
H30A C30 H30B 108.0 . . ?
C26 C25 C24 117.9(3) . . ?
C26 C25 H25 121.1 . . ?
C24 C25 H25 121.1 . . ?
N31 C36 C35 123.5(4) . . ?
N31 C36 H36 118.3 . . ?
C35 C36 H36 118.3 . . ?
N10 C11 C10 106.8(3) . . ?
N10 C11 H11A 110.4 . . ?
C10 C11 H11A 110.4 . . ?
N10 C11 H11B 110.4 . . ?
C10 C11 H11B 110.4 . . ?
H11A C11 H11B 108.6 . . ?
C33 C34 C35 121.1(3) . . ?
C33 C34 H34 119.4 . . ?
C35 C34 H34 119.4 . . ?
C23 C24 C25 120.6(3) . . ?
C23 C24 H24 119.7 . . ?
C25 C24 H24 119.7 . . ?

_refine_diff_density_max         1.669
_refine_diff_density_min         -0.852
_refine_diff_density_rms         0.132


_chemical_properties_physical    
', Air-sensitive,Moisture-sensitive,Oxygen-sensitive'
####################################################################### 
# 
# 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_shelx_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1510089'
_audit_update_record             
;
2016-10-16 deposited with the CCDC.
2017-08-14 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            'C42 H48 I2 N14 U2'
_chemical_formula_weight         1478.80

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'
I I -0.4742 1.8119 '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                   13.6661(9)
_cell_length_b                   9.5267(6)
_cell_length_c                   16.5783(11)
_cell_angle_alpha                90
_cell_angle_beta                 94.929(3)
_cell_angle_gamma                90
_cell_volume                     2150.4(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3585
_cell_measurement_theta_min      1.85
_cell_measurement_theta_max      25.40

_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.284
_exptl_crystal_F_000             1376
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_exptl_absorpt_coefficient_mu    9.007
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.489
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_process_details   'Blessing, 1995'
_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 Kappa Quazar'
_diffrn_measurement_method       'omega phi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            29570
_diffrn_reflns_av_unetI/netI     0.0375
_diffrn_reflns_av_R_equivalents  0.0957
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.855
_diffrn_reflns_theta_max         25.404
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             3953
_reflns_number_gt                3585
_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 Apex3 suite, 2015'
_computing_cell_refinement       'Bruker Apex3 suite, 2015'
_computing_data_reduction        'Bruker Apex3 suite, 2015'
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0551P)²+3.6441P] 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         3953
_refine_ls_number_parameters     271
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0363
_refine_ls_R_factor_gt           0.0330
_refine_ls_wR_factor_ref         0.0897
_refine_ls_wR_factor_gt          0.0869
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_restrained_S_all      1.099
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.33799(2) 0.44340(2) 0.56012(2) 0.01417(10) Uani 1 1 d . . . . .
I1 I 0.57045(2) 0.34147(4) 0.57263(2) 0.01968(12) Uani 1 1 d . . . . .
N20 N 0.3305(3) 0.2231(5) 0.4991(3) 0.0197(10) Uani 1 1 d . . . . .
N1 N 0.2907(3) 0.2199(5) 0.6518(3) 0.0207(10) Uani 1 1 d . . . . .
N11 N 0.4273(3) 0.6529(5) 0.6400(3) 0.0224(10) Uani 1 1 d . . . . .
N31 N 0.2033(3) 0.6303(5) 0.5279(3) 0.0179(10) Uani 1 1 d . . . . .
N10 N 0.3874(4) 0.4538(5) 0.6979(3) 0.0201(11) Uani 1 1 d . . . . .
N21 N 0.2614(3) 0.3824(5) 0.4147(3) 0.0183(10) Uani 1 1 d . . . . .
C32 C 0.1368(4) 0.5528(6) 0.5665(3) 0.0181(12) Uani 1 1 d . . . . .
N30 N 0.1764(4) 0.4293(5) 0.5890(3) 0.0205(11) Uani 1 1 d . . . . .
C16 C 0.4782(4) 0.7739(6) 0.6374(4) 0.0223(12) Uani 1 1 d . . . . .
H16 H 0.4659 0.8328 0.5914 0.027 Uiso 1 1 calc R U . . .
C26 C 0.2127(4) 0.4250(6) 0.3469(4) 0.0207(12) Uani 1 1 d . . . . .
H26 H 0.2031 0.5228 0.3384 0.025 Uiso 1 1 calc R U . . .
C22 C 0.2763(4) 0.2426(6) 0.4280(3) 0.0187(11) Uani 1 1 d . . . . .
C12 C 0.4474(4) 0.5674(5) 0.7052(3) 0.0184(12) Uani 1 1 d . . . . .
C23 C 0.2358(4) 0.1427(6) 0.3720(3) 0.0211(12) Uani 1 1 d . . . . .
H23 H 0.2426 0.0450 0.3825 0.025 Uiso 1 1 calc R U . . .
C36 C 0.1775(4) 0.7573(6) 0.4991(3) 0.0224(12) Uani 1 1 d . . . . .
H36 H 0.2239 0.8102 0.4724 0.027 Uiso 1 1 calc R U . . .
C33 C 0.0424(4) 0.6047(7) 0.5776(3) 0.0241(13) Uani 1 1 d . . . . .
H33 H -0.0029 0.5510 0.6053 0.029 Uiso 1 1 calc R U . . .
C31 C 0.1253(4) 0.3266(7) 0.6353(4) 0.0257(13) Uani 1 1 d . . . . .
H31A H 0.0574 0.3122 0.6108 0.031 Uiso 1 1 calc R U . . .
H31B H 0.1226 0.3586 0.6919 0.031 Uiso 1 1 calc R U . . .
C35 C 0.0849(4) 0.8151(6) 0.5068(4) 0.0252(13) Uani 1 1 d . . . . .
H35 H 0.0678 0.9053 0.4855 0.030 Uiso 1 1 calc R U . . .
C13 C 0.5203(4) 0.5997(7) 0.7675(4) 0.0261(13) Uani 1 1 d . . . . .
H13 H 0.5353 0.5371 0.8115 0.031 Uiso 1 1 calc R U . . .
C30 C 0.1845(4) 0.1911(6) 0.6326(4) 0.0257(13) Uani 1 1 d . . . . .
H30A H 0.1618 0.1234 0.6723 0.031 Uiso 1 1 calc R U . . .
H30B H 0.1738 0.1487 0.5781 0.031 Uiso 1 1 calc R U . . .
C21 C 0.3392(5) 0.0835(6) 0.5359(4) 0.0242(13) Uani 1 1 d . . . . .
H21A H 0.3969 0.0340 0.5173 0.029 Uiso 1 1 calc R U . . .
H21B H 0.2798 0.0274 0.5196 0.029 Uiso 1 1 calc R U . . .
C11 C 0.3999(4) 0.3387(6) 0.7560(3) 0.0214(12) Uani 1 1 d . . . . .
H11A H 0.4037 0.3751 0.8121 0.026 Uiso 1 1 calc R U . . .
H11B H 0.4609 0.2860 0.7484 0.026 Uiso 1 1 calc R U . . .
C34 C 0.0179(4) 0.7356(7) 0.5472(4) 0.0302(15) Uani 1 1 d . . . . .
H34 H -0.0455 0.7727 0.5537 0.036 Uiso 1 1 calc R U . . .
C25 C 0.1752(4) 0.3329(6) 0.2879(3) 0.0235(13) Uani 1 1 d . . . . .
H25 H 0.1426 0.3669 0.2388 0.028 Uiso 1 1 calc R U . . .
C24 C 0.1858(4) 0.1913(7) 0.3012(3) 0.0262(13) Uani 1 1 d . . . . .
H24 H 0.1588 0.1264 0.2618 0.031 Uiso 1 1 calc R U . . .
C10 C 0.3113(4) 0.2450(7) 0.7399(3) 0.0250(13) Uani 1 1 d . . . . .
H10A H 0.3234 0.1543 0.7681 0.030 Uiso 1 1 calc R U . . .
H10B H 0.2536 0.2897 0.7614 0.030 Uiso 1 1 calc R U . . .
C20 C 0.3508(5) 0.1002(7) 0.6273(3) 0.0244(12) Uani 1 1 d . . . . .
H20A H 0.3296 0.0131 0.6533 0.029 Uiso 1 1 calc R U . . .
H20B H 0.4207 0.1168 0.6455 0.029 Uiso 1 1 calc R U . . .
C15 C 0.5461(5) 0.8156(7) 0.6973(4) 0.0306(14) Uani 1 1 d . . . . .
H15 H 0.5775 0.9043 0.6951 0.037 Uiso 1 1 calc R U . . .
C14 C 0.5686(4) 0.7234(7) 0.7626(4) 0.0290(14) Uani 1 1 d . . . . .
H14 H 0.6182 0.7482 0.8038 0.035 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 N30 2.304(5) . ?
U1 N10 2.327(5) . ?
U1 N20 2.328(5) . ?
U1 N31 2.584(4) . ?
U1 N21 2.609(4) . ?
U1 N11 2.637(5) . ?
U1 N1 2.725(5) . ?
U1 C32 2.951(6) . ?
U1 C12 2.966(6) . ?
U1 C22 2.975(5) . ?
U1 I1 3.3114(4) . ?
U1 I1 3.3291(4) 3_666 ?
I1 U1 3.3291(4) 3_666 ?
N20 C22 1.351(7) . ?
N20 C21 1.463(7) . ?
N1 C20 1.482(8) . ?
N1 C10 1.484(7) . ?
N1 C30 1.485(7) . ?
N11 C16 1.349(8) . ?
N11 C12 1.361(7) . ?
N31 C36 1.337(7) . ?
N31 C32 1.371(7) . ?
N10 C12 1.357(7) . ?
N10 C11 1.460(7) . ?
N21 C26 1.320(7) . ?
N21 C22 1.362(7) . ?
C32 N30 1.335(7) . ?
C32 C33 1.408(8) . ?
N30 C31 1.457(7) . ?
C16 C15 1.359(9) . ?
C16 H16 0.9500 . ?
C26 C25 1.379(8) . ?
C26 H26 0.9500 . ?
C22 C23 1.408(8) . ?
C12 C13 1.407(8) . ?
C23 C24 1.386(8) . ?
C23 H23 0.9500 . ?
C36 C35 1.396(8) . ?
C36 H36 0.9500 . ?
C33 C34 1.376(9) . ?
C33 H33 0.9500 . ?
C31 C30 1.526(9) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C35 C34 1.402(9) . ?
C35 H35 0.9500 . ?
C13 C14 1.356(9) . ?
C13 H13 0.9500 . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C21 C20 1.519(8) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C11 C10 1.509(8) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C34 H34 0.9500 . ?
C25 C24 1.373(9) . ?
C25 H25 0.9500 . ?
C24 H24 0.9500 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C15 C14 1.407(10) . ?
C15 H15 0.9500 . ?
C14 H14 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
N30 U1 N10 90.04(17) . . ?
N30 U1 N20 91.74(17) . . ?
N10 U1 N20 117.57(16) . . ?
N30 U1 N31 53.44(15) . . ?
N10 U1 N31 108.35(15) . . ?
N20 U1 N31 121.83(15) . . ?
N30 U1 N21 82.15(16) . . ?
N10 U1 N21 167.26(15) . . ?
N20 U1 N21 53.05(15) . . ?
N31 U1 N21 74.95(14) . . ?
N30 U1 N11 110.52(16) . . ?
N10 U1 N11 52.54(16) . . ?
N20 U1 N11 154.40(16) . . ?
N31 U1 N11 82.72(14) . . ?
N21 U1 N11 139.86(14) . . ?
N30 U1 N1 63.97(15) . . ?
N10 U1 N1 63.18(15) . . ?
N20 U1 N1 62.24(15) . . ?
N31 U1 N1 117.05(14) . . ?
N21 U1 N1 104.21(14) . . ?
N11 U1 N1 115.64(14) . . ?
N30 U1 C32 25.88(16) . . ?
N10 U1 C32 98.18(16) . . ?
N20 U1 C32 109.12(15) . . ?
N31 U1 C32 27.68(15) . . ?
N21 U1 C32 79.08(15) . . ?
N11 U1 C32 96.17(14) . . ?
N1 U1 C32 89.41(15) . . ?
N30 U1 C12 106.28(17) . . ?
N10 U1 C12 26.34(16) . . ?
N20 U1 C12 135.36(15) . . ?
N31 U1 C12 101.18(14) . . ?
N21 U1 C12 166.39(15) . . ?
N11 U1 C12 27.32(15) . . ?
N1 U1 C12 89.21(14) . . ?
C32 U1 C12 103.70(15) . . ?
N30 U1 C22 84.22(16) . . ?
N10 U1 C22 142.18(15) . . ?
N20 U1 C22 26.04(15) . . ?
N31 U1 C22 97.98(14) . . ?
N21 U1 C22 27.23(15) . . ?
N11 U1 C22 161.17(14) . . ?
N1 U1 C22 80.94(14) . . ?
C32 U1 C22 92.71(14) . . ?
C12 U1 C22 160.80(15) . . ?
N30 U1 I1 154.36(11) . . ?
N10 U1 I1 75.84(12) . . ?
N20 U1 I1 76.64(11) . . ?
N31 U1 I1 151.38(10) . . ?
N21 U1 I1 107.40(10) . . ?
N11 U1 I1 77.89(10) . . ?
N1 U1 I1 90.46(10) . . ?
C32 U1 I1 173.32(10) . . ?
C12 U1 I1 69.63(11) . . ?
C22 U1 I1 93.86(10) . . ?
N30 U1 I1 126.51(12) . 3_666 ?
N10 U1 I1 121.92(12) . 3_666 ?
N20 U1 I1 105.84(11) . 3_666 ?
N31 U1 I1 74.98(10) . 3_666 ?
N21 U1 I1 70.74(10) . 3_666 ?
N11 U1 I1 71.47(10) . 3_666 ?
N1 U1 I1 165.94(10) . 3_666 ?
C32 U1 I1 102.16(11) . 3_666 ?
C12 U1 I1 95.68(11) . 3_666 ?
C22 U1 I1 90.45(10) . 3_666 ?
I1 U1 I1 78.983(11) . 3_666 ?
U1 I1 U1 101.019(10) . 3_666 ?
C22 N20 C21 120.5(5) . . ?
C22 N20 U1 104.8(4) . . ?
C21 N20 U1 129.8(4) . . ?
C20 N1 C10 109.3(4) . . ?
C20 N1 C30 110.7(5) . . ?
C10 N1 C30 109.9(4) . . ?
C20 N1 U1 106.6(3) . . ?
C10 N1 U1 112.9(3) . . ?
C30 N1 U1 107.4(3) . . ?
C16 N11 C12 117.9(5) . . ?
C16 N11 U1 148.0(4) . . ?
C12 N11 U1 89.9(3) . . ?
C36 N31 C32 119.3(5) . . ?
C36 N31 U1 149.2(4) . . ?
C32 N31 U1 91.2(3) . . ?
C12 N10 C11 120.3(5) . . ?
C12 N10 U1 104.1(4) . . ?
C11 N10 U1 128.5(3) . . ?
C26 N21 C22 119.7(5) . . ?
C26 N21 U1 148.3(4) . . ?
C22 N21 U1 91.5(3) . . ?
N30 C32 N31 109.7(5) . . ?
N30 C32 C33 128.8(6) . . ?
N31 C32 C33 121.5(5) . . ?
N30 C32 U1 48.9(3) . . ?
N31 C32 U1 61.1(3) . . ?
C33 C32 U1 174.5(4) . . ?
C32 N30 C31 122.6(5) . . ?
C32 N30 U1 105.2(4) . . ?
C31 N30 U1 131.2(4) . . ?
N11 C16 C15 123.2(6) . . ?
N11 C16 H16 118.4 . . ?
C15 C16 H16 118.4 . . ?
N21 C26 C25 122.5(5) . . ?
N21 C26 H26 118.7 . . ?
C25 C26 H26 118.7 . . ?
N20 C22 N21 109.8(5) . . ?
N20 C22 C23 129.6(5) . . ?
N21 C22 C23 120.7(5) . . ?
N20 C22 U1 49.1(3) . . ?
N21 C22 U1 61.2(3) . . ?
C23 C22 U1 171.8(4) . . ?
N10 C12 N11 109.1(5) . . ?
N10 C12 C13 128.6(5) . . ?
N11 C12 C13 122.2(5) . . ?
N10 C12 U1 49.6(3) . . ?
N11 C12 U1 62.7(3) . . ?
C13 C12 U1 163.5(4) . . ?
C24 C23 C22 117.9(5) . . ?
C24 C23 H23 121.0 . . ?
C22 C23 H23 121.0 . . ?
N31 C36 C35 122.6(6) . . ?
N31 C36 H36 118.7 . . ?
C35 C36 H36 118.7 . . ?
C34 C33 C32 117.9(6) . . ?
C34 C33 H33 121.1 . . ?
C32 C33 H33 121.1 . . ?
N30 C31 C30 105.9(4) . . ?
N30 C31 H31A 110.6 . . ?
C30 C31 H31A 110.6 . . ?
N30 C31 H31B 110.6 . . ?
C30 C31 H31B 110.6 . . ?
H31A C31 H31B 108.7 . . ?
C36 C35 C34 117.7(5) . . ?
C36 C35 H35 121.2 . . ?
C34 C35 H35 121.2 . . ?
C14 C13 C12 117.6(6) . . ?
C14 C13 H13 121.2 . . ?
C12 C13 H13 121.2 . . ?
N1 C30 C31 110.4(5) . . ?
N1 C30 H30A 109.6 . . ?
C31 C30 H30A 109.6 . . ?
N1 C30 H30B 109.6 . . ?
C31 C30 H30B 109.6 . . ?
H30A C30 H30B 108.1 . . ?
N20 C21 C20 108.5(5) . . ?
N20 C21 H21A 110.0 . . ?
C20 C21 H21A 110.0 . . ?
N20 C21 H21B 110.0 . . ?
C20 C21 H21B 110.0 . . ?
H21A C21 H21B 108.4 . . ?
N10 C11 C10 106.3(5) . . ?
N10 C11 H11A 110.5 . . ?
C10 C11 H11A 110.5 . . ?
N10 C11 H11B 110.5 . . ?
C10 C11 H11B 110.5 . . ?
H11A C11 H11B 108.7 . . ?
C33 C34 C35 121.1(5) . . ?
C33 C34 H34 119.5 . . ?
C35 C34 H34 119.5 . . ?
C24 C25 C26 118.9(5) . . ?
C24 C25 H25 120.6 . . ?
C26 C25 H25 120.6 . . ?
C25 C24 C23 120.2(5) . . ?
C25 C24 H24 119.9 . . ?
C23 C24 H24 119.9 . . ?
N1 C10 C11 110.5(4) . . ?
N1 C10 H10A 109.5 . . ?
C11 C10 H10A 109.5 . . ?
N1 C10 H10B 109.5 . . ?
C11 C10 H10B 109.5 . . ?
H10A C10 H10B 108.1 . . ?
N1 C20 C21 109.9(5) . . ?
N1 C20 H20A 109.7 . . ?
C21 C20 H20A 109.7 . . ?
N1 C20 H20B 109.7 . . ?
C21 C20 H20B 109.7 . . ?
H20A C20 H20B 108.2 . . ?
C16 C15 C14 118.0(6) . . ?
C16 C15 H15 121.0 . . ?
C14 C15 H15 121.0 . . ?
C13 C14 C15 120.9(6) . . ?
C13 C14 H14 119.5 . . ?
C15 C14 H14 119.5 . . ?

_refine_diff_density_max         2.912
_refine_diff_density_min         -1.239
_refine_diff_density_rms         0.205


_chemical_properties_physical    
', Air-sensitive,Moisture-sensitive,Oxygen-sensitive'
####################################################################### 
# 
# 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_shelx_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 1516433'
_audit_update_record             
;
2017-01-10 deposited with the CCDC.
2017-08-14 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            'C62 H88 I2 N14 O5 U2'
_chemical_formula_weight         1839.32

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'
I I -0.4742 1.8119 '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'

_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                   12.6307(6)
_cell_length_b                   14.3188(6)
_cell_length_c                   18.4904(8)
_cell_angle_alpha                90.085(2)
_cell_angle_beta                 104.405(2)
_cell_angle_gamma                90.472(2)
_cell_volume                     3238.8(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    11675
_cell_measurement_theta_min      1.14
_cell_measurement_theta_max      29.23

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.886
_exptl_crystal_F_000             1776
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_exptl_absorpt_coefficient_mu    6.006
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.648
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_process_details   'Blessing, 1995'
_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 Quazar'
_diffrn_measurement_method       'omega phi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            75321
_diffrn_reflns_av_unetI/netI     0.1042
_diffrn_reflns_av_R_equivalents  0.0807
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.137
_diffrn_reflns_theta_max         29.227
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             17397
_reflns_number_gt                11675
_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 Apex III suite, 2016'
_computing_cell_refinement       'Bruker Apex III suite, 2016'
_computing_data_reduction        'Bruker Apex III suite, 2016'
_computing_structure_solution    shelXT
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Diamond 3D'
_computing_publication_material  WinGX
_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)+(0.0422P)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         17397
_refine_ls_number_parameters     766
_refine_ls_number_restraints     49
_refine_ls_R_factor_all          0.0884
_refine_ls_R_factor_gt           0.0513
_refine_ls_wR_factor_ref         0.1109
_refine_ls_wR_factor_gt          0.1001
_refine_ls_goodness_of_fit_ref   0.987
_refine_ls_restrained_S_all      0.998
_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
U1A U 0.64091(2) 0.72392(2) 0.24030(2) 0.01769(7) Uani 1 1 d . . . . .
U1 U 0.69306(2) 0.80345(2) 0.74644(2) 0.01608(7) Uani 1 1 d . . . . .
I1A I 0.71010(4) 0.90555(3) 0.34814(2) 0.02618(11) Uani 1 1 d . . . . .
I1 I 0.78197(4) 0.62816(3) 0.85196(3) 0.03173(12) Uani 1 1 d . . . . .
O10A O 0.5882(4) 0.8631(3) 0.1511(2) 0.0259(11) Uani 1 1 d . . . . .
N1 N 0.6295(4) 0.9208(4) 0.6232(3) 0.0201(12) Uani 1 1 d . . . . .
O400 O 1.0134(4) 0.8510(3) 0.5143(2) 0.0321(12) Uani 1 1 d . . . . .
O100 O 0.6409(4) 0.6635(3) 0.6578(3) 0.0334(12) Uani 1 1 d . . . . .
N11 N 0.5311(4) 0.7587(3) 0.8046(3) 0.0171(11) Uani 1 1 d . . . . .
O300 O 0.2089(4) 0.6295(3) -0.0487(3) 0.0377(13) Uani 1 1 d . . . . .
O500 O 0.9845(4) 0.5719(4) 0.6527(2) 0.0390(14) Uani 1 1 d . . . . .
N21 N 0.9004(4) 0.8438(3) 0.7823(3) 0.0177(11) Uani 1 1 d . . . . .
N30 N 0.6933(4) 0.9627(3) 0.7718(3) 0.0172(11) Uani 1 1 d . . . . .
N10 N 0.5058(4) 0.8150(3) 0.6899(3) 0.0173(11) Uani 1 1 d . . . . .
N31A N 0.7420(4) 0.6493(3) 0.3632(3) 0.0195(12) Uani 1 1 d . . . . .
N20 N 0.8112(4) 0.8078(4) 0.6659(3) 0.0196(12) Uani 1 1 d . . . . .
N11A N 0.8467(5) 0.7611(4) 0.2461(4) 0.0337(15) Uani 1 1 d . . . . .
N31 N 0.7469(4) 0.8804(4) 0.8759(3) 0.0186(12) Uani 1 1 d . . . . .
N10A N 0.7315(6) 0.7006(4) 0.1465(3) 0.0302(15) Uani 1 1 d . . . . .
N30A N 0.6452(5) 0.5680(4) 0.2671(3) 0.0225(12) Uani 1 1 d . . . . .
N21A N 0.5052(5) 0.7300(3) 0.3244(3) 0.0242(13) Uani 1 1 d . . . . .
C26 C 0.9829(5) 0.8815(4) 0.8340(4) 0.0225(15) Uani 1 1 d . . . . .
H26 H 0.9816 0.8756 0.8849 0.027 Uiso 1 1 calc R U . . .
C32 C 0.7468(5) 0.9709(4) 0.8471(3) 0.0104(12) Uani 1 1 d . U . . .
C22 C 0.9002(5) 0.8507(4) 0.7097(3) 0.0169(13) Uani 1 1 d . . . . .
C12A C 0.8335(7) 0.7346(5) 0.1740(4) 0.0347(19) Uani 1 1 d . . . . .
C36A C 0.8108(5) 0.6607(5) 0.4300(3) 0.0217(15) Uani 1 1 d . . . . .
H36A H 0.8299 0.7223 0.4478 0.026 Uiso 1 1 calc R U . . .
C14 C 0.3118(6) 0.7652(4) 0.8045(4) 0.0238(15) Uani 1 1 d . . . . .
H14 H 0.2368 0.7671 0.8051 0.029 Uiso 1 1 calc R U . . .
C31 C 0.6886(5) 1.0407(4) 0.7212(3) 0.0217(15) Uani 1 1 d . . . . .
H31A H 0.7614 1.0525 0.7118 0.026 Uiso 1 1 calc R U . . .
H31B H 0.6652 1.0979 0.7428 0.026 Uiso 1 1 calc R U . . .
C24 C 1.0685(6) 0.9363(4) 0.7425(4) 0.0260(16) Uani 1 1 d . . . . .
H24 H 1.1275 0.9672 0.7289 0.031 Uiso 1 1 calc R U . . .
C25 C 1.0698(5) 0.9284(4) 0.8178(4) 0.0232(15) Uani 1 1 d . . . . .
H25 H 1.1275 0.9541 0.8560 0.028 Uiso 1 1 calc R U . . .
C20 C 0.7148(6) 0.9248(5) 0.5814(3) 0.0269(16) Uani 1 1 d . . . . .
H20A H 0.7667 0.9762 0.6014 0.032 Uiso 1 1 calc R U . . .
H20B H 0.6806 0.9380 0.5283 0.032 Uiso 1 1 calc R U . . .
C36 C 0.7968(5) 0.8687(5) 0.9485(3) 0.0265(16) Uani 1 1 d . . . . .
H36 H 0.7989 0.8079 0.9693 0.032 Uiso 1 1 calc R U . . .
C23 C 0.9849(5) 0.9008(4) 0.6880(4) 0.0204(14) Uani 1 1 d . . . . .
H23 H 0.9832 0.9092 0.6367 0.025 Uiso 1 1 calc R U . . .
C30 C 0.6056(6) 1.0140(4) 0.6484(3) 0.0247(16) Uani 1 1 d . . . . .
H30A H 0.5309 1.0142 0.6564 0.030 Uiso 1 1 calc R U . . .
H30B H 0.6085 1.0606 0.6094 0.030 Uiso 1 1 calc R U . . .
C32A C 0.7163(5) 0.5587(4) 0.3374(3) 0.0134(12) Uani 1 1 d . U . . .
C16 C 0.4977(5) 0.7314(4) 0.8641(3) 0.0216(14) Uani 1 1 d . . . . .
H16 H 0.5509 0.7104 0.9066 0.026 Uiso 1 1 calc R U . . .
C12 C 0.4564(5) 0.7923(4) 0.7430(3) 0.0201(14) Uani 1 1 d . . . . .
C13 C 0.3438(5) 0.7947(4) 0.7428(3) 0.0194(14) Uani 1 1 d . . . . .
H13 H 0.2913 0.8165 0.7002 0.023 Uiso 1 1 calc R U . . .
C33A C 0.7578(7) 0.4836(5) 0.3786(4) 0.038(2) Uani 1 1 d . . . . .
H33A H 0.7381 0.4222 0.3605 0.046 Uiso 1 1 calc R U . . .
C34 C 0.8415(6) 1.0279(5) 0.9633(4) 0.0312(17) Uani 1 1 d . . . . .
H34 H 0.8747 1.0788 0.9939 0.037 Uiso 1 1 calc R U . . .
C22A C 0.4174(6) 0.7147(5) 0.2651(4) 0.0299(17) Uani 1 1 d . . . . .
C21 C 0.7760(6) 0.8340(5) 0.5875(3) 0.0266(16) Uani 1 1 d . . . . .
H21A H 0.7280 0.7845 0.5589 0.032 Uiso 1 1 calc R U . . .
H21B H 0.8404 0.8413 0.5664 0.032 Uiso 1 1 calc R U . . .
C23A C 0.3142(6) 0.6947(5) 0.2781(5) 0.0373(19) Uani 1 1 d . . . . .
H23A H 0.2533 0.6798 0.2378 0.045 Uiso 1 1 calc R U . . .
C103 C 0.7213(6) 0.6016(5) 0.6376(4) 0.0365(19) Uani 1 1 d . . . . .
H10A H 0.7586 0.5624 0.6803 0.044 Uiso 1 1 calc R U . . .
H10B H 0.7767 0.6374 0.6192 0.044 Uiso 1 1 calc R U . . .
N20A N 0.4485(5) 0.7203(5) 0.2008(3) 0.0411(17) Uani 1 1 d . . . . .
C15 C 0.3897(5) 0.7322(4) 0.8670(4) 0.0232(15) Uani 1 1 d . . . . .
H15 H 0.3686 0.7109 0.9100 0.028 Uiso 1 1 calc R U . . .
C11 C 0.4458(5) 0.8552(5) 0.6204(3) 0.0226(15) Uani 1 1 d . . . . .
H11A H 0.4082 0.9126 0.6299 0.027 Uiso 1 1 calc R U . . .
H11B H 0.3903 0.8103 0.5926 0.027 Uiso 1 1 calc R U . . .
C10 C 0.5292(6) 0.8781(5) 0.5756(3) 0.0263(16) Uani 1 1 d . . . . .
H10C H 0.5484 0.8201 0.5527 0.032 Uiso 1 1 calc R U . . .
H10D H 0.4963 0.9217 0.5348 0.032 Uiso 1 1 calc R U . . .
C33 C 0.7915(6) 1.0443(5) 0.8894(4) 0.0284(16) Uani 1 1 d . . . . .
H33 H 0.7887 1.1054 0.8691 0.034 Uiso 1 1 calc R U . . .
C35A C 0.8555(5) 0.5864(4) 0.4743(3) 0.0230(15) Uani 1 1 d . . . . .
H35A H 0.9034 0.5963 0.5223 0.028 Uiso 1 1 calc R U . . .
N1A N 0.5456(6) 0.6059(4) 0.1238(3) 0.0412(18) Uani 1 1 d D . . . .
C26A C 0.4919(6) 0.7318(4) 0.3937(4) 0.0317(18) Uani 1 1 d . . . . .
H26A H 0.5535 0.7442 0.4341 0.038 Uiso 1 1 calc R U . . .
C35 C 0.8449(6) 0.9413(5) 0.9937(4) 0.0332(18) Uani 1 1 d . . . . .
H35 H 0.8796 0.9313 1.0449 0.040 Uiso 1 1 calc R U . . .
C102 C 0.6493(6) 0.5439(5) 0.5764(4) 0.0357(18) Uani 1 1 d . . . . .
H10E H 0.6831 0.4829 0.5712 0.043 Uiso 1 1 calc R U . . .
H10F H 0.6347 0.5770 0.5280 0.043 Uiso 1 1 calc R U . . .
C34A C 0.8288(7) 0.4979(5) 0.4471(4) 0.0372(19) Uani 1 1 d . . . . .
H34A H 0.8600 0.4456 0.4761 0.045 Uiso 1 1 calc R U . . .
C403 C 1.0814(6) 0.7752(5) 0.5481(4) 0.0311(17) Uani 1 1 d . . . . .
H40A H 1.0367 0.7201 0.5543 0.037 Uiso 1 1 calc R U . . .
H40B H 1.1281 0.7937 0.5974 0.037 Uiso 1 1 calc R U . . .
C101 C 0.5455(7) 0.5312(5) 0.6023(5) 0.043(2) Uani 1 1 d . . . . .
H10G H 0.4807 0.5305 0.5592 0.052 Uiso 1 1 calc R U . . .
H10H H 0.5471 0.4721 0.6301 0.052 Uiso 1 1 calc R U . . .
C300 C 0.1531(7) 0.5617(5) -0.0155(4) 0.043(2) Uani 1 1 d . . . . .
H30C H 0.2060 0.5251 0.0221 0.052 Uiso 1 1 calc R U . . .
H30D H 0.1112 0.5183 -0.0540 0.052 Uiso 1 1 calc R U . . .
C301 C 0.0776(6) 0.6129(5) 0.0208(5) 0.048(2) Uani 1 1 d . . . . .
H30E H 0.0020 0.5884 0.0031 0.058 Uiso 1 1 calc R U . . .
H30F H 0.1010 0.6063 0.0758 0.058 Uiso 1 1 calc R U . . .
C400 C 1.0777(6) 0.9106(5) 0.4791(4) 0.0340(18) Uani 1 1 d . . . . .
H40C H 1.1075 0.9642 0.5120 0.041 Uiso 1 1 calc R U . . .
H40D H 1.0324 0.9349 0.4314 0.041 Uiso 1 1 calc R U . . .
C200 C 0.6679(6) 0.9133(5) 0.1218(4) 0.0330(18) Uani 1 1 d . . . . .
H20C H 0.6781 0.8820 0.0763 0.040 Uiso 1 1 calc R U . . .
H20D H 0.7391 0.9157 0.1592 0.040 Uiso 1 1 calc R U . . .
C16A C 0.9420(6) 0.7981(5) 0.2842(5) 0.041(2) Uani 1 1 d . . . . .
H16A H 0.9500 0.8152 0.3349 0.050 Uiso 1 1 calc R U . . .
C11A C 0.6935(7) 0.6680(5) 0.0714(4) 0.040(2) Uani 1 1 d . . . . .
H11C H 0.6499 0.7169 0.0400 0.048 Uiso 1 1 calc R U . . .
H11D H 0.7563 0.6527 0.0505 0.048 Uiso 1 1 calc R U . . .
C31A C 0.6079(9) 0.4858(5) 0.2198(4) 0.061(3) Uani 1 1 d . . . . .
H31C H 0.6719 0.4510 0.2126 0.074 Uiso 1 1 calc R U . . .
H31D H 0.5652 0.4439 0.2446 0.074 Uiso 1 1 calc R U . . .
C303 C 0.1382(6) 0.7092(5) -0.0644(4) 0.039(2) Uani 1 1 d . . . . .
H30G H 0.0836 0.7016 -0.1128 0.047 Uiso 1 1 calc R U . . .
H30H H 0.1809 0.7672 -0.0658 0.047 Uiso 1 1 calc R U . . .
C402 C 1.1488(7) 0.7549(5) 0.4946(4) 0.041(2) Uani 1 1 d . . . . .
H40E H 1.1084 0.7140 0.4535 0.049 Uiso 1 1 calc R U . . .
H40F H 1.2179 0.7241 0.5200 0.049 Uiso 1 1 calc R U . . .
C302 C 0.0836(6) 0.7117(5) -0.0008(4) 0.0381(19) Uani 1 1 d . . . . .
H30I H 0.1273 0.7492 0.0413 0.046 Uiso 1 1 calc R U . . .
H30J H 0.0096 0.7387 -0.0171 0.046 Uiso 1 1 calc R U . . .
C500 C 0.9695(7) 0.4747(6) 0.6601(4) 0.046(2) Uani 1 1 d . . . . .
H50A H 1.0261 0.4397 0.6429 0.055 Uiso 1 1 calc R U . . .
H50B H 0.8967 0.4548 0.6297 0.055 Uiso 1 1 calc R U . . .
C30A C 0.5425(8) 0.5138(5) 0.1499(4) 0.046(2) Uani 1 1 d . . . . .
H30K H 0.4657 0.5001 0.1502 0.055 Uiso 1 1 calc R U . . .
H30L H 0.5604 0.4722 0.1119 0.055 Uiso 1 1 calc R U . . .
C13A C 0.9194(8) 0.7452(8) 0.1388(5) 0.070(3) Uani 1 1 d . . . . .
H13A H 0.9136 0.7246 0.0891 0.085 Uiso 1 1 calc R U . . .
C201 C 0.6253(7) 1.0086(5) 0.1041(5) 0.048(2) Uani 1 1 d . . . . .
H20E H 0.6735 1.0550 0.1365 0.057 Uiso 1 1 calc R U . . .
H20F H 0.6222 1.0238 0.0513 0.057 Uiso 1 1 calc R U . . .
C401 C 1.1712(7) 0.8506(5) 0.4651(5) 0.043(2) Uani 1 1 d . . . . .
H40G H 1.1688 0.8476 0.4112 0.052 Uiso 1 1 calc R U . . .
H40H H 1.2434 0.8755 0.4926 0.052 Uiso 1 1 calc R U . . .
C25A C 0.3913(7) 0.7164(5) 0.4084(5) 0.045(2) Uani 1 1 d . . . . .
H25A H 0.3832 0.7190 0.4581 0.054 Uiso 1 1 calc R U . . .
C21A C 0.3820(7) 0.6811(8) 0.1308(4) 0.065(3) Uani 1 1 d . U . . .
H21C H 0.3315 0.7294 0.1041 0.077 Uiso 1 1 calc R U . . .
H21D H 0.3375 0.6284 0.1420 0.077 Uiso 1 1 calc R U . . .
C20A C 0.4560(9) 0.6456(7) 0.0790(6) 0.089(4) Uani 1 1 d D U . . .
H20G H 0.4154 0.5994 0.0424 0.106 Uiso 1 1 calc R U . . .
H20H H 0.4777 0.6986 0.0514 0.106 Uiso 1 1 calc R U . . .
C24A C 0.3036(7) 0.6971(5) 0.3499(5) 0.044(2) Uani 1 1 d . . . . .
H24A H 0.2341 0.6853 0.3593 0.053 Uiso 1 1 calc R U . . .
C202 C 0.5164(7) 1.0107(5) 0.1169(5) 0.047(2) Uani 1 1 d . . . . .
H20I H 0.5095 1.0654 0.1482 0.057 Uiso 1 1 calc R U . . .
H20J H 0.4610 1.0159 0.0687 0.057 Uiso 1 1 calc R U . . .
C203 C 0.4986(7) 0.9257(7) 0.1541(5) 0.065(3) Uani 1 1 d . . . . .
H20K H 0.4276 0.8969 0.1287 0.078 Uiso 1 1 calc R U . . .
H20L H 0.4983 0.9389 0.2066 0.078 Uiso 1 1 calc R U . . .
C503 C 1.0380(8) 0.6106(7) 0.7245(5) 0.068(3) Uani 1 1 d . . . . .
H50C H 0.9887 0.6532 0.7427 0.082 Uiso 1 1 calc R U . . .
H50D H 1.1051 0.6454 0.7221 0.082 Uiso 1 1 calc R U . . .
C10A C 0.6292(9) 0.5886(8) 0.0719(6) 0.076(3) Uani 1 1 d . U . . .
H10I H 0.6767 0.5349 0.0912 0.091 Uiso 1 1 calc R U . . .
H10J H 0.5875 0.5736 0.0203 0.091 Uiso 1 1 calc R U . . .
C100 C 0.5427(8) 0.6119(6) 0.6509(7) 0.087(4) Uani 1 1 d . . . . .
H10K H 0.4788 0.6514 0.6289 0.104 Uiso 1 1 calc R U . . .
H10L H 0.5365 0.5905 0.7006 0.104 Uiso 1 1 calc R U . . .
C14A C 1.0161(9) 0.7890(9) 0.1830(7) 0.094(4) Uani 1 1 d . U . . .
H14A H 1.0748 0.8020 0.1607 0.113 Uiso 1 1 calc R U . . .
C15A C 1.0268(8) 0.8121(7) 0.2535(6) 0.073(3) Uani 1 1 d . U . . .
H15A H 1.0934 0.8383 0.2822 0.088 Uiso 1 1 calc R U . . .
C501 C 0.9788(13) 0.4565(8) 0.7415(6) 0.125(7) Uani 1 1 d . . . . .
H50E H 1.0024 0.3919 0.7558 0.150 Uiso 1 1 calc R U . . .
H50F H 0.9096 0.4692 0.7555 0.150 Uiso 1 1 calc R U . . .
C502 C 1.0652(12) 0.5263(10) 0.7744(7) 0.117(5) Uani 1 1 d . U . . .
H50G H 1.1385 0.5023 0.7744 0.140 Uiso 1 1 calc R U . . .
H50H H 1.0637 0.5418 0.8263 0.140 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
U1A N30A 2.286(5) . ?
U1A N10A 2.328(5) . ?
U1A N20A 2.358(6) . ?
U1A N31A 2.553(5) . ?
U1A O10A 2.573(4) . ?
U1A N21A 2.587(5) . ?
U1A N11A 2.625(6) . ?
U1A N1A 2.759(6) . ?
U1A C22A 2.972(7) . ?
U1A C12A 2.987(7) . ?
U1A C32A 2.988(6) . ?
U1A I1A 3.2533(5) . ?
U1 N30 2.327(5) . ?
U1 N10 2.343(5) . ?
U1 N20 2.357(5) . ?
U1 O100 2.562(5) . ?
U1 N31 2.563(5) . ?
U1 N21 2.597(5) . ?
U1 N11 2.613(5) . ?
U1 N1 2.789(5) . ?
U1 C22 2.936(6) . ?
U1 C12 2.977(7) . ?
U1 C32 3.002(5) . ?
U1 I1 3.2153(5) . ?
O10A C200 1.443(8) . ?
O10A C203 1.461(9) . ?
N1 C30 1.471(8) . ?
N1 C20 1.475(8) . ?
N1 C10 1.479(8) . ?
O400 C403 1.434(8) . ?
O400 C400 1.437(8) . ?
O100 C100 1.418(9) . ?
O100 C103 1.470(8) . ?
N11 C16 1.329(7) . ?
N11 C12 1.376(8) . ?
O300 C300 1.422(8) . ?
O300 C303 1.441(8) . ?
O500 C500 1.414(9) . ?
O500 C503 1.440(9) . ?
N21 C26 1.336(8) . ?
N21 C22 1.346(7) . ?
N30 C32 1.393(7) . ?
N30 C31 1.450(7) . ?
N10 C12 1.328(8) . ?
N10 C11 1.443(7) . ?
N31A C36A 1.331(7) . ?
N31A C32A 1.388(7) . ?
N20 C22 1.354(8) . ?
N20 C21 1.456(8) . ?
N11A C16A 1.338(9) . ?
N11A C12A 1.356(9) . ?
N31 C36 1.346(7) . ?
N31 C32 1.402(7) . ?
N10A C12A 1.348(10) . ?
N10A C11A 1.430(9) . ?
N30A C32A 1.392(7) . ?
N30A C31A 1.468(9) . ?
N21A C26A 1.333(8) . ?
N21A C22A 1.367(9) . ?
C26 C25 1.377(9) . ?
C26 H26 0.9500 . ?
C32 C33 1.343(8) . ?
C22 C23 1.423(9) . ?
C12A C13A 1.403(11) . ?
C36A C35A 1.381(8) . ?
C36A H36A 0.9500 . ?
C14 C13 1.368(8) . ?
C14 C15 1.403(9) . ?
C14 H14 0.9500 . ?
C31 C30 1.533(9) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C24 C23 1.360(9) . ?
C24 C25 1.395(9) . ?
C24 H24 0.9500 . ?
C25 H25 0.9500 . ?
C20 C21 1.508(9) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C36 C35 1.372(10) . ?
C36 H36 0.9500 . ?
C23 H23 0.9500 . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C32A C33A 1.350(8) . ?
C16 C15 1.379(9) . ?
C16 H16 0.9500 . ?
C12 C13 1.422(9) . ?
C13 H13 0.9500 . ?
C33A C34A 1.372(10) . ?
C33A H33A 0.9500 . ?
C34 C35 1.360(10) . ?
C34 C33 1.375(9) . ?
C34 H34 0.9500 . ?
C22A N20A 1.345(9) . ?
C22A C23A 1.411(10) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C23A C24A 1.367(11) . ?
C23A H23A 0.9500 . ?
C103 C102 1.505(10) . ?
C103 H10A 0.9900 . ?
C103 H10B 0.9900 . ?
N20A C21A 1.464(10) . ?
C15 H15 0.9500 . ?
C11 C10 1.527(9) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C10 H10C 0.9900 . ?
C10 H10D 0.9900 . ?
C33 H33 0.9500 . ?
C35A C34A 1.371(9) . ?
C35A H35A 0.9500 . ?
N1A C20A 1.355(10) . ?
N1A C30A 1.408(9) . ?
N1A C10A 1.615(11) . ?
C26A C25A 1.380(10) . ?
C26A H26A 0.9500 . ?
C35 H35 0.9500 . ?
C102 C101 1.512(10) . ?
C102 H10E 0.9900 . ?
C102 H10F 0.9900 . ?
C34A H34A 0.9500 . ?
C403 C402 1.486(9) . ?
C403 H40A 0.9900 . ?
C403 H40B 0.9900 . ?
C101 C100 1.469(10) . ?
C101 H10G 0.9900 . ?
C101 H10H 0.9900 . ?
C300 C301 1.491(11) . ?
C300 H30C 0.9900 . ?
C300 H30D 0.9900 . ?
C301 C302 1.478(10) . ?
C301 H30E 0.9900 . ?
C301 H30F 0.9900 . ?
C400 C401 1.541(9) . ?
C400 H40C 0.9900 . ?
C400 H40D 0.9900 . ?
C200 C201 1.479(9) . ?
C200 H20C 0.9900 . ?
C200 H20D 0.9900 . ?
C16A C15A 1.345(12) . ?
C16A H16A 0.9500 . ?
C11A C10A 1.392(12) . ?
C11A H11C 0.9900 . ?
C11A H11D 0.9900 . ?
C31A C30A 1.411(9) . ?
C31A H31C 0.9900 . ?
C31A H31D 0.9900 . ?
C303 C302 1.503(10) . ?
C303 H30G 0.9900 . ?
C303 H30H 0.9900 . ?
C402 C401 1.526(9) . ?
C402 H40E 0.9900 . ?
C402 H40F 0.9900 . ?
C302 H30I 0.9900 . ?
C302 H30J 0.9900 . ?
C500 C501 1.505(11) . ?
C500 H50A 0.9900 . ?
C500 H50B 0.9900 . ?
C30A H30K 0.9900 . ?
C30A H30L 0.9900 . ?
C13A C14A 1.429(16) . ?
C13A H13A 0.9500 . ?
C201 C202 1.454(11) . ?
C201 H20E 0.9900 . ?
C201 H20F 0.9900 . ?
C401 H40G 0.9900 . ?
C401 H40H 0.9900 . ?
C25A C24A 1.369(11) . ?
C25A H25A 0.9500 . ?
C21A C20A 1.581(14) . ?
C21A H21C 0.9900 . ?
C21A H21D 0.9900 . ?
C20A H20G 0.9900 . ?
C20A H20H 0.9900 . ?
C24A H24A 0.9500 . ?
C202 C203 1.442(11) . ?
C202 H20I 0.9900 . ?
C202 H20J 0.9900 . ?
C203 H20K 0.9900 . ?
C203 H20L 0.9900 . ?
C503 C502 1.510(15) . ?
C503 H50C 0.9900 . ?
C503 H50D 0.9900 . ?
C10A H10I 0.9900 . ?
C10A H10J 0.9900 . ?
C100 H10K 0.9900 . ?
C100 H10L 0.9900 . ?
C14A C15A 1.319(15) . ?
C14A H14A 0.9500 . ?
C15A H15A 0.9500 . ?
C501 C502 1.486(18) . ?
C501 H50E 0.9900 . ?
C501 H50F 0.9900 . ?
C502 H50G 0.9900 . ?
C502 H50H 0.9900 . ?

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
N30A U1A N10A 91.68(18) . . ?
N30A U1A N20A 91.2(2) . . ?
N10A U1A N20A 115.3(2) . . ?
N30A U1A N31A 54.05(17) . . ?
N10A U1A N31A 111.78(19) . . ?
N20A U1A N31A 121.26(18) . . ?
N30A U1A O10A 152.56(16) . . ?
N10A U1A O10A 74.53(17) . . ?
N20A U1A O10A 74.28(18) . . ?
N31A U1A O10A 153.16(16) . . ?
N30A U1A N21A 83.69(17) . . ?
N10A U1A N21A 167.3(2) . . ?
N20A U1A N21A 53.18(19) . . ?
N31A U1A N21A 74.96(17) . . ?
O10A U1A N21A 104.55(15) . . ?
N30A U1A N11A 102.22(19) . . ?
N10A U1A N11A 52.7(2) . . ?
N20A U1A N11A 161.7(2) . . ?
N31A U1A N11A 77.02(19) . . ?
O10A U1A N11A 88.30(17) . . ?
N21A U1A N11A 139.94(19) . . ?
N30A U1A N1A 63.74(17) . . ?
N10A U1A N1A 61.9(2) . . ?
N20A U1A N1A 62.2(2) . . ?
N31A U1A N1A 117.47(16) . . ?
O10A U1A N1A 88.82(15) . . ?
N21A U1A N1A 105.5(2) . . ?
N11A U1A N1A 112.7(2) . . ?
N30A U1A C22A 84.40(19) . . ?
N10A U1A C22A 140.5(2) . . ?
N20A U1A C22A 26.11(19) . . ?
N31A U1A C22A 97.51(18) . . ?
O10A U1A C22A 91.35(16) . . ?
N21A U1A C22A 27.37(18) . . ?
N11A U1A C22A 165.83(19) . . ?
N1A U1A C22A 81.4(2) . . ?
N30A U1A C12A 98.94(18) . . ?
N10A U1A C12A 25.8(2) . . ?
N20A U1A C12A 139.1(2) . . ?
N31A U1A C12A 96.11(18) . . ?
O10A U1A C12A 79.00(16) . . ?
N21A U1A C12A 166.9(2) . . ?
N11A U1A C12A 27.0(2) . . ?
N1A U1A C12A 87.1(2) . . ?
C22A U1A C12A 165.2(2) . . ?
N30A U1A C32A 26.58(16) . . ?
N10A U1A C32A 100.91(17) . . ?
N20A U1A C32A 109.02(19) . . ?
N31A U1A C32A 27.62(15) . . ?
O10A U1A C32A 175.32(14) . . ?
N21A U1A C32A 80.13(16) . . ?
N11A U1A C32A 88.05(17) . . ?
N1A U1A C32A 89.88(16) . . ?
C22A U1A C32A 92.91(17) . . ?
C12A U1A C32A 96.44(17) . . ?
N30A U1A I1A 131.06(12) . . ?
N10A U1A I1A 117.77(15) . . ?
N20A U1A I1A 107.41(17) . . ?
N31A U1A I1A 78.10(11) . . ?
O10A U1A I1A 76.15(10) . . ?
N21A U1A I1A 73.64(12) . . ?
N11A U1A I1A 73.00(12) . . ?
N1A U1A I1A 163.96(13) . . ?
C22A U1A I1A 93.17(14) . . ?
C12A U1A I1A 95.38(16) . . ?
C32A U1A I1A 105.54(11) . . ?
N30 U1 N10 87.86(18) . . ?
N30 U1 N20 97.84(17) . . ?
N10 U1 N20 116.32(17) . . ?
N30 U1 O100 151.53(16) . . ?
N10 U1 O100 72.92(16) . . ?
N20 U1 O100 73.45(16) . . ?
N30 U1 N31 53.70(16) . . ?
N10 U1 N31 112.74(16) . . ?
N20 U1 N31 121.22(17) . . ?
O100 U1 N31 153.52(16) . . ?
N30 U1 N21 77.79(17) . . ?
N10 U1 N21 159.86(16) . . ?
N20 U1 N21 53.13(17) . . ?
O100 U1 N21 114.34(15) . . ?
N31 U1 N21 69.77(16) . . ?
N30 U1 N11 96.51(16) . . ?
N10 U1 N11 52.87(16) . . ?
N20 U1 N11 161.65(17) . . ?
O100 U1 N11 88.52(15) . . ?
N31 U1 N11 76.72(16) . . ?
N21 U1 N11 142.09(15) . . ?
N30 U1 N1 63.68(15) . . ?
N10 U1 N1 62.22(16) . . ?
N20 U1 N1 64.47(17) . . ?
O100 U1 N1 88.49(15) . . ?
N31 U1 N1 117.38(15) . . ?
N21 U1 N1 98.40(15) . . ?
N11 U1 N1 112.69(15) . . ?
N30 U1 C22 82.60(17) . . ?
N10 U1 C22 137.51(17) . . ?
N20 U1 C22 26.89(16) . . ?
O100 U1 C22 97.35(15) . . ?
N31 U1 C22 94.38(17) . . ?
N21 U1 C22 27.29(16) . . ?
N11 U1 C22 169.30(16) . . ?
N1 U1 C22 76.55(16) . . ?
N30 U1 C12 89.99(17) . . ?
N10 U1 C12 25.53(16) . . ?
N20 U1 C12 141.05(17) . . ?
O100 U1 C12 81.61(15) . . ?
N31 U1 C12 94.06(16) . . ?
N21 U1 C12 163.48(16) . . ?
N11 U1 C12 27.53(15) . . ?
N1 U1 C12 85.81(16) . . ?
C22 U1 C12 162.35(17) . . ?
N30 U1 C32 26.66(15) . . ?
N10 U1 C32 105.12(16) . . ?
N20 U1 C32 107.07(16) . . ?
O100 U1 C32 177.90(15) . . ?
N31 U1 C32 27.79(14) . . ?
N21 U1 C32 67.26(15) . . ?
N11 U1 C32 90.82(15) . . ?
N1 U1 C32 89.93(14) . . ?
C22 U1 C32 83.61(16) . . ?
C12 U1 C32 96.91(16) . . ?
N30 U1 I1 131.56(12) . . ?
N10 U1 I1 119.64(12) . . ?
N20 U1 I1 102.74(13) . . ?
O100 U1 I1 76.85(11) . . ?
N31 U1 I1 78.25(11) . . ?
N21 U1 I1 80.49(11) . . ?
N11 U1 I1 75.73(10) . . ?
N1 U1 I1 163.12(10) . . ?
C22 U1 I1 96.83(12) . . ?
C12 U1 I1 100.05(12) . . ?
C32 U1 I1 104.91(10) . . ?
C200 O10A C203 109.1(5) . . ?
C200 O10A U1A 122.0(4) . . ?
C203 O10A U1A 122.5(4) . . ?
C30 N1 C20 111.7(5) . . ?
C30 N1 C10 110.1(5) . . ?
C20 N1 C10 109.3(5) . . ?
C30 N1 U1 109.4(3) . . ?
C20 N1 U1 110.4(4) . . ?
C10 N1 U1 105.7(4) . . ?
C403 O400 C400 107.6(5) . . ?
C100 O100 C103 108.0(5) . . ?
C100 O100 U1 122.6(4) . . ?
C103 O100 U1 123.6(4) . . ?
C16 N11 C12 119.7(6) . . ?
C16 N11 U1 148.5(4) . . ?
C12 N11 U1 91.1(4) . . ?
C300 O300 C303 106.2(6) . . ?
C500 O500 C503 109.2(6) . . ?
C26 N21 C22 119.4(5) . . ?
C26 N21 U1 145.6(4) . . ?
C22 N21 U1 90.5(4) . . ?
C32 N30 C31 121.1(5) . . ?
C32 N30 U1 104.8(3) . . ?
C31 N30 U1 128.9(4) . . ?
C12 N10 C11 121.2(5) . . ?
C12 N10 U1 105.0(4) . . ?
C11 N10 U1 132.7(4) . . ?
C36A N31A C32A 118.0(5) . . ?
C36A N31A U1A 147.5(4) . . ?
C32A N31A U1A 93.9(3) . . ?
C22 N20 C21 118.8(5) . . ?
C22 N20 U1 101.1(4) . . ?
C21 N20 U1 123.4(4) . . ?
C16A N11A C12A 120.0(7) . . ?
C16A N11A U1A 148.1(5) . . ?
C12A N11A U1A 91.6(5) . . ?
C36 N31 C32 117.0(5) . . ?
C36 N31 U1 145.7(4) . . ?
C32 N31 U1 93.8(3) . . ?
C12A N10A C11A 122.6(6) . . ?
C12A N10A U1A 105.6(4) . . ?
C11A N10A U1A 131.5(5) . . ?
C32A N30A C31A 120.8(5) . . ?
C32A N30A U1A 106.1(4) . . ?
C31A N30A U1A 131.6(4) . . ?
C26A N21A C22A 120.1(6) . . ?
C26A N21A U1A 147.1(5) . . ?
C22A N21A U1A 92.2(4) . . ?
N21 C26 C25 123.9(6) . . ?
N21 C26 H26 118.0 . . ?
C25 C26 H26 118.0 . . ?
C33 C32 N30 132.3(6) . . ?
C33 C32 N31 122.6(5) . . ?
N30 C32 N31 105.1(5) . . ?
C33 C32 U1 168.1(5) . . ?
N30 C32 U1 48.6(3) . . ?
N31 C32 U1 58.4(3) . . ?
N21 C22 N20 111.1(5) . . ?
N21 C22 C23 120.3(6) . . ?
N20 C22 C23 128.6(6) . . ?
N21 C22 U1 62.2(3) . . ?
N20 C22 U1 52.0(3) . . ?
C23 C22 U1 162.4(4) . . ?
N10A C12A N11A 109.9(6) . . ?
N10A C12A C13A 129.6(8) . . ?
N11A C12A C13A 120.5(8) . . ?
N10A C12A U1A 48.6(3) . . ?
N11A C12A U1A 61.4(4) . . ?
C13A C12A U1A 175.3(5) . . ?
N31A C36A C35A 122.6(6) . . ?
N31A C36A H36A 118.7 . . ?
C35A C36A H36A 118.7 . . ?
C13 C14 C15 120.0(6) . . ?
C13 C14 H14 120.0 . . ?
C15 C14 H14 120.0 . . ?
N30 C31 C30 106.8(5) . . ?
N30 C31 H31A 110.4 . . ?
C30 C31 H31A 110.4 . . ?
N30 C31 H31B 110.4 . . ?
C30 C31 H31B 110.4 . . ?
H31A C31 H31B 108.6 . . ?
C23 C24 C25 121.6(7) . . ?
C23 C24 H24 119.2 . . ?
C25 C24 H24 119.2 . . ?
C26 C25 C24 116.4(6) . . ?
C26 C25 H25 121.8 . . ?
C24 C25 H25 121.8 . . ?
N1 C20 C21 111.1(5) . . ?
N1 C20 H20A 109.4 . . ?
C21 C20 H20A 109.4 . . ?
N1 C20 H20B 109.4 . . ?
C21 C20 H20B 109.4 . . ?
H20A C20 H20B 108.0 . . ?
N31 C36 C35 122.5(7) . . ?
N31 C36 H36 118.7 . . ?
C35 C36 H36 118.7 . . ?
C24 C23 C22 118.3(6) . . ?
C24 C23 H23 120.9 . . ?
C22 C23 H23 120.9 . . ?
N1 C30 C31 110.4(5) . . ?
N1 C30 H30A 109.6 . . ?
C31 C30 H30A 109.6 . . ?
N1 C30 H30B 109.6 . . ?
C31 C30 H30B 109.6 . . ?
H30A C30 H30B 108.1 . . ?
C33A C32A N31A 121.8(6) . . ?
C33A C32A N30A 132.7(6) . . ?
N31A C32A N30A 105.4(5) . . ?
C33A C32A U1A 175.1(5) . . ?
N31A C32A U1A 58.5(3) . . ?
N30A C32A U1A 47.3(3) . . ?
N11 C16 C15 123.2(6) . . ?
N11 C16 H16 118.4 . . ?
C15 C16 H16 118.4 . . ?
N10 C12 N11 110.3(6) . . ?
N10 C12 C13 130.1(6) . . ?
N11 C12 C13 119.5(6) . . ?
N10 C12 U1 49.5(3) . . ?
N11 C12 U1 61.3(3) . . ?
C13 C12 U1 175.4(4) . . ?
C14 C13 C12 119.4(6) . . ?
C14 C13 H13 120.3 . . ?
C12 C13 H13 120.3 . . ?
C32A C33A C34A 118.7(7) . . ?
C32A C33A H33A 120.6 . . ?
C34A C33A H33A 120.6 . . ?
C35 C34 C33 122.0(7) . . ?
C35 C34 H34 119.0 . . ?
C33 C34 H34 119.0 . . ?
N20A C22A N21A 110.1(6) . . ?
N20A C22A C23A 130.3(7) . . ?
N21A C22A C23A 119.6(7) . . ?
N20A C22A U1A 50.5(3) . . ?
N21A C22A U1A 60.4(3) . . ?
C23A C22A U1A 170.8(5) . . ?
N20 C21 C20 108.9(5) . . ?
N20 C21 H21A 109.9 . . ?
C20 C21 H21A 109.9 . . ?
N20 C21 H21B 109.9 . . ?
C20 C21 H21B 109.9 . . ?
H21A C21 H21B 108.3 . . ?
C24A C23A C22A 118.5(8) . . ?
C24A C23A H23A 120.7 . . ?
C22A C23A H23A 120.7 . . ?
O100 C103 C102 101.3(6) . . ?
O100 C103 H10A 111.5 . . ?
C102 C103 H10A 111.5 . . ?
O100 C103 H10B 111.5 . . ?
C102 C103 H10B 111.5 . . ?
H10A C103 H10B 109.3 . . ?
C22A N20A C21A 122.0(6) . . ?
C22A N20A U1A 103.4(4) . . ?
C21A N20A U1A 126.8(5) . . ?
C16 C15 C14 118.1(6) . . ?
C16 C15 H15 120.9 . . ?
C14 C15 H15 120.9 . . ?
N10 C11 C10 106.7(5) . . ?
N10 C11 H11A 110.4 . . ?
C10 C11 H11A 110.4 . . ?
N10 C11 H11B 110.4 . . ?
C10 C11 H11B 110.4 . . ?
H11A C11 H11B 108.6 . . ?
N1 C10 C11 111.5(5) . . ?
N1 C10 H10C 109.3 . . ?
C11 C10 H10C 109.3 . . ?
N1 C10 H10D 109.3 . . ?
C11 C10 H10D 109.3 . . ?
H10C C10 H10D 108.0 . . ?
C32 C33 C34 117.7(7) . . ?
C32 C33 H33 121.2 . . ?
C34 C33 H33 121.2 . . ?
C34A C35A C36A 118.0(6) . . ?
C34A C35A H35A 121.0 . . ?
C36A C35A H35A 121.0 . . ?
C20A N1A C30A 121.3(8) . . ?
C20A N1A C10A 105.9(7) . . ?
C30A N1A C10A 97.7(7) . . ?
C20A N1A U1A 110.7(5) . . ?
C30A N1A U1A 110.2(4) . . ?
C10A N1A U1A 109.7(5) . . ?
N21A C26A C25A 122.0(8) . . ?
N21A C26A H26A 119.0 . . ?
C25A C26A H26A 119.0 . . ?
C34 C35 C36 118.2(6) . . ?
C34 C35 H35 120.9 . . ?
C36 C35 H35 120.9 . . ?
C103 C102 C101 103.5(6) . . ?
C103 C102 H10E 111.1 . . ?
C101 C102 H10E 111.1 . . ?
C103 C102 H10F 111.1 . . ?
C101 C102 H10F 111.1 . . ?
H10E C102 H10F 109.0 . . ?
C33A C34A C35A 120.9(7) . . ?
C33A C34A H34A 119.5 . . ?
C35A C34A H34A 119.5 . . ?
O400 C403 C402 104.1(5) . . ?
O400 C403 H40A 110.9 . . ?
C402 C403 H40A 110.9 . . ?
O400 C403 H40B 110.9 . . ?
C402 C403 H40B 110.9 . . ?
H40A C403 H40B 109.0 . . ?
C100 C101 C102 105.1(6) . . ?
C100 C101 H10G 110.7 . . ?
C102 C101 H10G 110.7 . . ?
C100 C101 H10H 110.7 . . ?
C102 C101 H10H 110.7 . . ?
H10G C101 H10H 108.8 . . ?
O300 C300 C301 107.4(6) . . ?
O300 C300 H30C 110.2 . . ?
C301 C300 H30C 110.2 . . ?
O300 C300 H30D 110.2 . . ?
C301 C300 H30D 110.2 . . ?
H30C C300 H30D 108.5 . . ?
C302 C301 C300 105.7(6) . . ?
C302 C301 H30E 110.6 . . ?
C300 C301 H30E 110.6 . . ?
C302 C301 H30F 110.6 . . ?
C300 C301 H30F 110.6 . . ?
H30E C301 H30F 108.7 . . ?
O400 C400 C401 106.7(5) . . ?
O400 C400 H40C 110.4 . . ?
C401 C400 H40C 110.4 . . ?
O400 C400 H40D 110.4 . . ?
C401 C400 H40D 110.4 . . ?
H40C C400 H40D 108.6 . . ?
O10A C200 C201 106.9(6) . . ?
O10A C200 H20C 110.3 . . ?
C201 C200 H20C 110.3 . . ?
O10A C200 H20D 110.3 . . ?
C201 C200 H20D 110.3 . . ?
H20C C200 H20D 108.6 . . ?
N11A C16A C15A 122.7(9) . . ?
N11A C16A H16A 118.7 . . ?
C15A C16A H16A 118.7 . . ?
C10A C11A N10A 108.1(7) . . ?
C10A C11A H11C 110.1 . . ?
N10A C11A H11C 110.1 . . ?
C10A C11A H11D 110.1 . . ?
N10A C11A H11D 110.1 . . ?
H11C C11A H11D 108.4 . . ?
C30A C31A N30A 110.0(6) . . ?
C30A C31A H31C 109.7 . . ?
N30A C31A H31C 109.7 . . ?
C30A C31A H31D 109.7 . . ?
N30A C31A H31D 109.7 . . ?
H31C C31A H31D 108.2 . . ?
O300 C303 C302 104.3(5) . . ?
O300 C303 H30G 110.9 . . ?
C302 C303 H30G 110.9 . . ?
O300 C303 H30H 110.9 . . ?
C302 C303 H30H 110.9 . . ?
H30G C303 H30H 108.9 . . ?
C403 C402 C401 104.3(6) . . ?
C403 C402 H40E 110.9 . . ?
C401 C402 H40E 110.9 . . ?
C403 C402 H40F 110.9 . . ?
C401 C402 H40F 110.9 . . ?
H40E C402 H40F 108.9 . . ?
C301 C302 C303 104.5(7) . . ?
C301 C302 H30I 110.8 . . ?
C303 C302 H30I 110.8 . . ?
C301 C302 H30J 110.8 . . ?
C303 C302 H30J 110.8 . . ?
H30I C302 H30J 108.9 . . ?
O500 C500 C501 106.8(7) . . ?
O500 C500 H50A 110.4 . . ?
C501 C500 H50A 110.4 . . ?
O500 C500 H50B 110.4 . . ?
C501 C500 H50B 110.4 . . ?
H50A C500 H50B 108.6 . . ?
C31A C30A N1A 121.7(7) . . ?
C31A C30A H30K 106.9 . . ?
N1A C30A H30K 106.9 . . ?
C31A C30A H30L 106.9 . . ?
N1A C30A H30L 106.9 . . ?
H30K C30A H30L 106.7 . . ?
C12A C13A C14A 115.4(9) . . ?
C12A C13A H13A 122.3 . . ?
C14A C13A H13A 122.3 . . ?
C202 C201 C200 107.2(7) . . ?
C202 C201 H20E 110.3 . . ?
C200 C201 H20E 110.3 . . ?
C202 C201 H20F 110.3 . . ?
C200 C201 H20F 110.3 . . ?
H20E C201 H20F 108.5 . . ?
C402 C401 C400 103.1(6) . . ?
C402 C401 H40G 111.1 . . ?
C400 C401 H40G 111.1 . . ?
C402 C401 H40H 111.1 . . ?
C400 C401 H40H 111.1 . . ?
H40G C401 H40H 109.1 . . ?
C24A C25A C26A 118.5(7) . . ?
C24A C25A H25A 120.7 . . ?
C26A C25A H25A 120.7 . . ?
N20A C21A C20A 111.2(7) . . ?
N20A C21A H21C 109.4 . . ?
C20A C21A H21C 109.4 . . ?
N20A C21A H21D 109.4 . . ?
C20A C21A H21D 109.4 . . ?
H21C C21A H21D 108.0 . . ?
N1A C20A C21A 107.4(8) . . ?
N1A C20A H20G 110.2 . . ?
C21A C20A H20G 110.2 . . ?
N1A C20A H20H 110.2 . . ?
C21A C20A H20H 110.2 . . ?
H20G C20A H20H 108.5 . . ?
C23A C24A C25A 121.1(7) . . ?
C23A C24A H24A 119.4 . . ?
C25A C24A H24A 119.4 . . ?
C203 C202 C201 108.7(7) . . ?
C203 C202 H20I 110.0 . . ?
C201 C202 H20I 110.0 . . ?
C203 C202 H20J 110.0 . . ?
C201 C202 H20J 110.0 . . ?
H20I C202 H20J 108.3 . . ?
C202 C203 O10A 106.9(6) . . ?
C202 C203 H20K 110.3 . . ?
O10A C203 H20K 110.3 . . ?
C202 C203 H20L 110.3 . . ?
O10A C203 H20L 110.3 . . ?
H20K C203 H20L 108.6 . . ?
O500 C503 C502 104.0(8) . . ?
O500 C503 H50C 111.0 . . ?
C502 C503 H50C 111.0 . . ?
O500 C503 H50D 111.0 . . ?
C502 C503 H50D 111.0 . . ?
H50C C503 H50D 109.0 . . ?
C11A C10A N1A 110.1(7) . . ?
C11A C10A H10I 109.6 . . ?
N1A C10A H10I 109.6 . . ?
C11A C10A H10J 109.6 . . ?
N1A C10A H10J 109.6 . . ?
H10I C10A H10J 108.1 . . ?
O100 C100 C101 107.8(7) . . ?
O100 C100 H10K 110.2 . . ?
C101 C100 H10K 110.2 . . ?
O100 C100 H10L 110.2 . . ?
C101 C100 H10L 110.2 . . ?
H10K C100 H10L 108.5 . . ?
C15A C14A C13A 122.3(10) . . ?
C15A C14A H14A 118.8 . . ?
C13A C14A H14A 118.8 . . ?
C14A C15A C16A 119.0(11) . . ?
C14A C15A H15A 120.5 . . ?
C16A C15A H15A 120.5 . . ?
C500 C501 C502 99.1(11) . . ?
C500 C501 H50E 111.9 . . ?
C502 C501 H50E 111.9 . . ?
C500 C501 H50F 111.9 . . ?
C502 C501 H50F 111.9 . . ?
H50E C501 H50F 109.6 . . ?
C501 C502 C503 104.6(9) . . ?
C501 C502 H50G 110.8 . . ?
C503 C502 H50G 110.8 . . ?
C501 C502 H50H 110.8 . . ?
C503 C502 H50H 110.8 . . ?
H50G C502 H50H 108.9 . . ?

_refine_diff_density_max         3.519
_refine_diff_density_min         -1.299
_refine_diff_density_rms         0.224


_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
####################################################################### 
# 
# 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_shelx_CCDC3
_database_code_depnum_ccdc_archive 'CCDC 1526524'
_audit_update_record             
;
2017-01-10 deposited with the CCDC.
2017-08-14 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            'C62 H64 N16 O4 U2'
_chemical_formula_weight         1573.35

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'

_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, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-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                   9.5899(6)
_cell_length_b                   20.9064(13)
_cell_length_c                   28.9404(17)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5802.3(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3859
_cell_measurement_theta_min      1.41
_cell_measurement_theta_max      25.44

_exptl_crystal_description       plate
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.801
_exptl_crystal_F_000             3056
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.01
_exptl_absorpt_coefficient_mu    5.639
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.642
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_process_details   'Blessing, 1995'
_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 Quazar'
_diffrn_measurement_method       'omega phi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            55064
_diffrn_reflns_av_unetI/netI     0.0549
_diffrn_reflns_av_R_equivalents  0.0898
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         1.407
_diffrn_reflns_theta_max         25.441
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             5360
_reflns_number_gt                3859
_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 ApexIII suite, 2016'
_computing_cell_refinement       'Bruker ApexIII suite, 2016'
_computing_data_reduction        'Bruker ApexIII suite, 2016'
_computing_structure_solution    ShelXT
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Diamond, 3D'
_computing_publication_material  WinGX
_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)+(0.0531P)²+8.8394P] 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         5360
_refine_ls_number_parameters     380
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0714
_refine_ls_R_factor_gt           0.0454
_refine_ls_wR_factor_ref         0.1080
_refine_ls_wR_factor_gt          0.0971
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_restrained_S_all      1.044
_refine_ls_shift/su_max          0.003
_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
C1 C 0.5154(7) 0.4559(3) 0.5374(2) 0.0209(15) Uani 1 1 d . . . . .
C2 C 0.6064(7) 0.5001(3) 0.4666(2) 0.0218(15) Uani 1 1 d . . . . .
C3 C 0.6153(7) 0.4566(3) 0.5039(2) 0.0223(15) Uani 1 1 d . . . . .
H3 H 0.6914 0.4277 0.5056 0.027 Uiso 1 1 calc R U . . .
C10 C -0.0186(8) 0.3651(4) 0.6682(2) 0.049(2) Uani 1 1 d . . . . .
H10A H -0.1101 0.3788 0.6806 0.059 Uiso 1 1 calc R U . . .
H10B H -0.0003 0.3211 0.6792 0.059 Uiso 1 1 calc R U . . .
C11 C -0.0225(8) 0.3660(5) 0.6158(2) 0.051(2) Uani 1 1 d . . . . .
H11A H -0.0759 0.3288 0.6042 0.062 Uiso 1 1 calc R U . . .
H11B H -0.0684 0.4055 0.6048 0.062 Uiso 1 1 calc R U . . .
C12 C 0.1507(8) 0.3381(4) 0.5580(2) 0.0327(18) Uani 1 1 d . . . . .
C13 C 0.0640(9) 0.3120(4) 0.5236(2) 0.039(2) Uani 1 1 d . . . . .
H13 H -0.0343 0.3111 0.5275 0.047 Uiso 1 1 calc R U . . .
C14 C 0.1242(9) 0.2880(4) 0.4846(3) 0.045(2) Uani 1 1 d . . . . .
H14 H 0.0677 0.2686 0.4615 0.054 Uiso 1 1 calc R U . . .
C15 C 0.2654(10) 0.2916(4) 0.4784(3) 0.047(2) Uani 1 1 d . . . . .
H15 H 0.3075 0.2753 0.4511 0.056 Uiso 1 1 calc R U . . .
C16 C 0.3451(8) 0.3192(4) 0.5124(2) 0.0375(19) Uani 1 1 d . . . . .
H16 H 0.4426 0.3233 0.5075 0.045 Uiso 1 1 calc R U . . .
C20 C 0.0416(8) 0.4746(4) 0.6870(3) 0.047(2) Uani 1 1 d . . . . .
H20A H -0.0313 0.4784 0.7111 0.056 Uiso 1 1 calc R U . . .
H20B H -0.0011 0.4857 0.6569 0.056 Uiso 1 1 calc R U . . .
C21 C 0.1586(8) 0.5211(4) 0.6974(3) 0.041(2) Uani 1 1 d . . . . .
H21A H 0.1344 0.5645 0.6863 0.050 Uiso 1 1 calc R U . . .
H21B H 0.1758 0.5233 0.7311 0.050 Uiso 1 1 calc R U . . .
C22 C 0.4057(8) 0.5259(4) 0.6783(2) 0.0325(19) Uani 1 1 d . . . . .
C23 C 0.4405(9) 0.5835(4) 0.7009(2) 0.037(2) Uani 1 1 d . . . . .
H23 H 0.3719 0.6070 0.7174 0.045 Uiso 1 1 calc R U . . .
C24 C 0.5750(10) 0.6046(4) 0.6986(2) 0.044(2) Uani 1 1 d . . . . .
H24 H 0.5997 0.6436 0.7133 0.053 Uiso 1 1 calc R U . . .
C25 C 0.6760(8) 0.5701(4) 0.6751(2) 0.039(2) Uani 1 1 d . . . . .
H25 H 0.7694 0.5851 0.6731 0.047 Uiso 1 1 calc R U . . .
C26 C 0.6369(8) 0.5141(4) 0.6550(2) 0.0335(18) Uani 1 1 d . . . . .
H26 H 0.7055 0.4900 0.6390 0.040 Uiso 1 1 calc R U . . .
C30 C 0.1398(8) 0.3874(4) 0.7316(2) 0.043(2) Uani 1 1 d . . . . .
H30A H 0.0580 0.3783 0.7513 0.052 Uiso 1 1 calc R U . . .
H30B H 0.1941 0.4222 0.7463 0.052 Uiso 1 1 calc R U . . .
C31 C 0.2301(8) 0.3277(4) 0.7279(2) 0.041(2) Uani 1 1 d . . . . .
H31A H 0.2770 0.3188 0.7577 0.049 Uiso 1 1 calc R U . . .
H31B H 0.1726 0.2901 0.7194 0.049 Uiso 1 1 calc R U . . .
C32 C 0.4385(8) 0.3008(4) 0.6832(2) 0.0307(18) Uani 1 1 d . . . . .
C33 C 0.4770(9) 0.2435(4) 0.7052(2) 0.037(2) Uani 1 1 d . . . . .
H33 H 0.4217 0.2261 0.7294 0.044 Uiso 1 1 calc R U . . .
C34 C 0.5942(9) 0.2141(4) 0.6912(2) 0.041(2) Uani 1 1 d . . . . .
H34 H 0.6243 0.1765 0.7067 0.049 Uiso 1 1 calc R U . . .
C35 C 0.6719(8) 0.2374(4) 0.6545(2) 0.0347(18) Uani 1 1 d . . . . .
H35 H 0.7550 0.2166 0.6448 0.042 Uiso 1 1 calc R U . . .
C36 C 0.6248(8) 0.2917(3) 0.6326(2) 0.0262(16) Uani 1 1 d . . . . .
H36 H 0.6754 0.3074 0.6068 0.031 Uiso 1 1 calc R U . . .
C40 C 0.8243(8) 0.4689(4) 0.4316(2) 0.0306(18) Uani 1 1 d . . . . .
C41 C 0.8170(8) 0.4080(4) 0.4137(3) 0.0354(19) Uani 1 1 d . . . . .
C42 C 0.9378(9) 0.3733(4) 0.4054(3) 0.041(2) Uani 1 1 d . . . . .
H42 H 0.9332 0.3313 0.3930 0.049 Uiso 1 1 calc R U . . .
C43 C 1.0661(9) 0.4016(4) 0.4155(3) 0.047(2) Uani 1 1 d . . . . .
H43 H 1.1497 0.3795 0.4081 0.056 Uiso 1 1 calc R U . . .
C44 C 1.0734(8) 0.4610(4) 0.4360(2) 0.041(2) Uani 1 1 d . . . . .
H44 H 1.1601 0.4791 0.4449 0.050 Uiso 1 1 calc R U . . .
C45 C 0.9506(8) 0.4926(4) 0.4428(2) 0.0341(19) Uani 1 1 d . . . . .
H45 H 0.9544 0.5340 0.4563 0.041 Uiso 1 1 calc R U . . .
C46 C 0.6747(10) 0.3183(4) 0.3916(3) 0.055(2) Uani 1 1 d . . . . .
H46A H 0.7302 0.3109 0.3636 0.082 Uiso 1 1 calc R U . . .
H46B H 0.5771 0.3073 0.3855 0.082 Uiso 1 1 calc R U . . .
H46C H 0.7103 0.2916 0.4167 0.082 Uiso 1 1 calc R U . . .
N1 N 0.0919(6) 0.4085(3) 0.68546(18) 0.0342(16) Uani 1 1 d . . . . .
N2 N 0.6994(6) 0.5072(3) 0.43376(18) 0.0255(14) Uani 1 1 d . . . . .
N10 N 0.1179(7) 0.3633(3) 0.59935(19) 0.0347(15) Uani 1 1 d . . . . .
N11 N 0.2907(6) 0.3406(3) 0.5520(2) 0.0344(16) Uani 1 1 d . . . . .
N20 N 0.2820(7) 0.4972(3) 0.67351(18) 0.0334(15) Uani 1 1 d . . . . .
N21 N 0.5082(6) 0.4916(3) 0.65658(17) 0.0279(14) Uani 1 1 d . . . . .
N30 N 0.3326(6) 0.3410(3) 0.6920(2) 0.0360(16) Uani 1 1 d . . . . .
N31 N 0.5119(6) 0.3227(3) 0.64611(17) 0.0264(14) Uani 1 1 d . . . . .
O1 O 0.5172(5) 0.4189(2) 0.57300(13) 0.0233(11) Uani 1 1 d . . . . .
O2 O 0.6842(5) 0.3852(3) 0.40465(17) 0.0385(13) Uani 1 1 d . . . . .
U1 U 0.32755(2) 0.40830(2) 0.62654(2) 0.02288(11) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.288(7) . ?
C1 C3 1.363(9) . ?
C1 C2 1.491(9) 5_666 ?
C2 N2 1.312(8) . ?
C2 C3 1.413(9) . ?
C2 C1 1.491(9) 5_666 ?
C3 H3 0.9500 . ?
C10 N1 1.482(10) . ?
C10 C11 1.517(9) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 N10 1.429(9) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 N10 1.346(9) . ?
C12 N11 1.354(9) . ?
C12 C13 1.407(10) . ?
C12 U1 2.995(7) . ?
C13 C14 1.363(10) . ?
C13 H13 0.9500 . ?
C14 C15 1.368(12) . ?
C14 H14 0.9500 . ?
C15 C16 1.373(10) . ?
C15 H15 0.9500 . ?
C16 N11 1.337(9) . ?
C16 H16 0.9500 . ?
C20 N1 1.464(10) . ?
C20 C21 1.515(11) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 N20 1.459(9) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 N20 1.336(10) . ?
C22 N21 1.370(9) . ?
C22 C23 1.409(10) . ?
C22 U1 2.975(8) . ?
C23 C24 1.365(11) . ?
C23 H23 0.9500 . ?
C24 C25 1.387(11) . ?
C24 H24 0.9500 . ?
C25 C26 1.360(10) . ?
C25 H25 0.9500 . ?
C26 N21 1.322(9) . ?
C26 H26 0.9500 . ?
C30 N1 1.479(9) . ?
C30 C31 1.524(11) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 N30 1.457(9) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 N30 1.342(9) . ?
C32 N31 1.363(8) . ?
C32 C33 1.407(10) . ?
C32 U1 2.978(7) . ?
C33 C34 1.345(11) . ?
C33 H33 0.9500 . ?
C34 C35 1.386(10) . ?
C34 H34 0.9500 . ?
C35 C36 1.375(10) . ?
C35 H35 0.9500 . ?
C36 N31 1.322(9) . ?
C36 H36 0.9500 . ?
C40 C45 1.349(10) . ?
C40 C41 1.375(10) . ?
C40 N2 1.442(8) . ?
C41 O2 1.385(9) . ?
C41 C42 1.388(10) . ?
C42 C43 1.396(12) . ?
C42 H42 0.9500 . ?
C43 C44 1.377(11) . ?
C43 H43 0.9500 . ?
C44 C45 1.365(10) . ?
C44 H44 0.9500 . ?
C45 H45 0.9500 . ?
C46 O2 1.451(10) . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
N1 U1 2.831(5) . ?
N2 U1 2.497(5) 5_666 ?
N10 U1 2.355(6) . ?
N11 U1 2.604(6) . ?
N20 U1 2.344(6) . ?
N21 U1 2.605(6) . ?
N30 U1 2.360(6) . ?
N31 U1 2.578(6) . ?
O1 U1 2.400(4) . ?
U1 N2 2.497(5) 5_666 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 C3 124.5(6) . . ?
O1 C1 C2 116.3(5) . 5_666 ?
C3 C1 C2 119.2(6) . 5_666 ?
N2 C2 C3 125.8(6) . . ?
N2 C2 C1 114.0(6) . 5_666 ?
C3 C2 C1 120.2(6) . 5_666 ?
C1 C3 C2 120.5(6) . . ?
C1 C3 H3 119.7 . . ?
C2 C3 H3 119.7 . . ?
N1 C10 C11 110.3(6) . . ?
N1 C10 H10A 109.6 . . ?
C11 C10 H10A 109.6 . . ?
N1 C10 H10B 109.6 . . ?
C11 C10 H10B 109.6 . . ?
H10A C10 H10B 108.1 . . ?
N10 C11 C10 108.0(6) . . ?
N10 C11 H11A 110.1 . . ?
C10 C11 H11A 110.1 . . ?
N10 C11 H11B 110.1 . . ?
C10 C11 H11B 110.1 . . ?
H11A C11 H11B 108.4 . . ?
N10 C12 N11 109.3(6) . . ?
N10 C12 C13 130.0(7) . . ?
N11 C12 C13 120.7(7) . . ?
N10 C12 U1 49.5(4) . . ?
N11 C12 U1 60.3(4) . . ?
C13 C12 U1 173.5(5) . . ?
C14 C13 C12 118.6(8) . . ?
C14 C13 H13 120.7 . . ?
C12 C13 H13 120.7 . . ?
C13 C14 C15 120.5(7) . . ?
C13 C14 H14 119.8 . . ?
C15 C14 H14 119.8 . . ?
C14 C15 C16 118.7(8) . . ?
C14 C15 H15 120.7 . . ?
C16 C15 H15 120.7 . . ?
N11 C16 C15 122.5(8) . . ?
N11 C16 H16 118.7 . . ?
C15 C16 H16 118.7 . . ?
N1 C20 C21 111.6(7) . . ?
N1 C20 H20A 109.3 . . ?
C21 C20 H20A 109.3 . . ?
N1 C20 H20B 109.3 . . ?
C21 C20 H20B 109.3 . . ?
H20A C20 H20B 108.0 . . ?
N20 C21 C20 106.7(6) . . ?
N20 C21 H21A 110.4 . . ?
C20 C21 H21A 110.4 . . ?
N20 C21 H21B 110.4 . . ?
C20 C21 H21B 110.4 . . ?
H21A C21 H21B 108.6 . . ?
N20 C22 N21 110.7(6) . . ?
N20 C22 C23 129.9(7) . . ?
N21 C22 C23 119.3(7) . . ?
N20 C22 U1 49.7(4) . . ?
N21 C22 U1 61.1(4) . . ?
C23 C22 U1 177.2(5) . . ?
C24 C23 C22 118.5(7) . . ?
C24 C23 H23 120.7 . . ?
C22 C23 H23 120.7 . . ?
C23 C24 C25 121.0(8) . . ?
C23 C24 H24 119.5 . . ?
C25 C24 H24 119.5 . . ?
C26 C25 C24 117.7(8) . . ?
C26 C25 H25 121.2 . . ?
C24 C25 H25 121.2 . . ?
N21 C26 C25 123.3(7) . . ?
N21 C26 H26 118.3 . . ?
C25 C26 H26 118.3 . . ?
N1 C30 C31 111.0(6) . . ?
N1 C30 H30A 109.4 . . ?
C31 C30 H30A 109.4 . . ?
N1 C30 H30B 109.4 . . ?
C31 C30 H30B 109.4 . . ?
H30A C30 H30B 108.0 . . ?
N30 C31 C30 106.0(6) . . ?
N30 C31 H31A 110.5 . . ?
C30 C31 H31A 110.5 . . ?
N30 C31 H31B 110.5 . . ?
C30 C31 H31B 110.5 . . ?
H31A C31 H31B 108.7 . . ?
N30 C32 N31 109.2(6) . . ?
N30 C32 C33 130.2(7) . . ?
N31 C32 C33 120.5(7) . . ?
N30 C32 U1 50.3(3) . . ?
N31 C32 U1 59.8(4) . . ?
C33 C32 U1 170.4(5) . . ?
C34 C33 C32 118.2(7) . . ?
C34 C33 H33 120.9 . . ?
C32 C33 H33 120.9 . . ?
C33 C34 C35 121.4(7) . . ?
C33 C34 H34 119.3 . . ?
C35 C34 H34 119.3 . . ?
C36 C35 C34 117.8(7) . . ?
C36 C35 H35 121.1 . . ?
C34 C35 H35 121.1 . . ?
N31 C36 C35 122.5(7) . . ?
N31 C36 H36 118.7 . . ?
C35 C36 H36 118.7 . . ?
C45 C40 C41 118.4(7) . . ?
C45 C40 N2 122.1(7) . . ?
C41 C40 N2 119.2(7) . . ?
C40 C41 O2 115.9(7) . . ?
C40 C41 C42 120.4(8) . . ?
O2 C41 C42 123.6(7) . . ?
C41 C42 C43 118.6(8) . . ?
C41 C42 H42 120.7 . . ?
C43 C42 H42 120.7 . . ?
C44 C43 C42 121.1(8) . . ?
C44 C43 H43 119.4 . . ?
C42 C43 H43 119.4 . . ?
C45 C44 C43 117.1(8) . . ?
C45 C44 H44 121.5 . . ?
C43 C44 H44 121.5 . . ?
C40 C45 C44 124.2(8) . . ?
C40 C45 H45 117.9 . . ?
C44 C45 H45 117.9 . . ?
O2 C46 H46A 109.5 . . ?
O2 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
O2 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C20 N1 C30 110.8(6) . . ?
C20 N1 C10 110.6(6) . . ?
C30 N1 C10 110.1(6) . . ?
C20 N1 U1 106.5(4) . . ?
C30 N1 U1 107.2(4) . . ?
C10 N1 U1 111.5(4) . . ?
C2 N2 C40 122.2(6) . . ?
C2 N2 U1 121.1(5) . 5_666 ?
C40 N2 U1 116.7(4) . 5_666 ?
C12 N10 C11 122.2(7) . . ?
C12 N10 U1 104.7(5) . . ?
C11 N10 U1 132.6(5) . . ?
C16 N11 C12 118.9(6) . . ?
C16 N11 U1 147.1(5) . . ?
C12 N11 U1 92.9(4) . . ?
C22 N20 C21 121.1(6) . . ?
C22 N20 U1 104.5(5) . . ?
C21 N20 U1 134.2(5) . . ?
C26 N21 C22 120.0(6) . . ?
C26 N21 U1 147.9(5) . . ?
C22 N21 U1 91.5(4) . . ?
C32 N30 C31 121.7(6) . . ?
C32 N30 U1 103.7(4) . . ?
C31 N30 U1 132.3(5) . . ?
C36 N31 C32 119.4(6) . . ?
C36 N31 U1 146.9(4) . . ?
C32 N31 U1 93.0(4) . . ?
C1 O1 U1 124.2(4) . . ?
C41 O2 C46 116.1(6) . . ?
N20 U1 N10 110.6(2) . . ?
N20 U1 N30 90.6(2) . . ?
N10 U1 N30 92.7(2) . . ?
N20 U1 O1 116.25(18) . . ?
N10 U1 O1 117.92(17) . . ?
N30 U1 O1 123.90(18) . . ?
N20 U1 N2 79.9(2) . 5_666 ?
N10 U1 N2 87.7(2) . 5_666 ?
N30 U1 N2 170.1(2) . 5_666 ?
O1 U1 N2 64.02(16) . 5_666 ?
N20 U1 N31 123.42(19) . . ?
N10 U1 N31 112.43(19) . . ?
N30 U1 N31 52.84(19) . . ?
O1 U1 N31 71.71(15) . . ?
N2 U1 N31 135.69(17) 5_666 . ?
N20 U1 N11 152.4(2) . . ?
N10 U1 N11 52.43(19) . . ?
N30 U1 N11 110.1(2) . . ?
O1 U1 N11 67.55(17) . . ?
N2 U1 N11 77.95(19) 5_666 . ?
N31 U1 N11 84.14(18) . . ?
N20 U1 N21 53.1(2) . . ?
N10 U1 N21 161.1(2) . . ?
N30 U1 N21 96.7(2) . . ?
O1 U1 N21 69.50(15) . . ?
N2 U1 N21 80.17(18) 5_666 . ?
N31 U1 N21 86.25(18) . . ?
N11 U1 N21 136.87(18) . . ?
N20 U1 N1 60.1(2) . . ?
N10 U1 N1 61.35(18) . . ?
N30 U1 N1 62.2(2) . . ?
O1 U1 N1 173.64(16) . . ?
N2 U1 N1 109.70(18) 5_666 . ?
N31 U1 N1 114.59(17) . . ?
N11 U1 N1 113.05(19) . . ?
N21 U1 N1 109.19(17) . . ?
N20 U1 C22 25.8(2) . . ?
N10 U1 C22 135.5(2) . . ?
N30 U1 C22 94.8(2) . . ?
O1 U1 C22 93.32(17) . . ?
N2 U1 C22 78.07(19) 5_666 . ?
N31 U1 C22 106.89(19) . . ?
N11 U1 C22 154.20(19) . . ?
N21 U1 C22 27.41(18) . . ?
N1 U1 C22 84.05(19) . . ?
N20 U1 C32 110.2(2) . . ?
N10 U1 C32 100.8(2) . . ?
N30 U1 C32 25.97(19) . . ?
O1 U1 C32 98.88(18) . . ?
N2 U1 C32 162.89(19) 5_666 . ?
N31 U1 C32 27.20(18) . . ?
N11 U1 C32 95.45(19) . . ?
N21 U1 C32 94.75(18) . . ?
N1 U1 C32 87.41(19) . . ?
C22 U1 C32 104.85(19) . . ?
N20 U1 C12 131.9(2) . . ?
N10 U1 C12 25.76(19) . . ?
N30 U1 C12 104.5(2) . . ?
O1 U1 C12 92.67(18) . . ?
N2 U1 C12 79.91(19) 5_666 . ?
N31 U1 C12 101.16(19) . . ?
N11 U1 C12 26.84(18) . . ?
N21 U1 C12 157.69(17) . . ?
N1 U1 C12 87.0(2) . . ?
C22 U1 C12 151.8(2) . . ?
C32 U1 C12 101.39(19) . . ?

_refine_diff_density_max         2.660
_refine_diff_density_min         -0.628
_refine_diff_density_rms         0.181


_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
####################################################################### 
# 
# 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_shelx_CCDC4
_database_code_depnum_ccdc_archive 'CCDC 1510091'
_audit_update_record             
;
2017-01-10 deposited with the CCDC.
2017-08-14 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            'C72 H84 N16 O2 Th2'
_chemical_formula_weight         1669.63

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Th Th -7.2400 8.8979 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

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

_cell_length_a                   27.6164(6)
_cell_length_b                   16.1837(3)
_cell_length_c                   22.0451(5)
_cell_angle_alpha                90
_cell_angle_beta                 127.6900(10)
_cell_angle_gamma                90
_cell_volume                     7796.8(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5832
_cell_measurement_theta_min      1.57
_cell_measurement_theta_max      26.53

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.422
_exptl_crystal_F_000             3296
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_exptl_absorpt_coefficient_mu    3.861
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.665
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_process_details   multi-scan
_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 Quazar'
_diffrn_measurement_method       'omega phi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            34355
_diffrn_reflns_av_unetI/netI     0.0752
_diffrn_reflns_av_R_equivalents  0.0736
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         1.566
_diffrn_reflns_theta_max         26.525
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             8062
_reflns_number_gt                5832
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker ApexIII suite, 2016'
_computing_cell_refinement       'Bruker ApexIII suite, 2016'
_computing_data_reduction        'Bruker ApexIII suite, 2016'
_computing_structure_solution    'direct methods'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Diamond 3D'
_computing_publication_material  WinGX
_refine_special_details          ', SQUEEZE'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0398P)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         8062
_refine_ls_number_parameters     415
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0672
_refine_ls_R_factor_gt           0.0423
_refine_ls_wR_factor_ref         0.0934
_refine_ls_wR_factor_gt          0.0858
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_restrained_S_all      1.005
_refine_ls_shift/su_max          0.003
_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
Th1 Th 0.29467(2) 0.46261(2) 0.85435(2) 0.02190(8) Uani 1 1 d . . . . .
O1 O 0.38354(15) 0.5104(2) 0.8691(2) 0.0244(9) Uani 1 1 d . . . . .
N2 N 0.59794(18) 0.5437(3) 1.0042(2) 0.0207(10) Uani 1 1 d . . . . .
N11 N 0.34513(19) 0.3379(3) 0.8388(3) 0.0258(11) Uani 1 1 d . . . . .
N21 N 0.30220(16) 0.6207(3) 0.8742(2) 0.0195(10) Uani 1 1 d . . . . .
N30 N 0.19554(19) 0.4577(3) 0.7274(3) 0.0248(10) Uani 1 1 d . . . . .
N20 N 0.2547(2) 0.5451(3) 0.9071(3) 0.0261(11) Uani 1 1 d . . . . .
N10 N 0.2898(2) 0.3181(3) 0.8807(3) 0.0316(12) Uani 1 1 d . . . . .
N31 N 0.26929(19) 0.5024(3) 0.7232(3) 0.0238(10) Uani 1 1 d . . . . .
C12 C 0.3149(2) 0.2812(4) 0.8501(3) 0.0279(14) Uani 1 1 d . . . . .
C2 C 0.5489(2) 0.5242(3) 0.9983(3) 0.0216(12) Uani 1 1 d . . . . .
N1 N 0.18707(19) 0.4045(3) 0.8364(3) 0.0291(11) Uani 1 1 d . . . . .
C40 C 0.5887(2) 0.5710(4) 0.9349(3) 0.0231(13) Uani 1 1 d . . . . .
C45 C 0.5940(2) 0.5101(4) 0.8933(3) 0.0269(14) Uani 1 1 d . . . . .
C32 C 0.2085(2) 0.4821(3) 0.6809(3) 0.0247(13) Uani 1 1 d . . . . .
C33 C 0.1707(3) 0.4910(4) 0.6007(3) 0.0270(13) Uani 1 1 d . . . . .
H33 H 0.1285 0.4769 0.5705 0.032 Uiso 1 1 calc R U . . .
C3 C 0.4876(2) 0.5265(3) 0.9297(3) 0.0196(12) Uani 1 1 d . . . . .
H3 H 0.4800 0.5429 0.8831 0.024 Uiso 1 1 calc R U . . .
C44 C 0.5878(2) 0.5367(4) 0.8284(3) 0.0301(14) Uani 1 1 d . . . . .
H44 H 0.5907 0.4972 0.7989 0.036 Uiso 1 1 calc R U . . .
C34 C 0.1953(3) 0.5202(4) 0.5668(3) 0.0293(14) Uani 1 1 d . . . . .
H34 H 0.1697 0.5273 0.5127 0.035 Uiso 1 1 calc R U . . .
C21 C 0.2069(2) 0.5284(4) 0.9156(4) 0.0313(14) Uani 1 1 d . . . . .
H21A H 0.1696 0.5606 0.8775 0.038 Uiso 1 1 calc R U . . .
H21B H 0.2213 0.5443 0.9676 0.038 Uiso 1 1 calc R U . . .
C41 C 0.5765(2) 0.6537(4) 0.9123(3) 0.0267(13) Uani 1 1 d . . . . .
C1 C 0.4391(2) 0.5055(3) 0.9293(3) 0.0214(12) Uani 1 1 d . . . . .
C49 C 0.6017(2) 0.4191(4) 0.9129(3) 0.0295(14) Uani 1 1 d . . . . .
H49 H 0.6215 0.4151 0.9688 0.035 Uiso 1 1 calc R U . . .
C36 C 0.2924(2) 0.5296(3) 0.6891(3) 0.0259(13) Uani 1 1 d . . . . .
H36 H 0.3347 0.5427 0.7195 0.031 Uiso 1 1 calc R U . . .
C31 C 0.1348(2) 0.4326(4) 0.6987(3) 0.0350(15) Uani 1 1 d . . . . .
H31A H 0.1266 0.3753 0.6789 0.042 Uiso 1 1 calc R U . . .
H31B H 0.1038 0.4695 0.6566 0.042 Uiso 1 1 calc R U . . .
C43 C 0.5778(2) 0.6173(4) 0.8063(3) 0.0335(15) Uani 1 1 d . . . . .
H43 H 0.5747 0.6339 0.7627 0.040 Uiso 1 1 calc R U . . .
C26 C 0.3216(3) 0.6941(4) 0.8667(4) 0.0385(16) Uani 1 1 d . . . . .
H26 H 0.3508 0.6934 0.8573 0.046 Uiso 1 1 calc R U . . .
C11 C 0.2474(2) 0.2764(4) 0.8883(3) 0.0376(15) Uani 1 1 d . U . . .
H11A H 0.2613 0.2819 0.9414 0.045 Uiso 1 1 calc R U . . .
H11B H 0.2456 0.2169 0.8767 0.045 Uiso 1 1 calc R U . . .
C16 C 0.3743(2) 0.3136(4) 0.8103(3) 0.0321(14) Uani 1 1 d . . . . .
H16 H 0.3947 0.3543 0.8023 0.039 Uiso 1 1 calc R U . . .
C13 C 0.3120(3) 0.1981(4) 0.8290(3) 0.0359(15) Uani 1 1 d . . . . .
H13 H 0.2891 0.1586 0.8339 0.043 Uiso 1 1 calc R U . . .
C51 C 0.6435(3) 0.3745(4) 0.9002(3) 0.0369(16) Uani 1 1 d . . . . .
H51A H 0.6465 0.3161 0.9139 0.055 Uiso 1 1 calc R U . . .
H51B H 0.6265 0.3790 0.8462 0.055 Uiso 1 1 calc R U . . .
H51C H 0.6842 0.3996 0.9324 0.055 Uiso 1 1 calc R U . . .
C20 C 0.1931(3) 0.4370(4) 0.9029(4) 0.0392(16) Uani 1 1 d . . . . .
H20A H 0.2263 0.4067 0.9494 0.047 Uiso 1 1 calc R U . . .
H20B H 0.1546 0.4264 0.8958 0.047 Uiso 1 1 calc R U . . .
C22 C 0.2661(2) 0.6232(4) 0.8986(3) 0.0294(14) Uani 1 1 d . . . . .
C46 C 0.5650(2) 0.7179(4) 0.9521(3) 0.0310(14) Uani 1 1 d . . . . .
H46 H 0.5792 0.6952 1.0027 0.037 Uiso 1 1 calc R U . . .
C42 C 0.5722(2) 0.6748(4) 0.8480(3) 0.0319(15) Uani 1 1 d . . . . .
H42 H 0.5651 0.7309 0.8321 0.038 Uiso 1 1 calc R U . . .
C35 C 0.2564(3) 0.5394(4) 0.6096(3) 0.0310(14) Uani 1 1 d . . . . .
H35 H 0.2736 0.5587 0.5859 0.037 Uiso 1 1 calc R U . . .
C48 C 0.5992(3) 0.8000(4) 0.9661(4) 0.0411(16) Uani 1 1 d . . . . .
H48A H 0.5902 0.8393 0.9919 0.062 Uiso 1 1 calc R U . . .
H48B H 0.6433 0.7896 0.9983 0.062 Uiso 1 1 calc R U . . .
H48C H 0.5856 0.8232 0.9168 0.062 Uiso 1 1 calc R U . . .
C47 C 0.4958(3) 0.7375(4) 0.9039(4) 0.0405(16) Uani 1 1 d . . . . .
H47A H 0.4892 0.7791 0.9305 0.061 Uiso 1 1 calc R U . . .
H47B H 0.4811 0.7589 0.8536 0.061 Uiso 1 1 calc R U . . .
H47C H 0.4733 0.6870 0.8970 0.061 Uiso 1 1 calc R U . . .
C23 C 0.2460(3) 0.6982(4) 0.9067(4) 0.0382(16) Uani 1 1 d . . . . .
H23 H 0.2199 0.6992 0.9211 0.046 Uiso 1 1 calc R U . . .
C25 C 0.3016(3) 0.7690(4) 0.8718(4) 0.0439(18) Uani 1 1 d . . . . .
H25 H 0.3131 0.8187 0.8607 0.053 Uiso 1 1 calc R U . . .
C14 C 0.3431(3) 0.1757(4) 0.8013(4) 0.0421(16) Uani 1 1 d . . . . .
H14 H 0.3422 0.1197 0.7878 0.051 Uiso 1 1 calc R U . . .
C24 C 0.2639(3) 0.7703(4) 0.8939(4) 0.0459(18) Uani 1 1 d . . . . .
H24 H 0.2506 0.8216 0.9001 0.055 Uiso 1 1 calc R U . . .
C10 C 0.1855(3) 0.3147(5) 0.8335(4) 0.0468(17) Uani 1 1 d . U . . .
H10A H 0.1677 0.2966 0.7808 0.056 Uiso 1 1 calc R U . . .
H10B H 0.1584 0.2945 0.8456 0.056 Uiso 1 1 calc R U . . .
C15 C 0.3761(3) 0.2336(4) 0.7925(4) 0.0432(17) Uani 1 1 d . . . . .
H15 H 0.3987 0.2178 0.7748 0.052 Uiso 1 1 calc R U . . .
C30 C 0.1323(3) 0.4380(4) 0.7650(3) 0.0406(17) Uani 1 1 d . . . . .
H30A H 0.1274 0.4966 0.7732 0.049 Uiso 1 1 calc R U . . .
H30B H 0.0960 0.4073 0.7519 0.049 Uiso 1 1 calc R U . . .
C50 C 0.5404(3) 0.3738(4) 0.8703(4) 0.0509(19) Uani 1 1 d . . . . .
H50A H 0.5477 0.3153 0.8847 0.076 Uiso 1 1 calc R U . . .
H50B H 0.5158 0.3982 0.8840 0.076 Uiso 1 1 calc R U . . .
H50C H 0.5184 0.3789 0.8149 0.076 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
Th1 O1 2.398(3) . ?
Th1 N20 2.433(4) . ?
Th1 N10 2.434(5) . ?
Th1 N30 2.442(4) . ?
Th1 N21 2.582(4) . ?
Th1 N11 2.593(4) . ?
Th1 N31 2.604(4) . ?
Th1 N2 2.687(4) 5_667 ?
Th1 N1 2.904(4) . ?
Th1 C12 3.001(6) . ?
Th1 C32 3.042(6) . ?
Th1 C22 3.045(6) . ?
O1 C1 1.277(6) . ?
N2 C2 1.315(6) . ?
N2 C40 1.456(6) . ?
N2 Th1 2.687(4) 5_667 ?
N11 C16 1.348(6) . ?
N11 C12 1.362(7) . ?
N21 C26 1.354(7) . ?
N21 C22 1.394(6) . ?
N30 C32 1.336(7) . ?
N30 C31 1.443(6) . ?
N20 C22 1.342(7) . ?
N20 C21 1.468(6) . ?
N10 C12 1.366(7) . ?
N10 C11 1.446(7) . ?
N31 C36 1.325(6) . ?
N31 C32 1.372(7) . ?
C12 C13 1.408(8) . ?
C2 C3 1.423(7) . ?
C2 C1 1.499(7) 5_667 ?
N1 C10 1.455(8) . ?
N1 C30 1.465(7) . ?
N1 C20 1.469(7) . ?
C40 C41 1.397(8) . ?
C40 C45 1.413(8) . ?
C45 C44 1.401(8) . ?
C45 C49 1.511(8) . ?
C32 C33 1.407(8) . ?
C33 C34 1.366(8) . ?
C33 H33 0.9500 . ?
C3 C1 1.378(6) . ?
C3 H3 0.9500 . ?
C44 C43 1.361(8) . ?
C44 H44 0.9500 . ?
C34 C35 1.374(8) . ?
C34 H34 0.9500 . ?
C21 C20 1.510(9) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C41 C42 1.389(7) . ?
C41 C46 1.513(8) . ?
C1 C2 1.499(7) 5_667 ?
C49 C51 1.523(7) . ?
C49 C50 1.532(8) . ?
C49 H49 1.0000 . ?
C36 C35 1.398(8) . ?
C36 H36 0.9500 . ?
C31 C30 1.507(8) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C43 C42 1.381(8) . ?
C43 H43 0.9500 . ?
C26 C25 1.365(9) . ?
C26 H26 0.9500 . ?
C11 C10 1.498(8) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C16 C15 1.362(9) . ?
C16 H16 0.9500 . ?
C13 C14 1.372(8) . ?
C13 H13 0.9500 . ?
C51 H51A 0.9800 . ?
C51 H51B 0.9800 . ?
C51 H51C 0.9800 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C22 C23 1.391(8) . ?
C46 C48 1.548(8) . ?
C46 C47 1.549(7) . ?
C46 H46 1.0000 . ?
C42 H42 0.9500 . ?
C35 H35 0.9500 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C23 C24 1.361(9) . ?
C23 H23 0.9500 . ?
C25 C24 1.395(8) . ?
C25 H25 0.9500 . ?
C14 C15 1.402(9) . ?
C14 H14 0.9500 . ?
C24 H24 0.9500 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C15 H15 0.9500 . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C50 H50A 0.9800 . ?
C50 H50B 0.9800 . ?
C50 H50C 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
O1 Th1 N20 118.94(14) . . ?
O1 Th1 N10 118.60(14) . . ?
N20 Th1 N10 107.81(15) . . ?
O1 Th1 N30 120.22(13) . . ?
N20 Th1 N30 92.71(15) . . ?
N10 Th1 N30 93.16(16) . . ?
O1 Th1 N21 71.83(12) . . ?
N20 Th1 N21 52.30(13) . . ?
N10 Th1 N21 157.26(15) . . ?
N30 Th1 N21 98.30(14) . . ?
O1 Th1 N11 71.36(13) . . ?
N20 Th1 N11 158.14(15) . . ?
N10 Th1 N11 52.83(14) . . ?
N30 Th1 N11 98.03(14) . . ?
N21 Th1 N11 143.11(12) . . ?
O1 Th1 N31 68.26(12) . . ?
N20 Th1 N31 120.11(15) . . ?
N10 Th1 N31 119.07(15) . . ?
N30 Th1 N31 51.97(13) . . ?
N21 Th1 N31 83.24(14) . . ?
N11 Th1 N31 81.22(14) . . ?
O1 Th1 N2 62.78(12) . 5_667 ?
N20 Th1 N2 88.16(14) . 5_667 ?
N10 Th1 N2 82.50(15) . 5_667 ?
N30 Th1 N2 175.63(14) . 5_667 ?
N21 Th1 N2 85.62(13) . 5_667 ?
N11 Th1 N2 79.77(13) . 5_667 ?
N31 Th1 N2 130.86(12) . 5_667 ?
O1 Th1 N1 179.90(14) . . ?
N20 Th1 N1 61.15(14) . . ?
N10 Th1 N1 61.32(14) . . ?
N30 Th1 N1 59.76(13) . . ?
N21 Th1 N1 108.27(12) . . ?
N11 Th1 N1 108.54(14) . . ?
N31 Th1 N1 111.73(13) . . ?
N2 Th1 N1 117.23(12) 5_667 . ?
O1 Th1 C12 97.15(14) . . ?
N20 Th1 C12 134.38(15) . . ?
N10 Th1 C12 26.58(14) . . ?
N30 Th1 C12 91.84(15) . . ?
N21 Th1 C12 167.76(13) . . ?
N11 Th1 C12 26.92(13) . . ?
N31 Th1 C12 97.82(15) . . ?
N2 Th1 C12 84.51(14) 5_667 . ?
N1 Th1 C12 82.75(14) . . ?
O1 Th1 C32 94.96(13) . . ?
N20 Th1 C32 108.01(15) . . ?
N10 Th1 C32 106.52(16) . . ?
N30 Th1 C32 25.28(13) . . ?
N21 Th1 C32 91.77(14) . . ?
N11 Th1 C32 89.13(14) . . ?
N31 Th1 C32 26.71(13) . . ?
N2 Th1 C32 157.29(13) 5_667 . ?
N1 Th1 C32 85.02(13) . . ?
C12 Th1 C32 94.55(15) . . ?
O1 Th1 C22 97.24(14) . . ?
N20 Th1 C22 25.36(14) . . ?
N10 Th1 C22 132.91(15) . . ?
N30 Th1 C22 93.80(15) . . ?
N21 Th1 C22 27.12(13) . . ?
N11 Th1 C22 166.61(14) . . ?
N31 Th1 C22 101.43(15) . . ?
N2 Th1 C22 88.82(14) 5_667 . ?
N1 Th1 C22 82.86(14) . . ?
C12 Th1 C22 159.20(15) . . ?
C32 Th1 C22 99.08(15) . . ?
C1 O1 Th1 126.9(3) . . ?
C2 N2 C40 117.3(4) . . ?
C2 N2 Th1 116.5(3) . 5_667 ?
C40 N2 Th1 126.2(3) . 5_667 ?
C16 N11 C12 119.8(5) . . ?
C16 N11 Th1 144.3(4) . . ?
C12 N11 Th1 93.5(3) . . ?
C26 N21 C22 116.8(5) . . ?
C26 N21 Th1 147.7(4) . . ?
C22 N21 Th1 95.3(3) . . ?
C32 N30 C31 122.1(5) . . ?
C32 N30 Th1 103.4(3) . . ?
C31 N30 Th1 134.4(3) . . ?
C22 N20 C21 119.7(5) . . ?
C22 N20 Th1 103.7(3) . . ?
C21 N20 Th1 131.8(4) . . ?
C12 N10 C11 123.0(5) . . ?
C12 N10 Th1 100.6(3) . . ?
C11 N10 Th1 130.0(4) . . ?
C36 N31 C32 120.5(5) . . ?
C36 N31 Th1 144.7(4) . . ?
C32 N31 Th1 94.7(3) . . ?
N11 C12 N10 110.4(5) . . ?
N11 C12 C13 120.1(5) . . ?
N10 C12 C13 129.4(5) . . ?
N11 C12 Th1 59.6(3) . . ?
N10 C12 Th1 52.9(3) . . ?
C13 C12 Th1 165.9(4) . . ?
N2 C2 C3 125.7(5) . . ?
N2 C2 C1 115.3(5) . 5_667 ?
C3 C2 C1 119.0(4) . 5_667 ?
C10 N1 C30 109.8(5) . . ?
C10 N1 C20 112.5(5) . . ?
C30 N1 C20 110.7(5) . . ?
C10 N1 Th1 109.3(3) . . ?
C30 N1 Th1 108.9(3) . . ?
C20 N1 Th1 105.4(3) . . ?
C41 C40 C45 122.4(5) . . ?
C41 C40 N2 121.0(5) . . ?
C45 C40 N2 116.7(5) . . ?
C44 C45 C40 116.8(6) . . ?
C44 C45 C49 119.9(6) . . ?
C40 C45 C49 123.2(5) . . ?
N30 C32 N31 109.8(5) . . ?
N30 C32 C33 130.8(5) . . ?
N31 C32 C33 119.3(5) . . ?
N30 C32 Th1 51.3(3) . . ?
N31 C32 Th1 58.6(3) . . ?
C33 C32 Th1 177.7(4) . . ?
C34 C33 C32 119.2(5) . . ?
C34 C33 H33 120.4 . . ?
C32 C33 H33 120.4 . . ?
C1 C3 C2 121.4(5) . . ?
C1 C3 H3 119.3 . . ?
C2 C3 H3 119.3 . . ?
C43 C44 C45 122.1(6) . . ?
C43 C44 H44 118.9 . . ?
C45 C44 H44 118.9 . . ?
C33 C34 C35 121.0(6) . . ?
C33 C34 H34 119.5 . . ?
C35 C34 H34 119.5 . . ?
N20 C21 C20 107.5(4) . . ?
N20 C21 H21A 110.2 . . ?
C20 C21 H21A 110.2 . . ?
N20 C21 H21B 110.2 . . ?
C20 C21 H21B 110.2 . . ?
H21A C21 H21B 108.5 . . ?
C42 C41 C40 116.8(5) . . ?
C42 C41 C46 120.4(5) . . ?
C40 C41 C46 122.7(5) . . ?
O1 C1 C3 122.5(5) . . ?
O1 C1 C2 118.0(4) . 5_667 ?
C3 C1 C2 119.5(5) . 5_667 ?
C45 C49 C51 113.6(5) . . ?
C45 C49 C50 112.4(5) . . ?
C51 C49 C50 109.7(5) . . ?
C45 C49 H49 106.9 . . ?
C51 C49 H49 106.9 . . ?
C50 C49 H49 106.9 . . ?
N31 C36 C35 121.9(5) . . ?
N31 C36 H36 119.0 . . ?
C35 C36 H36 119.0 . . ?
N30 C31 C30 106.7(5) . . ?
N30 C31 H31A 110.4 . . ?
C30 C31 H31A 110.4 . . ?
N30 C31 H31B 110.4 . . ?
C30 C31 H31B 110.4 . . ?
H31A C31 H31B 108.6 . . ?
C44 C43 C42 119.3(5) . . ?
C44 C43 H43 120.4 . . ?
C42 C43 H43 120.4 . . ?
N21 C26 C25 124.1(6) . . ?
N21 C26 H26 118.0 . . ?
C25 C26 H26 118.0 . . ?
N10 C11 C10 108.7(5) . . ?
N10 C11 H11A 109.9 . . ?
C10 C11 H11A 109.9 . . ?
N10 C11 H11B 109.9 . . ?
C10 C11 H11B 109.9 . . ?
H11A C11 H11B 108.3 . . ?
N11 C16 C15 123.2(6) . . ?
N11 C16 H16 118.4 . . ?
C15 C16 H16 118.4 . . ?
C14 C13 C12 118.2(6) . . ?
C14 C13 H13 120.9 . . ?
C12 C13 H13 120.9 . . ?
C49 C51 H51A 109.5 . . ?
C49 C51 H51B 109.5 . . ?
H51A C51 H51B 109.5 . . ?
C49 C51 H51C 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
N1 C20 C21 113.4(5) . . ?
N1 C20 H20A 108.9 . . ?
C21 C20 H20A 108.9 . . ?
N1 C20 H20B 108.9 . . ?
C21 C20 H20B 108.9 . . ?
H20A C20 H20B 107.7 . . ?
N20 C22 C23 131.3(5) . . ?
N20 C22 N21 108.0(5) . . ?
C23 C22 N21 120.6(5) . . ?
N20 C22 Th1 50.9(3) . . ?
C23 C22 Th1 171.1(4) . . ?
N21 C22 Th1 57.6(3) . . ?
C41 C46 C48 112.7(5) . . ?
C41 C46 C47 110.6(5) . . ?
C48 C46 C47 107.8(5) . . ?
C41 C46 H46 108.5 . . ?
C48 C46 H46 108.5 . . ?
C47 C46 H46 108.5 . . ?
C43 C42 C41 122.6(6) . . ?
C43 C42 H42 118.7 . . ?
C41 C42 H42 118.7 . . ?
C34 C35 C36 118.0(5) . . ?
C34 C35 H35 121.0 . . ?
C36 C35 H35 121.0 . . ?
C46 C48 H48A 109.5 . . ?
C46 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C46 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C46 C47 H47A 109.5 . . ?
C46 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
C46 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C24 C23 C22 120.0(6) . . ?
C24 C23 H23 120.0 . . ?
C22 C23 H23 120.0 . . ?
C26 C25 C24 117.9(6) . . ?
C26 C25 H25 121.0 . . ?
C24 C25 H25 121.0 . . ?
C13 C14 C15 121.5(6) . . ?
C13 C14 H14 119.3 . . ?
C15 C14 H14 119.3 . . ?
C23 C24 C25 120.1(6) . . ?
C23 C24 H24 119.9 . . ?
C25 C24 H24 119.9 . . ?
N1 C10 C11 112.9(5) . . ?
N1 C10 H10A 109.0 . . ?
C11 C10 H10A 109.0 . . ?
N1 C10 H10B 109.0 . . ?
C11 C10 H10B 109.0 . . ?
H10A C10 H10B 107.8 . . ?
C16 C15 C14 117.0(6) . . ?
C16 C15 H15 121.5 . . ?
C14 C15 H15 121.5 . . ?
N1 C30 C31 113.1(5) . . ?
N1 C30 H30A 109.0 . . ?
C31 C30 H30A 109.0 . . ?
N1 C30 H30B 109.0 . . ?
C31 C30 H30B 109.0 . . ?
H30A C30 H30B 107.8 . . ?
C49 C50 H50A 109.5 . . ?
C49 C50 H50B 109.5 . . ?
H50A C50 H50B 109.5 . . ?
C49 C50 H50C 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?

_refine_diff_density_max         1.888
_refine_diff_density_min         -0.905
_refine_diff_density_rms         0.146



_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
####################################################################### 
# 
# 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_shelx_CCDC5
_database_code_depnum_ccdc_archive 'CCDC 1526526'
_audit_update_record             
;
2017-01-10 deposited with the CCDC.
2017-08-14 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            'C78 H90 N16 O8 Th2'
_chemical_formula_weight         1843.73

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Th Th -7.2400 8.8979 '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                   15.2776(14)
_cell_length_b                   13.5330(15)
_cell_length_c                   18.3130(14)
_cell_angle_alpha                90
_cell_angle_beta                 90.453(5)
_cell_angle_gamma                90
_cell_volume                     3786.1(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5909
_cell_measurement_theta_min      1.73
_cell_measurement_theta_max      25.40

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.617
_exptl_crystal_F_000             1828
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_exptl_absorpt_coefficient_mu    3.990
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.675
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_process_details   'Blessing, 1995'
_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 Quazar'
_diffrn_measurement_method       'omega phi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            125549
_diffrn_reflns_av_unetI/netI     0.0254
_diffrn_reflns_av_R_equivalents  0.0558
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.729
_diffrn_reflns_theta_max         25.397
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             6960
_reflns_number_gt                5909
_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 ApexIII suite, 2016'
_computing_cell_refinement       'Bruker ApexIII suite, 2016'
_computing_data_reduction        'Bruker ApexIII suite, 2016'
_computing_structure_solution    ShelXT
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Diamond 3D'
_computing_publication_material  WinGX
_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)+(0.0429P)²+17.2598P] 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         6960
_refine_ls_number_parameters     465
_refine_ls_number_restraints     34
_refine_ls_R_factor_all          0.0476
_refine_ls_R_factor_gt           0.0379
_refine_ls_wR_factor_ref         0.0918
_refine_ls_wR_factor_gt          0.0870
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_restrained_S_all      1.073
_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
Th1 Th 0.74832(2) 0.32207(2) 0.47174(2) 0.02516(8) Uani 1 1 d . . . . .
O1 O 0.6624(2) 0.4641(3) 0.44505(19) 0.0303(8) Uani 1 1 d . . . . .
N2 N 0.5989(3) 0.3434(3) 0.5448(2) 0.0252(10) Uani 1 1 d . . . . .
N21 N 0.7619(3) 0.4376(3) 0.5889(2) 0.0256(9) Uani 1 1 d . . . . .
O100 O 0.7744(4) 0.3298(5) 0.3274(3) 0.0836(13) Uani 1 1 d . . . . .
N1 N 0.8517(3) 0.1469(4) 0.5074(3) 0.0423(13) Uani 1 1 d . . . . .
N31 N 0.8482(3) 0.4686(4) 0.4295(2) 0.0311(10) Uani 1 1 d . . . . .
N30 N 0.9074(3) 0.3229(4) 0.4546(3) 0.0353(11) Uani 1 1 d . . . . .
N11 N 0.6072(3) 0.2702(4) 0.3877(2) 0.0364(12) Uani 1 1 d . . . . .
N10 N 0.7076(3) 0.1594(4) 0.4218(3) 0.0426(13) Uani 1 1 d . . . . .
C32 C 0.9233(4) 0.4147(5) 0.4315(3) 0.0341(13) Uani 1 1 d . . . . .
C2 C 0.5481(3) 0.4164(4) 0.5266(3) 0.0252(11) Uani 1 1 d . . . . .
C26 C 0.7574(4) 0.5287(4) 0.6149(3) 0.0345(13) Uani 1 1 d . . . . .
H26 H 0.7460 0.5813 0.5818 0.041 Uiso 1 1 calc R U . . .
C40 C 0.5745(3) 0.2795(5) 0.6035(3) 0.0326(13) Uani 1 1 d . . . . .
C22 C 0.7767(3) 0.3609(4) 0.6357(3) 0.0276(12) Uani 1 1 d . . . . .
N20 N 0.7760(3) 0.2771(4) 0.5974(3) 0.0337(11) Uani 1 1 d . U . . .
C23 C 0.7884(3) 0.3773(5) 0.7107(3) 0.0349(13) Uani 1 1 d . . . . .
H23 H 0.7982 0.3239 0.7434 0.042 Uiso 1 1 calc R U . . .
C45 C 0.5665(4) 0.3147(5) 0.6750(3) 0.0389(15) Uani 1 1 d . . . . .
C33 C 1.0030(4) 0.4592(5) 0.4101(3) 0.0420(15) Uani 1 1 d . . . . .
H33 H 1.0560 0.4226 0.4105 0.050 Uiso 1 1 calc R U . . .
C3 C 0.4638(3) 0.4373(4) 0.5548(3) 0.0279(12) Uani 1 1 d . . . . .
H3 H 0.4405 0.3955 0.5915 0.033 Uiso 1 1 calc R U . . .
C36 C 0.8496(4) 0.5615(5) 0.4085(3) 0.0384(14) Uani 1 1 d . . . . .
H36 H 0.7963 0.5976 0.4080 0.046 Uiso 1 1 calc R U . . .
C12 C 0.6350(4) 0.1753(5) 0.3814(3) 0.0397(15) Uani 1 1 d . . . . .
C24 C 0.7853(4) 0.4731(5) 0.7353(3) 0.0407(15) Uani 1 1 d . . . . .
H24 H 0.7947 0.4865 0.7857 0.049 Uiso 1 1 calc R U . . .
C21 C 0.8024(4) 0.1835(4) 0.6339(3) 0.0388(14) Uani 1 1 d . U . . .
H21A H 0.7573 0.1630 0.6693 0.047 Uiso 1 1 calc R U . . .
H21B H 0.8585 0.1926 0.6604 0.047 Uiso 1 1 calc R U . . .
C1 C 0.5849(3) 0.4840(4) 0.4693(3) 0.0276(12) Uani 1 1 d . . . . .
C41 C 0.5675(4) 0.1790(5) 0.5900(5) 0.0470(18) Uani 1 1 d D . . . .
C30 C 0.9436(4) 0.1756(5) 0.5213(4) 0.0491(17) Uani 1 1 d . . . . .
H30A H 0.9813 0.1161 0.5199 0.059 Uiso 1 1 calc R U . . .
H30B H 0.9489 0.2052 0.5706 0.059 Uiso 1 1 calc R U . . .
C20 C 0.8121(4) 0.1061(5) 0.5747(4) 0.0488(17) Uani 1 1 d . . . . .
H20A H 0.8492 0.0515 0.5934 0.059 Uiso 1 1 calc R U . . .
H20B H 0.7538 0.0784 0.5627 0.059 Uiso 1 1 calc R U . . .
C34 C 1.0020(4) 0.5547(6) 0.3891(3) 0.0494(18) Uani 1 1 d . . . . .
H34 H 1.0551 0.5857 0.3753 0.059 Uiso 1 1 calc R U . . .
C25 C 0.7685(4) 0.5504(5) 0.6875(3) 0.0417(15) Uani 1 1 d . . . . .
H25 H 0.7649 0.6166 0.7046 0.050 Uiso 1 1 calc R U . . .
C13 C 0.5888(5) 0.1087(6) 0.3349(4) 0.0536(19) Uani 1 1 d . . . . .
H13 H 0.6076 0.0421 0.3298 0.064 Uiso 1 1 calc R U . . .
C44 C 0.5496(4) 0.2437(7) 0.7303(4) 0.057(2) Uani 1 1 d . . . . .
H44 H 0.5439 0.2647 0.7795 0.068 Uiso 1 1 calc R U . . .
C35 C 0.9249(4) 0.6084(6) 0.3872(3) 0.0497(17) Uani 1 1 d . . . . .
H35 H 0.9241 0.6754 0.3716 0.060 Uiso 1 1 calc R U . . .
C14 C 0.5165(5) 0.1429(7) 0.2977(4) 0.064(2) Uani 1 1 d . . . . .
H14 H 0.4847 0.0994 0.2666 0.076 Uiso 1 1 calc R U . . .
C31 C 0.9751(4) 0.2505(5) 0.4639(4) 0.0483(17) Uani 1 1 d . . . . .
H31A H 1.0299 0.2825 0.4806 0.058 Uiso 1 1 calc R U . . .
H31B H 0.9864 0.2166 0.4170 0.058 Uiso 1 1 calc R U . . .
C16 C 0.5372(5) 0.3012(6) 0.3512(4) 0.0522(19) Uani 1 1 d . . . . .
H16 H 0.5187 0.3678 0.3567 0.063 Uiso 1 1 calc R U . . .
C42 C 0.5505(4) 0.1134(6) 0.6456(5) 0.060(2) Uani 1 1 d D . . . .
H42 H 0.5454 0.0450 0.6351 0.072 Uiso 1 1 calc R U . . .
C10 C 0.8450(5) 0.0769(5) 0.4473(5) 0.062(2) Uani 1 1 d . . . . .
H10A H 0.8700 0.0127 0.4628 0.074 Uiso 1 1 calc R U . . .
H10B H 0.8795 0.1015 0.4056 0.074 Uiso 1 1 calc R U . . .
C43 C 0.5413(4) 0.1446(7) 0.7136(5) 0.066(2) Uani 1 1 d . . . . .
H43 H 0.5288 0.0985 0.7512 0.079 Uiso 1 1 calc R U . . .
C11 C 0.7507(5) 0.0619(5) 0.4231(5) 0.072(2) Uani 1 1 d . U . . .
H11A H 0.7486 0.0317 0.3739 0.086 Uiso 1 1 calc R U . . .
H11B H 0.7203 0.0174 0.4576 0.086 Uiso 1 1 calc R U . . .
C100 C 0.7328(6) 0.3991(8) 0.2795(4) 0.0836(13) Uani 1 1 d . . . . .
H10C H 0.7722 0.4550 0.2680 0.100 Uiso 1 1 calc R U . . .
H10D H 0.6782 0.4252 0.3010 0.100 Uiso 1 1 calc R U . . .
C101 C 0.7135(6) 0.3364(7) 0.2114(4) 0.0836(13) Uani 1 1 d . . . . .
H10E H 0.6606 0.2953 0.2180 0.100 Uiso 1 1 calc R U . . .
H10F H 0.7057 0.3784 0.1675 0.100 Uiso 1 1 calc R U . . .
C15 C 0.4898(5) 0.2386(7) 0.3048(4) 0.069(2) Uani 1 1 d . . . . .
H15 H 0.4400 0.2622 0.2788 0.082 Uiso 1 1 calc R U . . .
C103 C 0.8153(6) 0.2516(8) 0.2839(4) 0.0836(13) Uani 1 1 d . . . . .
H10G H 0.7919 0.1861 0.2979 0.100 Uiso 1 1 calc R U . . .
H10H H 0.8795 0.2513 0.2918 0.100 Uiso 1 1 calc R U . . .
C102 C 0.7940(6) 0.2736(8) 0.2057(4) 0.0836(13) Uani 1 1 d . . . . .
H10I H 0.7820 0.2123 0.1779 0.100 Uiso 1 1 calc R U . . .
H10J H 0.8423 0.3101 0.1820 0.100 Uiso 1 1 calc R U . . .
O2 O 0.5744(3) 0.4071(4) 0.6848(2) 0.0300(14) Uani 0.754(8) 1 d D . P A 1
C46 C 0.5602(6) 0.4436(7) 0.7566(4) 0.044(2) Uani 0.754(8) 1 d D . P A 1
H46A H 0.6013 0.4117 0.7906 0.053 Uiso 0.754(8) 1 calc R U P A 1
H46B H 0.5001 0.4290 0.7713 0.053 Uiso 0.754(8) 1 calc R U P A 1
H46C H 0.5697 0.5152 0.7574 0.053 Uiso 0.754(8) 1 calc R U P A 1
O2A O 0.5702(11) 0.1467(11) 0.5273(8) 0.035(4) Uani 0.246(8) 1 d D . P A 2
C46A C 0.559(2) 0.0479(16) 0.5171(12) 0.072(10) Uani 0.246(8) 1 d D U P A 2
H46D H 0.5630 0.0327 0.4649 0.086 Uiso 0.246(8) 1 calc R U P A 2
H46E H 0.6053 0.0120 0.5437 0.086 Uiso 0.246(8) 1 calc R U P A 2
H46F H 0.5019 0.0279 0.5354 0.086 Uiso 0.246(8) 1 calc R U P A 2
C200 C 0.6863(6) -0.1140(9) 0.5912(5) 0.086(3) Uani 1 1 d . . . . .
C201 C 0.7617(11) -0.1737(7) 0.5827(6) 0.115(5) Uani 1 1 d . . . . .
H20C H 0.7595 -0.2307 0.6166 0.138 Uiso 1 1 calc R U . . .
H20D H 0.8150 -0.1349 0.5940 0.138 Uiso 1 1 calc R U . . .
C202 C 0.7637(7) -0.2082(8) 0.5074(6) 0.086(3) Uani 1 1 d . . . . .
H20E H 0.7951 -0.2719 0.5030 0.103 Uiso 1 1 calc R U . . .
H20F H 0.7906 -0.1589 0.4746 0.103 Uiso 1 1 calc R U . . .
C203 C 0.6685(8) -0.2194(9) 0.4929(6) 0.098(3) Uani 1 1 d . . . . .
H20G H 0.6547 -0.2036 0.4413 0.118 Uiso 1 1 calc R U . . .
H20H H 0.6496 -0.2879 0.5031 0.118 Uiso 1 1 calc R U . . .
O200 O 0.6258(12) -0.1519(13) 0.5405(10) 0.257(7) Uani 1 1 d . 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
Th1 O1 2.376(4) . ?
Th1 N20 2.415(5) . ?
Th1 N30 2.453(4) . ?
Th1 N10 2.462(5) . ?
Th1 N31 2.623(5) . ?
Th1 N21 2.661(4) . ?
Th1 N2 2.671(4) . ?
Th1 O100 2.678(5) . ?
Th1 N11 2.731(4) . ?
Th1 N1 2.920(5) . ?
Th1 C32 3.049(6) . ?
Th1 C22 3.075(5) . ?
O1 C1 1.296(6) . ?
N2 C2 1.299(7) . ?
N2 C40 1.432(7) . ?
N21 C26 1.324(7) . ?
N21 C22 1.363(7) . ?
O100 C100 1.430(12) . ?
O100 C103 1.468(11) . ?
N1 C10 1.456(9) . ?
N1 C30 1.477(8) . ?
N1 C20 1.484(9) . ?
N31 C36 1.314(8) . ?
N31 C32 1.361(7) . ?
N30 C32 1.334(8) . ?
N30 C31 1.435(8) . ?
N11 C16 1.325(8) . ?
N11 C12 1.357(8) . ?
N10 C12 1.346(8) . ?
N10 C11 1.474(9) . ?
C32 C33 1.416(8) . ?
C2 C3 1.420(7) . ?
C2 C1 1.504(7) . ?
C26 C25 1.371(8) . ?
C26 H26 0.9500 . ?
C40 C41 1.387(9) . ?
C40 C45 1.400(9) . ?
C22 N20 1.333(7) . ?
C22 C23 1.401(8) . ?
N20 C21 1.486(8) . ?
C23 C24 1.373(9) . ?
C23 H23 0.9500 . ?
C45 O2 1.269(8) . ?
C45 C44 1.420(9) . ?
C33 C34 1.349(10) . ?
C33 H33 0.9500 . ?
C3 C1 1.370(7) 3_666 ?
C3 H3 0.9500 . ?
C36 C35 1.373(8) . ?
C36 H36 0.9500 . ?
C12 C13 1.423(8) . ?
C24 C25 1.388(9) . ?
C24 H24 0.9500 . ?
C21 C20 1.516(9) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C1 C3 1.370(7) 3_666 ?
C41 O2A 1.230(13) . ?
C41 C42 1.378(9) . ?
C30 C31 1.539(10) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C34 C35 1.384(10) . ?
C34 H34 0.9500 . ?
C25 H25 0.9500 . ?
C13 C14 1.374(11) . ?
C13 H13 0.9500 . ?
C44 C43 1.381(12) . ?
C44 H44 0.9500 . ?
C35 H35 0.9500 . ?
C14 C15 1.365(12) . ?
C14 H14 0.9500 . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C16 C15 1.397(9) . ?
C16 H16 0.9500 . ?
C42 C43 1.323(12) . ?
C42 H42 0.9500 . ?
C10 C11 1.517(10) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C43 H43 0.9500 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C100 C101 1.536(10) . ?
C100 H10C 0.9900 . ?
C100 H10D 0.9900 . ?
C101 C102 1.499(14) . ?
C101 H10E 0.9900 . ?
C101 H10F 0.9900 . ?
C15 H15 0.9500 . ?
C103 C102 1.497(11) . ?
C103 H10G 0.9900 . ?
C103 H10H 0.9900 . ?
C102 H10I 0.9900 . ?
C102 H10J 0.9900 . ?
O2 C46 1.422(8) . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
O2A C46A 1.359(17) . ?
C46A H46D 0.9800 . ?
C46A H46E 0.9800 . ?
C46A H46F 0.9800 . ?
C200 O200 1.402(18) . ?
C200 C201 1.417(16) . ?
C201 C202 1.457(15) . ?
C201 H20C 0.9900 . ?
C201 H20D 0.9900 . ?
C202 C203 1.483(14) . ?
C202 H20E 0.9900 . ?
C202 H20F 0.9900 . ?
C203 O200 1.423(18) . ?
C203 H20G 0.9900 . ?
C203 H20H 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Th1 N20 119.48(14) . . ?
O1 Th1 N30 121.07(14) . . ?
N20 Th1 N30 87.54(16) . . ?
O1 Th1 N10 120.63(16) . . ?
N20 Th1 N10 99.82(18) . . ?
N30 Th1 N10 101.79(16) . . ?
O1 Th1 N31 69.48(13) . . ?
N20 Th1 N31 111.95(15) . . ?
N30 Th1 N31 51.63(15) . . ?
N10 Th1 N31 135.43(16) . . ?
O1 Th1 N21 74.35(12) . . ?
N20 Th1 N21 50.77(15) . . ?
N30 Th1 N21 91.68(14) . . ?
N10 Th1 N21 147.40(16) . . ?
N31 Th1 N21 75.64(13) . . ?
O1 Th1 N2 62.78(12) . . ?
N20 Th1 N2 72.16(14) . . ?
N30 Th1 N2 156.24(16) . . ?
N10 Th1 N2 93.92(15) . . ?
N31 Th1 N2 124.58(14) . . ?
N21 Th1 N2 66.06(13) . . ?
O1 Th1 O100 81.47(18) . . ?
N20 Th1 O100 157.6(2) . . ?
N30 Th1 O100 73.63(18) . . ?
N10 Th1 O100 73.00(18) . . ?
N31 Th1 O100 65.65(15) . . ?
N21 Th1 O100 139.59(15) . . ?
N2 Th1 O100 128.65(17) . . ?
O1 Th1 N11 70.11(15) . . ?
N20 Th1 N11 127.14(15) . . ?
N30 Th1 N11 135.05(15) . . ?
N10 Th1 N11 50.56(17) . . ?
N31 Th1 N11 119.13(14) . . ?
N21 Th1 N11 131.42(14) . . ?
N2 Th1 N11 68.65(13) . . ?
O100 Th1 N11 64.97(16) . . ?
O1 Th1 N1 178.75(13) . . ?
N20 Th1 N1 59.45(16) . . ?
N30 Th1 N1 59.84(16) . . ?
N10 Th1 N1 59.46(16) . . ?
N31 Th1 N1 111.39(14) . . ?
N21 Th1 N1 104.92(14) . . ?
N2 Th1 N1 116.03(14) . . ?
O100 Th1 N1 99.7(2) . . ?
N11 Th1 N1 109.93(15) . . ?
O1 Th1 C32 95.85(14) . . ?
N20 Th1 C32 100.75(15) . . ?
N30 Th1 C32 25.22(16) . . ?
N10 Th1 C32 119.82(16) . . ?
N31 Th1 C32 26.42(15) . . ?
N21 Th1 C32 83.70(14) . . ?
N2 Th1 C32 146.24(15) . . ?
O100 Th1 C32 66.91(15) . . ?
N11 Th1 C32 131.28(14) . . ?
N1 Th1 C32 85.04(16) . . ?
O1 Th1 C22 97.82(13) . . ?
N20 Th1 C22 24.53(16) . . ?
N30 Th1 C22 89.53(15) . . ?
N10 Th1 C22 123.28(17) . . ?
N31 Th1 C22 94.64(14) . . ?
N21 Th1 C22 26.24(14) . . ?
N2 Th1 C22 66.86(13) . . ?
O100 Th1 C22 159.36(15) . . ?
N11 Th1 C22 134.33(13) . . ?
N1 Th1 C22 81.27(15) . . ?
C32 Th1 C22 92.77(14) . . ?
C1 O1 Th1 127.0(3) . . ?
C2 N2 C40 119.6(4) . . ?
C2 N2 Th1 117.7(3) . . ?
C40 N2 Th1 122.7(3) . . ?
C26 N21 C22 119.4(5) . . ?
C26 N21 Th1 146.4(4) . . ?
C22 N21 Th1 94.1(3) . . ?
C100 O100 C103 109.2(6) . . ?
C100 O100 Th1 124.2(5) . . ?
C103 O100 Th1 125.1(5) . . ?
C10 N1 C30 111.3(5) . . ?
C10 N1 C20 111.0(6) . . ?
C30 N1 C20 110.4(5) . . ?
C10 N1 Th1 108.9(4) . . ?
C30 N1 Th1 109.7(4) . . ?
C20 N1 Th1 105.3(3) . . ?
C36 N31 C32 120.4(5) . . ?
C36 N31 Th1 145.1(4) . . ?
C32 N31 Th1 94.5(3) . . ?
C32 N30 C31 122.7(5) . . ?
C32 N30 Th1 103.2(3) . . ?
C31 N30 Th1 134.1(4) . . ?
C16 N11 C12 120.6(5) . . ?
C16 N11 Th1 146.5(5) . . ?
C12 N11 Th1 92.6(3) . . ?
C12 N10 C11 121.2(5) . . ?
C12 N10 Th1 105.4(4) . . ?
C11 N10 Th1 133.0(4) . . ?
N30 C32 N31 110.6(5) . . ?
N30 C32 C33 130.1(6) . . ?
N31 C32 C33 119.3(6) . . ?
N30 C32 Th1 51.5(3) . . ?
N31 C32 Th1 59.1(3) . . ?
C33 C32 Th1 177.6(4) . . ?
N2 C2 C3 126.8(5) . . ?
N2 C2 C1 114.6(4) . . ?
C3 C2 C1 118.6(5) . . ?
N21 C26 C25 122.9(6) . . ?
N21 C26 H26 118.6 . . ?
C25 C26 H26 118.6 . . ?
C41 C40 C45 119.6(6) . . ?
C41 C40 N2 118.6(6) . . ?
C45 C40 N2 121.5(6) . . ?
N20 C22 N21 108.5(5) . . ?
N20 C22 C23 130.6(6) . . ?
N21 C22 C23 121.0(5) . . ?
N20 C22 Th1 48.8(3) . . ?
N21 C22 Th1 59.7(3) . . ?
C23 C22 Th1 178.9(4) . . ?
C22 N20 C21 119.2(5) . . ?
C22 N20 Th1 106.7(4) . . ?
C21 N20 Th1 133.5(4) . . ?
C24 C23 C22 117.9(6) . . ?
C24 C23 H23 121.1 . . ?
C22 C23 H23 121.1 . . ?
O2 C45 C40 117.3(5) . . ?
O2 C45 C44 125.7(6) . . ?
C40 C45 C44 117.0(7) . . ?
C34 C33 C32 118.7(6) . . ?
C34 C33 H33 120.7 . . ?
C32 C33 H33 120.7 . . ?
C1 C3 C2 121.9(5) 3_666 . ?
C1 C3 H3 119.0 3_666 . ?
C2 C3 H3 119.0 . . ?
N31 C36 C35 122.8(6) . . ?
N31 C36 H36 118.6 . . ?
C35 C36 H36 118.6 . . ?
N10 C12 N11 111.2(5) . . ?
N10 C12 C13 129.0(7) . . ?
N11 C12 C13 119.7(6) . . ?
N10 C12 Th1 49.9(3) . . ?
N11 C12 Th1 61.5(3) . . ?
C13 C12 Th1 174.9(4) . . ?
C23 C24 C25 120.7(5) . . ?
C23 C24 H24 119.6 . . ?
C25 C24 H24 119.6 . . ?
N20 C21 C20 107.2(5) . . ?
N20 C21 H21A 110.3 . . ?
C20 C21 H21A 110.3 . . ?
N20 C21 H21B 110.3 . . ?
C20 C21 H21B 110.3 . . ?
H21A C21 H21B 108.5 . . ?
O1 C1 C3 123.1(5) . 3_666 ?
O1 C1 C2 117.4(5) . . ?
C3 C1 C2 119.5(5) 3_666 . ?
O2A C41 C42 118.0(10) . . ?
O2A C41 C40 120.9(9) . . ?
C42 C41 C40 121.0(8) . . ?
N1 C30 C31 110.9(6) . . ?
N1 C30 H30A 109.5 . . ?
C31 C30 H30A 109.5 . . ?
N1 C30 H30B 109.5 . . ?
C31 C30 H30B 109.5 . . ?
H30A C30 H30B 108.0 . . ?
N1 C20 C21 112.3(5) . . ?
N1 C20 H20A 109.2 . . ?
C21 C20 H20A 109.2 . . ?
N1 C20 H20B 109.2 . . ?
C21 C20 H20B 109.2 . . ?
H20A C20 H20B 107.9 . . ?
C33 C34 C35 121.2(6) . . ?
C33 C34 H34 119.4 . . ?
C35 C34 H34 119.4 . . ?
C26 C25 C24 118.1(6) . . ?
C26 C25 H25 120.9 . . ?
C24 C25 H25 120.9 . . ?
C14 C13 C12 118.4(7) . . ?
C14 C13 H13 120.8 . . ?
C12 C13 H13 120.8 . . ?
C43 C44 C45 121.1(7) . . ?
C43 C44 H44 119.4 . . ?
C45 C44 H44 119.4 . . ?
C36 C35 C34 117.7(7) . . ?
C36 C35 H35 121.2 . . ?
C34 C35 H35 121.2 . . ?
C15 C14 C13 120.8(6) . . ?
C15 C14 H14 119.6 . . ?
C13 C14 H14 119.6 . . ?
N30 C31 C30 107.6(5) . . ?
N30 C31 H31A 110.2 . . ?
C30 C31 H31A 110.2 . . ?
N30 C31 H31B 110.2 . . ?
C30 C31 H31B 110.2 . . ?
H31A C31 H31B 108.5 . . ?
N11 C16 C15 121.8(8) . . ?
N11 C16 H16 119.1 . . ?
C15 C16 H16 119.1 . . ?
C43 C42 C41 120.9(8) . . ?
C43 C42 H42 119.6 . . ?
C41 C42 H42 119.6 . . ?
N1 C10 C11 111.7(5) . . ?
N1 C10 H10A 109.3 . . ?
C11 C10 H10A 109.3 . . ?
N1 C10 H10B 109.3 . . ?
C11 C10 H10B 109.3 . . ?
H10A C10 H10B 107.9 . . ?
C42 C43 C44 120.5(7) . . ?
C42 C43 H43 119.8 . . ?
C44 C43 H43 119.8 . . ?
N10 C11 C10 107.9(5) . . ?
N10 C11 H11A 110.1 . . ?
C10 C11 H11A 110.1 . . ?
N10 C11 H11B 110.1 . . ?
C10 C11 H11B 110.1 . . ?
H11A C11 H11B 108.4 . . ?
O100 C100 C101 102.6(8) . . ?
O100 C100 H10C 111.3 . . ?
C101 C100 H10C 111.3 . . ?
O100 C100 H10D 111.3 . . ?
C101 C100 H10D 111.3 . . ?
H10C C100 H10D 109.2 . . ?
C102 C101 C100 102.6(8) . . ?
C102 C101 H10E 111.3 . . ?
C100 C101 H10E 111.3 . . ?
C102 C101 H10F 111.3 . . ?
C100 C101 H10F 111.3 . . ?
H10E C101 H10F 109.2 . . ?
C14 C15 C16 118.7(7) . . ?
C14 C15 H15 120.7 . . ?
C16 C15 H15 120.7 . . ?
O100 C103 C102 106.6(9) . . ?
O100 C103 H10G 110.4 . . ?
C102 C103 H10G 110.4 . . ?
O100 C103 H10H 110.4 . . ?
C102 C103 H10H 110.4 . . ?
H10G C103 H10H 108.6 . . ?
C103 C102 C101 102.6(7) . . ?
C103 C102 H10I 111.2 . . ?
C101 C102 H10I 111.2 . . ?
C103 C102 H10J 111.2 . . ?
C101 C102 H10J 111.2 . . ?
H10I C102 H10J 109.2 . . ?
C45 O2 C46 117.2(6) . . ?
O2 C46 H46A 109.5 . . ?
O2 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
O2 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C41 O2A C46A 118.3(15) . . ?
O2A C46A H46D 109.5 . . ?
O2A C46A H46E 109.5 . . ?
H46D C46A H46E 109.5 . . ?
O2A C46A H46F 109.5 . . ?
H46D C46A H46F 109.5 . . ?
H46E C46A H46F 109.5 . . ?
O200 C200 C201 104.5(10) . . ?
C200 C201 C202 108.0(9) . . ?
C200 C201 H20C 110.1 . . ?
C202 C201 H20C 110.1 . . ?
C200 C201 H20D 110.1 . . ?
C202 C201 H20D 110.1 . . ?
H20C C201 H20D 108.4 . . ?
C201 C202 C203 100.0(10) . . ?
C201 C202 H20E 111.8 . . ?
C203 C202 H20E 111.8 . . ?
C201 C202 H20F 111.8 . . ?
C203 C202 H20F 111.8 . . ?
H20E C202 H20F 109.5 . . ?
O200 C203 C202 106.2(11) . . ?
O200 C203 H20G 110.5 . . ?
C202 C203 H20G 110.5 . . ?
O200 C203 H20H 110.5 . . ?
C202 C203 H20H 110.5 . . ?
H20G C203 H20H 108.7 . . ?
C200 O200 C203 109.7(14) . . ?

_refine_diff_density_max         2.381
_refine_diff_density_min         -1.050
_refine_diff_density_rms         0.128


_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
####################################################################### 
# 
# 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_shelx_CCDC6
_database_code_depnum_ccdc_archive 'CCDC 1526525'
_audit_update_record             
;
2017-01-10 deposited with the CCDC.
2017-08-14 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            'C90 H120 K N16 O14 U2'
_chemical_formula_weight         2165.17

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'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      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                   10.1836(3)
_cell_length_b                   13.3551(4)
_cell_length_c                   17.9008(5)
_cell_angle_alpha                110.8110(10)
_cell_angle_beta                 91.9630(10)
_cell_angle_gamma                100.2950(10)
_cell_volume                     2226.40(11)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    7510
_cell_measurement_theta_min      1.22
_cell_measurement_theta_max      25.36

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.615
_exptl_crystal_F_000             1087
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_exptl_absorpt_coefficient_mu    3.752
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.644
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_process_details   'Blessing, 1995'
_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 Quazar'
_diffrn_measurement_method       'omega phi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            96441
_diffrn_reflns_av_unetI/netI     0.0238
_diffrn_reflns_av_R_equivalents  0.0413
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.224
_diffrn_reflns_theta_max         25.359
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             8165
_reflns_number_gt                7510
_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 ApexIII suite, 2016'
_computing_cell_refinement       'Bruker ApexIII suite, 2016'
_computing_data_reduction        'Bruker ApexIII suite, 2016'
_computing_structure_solution    patterson
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Diamond 3D'
_computing_publication_material  WinGX
_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)+(0.0541P)²+7.8263P] 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         8165
_refine_ls_number_parameters     509
_refine_ls_number_restraints     21
_refine_ls_R_factor_all          0.0415
_refine_ls_R_factor_gt           0.0374
_refine_ls_wR_factor_ref         0.0958
_refine_ls_wR_factor_gt          0.0934
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_restrained_S_all      1.074
_refine_ls_shift/su_max          0.003
_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 0.50768(2) 0.83393(2) 0.73826(2) 0.02415(8) Uani 1 1 d . . . . .
K1 K 0.5000 0.5000 1.0000 0.0314(3) Uani 1 2 d S . P . .
O1 O 0.3983(3) 0.8558(3) 0.84911(19) 0.0257(7) Uani 1 1 d . . . . .
N2 N 0.6391(4) 0.9706(3) 0.8655(2) 0.0236(8) Uani 1 1 d . . . . .
C3 C 0.3687(5) 0.9375(4) 0.9880(3) 0.0209(9) Uani 1 1 d . . . . .
H3 H 0.2800 0.8956 0.9800 0.025 Uiso 1 1 calc R U . . .
C2 C 0.5782(5) 0.9887(4) 0.9342(3) 0.0204(9) Uani 1 1 d . . . . .
C40 C 0.7676(5) 1.0371(4) 0.8707(3) 0.0256(10) Uani 1 1 d . . . . .
C1 C 0.4432(5) 0.9246(3) 0.9229(3) 0.0205(9) Uani 1 1 d . . . . .
O2 O 0.8743(4) 0.9106(3) 0.8999(3) 0.0448(10) Uani 1 1 d . . . . .
N21 N 0.3515(4) 0.9628(3) 0.7190(3) 0.0325(10) Uani 1 1 d . . . . .
N20 N 0.5627(5) 0.9817(4) 0.6887(3) 0.0342(10) Uani 1 1 d . . . . .
N11 N 0.4741(5) 0.6312(4) 0.7389(3) 0.0388(11) Uani 1 1 d . . . . .
N30 N 0.4469(5) 0.7216(4) 0.6008(3) 0.0389(11) Uani 1 1 d . . . . .
C22 C 0.4447(6) 1.0089(4) 0.6808(3) 0.0320(12) Uani 1 1 d . . . . .
N10 N 0.6770(5) 0.7269(5) 0.7374(3) 0.0489(13) Uani 1 1 d . . . . .
N31 N 0.2717(5) 0.7144(4) 0.6705(3) 0.0395(11) Uani 1 1 d . . . . .
C41 C 0.8872(5) 1.0056(4) 0.8849(3) 0.0322(11) Uani 1 1 d . . . . .
N1 N 0.7127(6) 0.8282(5) 0.6290(4) 0.0583(16) Uani 1 1 d D U . . .
C42 C 1.0118(6) 1.0688(5) 0.8842(4) 0.0407(13) Uani 1 1 d . . . . .
H42 H 1.0921 1.0455 0.8926 0.049 Uiso 1 1 calc R U . . .
C32 C 0.3267(6) 0.6633(5) 0.6028(3) 0.0395(14) Uani 1 1 d . . . . .
C26 C 0.2282(6) 0.9821(4) 0.7185(4) 0.0405(13) Uani 1 1 d . . . . .
H26 H 0.1648 0.9488 0.7448 0.049 Uiso 1 1 calc R U . . .
C45 C 0.7790(6) 1.1340(4) 0.8578(4) 0.0406(14) Uani 1 1 d . . . . .
H45 H 0.6994 1.1577 0.8489 0.049 Uiso 1 1 calc R U . . .
C25 C 0.1867(7) 1.0484(5) 0.6817(4) 0.0506(16) Uani 1 1 d . . . . .
H25 H 0.0985 1.0626 0.6842 0.061 Uiso 1 1 calc R U . . .
C24 C 0.2792(7) 1.0933(5) 0.6410(4) 0.0503(16) Uani 1 1 d . . . . .
H24 H 0.2537 1.1377 0.6140 0.060 Uiso 1 1 calc R U . . .
C21 C 0.6675(6) 1.0076(5) 0.6413(4) 0.0449(14) Uani 1 1 d . . . . .
H21A H 0.7075 1.0868 0.6641 0.054 Uiso 1 1 calc R U . . .
H21B H 0.6293 0.9886 0.5852 0.054 Uiso 1 1 calc R U . . .
C23 C 0.4065(7) 1.0740(5) 0.6394(4) 0.0423(14) Uani 1 1 d . . . . .
H23 H 0.4690 1.1039 0.6109 0.051 Uiso 1 1 calc R U . . .
C43 C 1.0175(6) 1.1653(5) 0.8713(4) 0.0516(17) Uani 1 1 d . . . . .
H43 H 1.1021 1.2094 0.8721 0.062 Uiso 1 1 calc R U . . .
C12 C 0.6017(7) 0.6272(6) 0.7201(3) 0.0480(17) Uani 1 1 d . . . . .
C16 C 0.3863(9) 0.5384(5) 0.7241(4) 0.061(2) Uani 1 1 d . . . . .
H16 H 0.2968 0.5408 0.7368 0.073 Uiso 1 1 calc R U . . .
C33 C 0.2570(8) 0.5595(5) 0.5469(4) 0.0534(18) Uani 1 1 d . . . . .
H33 H 0.2953 0.5222 0.4999 0.064 Uiso 1 1 calc R U . . .
C20 C 0.7736(6) 0.9422(6) 0.6431(4) 0.0516(17) Uani 1 1 d . . . . .
H20A H 0.8338 0.9445 0.6012 0.062 Uiso 1 1 calc R U . . .
H20B H 0.8282 0.9755 0.6959 0.062 Uiso 1 1 calc R U . . .
C36 C 0.1525(6) 0.6686(5) 0.6839(5) 0.061(2) Uani 1 1 d . . . . .
H36 H 0.1160 0.7049 0.7320 0.073 Uiso 1 1 calc R U . . .
C34 C 0.1356(8) 0.5154(5) 0.5622(5) 0.065(2) Uani 1 1 d . . . . .
H34 H 0.0884 0.4463 0.5256 0.078 Uiso 1 1 calc R U . . .
C44 C 0.9014(6) 1.1981(5) 0.8574(5) 0.0569(19) Uani 1 1 d . . . . .
H44 H 0.9053 1.2639 0.8477 0.068 Uiso 1 1 calc R U . . .
C15 C 0.4238(15) 0.4356(6) 0.6896(5) 0.096(4) Uani 1 1 d . . . . .
H15 H 0.3607 0.3694 0.6795 0.115 Uiso 1 1 calc R U . . .
C30 C 0.6470(10) 0.7687(7) 0.5466(4) 0.092(3) Uani 1 1 d D . . . .
H30A H 0.7146 0.7393 0.5111 0.111 Uiso 1 1 calc R U . . .
H30B H 0.6114 0.8203 0.5271 0.111 Uiso 1 1 calc R U . . .
C35 C 0.0795(7) 0.5691(5) 0.6300(6) 0.073(3) Uani 1 1 d . . . . .
H35 H -0.0071 0.5391 0.6398 0.087 Uiso 1 1 calc R U . . .
C31 C 0.5345(10) 0.6761(6) 0.5412(4) 0.073(3) Uani 1 1 d . . . . .
H31A H 0.4848 0.6443 0.4868 0.088 Uiso 1 1 calc R U . . .
H31B H 0.5700 0.6179 0.5523 0.088 Uiso 1 1 calc R U . . .
C46 C 0.9940(6) 0.8703(6) 0.9043(5) 0.0540(17) Uani 1 1 d . . . . .
H46A H 1.0360 0.8599 0.8544 0.081 Uiso 1 1 calc R U . . .
H46B H 0.9717 0.8002 0.9117 0.081 Uiso 1 1 calc R U . . .
H46C H 1.0564 0.9231 0.9498 0.081 Uiso 1 1 calc R U . . .
C13 C 0.6400(12) 0.5251(8) 0.6843(4) 0.084(3) Uani 1 1 d . . . . .
H13 H 0.7288 0.5232 0.6701 0.100 Uiso 1 1 calc R U . . .
C11 C 0.8067(8) 0.7425(10) 0.7104(5) 0.087(3) Uani 1 1 d D U . . .
H11A H 0.8666 0.8045 0.7531 0.104 Uiso 1 1 calc R U . . .
H11B H 0.8438 0.6762 0.7024 0.104 Uiso 1 1 calc R U . . .
C14 C 0.5544(18) 0.4337(10) 0.6708(5) 0.115(6) Uani 1 1 d . . . . .
H14 H 0.5817 0.3658 0.6481 0.138 Uiso 1 1 calc R U . . .
C10 C 0.8090(10) 0.7636(10) 0.6378(7) 0.109(3) Uani 1 1 d D U . . .
H10A H 0.7904 0.6929 0.5917 0.131 Uiso 1 1 calc R U . . .
H10B H 0.9003 0.8027 0.6357 0.131 Uiso 1 1 calc R U . . .
O200 O 0.7154(6) 0.4685(5) 1.0720(5) 0.0994(15) Uani 1 1 d . . . . .
C200 C 0.7301(10) 0.3633(7) 1.0669(8) 0.0994(15) Uani 1 1 d . . . . .
H20C H 0.7107 0.3108 1.0106 0.119 Uiso 1 1 calc R U . . .
H20D H 0.6689 0.3363 1.1004 0.119 Uiso 1 1 calc R U . . .
C203 C 0.8138(10) 0.5477(7) 1.1157(8) 0.0994(15) Uani 1 1 d . . . . .
H20E H 0.7797 0.6001 1.1615 0.119 Uiso 1 1 calc R U . . .
H20F H 0.8574 0.5877 1.0830 0.119 Uiso 1 1 calc R U . . .
O100 O 0.6490(4) 0.7054(3) 1.0109(2) 0.0325(8) Uani 1 1 d . . . . .
O101 O 0.4521(4) 0.6948(3) 1.1152(2) 0.0344(8) Uani 1 1 d . . . . .
O102 O 0.3524(4) 0.4867(3) 1.1243(2) 0.0375(9) Uani 1 1 d . . . . .
C201 C 0.8680(10) 0.3775(7) 1.0962(7) 0.0994(15) Uani 1 1 d . . . . .
H20G H 0.9233 0.3558 1.0510 0.119 Uiso 1 1 calc R U . . .
H20H H 0.8760 0.3327 1.1293 0.119 Uiso 1 1 calc R U . . .
C202 C 0.9114(10) 0.4955(7) 1.1454(7) 0.0994(15) Uani 1 1 d . . . . .
H20I H 1.0043 0.5237 1.1371 0.119 Uiso 1 1 calc R U . . .
H20J H 0.9070 0.5091 1.2033 0.119 Uiso 1 1 calc R U . . .
C100 C 0.5985(6) 0.7981(4) 1.0569(4) 0.0367(13) Uani 1 1 d . . . . .
H10C H 0.5190 0.8036 1.0263 0.044 Uiso 1 1 calc R U . . .
H10D H 0.6677 0.8654 1.0683 0.044 Uiso 1 1 calc R U . . .
C104 C 0.6758(6) 0.7060(4) 0.9335(4) 0.0371(13) Uani 1 1 d . . . . .
H10E H 0.7345 0.7762 0.9386 0.045 Uiso 1 1 calc R U . . .
H10F H 0.5910 0.6972 0.9009 0.045 Uiso 1 1 calc R U . . .
C101 C 0.5608(6) 0.7872(4) 1.1332(4) 0.0383(13) Uani 1 1 d . . . . .
H10G H 0.6386 0.7768 1.1622 0.046 Uiso 1 1 calc R U . . .
H10H H 0.5330 0.8545 1.1680 0.046 Uiso 1 1 calc R U . . .
C105 C 0.2564(6) 0.3869(4) 1.1060(4) 0.0387(13) Uani 1 1 d . . . . .
H10I H 0.1796 0.3845 1.0695 0.046 Uiso 1 1 calc R U . . .
H10J H 0.2221 0.3817 1.1558 0.046 Uiso 1 1 calc R U . . .
C102 C 0.4095(6) 0.6801(5) 1.1857(3) 0.0405(13) Uani 1 1 d . . . . .
H10K H 0.3780 0.7456 1.2202 0.049 Uiso 1 1 calc R U . . .
H10L H 0.4853 0.6697 1.2164 0.049 Uiso 1 1 calc R U . . .
C103 C 0.2973(6) 0.5810(5) 1.1616(4) 0.0407(13) Uani 1 1 d . . . . .
H10M H 0.2550 0.5763 1.2096 0.049 Uiso 1 1 calc R U . . .
H10N H 0.2279 0.5860 1.1238 0.049 Uiso 1 1 calc R U . . .
O300 O 0.7913(9) 0.2676(7) 0.6222(5) 0.1153(17) Uani 1 1 d . . . . .
C301 C 0.8762(13) 0.2159(11) 0.5019(7) 0.1153(17) Uani 1 1 d . . . . .
H30C H 0.9030 0.2850 0.4923 0.138 Uiso 1 1 calc R U . . .
H30D H 0.8679 0.1530 0.4505 0.138 Uiso 1 1 calc R U . . .
C300 C 0.7556(13) 0.2130(11) 0.5399(7) 0.1153(17) Uani 1 1 d . . . . .
H30E H 0.6938 0.2494 0.5198 0.138 Uiso 1 1 calc R U . . .
H30F H 0.7100 0.1363 0.5283 0.138 Uiso 1 1 calc R U . . .
C302 C 0.9724(13) 0.2085(11) 0.5646(7) 0.1153(17) Uani 1 1 d . . . . .
H30G H 0.9678 0.1316 0.5592 0.138 Uiso 1 1 calc R U . . .
H30H H 1.0657 0.2416 0.5607 0.138 Uiso 1 1 calc R U . . .
C303 C 0.9255(14) 0.2706(11) 0.6398(8) 0.1153(17) Uani 1 1 d . . . . .
H30I H 0.9367 0.2373 0.6804 0.138 Uiso 1 1 calc R U . . .
H30J H 0.9767 0.3471 0.6612 0.138 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 O1 2.263(3) . ?
U1 N30 2.372(4) . ?
U1 N10 2.425(5) . ?
U1 N20 2.425(4) . ?
U1 N2 2.505(4) . ?
U1 N31 2.617(5) . ?
U1 N21 2.640(4) . ?
U1 N11 2.672(5) . ?
U1 N1 2.901(5) . ?
U1 C32 2.956(6) . ?
U1 C12 2.995(6) . ?
U1 C22 3.021(5) . ?
K1 O200 2.677(6) 2_667 ?
K1 O200 2.677(6) . ?
K1 O102 2.768(4) . ?
K1 O102 2.768(4) 2_667 ?
K1 O101 2.823(3) . ?
K1 O101 2.823(3) 2_667 ?
K1 O100 2.824(3) . ?
K1 O100 2.824(3) 2_667 ?
O1 C1 1.321(6) . ?
N2 C2 1.360(6) . ?
N2 C40 1.425(6) . ?
C3 C1 1.388(6) . ?
C3 C2 1.409(6) 2_677 ?
C2 C3 1.409(6) 2_677 ?
C2 C1 1.449(7) . ?
C40 C45 1.379(7) . ?
C40 C41 1.401(7) . ?
O2 C41 1.372(6) . ?
O2 C46 1.429(7) . ?
N21 C26 1.327(7) . ?
N21 C22 1.373(7) . ?
N20 C22 1.332(7) . ?
N20 C21 1.455(7) . ?
N11 C16 1.327(8) . ?
N11 C12 1.359(8) . ?
N30 C32 1.337(8) . ?
N30 C31 1.450(8) . ?
C22 C23 1.419(8) . ?
N10 C12 1.335(9) . ?
N10 C11 1.428(9) . ?
N31 C36 1.328(8) . ?
N31 C32 1.358(8) . ?
C41 C42 1.395(8) . ?
N1 C10 1.456(7) . ?
N1 C20 1.465(9) . ?
N1 C30 1.472(8) . ?
C42 C43 1.379(9) . ?
C32 C33 1.427(8) . ?
C26 C25 1.388(9) . ?
C45 C44 1.382(8) . ?
C25 C24 1.391(10) . ?
C24 C23 1.365(9) . ?
C21 C20 1.511(9) . ?
C43 C44 1.376(9) . ?
C12 C13 1.417(9) . ?
C16 C15 1.419(13) . ?
C33 C34 1.353(11) . ?
C36 C35 1.392(9) . ?
C34 C35 1.374(12) . ?
C15 C14 1.384(17) . ?
C30 C31 1.501(11) . ?
C13 C14 1.306(18) . ?
C11 C10 1.424(8) . ?
O200 C203 1.310(10) . ?
O200 C200 1.410(10) . ?
C200 C201 1.438(12) . ?
C203 C202 1.494(11) . ?
O100 C100 1.416(6) . ?
O100 C104 1.424(7) . ?
O101 C102 1.415(7) . ?
O101 C101 1.434(7) . ?
O102 C103 1.423(7) . ?
O102 C105 1.429(7) . ?
C201 C202 1.481(12) . ?
C100 C101 1.480(8) . ?
C104 C105 1.494(8) 2_667 ?
C105 C104 1.494(8) 2_667 ?
C102 C103 1.505(9) . ?
O300 C303 1.382(14) . ?
O300 C300 1.393(15) . ?
C301 C300 1.425(15) . ?
C301 C302 1.505(16) . ?
C302 C303 1.456(15) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 U1 N30 132.64(16) . . ?
O1 U1 N10 109.74(15) . . ?
N30 U1 N10 86.92(18) . . ?
O1 U1 N20 120.88(14) . . ?
N30 U1 N20 84.78(16) . . ?
N10 U1 N20 117.25(17) . . ?
O1 U1 N2 65.72(12) . . ?
N30 U1 N2 161.64(16) . . ?
N10 U1 N2 85.51(17) . . ?
N20 U1 N2 83.87(14) . . ?
O1 U1 N31 80.48(14) . . ?
N30 U1 N31 52.54(17) . . ?
N10 U1 N31 113.39(18) . . ?
N20 U1 N31 109.46(16) . . ?
N2 U1 N31 145.54(14) . . ?
O1 U1 N21 81.00(13) . . ?
N30 U1 N21 88.26(15) . . ?
N10 U1 N21 168.65(16) . . ?
N20 U1 N21 52.00(15) . . ?
N2 U1 N21 96.03(13) . . ?
N31 U1 N21 71.16(14) . . ?
O1 U1 N11 80.25(14) . . ?
N30 U1 N11 76.63(15) . . ?
N10 U1 N11 51.70(18) . . ?
N20 U1 N11 158.46(15) . . ?
N2 U1 N11 111.03(13) . . ?
N31 U1 N11 67.33(15) . . ?
N21 U1 N11 136.59(15) . . ?
O1 U1 N1 164.03(15) . . ?
N30 U1 N1 62.21(18) . . ?
N10 U1 N1 60.92(16) . . ?
N20 U1 N1 60.42(15) . . ?
N2 U1 N1 99.56(16) . . ?
N31 U1 N1 114.73(17) . . ?
N21 U1 N1 107.77(15) . . ?
N11 U1 N1 100.63(16) . . ?
O1 U1 C32 106.43(16) . . ?
N30 U1 C32 26.26(18) . . ?
N10 U1 C32 96.03(18) . . ?
N20 U1 C32 102.30(16) . . ?
N2 U1 C32 171.97(16) . . ?
N31 U1 C32 27.35(17) . . ?
N21 U1 C32 84.02(14) . . ?
N11 U1 C32 64.59(15) . . ?
N1 U1 C32 88.04(19) . . ?
O1 U1 C12 100.34(15) . . ?
N30 U1 C12 75.41(16) . . ?
N10 U1 C12 25.9(2) . . ?
N20 U1 C12 136.77(17) . . ?
N2 U1 C12 103.60(15) . . ?
N31 U1 C12 88.35(18) . . ?
N21 U1 C12 159.06(18) . . ?
N11 U1 C12 26.99(18) . . ?
N1 U1 C12 76.36(17) . . ?
C32 U1 C12 75.52(17) . . ?
O1 U1 C22 104.24(13) . . ?
N30 U1 C22 82.60(15) . . ?
N10 U1 C22 141.84(17) . . ?
N20 U1 C22 25.43(15) . . ?
N2 U1 C22 93.13(13) . . ?
N31 U1 C22 88.61(15) . . ?
N21 U1 C22 27.00(14) . . ?
N11 U1 C22 154.71(14) . . ?
N1 U1 C22 81.87(15) . . ?
C32 U1 C22 90.51(14) . . ?
C12 U1 C22 154.37(14) . . ?
O200 K1 O200 180.0 2_667 . ?
O200 K1 O102 89.3(2) 2_667 . ?
O200 K1 O102 90.7(2) . . ?
O200 K1 O102 90.7(2) 2_667 2_667 ?
O200 K1 O102 89.3(2) . 2_667 ?
O102 K1 O102 180.0 . 2_667 ?
O200 K1 O101 77.94(17) 2_667 . ?
O200 K1 O101 102.06(17) . . ?
O102 K1 O101 61.23(11) . . ?
O102 K1 O101 118.77(11) 2_667 . ?
O200 K1 O101 102.06(17) 2_667 2_667 ?
O200 K1 O101 77.94(17) . 2_667 ?
O102 K1 O101 118.77(11) . 2_667 ?
O102 K1 O101 61.23(11) 2_667 2_667 ?
O101 K1 O101 180.0 . 2_667 ?
O200 K1 O100 91.19(15) 2_667 . ?
O200 K1 O100 88.81(15) . . ?
O102 K1 O100 119.17(11) . . ?
O102 K1 O100 60.83(11) 2_667 . ?
O101 K1 O100 59.55(11) . . ?
O101 K1 O100 120.45(11) 2_667 . ?
O200 K1 O100 88.81(15) 2_667 2_667 ?
O200 K1 O100 91.19(15) . 2_667 ?
O102 K1 O100 60.83(11) . 2_667 ?
O102 K1 O100 119.17(11) 2_667 2_667 ?
O101 K1 O100 120.45(11) . 2_667 ?
O101 K1 O100 59.55(11) 2_667 2_667 ?
O100 K1 O100 180.0 . 2_667 ?
C1 O1 U1 126.4(3) . . ?
C2 N2 C40 117.4(4) . . ?
C2 N2 U1 117.2(3) . . ?
C40 N2 U1 125.2(3) . . ?
C1 C3 C2 121.4(4) . 2_677 ?
N2 C2 C3 127.1(4) . 2_677 ?
N2 C2 C1 114.2(4) . . ?
C3 C2 C1 118.7(4) 2_677 . ?
C45 C40 C41 117.0(5) . . ?
C45 C40 N2 120.6(5) . . ?
C41 C40 N2 122.3(4) . . ?
O1 C1 C3 123.7(4) . . ?
O1 C1 C2 116.4(4) . . ?
C3 C1 C2 119.9(4) . . ?
C41 O2 C46 116.8(4) . . ?
C26 N21 C22 119.5(5) . . ?
C26 N21 U1 146.7(4) . . ?
C22 N21 U1 92.2(3) . . ?
C22 N20 C21 118.9(5) . . ?
C22 N20 U1 103.2(3) . . ?
C21 N20 U1 132.3(4) . . ?
C16 N11 C12 119.2(6) . . ?
C16 N11 U1 144.8(4) . . ?
C12 N11 U1 89.9(4) . . ?
C32 N30 C31 121.0(5) . . ?
C32 N30 U1 102.0(3) . . ?
C31 N30 U1 127.9(5) . . ?
N20 C22 N21 110.9(5) . . ?
N20 C22 C23 129.6(5) . . ?
N21 C22 C23 119.4(5) . . ?
N20 C22 U1 51.4(3) . . ?
N21 C22 U1 60.8(3) . . ?
C23 C22 U1 168.8(4) . . ?
C12 N10 C11 121.7(7) . . ?
C12 N10 U1 101.7(4) . . ?
C11 N10 U1 126.2(5) . . ?
C36 N31 C32 119.9(5) . . ?
C36 N31 U1 144.6(5) . . ?
C32 N31 U1 90.4(3) . . ?
O2 C41 C42 122.6(5) . . ?
O2 C41 C40 116.3(4) . . ?
C42 C41 C40 121.1(5) . . ?
C10 N1 C20 113.7(7) . . ?
C10 N1 C30 104.0(8) . . ?
C20 N1 C30 112.4(6) . . ?
C10 N1 U1 112.3(4) . . ?
C20 N1 U1 106.6(4) . . ?
C30 N1 U1 107.8(4) . . ?
C43 C42 C41 119.5(5) . . ?
N30 C32 N31 110.8(5) . . ?
N30 C32 C33 129.3(6) . . ?
N31 C32 C33 119.8(6) . . ?
N30 C32 U1 51.7(3) . . ?
N31 C32 U1 62.3(3) . . ?
C33 C32 U1 162.3(4) . . ?
N21 C26 C25 123.6(6) . . ?
C40 C45 C44 122.7(6) . . ?
C26 C25 C24 117.5(6) . . ?
C23 C24 C25 120.5(6) . . ?
N20 C21 C20 108.3(5) . . ?
C24 C23 C22 119.5(6) . . ?
C44 C43 C42 120.4(5) . . ?
N10 C12 N11 112.0(5) . . ?
N10 C12 C13 127.7(8) . . ?
N11 C12 C13 120.4(8) . . ?
N10 C12 U1 52.4(3) . . ?
N11 C12 U1 63.1(3) . . ?
C13 C12 U1 160.9(4) . . ?
N11 C16 C15 121.1(9) . . ?
C34 C33 C32 118.7(7) . . ?
N1 C20 C21 111.1(5) . . ?
N31 C36 C35 122.1(7) . . ?
C33 C34 C35 120.9(6) . . ?
C43 C44 C45 119.2(6) . . ?
C14 C15 C16 118.6(9) . . ?
N1 C30 C31 112.5(6) . . ?
C34 C35 C36 118.4(7) . . ?
N30 C31 C30 106.7(6) . . ?
C14 C13 C12 120.5(11) . . ?
C10 C11 N10 114.8(7) . . ?
C13 C14 C15 120.2(9) . . ?
C11 C10 N1 113.9(7) . . ?
C203 O200 C200 114.3(6) . . ?
C203 O200 K1 123.9(5) . . ?
C200 O200 K1 121.9(5) . . ?
O200 C200 C201 104.7(7) . . ?
O200 C203 C202 106.7(7) . . ?
C100 O100 C104 112.0(4) . . ?
C100 O100 K1 116.2(3) . . ?
C104 O100 K1 111.1(3) . . ?
C102 O101 C101 111.8(4) . . ?
C102 O101 K1 112.3(3) . . ?
C101 O101 K1 114.1(3) . . ?
C103 O102 C105 112.7(4) . . ?
C103 O102 K1 113.2(3) . . ?
C105 O102 K1 115.1(3) . . ?
C200 C201 C202 105.4(8) . . ?
C201 C202 C203 104.0(7) . . ?
O100 C100 C101 109.2(4) . . ?
O100 C104 C105 107.7(4) . 2_667 ?
O101 C101 C100 108.6(4) . . ?
O102 C105 C104 108.1(5) . 2_667 ?
O101 C102 C103 108.5(5) . . ?
O102 C103 C102 108.0(5) . . ?
C303 O300 C300 109.2(9) . . ?
C300 C301 C302 100.4(9) . . ?
O300 C300 C301 107.2(12) . . ?
C303 C302 C301 103.1(10) . . ?
O300 C303 C302 106.3(12) . . ?

_refine_diff_density_max         2.559
_refine_diff_density_min         -1.406
_refine_diff_density_rms         0.123


_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
