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

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
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data_mr1522
_database_code_depnum_ccdc_archive 'CCDC 1893558'
loop_
_audit_author_name
_audit_author_address
'Frank W. Heinemann'
;Friedrich-Alexander-Universit?t Erlangen-N?rnberg
Germany
;
_audit_update_record             
;
2019-01-25 deposited with the CCDC.	2019-03-25 downloaded from the CCDC.
;
_audit_creation_date             2019-01-24
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C60 H79 N3 O4 U, 2(C4 H8 O)'
_chemical_formula_sum            'C68 H95 N3 O6 U'
_chemical_formula_weight         1288.49
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.4689(11)
_cell_length_b                   12.8625(13)
_cell_length_c                   23.576(2)
_cell_angle_alpha                75.002(3)
_cell_angle_beta                 83.542(3)
_cell_angle_gamma                80.041(3)
_cell_volume                     3012.6(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9751
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.13
_cell_measurement_theta_min      2.23
_shelx_estimated_absorpt_T_max   0.922
_shelx_estimated_absorpt_T_min   0.771
_exptl_absorpt_coefficient_mu    2.748
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6648
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.0697 before and 0.0564 after correction.
The Ratio of minimum to maximum transmission is 0.8918.
The λ/2 correction factor is 0.00150.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.420
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0698
_diffrn_reflns_av_unetI/netI     0.0534
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            83017
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.205
_diffrn_reflns_theta_min         1.658
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_radiation_source         'ImuS micro-focus tube'
_diffrn_radiation_monochromator  'Quazar focussing montel optics'
_diffrn_measurement_device_type  'Bruker Kappa APEX II CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 83.33
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                11542
_reflns_number_total             13383
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELX XT 2014/5 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2015)'
_computing_molecular_graphics    'SHELXTL 6.12 (Bruker AXS, 2002)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_refine_diff_density_max         3.308
_refine_diff_density_min         -1.977
_refine_diff_density_rms         0.120
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     755
_refine_ls_number_reflns         13383
_refine_ls_number_restraints     210
_refine_ls_R_factor_all          0.0523
_refine_ls_R_factor_gt           0.0390
_refine_ls_restrained_S_all      1.095
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0252P)²+7.5131P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0774
_refine_ls_wR_factor_ref         0.0811
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Uiso/Uaniso restraints and constraints
O100 \\sim C101 \\sim C102 \\sim C103 \\sim C104: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02
O200 \\sim C201 \\sim C202 \\sim C203 \\sim C204 \\sim O210 \\sim C211 \\sim
C212 \\sim C213 \\sim C214: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
3. Same fragment restrains
{O100, C101, C102, C103, C104} sigma for 1-2: 0.02, 1-3: 0.04
as
{O200, C201, C202, C203, C204}
{O100, C101, C102, C103, C104} sigma for 1-2: 0.02, 1-3: 0.04
as
{O210, C211, C212, C213, C214}
4. Others
 Sof(O210)=Sof(C211)=Sof(H21C)=Sof(H21D)=Sof(C212)=Sof(H21E)=Sof(H21F)=
 Sof(C213)=Sof(H21G)=Sof(H21H)=Sof(C214)=Sof(H21I)=Sof(H21J)=1-FVAR(1)
 Sof(O200)=Sof(C201)=Sof(H20C)=Sof(H20D)=Sof(C202)=Sof(H20E)=Sof(H20F)=
 Sof(C203)=Sof(H20G)=Sof(H20H)=Sof(C204)=Sof(H20I)=Sof(H20J)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C15(H15), C16(H16), C17(H17), C33(H33), C34(H34), C35(H35), C51(H51),
 C52(H52), C53(H53)
5.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B),
 C7(H7A,H7B), C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B),
 C22(H22A,H22B), C23(H23A,H23B), C25(H25A,H25B), C36(H36A,H36B), C37(H37A,H37B),
  C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B), C41(H41A,H41B), C43(H43A,
 H43B), C54(H54A,H54B), C55(H55A,H55B), C56(H56A,H56B), C57(H57A,H57B),
 C58(H58A,H58B), C59(H59A,H59B), C101(H10A,H10B), C102(H10C,H10D), C103(H10E,
 H10F), C104(H10G,H10H), C201(H20C,H20D), C202(H20E,H20F), C203(H20G,H20H),
 C204(H20I,H20J), C211(H21C,H21D), C212(H21E,H21F), C213(H21G,H21H), C214(H21I,
 H21J)
5.c Aromatic/amide H refined with riding coordinates:
 C11(H11), C13(H13), C29(H29), C31(H31), C47(H47), C49(H49)
5.d Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C42(H42A,H42B,H42C), C60(H60A,H60B,H60C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.11648(2) 0.39551(2) 0.26776(2) 0.01353(5) Uani 1 1 d . . . . .
O1 O 0.1732(3) 0.5548(2) 0.22373(12) 0.0183(6) Uani 1 1 d . . . . .
O2 O 0.1321(3) 0.2652(2) 0.22163(12) 0.0174(6) Uani 1 1 d . . . . .
O3 O 0.0006(3) 0.3786(2) 0.35261(11) 0.0189(6) Uani 1 1 d . . . . .
O4 O -0.0598(3) 0.4560(2) 0.22987(13) 0.0221(7) Uani 1 1 d . . . . .
H4 H -0.130(5) 0.475(4) 0.216(2) 0.033 Uiso 1 1 d R . . . .
N1 N 0.2942(3) 0.4449(3) 0.32965(14) 0.0175(7) Uani 1 1 d . . . . .
N2 N 0.3688(3) 0.3257(3) 0.23942(15) 0.0177(7) Uani 1 1 d . . . . .
N3 N 0.2340(3) 0.2262(3) 0.34935(15) 0.0189(7) Uani 1 1 d . . . . .
C1 C 0.4313(4) 0.4305(3) 0.30522(19) 0.0219(9) Uani 1 1 d . . . . .
H1A H 0.481456 0.368656 0.332133 0.026 Uiso 1 1 calc R . . . .
H1B H 0.469235 0.496750 0.303428 0.026 Uiso 1 1 calc R . . . .
C2 C 0.4451(4) 0.4096(3) 0.24453(19) 0.0206(9) Uani 1 1 d . . . . .
H2A H 0.416590 0.478508 0.215674 0.025 Uiso 1 1 calc R . . . .
H2B H 0.538039 0.386001 0.234273 0.025 Uiso 1 1 calc R . . . .
C3 C 0.4218(4) 0.2158(3) 0.27436(19) 0.0227(9) Uani 1 1 d . . . . .
H3A H 0.490169 0.223346 0.298195 0.027 Uiso 1 1 calc R . . . .
H3B H 0.463189 0.171074 0.246944 0.027 Uiso 1 1 calc R . . . .
C4 C 0.3201(4) 0.1562(3) 0.31523(19) 0.0215(9) Uani 1 1 d . . . . .
H4A H 0.266432 0.129532 0.291573 0.026 Uiso 1 1 calc R . . . .
H4B H 0.364608 0.092063 0.342913 0.026 Uiso 1 1 calc R . . . .
C5 C 0.3075(4) 0.2550(3) 0.39214(18) 0.0210(9) Uani 1 1 d . . . . .
H5A H 0.401744 0.233509 0.383487 0.025 Uiso 1 1 calc R . . . .
H5B H 0.283650 0.213127 0.432352 0.025 Uiso 1 1 calc R . . . .
C6 C 0.2813(4) 0.3753(3) 0.39030(18) 0.0208(9) Uani 1 1 d . . . . .
H6A H 0.192275 0.393291 0.407749 0.025 Uiso 1 1 calc R . . . .
H6B H 0.343034 0.391525 0.414569 0.025 Uiso 1 1 calc R . . . .
C7 C 0.2490(4) 0.5603(3) 0.33278(17) 0.0193(9) Uani 1 1 d . . . . .
H7A H 0.292258 0.574102 0.364792 0.023 Uiso 1 1 calc R . . . .
H7B H 0.154405 0.568699 0.343779 0.023 Uiso 1 1 calc R . . . .
C8 C 0.2735(4) 0.6456(3) 0.27769(17) 0.0174(8) Uani 1 1 d . . . . .
C9 C 0.2291(4) 0.6412(3) 0.22413(18) 0.0169(8) Uani 1 1 d . . . . .
C10 C 0.2451(4) 0.7252(3) 0.17286(18) 0.0176(8) Uani 1 1 d . . . . .
C11 C 0.3052(4) 0.8102(3) 0.17816(19) 0.0204(9) Uani 1 1 d . . . . .
H11 H 0.316627 0.867177 0.144028 0.024 Uiso 1 1 calc R . . . .
C12 C 0.3500(4) 0.8171(3) 0.23069(19) 0.0209(9) Uani 1 1 d . . . . .
C13 C 0.3321(4) 0.7337(3) 0.27987(18) 0.0195(9) Uani 1 1 d . . . . .
H13 H 0.360552 0.736545 0.316240 0.023 Uiso 1 1 calc R . . . .
C14 C 0.1970(4) 0.7227(3) 0.11421(18) 0.0211(9) Uani 1 1 d . . . . .
C15 C 0.0039(5) 0.7147(5) 0.0611(2) 0.0448(14) Uani 1 1 d . . . . .
H15 H -0.091960 0.713353 0.065566 0.054 Uiso 1 1 calc R . . . .
C16 C 0.2193(6) 0.6120(4) 0.0371(2) 0.0425(14) Uani 1 1 d . . . . .
H16 H 0.264370 0.543665 0.026614 0.051 Uiso 1 1 calc R . . . .
C17 C 0.1797(5) 0.8146(4) 0.0059(2) 0.0386(13) Uani 1 1 d . . . . .
H17 H 0.199390 0.879688 -0.025631 0.046 Uiso 1 1 calc R . . . .
C18 C 0.0496(4) 0.7214(4) 0.1199(2) 0.0304(11) Uani 1 1 d . . . . .
H18A H 0.003650 0.788400 0.130636 0.036 Uiso 1 1 calc R . . . .
H18B H 0.028344 0.658071 0.151469 0.036 Uiso 1 1 calc R . . . .
C19 C 0.2271(5) 0.8208(4) 0.06421(18) 0.0259(10) Uani 1 1 d . . . . .
H19A H 0.322009 0.822232 0.059453 0.031 Uiso 1 1 calc R . . . .
H19B H 0.183852 0.889008 0.074478 0.031 Uiso 1 1 calc R . . . .
C20 C 0.0732(6) 0.6114(5) 0.0449(2) 0.0537(17) Uani 1 1 d . . . . .
H20A H 0.041799 0.606040 0.007798 0.064 Uiso 1 1 calc R . . . .
H20B H 0.053466 0.547160 0.076215 0.064 Uiso 1 1 calc R . . . .
C21 C 0.2512(6) 0.7109(4) -0.0111(2) 0.0436(14) Uani 1 1 d . . . . .
H21A H 0.223210 0.707103 -0.049154 0.052 Uiso 1 1 calc R . . . .
H21B H 0.346133 0.711958 -0.015404 0.052 Uiso 1 1 calc R . . . .
C22 C 0.2648(5) 0.6193(4) 0.09521(19) 0.0283(10) Uani 1 1 d . . . . .
H22A H 0.359991 0.619145 0.090909 0.034 Uiso 1 1 calc R . . . .
H22B H 0.246616 0.554285 0.126360 0.034 Uiso 1 1 calc R . . . .
C23 C 0.0335(6) 0.8137(5) 0.0128(2) 0.0485(15) Uani 1 1 d . . . . .
H23A H 0.002445 0.810475 -0.024749 0.058 Uiso 1 1 calc R . . . .
H23B H -0.011902 0.881076 0.023275 0.058 Uiso 1 1 calc R . . . .
C24 C 0.4160(5) 0.9113(4) 0.2331(2) 0.0329(12) Uani 1 1 d . . . . .
H24A H 0.504012 0.903148 0.213979 0.049 Uiso 1 1 calc GR . . . .
H24B H 0.420794 0.912080 0.274225 0.049 Uiso 1 1 calc GR . . . .
H24C H 0.365983 0.979738 0.212547 0.049 Uiso 1 1 calc GR . . . .
C25 C 0.3758(4) 0.3283(3) 0.17561(18) 0.0201(9) Uani 1 1 d . . . . .
H25A H 0.468330 0.324014 0.160746 0.024 Uiso 1 1 calc R . . . .
H25B H 0.330648 0.399963 0.154888 0.024 Uiso 1 1 calc R . . . .
C26 C 0.3201(4) 0.2417(3) 0.15823(18) 0.0169(8) Uani 1 1 d . . . . .
C27 C 0.1965(4) 0.2163(3) 0.18019(17) 0.0164(8) Uani 1 1 d . . . . .
C28 C 0.1418(4) 0.1425(3) 0.15867(17) 0.0164(8) Uani 1 1 d . . . . .
C29 C 0.2126(4) 0.1010(3) 0.11379(18) 0.0198(9) Uani 1 1 d . . . . .
H29 H 0.175260 0.053371 0.097934 0.024 Uiso 1 1 calc R . . . .
C30 C 0.3349(4) 0.1254(3) 0.09096(18) 0.0220(9) Uani 1 1 d . . . . .
C31 C 0.3885(4) 0.1954(3) 0.11430(18) 0.0203(9) Uani 1 1 d . . . . .
H31 H 0.473032 0.211918 0.100141 0.024 Uiso 1 1 calc R . . . .
C32 C 0.0103(4) 0.1079(3) 0.18397(17) 0.0167(8) Uani 1 1 d . . . . .
C33 C -0.2284(4) 0.1744(4) 0.20243(19) 0.0234(10) Uani 1 1 d . . . . .
H33 H -0.296798 0.240195 0.197052 0.028 Uiso 1 1 calc R . . . .
C34 C -0.1152(4) 0.0197(4) 0.2763(2) 0.0327(12) Uani 1 1 d . . . . .
H34 H -0.109382 -0.014950 0.319251 0.039 Uiso 1 1 calc R . . . .
C35 C -0.1607(4) -0.0080(4) 0.1809(2) 0.0274(10) Uani 1 1 d . . . . .
H35 H -0.183558 -0.060898 0.160583 0.033 Uiso 1 1 calc R . . . .
C36 C -0.0983(4) 0.2082(3) 0.17565(18) 0.0188(9) Uani 1 1 d . . . . .
H36A H -0.076215 0.262280 0.194728 0.023 Uiso 1 1 calc R . . . .
H36B H -0.104407 0.242762 0.133141 0.023 Uiso 1 1 calc R . . . .
C37 C -0.0304(4) 0.0252(4) 0.1548(2) 0.0241(9) Uani 1 1 d . . . . .
H37A H -0.035352 0.057772 0.112067 0.029 Uiso 1 1 calc R . . . .
H37B H 0.036701 -0.040344 0.159992 0.029 Uiso 1 1 calc R . . . .
C38 C -0.2185(4) 0.1220(4) 0.26834(19) 0.0305(11) Uani 1 1 d . . . . .
H38A H -0.303663 0.102196 0.286503 0.037 Uiso 1 1 calc R . . . .
H38B H -0.193942 0.174315 0.287981 0.037 Uiso 1 1 calc R . . . .
C39 C -0.1540(5) -0.0611(4) 0.2464(2) 0.0375(13) Uani 1 1 d . . . . .
H39A H -0.089062 -0.128128 0.252412 0.045 Uiso 1 1 calc R . . . .
H39B H -0.239624 -0.081244 0.263595 0.045 Uiso 1 1 calc R . . . .
C40 C 0.0161(4) 0.0518(4) 0.25001(19) 0.0250(10) Uani 1 1 d . . . . .
H40A H 0.082962 -0.013877 0.255287 0.030 Uiso 1 1 calc R . . . .
H40B H 0.041291 0.101952 0.270906 0.030 Uiso 1 1 calc R . . . .
C41 C -0.2657(4) 0.0926(4) 0.1725(2) 0.0257(10) Uani 1 1 d . . . . .
H41A H -0.273555 0.126154 0.129994 0.031 Uiso 1 1 calc R . . . .
H41B H -0.350661 0.071261 0.190009 0.031 Uiso 1 1 calc R . . . .
C42 C 0.4086(5) 0.0756(4) 0.0434(2) 0.0343(12) Uani 1 1 d . . . . .
H42A H 0.457602 0.004769 0.061372 0.051 Uiso 1 1 calc GR . . . .
H42B H 0.468888 0.123791 0.020445 0.051 Uiso 1 1 calc GR . . . .
H42C H 0.347192 0.065815 0.017412 0.051 Uiso 1 1 calc GR . . . .
C43 C 0.1274(4) 0.1653(3) 0.38089(18) 0.0213(9) Uani 1 1 d . . . . .
H43A H 0.166628 0.091046 0.401103 0.026 Uiso 1 1 calc R . . . .
H43B H 0.071660 0.157829 0.351333 0.026 Uiso 1 1 calc R . . . .
C44 C 0.0424(4) 0.2159(3) 0.42557(18) 0.0209(9) Uani 1 1 d . . . . .
C45 C -0.0231(4) 0.3225(3) 0.40769(17) 0.0173(8) Uani 1 1 d . . . . .
C46 C -0.1128(4) 0.3681(3) 0.44790(17) 0.0172(8) Uani 1 1 d . . . . .
C47 C -0.1268(4) 0.3039(3) 0.50507(18) 0.0220(9) Uani 1 1 d . . . . .
H47 H -0.185336 0.333537 0.532680 0.026 Uiso 1 1 calc R . . . .
C48 C -0.0600(4) 0.1988(4) 0.52430(18) 0.0241(10) Uani 1 1 d . . . . .
C49 C 0.0234(4) 0.1560(3) 0.48335(19) 0.0235(10) Uani 1 1 d . . . . .
H49 H 0.068834 0.084093 0.494970 0.028 Uiso 1 1 calc R . . . .
C50 C -0.1913(4) 0.4810(3) 0.42874(17) 0.0167(8) Uani 1 1 d . . . . .
C51 C -0.3499(4) 0.6007(3) 0.35639(18) 0.0208(9) Uani 1 1 d . . . . .
H51 H -0.401400 0.602857 0.322736 0.025 Uiso 1 1 calc R . . . .
C52 C -0.1784(4) 0.6819(4) 0.3884(2) 0.0266(10) Uani 1 1 d . . . . .
H52 H -0.117206 0.736644 0.375249 0.032 Uiso 1 1 calc R . . . .
C53 C -0.3636(4) 0.6254(4) 0.45851(19) 0.0250(10) Uani 1 1 d . . . . .
H53 H -0.424260 0.642523 0.491910 0.030 Uiso 1 1 calc R . . . .
C54 C -0.2736(4) 0.4866(3) 0.37689(17) 0.0182(9) Uani 1 1 d . . . . .
H54A H -0.215566 0.467684 0.343721 0.022 Uiso 1 1 calc R . . . .
H54B H -0.334783 0.432879 0.389636 0.022 Uiso 1 1 calc R . . . .
C55 C -0.2860(4) 0.5111(4) 0.47847(18) 0.0225(9) Uani 1 1 d . . . . .
H55A H -0.236724 0.508308 0.512429 0.027 Uiso 1 1 calc R . . . .
H55B H -0.346887 0.457179 0.491477 0.027 Uiso 1 1 calc R . . . .
C56 C -0.2562(4) 0.6838(4) 0.33679(19) 0.0264(10) Uani 1 1 d . . . . .
H56A H -0.305588 0.757382 0.322738 0.032 Uiso 1 1 calc R . . . .
H56B H -0.196122 0.666384 0.303857 0.032 Uiso 1 1 calc R . . . .
C57 C -0.2703(4) 0.7098(4) 0.4391(2) 0.0299(11) Uani 1 1 d . . . . .
H57A H -0.320017 0.783641 0.426120 0.036 Uiso 1 1 calc R . . . .
H57B H -0.219931 0.708849 0.472365 0.036 Uiso 1 1 calc R . . . .
C58 C -0.1005(4) 0.5685(3) 0.40875(19) 0.0224(9) Uani 1 1 d . . . . .
H58A H -0.049184 0.567094 0.441809 0.027 Uiso 1 1 calc R . . . .
H58B H -0.039092 0.551845 0.376045 0.027 Uiso 1 1 calc R . . . .
C59 C -0.4419(4) 0.6285(4) 0.40713(19) 0.0248(10) Uani 1 1 d . . . . .
H59A H -0.492267 0.701982 0.393927 0.030 Uiso 1 1 calc R . . . .
H59B H -0.503898 0.575490 0.419882 0.030 Uiso 1 1 calc R . . . .
C60 C -0.0808(5) 0.1356(4) 0.5871(2) 0.0340(11) Uani 1 1 d . . . . .
H60A H -0.028762 0.063059 0.592517 0.051 Uiso 1 1 calc GR . . . .
H60B H -0.172981 0.128347 0.596055 0.051 Uiso 1 1 calc GR . . . .
H60C H -0.054035 0.174068 0.613554 0.051 Uiso 1 1 calc GR . . . .
O100 O 0.7030(4) 0.5309(4) 0.1742(2) 0.0816(15) Uani 1 1 d D U . . .
C101 C 0.7130(9) 0.5272(8) 0.1148(4) 0.104(3) Uani 1 1 d D U . . .
H10A H 0.664799 0.470230 0.110483 0.125 Uiso 1 1 calc R . . . .
H10B H 0.805396 0.507538 0.102031 0.125 Uiso 1 1 calc R . . . .
C102 C 0.6615(8) 0.6302(8) 0.0778(4) 0.099(3) Uani 1 1 d D U . . .
H10C H 0.578965 0.625638 0.062410 0.119 Uiso 1 1 calc R . . . .
H10D H 0.724306 0.653928 0.044139 0.119 Uiso 1 1 calc R . . . .
C103 C 0.6395(8) 0.7070(7) 0.1175(4) 0.106(3) Uani 1 1 d D U . . .
H10E H 0.706674 0.755611 0.108117 0.127 Uiso 1 1 calc R . . . .
H10F H 0.552947 0.752315 0.112617 0.127 Uiso 1 1 calc R . . . .
C104 C 0.6473(8) 0.6400(6) 0.1774(4) 0.087(2) Uani 1 1 d D U . . .
H10G H 0.702407 0.668842 0.199364 0.104 Uiso 1 1 calc R . . . .
H10H H 0.559519 0.640318 0.197956 0.104 Uiso 1 1 calc R . . . .
O200 O 0.6547(12) -0.0055(9) 0.4965(5) 0.070(3) Uani 0.439(8) 1 d D U P A 1
C201 C 0.678(2) 0.0334(13) 0.4349(7) 0.059(3) Uani 0.439(8) 1 d D U P A 1
H20C H 0.602410 0.029569 0.414072 0.071 Uiso 0.439(8) 1 calc R . P A 1
H20D H 0.755915 -0.010046 0.420027 0.071 Uiso 0.439(8) 1 calc R . P A 1
C202 C 0.6977(17) 0.1450(13) 0.4263(7) 0.052(3) Uani 0.439(8) 1 d D U P A 1
H20E H 0.668359 0.189995 0.387856 0.063 Uiso 0.439(8) 1 calc R . P A 1
H20F H 0.790561 0.149592 0.428167 0.063 Uiso 0.439(8) 1 calc R . P A 1
C203 C 0.6165(16) 0.1812(12) 0.4761(7) 0.054(2) Uani 0.439(8) 1 d D U P A 1
H20G H 0.649944 0.241571 0.485731 0.065 Uiso 0.439(8) 1 calc R . P A 1
H20H H 0.524756 0.205160 0.466459 0.065 Uiso 0.439(8) 1 calc R . P A 1
C204 C 0.6293(17) 0.0832(11) 0.5249(6) 0.066(3) Uani 0.439(8) 1 d D U P A 1
H20I H 0.701970 0.082029 0.548622 0.079 Uiso 0.439(8) 1 calc R . P A 1
H20J H 0.548092 0.079673 0.550818 0.079 Uiso 0.439(8) 1 calc R . P A 1
O210 O 0.5879(7) 0.2360(6) 0.4446(3) 0.053(2) Uani 0.561(8) 1 d D U P A 2
C211 C 0.5806(12) 0.1576(9) 0.5009(5) 0.057(3) Uani 0.561(8) 1 d D U P A 2
H21C H 0.489666 0.144774 0.512535 0.069 Uiso 0.561(8) 1 calc R . P A 2
H21D H 0.611907 0.184741 0.531704 0.069 Uiso 0.561(8) 1 calc R . P A 2
C212 C 0.6629(13) 0.0567(10) 0.4941(5) 0.057(2) Uani 0.561(8) 1 d D U P A 2
H21E H 0.617916 -0.006974 0.511831 0.069 Uiso 0.561(8) 1 calc R . P A 2
H21F H 0.745608 0.046474 0.512893 0.069 Uiso 0.561(8) 1 calc R . P A 2
C213 C 0.6874(17) 0.0712(10) 0.4285(6) 0.054(2) Uani 0.561(8) 1 d D U P A 2
H21G H 0.771850 0.029659 0.418299 0.065 Uiso 0.561(8) 1 calc R . P A 2
H21H H 0.617091 0.048745 0.411731 0.065 Uiso 0.561(8) 1 calc R . P A 2
C214 C 0.6884(12) 0.1892(9) 0.4084(5) 0.049(2) Uani 0.561(8) 1 d D U P A 2
H21I H 0.773701 0.207560 0.413517 0.059 Uiso 0.561(8) 1 calc R . P A 2
H21J H 0.670159 0.215798 0.366347 0.059 Uiso 0.561(8) 1 calc R . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 O1 2.193(3) . ?
U1 O2 2.198(3) . ?
U1 O3 2.200(3) . ?
U1 O4 2.079(3) . ?
U1 N1 2.737(3) . ?
U1 N2 2.706(3) . ?
U1 N3 2.719(3) . ?
O1 C9 1.345(5) . ?
O2 C27 1.352(5) . ?
O3 C45 1.331(5) . ?
O4 H4 0.82(5) . ?
N1 C1 1.485(5) . ?
N1 C6 1.483(5) . ?
N1 C7 1.496(5) . ?
N2 C2 1.484(5) . ?
N2 C3 1.488(5) . ?
N2 C25 1.490(5) . ?
N3 C4 1.484(5) . ?
N3 C5 1.488(5) . ?
N3 C43 1.492(5) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.510(6) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C4 1.523(6) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C5 C6 1.515(6) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C7 C8 1.497(6) . ?
C8 C9 1.411(5) . ?
C8 C13 1.394(6) . ?
C9 C10 1.414(6) . ?
C10 C11 1.390(6) . ?
C10 C14 1.533(6) . ?
C11 H11 0.9500 . ?
C11 C12 1.401(6) . ?
C12 C13 1.381(6) . ?
C12 C24 1.511(6) . ?
C13 H13 0.9500 . ?
C14 C18 1.537(6) . ?
C14 C19 1.538(6) . ?
C14 C22 1.545(6) . ?
C15 H15 1.0000 . ?
C15 C18 1.543(7) . ?
C15 C20 1.519(8) . ?
C15 C23 1.523(7) . ?
C16 H16 1.0000 . ?
C16 C20 1.521(8) . ?
C16 C21 1.528(7) . ?
C16 C22 1.530(6) . ?
C17 H17 1.0000 . ?
C17 C19 1.538(6) . ?
C17 C21 1.538(8) . ?
C17 C23 1.522(8) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 C26 1.504(6) . ?
C26 C27 1.399(6) . ?
C26 C31 1.395(6) . ?
C27 C28 1.410(5) . ?
C28 C29 1.391(5) . ?
C28 C32 1.529(5) . ?
C29 H29 0.9500 . ?
C29 C30 1.387(6) . ?
C30 C31 1.388(6) . ?
C30 C42 1.507(6) . ?
C31 H31 0.9500 . ?
C32 C36 1.551(5) . ?
C32 C37 1.545(6) . ?
C32 C40 1.540(6) . ?
C33 H33 1.0000 . ?
C33 C36 1.521(6) . ?
C33 C38 1.533(6) . ?
C33 C41 1.532(6) . ?
C34 H34 1.0000 . ?
C34 C38 1.538(7) . ?
C34 C39 1.526(7) . ?
C34 C40 1.522(6) . ?
C35 H35 1.0000 . ?
C35 C37 1.516(6) . ?
C35 C39 1.522(7) . ?
C35 C41 1.532(6) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C43 C44 1.506(6) . ?
C44 C45 1.403(6) . ?
C44 C49 1.392(6) . ?
C45 C46 1.422(6) . ?
C46 C47 1.393(6) . ?
C46 C50 1.524(6) . ?
C47 H47 0.9500 . ?
C47 C48 1.396(6) . ?
C48 C49 1.384(6) . ?
C48 C60 1.505(6) . ?
C49 H49 0.9500 . ?
C50 C54 1.553(5) . ?
C50 C55 1.532(6) . ?
C50 C58 1.544(6) . ?
C51 H51 1.0000 . ?
C51 C54 1.530(6) . ?
C51 C56 1.524(6) . ?
C51 C59 1.526(6) . ?
C52 H52 1.0000 . ?
C52 C56 1.533(6) . ?
C52 C57 1.524(6) . ?
C52 C58 1.529(6) . ?
C53 H53 1.0000 . ?
C53 C55 1.536(6) . ?
C53 C57 1.534(6) . ?
C53 C59 1.526(6) . ?
C54 H54A 0.9900 . ?
C54 H54B 0.9900 . ?
C55 H55A 0.9900 . ?
C55 H55B 0.9900 . ?
C56 H56A 0.9900 . ?
C56 H56B 0.9900 . ?
C57 H57A 0.9900 . ?
C57 H57B 0.9900 . ?
C58 H58A 0.9900 . ?
C58 H58B 0.9900 . ?
C59 H59A 0.9900 . ?
C59 H59B 0.9900 . ?
C60 H60A 0.9800 . ?
C60 H60B 0.9800 . ?
C60 H60C 0.9800 . ?
O100 C101 1.406(9) . ?
O100 C104 1.441(8) . ?
C101 H10A 0.9900 . ?
C101 H10B 0.9900 . ?
C101 C102 1.437(10) . ?
C102 H10C 0.9900 . ?
C102 H10D 0.9900 . ?
C102 C103 1.503(11) . ?
C103 H10E 0.9900 . ?
C103 H10F 0.9900 . ?
C103 C104 1.454(10) . ?
C104 H10G 0.9900 . ?
C104 H10H 0.9900 . ?
O200 C201 1.416(14) . ?
O200 C204 1.440(14) . ?
C201 H20C 0.9900 . ?
C201 H20D 0.9900 . ?
C201 C202 1.446(15) . ?
C202 H20E 0.9900 . ?
C202 H20F 0.9900 . ?
C202 C203 1.496(15) . ?
C203 H20G 0.9900 . ?
C203 H20H 0.9900 . ?
C203 C204 1.468(15) . ?
C204 H20I 0.9900 . ?
C204 H20J 0.9900 . ?
O210 C211 1.448(12) . ?
O210 C214 1.430(11) . ?
C211 H21C 0.9900 . ?
C211 H21D 0.9900 . ?
C211 C212 1.464(13) . ?
C212 H21E 0.9900 . ?
C212 H21F 0.9900 . ?
C212 C213 1.506(13) . ?
C213 H21G 0.9900 . ?
C213 H21H 0.9900 . ?
C213 C214 1.470(13) . ?
C214 H21I 0.9900 . ?
C214 H21J 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 U1 O2 121.82(10) . . ?
O1 U1 O3 118.49(10) . . ?
O1 U1 N1 69.53(10) . . ?
O1 U1 N2 82.25(10) . . ?
O1 U1 N3 131.19(10) . . ?
O2 U1 O3 118.19(10) . . ?
O2 U1 N1 130.19(10) . . ?
O2 U1 N2 69.53(10) . . ?
O2 U1 N3 80.31(10) . . ?
O3 U1 N1 82.50(10) . . ?
O3 U1 N2 132.19(10) . . ?
O3 U1 N3 70.27(10) . . ?
O4 U1 O1 85.92(11) . . ?
O4 U1 O2 86.22(11) . . ?
O4 U1 O3 85.63(11) . . ?
O4 U1 N1 142.88(11) . . ?
O4 U1 N2 141.24(11) . . ?
O4 U1 N3 141.97(11) . . ?
N2 U1 N1 64.28(10) . . ?
N2 U1 N3 64.73(10) . . ?
N3 U1 N1 64.16(10) . . ?
C9 O1 U1 150.8(2) . . ?
C27 O2 U1 147.8(2) . . ?
C45 O3 U1 150.0(3) . . ?
U1 O4 H4 175(4) . . ?
C1 N1 U1 115.7(2) . . ?
C1 N1 C7 111.0(3) . . ?
C6 N1 U1 106.3(2) . . ?
C6 N1 C1 110.3(3) . . ?
C6 N1 C7 107.5(3) . . ?
C7 N1 U1 105.7(2) . . ?
C2 N2 U1 107.3(2) . . ?
C2 N2 C3 111.4(3) . . ?
C2 N2 C25 106.4(3) . . ?
C3 N2 U1 115.1(2) . . ?
C3 N2 C25 110.9(3) . . ?
C25 N2 U1 105.3(2) . . ?
C4 N3 U1 105.5(2) . . ?
C4 N3 C5 111.0(3) . . ?
C4 N3 C43 107.9(3) . . ?
C5 N3 U1 116.3(2) . . ?
C5 N3 C43 110.3(3) . . ?
C43 N3 U1 105.3(2) . . ?
N1 C1 H1A 109.0 . . ?
N1 C1 H1B 109.0 . . ?
N1 C1 C2 113.0(3) . . ?
H1A C1 H1B 107.8 . . ?
C2 C1 H1A 109.0 . . ?
C2 C1 H1B 109.0 . . ?
N2 C2 C1 113.5(3) . . ?
N2 C2 H2A 108.9 . . ?
N2 C2 H2B 108.9 . . ?
C1 C2 H2A 108.9 . . ?
C1 C2 H2B 108.9 . . ?
H2A C2 H2B 107.7 . . ?
N2 C3 H3A 108.8 . . ?
N2 C3 H3B 108.8 . . ?
N2 C3 C4 113.9(3) . . ?
H3A C3 H3B 107.7 . . ?
C4 C3 H3A 108.8 . . ?
C4 C3 H3B 108.8 . . ?
N3 C4 C3 112.6(3) . . ?
N3 C4 H4A 109.1 . . ?
N3 C4 H4B 109.1 . . ?
C3 C4 H4A 109.1 . . ?
C3 C4 H4B 109.1 . . ?
H4A C4 H4B 107.8 . . ?
N3 C5 H5A 109.0 . . ?
N3 C5 H5B 109.0 . . ?
N3 C5 C6 112.7(3) . . ?
H5A C5 H5B 107.8 . . ?
C6 C5 H5A 109.0 . . ?
C6 C5 H5B 109.0 . . ?
N1 C6 C5 112.6(3) . . ?
N1 C6 H6A 109.1 . . ?
N1 C6 H6B 109.1 . . ?
C5 C6 H6A 109.1 . . ?
C5 C6 H6B 109.1 . . ?
H6A C6 H6B 107.8 . . ?
N1 C7 H7A 108.3 . . ?
N1 C7 H7B 108.3 . . ?
N1 C7 C8 116.0(3) . . ?
H7A C7 H7B 107.4 . . ?
C8 C7 H7A 108.3 . . ?
C8 C7 H7B 108.3 . . ?
C9 C8 C7 120.1(4) . . ?
C13 C8 C7 120.1(4) . . ?
C13 C8 C9 119.6(4) . . ?
O1 C9 C8 117.9(4) . . ?
O1 C9 C10 121.9(4) . . ?
C8 C9 C10 120.2(4) . . ?
C9 C10 C14 121.2(4) . . ?
C11 C10 C9 117.1(4) . . ?
C11 C10 C14 121.7(4) . . ?
C10 C11 H11 117.9 . . ?
C10 C11 C12 124.1(4) . . ?
C12 C11 H11 117.9 . . ?
C11 C12 C24 121.3(4) . . ?
C13 C12 C11 117.1(4) . . ?
C13 C12 C24 121.6(4) . . ?
C8 C13 H13 119.1 . . ?
C12 C13 C8 121.9(4) . . ?
C12 C13 H13 119.1 . . ?
C10 C14 C18 110.9(4) . . ?
C10 C14 C19 112.3(3) . . ?
C10 C14 C22 110.1(3) . . ?
C18 C14 C19 108.3(3) . . ?
C18 C14 C22 108.0(4) . . ?
C19 C14 C22 107.0(4) . . ?
C18 C15 H15 109.2 . . ?
C20 C15 H15 109.2 . . ?
C20 C15 C18 109.7(4) . . ?
C20 C15 C23 109.8(5) . . ?
C23 C15 H15 109.2 . . ?
C23 C15 C18 109.7(4) . . ?
C20 C16 H16 109.8 . . ?
C20 C16 C21 110.2(5) . . ?
C20 C16 C22 108.3(4) . . ?
C21 C16 H16 109.8 . . ?
C21 C16 C22 108.9(4) . . ?
C22 C16 H16 109.8 . . ?
C19 C17 H17 109.2 . . ?
C21 C17 H17 109.2 . . ?
C21 C17 C19 109.3(4) . . ?
C23 C17 H17 109.2 . . ?
C23 C17 C19 109.7(4) . . ?
C23 C17 C21 110.4(4) . . ?
C14 C18 C15 110.1(4) . . ?
C14 C18 H18A 109.6 . . ?
C14 C18 H18B 109.6 . . ?
C15 C18 H18A 109.6 . . ?
C15 C18 H18B 109.6 . . ?
H18A C18 H18B 108.1 . . ?
C14 C19 C17 110.9(4) . . ?
C14 C19 H19A 109.5 . . ?
C14 C19 H19B 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
H19A C19 H19B 108.1 . . ?
C15 C20 C16 110.3(4) . . ?
C15 C20 H20A 109.6 . . ?
C15 C20 H20B 109.6 . . ?
C16 C20 H20A 109.6 . . ?
C16 C20 H20B 109.6 . . ?
H20A C20 H20B 108.1 . . ?
C16 C21 C17 108.7(4) . . ?
C16 C21 H21A 109.9 . . ?
C16 C21 H21B 109.9 . . ?
C17 C21 H21A 109.9 . . ?
C17 C21 H21B 109.9 . . ?
H21A C21 H21B 108.3 . . ?
C14 C22 H22A 109.2 . . ?
C14 C22 H22B 109.2 . . ?
C16 C22 C14 112.3(4) . . ?
C16 C22 H22A 109.2 . . ?
C16 C22 H22B 109.2 . . ?
H22A C22 H22B 107.9 . . ?
C15 C23 H23A 109.9 . . ?
C15 C23 H23B 109.9 . . ?
C17 C23 C15 108.9(4) . . ?
C17 C23 H23A 109.9 . . ?
C17 C23 H23B 109.9 . . ?
H23A C23 H23B 108.3 . . ?
C12 C24 H24A 109.5 . . ?
C12 C24 H24B 109.5 . . ?
C12 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
N2 C25 H25A 107.9 . . ?
N2 C25 H25B 107.9 . . ?
N2 C25 C26 117.8(3) . . ?
H25A C25 H25B 107.2 . . ?
C26 C25 H25A 107.9 . . ?
C26 C25 H25B 107.9 . . ?
C27 C26 C25 121.5(4) . . ?
C31 C26 C25 118.1(4) . . ?
C31 C26 C27 120.0(4) . . ?
O2 C27 C26 118.1(3) . . ?
O2 C27 C28 121.8(4) . . ?
C26 C27 C28 120.1(4) . . ?
C27 C28 C32 121.6(3) . . ?
C29 C28 C27 117.5(4) . . ?
C29 C28 C32 120.9(4) . . ?
C28 C29 H29 118.3 . . ?
C30 C29 C28 123.5(4) . . ?
C30 C29 H29 118.3 . . ?
C29 C30 C31 117.8(4) . . ?
C29 C30 C42 121.1(4) . . ?
C31 C30 C42 121.1(4) . . ?
C26 C31 H31 119.5 . . ?
C30 C31 C26 121.0(4) . . ?
C30 C31 H31 119.5 . . ?
C28 C32 C36 110.4(3) . . ?
C28 C32 C37 113.2(3) . . ?
C28 C32 C40 110.0(3) . . ?
C37 C32 C36 107.4(3) . . ?
C40 C32 C36 109.4(3) . . ?
C40 C32 C37 106.3(3) . . ?
C36 C33 H33 109.3 . . ?
C36 C33 C38 109.2(3) . . ?
C36 C33 C41 110.3(4) . . ?
C38 C33 H33 109.3 . . ?
C41 C33 H33 109.3 . . ?
C41 C33 C38 109.4(4) . . ?
C38 C34 H34 109.1 . . ?
C39 C34 H34 109.1 . . ?
C39 C34 C38 109.7(4) . . ?
C40 C34 H34 109.1 . . ?
C40 C34 C38 109.3(4) . . ?
C40 C34 C39 110.6(4) . . ?
C37 C35 H35 109.3 . . ?
C37 C35 C39 110.0(4) . . ?
C37 C35 C41 109.7(4) . . ?
C39 C35 H35 109.3 . . ?
C39 C35 C41 109.1(4) . . ?
C41 C35 H35 109.3 . . ?
C32 C36 H36A 109.5 . . ?
C32 C36 H36B 109.5 . . ?
C33 C36 C32 110.5(3) . . ?
C33 C36 H36A 109.5 . . ?
C33 C36 H36B 109.5 . . ?
H36A C36 H36B 108.1 . . ?
C32 C37 H37A 109.2 . . ?
C32 C37 H37B 109.2 . . ?
C35 C37 C32 112.0(4) . . ?
C35 C37 H37A 109.2 . . ?
C35 C37 H37B 109.2 . . ?
H37A C37 H37B 107.9 . . ?
C33 C38 C34 109.0(4) . . ?
C33 C38 H38A 109.9 . . ?
C33 C38 H38B 109.9 . . ?
C34 C38 H38A 109.9 . . ?
C34 C38 H38B 109.9 . . ?
H38A C38 H38B 108.3 . . ?
C34 C39 H39A 110.0 . . ?
C34 C39 H39B 110.0 . . ?
C35 C39 C34 108.5(4) . . ?
C35 C39 H39A 110.0 . . ?
C35 C39 H39B 110.0 . . ?
H39A C39 H39B 108.4 . . ?
C32 C40 H40A 109.5 . . ?
C32 C40 H40B 109.5 . . ?
C34 C40 C32 110.6(3) . . ?
C34 C40 H40A 109.5 . . ?
C34 C40 H40B 109.5 . . ?
H40A C40 H40B 108.1 . . ?
C33 C41 C35 109.1(3) . . ?
C33 C41 H41A 109.9 . . ?
C33 C41 H41B 109.9 . . ?
C35 C41 H41A 109.9 . . ?
C35 C41 H41B 109.9 . . ?
H41A C41 H41B 108.3 . . ?
C30 C42 H42A 109.5 . . ?
C30 C42 H42B 109.5 . . ?
C30 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
N3 C43 H43A 108.4 . . ?
N3 C43 H43B 108.4 . . ?
N3 C43 C44 115.4(3) . . ?
H43A C43 H43B 107.5 . . ?
C44 C43 H43A 108.4 . . ?
C44 C43 H43B 108.4 . . ?
C45 C44 C43 119.3(4) . . ?
C49 C44 C43 120.6(4) . . ?
C49 C44 C45 120.1(4) . . ?
O3 C45 C44 118.4(4) . . ?
O3 C45 C46 121.5(4) . . ?
C44 C45 C46 120.1(4) . . ?
C45 C46 C50 121.3(3) . . ?
C47 C46 C45 116.9(4) . . ?
C47 C46 C50 121.9(4) . . ?
C46 C47 H47 118.0 . . ?
C46 C47 C48 124.0(4) . . ?
C48 C47 H47 118.0 . . ?
C47 C48 C60 120.4(4) . . ?
C49 C48 C47 117.4(4) . . ?
C49 C48 C60 122.2(4) . . ?
C44 C49 H49 119.2 . . ?
C48 C49 C44 121.5(4) . . ?
C48 C49 H49 119.2 . . ?
C46 C50 C54 110.4(3) . . ?
C46 C50 C55 112.1(3) . . ?
C46 C50 C58 110.7(3) . . ?
C55 C50 C54 107.1(3) . . ?
C55 C50 C58 107.6(3) . . ?
C58 C50 C54 108.7(3) . . ?
C54 C51 H51 109.5 . . ?
C56 C51 H51 109.5 . . ?
C56 C51 C54 109.8(3) . . ?
C56 C51 C59 109.1(4) . . ?
C59 C51 H51 109.5 . . ?
C59 C51 C54 109.5(3) . . ?
C56 C52 H52 109.3 . . ?
C57 C52 H52 109.3 . . ?
C57 C52 C56 110.0(4) . . ?
C57 C52 C58 109.9(4) . . ?
C58 C52 H52 109.3 . . ?
C58 C52 C56 109.1(4) . . ?
C55 C53 H53 109.4 . . ?
C57 C53 H53 109.4 . . ?
C57 C53 C55 109.8(4) . . ?
C59 C53 H53 109.4 . . ?
C59 C53 C55 109.1(4) . . ?
C59 C53 C57 109.6(4) . . ?
C50 C54 H54A 109.5 . . ?
C50 C54 H54B 109.5 . . ?
C51 C54 C50 110.7(3) . . ?
C51 C54 H54A 109.5 . . ?
C51 C54 H54B 109.5 . . ?
H54A C54 H54B 108.1 . . ?
C50 C55 C53 111.5(3) . . ?
C50 C55 H55A 109.3 . . ?
C50 C55 H55B 109.3 . . ?
C53 C55 H55A 109.3 . . ?
C53 C55 H55B 109.3 . . ?
H55A C55 H55B 108.0 . . ?
C51 C56 C52 109.8(3) . . ?
C51 C56 H56A 109.7 . . ?
C51 C56 H56B 109.7 . . ?
C52 C56 H56A 109.7 . . ?
C52 C56 H56B 109.7 . . ?
H56A C56 H56B 108.2 . . ?
C52 C57 C53 108.6(4) . . ?
C52 C57 H57A 110.0 . . ?
C52 C57 H57B 110.0 . . ?
C53 C57 H57A 110.0 . . ?
C53 C57 H57B 110.0 . . ?
H57A C57 H57B 108.4 . . ?
C50 C58 H58A 109.4 . . ?
C50 C58 H58B 109.4 . . ?
C52 C58 C50 111.1(3) . . ?
C52 C58 H58A 109.4 . . ?
C52 C58 H58B 109.4 . . ?
H58A C58 H58B 108.0 . . ?
C51 C59 H59A 109.7 . . ?
C51 C59 H59B 109.7 . . ?
C53 C59 C51 109.6(3) . . ?
C53 C59 H59A 109.7 . . ?
C53 C59 H59B 109.7 . . ?
H59A C59 H59B 108.2 . . ?
C48 C60 H60A 109.5 . . ?
C48 C60 H60B 109.5 . . ?
C48 C60 H60C 109.5 . . ?
H60A C60 H60B 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
C101 O100 C104 107.8(6) . . ?
O100 C101 H10A 109.3 . . ?
O100 C101 H10B 109.3 . . ?
O100 C101 C102 111.4(8) . . ?
H10A C101 H10B 108.0 . . ?
C102 C101 H10A 109.3 . . ?
C102 C101 H10B 109.3 . . ?
C101 C102 H10C 110.9 . . ?
C101 C102 H10D 110.9 . . ?
C101 C102 C103 104.3(7) . . ?
H10C C102 H10D 108.9 . . ?
C103 C102 H10C 110.9 . . ?
C103 C102 H10D 110.9 . . ?
C102 C103 H10E 110.4 . . ?
C102 C103 H10F 110.4 . . ?
H10E C103 H10F 108.6 . . ?
C104 C103 C102 106.6(7) . . ?
C104 C103 H10E 110.4 . . ?
C104 C103 H10F 110.4 . . ?
O100 C104 C103 107.8(7) . . ?
O100 C104 H10G 110.1 . . ?
O100 C104 H10H 110.1 . . ?
C103 C104 H10G 110.1 . . ?
C103 C104 H10H 110.1 . . ?
H10G C104 H10H 108.5 . . ?
C201 O200 C204 110.8(10) . . ?
O200 C201 H20C 110.7 . . ?
O200 C201 H20D 110.7 . . ?
O200 C201 C202 105.1(12) . . ?
H20C C201 H20D 108.8 . . ?
C202 C201 H20C 110.7 . . ?
C202 C201 H20D 110.7 . . ?
C201 C202 H20E 111.0 . . ?
C201 C202 H20F 111.0 . . ?
C201 C202 C203 103.9(12) . . ?
H20E C202 H20F 109.0 . . ?
C203 C202 H20E 111.0 . . ?
C203 C202 H20F 111.0 . . ?
C202 C203 H20G 111.1 . . ?
C202 C203 H20H 111.1 . . ?
H20G C203 H20H 109.0 . . ?
C204 C203 C202 103.4(11) . . ?
C204 C203 H20G 111.1 . . ?
C204 C203 H20H 111.1 . . ?
O200 C204 C203 104.3(11) . . ?
O200 C204 H20I 110.9 . . ?
O200 C204 H20J 110.9 . . ?
C203 C204 H20I 110.9 . . ?
C203 C204 H20J 110.9 . . ?
H20I C204 H20J 108.9 . . ?
C214 O210 C211 106.9(8) . . ?
O210 C211 H21C 110.3 . . ?
O210 C211 H21D 110.3 . . ?
O210 C211 C212 107.0(9) . . ?
H21C C211 H21D 108.6 . . ?
C212 C211 H21C 110.3 . . ?
C212 C211 H21D 110.3 . . ?
C211 C212 H21E 110.8 . . ?
C211 C212 H21F 110.8 . . ?
C211 C212 C213 104.6(10) . . ?
H21E C212 H21F 108.9 . . ?
C213 C212 H21E 110.8 . . ?
C213 C212 H21F 110.8 . . ?
C212 C213 H21G 111.5 . . ?
C212 C213 H21H 111.5 . . ?
H21G C213 H21H 109.3 . . ?
C214 C213 C212 101.5(10) . . ?
C214 C213 H21G 111.5 . . ?
C214 C213 H21H 111.5 . . ?
O210 C214 C213 104.9(9) . . ?
O210 C214 H21I 110.8 . . ?
O210 C214 H21J 110.8 . . ?
C213 C214 H21I 110.8 . . ?
C213 C214 H21J 110.8 . . ?
H21I C214 H21J 108.8 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O4 H4 O100 0.82(5) 2.03(5) 2.840(5) 174(5) 1_455

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
U1 O1 C9 C8 -5.3(7) . . . . ?
U1 O1 C9 C10 174.1(3) . . . . ?
U1 O2 C27 C26 14.5(7) . . . . ?
U1 O2 C27 C28 -164.8(3) . . . . ?
U1 O3 C45 C44 -10.2(7) . . . . ?
U1 O3 C45 C46 170.1(3) . . . . ?
U1 N1 C1 C2 10.0(4) . . . . ?
U1 N1 C6 C5 59.8(4) . . . . ?
U1 N1 C7 C8 -76.0(3) . . . . ?
U1 N2 C2 C1 58.7(4) . . . . ?
U1 N2 C3 C4 6.8(4) . . . . ?
U1 N2 C25 C26 -73.7(4) . . . . ?
U1 N3 C4 C3 59.7(3) . . . . ?
U1 N3 C5 C6 11.7(4) . . . . ?
U1 N3 C43 C44 -77.1(3) . . . . ?
O1 C9 C10 C11 -179.5(4) . . . . ?
O1 C9 C10 C14 1.0(6) . . . . ?
O2 C27 C28 C29 176.6(3) . . . . ?
O2 C27 C28 C32 -4.2(6) . . . . ?
O3 C45 C46 C47 -177.7(4) . . . . ?
O3 C45 C46 C50 3.3(6) . . . . ?
N1 C1 C2 N2 -47.2(5) . . . . ?
N1 C7 C8 C9 54.2(5) . . . . ?
N1 C7 C8 C13 -130.2(4) . . . . ?
N2 C3 C4 N3 -46.4(5) . . . . ?
N2 C25 C26 C27 48.1(5) . . . . ?
N2 C25 C26 C31 -139.0(4) . . . . ?
N3 C5 C6 N1 -49.5(5) . . . . ?
N3 C43 C44 C45 57.3(5) . . . . ?
N3 C43 C44 C49 -125.9(4) . . . . ?
C1 N1 C6 C5 -66.3(4) . . . . ?
C1 N1 C7 C8 50.1(4) . . . . ?
C2 N2 C3 C4 129.1(4) . . . . ?
C2 N2 C25 C26 172.7(3) . . . . ?
C3 N2 C2 C1 -68.1(4) . . . . ?
C3 N2 C25 C26 51.4(5) . . . . ?
C4 N3 C5 C6 132.3(4) . . . . ?
C4 N3 C43 C44 170.5(3) . . . . ?
C5 N3 C4 C3 -67.1(4) . . . . ?
C5 N3 C43 C44 49.1(4) . . . . ?
C6 N1 C1 C2 130.7(4) . . . . ?
C6 N1 C7 C8 170.8(3) . . . . ?
C7 N1 C1 C2 -110.4(4) . . . . ?
C7 N1 C6 C5 172.6(3) . . . . ?
C7 C8 C9 O1 -4.5(6) . . . . ?
C7 C8 C9 C10 176.1(4) . . . . ?
C7 C8 C13 C12 -176.4(4) . . . . ?
C8 C9 C10 C11 -0.1(6) . . . . ?
C8 C9 C10 C14 -179.6(4) . . . . ?
C9 C8 C13 C12 -0.9(6) . . . . ?
C9 C10 C11 C12 -0.1(6) . . . . ?
C9 C10 C14 C18 59.8(5) . . . . ?
C9 C10 C14 C19 -178.8(4) . . . . ?
C9 C10 C14 C22 -59.6(5) . . . . ?
C10 C11 C12 C13 -0.2(6) . . . . ?
C10 C11 C12 C24 179.2(4) . . . . ?
C10 C14 C18 C15 -177.9(4) . . . . ?
C10 C14 C19 C17 179.0(4) . . . . ?
C10 C14 C22 C16 179.4(4) . . . . ?
C11 C10 C14 C18 -119.7(4) . . . . ?
C11 C10 C14 C19 1.7(6) . . . . ?
C11 C10 C14 C22 120.8(4) . . . . ?
C11 C12 C13 C8 0.7(6) . . . . ?
C13 C8 C9 O1 180.0(4) . . . . ?
C13 C8 C9 C10 0.5(6) . . . . ?
C14 C10 C11 C12 179.5(4) . . . . ?
C18 C14 C19 C17 -58.1(5) . . . . ?
C18 C14 C22 C16 58.2(5) . . . . ?
C18 C15 C20 C16 -61.0(6) . . . . ?
C18 C15 C23 C17 60.9(6) . . . . ?
C19 C14 C18 C15 58.4(5) . . . . ?
C19 C14 C22 C16 -58.3(5) . . . . ?
C19 C17 C21 C16 61.2(6) . . . . ?
C19 C17 C23 C15 -60.2(6) . . . . ?
C20 C15 C18 C14 59.9(5) . . . . ?
C20 C15 C23 C17 -59.8(6) . . . . ?
C20 C16 C21 C17 58.3(5) . . . . ?
C20 C16 C22 C14 -59.3(5) . . . . ?
C21 C16 C20 C15 -59.2(5) . . . . ?
C21 C16 C22 C14 60.4(6) . . . . ?
C21 C17 C19 C14 -61.4(5) . . . . ?
C21 C17 C23 C15 60.3(6) . . . . ?
C22 C14 C18 C15 -57.2(5) . . . . ?
C22 C14 C19 C17 58.1(5) . . . . ?
C22 C16 C20 C15 59.8(5) . . . . ?
C22 C16 C21 C17 -60.2(6) . . . . ?
C23 C15 C18 C14 -60.7(6) . . . . ?
C23 C15 C20 C16 59.6(5) . . . . ?
C23 C17 C19 C14 59.7(5) . . . . ?
C23 C17 C21 C16 -59.5(5) . . . . ?
C24 C12 C13 C8 -178.8(4) . . . . ?
C25 N2 C2 C1 171.0(3) . . . . ?
C25 N2 C3 C4 -112.6(4) . . . . ?
C25 C26 C27 O2 -5.6(6) . . . . ?
C25 C26 C27 C28 173.7(4) . . . . ?
C25 C26 C31 C30 -171.7(4) . . . . ?
C26 C27 C28 C29 -2.7(6) . . . . ?
C26 C27 C28 C32 176.6(3) . . . . ?
C27 C26 C31 C30 1.2(6) . . . . ?
C27 C28 C29 C30 2.3(6) . . . . ?
C27 C28 C32 C36 60.5(5) . . . . ?
C27 C28 C32 C37 -179.0(4) . . . . ?
C27 C28 C32 C40 -60.3(5) . . . . ?
C28 C29 C30 C31 -0.2(6) . . . . ?
C28 C29 C30 C42 178.4(4) . . . . ?
C28 C32 C36 C33 -178.3(3) . . . . ?
C28 C32 C37 C35 179.8(3) . . . . ?
C28 C32 C40 C34 178.4(4) . . . . ?
C29 C28 C32 C36 -120.3(4) . . . . ?
C29 C28 C32 C37 0.2(5) . . . . ?
C29 C28 C32 C40 118.9(4) . . . . ?
C29 C30 C31 C26 -1.6(6) . . . . ?
C31 C26 C27 O2 -178.3(3) . . . . ?
C31 C26 C27 C28 1.0(6) . . . . ?
C32 C28 C29 C30 -176.9(4) . . . . ?
C36 C32 C37 C35 -58.0(4) . . . . ?
C36 C32 C40 C34 56.9(5) . . . . ?
C36 C33 C38 C34 -61.6(5) . . . . ?
C36 C33 C41 C35 59.8(5) . . . . ?
C37 C32 C36 C33 57.8(4) . . . . ?
C37 C32 C40 C34 -58.7(5) . . . . ?
C37 C35 C39 C34 58.3(5) . . . . ?
C37 C35 C41 C33 -58.7(5) . . . . ?
C38 C33 C36 C32 59.8(4) . . . . ?
C38 C33 C41 C35 -60.3(5) . . . . ?
C38 C34 C39 C35 61.3(5) . . . . ?
C38 C34 C40 C32 -59.6(5) . . . . ?
C39 C34 C38 C33 -60.0(5) . . . . ?
C39 C34 C40 C32 61.4(5) . . . . ?
C39 C35 C37 C32 -60.4(5) . . . . ?
C39 C35 C41 C33 61.8(5) . . . . ?
C40 C32 C36 C33 -57.1(4) . . . . ?
C40 C32 C37 C35 59.0(4) . . . . ?
C40 C34 C38 C33 61.4(5) . . . . ?
C40 C34 C39 C35 -59.3(5) . . . . ?
C41 C33 C36 C32 -60.5(4) . . . . ?
C41 C33 C38 C34 59.2(5) . . . . ?
C41 C35 C37 C32 59.6(5) . . . . ?
C41 C35 C39 C34 -62.1(5) . . . . ?
C42 C30 C31 C26 179.8(4) . . . . ?
C43 N3 C4 C3 171.9(3) . . . . ?
C43 N3 C5 C6 -108.1(4) . . . . ?
C43 C44 C45 O3 -5.4(6) . . . . ?
C43 C44 C45 C46 174.3(4) . . . . ?
C43 C44 C49 C48 -176.3(4) . . . . ?
C44 C45 C46 C47 2.7(6) . . . . ?
C44 C45 C46 C50 -176.3(4) . . . . ?
C45 C44 C49 C48 0.4(6) . . . . ?
C45 C46 C47 C48 -0.9(6) . . . . ?
C45 C46 C50 C54 58.0(5) . . . . ?
C45 C46 C50 C55 177.3(3) . . . . ?
C45 C46 C50 C58 -62.4(5) . . . . ?
C46 C47 C48 C49 -1.0(6) . . . . ?
C46 C47 C48 C60 179.7(4) . . . . ?
C46 C50 C54 C51 -178.5(3) . . . . ?
C46 C50 C55 C53 179.6(3) . . . . ?
C46 C50 C58 C52 179.0(3) . . . . ?
C47 C46 C50 C54 -120.9(4) . . . . ?
C47 C46 C50 C55 -1.6(5) . . . . ?
C47 C46 C50 C58 118.7(4) . . . . ?
C47 C48 C49 C44 1.3(6) . . . . ?
C49 C44 C45 O3 177.8(4) . . . . ?
C49 C44 C45 C46 -2.5(6) . . . . ?
C50 C46 C47 C48 178.1(4) . . . . ?
C54 C50 C55 C53 -59.1(4) . . . . ?
C54 C50 C58 C52 57.6(4) . . . . ?
C54 C51 C56 C52 -60.6(5) . . . . ?
C54 C51 C59 C53 60.0(4) . . . . ?
C55 C50 C54 C51 59.1(4) . . . . ?
C55 C50 C58 C52 -58.1(4) . . . . ?
C55 C53 C57 C52 59.6(5) . . . . ?
C55 C53 C59 C51 -59.4(5) . . . . ?
C56 C51 C54 C50 59.1(4) . . . . ?
C56 C51 C59 C53 -60.1(5) . . . . ?
C56 C52 C57 C53 59.8(5) . . . . ?
C56 C52 C58 C50 -59.8(5) . . . . ?
C57 C52 C56 C51 -60.0(5) . . . . ?
C57 C52 C58 C50 60.9(5) . . . . ?
C57 C53 C55 C50 -59.8(4) . . . . ?
C57 C53 C59 C51 60.9(5) . . . . ?
C58 C50 C54 C51 -56.9(4) . . . . ?
C58 C50 C55 C53 57.6(4) . . . . ?
C58 C52 C56 C51 60.6(5) . . . . ?
C58 C52 C57 C53 -60.3(5) . . . . ?
C59 C51 C54 C50 -60.6(4) . . . . ?
C59 C51 C56 C52 59.4(5) . . . . ?
C59 C53 C55 C50 60.4(5) . . . . ?
C59 C53 C57 C52 -60.3(5) . . . . ?
C60 C48 C49 C44 -179.5(4) . . . . ?
O100 C101 C102 C103 10.0(10) . . . . ?
C101 O100 C104 C103 -7.6(9) . . . . ?
C101 C102 C103 C104 -14.2(10) . . . . ?
C102 C103 C104 O100 13.6(9) . . . . ?
C104 O100 C101 C102 -1.8(10) . . . . ?
O200 C201 C202 C203 -30.1(19) . . . . ?
C201 O200 C204 C203 9.1(19) . . . . ?
C201 C202 C203 C204 35.7(18) . . . . ?
C202 C203 C204 O200 -27.2(17) . . . . ?
C204 O200 C201 C202 13(2) . . . . ?
O210 C211 C212 C213 -14.9(14) . . . . ?
C211 O210 C214 C213 30.7(13) . . . . ?
C211 C212 C213 C214 32.6(14) . . . . ?
C212 C213 C214 O210 -38.9(13) . . . . ?
C214 O210 C211 C212 -9.4(13) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'

# start Validation Reply Form
_vrf_PLAT971_mr1522              
;
PROBLEM: Check Calcd Resid. Dens.  1.38A   From C13             3.25 eA-3  
RESPONSE: This residual density maximum seems to be an artefact as it is 
located very close to the hydrogen atom of a ligand's phenyl ring. It has 
no chemical significance nor could it be attributed to disorder. All further 
remaining residual density maxima are lower than 0.93 eA-3.
;
_vrf_PLAT972_mr1522              
;
PROBLEM: Check Calcd Resid. Dens.  2.37A   From C104           -2.68 eA-3  
RESPONSE: This negative electron density is in the region of the THF solvent
molecules, one of which is strongly dsiordered. It has no chemical significance.
;
####################################################################### 
# 
# 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_mr1529
_database_code_depnum_ccdc_archive 'CCDC 1893562'
loop_
_audit_author_name
_audit_author_address
'Frank W. Heinemann'
;Friedrich-Alexander-Universit?t Erlangen-N?rnberg
Germany
;
_audit_update_record             
;
2019-01-25 deposited with the CCDC.	2019-03-25 downloaded from the CCDC.
;
_audit_creation_date             2019-01-24
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C60 H78 N3 O3 Se1 U1, C18 H36 K1 N2 O6'
_chemical_formula_sum            'C78 H114 K N5 O9 Se U'
_chemical_formula_weight         1621.83
_chemical_absolute_configuration ad
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      hexagonal
_space_group_IT_number           173
_space_group_name_H-M_alt        'P 63'
_space_group_name_Hall           'P 6c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'

_cell_length_a                   14.920(2)
_cell_length_b                   14.920(2)
_cell_length_c                   19.254(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     3711.9(13)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    3851
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.37
_cell_measurement_theta_min      2.64
_shelx_estimated_absorpt_T_max   0.787
_shelx_estimated_absorpt_T_min   0.648
_exptl_absorpt_coefficient_mu    2.792
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.5972
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.1092 before and 0.0786 after correction.
The Ratio of minimum to maximum transmission is 0.8008.
The λ/2 correction factor is 0.00150.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.451
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1668
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0934
_diffrn_reflns_av_unetI/netI     0.0846
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            32183
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.718
_diffrn_reflns_theta_min         1.898
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_radiation_source         'ImuS micro-focus tube'
_diffrn_radiation_monochromator  'Quazar focussing montel optics'
_diffrn_measurement_device_type  'Bruker Kappa APEX II CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 83.33
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_reflns_Friedel_coverage         0.943
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                4280
_reflns_number_total             6397
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELX XT 2014/5 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2015)'
_computing_molecular_graphics    'SHELXTL 6.12 (Bruker AXS, 2002)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_refine_diff_density_max         0.898
_refine_diff_density_min         -0.784
_refine_diff_density_rms         0.096
_refine_ls_abs_structure_details 
;
 Flack x determined using 1751 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.007(6)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.975
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     287
_refine_ls_number_reflns         6397
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0741
_refine_ls_R_factor_gt           0.0349
_refine_ls_restrained_S_all      0.975
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w=1/[σ²(Fo²)] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0632
_refine_ls_wR_factor_ref         0.0735
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H22A,H22B} of C22, {H23A,H23B} of C23, {H25A,H25B} of C25,
   {H26A,H26B} of C26, {H24A,H24B} of C24, {H21A,H21B} of C21, {H19A,H19B} of
  C19, {H14A,H14B} of C14, {H3A,H3B} of C3, {H16A,H16B} of C16, {H18A,H18B} of
  C18, {H17A,H17B} of C17, {H15A,H15B} of C15
 At 1.5 times of:
  All C(H,H,H) groups, {H1A,H1B} of C1, {H2A,H2B} of C2
2.a Ternary CH refined with riding coordinates:
 C11(H11), C12(H12), C13(H13)
2.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C14(H14A,H14B), C15(H15A,H15B),
 C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B), C21(H21A,H21B),
  C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B), C26(H26A,H26B)
2.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C9(H9)
2.d Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.000000 0.000000 0.74768(2) 0.01199(9) Uani 1 3 d S T P . .
Se1 Se 0.000000 0.000000 0.88763(5) 0.0177(2) Uani 1 3 d S T P . .
O1 O -0.0187(3) 0.1379(3) 0.7537(3) 0.0163(9) Uani 1 1 d . . . . .
N1 N -0.1028(4) 0.0162(4) 0.6302(3) 0.0124(12) Uani 1 1 d . . . . .
C1 C -0.1619(5) -0.0890(5) 0.6006(3) 0.0158(14) Uani 1 1 d . . . . .
H1A H -0.203907 -0.088162 0.561131 0.024 Uiso 1 1 calc R . . . .
H1B H -0.209832 -0.136564 0.636321 0.024 Uiso 1 1 calc R . . . .
C2 C -0.0368(5) 0.0924(5) 0.5759(3) 0.0147(14) Uani 1 1 d . . . . .
H2A H -0.067477 0.135453 0.562843 0.022 Uiso 1 1 calc R . . . .
H2B H -0.035784 0.054509 0.533973 0.022 Uiso 1 1 calc R . . . .
C3 C -0.1787(5) 0.0438(5) 0.6586(3) 0.0143(14) Uani 1 1 d . . . . .
H3A H -0.210946 0.001813 0.700726 0.017 Uiso 1 1 calc R . . . .
H3B H -0.234165 0.025525 0.623915 0.017 Uiso 1 1 calc R . . . .
C4 C -0.1319(6) 0.1568(6) 0.6770(3) 0.0160(16) Uani 1 1 d . . . . .
C5 C -0.0548(5) 0.1977(5) 0.7294(3) 0.0172(16) Uani 1 1 d . . . . .
C6 C -0.0181(4) 0.3004(4) 0.7529(4) 0.0130(12) Uani 1 1 d . . . . .
C7 C -0.0487(6) 0.3603(6) 0.7149(3) 0.0199(15) Uani 1 1 d . . . . .
H7 H -0.021912 0.430341 0.728458 0.024 Uiso 1 1 calc R . . . .
C8 C -0.1158(6) 0.3239(6) 0.6583(4) 0.0199(16) Uani 1 1 d . . . . .
C9 C -0.1608(6) 0.2190(6) 0.6427(3) 0.0191(17) Uani 1 1 d . . . . .
H9 H -0.212458 0.189982 0.607665 0.023 Uiso 1 1 calc R . . . .
C10 C 0.0475(5) 0.3415(5) 0.8185(4) 0.0159(13) Uani 1 1 d . . . . .
C11 C 0.2194(6) 0.3939(6) 0.8755(4) 0.0206(17) Uani 1 1 d . . . . .
H11 H 0.289729 0.402864 0.868081 0.025 Uiso 1 1 calc R . . . .
C12 C 0.0563(5) 0.3018(5) 0.9461(3) 0.0165(14) Uani 1 1 d . . . . .
H12 H 0.019863 0.250086 0.983854 0.020 Uiso 1 1 calc R . . . .
C13 C 0.1226(6) 0.4848(6) 0.9079(4) 0.0216(16) Uani 1 1 d . . . . .
H13 H 0.129886 0.553042 0.921030 0.026 Uiso 1 1 calc R . . . .
C14 C 0.1568(5) 0.3549(5) 0.8087(3) 0.0171(15) Uani 1 1 d . . . . .
H14A H 0.150178 0.287768 0.795486 0.021 Uiso 1 1 calc R . . . .
H14B H 0.193300 0.404852 0.770712 0.021 Uiso 1 1 calc R . . . .
C15 C 0.0613(6) 0.4471(5) 0.8404(3) 0.0197(15) Uani 1 1 d . . . . .
H15A H 0.098047 0.498423 0.803186 0.024 Uiso 1 1 calc R . . . .
H15B H -0.007537 0.440634 0.846639 0.024 Uiso 1 1 calc R . . . .
C16 C 0.1635(5) 0.3136(6) 0.9336(3) 0.0172(16) Uani 1 1 d . . . . .
H16A H 0.155739 0.246155 0.919902 0.021 Uiso 1 1 calc R . . . .
H16B H 0.204735 0.336659 0.976887 0.021 Uiso 1 1 calc R . . . .
C17 C 0.0670(6) 0.4064(5) 0.9667(4) 0.0246(17) Uani 1 1 d . . . . .
H17A H -0.002277 0.398126 0.974655 0.029 Uiso 1 1 calc R . . . .
H17B H 0.107301 0.431669 1.010288 0.029 Uiso 1 1 calc R . . . .
C18 C -0.0063(5) 0.2643(5) 0.8792(3) 0.0144(14) Uani 1 1 d . . . . .
H18A H -0.075821 0.255604 0.886943 0.017 Uiso 1 1 calc R . . . .
H18B H -0.015307 0.196025 0.866410 0.017 Uiso 1 1 calc R . . . .
C19 C 0.2302(6) 0.4979(6) 0.8970(4) 0.0266(19) Uani 1 1 d . . . . .
H19A H 0.270696 0.522486 0.940490 0.032 Uiso 1 1 calc R . . . .
H19B H 0.267395 0.550129 0.860362 0.032 Uiso 1 1 calc R . . . .
C20 C -0.1428(7) 0.3947(6) 0.6178(4) 0.033(2) Uani 1 1 d . . . . .
H20A H -0.207802 0.352843 0.592612 0.049 Uiso 1 1 calc GR . . . .
H20B H -0.087295 0.435644 0.584666 0.049 Uiso 1 1 calc GR . . . .
H20C H -0.150647 0.441142 0.650019 0.049 Uiso 1 1 calc GR . . . .
K1 K 0.666667 0.333333 0.97497(13) 0.0211(6) Uani 1 3 d S T P . .
O2 O 0.8031(5) 0.5163(4) 0.9045(3) 0.0358(15) Uani 1 1 d . . . . .
O3 O 0.8285(5) 0.5055(5) 1.0476(3) 0.0452(17) Uani 1 1 d . . . . .
N2 N 0.666667 0.333333 0.8244(6) 0.033(3) Uani 1 3 d S T P . .
N3 N 0.666667 0.333333 1.1302(5) 0.052(4) Uani 1 3 d S T P . .
C21 C 0.7123(7) 0.4400(7) 0.7993(4) 0.043(2) Uani 1 1 d . . . . .
H21A H 0.663627 0.465282 0.809165 0.051 Uiso 1 1 calc R . . . .
H21B H 0.720307 0.440016 0.748232 0.051 Uiso 1 1 calc R . . . .
C22 C 0.8181(7) 0.5159(7) 0.8314(4) 0.041(2) Uani 1 1 d . . . . .
H22A H 0.868800 0.493292 0.821181 0.049 Uiso 1 1 calc R . . . .
H22B H 0.844489 0.586136 0.812108 0.049 Uiso 1 1 calc R . . . .
C23 C 0.8974(7) 0.5888(7) 0.9376(5) 0.046(3) Uani 1 1 d . . . . .
H23A H 0.928651 0.656243 0.913212 0.055 Uiso 1 1 calc R . . . .
H23B H 0.947264 0.563379 0.936385 0.055 Uiso 1 1 calc R . . . .
C24 C 0.8730(6) 0.6009(6) 1.0107(6) 0.054(3) Uani 1 1 d . . . . .
H24A H 0.937246 0.652215 1.034445 0.064 Uiso 1 1 calc R . . . .
H24B H 0.824184 0.627634 1.011084 0.064 Uiso 1 1 calc R . . . .
C25 C 0.8033(9) 0.5183(9) 1.1169(5) 0.064(3) Uani 1 1 d . . . . .
H25A H 0.747758 0.536209 1.116545 0.077 Uiso 1 1 calc R . . . .
H25B H 0.864821 0.575056 1.140030 0.077 Uiso 1 1 calc R . . . .
C26 C 0.7679(9) 0.4186(9) 1.1553(5) 0.070(4) Uani 1 1 d . . . . .
H26A H 0.820709 0.397468 1.150183 0.084 Uiso 1 1 calc R . . . .
H26B H 0.762053 0.430190 1.205310 0.084 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 Se1 2.6947(11) . ?
U1 O1 2.213(4) . ?
U1 O1 2.213(4) 2 ?
U1 O1 2.213(4) 3 ?
U1 N1 2.811(5) 2 ?
U1 N1 2.811(5) 3 ?
U1 N1 2.811(5) . ?
O1 C5 1.337(8) . ?
N1 C1 1.476(8) . ?
N1 C2 1.495(8) . ?
N1 C3 1.489(8) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.511(8) 2 ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C4 1.509(10) . ?
C4 C5 1.418(9) . ?
C4 C9 1.372(10) . ?
C5 C6 1.418(9) . ?
C6 C7 1.397(9) . ?
C6 C10 1.526(9) . ?
C7 H7 0.9500 . ?
C7 C8 1.393(9) . ?
C8 C9 1.393(10) . ?
C8 C20 1.519(9) . ?
C9 H9 0.9500 . ?
C10 C14 1.551(8) . ?
C10 C15 1.541(8) . ?
C10 C18 1.553(9) . ?
C11 H11 1.0000 . ?
C11 C14 1.525(9) . ?
C11 C16 1.543(9) . ?
C11 C19 1.534(10) . ?
C12 H12 1.0000 . ?
C12 C16 1.537(9) . ?
C12 C17 1.540(9) . ?
C12 C18 1.524(8) . ?
C13 H13 1.0000 . ?
C13 C15 1.527(9) . ?
C13 C17 1.539(10) . ?
C13 C19 1.532(10) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
K1 O2 2.807(6) 3_665 ?
K1 O2 2.807(6) 2_655 ?
K1 O2 2.807(6) . ?
K1 O3 2.860(6) . ?
K1 O3 2.860(6) 2_655 ?
K1 O3 2.860(6) 3_665 ?
K1 N2 2.898(12) . ?
K1 N3 2.990(11) . ?
O2 C22 1.425(9) . ?
O2 C23 1.426(10) . ?
O3 C24 1.424(10) . ?
O3 C25 1.424(11) . ?
N2 C21 1.465(9) 3_665 ?
N2 C21 1.465(9) . ?
N2 C21 1.465(9) 2_655 ?
N3 C26 1.487(10) . ?
N3 C26 1.487(10) 2_655 ?
N3 C26 1.487(10) 3_665 ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C21 C22 1.539(12) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C23 C24 1.488(12) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 C26 1.501(15) . ?
C26 H26A 0.9900 . ?
C26 H26B 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
Se1 U1 N1 143.60(11) . 3 ?
Se1 U1 N1 143.60(11) . 2 ?
Se1 U1 N1 143.60(11) . . ?
O1 U1 Se1 86.99(15) . . ?
O1 U1 Se1 86.99(15) 2 . ?
O1 U1 Se1 86.99(15) 3 . ?
O1 U1 O1 119.73(3) 2 3 ?
O1 U1 O1 119.73(3) . 3 ?
O1 U1 O1 119.73(3) . 2 ?
O1 U1 N1 82.75(18) . 3 ?
O1 U1 N1 68.56(18) . . ?
O1 U1 N1 128.21(18) 2 3 ?
O1 U1 N1 128.21(18) . 2 ?
O1 U1 N1 68.56(18) 2 2 ?
O1 U1 N1 68.56(18) 3 3 ?
O1 U1 N1 82.75(18) 2 . ?
O1 U1 N1 128.22(18) 3 . ?
O1 U1 N1 82.75(17) 3 2 ?
N1 U1 N1 61.86(18) . 2 ?
N1 U1 N1 61.86(18) 2 3 ?
N1 U1 N1 61.86(18) . 3 ?
C5 O1 U1 151.9(5) . . ?
C1 N1 U1 106.3(4) . . ?
C1 N1 C2 110.8(5) . . ?
C1 N1 C3 107.7(5) . . ?
C2 N1 U1 116.6(4) . . ?
C3 N1 U1 104.5(3) . . ?
C3 N1 C2 110.5(5) . . ?
N1 C1 H1A 109.1 . . ?
N1 C1 H1B 109.1 . . ?
N1 C1 C2 112.3(5) . 2 ?
H1A C1 H1B 107.9 . . ?
C2 C1 H1A 109.1 2 . ?
C2 C1 H1B 109.1 2 . ?
N1 C2 C1 112.2(5) . 3 ?
N1 C2 H2A 109.2 . . ?
N1 C2 H2B 109.2 . . ?
C1 C2 H2A 109.2 3 . ?
C1 C2 H2B 109.2 3 . ?
H2A C2 H2B 107.9 . . ?
N1 C3 H3A 108.8 . . ?
N1 C3 H3B 108.8 . . ?
N1 C3 C4 113.9(6) . . ?
H3A C3 H3B 107.7 . . ?
C4 C3 H3A 108.8 . . ?
C4 C3 H3B 108.8 . . ?
C5 C4 C3 118.0(6) . . ?
C9 C4 C3 121.1(6) . . ?
C9 C4 C5 120.9(7) . . ?
O1 C5 C4 118.2(6) . . ?
O1 C5 C6 122.8(6) . . ?
C4 C5 C6 118.9(6) . . ?
C5 C6 C10 121.5(6) . . ?
C7 C6 C5 116.8(6) . . ?
C7 C6 C10 121.7(6) . . ?
C6 C7 H7 117.9 . . ?
C8 C7 C6 124.2(7) . . ?
C8 C7 H7 117.9 . . ?
C7 C8 C20 121.3(7) . . ?
C9 C8 C7 117.1(6) . . ?
C9 C8 C20 121.6(7) . . ?
C4 C9 C8 121.2(7) . . ?
C4 C9 H9 119.4 . . ?
C8 C9 H9 119.4 . . ?
C6 C10 C14 111.9(5) . . ?
C6 C10 C15 111.6(5) . . ?
C6 C10 C18 109.5(5) . . ?
C14 C10 C18 107.9(5) . . ?
C15 C10 C14 107.9(5) . . ?
C15 C10 C18 107.9(6) . . ?
C14 C11 H11 109.4 . . ?
C14 C11 C16 109.0(6) . . ?
C14 C11 C19 110.3(6) . . ?
C16 C11 H11 109.4 . . ?
C19 C11 H11 109.4 . . ?
C19 C11 C16 109.4(6) . . ?
C16 C12 H12 109.6 . . ?
C16 C12 C17 110.4(6) . . ?
C17 C12 H12 109.6 . . ?
C18 C12 H12 109.6 . . ?
C18 C12 C16 108.8(5) . . ?
C18 C12 C17 108.9(5) . . ?
C15 C13 H13 109.3 . . ?
C15 C13 C17 110.5(6) . . ?
C15 C13 C19 109.0(6) . . ?
C17 C13 H13 109.3 . . ?
C19 C13 H13 109.3 . . ?
C19 C13 C17 109.2(6) . . ?
C10 C14 H14A 109.5 . . ?
C10 C14 H14B 109.5 . . ?
C11 C14 C10 110.5(5) . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
H14A C14 H14B 108.1 . . ?
C10 C15 H15A 109.4 . . ?
C10 C15 H15B 109.4 . . ?
C13 C15 C10 111.1(6) . . ?
C13 C15 H15A 109.4 . . ?
C13 C15 H15B 109.4 . . ?
H15A C15 H15B 108.0 . . ?
C11 C16 H16A 109.8 . . ?
C11 C16 H16B 109.8 . . ?
C12 C16 C11 109.3(6) . . ?
C12 C16 H16A 109.8 . . ?
C12 C16 H16B 109.8 . . ?
H16A C16 H16B 108.3 . . ?
C12 C17 H17A 109.9 . . ?
C12 C17 H17B 109.9 . . ?
C13 C17 C12 108.9(5) . . ?
C13 C17 H17A 109.9 . . ?
C13 C17 H17B 109.9 . . ?
H17A C17 H17B 108.3 . . ?
C10 C18 H18A 109.3 . . ?
C10 C18 H18B 109.3 . . ?
C12 C18 C10 111.7(5) . . ?
C12 C18 H18A 109.3 . . ?
C12 C18 H18B 109.3 . . ?
H18A C18 H18B 107.9 . . ?
C11 C19 H19A 109.8 . . ?
C11 C19 H19B 109.8 . . ?
C13 C19 C11 109.6(6) . . ?
C13 C19 H19A 109.8 . . ?
C13 C19 H19B 109.8 . . ?
H19A C19 H19B 108.2 . . ?
C8 C20 H20A 109.5 . . ?
C8 C20 H20B 109.5 . . ?
C8 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O2 K1 O2 98.60(17) 3_665 . ?
O2 K1 O2 98.60(17) 3_665 2_655 ?
O2 K1 O2 98.60(17) . 2_655 ?
O2 K1 O3 59.14(18) 3_665 3_665 ?
O2 K1 O3 59.14(18) . . ?
O2 K1 O3 118.94(17) . 2_655 ?
O2 K1 O3 137.58(17) . 3_665 ?
O2 K1 O3 137.58(17) 3_665 2_655 ?
O2 K1 O3 118.93(17) 2_655 3_665 ?
O2 K1 O3 59.14(18) 2_655 2_655 ?
O2 K1 O3 118.94(17) 3_665 . ?
O2 K1 O3 137.58(17) 2_655 . ?
O2 K1 N2 61.10(13) . . ?
O2 K1 N2 61.10(13) 2_655 . ?
O2 K1 N2 61.10(13) 3_665 . ?
O2 K1 N3 118.90(13) . . ?
O2 K1 N3 118.90(13) 2_655 . ?
O2 K1 N3 118.90(13) 3_665 . ?
O3 K1 O3 98.12(17) . 2_655 ?
O3 K1 O3 98.12(18) 3_665 2_655 ?
O3 K1 O3 98.12(18) 3_665 . ?
O3 K1 N2 119.28(13) 3_665 . ?
O3 K1 N2 119.28(14) . . ?
O3 K1 N2 119.28(13) 2_655 . ?
O3 K1 N3 60.72(14) . . ?
O3 K1 N3 60.72(14) 2_655 . ?
O3 K1 N3 60.72(13) 3_665 . ?
N2 K1 N3 180.0 . . ?
C22 O2 K1 120.8(5) . . ?
C22 O2 C23 110.3(7) . . ?
C23 O2 K1 118.9(5) . . ?
C24 O3 K1 114.6(5) . . ?
C24 O3 C25 110.8(8) . . ?
C25 O3 K1 114.7(6) . . ?
C21 N2 K1 109.3(5) 2_655 . ?
C21 N2 K1 109.3(5) . . ?
C21 N2 K1 109.3(5) 3_665 . ?
C21 N2 C21 109.6(5) 3_665 2_655 ?
C21 N2 C21 109.6(5) 3_665 . ?
C21 N2 C21 109.6(5) 2_655 . ?
C26 N3 K1 108.9(6) . . ?
C26 N3 K1 108.9(6) 3_665 . ?
C26 N3 K1 108.9(6) 2_655 . ?
C26 N3 C26 110.0(6) . 2_655 ?
C26 N3 C26 110.0(6) 3_665 . ?
C26 N3 C26 110.0(6) 3_665 2_655 ?
N2 C21 H21A 108.6 . . ?
N2 C21 H21B 108.6 . . ?
N2 C21 C22 114.5(7) . . ?
H21A C21 H21B 107.6 . . ?
C22 C21 H21A 108.6 . . ?
C22 C21 H21B 108.6 . . ?
O2 C22 C21 107.2(6) . . ?
O2 C22 H22A 110.3 . . ?
O2 C22 H22B 110.3 . . ?
C21 C22 H22A 110.3 . . ?
C21 C22 H22B 110.3 . . ?
H22A C22 H22B 108.5 . . ?
O2 C23 H23A 110.1 . . ?
O2 C23 H23B 110.1 . . ?
O2 C23 C24 107.8(7) . . ?
H23A C23 H23B 108.5 . . ?
C24 C23 H23A 110.1 . . ?
C24 C23 H23B 110.1 . . ?
O3 C24 C23 111.8(7) . . ?
O3 C24 H24A 109.3 . . ?
O3 C24 H24B 109.3 . . ?
C23 C24 H24A 109.3 . . ?
C23 C24 H24B 109.3 . . ?
H24A C24 H24B 107.9 . . ?
O3 C25 H25A 110.0 . . ?
O3 C25 H25B 110.0 . . ?
O3 C25 C26 108.3(9) . . ?
H25A C25 H25B 108.4 . . ?
C26 C25 H25A 110.0 . . ?
C26 C25 H25B 110.0 . . ?
N3 C26 C25 113.1(8) . . ?
N3 C26 H26A 109.0 . . ?
N3 C26 H26B 109.0 . . ?
C25 C26 H26A 109.0 . . ?
C25 C26 H26B 109.0 . . ?
H26A C26 H26B 107.8 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
U1 O1 C5 C4 13.8(13) . . . . ?
U1 O1 C5 C6 -165.1(6) . . . . ?
U1 N1 C1 C2 -63.3(5) . . . 2 ?
U1 N1 C2 C1 -10.6(6) . . . 3 ?
U1 N1 C3 C4 79.5(5) . . . . ?
O1 C5 C6 C7 169.0(6) . . . . ?
O1 C5 C6 C10 -13.7(10) . . . . ?
N1 C3 C4 C5 -62.3(7) . . . . ?
N1 C3 C4 C9 115.8(7) . . . . ?
C1 N1 C2 C1 -132.3(5) . . . 3 ?
C1 N1 C3 C4 -167.8(5) . . . . ?
C2 N1 C1 C2 64.3(7) . . . 2 ?
C2 N1 C3 C4 -46.7(7) . . . . ?
C3 N1 C1 C2 -174.8(5) . . . 2 ?
C3 N1 C2 C1 108.5(6) . . . 3 ?
C3 C4 C5 O1 7.9(9) . . . . ?
C3 C4 C5 C6 -173.1(6) . . . . ?
C3 C4 C9 C8 -178.3(6) . . . . ?
C4 C5 C6 C7 -10.0(9) . . . . ?
C4 C5 C6 C10 167.3(6) . . . . ?
C5 C4 C9 C8 -0.3(11) . . . . ?
C5 C6 C7 C8 3.2(10) . . . . ?
C5 C6 C10 C14 69.2(8) . . . . ?
C5 C6 C10 C15 -169.8(6) . . . . ?
C5 C6 C10 C18 -50.4(8) . . . . ?
C6 C7 C8 C9 5.1(11) . . . . ?
C6 C7 C8 C20 -177.8(7) . . . . ?
C6 C10 C14 C11 -178.8(5) . . . . ?
C6 C10 C15 C13 177.2(6) . . . . ?
C6 C10 C18 C12 179.9(5) . . . . ?
C7 C6 C10 C14 -113.6(7) . . . . ?
C7 C6 C10 C15 7.4(9) . . . . ?
C7 C6 C10 C18 126.8(6) . . . . ?
C7 C8 C9 C4 -6.5(11) . . . . ?
C9 C4 C5 O1 -170.2(6) . . . . ?
C9 C4 C5 C6 8.8(10) . . . . ?
C10 C6 C7 C8 -174.1(6) . . . . ?
C14 C10 C15 C13 -59.5(7) . . . . ?
C14 C10 C18 C12 57.9(7) . . . . ?
C14 C11 C16 C12 -61.7(7) . . . . ?
C14 C11 C19 C13 59.2(8) . . . . ?
C15 C10 C14 C11 58.1(7) . . . . ?
C15 C10 C18 C12 -58.4(7) . . . . ?
C15 C13 C17 C12 59.6(7) . . . . ?
C15 C13 C19 C11 -59.5(8) . . . . ?
C16 C11 C14 C10 61.1(7) . . . . ?
C16 C11 C19 C13 -60.7(8) . . . . ?
C16 C12 C17 C13 59.6(7) . . . . ?
C16 C12 C18 C10 -59.7(7) . . . . ?
C17 C12 C16 C11 -58.9(7) . . . . ?
C17 C12 C18 C10 60.7(7) . . . . ?
C17 C13 C15 C10 -59.2(8) . . . . ?
C17 C13 C19 C11 61.4(7) . . . . ?
C18 C10 C14 C11 -58.2(7) . . . . ?
C18 C10 C15 C13 56.8(7) . . . . ?
C18 C12 C16 C11 60.5(7) . . . . ?
C18 C12 C17 C13 -59.8(7) . . . . ?
C19 C11 C14 C10 -59.0(7) . . . . ?
C19 C11 C16 C12 59.0(7) . . . . ?
C19 C13 C15 C10 60.9(8) . . . . ?
C19 C13 C17 C12 -60.3(7) . . . . ?
C20 C8 C9 C4 176.4(7) . . . . ?
K1 O2 C22 C21 37.6(8) . . . . ?
K1 O2 C23 C24 -45.0(9) . . . . ?
K1 O3 C24 C23 -46.8(8) . . . . ?
K1 O3 C25 C26 54.5(10) . . . . ?
K1 N2 C21 C22 51.1(7) . . . . ?
K1 N3 C26 C25 44.6(11) . . . . ?
O2 C23 C24 O3 60.2(10) . . . . ?
O3 C25 C26 N3 -68.6(12) . . . . ?
N2 C21 C22 O2 -60.2(9) . . . . ?
C21 N2 C21 C22 -68.7(12) 3_665 . . . ?
C21 N2 C21 C22 170.9(7) 2_655 . . . ?
C22 O2 C23 C24 169.2(7) . . . . ?
C23 O2 C22 C21 -177.4(7) . . . . ?
C24 O3 C25 C26 -173.9(8) . . . . ?
C25 O3 C24 C23 -178.5(8) . . . . ?
C26 N3 C26 C25 -74.8(16) 2_655 . . . ?
C26 N3 C26 C25 163.9(10) 3_665 . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_mr1605
_database_code_depnum_ccdc_archive 'CCDC 1893561'
loop_
_audit_author_name
_audit_author_address
'Frank W. Heinemann'
;Friedrich-Alexander-Universit?t Erlangen-N?rnberg
Germany
;
_audit_update_record             
;
2019-01-25 deposited with the CCDC.	2019-03-25 downloaded from the CCDC.
;
_audit_creation_date             2019-01-24
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C60 H78 N3 O4 U1, C18 H36 K1 N2 O6'
_chemical_formula_sum            'C78 H114 K N5 O10 U'
_chemical_formula_weight         1558.87
_chemical_absolute_configuration ad
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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'
U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      hexagonal
_space_group_IT_number           173
_space_group_name_H-M_alt        'P 63'
_space_group_name_Hall           'P 6c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'

_cell_length_a                   14.825(2)
_cell_length_b                   14.825(2)
_cell_length_c                   19.561(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     3723.0(12)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9963
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.18
_cell_measurement_theta_min      2.62
_shelx_estimated_absorpt_T_max   0.914
_shelx_estimated_absorpt_T_min   0.856
_exptl_absorpt_coefficient_mu    2.296
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.6392
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.1225 before and 0.0865 after correction.
The Ratio of minimum to maximum transmission is 0.8570.
The λ/2 correction factor is 0.00150.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.391
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1616
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0825
_diffrn_reflns_av_unetI/netI     0.0339
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            121889
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.606
_diffrn_reflns_theta_min         1.586
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_radiation_source         'ImuS micro-focus tube'
_diffrn_radiation_monochromator  'Quazar focussing montel optics'
_diffrn_measurement_device_type  'Bruker Kappa APEX II CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 83.33
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_reflns_Friedel_coverage         0.941
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                5636
_reflns_number_total             6981
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELX XT 2014/5 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2015)'
_computing_molecular_graphics    'SHELXTL 6.12 (Bruker AXS, 2002)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_refine_diff_density_max         1.224
_refine_diff_density_min         -0.831
_refine_diff_density_rms         0.086
_refine_ls_abs_structure_details 
;
 Flack x determined using 2450 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.003(4)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     287
_refine_ls_number_reflns         6981
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0394
_refine_ls_R_factor_gt           0.0249
_refine_ls_restrained_S_all      1.098
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0231P)²+2.9517P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0589
_refine_ls_wR_factor_ref         0.0649
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H16A,H16B} of C16, {H17A,H17B} of C17, {H15A,H15B} of C15,
   {H14A,H14B} of C14, {H18A,H18B} of C18, {H3A,H3B} of C3, {H21A,H21B} of C21,
  {H23A,H23B} of C23, {H25A,H25B} of C25, {H22A,H22B} of C22, {H26A,H26B} of
  C26, {H24A,H24B} of C24, {H19A,H19B} of C19
 At 1.5 times of:
  All C(H,H,H) groups, {H2A,H2B} of C2, {H1A,H1B} of C1
2.a Ternary CH refined with riding coordinates:
 C11(H11), C12(H12), C13(H13)
2.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C14(H14A,H14B), C15(H15A,H15B),
 C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B), C21(H21A,H21B),
  C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B), C26(H26A,H26B)
2.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C9(H9)
2.d Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.000000 0.000000 0.75026(4) 0.01307(6) Uani 1 3 d S T P . .
O1 O -0.0235(2) 0.1408(2) 0.7545(2) 0.0197(5) Uani 1 1 d . . . . .
O2 O 0.000000 0.000000 0.8458(3) 0.0176(9) Uani 1 3 d S T P . .
N1 N -0.1020(3) 0.0214(3) 0.62810(18) 0.0159(7) Uani 1 1 d . . . . .
C1 C -0.1635(3) -0.0846(3) 0.6000(2) 0.0188(8) Uani 1 1 d . . . . .
H1A H -0.206417 -0.083400 0.561625 0.028 Uiso 1 1 calc R . . . .
H1B H -0.211338 -0.131074 0.635788 0.028 Uiso 1 1 calc R . . . .
C2 C -0.0323(3) 0.0967(3) 0.5747(2) 0.0182(8) Uani 1 1 d . . . . .
H2A H -0.060073 0.142400 0.561045 0.027 Uiso 1 1 calc R . . . .
H2B H -0.032329 0.057367 0.533729 0.027 Uiso 1 1 calc R . . . .
C3 C -0.1766(3) 0.0531(3) 0.6543(2) 0.0190(8) Uani 1 1 d . . . . .
H3A H -0.212942 0.009971 0.694736 0.023 Uiso 1 1 calc R . . . .
H3B H -0.229754 0.038198 0.618691 0.023 Uiso 1 1 calc R . . . .
C4 C -0.1267(3) 0.1658(3) 0.6738(2) 0.0179(8) Uani 1 1 d . . . . .
C5 C -0.0541(4) 0.2029(4) 0.7280(2) 0.0175(8) Uani 1 1 d . . . . .
C6 C -0.0168(3) 0.3062(3) 0.7525(3) 0.0153(6) Uani 1 1 d . . . . .
C7 C -0.0433(4) 0.3702(4) 0.7155(2) 0.0201(9) Uani 1 1 d . . . . .
H7 H -0.016253 0.440086 0.730345 0.024 Uiso 1 1 calc R . . . .
C8 C -0.1075(4) 0.3368(4) 0.6578(2) 0.0215(9) Uani 1 1 d . . . . .
C9 C -0.1512(4) 0.2334(4) 0.6393(2) 0.0205(10) Uani 1 1 d . . . . .
H9 H -0.198963 0.207552 0.602184 0.025 Uiso 1 1 calc R . . . .
C10 C 0.0471(3) 0.3428(3) 0.8184(2) 0.0155(8) Uani 1 1 d . . . . .
C11 C 0.2194(4) 0.3911(4) 0.8747(3) 0.0226(10) Uani 1 1 d . . . . .
H11 H 0.289851 0.399555 0.866857 0.027 Uiso 1 1 calc R . . . .
C12 C 0.0543(3) 0.2966(3) 0.9426(2) 0.0188(8) Uani 1 1 d . . . . .
H12 H 0.017152 0.242569 0.978626 0.023 Uiso 1 1 calc R . . . .
C13 C 0.1227(4) 0.4823(4) 0.9104(3) 0.0248(10) Uani 1 1 d . . . . .
H13 H 0.130587 0.550456 0.925223 0.030 Uiso 1 1 calc R . . . .
C14 C 0.1565(3) 0.3563(4) 0.8081(2) 0.0207(9) Uani 1 1 d . . . . .
H14A H 0.149677 0.289488 0.792853 0.025 Uiso 1 1 calc R . . . .
H14B H 0.193934 0.408874 0.772010 0.025 Uiso 1 1 calc R . . . .
C15 C 0.0613(4) 0.4481(3) 0.8435(2) 0.0206(9) Uani 1 1 d . . . . .
H15A H 0.098629 0.501943 0.808104 0.025 Uiso 1 1 calc R . . . .
H15B H -0.007897 0.441456 0.850367 0.025 Uiso 1 1 calc R . . . .
C16 C 0.1621(3) 0.3084(4) 0.9298(2) 0.0216(9) Uani 1 1 d . . . . .
H16A H 0.203076 0.329335 0.972683 0.026 Uiso 1 1 calc R . . . .
H16B H 0.153994 0.240992 0.914807 0.026 Uiso 1 1 calc R . . . .
C17 C 0.0658(4) 0.4006(4) 0.9663(2) 0.0253(10) Uani 1 1 d . . . . .
H17A H -0.003696 0.392510 0.974724 0.030 Uiso 1 1 calc R . . . .
H17B H 0.106038 0.423063 1.009500 0.030 Uiso 1 1 calc R . . . .
C18 C -0.0091(3) 0.2622(3) 0.8762(2) 0.0162(8) Uani 1 1 d . . . . .
H18A H -0.078539 0.254460 0.884298 0.019 Uiso 1 1 calc R . . . .
H18B H -0.019252 0.193678 0.861982 0.019 Uiso 1 1 calc R . . . .
C19 C 0.2312(4) 0.4951(4) 0.8985(3) 0.0277(11) Uani 1 1 d . . . . .
H19A H 0.269007 0.549242 0.863413 0.033 Uiso 1 1 calc R . . . .
H19B H 0.271980 0.517428 0.941415 0.033 Uiso 1 1 calc R . . . .
C20 C -0.1296(5) 0.4117(4) 0.6184(3) 0.0341(12) Uani 1 1 d . . . . .
H20A H -0.199019 0.373268 0.597751 0.051 Uiso 1 1 calc GR . . . .
H20B H -0.077270 0.445477 0.582448 0.051 Uiso 1 1 calc GR . . . .
H20C H -0.126925 0.464639 0.649678 0.051 Uiso 1 1 calc GR . . . .
K1 K 0.666667 0.333333 0.97309(8) 0.0154(3) Uani 1 3 d S T P . .
O3 O 0.8029(3) 0.5159(3) 0.9033(2) 0.0271(8) Uani 1 1 d . . . . .
O4 O 0.8280(3) 0.5058(3) 1.0449(2) 0.0325(8) Uani 1 1 d . . . . .
N2 N 0.666667 0.333333 0.8236(3) 0.0246(14) Uani 1 3 d S T P . .
N3 N 0.666667 0.333333 1.1266(4) 0.040(2) Uani 1 3 d S T P . .
C21 C 0.7144(5) 0.4411(4) 0.7988(3) 0.0334(12) Uani 1 1 d . . . . .
H21A H 0.665566 0.467101 0.807263 0.040 Uiso 1 1 calc R . . . .
H21B H 0.724461 0.441312 0.748747 0.040 Uiso 1 1 calc R . . . .
C22 C 0.8180(4) 0.5154(4) 0.8315(3) 0.0336(12) Uani 1 1 d . . . . .
H22A H 0.869235 0.492818 0.821697 0.040 Uiso 1 1 calc R . . . .
H22B H 0.845165 0.586406 0.812713 0.040 Uiso 1 1 calc R . . . .
C23 C 0.8965(4) 0.5869(4) 0.9371(3) 0.0373(13) Uani 1 1 d . . . . .
H23A H 0.930420 0.654537 0.912815 0.045 Uiso 1 1 calc R . . . .
H23B H 0.945126 0.559366 0.937370 0.045 Uiso 1 1 calc R . . . .
C24 C 0.8717(4) 0.6013(4) 1.0079(4) 0.0399(14) Uani 1 1 d . . . . .
H24A H 0.935921 0.654181 1.031110 0.048 Uiso 1 1 calc R . . . .
H24B H 0.821645 0.627115 1.007300 0.048 Uiso 1 1 calc R . . . .
C25 C 0.8038(6) 0.5189(6) 1.1131(3) 0.0447(17) Uani 1 1 d . . . . .
H25A H 0.748994 0.538469 1.113058 0.054 Uiso 1 1 calc R . . . .
H25B H 0.866478 0.575333 1.135625 0.054 Uiso 1 1 calc R . . . .
C26 C 0.7670(6) 0.4200(6) 1.1509(3) 0.0543(18) Uani 1 1 d . . . . .
H26A H 0.820481 0.398930 1.147293 0.065 Uiso 1 1 calc R . . . .
H26B H 0.760012 0.432452 1.199842 0.065 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 O1 2.283(3) 2 ?
U1 O1 2.283(3) . ?
U1 O1 2.283(3) 3 ?
U1 O2 1.868(5) . ?
U1 N1 2.929(4) 3 ?
U1 N1 2.929(4) 2 ?
U1 N1 2.929(4) . ?
O1 C5 1.319(5) . ?
N1 C1 1.473(6) . ?
N1 C2 1.501(6) . ?
N1 C3 1.491(5) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.520(6) 2 ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C4 1.500(6) . ?
C4 C5 1.411(6) . ?
C4 C9 1.398(6) . ?
C5 C6 1.427(6) . ?
C6 C7 1.396(6) . ?
C6 C10 1.528(6) . ?
C7 H7 0.9500 . ?
C7 C8 1.398(6) . ?
C8 C9 1.382(7) . ?
C8 C20 1.515(6) . ?
C9 H9 0.9500 . ?
C10 C14 1.545(6) . ?
C10 C15 1.547(6) . ?
C10 C18 1.551(6) . ?
C11 H11 1.0000 . ?
C11 C14 1.533(7) . ?
C11 C16 1.532(7) . ?
C11 C19 1.534(7) . ?
C12 H12 1.0000 . ?
C12 C16 1.538(6) . ?
C12 C17 1.536(6) . ?
C12 C18 1.532(6) . ?
C13 H13 1.0000 . ?
C13 C15 1.530(7) . ?
C13 C17 1.534(7) . ?
C13 C19 1.540(7) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
K1 O3 2.793(4) 3_665 ?
K1 O3 2.793(4) . ?
K1 O3 2.793(4) 2_655 ?
K1 O4 2.848(3) 3_665 ?
K1 O4 2.848(4) . ?
K1 O4 2.848(3) 2_655 ?
K1 N2 2.925(7) . ?
K1 N3 3.004(8) . ?
O3 C22 1.424(7) . ?
O3 C23 1.418(7) . ?
O4 C24 1.425(7) . ?
O4 C25 1.420(8) . ?
N2 C21 1.469(6) 2_655 ?
N2 C21 1.469(6) 3_665 ?
N2 C21 1.469(6) . ?
N3 C26 1.475(7) . ?
N3 C26 1.475(7) 3_665 ?
N3 C26 1.475(7) 2_655 ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C21 C22 1.513(8) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C23 C24 1.476(9) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 C26 1.481(11) . ?
C26 H26A 0.9900 . ?
C26 H26B 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 U1 O1 119.871(14) 2 3 ?
O1 U1 O1 119.872(14) 2 . ?
O1 U1 O1 119.870(15) 3 . ?
O1 U1 N1 66.87(12) 2 2 ?
O1 U1 N1 84.19(12) . 3 ?
O1 U1 N1 125.61(13) 2 3 ?
O1 U1 N1 125.61(13) . 2 ?
O1 U1 N1 84.19(12) 2 . ?
O1 U1 N1 66.87(12) 3 3 ?
O1 U1 N1 125.61(13) 3 . ?
O1 U1 N1 66.87(12) . . ?
O1 U1 N1 84.19(12) 3 2 ?
O2 U1 O1 87.93(11) . . ?
O2 U1 O1 87.93(11) . 2 ?
O2 U1 O1 87.93(11) . 3 ?
O2 U1 N1 144.67(7) . 3 ?
O2 U1 N1 144.67(7) . . ?
O2 U1 N1 144.67(7) . 2 ?
N1 U1 N1 60.11(11) . 2 ?
N1 U1 N1 60.11(11) 2 3 ?
N1 U1 N1 60.11(11) . 3 ?
C5 O1 U1 152.5(3) . . ?
C1 N1 U1 105.4(3) . . ?
C1 N1 C2 111.2(3) . . ?
C1 N1 C3 107.7(3) . . ?
C2 N1 U1 116.6(2) . . ?
C3 N1 U1 105.0(2) . . ?
C3 N1 C2 110.4(3) . . ?
N1 C1 H1A 108.9 . . ?
N1 C1 H1B 108.9 . . ?
N1 C1 C2 113.2(3) . 2 ?
H1A C1 H1B 107.7 . . ?
C2 C1 H1A 108.9 2 . ?
C2 C1 H1B 108.9 2 . ?
N1 C2 C1 112.1(4) . 3 ?
N1 C2 H2A 109.2 . . ?
N1 C2 H2B 109.2 . . ?
C1 C2 H2A 109.2 3 . ?
C1 C2 H2B 109.2 3 . ?
H2A C2 H2B 107.9 . . ?
N1 C3 H3A 108.7 . . ?
N1 C3 H3B 108.7 . . ?
N1 C3 C4 114.1(4) . . ?
H3A C3 H3B 107.6 . . ?
C4 C3 H3A 108.7 . . ?
C4 C3 H3B 108.7 . . ?
C5 C4 C3 118.7(4) . . ?
C9 C4 C3 121.0(4) . . ?
C9 C4 C5 120.3(4) . . ?
O1 C5 C4 119.0(4) . . ?
O1 C5 C6 122.2(4) . . ?
C4 C5 C6 118.8(4) . . ?
C5 C6 C10 120.2(4) . . ?
C7 C6 C5 117.7(4) . . ?
C7 C6 C10 122.0(4) . . ?
C6 C7 H7 118.3 . . ?
C6 C7 C8 123.4(4) . . ?
C8 C7 H7 118.3 . . ?
C7 C8 C20 120.6(5) . . ?
C9 C8 C7 117.6(4) . . ?
C9 C8 C20 121.8(4) . . ?
C4 C9 H9 119.3 . . ?
C8 C9 C4 121.5(4) . . ?
C8 C9 H9 119.3 . . ?
C6 C10 C14 111.1(3) . . ?
C6 C10 C15 111.9(3) . . ?
C6 C10 C18 110.1(3) . . ?
C14 C10 C15 107.8(3) . . ?
C14 C10 C18 108.6(3) . . ?
C15 C10 C18 107.2(3) . . ?
C14 C11 H11 109.5 . . ?
C14 C11 C19 110.0(4) . . ?
C16 C11 H11 109.5 . . ?
C16 C11 C14 109.2(4) . . ?
C16 C11 C19 109.2(4) . . ?
C19 C11 H11 109.5 . . ?
C16 C12 H12 109.3 . . ?
C17 C12 H12 109.3 . . ?
C17 C12 C16 110.3(4) . . ?
C18 C12 H12 109.3 . . ?
C18 C12 C16 109.2(3) . . ?
C18 C12 C17 109.4(4) . . ?
C15 C13 H13 109.4 . . ?
C15 C13 C17 110.4(4) . . ?
C15 C13 C19 108.8(4) . . ?
C17 C13 H13 109.4 . . ?
C17 C13 C19 109.5(4) . . ?
C19 C13 H13 109.4 . . ?
C10 C14 H14A 109.5 . . ?
C10 C14 H14B 109.5 . . ?
C11 C14 C10 110.8(4) . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
H14A C14 H14B 108.1 . . ?
C10 C15 H15A 109.3 . . ?
C10 C15 H15B 109.3 . . ?
C13 C15 C10 111.4(4) . . ?
C13 C15 H15A 109.3 . . ?
C13 C15 H15B 109.3 . . ?
H15A C15 H15B 108.0 . . ?
C11 C16 C12 109.5(4) . . ?
C11 C16 H16A 109.8 . . ?
C11 C16 H16B 109.8 . . ?
C12 C16 H16A 109.8 . . ?
C12 C16 H16B 109.8 . . ?
H16A C16 H16B 108.2 . . ?
C12 C17 H17A 110.0 . . ?
C12 C17 H17B 110.0 . . ?
C13 C17 C12 108.6(4) . . ?
C13 C17 H17A 110.0 . . ?
C13 C17 H17B 110.0 . . ?
H17A C17 H17B 108.4 . . ?
C10 C18 H18A 109.4 . . ?
C10 C18 H18B 109.4 . . ?
C12 C18 C10 111.0(3) . . ?
C12 C18 H18A 109.4 . . ?
C12 C18 H18B 109.4 . . ?
H18A C18 H18B 108.0 . . ?
C11 C19 C13 109.6(4) . . ?
C11 C19 H19A 109.8 . . ?
C11 C19 H19B 109.8 . . ?
C13 C19 H19A 109.8 . . ?
C13 C19 H19B 109.8 . . ?
H19A C19 H19B 108.2 . . ?
C8 C20 H20A 109.5 . . ?
C8 C20 H20B 109.5 . . ?
C8 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O3 K1 O3 98.16(11) 3_665 2_655 ?
O3 K1 O3 98.16(11) 3_665 . ?
O3 K1 O3 98.16(11) . 2_655 ?
O3 K1 O4 59.68(11) 3_665 3_665 ?
O3 K1 O4 59.68(11) . . ?
O3 K1 O4 119.35(11) . 2_655 ?
O3 K1 O4 137.49(11) . 3_665 ?
O3 K1 O4 137.49(11) 3_665 2_655 ?
O3 K1 O4 119.35(11) 2_655 3_665 ?
O3 K1 O4 59.68(11) 2_655 2_655 ?
O3 K1 O4 119.35(11) 3_665 . ?
O3 K1 O4 137.49(10) 2_655 . ?
O3 K1 N2 60.75(9) 3_665 . ?
O3 K1 N2 60.75(9) 2_655 . ?
O3 K1 N2 60.75(9) . . ?
O3 K1 N3 119.25(9) 3_665 . ?
O3 K1 N3 119.25(9) 2_655 . ?
O3 K1 N3 119.25(9) . . ?
O4 K1 O4 97.80(12) 3_665 . ?
O4 K1 O4 97.80(12) 3_665 2_655 ?
O4 K1 O4 97.80(12) . 2_655 ?
O4 K1 N2 119.53(9) 3_665 . ?
O4 K1 N2 119.53(9) . . ?
O4 K1 N2 119.53(9) 2_655 . ?
O4 K1 N3 60.47(9) . . ?
O4 K1 N3 60.47(9) 2_655 . ?
O4 K1 N3 60.47(9) 3_665 . ?
N2 K1 N3 180.0 . . ?
C22 O3 K1 121.1(3) . . ?
C23 O3 K1 117.2(3) . . ?
C23 O3 C22 111.4(4) . . ?
C24 O4 K1 113.8(3) . . ?
C25 O4 K1 115.5(4) . . ?
C25 O4 C24 111.2(5) . . ?
C21 N2 K1 109.3(3) 2_655 . ?
C21 N2 K1 109.3(3) 3_665 . ?
C21 N2 K1 109.3(3) . . ?
C21 N2 C21 109.7(3) 3_665 . ?
C21 N2 C21 109.7(3) 3_665 2_655 ?
C21 N2 C21 109.7(3) 2_655 . ?
C26 N3 K1 108.8(4) . . ?
C26 N3 K1 108.8(4) 2_655 . ?
C26 N3 K1 108.8(4) 3_665 . ?
C26 N3 C26 110.2(4) 3_665 . ?
C26 N3 C26 110.2(4) . 2_655 ?
C26 N3 C26 110.2(4) 3_665 2_655 ?
N2 C21 H21A 108.6 . . ?
N2 C21 H21B 108.6 . . ?
N2 C21 C22 114.5(4) . . ?
H21A C21 H21B 107.6 . . ?
C22 C21 H21A 108.6 . . ?
C22 C21 H21B 108.6 . . ?
O3 C22 C21 108.4(4) . . ?
O3 C22 H22A 110.0 . . ?
O3 C22 H22B 110.0 . . ?
C21 C22 H22A 110.0 . . ?
C21 C22 H22B 110.0 . . ?
H22A C22 H22B 108.4 . . ?
O3 C23 H23A 109.9 . . ?
O3 C23 H23B 109.9 . . ?
O3 C23 C24 108.8(4) . . ?
H23A C23 H23B 108.3 . . ?
C24 C23 H23A 109.9 . . ?
C24 C23 H23B 109.9 . . ?
O4 C24 C23 110.7(4) . . ?
O4 C24 H24A 109.5 . . ?
O4 C24 H24B 109.5 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 108.1 . . ?
O4 C25 H25A 109.9 . . ?
O4 C25 H25B 109.9 . . ?
O4 C25 C26 109.1(6) . . ?
H25A C25 H25B 108.3 . . ?
C26 C25 H25A 109.9 . . ?
C26 C25 H25B 109.9 . . ?
N3 C26 C25 114.4(5) . . ?
N3 C26 H26A 108.7 . . ?
N3 C26 H26B 108.7 . . ?
C25 C26 H26A 108.7 . . ?
C25 C26 H26B 108.7 . . ?
H26A C26 H26B 107.6 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
U1 O1 C5 C4 20.7(9) . . . . ?
U1 O1 C5 C6 -159.7(4) . . . . ?
U1 N1 C1 C2 -65.3(4) . . . 2 ?
U1 N1 C2 C1 -10.5(4) . . . 3 ?
U1 N1 C3 C4 77.8(4) . . . . ?
O1 C5 C6 C7 171.9(4) . . . . ?
O1 C5 C6 C10 -10.0(6) . . . . ?
N1 C3 C4 C5 -63.5(5) . . . . ?
N1 C3 C4 C9 116.4(5) . . . . ?
C1 N1 C2 C1 -131.4(4) . . . 3 ?
C1 N1 C3 C4 -170.2(4) . . . . ?
C2 N1 C1 C2 61.9(5) . . . 2 ?
C2 N1 C3 C4 -48.6(5) . . . . ?
C3 N1 C1 C2 -177.0(3) . . . 2 ?
C3 N1 C2 C1 109.1(4) . . . 3 ?
C3 C4 C5 O1 7.6(6) . . . . ?
C3 C4 C5 C6 -172.0(4) . . . . ?
C3 C4 C9 C8 178.6(4) . . . . ?
C4 C5 C6 C7 -8.5(6) . . . . ?
C4 C5 C6 C10 169.6(4) . . . . ?
C5 C4 C9 C8 -1.5(7) . . . . ?
C5 C6 C7 C8 2.7(6) . . . . ?
C5 C6 C10 C14 70.6(5) . . . . ?
C5 C6 C10 C15 -168.8(4) . . . . ?
C5 C6 C10 C18 -49.7(5) . . . . ?
C6 C7 C8 C9 3.8(7) . . . . ?
C6 C7 C8 C20 -177.6(4) . . . . ?
C6 C10 C14 C11 -179.0(4) . . . . ?
C6 C10 C15 C13 178.4(4) . . . . ?
C6 C10 C18 C12 179.3(3) . . . . ?
C7 C6 C10 C14 -111.3(4) . . . . ?
C7 C6 C10 C15 9.3(5) . . . . ?
C7 C6 C10 C18 128.3(4) . . . . ?
C7 C8 C9 C4 -4.4(7) . . . . ?
C9 C4 C5 O1 -172.3(4) . . . . ?
C9 C4 C5 C6 8.1(6) . . . . ?
C10 C6 C7 C8 -175.4(4) . . . . ?
C14 C10 C15 C13 -59.1(5) . . . . ?
C14 C10 C18 C12 57.4(4) . . . . ?
C14 C11 C16 C12 -61.0(5) . . . . ?
C14 C11 C19 C13 59.6(5) . . . . ?
C15 C10 C14 C11 58.0(5) . . . . ?
C15 C10 C18 C12 -58.8(4) . . . . ?
C15 C13 C17 C12 59.4(5) . . . . ?
C15 C13 C19 C11 -59.6(5) . . . . ?
C16 C11 C14 C10 60.3(5) . . . . ?
C16 C11 C19 C13 -60.2(5) . . . . ?
C16 C12 C17 C13 59.9(5) . . . . ?
C16 C12 C18 C10 -59.2(4) . . . . ?
C17 C12 C16 C11 -59.8(5) . . . . ?
C17 C12 C18 C10 61.6(4) . . . . ?
C17 C13 C15 C10 -59.6(5) . . . . ?
C17 C13 C19 C11 61.1(5) . . . . ?
C18 C10 C14 C11 -57.8(5) . . . . ?
C18 C10 C15 C13 57.6(5) . . . . ?
C18 C12 C16 C11 60.5(5) . . . . ?
C18 C12 C17 C13 -60.2(5) . . . . ?
C19 C11 C14 C10 -59.5(5) . . . . ?
C19 C11 C16 C12 59.3(5) . . . . ?
C19 C13 C15 C10 60.5(5) . . . . ?
C19 C13 C17 C12 -60.3(5) . . . . ?
C20 C8 C9 C4 177.0(5) . . . . ?
K1 O3 C22 C21 37.9(5) . . . . ?
K1 O3 C23 C24 -46.8(5) . . . . ?
K1 O4 C24 C23 -47.6(5) . . . . ?
K1 O4 C25 C26 53.1(6) . . . . ?
K1 N2 C21 C22 49.4(5) . . . . ?
K1 N3 C26 C25 42.8(6) . . . . ?
O3 C23 C24 O4 62.7(6) . . . . ?
O4 C25 C26 N3 -66.5(8) . . . . ?
N2 C21 C22 O3 -59.2(6) . . . . ?
C21 N2 C21 C22 -70.4(7) 3_665 . . . ?
C21 N2 C21 C22 169.1(4) 2_655 . . . ?
C22 O3 C23 C24 167.6(4) . . . . ?
C23 O3 C22 C21 -178.0(4) . . . . ?
C24 O4 C25 C26 -175.3(5) . . . . ?
C25 O4 C24 C23 180.0(5) . . . . ?
C26 N3 C26 C25 -76.3(10) 2_655 . . . ?
C26 N3 C26 C25 161.9(6) 3_665 . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_mr1601
_database_code_depnum_ccdc_archive 'CCDC 1893563'
loop_
_audit_author_name
_audit_author_address
'Frank W. Heinemann'
;Friedrich-Alexander-Universit?t Erlangen-N?rnberg
Germany
;
_audit_update_record             
;
2019-01-25 deposited with the CCDC.	2019-03-25 downloaded from the CCDC.
;
_audit_creation_date             2019-01-24
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C60 H78 N3 O3 Te1 U1, C18 H36 K1 N2 O6'
_chemical_formula_sum            'C78 H114 K N5 O9 Te U'
_chemical_formula_weight         1670.47
_chemical_absolute_configuration ad
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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'
Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      hexagonal
_space_group_IT_number           173
_space_group_name_H-M_alt        'P 63'
_space_group_name_Hall           'P 6c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x-y, x, z+1/2'
'y, -x+y, z+1/2'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'

_cell_length_a                   14.886(4)
_cell_length_b                   14.886(4)
_cell_length_c                   19.469(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     3736(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    1673
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      17.35
_cell_measurement_theta_min      2.62
_shelx_estimated_absorpt_T_max   0.949
_shelx_estimated_absorpt_T_min   0.690
_exptl_absorpt_coefficient_mu    2.670
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6163
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.1160 before and 0.0989 after correction.
The Ratio of minimum to maximum transmission is 0.8267.
The λ/2 correction factor is 0.00150.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.485
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             1704
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.025
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.3026
_diffrn_reflns_av_unetI/netI     0.1440
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            59372
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.009
_diffrn_reflns_theta_min         2.092
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_radiation_source         'ImuS micro-focus tube'
_diffrn_radiation_monochromator  'Quazar focussing montel optics'
_diffrn_measurement_device_type  'Bruker Kappa APEX II CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 83.33
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_reflns_Friedel_coverage         0.939
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                2656
_reflns_number_total             4920
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELX XT 2014/5 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2015)'
_computing_molecular_graphics    'SHELXTL 6.12 (Bruker AXS, 2002)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_refine_diff_density_max         1.207
_refine_diff_density_min         -3.290
_refine_diff_density_rms         0.164
_refine_ls_abs_structure_details 
;
 Flack x determined using 953 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.043(9)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     287
_refine_ls_number_reflns         4920
_refine_ls_number_restraints     25
_refine_ls_R_factor_all          0.1463
_refine_ls_R_factor_gt           0.0599
_refine_ls_restrained_S_all      0.999
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0639P)²+5.1165P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1247
_refine_ls_wR_factor_ref         0.1568
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H17A,H17B} of C17, {H22A,H22B} of C22, {H25A,H25B} of C25,
   {H24A,H24B} of C24, {H19A,H19B} of C19, {H26A,H26B} of C26, {H16A,H16B} of
  C16, {H18A,H18B} of C18, {H14A,H14B} of C14, {H21A,H21B} of C21, {H23A,H23B}
  of C23, {H15A,H15B} of C15, {H3A,H3B} of C3
 At 1.5 times of:
  All C(H,H,H) groups, {H2A,H2B} of C2, {H1A,H1B} of C1
2. Uiso/Uaniso restraints and constraints
Uanis(O1) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C23) \\sim
Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
3.a Ternary CH refined with riding coordinates:
 C11(H11), C12(H12), C13(H13)
3.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C14(H14A,H14B), C15(H15A,H15B),
 C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B), C21(H21A,H21B),
  C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B), C26(H26A,H26B)
3.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C9(H9)
3.d Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.000000 0.000000 0.74665(5) 0.0178(3) Uani 1 3 d S T P . .
Te1 Te 0.000000 0.000000 0.89774(10) 0.0257(5) Uani 1 3 d S T P . .
O1 O -0.0177(9) 0.1379(9) 0.7559(8) 0.021(3) Uani 1 1 d . U . . .
N1 N -0.1034(12) 0.0165(12) 0.6336(9) 0.023(4) Uani 1 1 d . . . . .
C1 C -0.1624(15) -0.0878(15) 0.6040(12) 0.027(5) Uani 1 1 d . U . . .
H1A H -0.204881 -0.086242 0.565406 0.041 Uiso 1 1 calc R . . . .
H1B H -0.210339 -0.135704 0.639270 0.041 Uiso 1 1 calc R . . . .
C2 C -0.0368(14) 0.0935(14) 0.5778(12) 0.031(5) Uani 1 1 d . . . . .
H2A H -0.066827 0.137347 0.564891 0.046 Uiso 1 1 calc R . . . .
H2B H -0.036105 0.055202 0.536404 0.046 Uiso 1 1 calc R . . . .
C3 C -0.1788(17) 0.0445(16) 0.6631(11) 0.027(5) Uani 1 1 d . . . . .
H3A H -0.209459 0.003103 0.705297 0.033 Uiso 1 1 calc R . . . .
H3B H -0.235769 0.025393 0.629773 0.033 Uiso 1 1 calc R . . . .
C4 C -0.1313(16) 0.1584(16) 0.6806(10) 0.022(5) Uani 1 1 d . . . . .
C5 C -0.0538(14) 0.1970(14) 0.7321(10) 0.022(5) Uani 1 1 d . . . . .
C6 C -0.0161(13) 0.3033(13) 0.7573(11) 0.020(4) Uani 1 1 d . U . . .
C7 C -0.0453(17) 0.3649(16) 0.7189(10) 0.028(5) Uani 1 1 d . . . . .
H7 H -0.017240 0.435560 0.731551 0.033 Uiso 1 1 calc R . . . .
C8 C -0.1154(17) 0.3260(17) 0.6617(12) 0.029(5) Uani 1 1 d . . . . .
C9 C -0.1586(17) 0.2220(17) 0.6473(11) 0.027(5) Uani 1 1 d . . . . .
H9 H -0.209971 0.192922 0.612413 0.032 Uiso 1 1 calc R . . . .
C10 C 0.0486(13) 0.3430(12) 0.8209(13) 0.022(4) Uani 1 1 d . . . . .
C11 C 0.2205(16) 0.3945(16) 0.8770(11) 0.024(5) Uani 1 1 d . . . . .
H11 H 0.290566 0.402739 0.868924 0.029 Uiso 1 1 calc R . . . .
C12 C 0.0562(15) 0.3024(14) 0.9451(11) 0.023(4) Uani 1 1 d . . . . .
H12 H 0.019692 0.250550 0.982438 0.028 Uiso 1 1 calc R . . . .
C13 C 0.1214(18) 0.4863(18) 0.9102(13) 0.033(6) Uani 1 1 d . . . . .
H13 H 0.127635 0.554046 0.923512 0.039 Uiso 1 1 calc R . . . .
C14 C 0.1565(14) 0.3575(14) 0.8133(12) 0.028(5) Uani 1 1 d . . . . .
H14A H 0.150128 0.290567 0.799339 0.034 Uiso 1 1 calc R . . . .
H14B H 0.193146 0.408029 0.775972 0.034 Uiso 1 1 calc R . . . .
C15 C 0.0619(15) 0.4488(14) 0.8428(11) 0.028(5) Uani 1 1 d . . . . .
H15A H 0.099550 0.500669 0.806451 0.033 Uiso 1 1 calc R . . . .
H15B H -0.007332 0.442157 0.848208 0.033 Uiso 1 1 calc R . . . .
C16 C 0.1642(16) 0.3164(16) 0.9349(11) 0.027(5) Uani 1 1 d . . . . .
H16A H 0.158287 0.248884 0.923160 0.032 Uiso 1 1 calc R . . . .
H16B H 0.204497 0.341694 0.978030 0.032 Uiso 1 1 calc R . . . .
C17 C 0.0661(18) 0.4078(16) 0.9661(11) 0.035(5) Uani 1 1 d . . . . .
H17A H -0.003731 0.398826 0.973434 0.042 Uiso 1 1 calc R . . . .
H17B H 0.105399 0.432334 1.009625 0.042 Uiso 1 1 calc R . . . .
C18 C -0.0061(15) 0.2650(15) 0.8807(10) 0.025(5) Uani 1 1 d . . . . .
H18A H -0.075606 0.256541 0.888468 0.030 Uiso 1 1 calc R . . . .
H18B H -0.015218 0.196536 0.867993 0.030 Uiso 1 1 calc R . . . .
C19 C 0.2310(16) 0.5000(15) 0.9014(13) 0.027(6) Uani 1 1 d . . . . .
H19A H 0.268832 0.521370 0.945600 0.033 Uiso 1 1 calc R . . . .
H19B H 0.270639 0.554843 0.867045 0.033 Uiso 1 1 calc R . . . .
C20 C -0.142(2) 0.3953(19) 0.6227(12) 0.044(6) Uani 1 1 d . . . . .
H20A H -0.205227 0.353279 0.596057 0.067 Uiso 1 1 calc GR . . . .
H20B H -0.084778 0.438835 0.591512 0.067 Uiso 1 1 calc GR . . . .
H20C H -0.153031 0.439411 0.654839 0.067 Uiso 1 1 calc GR . . . .
K1 K 0.666667 0.333333 0.9776(4) 0.026(2) Uani 1 3 d S T P . .
O2 O 0.8022(15) 0.5161(13) 0.9076(11) 0.048(5) Uani 1 1 d . . . . .
O3 O 0.8271(14) 0.5074(14) 1.0473(10) 0.051(5) Uani 1 1 d . . . . .
N2 N 0.666667 0.333333 0.826(2) 0.032(7) Uani 1 3 d S T P . .
N3 N 0.666667 0.333333 1.1285(17) 0.049(10) Uani 1 3 d S T P . .
C21 C 0.7129(19) 0.4394(19) 0.8034(12) 0.049(7) Uani 1 1 d . . . . .
H21A H 0.663384 0.463861 0.813057 0.058 Uiso 1 1 calc R . . . .
H21B H 0.721734 0.440687 0.752958 0.058 Uiso 1 1 calc R . . . .
C22 C 0.8167(18) 0.516(2) 0.8348(17) 0.055(8) Uani 1 1 d . . . . .
H22A H 0.869111 0.496082 0.824178 0.066 Uiso 1 1 calc R . . . .
H22B H 0.841009 0.586639 0.815892 0.066 Uiso 1 1 calc R . . . .
C23 C 0.8959(19) 0.5877(19) 0.9392(15) 0.046(7) Uani 1 1 d . U . . .
H23A H 0.928069 0.654691 0.914351 0.055 Uiso 1 1 calc R . . . .
H23B H 0.944983 0.561152 0.939017 0.055 Uiso 1 1 calc R . . . .
C24 C 0.8709(17) 0.6018(16) 1.0109(12) 0.043(7) Uani 1 1 d . . . . .
H24A H 0.934968 0.653911 1.034377 0.052 Uiso 1 1 calc R . . . .
H24B H 0.821514 0.628011 1.010391 0.052 Uiso 1 1 calc R . . . .
C25 C 0.802(3) 0.519(2) 1.1143(18) 0.068(11) Uani 1 1 d . . . . .
H25A H 0.746819 0.537564 1.113891 0.081 Uiso 1 1 calc R . . . .
H25B H 0.863999 0.576318 1.137101 0.081 Uiso 1 1 calc R . . . .
C26 C 0.766(3) 0.418(3) 1.1540(14) 0.072(10) Uani 1 1 d . . . . .
H26A H 0.819172 0.397411 1.150483 0.087 Uiso 1 1 calc R . . . .
H26B H 0.758095 0.430238 1.203118 0.087 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 Te1 2.942(2) . ?
U1 O1 2.204(11) . ?
U1 O1 2.204(11) 4 ?
U1 O1 2.204(11) 5 ?
U1 N1 2.767(17) 5 ?
U1 N1 2.767(17) . ?
U1 N1 2.767(17) 4 ?
O1 C5 1.32(2) . ?
N1 C1 1.47(2) . ?
N1 C2 1.53(3) . ?
N1 C3 1.49(3) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.54(2) 4 ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C4 1.51(3) . ?
C4 C5 1.41(3) . ?
C4 C9 1.37(3) . ?
C5 C6 1.47(3) . ?
C6 C7 1.41(3) . ?
C6 C10 1.50(3) . ?
C7 H7 0.9500 . ?
C7 C8 1.44(3) . ?
C8 C9 1.38(3) . ?
C8 C20 1.48(3) . ?
C9 H9 0.9500 . ?
C10 C14 1.52(2) . ?
C10 C15 1.55(2) . ?
C10 C18 1.56(3) . ?
C11 H11 1.0000 . ?
C11 C14 1.49(3) . ?
C11 C16 1.53(3) . ?
C11 C19 1.57(3) . ?
C12 H12 1.0000 . ?
C12 C16 1.53(3) . ?
C12 C17 1.56(2) . ?
C12 C18 1.49(3) . ?
C13 H13 1.0000 . ?
C13 C15 1.52(3) . ?
C13 C17 1.50(3) . ?
C13 C19 1.55(3) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
K1 O2 2.801(19) 5_665 ?
K1 O2 2.801(19) . ?
K1 O2 2.801(19) 4_655 ?
K1 O3 2.841(18) 5_665 ?
K1 O3 2.841(19) . ?
K1 O3 2.841(18) 4_655 ?
K1 N2 2.95(4) . ?
K1 N3 2.94(4) . ?
O2 C22 1.43(4) . ?
O2 C23 1.41(3) . ?
O3 C24 1.41(3) . ?
O3 C25 1.39(3) . ?
N2 C21 1.44(3) 4_655 ?
N2 C21 1.44(3) 5_665 ?
N2 C21 1.44(3) . ?
N3 C26 1.47(3) . ?
N3 C26 1.47(3) 5_665 ?
N3 C26 1.47(3) 4_655 ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C21 C22 1.52(3) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C23 C24 1.49(3) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 C26 1.53(4) . ?
C26 H26A 0.9900 . ?
C26 H26B 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 U1 Te1 85.3(4) 4 . ?
O1 U1 Te1 85.3(4) 5 . ?
O1 U1 Te1 85.3(4) . . ?
O1 U1 O1 119.34(12) . 4 ?
O1 U1 O1 119.34(12) 4 5 ?
O1 U1 O1 119.34(12) . 5 ?
O1 U1 N1 83.8(5) 4 . ?
O1 U1 N1 130.8(5) 4 5 ?
O1 U1 N1 83.8(5) . 5 ?
O1 U1 N1 69.6(5) 4 4 ?
O1 U1 N1 83.8(5) 5 4 ?
O1 U1 N1 130.8(5) 5 . ?
O1 U1 N1 69.6(5) . . ?
O1 U1 N1 130.8(5) . 4 ?
O1 U1 N1 69.6(5) 5 5 ?
N1 U1 Te1 142.7(3) . . ?
N1 U1 Te1 142.7(3) 4 . ?
N1 U1 Te1 142.7(3) 5 . ?
N1 U1 N1 63.3(6) . 4 ?
N1 U1 N1 63.3(6) . 5 ?
N1 U1 N1 63.3(6) 4 5 ?
C5 O1 U1 150.2(13) . . ?
C1 N1 U1 106.4(11) . . ?
C1 N1 C2 109.5(16) . . ?
C1 N1 C3 108.1(15) . . ?
C2 N1 U1 116.8(11) . . ?
C3 N1 U1 104.4(12) . . ?
C3 N1 C2 111.2(15) . . ?
N1 C1 H1A 108.9 . . ?
N1 C1 H1B 108.9 . . ?
N1 C1 C2 113.4(16) . 4 ?
H1A C1 H1B 107.7 . . ?
C2 C1 H1A 108.9 4 . ?
C2 C1 H1B 108.9 4 . ?
N1 C2 C1 110.0(17) . 5 ?
N1 C2 H2A 109.7 . . ?
N1 C2 H2B 109.7 . . ?
C1 C2 H2A 109.7 5 . ?
C1 C2 H2B 109.7 5 . ?
H2A C2 H2B 108.2 . . ?
N1 C3 H3A 108.8 . . ?
N1 C3 H3B 108.8 . . ?
N1 C3 C4 113.8(17) . . ?
H3A C3 H3B 107.7 . . ?
C4 C3 H3A 108.8 . . ?
C4 C3 H3B 108.8 . . ?
C5 C4 C3 116.3(19) . . ?
C9 C4 C3 122.3(19) . . ?
C9 C4 C5 121.3(19) . . ?
O1 C5 C4 119.9(18) . . ?
O1 C5 C6 122.2(17) . . ?
C4 C5 C6 117.8(18) . . ?
C5 C6 C10 121.6(16) . . ?
C7 C6 C5 116.5(18) . . ?
C7 C6 C10 121.9(17) . . ?
C6 C7 H7 118.4 . . ?
C6 C7 C8 123(2) . . ?
C8 C7 H7 118.4 . . ?
C7 C8 C20 121(2) . . ?
C9 C8 C7 117(2) . . ?
C9 C8 C20 123(2) . . ?
C4 C9 C8 123(2) . . ?
C4 C9 H9 118.3 . . ?
C8 C9 H9 118.3 . . ?
C6 C10 C14 113.7(19) . . ?
C6 C10 C15 111.1(15) . . ?
C6 C10 C18 109.3(14) . . ?
C14 C10 C15 107.1(14) . . ?
C14 C10 C18 107.5(16) . . ?
C15 C10 C18 107.8(18) . . ?
C14 C11 H11 110.4 . . ?
C14 C11 C16 109.0(17) . . ?
C14 C11 C19 110.3(16) . . ?
C16 C11 H11 110.4 . . ?
C16 C11 C19 106.2(18) . . ?
C19 C11 H11 110.4 . . ?
C16 C12 H12 109.1 . . ?
C16 C12 C17 109.5(16) . . ?
C17 C12 H12 109.1 . . ?
C18 C12 H12 109.1 . . ?
C18 C12 C16 110.9(18) . . ?
C18 C12 C17 109.0(17) . . ?
C15 C13 H13 109.6 . . ?
C15 C13 C19 109.5(19) . . ?
C17 C13 H13 109.6 . . ?
C17 C13 C15 110.2(18) . . ?
C17 C13 C19 108.3(18) . . ?
C19 C13 H13 109.6 . . ?
C10 C14 H14A 108.8 . . ?
C10 C14 H14B 108.8 . . ?
C11 C14 C10 114.0(19) . . ?
C11 C14 H14A 108.8 . . ?
C11 C14 H14B 108.8 . . ?
H14A C14 H14B 107.7 . . ?
C10 C15 H15A 109.3 . . ?
C10 C15 H15B 109.3 . . ?
C13 C15 C10 111.5(17) . . ?
C13 C15 H15A 109.3 . . ?
C13 C15 H15B 109.3 . . ?
H15A C15 H15B 108.0 . . ?
C11 C16 H16A 109.7 . . ?
C11 C16 H16B 109.7 . . ?
C12 C16 C11 109.7(16) . . ?
C12 C16 H16A 109.7 . . ?
C12 C16 H16B 109.7 . . ?
H16A C16 H16B 108.2 . . ?
C12 C17 H17A 109.8 . . ?
C12 C17 H17B 109.8 . . ?
C13 C17 C12 109.4(17) . . ?
C13 C17 H17A 109.8 . . ?
C13 C17 H17B 109.8 . . ?
H17A C17 H17B 108.2 . . ?
C10 C18 H18A 109.5 . . ?
C10 C18 H18B 109.5 . . ?
C12 C18 C10 110.8(17) . . ?
C12 C18 H18A 109.5 . . ?
C12 C18 H18B 109.5 . . ?
H18A C18 H18B 108.1 . . ?
C11 C19 H19A 109.8 . . ?
C11 C19 H19B 109.8 . . ?
C13 C19 C11 109.2(17) . . ?
C13 C19 H19A 109.8 . . ?
C13 C19 H19B 109.8 . . ?
H19A C19 H19B 108.3 . . ?
C8 C20 H20A 109.5 . . ?
C8 C20 H20B 109.5 . . ?
C8 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O2 K1 O2 98.3(6) 5_665 . ?
O2 K1 O2 98.3(6) 5_665 4_655 ?
O2 K1 O2 98.3(6) . 4_655 ?
O2 K1 O3 58.5(6) 5_665 5_665 ?
O2 K1 O3 58.5(6) . . ?
O2 K1 O3 119.4(5) . 4_655 ?
O2 K1 O3 136.9(5) . 5_665 ?
O2 K1 O3 136.9(5) 4_655 . ?
O2 K1 O3 119.4(5) 4_655 5_665 ?
O2 K1 O3 58.5(6) 4_655 4_655 ?
O2 K1 O3 119.4(5) 5_665 . ?
O2 K1 O3 136.9(5) 5_665 4_655 ?
O2 K1 N2 60.8(5) 4_655 . ?
O2 K1 N2 60.8(5) . . ?
O2 K1 N2 60.8(5) 5_665 . ?
O2 K1 N3 119.2(5) 4_655 . ?
O2 K1 N3 119.2(5) 5_665 . ?
O2 K1 N3 119.2(5) . . ?
O3 K1 O3 99.1(6) . 4_655 ?
O3 K1 O3 99.1(6) 5_665 4_655 ?
O3 K1 O3 99.1(6) 5_665 . ?
O3 K1 N2 118.5(4) . . ?
O3 K1 N2 118.5(4) 4_655 . ?
O3 K1 N2 118.5(4) 5_665 . ?
O3 K1 N3 61.5(4) 4_655 . ?
O3 K1 N3 61.5(4) . . ?
O3 K1 N3 61.5(4) 5_665 . ?
N3 K1 N2 180.000(12) . . ?
C22 O2 K1 121.3(15) . . ?
C23 O2 K1 118.9(17) . . ?
C23 O2 C22 109.9(19) . . ?
C24 O3 K1 115.4(14) . . ?
C25 O3 K1 114.1(18) . . ?
C25 O3 C24 111(2) . . ?
C21 N2 K1 107.7(18) 4_655 . ?
C21 N2 K1 107.7(18) 5_665 . ?
C21 N2 K1 107.7(18) . . ?
C21 N2 C21 111.1(17) 5_665 . ?
C21 N2 C21 111.1(17) 5_665 4_655 ?
C21 N2 C21 111.1(17) 4_655 . ?
C26 N3 K1 109.8(18) . . ?
C26 N3 K1 109.8(18) 4_655 . ?
C26 N3 K1 109.8(18) 5_665 . ?
C26 N3 C26 109.2(19) 5_665 . ?
C26 N3 C26 109.2(19) . 4_655 ?
C26 N3 C26 109.2(19) 5_665 4_655 ?
N2 C21 H21A 108.0 . . ?
N2 C21 H21B 108.0 . . ?
N2 C21 C22 117(2) . . ?
H21A C21 H21B 107.3 . . ?
C22 C21 H21A 108.0 . . ?
C22 C21 H21B 108.0 . . ?
O2 C22 C21 108(2) . . ?
O2 C22 H22A 110.2 . . ?
O2 C22 H22B 110.2 . . ?
C21 C22 H22A 110.2 . . ?
C21 C22 H22B 110.2 . . ?
H22A C22 H22B 108.5 . . ?
O2 C23 H23A 110.3 . . ?
O2 C23 H23B 110.3 . . ?
O2 C23 C24 107(2) . . ?
H23A C23 H23B 108.5 . . ?
C24 C23 H23A 110.3 . . ?
C24 C23 H23B 110.3 . . ?
O3 C24 C23 111(2) . . ?
O3 C24 H24A 109.5 . . ?
O3 C24 H24B 109.5 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 108.1 . . ?
O3 C25 H25A 109.8 . . ?
O3 C25 H25B 109.8 . . ?
O3 C25 C26 110(3) . . ?
H25A C25 H25B 108.2 . . ?
C26 C25 H25A 109.8 . . ?
C26 C25 H25B 109.8 . . ?
N3 C26 C25 113(3) . . ?
N3 C26 H26A 109.0 . . ?
N3 C26 H26B 109.0 . . ?
C25 C26 H26A 109.0 . . ?
C25 C26 H26B 109.0 . . ?
H26A C26 H26B 107.8 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
U1 O1 C5 C4 15(4) . . . . ?
U1 O1 C5 C6 -164.9(16) . . . . ?
U1 N1 C1 C2 -62.9(18) . . . 4 ?
U1 N1 C2 C1 -11.4(18) . . . 5 ?
U1 N1 C3 C4 80.4(16) . . . . ?
O1 C5 C6 C7 168.0(17) . . . . ?
O1 C5 C6 C10 -13(3) . . . . ?
N1 C3 C4 C5 -63(2) . . . . ?
N1 C3 C4 C9 114(2) . . . . ?
C1 N1 C2 C1 -132.4(16) . . . 5 ?
C1 N1 C3 C4 -166.6(17) . . . . ?
C2 N1 C1 C2 64(2) . . . 4 ?
C2 N1 C3 C4 -46(2) . . . . ?
C3 N1 C1 C2 -174.6(17) . . . 4 ?
C3 N1 C2 C1 108.1(17) . . . 5 ?
C3 C4 C5 O1 8(3) . . . . ?
C3 C4 C5 C6 -171.7(17) . . . . ?
C3 C4 C9 C8 -179(2) . . . . ?
C4 C5 C6 C7 -12(3) . . . . ?
C4 C5 C6 C10 167.2(17) . . . . ?
C5 C4 C9 C8 -1(3) . . . . ?
C5 C6 C7 C8 5(3) . . . . ?
C5 C6 C10 C14 69(2) . . . . ?
C5 C6 C10 C15 -170.3(17) . . . . ?
C5 C6 C10 C18 -51(2) . . . . ?
C6 C7 C8 C9 3(3) . . . . ?
C6 C7 C8 C20 -179(2) . . . . ?
C6 C10 C14 C11 -178.5(15) . . . . ?
C6 C10 C15 C13 176.1(17) . . . . ?
C6 C10 C18 C12 -179.8(15) . . . . ?
C7 C6 C10 C14 -112.0(19) . . . . ?
C7 C6 C10 C15 9(3) . . . . ?
C7 C6 C10 C18 127.8(19) . . . . ?
C7 C8 C9 C4 -6(3) . . . . ?
C9 C4 C5 O1 -169.6(19) . . . . ?
C9 C4 C5 C6 10(3) . . . . ?
C10 C6 C7 C8 -173.8(19) . . . . ?
C14 C10 C15 C13 -59(2) . . . . ?
C14 C10 C18 C12 56(2) . . . . ?
C14 C11 C16 C12 -57(2) . . . . ?
C14 C11 C19 C13 55(2) . . . . ?
C15 C10 C14 C11 58(2) . . . . ?
C15 C10 C18 C12 -59(2) . . . . ?
C15 C13 C17 C12 59(2) . . . . ?
C15 C13 C19 C11 -57(2) . . . . ?
C16 C11 C14 C10 59(2) . . . . ?
C16 C11 C19 C13 -63(2) . . . . ?
C16 C12 C17 C13 60(2) . . . . ?
C16 C12 C18 C10 -59(2) . . . . ?
C17 C12 C16 C11 -61(2) . . . . ?
C17 C12 C18 C10 61(2) . . . . ?
C17 C13 C15 C10 -58(2) . . . . ?
C17 C13 C19 C11 63(2) . . . . ?
C18 C10 C14 C11 -57(2) . . . . ?
C18 C10 C15 C13 56(2) . . . . ?
C18 C12 C16 C11 59(2) . . . . ?
C18 C12 C17 C13 -61(2) . . . . ?
C19 C11 C14 C10 -58(2) . . . . ?
C19 C11 C16 C12 62(2) . . . . ?
C19 C13 C15 C10 61(2) . . . . ?
C19 C13 C17 C12 -61(2) . . . . ?
C20 C8 C9 C4 177(2) . . . . ?
K1 O2 C22 C21 36(2) . . . . ?
K1 O2 C23 C24 -47(2) . . . . ?
K1 O3 C24 C23 -47(2) . . . . ?
K1 O3 C25 C26 53(3) . . . . ?
K1 N2 C21 C22 50(2) . . . . ?
K1 N3 C26 C25 43(3) . . . . ?
O2 C23 C24 O3 61(3) . . . . ?
O3 C25 C26 N3 -67(4) . . . . ?
N2 C21 C22 O2 -60(3) . . . . ?
C21 N2 C21 C22 -67(4) 5_665 . . . ?
C21 N2 C21 C22 168(2) 4_655 . . . ?
C22 O2 C23 C24 167(2) . . . . ?
C23 O2 C22 C21 -179.0(19) . . . . ?
C24 O3 C25 C26 -174(2) . . . . ?
C25 O3 C24 C23 -179(2) . . . . ?
C26 N3 C26 C25 -77(4) 4_655 . . . ?
C26 N3 C26 C25 163(3) 5_665 . . . ?

_olex2_submission_special_instructions 'No special instructions were received'

# start Validation Reply Form
_vrf_RINTA01_mr1601              
;
PROBLEM: The value of Rint is greater than 0.25
RESPONSE: he crystal under study was a tiny, weakly diffracting needle
(as were all crystals of the sample).
;
_vrf_PLAT232_mr1601              
;
PROBLEM: Hirshfeld Test Diff (M-X)  U1       --Te1      .       12.3 s.u.  
RESPONSE: The identity of the Te atom is without doubt. There might be some
slight unresolved disorder which can be not resolved due to the poor data 
quality.
;
_vrf_PLAT342_mr1601              
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............     0.0332 Ang.  
RESPONSE: The crystal under study was a tiny, weakly diffracting needle
and the overall data quality was rather poor.
;
_vrf_PLAT972_mr1601              
;
PROBLEM: Check Calcd Resid. Dens.  1.69A   From C2             -3.12 eA-3  
RESPONSE: This residual density is an artefact, probably due to the poor
data quality. It has no chemical meaning.
;
_vrf_PLAT973_mr1601              
;
PROBLEM: Check Calcd Positive Resid. Density on        U1       1.59 eA-3  
RESPONSE: This residual density is an artefact, probably due to the poor
data quality. It has no chemical meaning.
;
_vrf_PLAT987_mr1601              
;
PROBLEM: The Flack x is >> 0 -  Do a BASF/TWIN Refinement     Please Check 
RESPONSE: Refinement of the absolute structure parameter yielded a value of
0.044(9) which confidently confirmed that the refined model represents the 
true absolute structure.
;
# end Validation Reply Form






#===END OF ALL DATA





####################################################################### 
# 
# 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_mr1528
_database_code_depnum_ccdc_archive 'CCDC 1893560'
loop_
_audit_author_name
_audit_author_address
'Frank W. Heinemann'
;Friedrich-Alexander-Universit?t Erlangen-N?rnberg
Germany
;
_audit_update_record             
;
2019-01-25 deposited with the CCDC.	2019-03-25 downloaded from the CCDC.
;
_audit_creation_date             2019-01-24
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C60 H79 N3 O3 Te U, 3(C1 H2 Cl2)'
_chemical_formula_sum            'C63 H85 Cl6 N3 O3 Te U'
_chemical_formula_weight         1510.67
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   10.3450(4)
_cell_length_b                   25.1895(11)
_cell_length_c                   23.6311(9)
_cell_angle_alpha                90
_cell_angle_beta                 90.534(2)
_cell_angle_gamma                90
_cell_volume                     6157.7(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9627
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.04
_cell_measurement_theta_min      2.29
_shelx_estimated_absorpt_T_max   0.822
_shelx_estimated_absorpt_T_min   0.508
_exptl_absorpt_coefficient_mu    3.408
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6120
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0796 before and 0.0598 after correction.
The Ratio of minimum to maximum transmission is 0.8206.
The λ/2 correction factor is 0.0015.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.630
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             3016
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.075
_exptl_crystal_size_min          0.06
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0916
_diffrn_reflns_av_unetI/netI     0.0636
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            110112
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         2.128
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.981
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_monochromator  'Triumph curved graphite'
_diffrn_measurement_device_type  'Bruker Smart APEX II CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 83.33
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9464
_reflns_number_total             12556
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELX XT 2014/5 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2015)'
_computing_molecular_graphics    'SHELXTL 6.12 (Bruker AXS, 2002)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_refine_diff_density_max         2.317
_refine_diff_density_min         -3.020
_refine_diff_density_rms         0.182
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     780
_refine_ls_number_reflns         12556
_refine_ls_number_restraints     219
_refine_ls_R_factor_all          0.0920
_refine_ls_R_factor_gt           0.0597
_refine_ls_restrained_S_all      1.111
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0502P)²+67.7713P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1258
_refine_ls_wR_factor_ref         0.1386
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.9966(4)
 0.0034(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All Te(H) groups
3. Uiso/Uaniso restraints and constraints
C1 \\sim C6 \\sim N1: within 2A with sigma of 0.005 and sigma for terminal
atoms of 0.01
C100 \\sim Cl11 \\sim Cl12 \\sim C101 \\sim Cl13 \\sim Cl14: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
C200 \\sim Cl21 \\sim Cl22 \\sim C201 \\sim Cl23 \\sim Cl24: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
C300 \\sim Cl31 \\sim Cl32 \\sim C301 \\sim Cl33 \\sim Cl34: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N1) \\sim Ueq: with sigma of 0.003 and sigma for terminal atoms of 0.006
Uanis(Cl31) \\sim Ueq, Uanis(Cl32) \\sim Ueq, Uanis(Cl33) \\sim Ueq,
Uanis(Cl34) \\sim Ueq, Uanis(Cl24) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Same fragment restrains
{C100, Cl11, Cl12} sigma for 1-2: 0.02, 1-3: 0.04
as
{C101, Cl13, Cl14}
{C100, Cl11, Cl12} sigma for 1-2: 0.02, 1-3: 0.04
as
{C200, Cl21, Cl22}
{C100, Cl11, Cl12} sigma for 1-2: 0.02, 1-3: 0.04
as
{C201, Cl23, Cl24}
{C100, Cl11, Cl12} sigma for 1-2: 0.02, 1-3: 0.04
as
{C300, Cl31, Cl32}
{C100, Cl11, Cl12} sigma for 1-2: 0.02, 1-3: 0.04
as
{C301, Cl33, Cl34}
5. Others
 Sof(C301)=Sof(H30C)=Sof(H30D)=Sof(Cl33)=Sof(Cl34)=1-FVAR(1)
 Sof(C300)=Sof(H30A)=Sof(H30B)=Sof(Cl31)=Sof(Cl32)=FVAR(1)
 Sof(C201)=Sof(H20E)=Sof(H20F)=Sof(Cl23)=Sof(Cl24)=1-FVAR(2)
 Sof(C200)=Sof(H20C)=Sof(H20D)=Sof(Cl21)=Sof(Cl22)=FVAR(2)
 Sof(C101)=Sof(H10C)=Sof(H10D)=Sof(Cl13)=Sof(Cl14)=1-FVAR(3)
 Sof(C100)=Sof(H10A)=Sof(H10B)=Sof(Cl11)=Sof(Cl12)=FVAR(3)
6.a Ternary CH refined with riding coordinates:
 C15(H15), C16(H16), C17(H17), C33(H33), C34(H34), C35(H35), C51(H51),
 C52(H52), C53(H53)
6.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B),
 C7(H7A,H7B), C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B),
 C22(H22A,H22B), C23(H23A,H23B), C25(H25A,H25B), C36(H36A,H36B), C37(H37A,H37B),
  C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B), C41(H41A,H41B), C43(H43A,
 H43B), C54(H54A,H54B), C55(H55A,H55B), C56(H56A,H56B), C57(H57A,H57B),
 C58(H58A,H58B), C59(H59A,H59B), C100(H10A,H10B), C101(H10C,H10D), C200(H20C,
 H20D), C201(H20E,H20F), C300(H30A,H30B), C301(H30C,H30D)
6.c Me refined with riding coordinates:
 C24(H24A,H24B,H24C), C42(H42A,H42B,H42C), C60(H60A,H60B,H60C)
6.d Aromatic/amide H refined with riding coordinates:
 C11(H11), C13(H13), C29(H29), C31(H31), C47(H47), C49(H49)
6.e Idealised tetrahedral OH refined as rotating group:
 Te1(H1)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.14029(2) 0.18919(2) 0.35297(2) 0.01569(9) Uani 1 1 d . . . . .
Te1 Te -0.15178(6) 0.16013(3) 0.32492(3) 0.03208(16) Uani 1 1 d . . . . .
H1 H -0.166373 0.128660 0.334724 0.048 Uiso 1 1 calc GR . . . .
O1 O 0.1109(5) 0.1409(2) 0.4278(2) 0.0166(11) Uani 1 1 d . . . . .
O2 O 0.0512(5) 0.2659(2) 0.3393(2) 0.0214(12) Uani 1 1 d . . . . .
O3 O 0.1898(5) 0.1497(2) 0.2749(2) 0.0205(12) Uani 1 1 d . . . . .
N1 N 0.3659(6) 0.1543(3) 0.3895(3) 0.0233(13) Uani 1 1 d . U . . .
N2 N 0.2586(6) 0.2564(3) 0.4200(3) 0.0227(15) Uani 1 1 d . . . . .
N3 N 0.3433(6) 0.2387(3) 0.3066(3) 0.0240(16) Uani 1 1 d . . . . .
C1 C 0.4200(7) 0.1843(4) 0.4392(3) 0.0267(16) Uani 1 1 d . U . . .
H1A H 0.497385 0.204259 0.427139 0.032 Uiso 1 1 calc R . . . .
H1B H 0.447328 0.158741 0.468815 0.032 Uiso 1 1 calc R . . . .
C2 C 0.3222(8) 0.2227(4) 0.4639(3) 0.027(2) Uani 1 1 d . . . . .
H2A H 0.255249 0.202342 0.484201 0.033 Uiso 1 1 calc R . . . .
H2B H 0.366527 0.245946 0.491766 0.033 Uiso 1 1 calc R . . . .
C3 C 0.3541(8) 0.2934(4) 0.3940(4) 0.027(2) Uani 1 1 d . . . . .
H3A H 0.442380 0.283002 0.406096 0.033 Uiso 1 1 calc R . . . .
H3B H 0.337966 0.329838 0.407851 0.033 Uiso 1 1 calc R . . . .
C4 C 0.3464(7) 0.2932(4) 0.3294(3) 0.0248(19) Uani 1 1 d . . . . .
H4A H 0.267646 0.312324 0.316923 0.030 Uiso 1 1 calc R . . . .
H4B H 0.422239 0.312127 0.314048 0.030 Uiso 1 1 calc R . . . .
C5 C 0.4718(7) 0.2110(4) 0.3164(4) 0.031(2) Uani 1 1 d . . . . .
H5A H 0.518228 0.208471 0.280066 0.037 Uiso 1 1 calc R . . . .
H5B H 0.525349 0.232524 0.342703 0.037 Uiso 1 1 calc R . . . .
C6 C 0.4557(8) 0.1560(4) 0.3407(3) 0.0267(16) Uani 1 1 d . U . . .
H6A H 0.422772 0.132114 0.310619 0.032 Uiso 1 1 calc R . . . .
H6B H 0.541379 0.142598 0.353049 0.032 Uiso 1 1 calc R . . . .
C7 C 0.3510(7) 0.0968(4) 0.4047(3) 0.0240(19) Uani 1 1 d . . . . .
H7A H 0.437981 0.080610 0.407310 0.029 Uiso 1 1 calc R . . . .
H7B H 0.303628 0.078769 0.373540 0.029 Uiso 1 1 calc R . . . .
C8 C 0.2811(7) 0.0864(3) 0.4591(3) 0.0171(16) Uani 1 1 d . . . . .
C9 C 0.1581(7) 0.1076(3) 0.4679(3) 0.0156(16) Uani 1 1 d . . . . .
C10 C 0.0879(7) 0.0937(3) 0.5172(3) 0.0140(15) Uani 1 1 d . . . . .
C11 C 0.1500(7) 0.0591(3) 0.5553(3) 0.0153(15) Uani 1 1 d . . . . .
H11 H 0.104508 0.048948 0.588357 0.018 Uiso 1 1 calc R . . . .
C12 C 0.2733(7) 0.0388(3) 0.5480(3) 0.0164(16) Uani 1 1 d . . . . .
C13 C 0.3385(7) 0.0534(3) 0.4991(3) 0.0183(16) Uani 1 1 d . . . . .
H13 H 0.423553 0.040532 0.493017 0.022 Uiso 1 1 calc R . . . .
C14 C -0.0468(7) 0.1160(3) 0.5293(3) 0.0165(16) Uani 1 1 d . . . . .
C15 C -0.2749(7) 0.1264(4) 0.4918(3) 0.0248(19) Uani 1 1 d . . . . .
H15 H -0.334319 0.117751 0.459488 0.030 Uiso 1 1 calc R . . . .
C16 C -0.1722(7) 0.2007(3) 0.5463(3) 0.0204(18) Uani 1 1 d . . . . .
H16 H -0.164804 0.240099 0.549818 0.024 Uiso 1 1 calc R . . . .
C17 C -0.2381(7) 0.1174(3) 0.5954(3) 0.0245(18) Uani 1 1 d . . . . .
H17 H -0.272898 0.102370 0.631370 0.029 Uiso 1 1 calc R . . . .
C18 C -0.1410(7) 0.1017(3) 0.4806(3) 0.0190(17) Uani 1 1 d . . . . .
H18A H -0.149158 0.062668 0.477652 0.023 Uiso 1 1 calc R . . . .
H18B H -0.106918 0.115268 0.444360 0.023 Uiso 1 1 calc R . . . .
C19 C -0.1044(7) 0.0937(3) 0.5844(3) 0.0172(16) Uani 1 1 d . . . . .
H19A H -0.111461 0.054645 0.581514 0.021 Uiso 1 1 calc R . . . .
H19B H -0.045880 0.102143 0.616552 0.021 Uiso 1 1 calc R . . . .
C20 C -0.2627(7) 0.1869(4) 0.4969(3) 0.0251(18) Uani 1 1 d . . . . .
H20A H -0.228076 0.201719 0.461348 0.030 Uiso 1 1 calc R . . . .
H20B H -0.348947 0.202693 0.503365 0.030 Uiso 1 1 calc R . . . .
C21 C -0.2259(7) 0.1775(3) 0.6012(3) 0.0219(18) Uani 1 1 d . . . . .
H21A H -0.167329 0.186203 0.633216 0.026 Uiso 1 1 calc R . . . .
H21B H -0.311715 0.193114 0.608973 0.026 Uiso 1 1 calc R . . . .
C22 C -0.0389(7) 0.1769(3) 0.5354(3) 0.0179(17) Uani 1 1 d . . . . .
H22A H 0.020072 0.185987 0.567148 0.022 Uiso 1 1 calc R . . . .
H22B H -0.003031 0.192348 0.500356 0.022 Uiso 1 1 calc R . . . .
C23 C -0.3307(7) 0.1038(4) 0.5462(3) 0.0261(19) Uani 1 1 d . . . . .
H23A H -0.340172 0.064779 0.542894 0.031 Uiso 1 1 calc R . . . .
H23B H -0.417040 0.119251 0.553218 0.031 Uiso 1 1 calc R . . . .
C24 C 0.3342(8) 0.0037(3) 0.5921(3) 0.0233(18) Uani 1 1 d . . . . .
H24A H 0.420689 -0.006852 0.579839 0.035 Uiso 1 1 calc R . . . .
H24B H 0.340845 0.023060 0.627968 0.035 Uiso 1 1 calc R . . . .
H24C H 0.280753 -0.028036 0.597264 0.035 Uiso 1 1 calc R . . . .
C25 C 0.1485(8) 0.2875(4) 0.4463(3) 0.029(2) Uani 1 1 d . . . . .
H25A H 0.079559 0.262114 0.456688 0.034 Uiso 1 1 calc R . . . .
H25B H 0.180761 0.303995 0.481679 0.034 Uiso 1 1 calc R . . . .
C26 C 0.0901(8) 0.3297(3) 0.4103(3) 0.0204(17) Uani 1 1 d . . . . .
C27 C 0.0357(7) 0.3169(3) 0.3573(3) 0.0211(17) Uani 1 1 d . . . . .
C28 C -0.0302(8) 0.3557(3) 0.3252(3) 0.0241(18) Uani 1 1 d . . . . .
C29 C -0.0348(9) 0.4066(4) 0.3481(4) 0.031(2) Uani 1 1 d . . . . .
H29 H -0.077691 0.433557 0.326988 0.037 Uiso 1 1 calc R . . . .
C30 C 0.0200(9) 0.4204(4) 0.4003(4) 0.033(2) Uani 1 1 d . . . . .
C31 C 0.0844(9) 0.3806(4) 0.4306(4) 0.032(2) Uani 1 1 d . . . . .
H31 H 0.124778 0.388969 0.465743 0.038 Uiso 1 1 calc R . . . .
C32 C -0.1000(7) 0.3425(3) 0.2694(3) 0.0213(17) Uani 1 1 d . . . . .
C33 C -0.2798(8) 0.2879(4) 0.2254(3) 0.029(2) Uani 1 1 d . . . . .
H33 H -0.348447 0.261154 0.233714 0.035 Uiso 1 1 calc R . . . .
C34 C -0.0796(7) 0.3048(4) 0.1699(3) 0.0244(18) Uani 1 1 d . . . . .
H34 H -0.017501 0.289338 0.142222 0.029 Uiso 1 1 calc R . . . .
C35 C -0.2355(8) 0.3780(4) 0.1875(4) 0.033(2) Uani 1 1 d . . . . .
H35 H -0.275288 0.410783 0.171082 0.039 Uiso 1 1 calc R . . . .
C36 C -0.2094(7) 0.3020(4) 0.2803(3) 0.027(2) Uani 1 1 d . . . . .
H36A H -0.172276 0.269347 0.297282 0.032 Uiso 1 1 calc R . . . .
H36B H -0.271534 0.317164 0.307475 0.032 Uiso 1 1 calc R . . . .
C37 C -0.1635(8) 0.3923(4) 0.2421(3) 0.029(2) Uani 1 1 d . . . . .
H37A H -0.224630 0.408406 0.269121 0.034 Uiso 1 1 calc R . . . .
H37B H -0.095783 0.418921 0.233739 0.034 Uiso 1 1 calc R . . . .
C38 C -0.1846(8) 0.2640(4) 0.1832(4) 0.029(2) Uani 1 1 d . . . . .
H38A H -0.144674 0.231671 0.199576 0.035 Uiso 1 1 calc R . . . .
H38B H -0.230914 0.253916 0.148022 0.035 Uiso 1 1 calc R . . . .
C39 C -0.1419(8) 0.3543(4) 0.1447(4) 0.031(2) Uani 1 1 d . . . . .
H39A H -0.189123 0.344976 0.109455 0.037 Uiso 1 1 calc R . . . .
H39B H -0.074422 0.380617 0.135333 0.037 Uiso 1 1 calc R . . . .
C40 C -0.0069(7) 0.3190(3) 0.2254(3) 0.0198(17) Uani 1 1 d . . . . .
H40A H 0.034438 0.286723 0.241150 0.024 Uiso 1 1 calc R . . . .
H40B H 0.061933 0.345117 0.217231 0.024 Uiso 1 1 calc R . . . .
C41 C -0.3432(8) 0.3374(4) 0.2003(4) 0.038(2) Uani 1 1 d . . . . .
H41A H -0.405269 0.352676 0.227466 0.045 Uiso 1 1 calc R . . . .
H41B H -0.390702 0.328204 0.165084 0.045 Uiso 1 1 calc R . . . .
C42 C 0.0060(12) 0.4759(4) 0.4235(4) 0.050(3) Uani 1 1 d . . . . .
H42A H 0.050268 0.478352 0.460224 0.075 Uiso 1 1 calc R . . . .
H42B H 0.044568 0.501315 0.397107 0.075 Uiso 1 1 calc R . . . .
H42C H -0.085850 0.484181 0.428092 0.075 Uiso 1 1 calc R . . . .
C43 C 0.3154(8) 0.2434(3) 0.2444(3) 0.0231(18) Uani 1 1 d . . . . .
H43A H 0.376084 0.269598 0.228246 0.028 Uiso 1 1 calc R . . . .
H43B H 0.226958 0.257853 0.239494 0.028 Uiso 1 1 calc R . . . .
C44 C 0.3249(7) 0.1927(4) 0.2104(3) 0.0244(18) Uani 1 1 d . . . . .
C45 C 0.2569(8) 0.1475(4) 0.2265(3) 0.0248(19) Uani 1 1 d . . . . .
C46 C 0.2617(8) 0.1011(4) 0.1923(3) 0.0265(19) Uani 1 1 d . . . . .
C47 C 0.3313(8) 0.1045(4) 0.1417(4) 0.030(2) Uani 1 1 d . . . . .
H47 H 0.332336 0.074396 0.117402 0.036 Uiso 1 1 calc R . . . .
C48 C 0.3983(9) 0.1493(4) 0.1254(4) 0.033(2) Uani 1 1 d . . . . .
C49 C 0.3960(8) 0.1929(4) 0.1605(3) 0.027(2) Uani 1 1 d . . . . .
H49 H 0.443592 0.223747 0.150490 0.032 Uiso 1 1 calc R . . . .
C50 C 0.1926(8) 0.0494(4) 0.2091(3) 0.028(2) Uani 1 1 d . . . . .
C51 C -0.0225(9) 0.0052(4) 0.2292(5) 0.042(3) Uani 1 1 d . . . . .
H51 H -0.118096 0.011052 0.229796 0.050 Uiso 1 1 calc R . . . .
C52 C 0.1702(9) -0.0193(4) 0.2870(4) 0.033(2) Uani 1 1 d . . . . .
H52 H 0.201594 -0.029408 0.325652 0.040 Uiso 1 1 calc R . . . .
C53 C 0.1530(11) -0.0481(4) 0.1867(4) 0.048(3) Uani 1 1 d . . . . .
H53 H 0.172634 -0.077172 0.159310 0.057 Uiso 1 1 calc R . . . .
C54 C 0.0454(8) 0.0571(4) 0.2105(4) 0.034(2) Uani 1 1 d . . . . .
H54A H 0.013698 0.067442 0.172408 0.041 Uiso 1 1 calc R . . . .
H54B H 0.024091 0.086015 0.237159 0.041 Uiso 1 1 calc R . . . .
C55 C 0.2212(11) 0.0034(4) 0.1683(4) 0.041(2) Uani 1 1 d . . . . .
H55A H 0.315703 -0.002688 0.167187 0.049 Uiso 1 1 calc R . . . .
H55B H 0.191801 0.013210 0.129745 0.049 Uiso 1 1 calc R . . . .
C56 C 0.0245(9) -0.0097(4) 0.2882(4) 0.039(2) Uani 1 1 d . . . . .
H56A H -0.020273 -0.042224 0.301076 0.047 Uiso 1 1 calc R . . . .
H56B H 0.004728 0.019277 0.315087 0.047 Uiso 1 1 calc R . . . .
C57 C 0.1997(10) -0.0639(4) 0.2457(4) 0.041(2) Uani 1 1 d . . . . .
H57A H 0.155724 -0.096826 0.257753 0.049 Uiso 1 1 calc R . . . .
H57B H 0.293950 -0.070679 0.245213 0.049 Uiso 1 1 calc R . . . .
C58 C 0.2377(9) 0.0318(4) 0.2681(4) 0.031(2) Uani 1 1 d . . . . .
H58A H 0.219440 0.060380 0.295651 0.038 Uiso 1 1 calc R . . . .
H58B H 0.332360 0.025930 0.267847 0.038 Uiso 1 1 calc R . . . .
C59 C 0.0082(12) -0.0385(5) 0.1881(5) 0.053(3) Uani 1 1 d . . . . .
H59A H -0.023068 -0.028546 0.149811 0.063 Uiso 1 1 calc R . . . .
H59B H -0.036520 -0.071468 0.199507 0.063 Uiso 1 1 calc R . . . .
C60 C 0.4719(11) 0.1499(4) 0.0703(4) 0.044(3) Uani 1 1 d . . . . .
H60A H 0.462177 0.115461 0.051360 0.067 Uiso 1 1 calc R . . . .
H60B H 0.437585 0.177969 0.045716 0.067 Uiso 1 1 calc R . . . .
H60C H 0.563709 0.156539 0.078108 0.067 Uiso 1 1 calc R . . . .
C100 C 0.065(2) -0.1711(9) -0.0830(10) 0.101(5) Uani 0.726(7) 1 d D U P A 1
H10A H 0.135372 -0.197794 -0.083174 0.122 Uiso 0.726(7) 1 calc R . P A 1
H10B H 0.061728 -0.154912 -0.121115 0.122 Uiso 0.726(7) 1 calc R . P A 1
Cl11 Cl 0.1049(7) -0.1250(3) -0.0380(3) 0.117(3) Uani 0.726(7) 1 d D U P A 1
Cl12 Cl -0.0775(4) -0.20410(18) -0.0728(2) 0.0689(15) Uani 0.726(7) 1 d D U P A
1
C101 C -0.131(4) -0.173(3) -0.0667(13) 0.116(6) Uani 0.274(7) 1 d D U P A 2
H10C H -0.202723 -0.154644 -0.086264 0.139 Uiso 0.274(7) 1 calc R . P A 2
H10D H -0.137393 -0.211359 -0.076988 0.139 Uiso 0.274(7) 1 calc R . P A 2
Cl13 Cl -0.1531(18) -0.1682(8) 0.0007(9) 0.121(6) Uani 0.274(7) 1 d D U P A 2
Cl14 Cl 0.008(2) -0.1499(9) -0.0917(9) 0.117(5) Uani 0.274(7) 1 d D U P A 2
C200 C 0.1297(18) 0.4092(7) 0.7187(7) 0.056(4) Uani 0.658(18) 1 d D U P B 1
H20C H 0.041987 0.395562 0.710086 0.067 Uiso 0.658(18) 1 calc R . P B 1
H20D H 0.174018 0.381724 0.741732 0.067 Uiso 0.658(18) 1 calc R . P B 1
Cl21 Cl 0.1123(9) 0.4623(4) 0.7596(4) 0.0481(18) Uani 0.658(18) 1 d D U P B 1
Cl22 Cl 0.2098(5) 0.4134(4) 0.6560(3) 0.069(3) Uani 0.658(18) 1 d D U P B 1
C201 C 0.184(4) 0.4135(11) 0.6987(12) 0.068(5) Uani 0.342(18) 1 d D U P B 2
H20E H 0.125291 0.382949 0.692196 0.082 Uiso 0.342(18) 1 calc R . P B 2
H20F H 0.260933 0.400296 0.719309 0.082 Uiso 0.342(18) 1 calc R . P B 2
Cl23 Cl 0.110(2) 0.4566(9) 0.7386(9) 0.071(4) Uani 0.342(18) 1 d D U P B 2
Cl24 Cl 0.2305(16) 0.4379(8) 0.6350(8) 0.099(4) Uani 0.342(18) 1 d D U P B 2
C300 C -0.226(2) -0.1347(8) 0.0495(9) 0.098(6) Uani 0.537(7) 1 d D U P C 1
H30A H -0.312840 -0.118891 0.053147 0.117 Uiso 0.537(7) 1 calc R . P C 1
H30B H -0.193424 -0.127937 0.010831 0.117 Uiso 0.537(7) 1 calc R . P C 1
Cl31 Cl -0.2280(6) -0.1960(4) 0.0630(2) 0.088(3) Uani 0.537(7) 1 d D U P C 1
Cl32 Cl -0.1264(8) -0.1111(4) 0.0973(4) 0.112(3) Uani 0.537(7) 1 d D U P C 1
C301 C 0.145(4) 0.0217(11) -0.0179(17) 0.140(7) Uani 0.463(7) 1 d D U P C 2
H30C H 0.181464 0.007999 -0.053670 0.169 Uiso 0.463(7) 1 calc R . P C 2
H30D H 0.055492 0.032069 -0.027377 0.169 Uiso 0.463(7) 1 calc R . P C 2
Cl33 Cl 0.2159(13) 0.0775(6) -0.0110(6) 0.144(5) Uani 0.463(7) 1 d D U P C 2
Cl34 Cl 0.1259(17) -0.0317(8) 0.0190(7) 0.209(7) Uani 0.463(7) 1 d D U P C 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 Te1 3.1729(6) . ?
U1 O1 2.170(5) . ?
U1 O2 2.165(6) . ?
U1 O3 2.161(5) . ?
U1 N1 2.632(6) . ?
U1 N2 2.615(7) . ?
U1 N3 2.685(6) . ?
Te1 H1 0.8400 . ?
O1 C9 1.353(8) . ?
O2 C27 1.360(10) . ?
O3 C45 1.345(9) . ?
N1 C1 1.500(11) . ?
N1 C6 1.489(10) . ?
N1 C7 1.499(11) . ?
N2 C2 1.488(10) . ?
N2 C3 1.495(10) . ?
N2 C25 1.519(11) . ?
N3 C4 1.474(11) . ?
N3 C5 1.517(10) . ?
N3 C43 1.501(10) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.521(12) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C4 1.527(11) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C5 C6 1.508(12) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C7 C8 1.505(10) . ?
C8 C9 1.397(10) . ?
C8 C13 1.388(10) . ?
C9 C10 1.422(10) . ?
C10 C11 1.405(10) . ?
C10 C14 1.531(10) . ?
C11 H11 0.9500 . ?
C11 C12 1.386(10) . ?
C12 C13 1.393(10) . ?
C12 C24 1.500(10) . ?
C13 H13 0.9500 . ?
C14 C18 1.543(10) . ?
C14 C19 1.543(9) . ?
C14 C22 1.543(11) . ?
C15 H15 1.0000 . ?
C15 C18 1.544(10) . ?
C15 C20 1.533(13) . ?
C15 C23 1.526(11) . ?
C16 H16 1.0000 . ?
C16 C20 1.528(10) . ?
C16 C21 1.533(11) . ?
C16 C22 1.527(10) . ?
C17 H17 1.0000 . ?
C17 C19 1.531(10) . ?
C17 C21 1.524(12) . ?
C17 C23 1.539(11) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 C26 1.487(12) . ?
C26 C27 1.407(11) . ?
C26 C31 1.370(12) . ?
C27 C28 1.409(12) . ?
C28 C29 1.393(12) . ?
C28 C32 1.535(12) . ?
C29 H29 0.9500 . ?
C29 C30 1.396(13) . ?
C30 C31 1.396(13) . ?
C30 C42 1.511(13) . ?
C31 H31 0.9500 . ?
C32 C36 1.547(11) . ?
C32 C37 1.555(11) . ?
C32 C40 1.541(10) . ?
C33 H33 1.0000 . ?
C33 C36 1.523(11) . ?
C33 C38 1.532(12) . ?
C33 C41 1.526(13) . ?
C34 H34 1.0000 . ?
C34 C38 1.530(12) . ?
C34 C39 1.522(12) . ?
C34 C40 1.548(11) . ?
C35 H35 1.0000 . ?
C35 C37 1.527(13) . ?
C35 C39 1.527(12) . ?
C35 C41 1.544(13) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C43 C44 1.513(12) . ?
C44 C45 1.392(12) . ?
C44 C49 1.396(10) . ?
C45 C46 1.423(13) . ?
C46 C47 1.405(11) . ?
C46 C50 1.539(12) . ?
C47 H47 0.9500 . ?
C47 C48 1.382(13) . ?
C48 C49 1.376(13) . ?
C48 C60 1.516(11) . ?
C49 H49 0.9500 . ?
C50 C54 1.536(12) . ?
C50 C55 1.535(13) . ?
C50 C58 1.533(12) . ?
C51 H51 1.0000 . ?
C51 C54 1.550(13) . ?
C51 C56 1.520(14) . ?
C51 C59 1.504(16) . ?
C52 H52 1.0000 . ?
C52 C56 1.528(12) . ?
C52 C57 1.519(13) . ?
C52 C58 1.533(12) . ?
C53 H53 1.0000 . ?
C53 C55 1.543(14) . ?
C53 C57 1.523(14) . ?
C53 C59 1.517(16) . ?
C54 H54A 0.9900 . ?
C54 H54B 0.9900 . ?
C55 H55A 0.9900 . ?
C55 H55B 0.9900 . ?
C56 H56A 0.9900 . ?
C56 H56B 0.9900 . ?
C57 H57A 0.9900 . ?
C57 H57B 0.9900 . ?
C58 H58A 0.9900 . ?
C58 H58B 0.9900 . ?
C59 H59A 0.9900 . ?
C59 H59B 0.9900 . ?
C60 H60A 0.9800 . ?
C60 H60B 0.9800 . ?
C60 H60C 0.9800 . ?
C100 H10A 0.9900 . ?
C100 H10B 0.9900 . ?
C100 Cl11 1.626(17) . ?
C100 Cl12 1.711(18) . ?
C101 H10C 0.9900 . ?
C101 H10D 0.9900 . ?
C101 Cl13 1.62(2) . ?
C101 Cl14 1.67(2) . ?
Cl13 Cl33 2.39(2) 3 ?
C200 H20C 0.9900 . ?
C200 H20D 0.9900 . ?
C200 Cl21 1.661(15) . ?
C200 Cl22 1.707(15) . ?
C201 H20E 0.9900 . ?
C201 H20F 0.9900 . ?
C201 Cl23 1.629(19) . ?
C201 Cl24 1.70(2) . ?
C300 H30A 0.9900 . ?
C300 H30B 0.9900 . ?
C300 Cl31 1.576(19) . ?
C300 Cl32 1.632(18) . ?
C301 H30C 0.9900 . ?
C301 H30D 0.9900 . ?
C301 Cl33 1.591(19) . ?
C301 Cl34 1.616(19) . ?

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 Te1 84.29(13) . . ?
O1 U1 N1 71.09(19) . . ?
O1 U1 N2 86.4(2) . . ?
O1 U1 N3 135.14(19) . . ?
O2 U1 Te1 76.80(14) . . ?
O2 U1 O1 123.98(19) . . ?
O2 U1 N1 136.2(2) . . ?
O2 U1 N2 73.0(2) . . ?
O2 U1 N3 81.9(2) . . ?
O3 U1 Te1 87.05(14) . . ?
O3 U1 O1 118.2(2) . . ?
O3 U1 O2 112.9(2) . . ?
O3 U1 N1 84.8(2) . . ?
O3 U1 N2 134.6(2) . . ?
O3 U1 N3 70.9(2) . . ?
N1 U1 Te1 146.21(15) . . ?
N1 U1 N3 66.1(2) . . ?
N2 U1 Te1 135.66(15) . . ?
N2 U1 N1 67.0(2) . . ?
N2 U1 N3 65.4(2) . . ?
N3 U1 Te1 140.26(14) . . ?
U1 Te1 H1 109.5 . . ?
C9 O1 U1 149.9(4) . . ?
C27 O2 U1 147.9(5) . . ?
C45 O3 U1 150.8(6) . . ?
C1 N1 U1 114.3(5) . . ?
C6 N1 U1 107.1(4) . . ?
C6 N1 C1 111.1(6) . . ?
C6 N1 C7 106.3(6) . . ?
C7 N1 U1 107.9(4) . . ?
C7 N1 C1 109.8(6) . . ?
C2 N2 U1 104.8(5) . . ?
C2 N2 C3 110.6(6) . . ?
C2 N2 C25 109.7(6) . . ?
C3 N2 U1 117.5(5) . . ?
C3 N2 C25 110.4(7) . . ?
C25 N2 U1 103.5(4) . . ?
C4 N3 U1 107.3(4) . . ?
C4 N3 C5 110.9(7) . . ?
C4 N3 C43 106.7(6) . . ?
C5 N3 U1 114.3(5) . . ?
C43 N3 U1 107.0(4) . . ?
C43 N3 C5 110.3(6) . . ?
N1 C1 H1A 109.2 . . ?
N1 C1 H1B 109.2 . . ?
N1 C1 C2 112.1(6) . . ?
H1A C1 H1B 107.9 . . ?
C2 C1 H1A 109.2 . . ?
C2 C1 H1B 109.2 . . ?
N2 C2 C1 112.8(6) . . ?
N2 C2 H2A 109.0 . . ?
N2 C2 H2B 109.0 . . ?
C1 C2 H2A 109.0 . . ?
C1 C2 H2B 109.0 . . ?
H2A C2 H2B 107.8 . . ?
N2 C3 H3A 109.1 . . ?
N2 C3 H3B 109.1 . . ?
N2 C3 C4 112.4(6) . . ?
H3A C3 H3B 107.9 . . ?
C4 C3 H3A 109.1 . . ?
C4 C3 H3B 109.1 . . ?
N3 C4 C3 111.7(7) . . ?
N3 C4 H4A 109.3 . . ?
N3 C4 H4B 109.3 . . ?
C3 C4 H4A 109.3 . . ?
C3 C4 H4B 109.3 . . ?
H4A C4 H4B 108.0 . . ?
N3 C5 H5A 109.1 . . ?
N3 C5 H5B 109.1 . . ?
H5A C5 H5B 107.9 . . ?
C6 C5 N3 112.3(6) . . ?
C6 C5 H5A 109.1 . . ?
C6 C5 H5B 109.1 . . ?
N1 C6 C5 113.2(7) . . ?
N1 C6 H6A 108.9 . . ?
N1 C6 H6B 108.9 . . ?
C5 C6 H6A 108.9 . . ?
C5 C6 H6B 108.9 . . ?
H6A C6 H6B 107.7 . . ?
N1 C7 H7A 108.5 . . ?
N1 C7 H7B 108.5 . . ?
N1 C7 C8 115.1(7) . . ?
H7A C7 H7B 107.5 . . ?
C8 C7 H7A 108.5 . . ?
C8 C7 H7B 108.5 . . ?
C9 C8 C7 120.4(6) . . ?
C13 C8 C7 118.8(7) . . ?
C13 C8 C9 120.8(7) . . ?
O1 C9 C8 117.2(6) . . ?
O1 C9 C10 122.8(6) . . ?
C8 C9 C10 120.0(6) . . ?
C9 C10 C14 122.3(6) . . ?
C11 C10 C9 116.4(6) . . ?
C11 C10 C14 121.3(6) . . ?
C10 C11 H11 117.8 . . ?
C12 C11 C10 124.4(7) . . ?
C12 C11 H11 117.8 . . ?
C11 C12 C13 117.3(7) . . ?
C11 C12 C24 120.8(7) . . ?
C13 C12 C24 121.9(7) . . ?
C8 C13 C12 121.1(7) . . ?
C8 C13 H13 119.5 . . ?
C12 C13 H13 119.5 . . ?
C10 C14 C18 110.2(6) . . ?
C10 C14 C19 112.5(6) . . ?
C10 C14 C22 109.5(6) . . ?
C19 C14 C18 107.3(6) . . ?
C19 C14 C22 107.6(6) . . ?
C22 C14 C18 109.5(6) . . ?
C18 C15 H15 109.1 . . ?
C20 C15 H15 109.1 . . ?
C20 C15 C18 109.9(6) . . ?
C23 C15 H15 109.1 . . ?
C23 C15 C18 109.9(7) . . ?
C23 C15 C20 109.7(7) . . ?
C20 C16 H16 109.6 . . ?
C20 C16 C21 109.6(6) . . ?
C21 C16 H16 109.6 . . ?
C22 C16 H16 109.6 . . ?
C22 C16 C20 109.3(6) . . ?
C22 C16 C21 109.2(6) . . ?
C19 C17 H17 109.3 . . ?
C19 C17 C23 110.0(6) . . ?
C21 C17 H17 109.3 . . ?
C21 C17 C19 109.1(6) . . ?
C21 C17 C23 109.8(7) . . ?
C23 C17 H17 109.3 . . ?
C14 C18 C15 109.9(6) . . ?
C14 C18 H18A 109.7 . . ?
C14 C18 H18B 109.7 . . ?
C15 C18 H18A 109.7 . . ?
C15 C18 H18B 109.7 . . ?
H18A C18 H18B 108.2 . . ?
C14 C19 H19A 109.4 . . ?
C14 C19 H19B 109.4 . . ?
C17 C19 C14 111.1(6) . . ?
C17 C19 H19A 109.4 . . ?
C17 C19 H19B 109.4 . . ?
H19A C19 H19B 108.0 . . ?
C15 C20 H20A 109.8 . . ?
C15 C20 H20B 109.8 . . ?
C16 C20 C15 109.6(7) . . ?
C16 C20 H20A 109.8 . . ?
C16 C20 H20B 109.8 . . ?
H20A C20 H20B 108.2 . . ?
C16 C21 H21A 109.8 . . ?
C16 C21 H21B 109.8 . . ?
C17 C21 C16 109.5(6) . . ?
C17 C21 H21A 109.8 . . ?
C17 C21 H21B 109.8 . . ?
H21A C21 H21B 108.2 . . ?
C14 C22 H22A 109.4 . . ?
C14 C22 H22B 109.4 . . ?
C16 C22 C14 111.0(6) . . ?
C16 C22 H22A 109.4 . . ?
C16 C22 H22B 109.4 . . ?
H22A C22 H22B 108.0 . . ?
C15 C23 C17 108.4(6) . . ?
C15 C23 H23A 110.0 . . ?
C15 C23 H23B 110.0 . . ?
C17 C23 H23A 110.0 . . ?
C17 C23 H23B 110.0 . . ?
H23A C23 H23B 108.4 . . ?
C12 C24 H24A 109.5 . . ?
C12 C24 H24B 109.5 . . ?
C12 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
N2 C25 H25A 108.3 . . ?
N2 C25 H25B 108.3 . . ?
H25A C25 H25B 107.4 . . ?
C26 C25 N2 116.0(6) . . ?
C26 C25 H25A 108.3 . . ?
C26 C25 H25B 108.3 . . ?
C27 C26 C25 120.1(8) . . ?
C31 C26 C25 119.3(8) . . ?
C31 C26 C27 120.6(8) . . ?
O2 C27 C26 116.5(7) . . ?
O2 C27 C28 123.0(7) . . ?
C26 C27 C28 120.4(8) . . ?
C27 C28 C32 122.2(7) . . ?
C29 C28 C27 116.7(8) . . ?
C29 C28 C32 121.1(8) . . ?
C28 C29 H29 118.1 . . ?
C28 C29 C30 123.8(9) . . ?
C30 C29 H29 118.1 . . ?
C29 C30 C31 117.6(8) . . ?
C29 C30 C42 120.7(9) . . ?
C31 C30 C42 121.7(9) . . ?
C26 C31 C30 120.9(8) . . ?
C26 C31 H31 119.6 . . ?
C30 C31 H31 119.6 . . ?
C28 C32 C36 109.8(6) . . ?
C28 C32 C37 112.0(7) . . ?
C28 C32 C40 111.8(6) . . ?
C36 C32 C37 107.2(7) . . ?
C40 C32 C36 108.8(7) . . ?
C40 C32 C37 107.1(6) . . ?
C36 C33 H33 108.9 . . ?
C36 C33 C38 109.8(7) . . ?
C36 C33 C41 110.0(8) . . ?
C38 C33 H33 108.9 . . ?
C41 C33 H33 108.9 . . ?
C41 C33 C38 110.2(7) . . ?
C38 C34 H34 109.6 . . ?
C38 C34 C40 108.7(6) . . ?
C39 C34 H34 109.6 . . ?
C39 C34 C38 109.3(7) . . ?
C39 C34 C40 110.0(7) . . ?
C40 C34 H34 109.6 . . ?
C37 C35 H35 109.1 . . ?
C37 C35 C39 110.2(7) . . ?
C37 C35 C41 109.8(7) . . ?
C39 C35 H35 109.1 . . ?
C39 C35 C41 109.5(8) . . ?
C41 C35 H35 109.1 . . ?
C32 C36 H36A 109.5 . . ?
C32 C36 H36B 109.5 . . ?
C33 C36 C32 110.8(6) . . ?
C33 C36 H36A 109.5 . . ?
C33 C36 H36B 109.5 . . ?
H36A C36 H36B 108.1 . . ?
C32 C37 H37A 109.4 . . ?
C32 C37 H37B 109.4 . . ?
C35 C37 C32 111.1(7) . . ?
C35 C37 H37A 109.4 . . ?
C35 C37 H37B 109.4 . . ?
H37A C37 H37B 108.0 . . ?
C33 C38 H38A 109.8 . . ?
C33 C38 H38B 109.8 . . ?
C34 C38 C33 109.4(7) . . ?
C34 C38 H38A 109.8 . . ?
C34 C38 H38B 109.8 . . ?
H38A C38 H38B 108.2 . . ?
C34 C39 C35 109.3(7) . . ?
C34 C39 H39A 109.8 . . ?
C34 C39 H39B 109.8 . . ?
C35 C39 H39A 109.8 . . ?
C35 C39 H39B 109.8 . . ?
H39A C39 H39B 108.3 . . ?
C32 C40 C34 111.0(6) . . ?
C32 C40 H40A 109.4 . . ?
C32 C40 H40B 109.4 . . ?
C34 C40 H40A 109.4 . . ?
C34 C40 H40B 109.4 . . ?
H40A C40 H40B 108.0 . . ?
C33 C41 C35 108.0(7) . . ?
C33 C41 H41A 110.1 . . ?
C33 C41 H41B 110.1 . . ?
C35 C41 H41A 110.1 . . ?
C35 C41 H41B 110.1 . . ?
H41A C41 H41B 108.4 . . ?
C30 C42 H42A 109.5 . . ?
C30 C42 H42B 109.5 . . ?
C30 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
N3 C43 H43A 108.3 . . ?
N3 C43 H43B 108.3 . . ?
N3 C43 C44 116.1(7) . . ?
H43A C43 H43B 107.4 . . ?
C44 C43 H43A 108.3 . . ?
C44 C43 H43B 108.3 . . ?
C45 C44 C43 120.6(7) . . ?
C45 C44 C49 120.4(9) . . ?
C49 C44 C43 118.8(8) . . ?
O3 C45 C44 117.8(8) . . ?
O3 C45 C46 122.5(8) . . ?
C44 C45 C46 119.8(7) . . ?
C45 C46 C50 122.1(7) . . ?
C47 C46 C45 117.0(8) . . ?
C47 C46 C50 120.8(8) . . ?
C46 C47 H47 118.4 . . ?
C48 C47 C46 123.3(9) . . ?
C48 C47 H47 118.4 . . ?
C47 C48 C60 120.3(9) . . ?
C49 C48 C47 118.3(7) . . ?
C49 C48 C60 121.4(8) . . ?
C44 C49 H49 119.4 . . ?
C48 C49 C44 121.1(8) . . ?
C48 C49 H49 119.4 . . ?
C54 C50 C46 111.2(7) . . ?
C55 C50 C46 112.6(7) . . ?
C55 C50 C54 107.8(8) . . ?
C58 C50 C46 109.9(7) . . ?
C58 C50 C54 108.1(7) . . ?
C58 C50 C55 107.1(7) . . ?
C54 C51 H51 109.4 . . ?
C56 C51 H51 109.4 . . ?
C56 C51 C54 109.2(8) . . ?
C59 C51 H51 109.4 . . ?
C59 C51 C54 109.5(8) . . ?
C59 C51 C56 110.1(9) . . ?
C56 C52 H52 109.5 . . ?
C56 C52 C58 109.0(7) . . ?
C57 C52 H52 109.5 . . ?
C57 C52 C56 109.5(9) . . ?
C57 C52 C58 109.8(7) . . ?
C58 C52 H52 109.5 . . ?
C55 C53 H53 109.7 . . ?
C57 C53 H53 109.7 . . ?
C57 C53 C55 109.6(9) . . ?
C59 C53 H53 109.7 . . ?
C59 C53 C55 109.0(9) . . ?
C59 C53 C57 109.1(8) . . ?
C50 C54 C51 110.6(7) . . ?
C50 C54 H54A 109.5 . . ?
C50 C54 H54B 109.5 . . ?
C51 C54 H54A 109.5 . . ?
C51 C54 H54B 109.5 . . ?
H54A C54 H54B 108.1 . . ?
C50 C55 C53 111.5(7) . . ?
C50 C55 H55A 109.3 . . ?
C50 C55 H55B 109.3 . . ?
C53 C55 H55A 109.3 . . ?
C53 C55 H55B 109.3 . . ?
H55A C55 H55B 108.0 . . ?
C51 C56 C52 109.2(7) . . ?
C51 C56 H56A 109.8 . . ?
C51 C56 H56B 109.8 . . ?
C52 C56 H56A 109.8 . . ?
C52 C56 H56B 109.8 . . ?
H56A C56 H56B 108.3 . . ?
C52 C57 C53 109.3(8) . . ?
C52 C57 H57A 109.8 . . ?
C52 C57 H57B 109.8 . . ?
C53 C57 H57A 109.8 . . ?
C53 C57 H57B 109.8 . . ?
H57A C57 H57B 108.3 . . ?
C50 C58 C52 111.8(8) . . ?
C50 C58 H58A 109.3 . . ?
C50 C58 H58B 109.3 . . ?
C52 C58 H58A 109.3 . . ?
C52 C58 H58B 109.3 . . ?
H58A C58 H58B 107.9 . . ?
C51 C59 C53 110.2(9) . . ?
C51 C59 H59A 109.6 . . ?
C51 C59 H59B 109.6 . . ?
C53 C59 H59A 109.6 . . ?
C53 C59 H59B 109.6 . . ?
H59A C59 H59B 108.1 . . ?
C48 C60 H60A 109.5 . . ?
C48 C60 H60B 109.5 . . ?
C48 C60 H60C 109.5 . . ?
H60A C60 H60B 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
H10A C100 H10B 107.2 . . ?
Cl11 C100 H10A 107.8 . . ?
Cl11 C100 H10B 107.8 . . ?
Cl11 C100 Cl12 117.9(12) . . ?
Cl12 C100 H10A 107.8 . . ?
Cl12 C100 H10B 107.8 . . ?
H10C C101 H10D 107.3 . . ?
Cl13 C101 H10C 108.1 . . ?
Cl13 C101 H10D 108.1 . . ?
Cl13 C101 Cl14 117(2) . . ?
Cl14 C101 H10C 108.1 . . ?
Cl14 C101 H10D 108.1 . . ?
C101 Cl13 Cl33 103(3) . 3 ?
H20C C200 H20D 106.8 . . ?
Cl21 C200 H20C 107.1 . . ?
Cl21 C200 H20D 107.1 . . ?
Cl21 C200 Cl22 120.7(11) . . ?
Cl22 C200 H20C 107.1 . . ?
Cl22 C200 H20D 107.1 . . ?
H20E C201 H20F 107.6 . . ?
Cl23 C201 H20E 108.7 . . ?
Cl23 C201 H20F 108.7 . . ?
Cl23 C201 Cl24 114.2(17) . . ?
Cl24 C201 H20E 108.7 . . ?
Cl24 C201 H20F 108.7 . . ?
H30A C300 H30B 109.1 . . ?
Cl31 C300 H30A 111.1 . . ?
Cl31 C300 H30B 111.1 . . ?
Cl31 C300 Cl32 103.2(12) . . ?
Cl32 C300 H30A 111.1 . . ?
Cl32 C300 H30B 111.1 . . ?
H30C C301 H30D 105.0 . . ?
Cl33 C301 H30C 102.7 . . ?
Cl33 C301 H30D 102.7 . . ?
Cl33 C301 Cl34 138(3) . . ?
Cl34 C301 H30C 102.7 . . ?
Cl34 C301 H30D 102.7 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
U1 O1 C9 C8 -11.5(14) . . . . ?
U1 O1 C9 C10 168.6(6) . . . . ?
U1 O2 C27 C26 -7.5(12) . . . . ?
U1 O2 C27 C28 172.2(6) . . . . ?
U1 O3 C45 C44 -10.1(14) . . . . ?
U1 O3 C45 C46 169.0(7) . . . . ?
U1 N1 C1 C2 9.5(8) . . . . ?
U1 N1 C6 C5 59.4(8) . . . . ?
U1 N1 C7 C8 -75.0(7) . . . . ?
U1 N2 C2 C1 60.8(7) . . . . ?
U1 N2 C3 C4 11.8(9) . . . . ?
U1 N2 C25 C26 -78.8(7) . . . . ?
U1 N3 C4 C3 57.1(7) . . . . ?
U1 N3 C5 C6 10.9(9) . . . . ?
U1 N3 C43 C44 -73.2(7) . . . . ?
O1 C9 C10 C11 -179.3(7) . . . . ?
O1 C9 C10 C14 -0.6(11) . . . . ?
O2 C27 C28 C29 -177.9(7) . . . . ?
O2 C27 C28 C32 5.2(11) . . . . ?
O3 C45 C46 C47 177.8(7) . . . . ?
O3 C45 C46 C50 -1.4(12) . . . . ?
N1 C1 C2 N2 -48.7(9) . . . . ?
N1 C7 C8 C9 54.8(10) . . . . ?
N1 C7 C8 C13 -128.4(8) . . . . ?
N2 C3 C4 N3 -47.3(9) . . . . ?
N2 C25 C26 C27 58.4(10) . . . . ?
N2 C25 C26 C31 -124.6(8) . . . . ?
N3 C5 C6 N1 -47.9(10) . . . . ?
N3 C43 C44 C45 53.2(10) . . . . ?
N3 C43 C44 C49 -131.2(7) . . . . ?
C1 N1 C6 C5 -66.0(9) . . . . ?
C1 N1 C7 C8 50.1(8) . . . . ?
C2 N2 C3 C4 131.9(8) . . . . ?
C2 N2 C25 C26 169.9(7) . . . . ?
C3 N2 C2 C1 -66.7(9) . . . . ?
C3 N2 C25 C26 47.7(9) . . . . ?
C4 N3 C5 C6 132.3(8) . . . . ?
C4 N3 C43 C44 172.2(6) . . . . ?
C5 N3 C4 C3 -68.4(8) . . . . ?
C5 N3 C43 C44 51.8(9) . . . . ?
C6 N1 C1 C2 130.8(7) . . . . ?
C6 N1 C7 C8 170.4(6) . . . . ?
C7 N1 C1 C2 -111.9(7) . . . . ?
C7 N1 C6 C5 174.6(7) . . . . ?
C7 C8 C9 O1 -5.5(11) . . . . ?
C7 C8 C9 C10 174.4(7) . . . . ?
C7 C8 C13 C12 -174.4(7) . . . . ?
C8 C9 C10 C11 0.8(11) . . . . ?
C8 C9 C10 C14 179.5(7) . . . . ?
C9 C8 C13 C12 2.4(12) . . . . ?
C9 C10 C11 C12 0.8(11) . . . . ?
C9 C10 C14 C18 58.4(9) . . . . ?
C9 C10 C14 C19 178.2(7) . . . . ?
C9 C10 C14 C22 -62.1(9) . . . . ?
C10 C11 C12 C13 -0.8(11) . . . . ?
C10 C11 C12 C24 177.6(7) . . . . ?
C10 C14 C18 C15 -177.5(6) . . . . ?
C10 C14 C19 C17 179.3(6) . . . . ?
C10 C14 C22 C16 178.8(6) . . . . ?
C11 C10 C14 C18 -122.9(7) . . . . ?
C11 C10 C14 C19 -3.1(10) . . . . ?
C11 C10 C14 C22 116.6(7) . . . . ?
C11 C12 C13 C8 -0.8(11) . . . . ?
C13 C8 C9 O1 177.7(7) . . . . ?
C13 C8 C9 C10 -2.4(12) . . . . ?
C14 C10 C11 C12 -177.9(7) . . . . ?
C18 C14 C19 C17 -59.3(8) . . . . ?
C18 C14 C22 C16 57.9(7) . . . . ?
C18 C15 C20 C16 -60.5(8) . . . . ?
C18 C15 C23 C17 60.3(9) . . . . ?
C19 C14 C18 C15 59.6(8) . . . . ?
C19 C14 C22 C16 -58.5(8) . . . . ?
C19 C17 C21 C16 60.3(8) . . . . ?
C19 C17 C23 C15 -59.3(9) . . . . ?
C20 C15 C18 C14 58.9(8) . . . . ?
C20 C15 C23 C17 -60.6(8) . . . . ?
C20 C16 C21 C17 59.2(8) . . . . ?
C20 C16 C22 C14 -59.5(8) . . . . ?
C21 C16 C20 C15 -59.2(8) . . . . ?
C21 C16 C22 C14 60.3(8) . . . . ?
C21 C17 C19 C14 -60.4(8) . . . . ?
C21 C17 C23 C15 60.8(8) . . . . ?
C22 C14 C18 C15 -56.9(8) . . . . ?
C22 C14 C19 C17 58.5(8) . . . . ?
C22 C16 C20 C15 60.4(8) . . . . ?
C22 C16 C21 C17 -60.4(8) . . . . ?
C23 C15 C18 C14 -62.0(9) . . . . ?
C23 C15 C20 C16 60.5(8) . . . . ?
C23 C17 C19 C14 60.1(9) . . . . ?
C23 C17 C21 C16 -60.3(8) . . . . ?
C24 C12 C13 C8 -179.2(7) . . . . ?
C25 N2 C2 C1 171.3(7) . . . . ?
C25 N2 C3 C4 -106.4(8) . . . . ?
C25 C26 C27 O2 -6.1(10) . . . . ?
C25 C26 C27 C28 174.2(7) . . . . ?
C25 C26 C31 C30 -174.2(7) . . . . ?
C26 C27 C28 C29 1.7(11) . . . . ?
C26 C27 C28 C32 -175.2(7) . . . . ?
C27 C26 C31 C30 2.7(12) . . . . ?
C27 C28 C29 C30 -0.9(12) . . . . ?
C27 C28 C32 C36 61.8(9) . . . . ?
C27 C28 C32 C37 -179.3(7) . . . . ?
C27 C28 C32 C40 -59.1(10) . . . . ?
C28 C29 C30 C31 0.9(13) . . . . ?
C28 C29 C30 C42 -177.3(8) . . . . ?
C28 C32 C36 C33 -179.7(7) . . . . ?
C28 C32 C37 C35 -178.4(6) . . . . ?
C28 C32 C40 C34 178.7(7) . . . . ?
C29 C28 C32 C36 -115.0(8) . . . . ?
C29 C28 C32 C37 4.0(10) . . . . ?
C29 C28 C32 C40 124.2(8) . . . . ?
C29 C30 C31 C26 -1.8(12) . . . . ?
C31 C26 C27 O2 177.0(7) . . . . ?
C31 C26 C27 C28 -2.7(11) . . . . ?
C32 C28 C29 C30 176.1(8) . . . . ?
C36 C32 C37 C35 -57.9(8) . . . . ?
C36 C32 C40 C34 57.3(8) . . . . ?
C36 C33 C38 C34 -61.2(9) . . . . ?
C36 C33 C41 C35 61.0(9) . . . . ?
C37 C32 C36 C33 58.4(9) . . . . ?
C37 C32 C40 C34 -58.2(9) . . . . ?
C37 C35 C39 C34 59.4(10) . . . . ?
C37 C35 C41 C33 -60.3(9) . . . . ?
C38 C33 C36 C32 59.5(9) . . . . ?
C38 C33 C41 C35 -60.2(10) . . . . ?
C38 C34 C39 C35 60.5(9) . . . . ?
C38 C34 C40 C32 -59.7(9) . . . . ?
C39 C34 C38 C33 -59.6(9) . . . . ?
C39 C34 C40 C32 60.0(8) . . . . ?
C39 C35 C37 C32 -60.4(9) . . . . ?
C39 C35 C41 C33 60.8(9) . . . . ?
C40 C32 C36 C33 -57.1(9) . . . . ?
C40 C32 C37 C35 58.7(8) . . . . ?
C40 C34 C38 C33 60.6(8) . . . . ?
C40 C34 C39 C35 -58.9(9) . . . . ?
C41 C33 C36 C32 -61.9(9) . . . . ?
C41 C33 C38 C34 60.2(9) . . . . ?
C41 C35 C37 C32 60.3(9) . . . . ?
C41 C35 C39 C34 -61.5(9) . . . . ?
C42 C30 C31 C26 176.4(8) . . . . ?
C43 N3 C4 C3 171.5(6) . . . . ?
C43 N3 C5 C6 -109.7(8) . . . . ?
C43 C44 C45 O3 -4.3(11) . . . . ?
C43 C44 C45 C46 176.7(7) . . . . ?
C43 C44 C49 C48 -174.2(7) . . . . ?
C44 C45 C46 C47 -3.1(11) . . . . ?
C44 C45 C46 C50 177.7(7) . . . . ?
C45 C44 C49 C48 1.5(12) . . . . ?
C45 C46 C47 C48 2.9(12) . . . . ?
C45 C46 C50 C54 63.9(10) . . . . ?
C45 C46 C50 C55 -175.1(8) . . . . ?
C45 C46 C50 C58 -55.7(10) . . . . ?
C46 C47 C48 C49 -0.4(13) . . . . ?
C46 C47 C48 C60 179.6(8) . . . . ?
C46 C50 C54 C51 -178.2(8) . . . . ?
C46 C50 C55 C53 178.9(8) . . . . ?
C46 C50 C58 C52 179.3(7) . . . . ?
C47 C46 C50 C54 -115.3(9) . . . . ?
C47 C46 C50 C55 5.8(11) . . . . ?
C47 C46 C50 C58 125.1(8) . . . . ?
C47 C48 C49 C44 -1.9(13) . . . . ?
C49 C44 C45 O3 -179.8(7) . . . . ?
C49 C44 C45 C46 1.1(12) . . . . ?
C50 C46 C47 C48 -177.9(8) . . . . ?
C54 C50 C55 C53 -58.1(10) . . . . ?
C54 C50 C58 C52 57.8(10) . . . . ?
C54 C51 C56 C52 -61.2(11) . . . . ?
C54 C51 C59 C53 60.4(11) . . . . ?
C55 C50 C54 C51 57.9(10) . . . . ?
C55 C50 C58 C52 -58.1(9) . . . . ?
C55 C53 C57 C52 59.1(10) . . . . ?
C55 C53 C59 C51 -59.8(11) . . . . ?
C56 C51 C54 C50 60.5(10) . . . . ?
C56 C51 C59 C53 -59.6(11) . . . . ?
C56 C52 C57 C53 60.4(10) . . . . ?
C56 C52 C58 C50 -59.9(10) . . . . ?
C57 C52 C56 C51 -59.5(10) . . . . ?
C57 C52 C58 C50 60.1(10) . . . . ?
C57 C53 C55 C50 -60.0(11) . . . . ?
C57 C53 C59 C51 59.8(11) . . . . ?
C58 C50 C54 C51 -57.5(10) . . . . ?
C58 C50 C55 C53 58.0(11) . . . . ?
C58 C52 C56 C51 60.6(11) . . . . ?
C58 C52 C57 C53 -59.2(10) . . . . ?
C59 C51 C54 C50 -60.1(10) . . . . ?
C59 C51 C56 C52 59.0(11) . . . . ?
C59 C53 C55 C50 59.3(11) . . . . ?
C59 C53 C57 C52 -60.2(11) . . . . ?
C60 C48 C49 C44 178.2(8) . . . . ?
Cl14 C101 Cl13 Cl33 79(5) . . . 3 ?
Cl34 C301 Cl33 Cl13 -111(4) . . . 3 ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.9966(4)
2 0.0034(4)

# start Validation Reply Form
_vrf_PLAT232_mr1528              
;
PROBLEM: Hirshfeld Test Diff (M-X)  U1       --Te1      .       32.8 s.u.  
RESPONSE: The terminal TeH ligand seems to be affected by a higher thermal 
motion. Attempts to refine split positions here remained unsuccessful as the 
tentative alternative positions were too close together.
;
_vrf_PLAT260_mr1528              
;
PROBLEM: Large Average Ueq of Residue Including      Cl33      0.164 Check 
RESPONSE: This residue is formed by one fraction of a disordered 
dichloromethane molecule. Similarity and pseudo-isotropic restraints were
applied to the anisotropic displacement parameters of the corresponding atoms.
;
####################################################################### 
# 
# 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_mr1521sq
_database_code_depnum_ccdc_archive 'CCDC 1893559'
loop_
_audit_author_name
_audit_author_address
'Frank W. Heinemann'
;Friedrich-Alexander-Universit?t Erlangen-N?rnberg
Germany
;
_audit_update_record             
;
2019-01-25 deposited with the CCDC.	2019-03-25 downloaded from the CCDC.
;
_audit_creation_date             2015-10-30
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_shelxl_version_number           2014/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C60 H79 N3 O3 Se1 U1, 3.25(C4 H8 O)'
_chemical_formula_sum            'C73 H105 N3 O6.25 Se U'
_chemical_formula_weight         1441.58
_chemical_absolute_configuration ad
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      hexagonal
_space_group_IT_number           173
_space_group_name_H-M_alt        'P 63'
_space_group_name_Hall           'P 6c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'

_cell_length_a                   20.3282(6)
_cell_length_b                   20.3282(6)
_cell_length_c                   18.6007(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     6656.7(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9550
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.06
_cell_measurement_theta_min      2.28
_shelx_estimated_absorpt_T_max   0.676
_shelx_estimated_absorpt_T_min   0.453
_exptl_absorpt_coefficient_mu    3.039
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.6370
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0789 before and 0.0674 after correction.
The Ratio of minimum to maximum transmission is 0.8540.
The λ/2 correction factor is 0.0015.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.438
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             2960
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0436
_diffrn_reflns_av_unetI/netI     0.0365
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            134384
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.617
_diffrn_reflns_theta_min         1.157
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_monochromator  'Triumph curved graphite'
_diffrn_measurement_device_type  'Bruker Smart APEX II CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 83.33
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.937
_reflns_Friedel_fraction_full    0.993
_reflns_Friedel_fraction_max     0.990
_reflns_number_gt                10689
_reflns_number_total             12439
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELX XT 2014/5 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2015)'
_computing_molecular_graphics    'SHELXTL 6.12 (Bruker AXS, 2002)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_refine_diff_density_max         2.120
_refine_diff_density_min         -1.043
_refine_diff_density_rms         0.134
_refine_ls_abs_structure_details 
;
 Flack x determined using 4851 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.019(2)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     499
_refine_ls_number_reflns         12439
_refine_ls_number_restraints     167
_refine_ls_R_factor_all          0.0461
_refine_ls_R_factor_gt           0.0330
_refine_ls_restrained_S_all      1.077
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0525P)²+5.9766P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0840
_refine_ls_wR_factor_ref         0.0898
_refine_special_details          
;
 As some of the solvent molecules could not be modelled, the SQUEEZE
 routine of the programm PLATON was employed. Two voids were identified
 which were be big enough in size to accommodate two thf molecules.
 The electron count in each void in the unit cell was calculated to
 be approximately 70 e. One thf molecule has 40 e, so it has been
 assumed that two thf molecules were in each void. This approximation has
 been used in the subsequent calculation of the empirical formula,
 formula weight, density, linear absorption coefficient, and F(000).

 One of the two identified thf solvent molecule sites was occupied by
 approximately 50 % only and therefore, the site occupancy factor of this
 molecule (O200 - C205) was fixed at 0.5. DFIX, SIMU, and ISOR restraints
 were applied in the refinement of the thf molecules. DELU and ISOR
 restraints were applied in the refinement of the Se atoms.
;

_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All Se(H) groups
2. Restrained distances
 C101-C102 = C102-C103 = C103-C104
 1.54 with sigma of 0.02
 C201-C202 = C202-C203 = C203-C204
 1.54 with sigma of 0.02
3. Rigid bond restraints
 U1, Se1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 U2, Se2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
O100 \\sim C101 \\sim C102 \\sim C103 \\sim C104: within 2A with sigma of 0.005
and sigma for terminal atoms of 0.01
O200 \\sim C201 \\sim C202 \\sim C203 \\sim C204: within 2A with sigma of 0.005
and sigma for terminal atoms of 0.01
Uanis(O100) \\sim Ueq, Uanis(C101) \\sim Ueq, Uanis(C102) \\sim Ueq,
Uanis(C103) \\sim Ueq, Uanis(C104) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(O200) \\sim Ueq, Uanis(C201) \\sim Ueq, Uanis(C202) \\sim Ueq,
Uanis(C203) \\sim Ueq, Uanis(C204) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(Se1) \\sim Ueq, Uanis(Se2) \\sim Ueq: with sigma of 0.003 and sigma for
terminal atoms of 0.006
5. Same fragment restrains
{O200, C201, C202, C203, C204} sigma for 1-2: 0.02, 1-3: 0.04
as
{O100, C101, C102, C103, C104}
{O200, C204, C203, C202, C201} sigma for 1-2: 0.02, 1-3: 0.04
as
{O200, C201, C202, C203, C204}
6. Others
 Fixed Sof: H1(0.33333) H2(0.33333) O200(0.5) C201(0.5) H20D(0.5) H20E(0.5)
 C202(0.5) H20F(0.5) H20G(0.5) C203(0.5) H20H(0.5) H20I(0.5) C204(0.5)
 H20J(0.5) H20K(0.5)
7.a Ternary CH refined with riding coordinates:
 C11(H11), C12(H12), C13(H13), C31(H31), C32(H32), C33(H33)
7.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C14(H14A,H14B), C15(H15A,H15B),
 C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B), C21(H21A,H21B),
  C22(H22A,H22B), C23(H23A,H23B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,
 H36B), C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B), C101(H10A,H10B),
 C102(H10C,H10D), C103(H10E,H10F), C104(H10G,H10H), C201(H20D,H20E), C202(H20F,
 H20G), C203(H20H,H20I), C204(H20J,H20K)
7.c Me refined with riding coordinates:
 C20(H20A,H20B,H20C), C40(H40A,H40B,H40C)
7.d Aromatic/amide H refined with riding coordinates:
 C7(H7), C9(H9), C27(H27), C29(H29)
7.e Tetrahedral OH refined with riding coordinates:
 Se1(H1), Se2(H2)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.6667 0.3333 0.92315(2) 0.01722(8) Uani 1 3 d S TU P . .
Se1 Se 0.6667 0.3333 0.76640(7) 0.0474(3) Uani 1 3 d S TU P . .
H1 H 0.6222 0.3051 0.7513 0.071 Uiso 0.3333 1 calc R . . . .
O1 O 0.6906(2) 0.2417(2) 0.9085(2) 0.0234(9) Uani 1 1 d . . . . .
N1 N 0.6108(3) 0.2391(3) 1.0347(2) 0.0205(10) Uani 1 1 d . . . . .
C1 C 0.5504(3) 0.2502(3) 1.0663(3) 0.0222(11) Uani 1 1 d . . . . .
H1A H 0.5278 0.2157 1.1080 0.027 Uiso 1 1 calc R . . . .
H1B H 0.5098 0.2368 1.0303 0.027 Uiso 1 1 calc R . . . .
C2 C 0.6679(3) 0.2486(3) 1.0909(3) 0.0236(12) Uani 1 1 d . . . . .
H2A H 0.6608 0.1981 1.1033 0.028 Uiso 1 1 calc R . . . .
H2B H 0.6587 0.2702 1.1348 0.028 Uiso 1 1 calc R . . . .
C3 C 0.5731(3) 0.1598(3) 1.0051(4) 0.0241(12) Uani 1 1 d . . . . .
H3A H 0.5406 0.1567 0.9641 0.029 Uiso 1 1 calc R . . . .
H3B H 0.5393 0.1246 1.0427 0.029 Uiso 1 1 calc R . . . .
C4 C 0.6256(3) 0.1326(3) 0.9802(3) 0.0217(11) Uani 1 1 d . . . . .
C5 C 0.6815(3) 0.1739(3) 0.9285(3) 0.0206(10) Uani 1 1 d . . . . .
C6 C 0.7274(3) 0.1457(3) 0.9005(3) 0.0233(12) Uani 1 1 d . . . . .
C7 C 0.7136(3) 0.0757(3) 0.9273(4) 0.0257(11) Uani 1 1 d . . . . .
H7 H 0.7426 0.0549 0.9082 0.031 Uiso 1 1 calc R . . . .
C8 C 0.6603(4) 0.0345(4) 0.9802(4) 0.0289(13) Uani 1 1 d . . . . .
C9 C 0.6158(4) 0.0637(3) 1.0058(4) 0.0269(12) Uani 1 1 d . . . . .
H9 H 0.5781 0.0363 1.0411 0.032 Uiso 1 1 calc R . . . .
C10 C 0.7866(3) 0.1884(3) 0.8424(3) 0.0227(11) Uani 1 1 d . . . . .
C11 C 0.9075(4) 0.3113(4) 0.8131(4) 0.0368(15) Uani 1 1 d . . . . .
H11 H 0.9463 0.3618 0.8329 0.044 Uiso 1 1 calc R . . . .
C12 C 0.8099(4) 0.2467(4) 0.7194(4) 0.0335(15) Uani 1 1 d . . . . .
H12 H 0.7852 0.2557 0.6769 0.040 Uiso 1 1 calc R . . . .
C13 C 0.8864(4) 0.1896(4) 0.7598(4) 0.0355(14) Uani 1 1 d . . . . .
H13 H 0.9116 0.1603 0.7446 0.043 Uiso 1 1 calc R . . . .
C14 C 0.8492(4) 0.2661(4) 0.8716(4) 0.0307(14) Uani 1 1 d . . . . .
H14A H 0.8256 0.2956 0.8890 0.037 Uiso 1 1 calc R . . . .
H14B H 0.8750 0.2578 0.9127 0.037 Uiso 1 1 calc R . . . .
C15 C 0.8273(4) 0.1450(4) 0.8178(4) 0.0289(13) Uani 1 1 d . . . . .
H15A H 0.8526 0.1369 0.8596 0.035 Uiso 1 1 calc R . . . .
H15B H 0.7894 0.0946 0.7987 0.035 Uiso 1 1 calc R . . . .
C16 C 0.8686(4) 0.3231(4) 0.7501(5) 0.0408(17) Uani 1 1 d . . . . .
H16A H 0.9065 0.3532 0.7127 0.049 Uiso 1 1 calc R . . . .
H16B H 0.8434 0.3517 0.7655 0.049 Uiso 1 1 calc R . . . .
C17 C 0.8480(5) 0.2020(4) 0.6946(4) 0.0380(16) Uani 1 1 d . . . . .
H17A H 0.8862 0.2308 0.6569 0.046 Uiso 1 1 calc R . . . .
H17B H 0.8096 0.1525 0.6742 0.046 Uiso 1 1 calc R . . . .
C18 C 0.7492(4) 0.2001(4) 0.7744(3) 0.0277(13) Uani 1 1 d . . . . .
H18A H 0.7124 0.1501 0.7536 0.033 Uiso 1 1 calc R . . . .
H18B H 0.7213 0.2266 0.7877 0.033 Uiso 1 1 calc R . . . .
C19 C 0.9468(4) 0.2673(5) 0.7892(5) 0.0433(18) Uani 1 1 d . . . . .
H19A H 0.9734 0.2603 0.8305 0.052 Uiso 1 1 calc R . . . .
H19B H 0.9847 0.2961 0.7514 0.052 Uiso 1 1 calc R . . . .
C20 C 0.6497(5) -0.0401(4) 1.0063(4) 0.0389(16) Uani 1 1 d . . . . .
H20A H 0.6862 -0.0508 0.9821 0.058 Uiso 1 1 calc R . . . .
H20B H 0.6582 -0.0376 1.0584 0.058 Uiso 1 1 calc R . . . .
H20C H 0.5980 -0.0807 0.9955 0.058 Uiso 1 1 calc R . . . .
U2 U 1.0000 1.0000 0.01281(2) 0.01314(7) Uani 1 3 d S TU P . .
Se2 Se 1.0000 1.0000 0.16875(6) 0.0342(3) Uani 1 3 d S TU P . .
H2 H 1.0187 0.9739 0.1838 0.051 Uiso 0.3333 1 calc R . . . .
O2 O 0.8905(2) 0.8983(2) 0.02926(19) 0.0192(8) Uani 1 1 d . . . . .
N2 N 0.9123(2) 0.9866(3) -0.0967(2) 0.0155(9) Uani 1 1 d . . . . .
C21 C 0.9438(3) 1.0627(3) -0.1288(3) 0.0176(10) Uani 1 1 d . . . . .
H21A H 0.9406 1.0974 -0.0934 0.021 Uiso 1 1 calc R . . . .
H21B H 0.9127 1.0596 -0.1711 0.021 Uiso 1 1 calc R . . . .
C22 C 0.9046(3) 0.9304(3) -0.1522(3) 0.0181(10) Uani 1 1 d . . . . .
H22A H 0.9306 0.9579 -0.1966 0.022 Uiso 1 1 calc R . . . .
H22B H 0.8501 0.8973 -0.1637 0.022 Uiso 1 1 calc R . . . .
C23 C 0.8366(3) 0.9654(3) -0.0654(3) 0.0200(11) Uani 1 1 d . . . . .
H23A H 0.8078 0.9772 -0.1009 0.024 Uiso 1 1 calc R . . . .
H23B H 0.8444 0.9971 -0.0223 0.024 Uiso 1 1 calc R . . . .
C24 C 0.7899(3) 0.8835(3) -0.0446(3) 0.0194(10) Uani 1 1 d . . . . .
C25 C 0.8184(3) 0.8524(3) 0.0058(3) 0.0187(10) Uani 1 1 d . . . . .
C26 C 0.7725(3) 0.7761(3) 0.0281(3) 0.0212(11) Uani 1 1 d . . . . .
C27 C 0.7019(4) 0.7339(4) -0.0047(3) 0.0253(13) Uani 1 1 d . . . . .
H27 H 0.6712 0.6822 0.0090 0.030 Uiso 1 1 calc R . . . .
C28 C 0.6733(3) 0.7626(4) -0.0563(3) 0.0280(13) Uani 1 1 d . . . . .
C29 C 0.7180(3) 0.8387(3) -0.0747(4) 0.0233(10) Uani 1 1 d . . . . .
H29 H 0.6994 0.8606 -0.1084 0.028 Uiso 1 1 calc R . . . .
C30 C 0.7973(3) 0.7433(3) 0.0902(3) 0.0183(10) Uani 1 1 d . . . . .
C31 C 0.8970(4) 0.7148(3) 0.1383(4) 0.0248(12) Uani 1 1 d . . . . .
H31 H 0.9466 0.7178 0.1274 0.030 Uiso 1 1 calc R . . . .
C32 C 0.8306(3) 0.7587(3) 0.2227(3) 0.0211(11) Uani 1 1 d . . . . .
H32 H 0.8367 0.7897 0.2666 0.025 Uiso 1 1 calc R . . . .
C33 C 0.7608(5) 0.6284(4) 0.1694(3) 0.0270(15) Uani 1 1 d . . . . .
H33 H 0.7210 0.5744 0.1783 0.032 Uiso 1 1 calc R . . . .
C34 C 0.8733(3) 0.7458(3) 0.0743(3) 0.0217(11) Uani 1 1 d . . . . .
H34A H 0.8676 0.7151 0.0310 0.026 Uiso 1 1 calc R . . . .
H34B H 0.9133 0.7989 0.0645 0.026 Uiso 1 1 calc R . . . .
C35 C 0.7369(3) 0.6592(3) 0.1058(3) 0.0227(11) Uani 1 1 d . . . . .
H35A H 0.6875 0.6556 0.1165 0.027 Uiso 1 1 calc R . . . .
H35B H 0.7303 0.6280 0.0627 0.027 Uiso 1 1 calc R . . . .
C36 C 0.9057(3) 0.7627(3) 0.2057(3) 0.0228(12) Uani 1 1 d . . . . .
H36A H 0.9217 0.7432 0.2470 0.027 Uiso 1 1 calc R . . . .
H36B H 0.9454 0.8161 0.1972 0.027 Uiso 1 1 calc R . . . .
C37 C 0.7700(4) 0.6758(3) 0.2368(3) 0.0234(12) Uani 1 1 d . . . . .
H37A H 0.7211 0.6726 0.2487 0.028 Uiso 1 1 calc R . . . .
H37B H 0.7854 0.6558 0.2780 0.028 Uiso 1 1 calc R . . . .
C38 C 0.8060(4) 0.7898(3) 0.1591(3) 0.0192(11) Uani 1 1 d . . . . .
H38A H 0.8445 0.8438 0.1509 0.023 Uiso 1 1 calc R . . . .
H38B H 0.7571 0.7870 0.1705 0.023 Uiso 1 1 calc R . . . .
C39 C 0.8368(4) 0.6324(4) 0.1530(4) 0.0297(13) Uani 1 1 d . . . . .
H39A H 0.8524 0.6127 0.1945 0.036 Uiso 1 1 calc R . . . .
H39B H 0.8313 0.6006 0.1106 0.036 Uiso 1 1 calc R . . . .
C40 C 0.5967(4) 0.7140(4) -0.0910(4) 0.0421(18) Uani 1 1 d . . . . .
H40A H 0.5734 0.6623 -0.0717 0.063 Uiso 1 1 calc R . . . .
H40B H 0.5640 0.7355 -0.0807 0.063 Uiso 1 1 calc R . . . .
H40C H 0.6031 0.7128 -0.1431 0.063 Uiso 1 1 calc R . . . .
O100 O 0.5446(8) 1.0048(8) 0.7638(10) 0.161(4) Uani 1 1 d D U . . .
C101 C 0.4932(13) 0.9561(13) 0.6999(12) 0.154(4) Uani 1 1 d D U . . .
H10A H 0.4757 0.9850 0.6705 0.185 Uiso 1 1 calc R . . . .
H10B H 0.5199 0.9374 0.6687 0.185 Uiso 1 1 calc R . . . .
C102 C 0.4343(12) 0.8979(13) 0.7361(13) 0.170(5) Uani 1 1 d D U . . .
H10C H 0.4044 0.8543 0.7037 0.204 Uiso 1 1 calc R . . . .
H10D H 0.4003 0.9146 0.7569 0.204 Uiso 1 1 calc R . . . .
C103 C 0.4706(14) 0.8775(12) 0.7925(13) 0.172(5) Uani 1 1 d D U . . .
H10E H 0.4333 0.8371 0.8244 0.206 Uiso 1 1 calc R . . . .
H10F H 0.5066 0.8626 0.7731 0.206 Uiso 1 1 calc R . . . .
C104 C 0.5089(14) 0.9514(12) 0.8273(11) 0.164(4) Uani 1 1 d D U . . .
H10G H 0.5480 0.9554 0.8615 0.197 Uiso 1 1 calc R . . . .
H10H H 0.4723 0.9618 0.8529 0.197 Uiso 1 1 calc R . . . .
O200 O 0.4911(10) 0.4171(10) 0.5459(10) 0.087(4) Uani 0.5 1 d D U . . .
C201 C 0.5627(13) 0.4456(16) 0.5064(13) 0.091(4) Uani 0.5 1 d D U . . .
H20D H 0.5558 0.4145 0.4630 0.109 Uiso 0.5 1 calc R . . . .
H20E H 0.5833 0.4992 0.4918 0.109 Uiso 0.5 1 calc R . . . .
C202 C 0.6113(12) 0.4383(15) 0.5578(15) 0.096(4) Uani 0.5 1 d D U . . .
H20F H 0.6337 0.4822 0.5911 0.116 Uiso 0.5 1 calc R . . . .
H20G H 0.6528 0.4350 0.5334 0.116 Uiso 0.5 1 calc R . . . .
C203 C 0.5615(13) 0.3681(15) 0.5963(16) 0.098(4) Uani 0.5 1 d D U . . .
H20H H 0.5607 0.3243 0.5721 0.118 Uiso 0.5 1 calc R . . . .
H20I H 0.5796 0.3710 0.6462 0.118 Uiso 0.5 1 calc R . . . .
C204 C 0.4873(13) 0.3594(15) 0.5963(15) 0.091(4) Uani 0.5 1 d D U . . .
H20J H 0.4735 0.3679 0.6450 0.110 Uiso 0.5 1 calc R . . . .
H20K H 0.4491 0.3078 0.5801 0.110 Uiso 0.5 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 Se1 2.9156(14) . ?
U1 O1 2.164(4) . ?
U1 O1 2.164(4) 2_655 ?
U1 O1 2.164(4) 3_665 ?
U1 N1 2.662(5) . ?
U1 N1 2.662(5) 3_665 ?
U1 N1 2.662(5) 2_655 ?
Se1 H1 0.8400 . ?
O1 C5 1.348(6) . ?
N1 C1 1.479(7) . ?
N1 C2 1.501(8) . ?
N1 C3 1.501(7) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.527(8) 3_665 ?
C2 C1 1.527(8) 2_655 ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C4 1.501(8) . ?
C4 C5 1.403(8) . ?
C4 C9 1.395(8) . ?
C5 C6 1.416(8) . ?
C6 C7 1.399(8) . ?
C6 C10 1.524(8) . ?
C7 H7 0.9500 . ?
C7 C8 1.391(9) . ?
C8 C9 1.390(9) . ?
C8 C20 1.504(8) . ?
C9 H9 0.9500 . ?
C10 C14 1.549(9) . ?
C10 C15 1.551(8) . ?
C10 C18 1.554(9) . ?
C11 H11 1.0000 . ?
C11 C14 1.531(10) . ?
C11 C16 1.499(12) . ?
C11 C19 1.532(10) . ?
C12 H12 1.0000 . ?
C12 C16 1.520(11) . ?
C12 C17 1.530(10) . ?
C12 C18 1.517(9) . ?
C13 H13 1.0000 . ?
C13 C15 1.530(9) . ?
C13 C17 1.531(11) . ?
C13 C19 1.537(11) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
U2 Se2 2.9006(11) . ?
U2 O2 2.173(4) 2_765 ?
U2 O2 2.173(4) . ?
U2 O2 2.173(4) 3_675 ?
U2 N2 2.629(4) . ?
U2 N2 2.629(4) 3_675 ?
U2 N2 2.629(4) 2_765 ?
Se2 H2 0.8400 . ?
O2 C25 1.357(6) . ?
N2 C21 1.474(7) . ?
N2 C22 1.489(7) . ?
N2 C23 1.493(7) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C21 C22 1.518(8) 3_675 ?
C22 C21 1.518(8) 2_765 ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C23 C24 1.497(8) . ?
C24 C25 1.407(8) . ?
C24 C29 1.396(8) . ?
C25 C26 1.416(8) . ?
C26 C27 1.392(8) . ?
C26 C30 1.539(8) . ?
C27 H27 0.9500 . ?
C27 C28 1.392(9) . ?
C28 C29 1.389(9) . ?
C28 C40 1.509(9) . ?
C29 H29 0.9500 . ?
C30 C34 1.548(8) . ?
C30 C35 1.553(8) . ?
C30 C38 1.551(8) . ?
C31 H31 1.0000 . ?
C31 C34 1.533(9) . ?
C31 C36 1.542(8) . ?
C31 C39 1.527(9) . ?
C32 H32 1.0000 . ?
C32 C36 1.522(9) . ?
C32 C37 1.532(8) . ?
C32 C38 1.538(8) . ?
C33 H33 1.0000 . ?
C33 C35 1.527(9) . ?
C33 C37 1.534(8) . ?
C33 C39 1.538(11) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
O100 C101 1.566(19) . ?
O100 C104 1.520(19) . ?
C101 H10A 0.9900 . ?
C101 H10B 0.9900 . ?
C101 C102 1.367(16) . ?
C102 H10C 0.9900 . ?
C102 H10D 0.9900 . ?
C102 C103 1.457(18) . ?
C103 H10E 0.9900 . ?
C103 H10F 0.9900 . ?
C103 C104 1.454(16) . ?
C104 H10G 0.9900 . ?
C104 H10H 0.9900 . ?
O200 C201 1.47(2) . ?
O200 C204 1.47(2) . ?
C201 H20D 0.9900 . ?
C201 H20E 0.9900 . ?
C201 C202 1.434(17) . ?
C202 H20F 0.9900 . ?
C202 H20G 0.9900 . ?
C202 C203 1.460(19) . ?
C203 H20H 0.9900 . ?
C203 H20I 0.9900 . ?
C203 C204 1.428(17) . ?
C204 H20J 0.9900 . ?
C204 H20K 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 U1 Se1 82.78(11) 2_655 . ?
O1 U1 Se1 82.78(11) 3_665 . ?
O1 U1 Se1 82.78(11) . . ?
O1 U1 O1 118.45(5) . 2_655 ?
O1 U1 O1 118.44(5) 2_655 3_665 ?
O1 U1 O1 118.45(5) . 3_665 ?
O1 U1 N1 71.15(15) 2_655 2_655 ?
O1 U1 N1 71.15(15) 3_665 3_665 ?
O1 U1 N1 84.94(15) 2_655 3_665 ?
O1 U1 N1 134.81(15) 2_655 . ?
O1 U1 N1 134.81(15) . 3_665 ?
O1 U1 N1 134.81(15) 3_665 2_655 ?
O1 U1 N1 84.94(15) . 2_655 ?
O1 U1 N1 71.15(15) . . ?
O1 U1 N1 84.94(15) 3_665 . ?
N1 U1 Se1 141.18(10) 2_655 . ?
N1 U1 Se1 141.18(10) 3_665 . ?
N1 U1 Se1 141.18(10) . . ?
N1 U1 N1 65.76(17) 2_655 . ?
N1 U1 N1 65.76(17) . 3_665 ?
N1 U1 N1 65.76(17) 2_655 3_665 ?
U1 Se1 H1 109.5 . . ?
C5 O1 U1 150.5(4) . . ?
C1 N1 U1 106.7(3) . . ?
C1 N1 C2 110.5(4) . . ?
C1 N1 C3 107.0(4) . . ?
C2 N1 U1 115.2(3) . . ?
C3 N1 U1 107.0(3) . . ?
C3 N1 C2 109.9(4) . . ?
N1 C1 H1A 109.2 . . ?
N1 C1 H1B 109.2 . . ?
N1 C1 C2 111.9(5) . 3_665 ?
H1A C1 H1B 107.9 . . ?
C2 C1 H1A 109.2 3_665 . ?
C2 C1 H1B 109.2 3_665 . ?
N1 C2 C1 112.8(5) . 2_655 ?
N1 C2 H2A 109.0 . . ?
N1 C2 H2B 109.0 . . ?
C1 C2 H2A 109.0 2_655 . ?
C1 C2 H2B 109.0 2_655 . ?
H2A C2 H2B 107.8 . . ?
N1 C3 H3A 108.4 . . ?
N1 C3 H3B 108.4 . . ?
N1 C3 C4 115.6(5) . . ?
H3A C3 H3B 107.4 . . ?
C4 C3 H3A 108.4 . . ?
C4 C3 H3B 108.4 . . ?
C5 C4 C3 120.2(5) . . ?
C9 C4 C3 119.6(5) . . ?
C9 C4 C5 120.2(5) . . ?
O1 C5 C4 117.3(5) . . ?
O1 C5 C6 122.1(5) . . ?
C4 C5 C6 120.6(5) . . ?
C5 C6 C10 121.5(5) . . ?
C7 C6 C5 116.4(5) . . ?
C7 C6 C10 122.1(5) . . ?
C6 C7 H7 117.8 . . ?
C8 C7 C6 124.3(5) . . ?
C8 C7 H7 117.8 . . ?
C7 C8 C20 120.7(6) . . ?
C9 C8 C7 117.6(5) . . ?
C9 C8 C20 121.7(6) . . ?
C4 C9 H9 119.5 . . ?
C8 C9 C4 120.9(6) . . ?
C8 C9 H9 119.5 . . ?
C6 C10 C14 110.1(5) . . ?
C6 C10 C15 112.3(5) . . ?
C6 C10 C18 110.9(5) . . ?
C14 C10 C15 106.4(5) . . ?
C14 C10 C18 110.1(5) . . ?
C15 C10 C18 106.8(5) . . ?
C14 C11 H11 109.4 . . ?
C14 C11 C19 109.2(6) . . ?
C16 C11 H11 109.4 . . ?
C16 C11 C14 109.8(6) . . ?
C16 C11 C19 109.7(7) . . ?
C19 C11 H11 109.4 . . ?
C16 C12 H12 108.7 . . ?
C16 C12 C17 110.4(6) . . ?
C17 C12 H12 108.7 . . ?
C18 C12 H12 108.7 . . ?
C18 C12 C16 111.2(6) . . ?
C18 C12 C17 109.2(6) . . ?
C15 C13 H13 109.2 . . ?
C15 C13 C17 110.1(6) . . ?
C15 C13 C19 110.2(6) . . ?
C17 C13 H13 109.2 . . ?
C17 C13 C19 108.9(6) . . ?
C19 C13 H13 109.2 . . ?
C10 C14 H14A 109.4 . . ?
C10 C14 H14B 109.4 . . ?
C11 C14 C10 111.0(5) . . ?
C11 C14 H14A 109.4 . . ?
C11 C14 H14B 109.4 . . ?
H14A C14 H14B 108.0 . . ?
C10 C15 H15A 109.5 . . ?
C10 C15 H15B 109.5 . . ?
C13 C15 C10 110.8(5) . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
H15A C15 H15B 108.1 . . ?
C11 C16 C12 109.8(6) . . ?
C11 C16 H16A 109.7 . . ?
C11 C16 H16B 109.7 . . ?
C12 C16 H16A 109.7 . . ?
C12 C16 H16B 109.7 . . ?
H16A C16 H16B 108.2 . . ?
C12 C17 C13 108.1(6) . . ?
C12 C17 H17A 110.1 . . ?
C12 C17 H17B 110.1 . . ?
C13 C17 H17A 110.1 . . ?
C13 C17 H17B 110.1 . . ?
H17A C17 H17B 108.4 . . ?
C10 C18 H18A 109.7 . . ?
C10 C18 H18B 109.7 . . ?
C12 C18 C10 109.7(5) . . ?
C12 C18 H18A 109.7 . . ?
C12 C18 H18B 109.7 . . ?
H18A C18 H18B 108.2 . . ?
C11 C19 C13 108.8(6) . . ?
C11 C19 H19A 109.9 . . ?
C11 C19 H19B 109.9 . . ?
C13 C19 H19A 109.9 . . ?
C13 C19 H19B 109.9 . . ?
H19A C19 H19B 108.3 . . ?
C8 C20 H20A 109.5 . . ?
C8 C20 H20B 109.5 . . ?
C8 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O2 U2 Se2 81.90(9) 2_765 . ?
O2 U2 Se2 81.90(9) . . ?
O2 U2 Se2 81.90(9) 3_675 . ?
O2 U2 O2 118.05(4) . 3_675 ?
O2 U2 O2 118.05(4) 2_765 3_675 ?
O2 U2 O2 118.05(4) 2_765 . ?
O2 U2 N2 136.23(13) . 3_675 ?
O2 U2 N2 85.04(14) 3_675 . ?
O2 U2 N2 85.05(14) . 2_765 ?
O2 U2 N2 72.04(13) 3_675 3_675 ?
O2 U2 N2 72.04(13) 2_765 2_765 ?
O2 U2 N2 136.23(13) 2_765 . ?
O2 U2 N2 136.23(13) 3_675 2_765 ?
O2 U2 N2 72.04(13) . . ?
O2 U2 N2 85.05(14) 2_765 3_675 ?
N2 U2 Se2 140.76(9) 2_765 . ?
N2 U2 Se2 140.76(9) . . ?
N2 U2 Se2 140.76(9) 3_675 . ?
N2 U2 N2 66.43(15) 2_765 3_675 ?
N2 U2 N2 66.43(15) 2_765 . ?
N2 U2 N2 66.43(15) 3_675 . ?
U2 Se2 H2 109.5 . . ?
C25 O2 U2 148.2(3) . . ?
C21 N2 U2 106.9(3) . . ?
C21 N2 C22 110.4(4) . . ?
C21 N2 C23 107.8(4) . . ?
C22 N2 U2 115.0(3) . . ?
C22 N2 C23 110.4(4) . . ?
C23 N2 U2 106.0(3) . . ?
N2 C21 H21A 109.1 . . ?
N2 C21 H21B 109.1 . . ?
N2 C21 C22 112.4(4) . 3_675 ?
H21A C21 H21B 107.9 . . ?
C22 C21 H21A 109.1 3_675 . ?
C22 C21 H21B 109.1 3_675 . ?
N2 C22 C21 113.3(4) . 2_765 ?
N2 C22 H22A 108.9 . . ?
N2 C22 H22B 108.9 . . ?
C21 C22 H22A 108.9 2_765 . ?
C21 C22 H22B 108.9 2_765 . ?
H22A C22 H22B 107.7 . . ?
N2 C23 H23A 108.7 . . ?
N2 C23 H23B 108.7 . . ?
N2 C23 C24 114.3(4) . . ?
H23A C23 H23B 107.6 . . ?
C24 C23 H23A 108.7 . . ?
C24 C23 H23B 108.7 . . ?
C25 C24 C23 119.8(5) . . ?
C29 C24 C23 119.8(5) . . ?
C29 C24 C25 120.4(5) . . ?
O2 C25 C24 116.8(5) . . ?
O2 C25 C26 123.6(5) . . ?
C24 C25 C26 119.6(5) . . ?
C25 C26 C30 121.1(5) . . ?
C27 C26 C25 117.3(5) . . ?
C27 C26 C30 121.5(5) . . ?
C26 C27 H27 117.9 . . ?
C28 C27 C26 124.2(6) . . ?
C28 C27 H27 117.9 . . ?
C27 C28 C40 122.1(6) . . ?
C29 C28 C27 117.3(5) . . ?
C29 C28 C40 120.7(6) . . ?
C24 C29 H29 119.4 . . ?
C28 C29 C24 121.1(5) . . ?
C28 C29 H29 119.4 . . ?
C26 C30 C34 112.3(5) . . ?
C26 C30 C35 111.5(5) . . ?
C26 C30 C38 108.6(4) . . ?
C34 C30 C35 107.4(5) . . ?
C34 C30 C38 109.2(4) . . ?
C38 C30 C35 107.7(5) . . ?
C34 C31 H31 109.4 . . ?
C34 C31 C36 109.4(5) . . ?
C36 C31 H31 109.4 . . ?
C39 C31 H31 109.4 . . ?
C39 C31 C34 110.3(5) . . ?
C39 C31 C36 108.8(5) . . ?
C36 C32 H32 109.4 . . ?
C36 C32 C37 109.1(5) . . ?
C36 C32 C38 110.0(5) . . ?
C37 C32 H32 109.4 . . ?
C37 C32 C38 109.7(5) . . ?
C38 C32 H32 109.4 . . ?
C35 C33 H33 109.3 . . ?
C35 C33 C37 109.9(6) . . ?
C35 C33 C39 110.1(5) . . ?
C37 C33 H33 109.3 . . ?
C37 C33 C39 108.9(6) . . ?
C39 C33 H33 109.3 . . ?
C30 C34 H34A 109.5 . . ?
C30 C34 H34B 109.5 . . ?
C31 C34 C30 110.6(5) . . ?
C31 C34 H34A 109.5 . . ?
C31 C34 H34B 109.5 . . ?
H34A C34 H34B 108.1 . . ?
C30 C35 H35A 109.5 . . ?
C30 C35 H35B 109.5 . . ?
C33 C35 C30 110.9(5) . . ?
C33 C35 H35A 109.5 . . ?
C33 C35 H35B 109.5 . . ?
H35A C35 H35B 108.0 . . ?
C31 C36 H36A 109.7 . . ?
C31 C36 H36B 109.7 . . ?
C32 C36 C31 109.9(5) . . ?
C32 C36 H36A 109.7 . . ?
C32 C36 H36B 109.7 . . ?
H36A C36 H36B 108.2 . . ?
C32 C37 C33 109.2(5) . . ?
C32 C37 H37A 109.8 . . ?
C32 C37 H37B 109.8 . . ?
C33 C37 H37A 109.8 . . ?
C33 C37 H37B 109.8 . . ?
H37A C37 H37B 108.3 . . ?
C30 C38 H38A 109.6 . . ?
C30 C38 H38B 109.6 . . ?
C32 C38 C30 110.3(5) . . ?
C32 C38 H38A 109.6 . . ?
C32 C38 H38B 109.6 . . ?
H38A C38 H38B 108.1 . . ?
C31 C39 C33 109.0(5) . . ?
C31 C39 H39A 109.9 . . ?
C31 C39 H39B 109.9 . . ?
C33 C39 H39A 109.9 . . ?
C33 C39 H39B 109.9 . . ?
H39A C39 H39B 108.3 . . ?
C28 C40 H40A 109.5 . . ?
C28 C40 H40B 109.5 . . ?
C28 C40 H40C 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C104 O100 C101 102.0(14) . . ?
O100 C101 H10A 111.6 . . ?
O100 C101 H10B 111.6 . . ?
H10A C101 H10B 109.4 . . ?
C102 C101 O100 101.1(15) . . ?
C102 C101 H10A 111.6 . . ?
C102 C101 H10B 111.6 . . ?
C101 C102 H10C 110.8 . . ?
C101 C102 H10D 110.8 . . ?
C101 C102 C103 104.6(17) . . ?
H10C C102 H10D 108.9 . . ?
C103 C102 H10C 110.8 . . ?
C103 C102 H10D 110.8 . . ?
C102 C103 H10E 112.5 . . ?
C102 C103 H10F 112.5 . . ?
H10E C103 H10F 110.0 . . ?
C104 C103 C102 96.4(16) . . ?
C104 C103 H10E 112.5 . . ?
C104 C103 H10F 112.5 . . ?
O100 C104 H10G 111.3 . . ?
O100 C104 H10H 111.3 . . ?
C103 C104 O100 102.2(15) . . ?
C103 C104 H10G 111.3 . . ?
C103 C104 H10H 111.3 . . ?
H10G C104 H10H 109.2 . . ?
C201 O200 C204 106.3(16) . . ?
O200 C201 H20D 111.2 . . ?
O200 C201 H20E 111.2 . . ?
H20D C201 H20E 109.1 . . ?
C202 C201 O200 102.9(17) . . ?
C202 C201 H20D 111.2 . . ?
C202 C201 H20E 111.2 . . ?
C201 C202 H20F 110.8 . . ?
C201 C202 H20G 110.8 . . ?
C201 C202 C203 104.6(16) . . ?
H20F C202 H20G 108.9 . . ?
C203 C202 H20F 110.8 . . ?
C203 C202 H20G 110.8 . . ?
C202 C203 H20H 110.3 . . ?
C202 C203 H20I 110.3 . . ?
H20H C203 H20I 108.6 . . ?
C204 C203 C202 107.0(16) . . ?
C204 C203 H20H 110.3 . . ?
C204 C203 H20I 110.3 . . ?
O200 C204 H20J 110.6 . . ?
O200 C204 H20K 110.6 . . ?
C203 C204 O200 105.7(16) . . ?
C203 C204 H20J 110.6 . . ?
C203 C204 H20K 110.6 . . ?
H20J C204 H20K 108.7 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
U1 O1 C5 C4 9.4(11) . . . . ?
U1 O1 C5 C6 -168.7(5) . . . . ?
U1 N1 C1 C2 -59.3(5) . . . 3_665 ?
U1 N1 C2 C1 -11.3(6) . . . 2_655 ?
U1 N1 C3 C4 74.7(5) . . . . ?
O1 C5 C6 C7 178.0(5) . . . . ?
O1 C5 C6 C10 -4.0(9) . . . . ?
N1 C3 C4 C5 -56.0(8) . . . . ?
N1 C3 C4 C9 127.7(6) . . . . ?
C1 N1 C2 C1 -132.4(5) . . . 2_655 ?
C1 N1 C3 C4 -171.2(5) . . . . ?
C2 N1 C1 C2 66.7(6) . . . 3_665 ?
C2 N1 C3 C4 -51.1(7) . . . . ?
C3 N1 C1 C2 -173.7(5) . . . 3_665 ?
C3 N1 C2 C1 109.7(5) . . . 2_655 ?
C3 C4 C5 O1 6.8(8) . . . . ?
C3 C4 C5 C6 -175.0(6) . . . . ?
C3 C4 C9 C8 175.8(6) . . . . ?
C4 C5 C6 C7 0.0(9) . . . . ?
C4 C5 C6 C10 177.9(6) . . . . ?
C5 C4 C9 C8 -0.5(10) . . . . ?
C5 C6 C7 C8 -2.1(10) . . . . ?
C5 C6 C10 C14 64.1(7) . . . . ?
C5 C6 C10 C15 -177.4(6) . . . . ?
C5 C6 C10 C18 -58.1(7) . . . . ?
C6 C7 C8 C9 2.7(10) . . . . ?
C6 C7 C8 C20 -179.5(7) . . . . ?
C6 C10 C14 C11 -177.7(5) . . . . ?
C6 C10 C15 C13 -179.8(6) . . . . ?
C6 C10 C18 C12 176.6(5) . . . . ?
C7 C6 C10 C14 -118.1(6) . . . . ?
C7 C6 C10 C15 0.3(8) . . . . ?
C7 C6 C10 C18 119.7(6) . . . . ?
C7 C8 C9 C4 -1.4(10) . . . . ?
C9 C4 C5 O1 -176.9(5) . . . . ?
C9 C4 C5 C6 1.2(9) . . . . ?
C10 C6 C7 C8 -180.0(6) . . . . ?
C14 C10 C15 C13 -59.2(7) . . . . ?
C14 C10 C18 C12 54.4(6) . . . . ?
C14 C11 C16 C12 -60.4(8) . . . . ?
C14 C11 C19 C13 59.7(8) . . . . ?
C15 C10 C14 C11 60.3(7) . . . . ?
C15 C10 C18 C12 -60.7(6) . . . . ?
C15 C13 C17 C12 59.9(8) . . . . ?
C15 C13 C19 C11 -59.3(8) . . . . ?
C16 C11 C14 C10 58.2(7) . . . . ?
C16 C11 C19 C13 -60.7(8) . . . . ?
C16 C12 C17 C13 60.2(8) . . . . ?
C16 C12 C18 C10 -57.9(7) . . . . ?
C17 C12 C16 C11 -60.0(8) . . . . ?
C17 C12 C18 C10 64.2(7) . . . . ?
C17 C13 C15 C10 -59.6(7) . . . . ?
C17 C13 C19 C11 61.5(8) . . . . ?
C18 C10 C14 C11 -55.1(7) . . . . ?
C18 C10 C15 C13 58.4(7) . . . . ?
C18 C12 C16 C11 61.4(7) . . . . ?
C18 C12 C17 C13 -62.3(8) . . . . ?
C19 C11 C14 C10 -62.1(8) . . . . ?
C19 C11 C16 C12 59.6(8) . . . . ?
C19 C13 C15 C10 60.4(7) . . . . ?
C19 C13 C17 C12 -60.9(7) . . . . ?
C20 C8 C9 C4 -179.1(7) . . . . ?
U2 O2 C25 C24 -17.9(10) . . . . ?
U2 O2 C25 C26 160.7(5) . . . . ?
U2 N2 C21 C22 57.6(5) . . . 3_675 ?
U2 N2 C22 C21 10.4(5) . . . 2_765 ?
U2 N2 C23 C24 -78.2(4) . . . . ?
O2 C25 C26 C27 -175.0(5) . . . . ?
O2 C25 C26 C30 9.7(8) . . . . ?
N2 C23 C24 C25 58.6(7) . . . . ?
N2 C23 C24 C29 -122.1(6) . . . . ?
C21 N2 C22 C21 131.4(5) . . . 2_765 ?
C21 N2 C23 C24 167.6(4) . . . . ?
C22 N2 C21 C22 -68.1(6) . . . 3_675 ?
C22 N2 C23 C24 47.0(6) . . . . ?
C23 N2 C21 C22 171.2(4) . . . 3_675 ?
C23 N2 C22 C21 -109.6(5) . . . 2_765 ?
C23 C24 C25 O2 -4.6(8) . . . . ?
C23 C24 C25 C26 176.8(5) . . . . ?
C23 C24 C29 C28 -179.8(6) . . . . ?
C24 C25 C26 C27 3.5(8) . . . . ?
C24 C25 C26 C30 -171.8(5) . . . . ?
C25 C24 C29 C28 -0.5(9) . . . . ?
C25 C26 C27 C28 -1.6(9) . . . . ?
C25 C26 C30 C34 -60.7(7) . . . . ?
C25 C26 C30 C35 178.7(5) . . . . ?
C25 C26 C30 C38 60.2(7) . . . . ?
C26 C27 C28 C29 -1.3(10) . . . . ?
C26 C27 C28 C40 179.1(6) . . . . ?
C26 C30 C34 C31 178.3(4) . . . . ?
C26 C30 C35 C33 -177.8(5) . . . . ?
C26 C30 C38 C32 179.9(5) . . . . ?
C27 C26 C30 C34 124.2(6) . . . . ?
C27 C26 C30 C35 3.6(7) . . . . ?
C27 C26 C30 C38 -114.9(6) . . . . ?
C27 C28 C29 C24 2.4(9) . . . . ?
C29 C24 C25 O2 176.1(5) . . . . ?
C29 C24 C25 C26 -2.5(8) . . . . ?
C30 C26 C27 C28 173.7(6) . . . . ?
C34 C30 C35 C33 58.7(6) . . . . ?
C34 C30 C38 C32 -57.4(6) . . . . ?
C34 C31 C36 C32 60.0(6) . . . . ?
C34 C31 C39 C33 -59.3(7) . . . . ?
C35 C30 C34 C31 -58.6(6) . . . . ?
C35 C30 C38 C32 58.9(6) . . . . ?
C35 C33 C37 C32 -59.6(7) . . . . ?
C35 C33 C39 C31 59.1(7) . . . . ?
C36 C31 C34 C30 -59.1(6) . . . . ?
C36 C31 C39 C33 60.7(7) . . . . ?
C36 C32 C37 C33 -60.4(6) . . . . ?
C36 C32 C38 C30 59.1(6) . . . . ?
C37 C32 C36 C31 60.2(6) . . . . ?
C37 C32 C38 C30 -60.8(6) . . . . ?
C37 C33 C35 C30 59.9(7) . . . . ?
C37 C33 C39 C31 -61.4(7) . . . . ?
C38 C30 C34 C31 57.8(6) . . . . ?
C38 C30 C35 C33 -58.8(6) . . . . ?
C38 C32 C36 C31 -60.1(6) . . . . ?
C38 C32 C37 C33 60.0(7) . . . . ?
C39 C31 C34 C30 60.5(6) . . . . ?
C39 C31 C36 C32 -60.5(6) . . . . ?
C39 C33 C35 C30 -60.1(6) . . . . ?
C39 C33 C37 C32 61.1(7) . . . . ?
C40 C28 C29 C24 -178.0(6) . . . . ?
O100 C101 C102 C103 -44(2) . . . . ?
C101 O100 C104 C103 23(2) . . . . ?
C101 C102 C103 C104 59(2) . . . . ?
C102 C103 C104 O100 -47(2) . . . . ?
C104 O100 C101 C102 12(2) . . . . ?
O200 C201 C202 C203 37(3) . . . . ?
C201 O200 C204 C203 13(3) . . . . ?
C201 C202 C203 C204 -30(3) . . . . ?
C202 C203 C204 O200 10(3) . . . . ?
C204 O200 C201 C202 -31(3) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'


# SQUEEZE RESULTS (APPEND TO CIF)
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 0.052 0.849 0.109 7.6 -0.9
2 0.151 0.203 0.109 7.6 -0.9
3 0.797 0.948 0.109 7.6 -0.9
4 0.667 0.333 0.330 138.1 68.7
5 0.203 0.052 0.609 7.6 -0.7
6 0.849 0.797 0.609 7.6 -0.8
7 0.948 0.151 0.609 7.6 -0.8
8 0.333 0.667 0.830 138.0 71.9
_platon_squeeze_details          
;
 Spek, A.L. (2003), J.Appl.Cryst. 36, 7-13
;


# start Validation Reply Form
_vrf_CHEMW03_mr1521sq            
;
PROBLEM: WARNING: The ratio of given/expected molecular weight as
RESPONSE: This discrepancy is due to the fact that part of the included solvent
molecules could not be modelled and the SQUEEZE routine was employed.
Please refer to the _refine_special_details section.          

;
_vrf_PLAT413_mr1521sq            
;
PROBLEM: Short Inter XH3 .. XHn     H20C   ..  H20E    ..       1.98 Ang.  
RESPONSE: This apparent short inter H...H contact is between two hydrogen 
atoms of the solvent thf molecule O200 - C204 that is occupied by only 50 %.
;
_vrf_PLAT987_mr1521sq            
;
PROBLEM: The Flack x is >> 0 -  Do a BASF/TWIN Refinement     Please Check
RESPONSE: Refinement of the absolute structure parameter yielded a value of 
0.019(2) which confidently confirms that the refined model represents the 
true absolute structure.
;
