# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_2_2toluene
_database_code_depnum_ccdc_archive 'CCDC 1812761'
_audit_update_record             
;
2017-12-20 deposited with the CCDC.
2018-03-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        '[{pinBO(py)UOU(py)OBpin}(LA)]'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C80 H82 B2 N10 O7 U2, 2(C7 H8)'
_chemical_formula_sum            'C94 H98 B2 N10 O7 U2'
_chemical_formula_weight         1977.50

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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   14.7593(5)
_cell_length_b                   15.6981(6)
_cell_length_c                   20.1394(7)
_cell_angle_alpha                74.615(2)
_cell_angle_beta                 87.841(2)
_cell_angle_gamma                69.604(2)
_cell_volume                     4209.1(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9288
_cell_measurement_theta_min      2.42
_cell_measurement_theta_max      28.19

_exptl_crystal_description       slab
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.560
_exptl_crystal_F_000             1964
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.820
_exptl_crystal_size_mid          0.440
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    3.905
_shelx_estimated_absorpt_T_min   0.142
_shelx_estimated_absorpt_T_max   0.509
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.1950
_exptl_absorpt_correction_T_max  0.6435
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            192088
_diffrn_reflns_av_unetI/netI     0.0156
_diffrn_reflns_av_R_equivalents  0.0284
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         1.758
_diffrn_reflns_theta_max         28.316
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             20508
_reflns_number_gt                17854
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_refine_special_details          
;
Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.

The axially coordinated OBpin ligand (O(1), B(1), O(4), O(5), C(69), C(70), 
C(71), C(72), C(73), C(74)) was positionally/rotationally disordered over 
two positions, so was split into two parts and refined with an occupancy 
ratio of 0.79:0.21. The minor component is rotated nearly 90 degrees to the 
major component, and anisotropic refinement of the thermal parameters of the 
minor component resulted in unstable refinement. As a result, they were 
refined isotropically. The thermal parameters of both parts were also 
restrained through the use of the RIGU command, and the thermal and positional
parameters of B(1) and B(1A) were refined to be equal to one another through 
the use of the EADP and EXYZ commands, respectively. Second, C(8) was 
positionally disordered over two positions, so was split into two parts and 
refined anisotropically with an occupancy ratio of 0.67:0.33. The thermal 
parameters of C(8) and C(8A) were refined to be similar to one another through 
the use of the SIMU command. Finally, both molecules of toluene within the 
lattice were positionally disordered over two positions. Both were split into 
two parts and refined anisotropically in a 0.56:0.44 (C(100)-C(106):C(110)-
C(116); C(120)-C(126):C(130)-C(136)) ratio.
Furthermore, the aryl C- and H-atoms of toluene C(130)-C(135) were restained to 
lie in a common plane through the use of the FLAT command, the thermal 
parameters of toluenes C(120)-C(126) and C(130)-C(136) were restrained with the 
RIGU command, and the C(100)-C(106), C(110)-C(116) and C(120)-C(126) bond 
lengths were fixed at 1.52 Angstroms using the DFIX command.    
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0134P)²+10.1197P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         20508
_refine_ls_number_parameters     1140
_refine_ls_number_restraints     238
_refine_ls_R_factor_all          0.0335
_refine_ls_R_factor_gt           0.0248
_refine_ls_wR_factor_ref         0.0568
_refine_ls_wR_factor_gt          0.0516
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_restrained_S_all      1.135
_refine_ls_shift/su_max          0.032
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.51973(2) 0.49951(2) 0.26662(2) 0.01783(3) Uani 1 1 d . . . . .
U2 U 0.49225(2) 0.23229(2) 0.29226(2) 0.01614(3) Uani 1 1 d . . . . .
O1 O 0.55091(16) 0.62867(14) 0.23435(11) 0.0275(4) Uani 1 1 d . . . . .
O2 O 0.64719(14) 0.15546(14) 0.29840(10) 0.0245(4) Uani 1 1 d . . . . .
O3 O 0.50124(13) 0.36676(13) 0.28083(10) 0.0202(4) Uani 1 1 d . . . . .
N1 N 0.49248(18) 0.53444(17) 0.13445(12) 0.0239(5) Uani 1 1 d . . . . .
N2 N 0.35232(18) 0.59990(18) 0.22676(13) 0.0262(5) Uani 1 1 d . . . . .
N3 N 0.43998(17) 0.56784(17) 0.35836(12) 0.0241(5) Uani 1 1 d . . . . .
N4 N 0.63645(17) 0.44694(17) 0.37427(12) 0.0224(5) Uani 1 1 d . . . . .
N5 N 0.53064(17) 0.20131(17) 0.17285(12) 0.0221(5) Uani 1 1 d . . . . .
N6 N 0.34576(16) 0.25855(16) 0.21964(12) 0.0202(5) Uani 1 1 d . . . . .
N7 N 0.34500(17) 0.26075(17) 0.35872(12) 0.0223(5) Uani 1 1 d . . . . .
N8 N 0.53201(17) 0.17087(17) 0.42296(12) 0.0218(5) Uani 1 1 d . . . . .
N9 N 0.69602(18) 0.43493(18) 0.22828(13) 0.0251(5) Uani 1 1 d . . . . .
N10 N 0.47511(18) 0.06308(18) 0.32046(13) 0.0258(5) Uani 1 1 d . . . . .
C1 C 0.4044(2) 0.5903(2) 0.11171(16) 0.0296(6) Uani 1 1 d . . . . .
H1 H 0.389234 0.610736 0.064396 0.036 Uiso 1 1 calc R U . . .
C2 C 0.3317(2) 0.6205(2) 0.15615(17) 0.0322(7) Uani 1 1 d . . . . .
C3 C 0.2362(3) 0.6822(3) 0.1392(2) 0.0469(10) Uani 1 1 d . . . . .
H3 H 0.204704 0.706522 0.095510 0.056 Uiso 1 1 calc R U . . .
C4 C 0.1977(3) 0.7003(3) 0.1995(2) 0.0457(9) Uani 1 1 d . . . . .
H4 H 0.134880 0.738508 0.204315 0.055 Uiso 1 1 calc R U . . .
C5 C 0.2714(2) 0.6499(2) 0.25278(17) 0.0298(7) Uani 1 1 d . . . . .
C6 C 0.2615(2) 0.6500(2) 0.32781(18) 0.0322(7) Uani 1 1 d . . . . .
C7 C 0.2250(3) 0.5680(4) 0.3635(3) 0.0611(12) Uani 1 1 d . . . . .
H7AA H 0.163985 0.579985 0.339778 0.073 Uiso 0.670(8) 1 calc R U P A 1
H7AB H 0.270769 0.510507 0.355518 0.073 Uiso 0.670(8) 1 calc R U P A 1
H7BC H 0.181266 0.588867 0.397857 0.073 Uiso 0.330(8) 1 calc R U P A 2
H7BD H 0.186484 0.560594 0.328908 0.073 Uiso 0.330(8) 1 calc R U P A 2
C8 C 0.2104(6) 0.5494(7) 0.4353(3) 0.075(2) Uani 0.670(8) 1 d . U P A 1
H8A H 0.270716 0.533140 0.460536 0.113 Uiso 0.670(8) 1 calc R U P A 1
H8B H 0.186807 0.497972 0.449069 0.113 Uiso 0.670(8) 1 calc R U P A 1
H8C H 0.164006 0.604644 0.444786 0.113 Uiso 0.670(8) 1 calc R U P A 1
C8A C 0.2915(13) 0.4769(13) 0.3964(7) 0.074(3) Uani 0.330(8) 1 d . U P A 2
H8AA H 0.325640 0.447634 0.362137 0.111 Uiso 0.330(8) 1 calc R U P A 2
H8AB H 0.256966 0.438958 0.422897 0.111 Uiso 0.330(8) 1 calc R U P A 2
H8AC H 0.336922 0.482457 0.426416 0.111 Uiso 0.330(8) 1 calc R U P A 2
C9 C 0.1858(3) 0.7457(3) 0.3326(2) 0.0488(10) Uani 1 1 d . . . . .
H9A H 0.123913 0.752274 0.312890 0.059 Uiso 1 1 calc R U . . .
H9B H 0.178054 0.744009 0.380911 0.059 Uiso 1 1 calc R U . . .
C10 C 0.2105(3) 0.8322(3) 0.2966(3) 0.0618(13) Uani 1 1 d . . . . .
H10A H 0.277165 0.820701 0.307689 0.093 Uiso 1 1 calc R U . . .
H10B H 0.169904 0.885378 0.311742 0.093 Uiso 1 1 calc R U . . .
H10C H 0.200109 0.845240 0.247592 0.093 Uiso 1 1 calc R U . . .
C11 C 0.3553(2) 0.6341(2) 0.36557(15) 0.0264(6) Uani 1 1 d . . . . .
C12 C 0.3664(2) 0.6761(2) 0.41703(17) 0.0319(7) Uani 1 1 d . . . . .
H12 H 0.318440 0.723180 0.431437 0.038 Uiso 1 1 calc R U . . .
C13 C 0.4621(2) 0.6339(2) 0.44206(16) 0.0306(7) Uani 1 1 d . . . . .
H13 H 0.490959 0.646830 0.476639 0.037 Uiso 1 1 calc R U . . .
C14 C 0.5068(2) 0.5683(2) 0.40527(15) 0.0264(6) Uani 1 1 d . . . . .
C15 C 0.6025(2) 0.5057(2) 0.41238(15) 0.0265(6) Uani 1 1 d . . . . .
H15 H 0.644125 0.505842 0.445856 0.032 Uiso 1 1 calc R U . . .
C16 C 0.7350(2) 0.3852(2) 0.39339(15) 0.0238(6) Uani 1 1 d . . . . .
C17 C 0.8091(2) 0.4192(2) 0.38859(17) 0.0307(7) Uani 1 1 d . . . . .
H17 H 0.797601 0.482474 0.366662 0.037 Uiso 1 1 calc R U . . .
C18 C 0.9033(2) 0.3591(3) 0.41672(18) 0.0344(7) Uani 1 1 d . . . . .
H18 H 0.953247 0.383107 0.412365 0.041 Uiso 1 1 calc R U . . .
C19 C 0.9218(2) 0.2671(2) 0.44984(17) 0.0313(7) Uani 1 1 d . . . . .
H19 H 0.983538 0.229324 0.469490 0.038 Uiso 1 1 calc R U . . .
C20 C 0.8473(2) 0.2273(2) 0.45491(15) 0.0254(6) Uani 1 1 d . . . . .
C21 C 0.8621(2) 0.1339(2) 0.48952(16) 0.0287(6) Uani 1 1 d . . . . .
H21 H 0.922501 0.095868 0.511400 0.034 Uiso 1 1 calc R U . . .
C22 C 0.7900(2) 0.0950(2) 0.49270(15) 0.0268(6) Uani 1 1 d . . . . .
C23 C 0.8048(2) -0.0008(2) 0.52813(17) 0.0343(7) Uani 1 1 d . . . . .
H23 H 0.864432 -0.039405 0.551107 0.041 Uiso 1 1 calc R U . . .
C24 C 0.7332(3) -0.0365(2) 0.52874(18) 0.0381(8) Uani 1 1 d . . . . .
H24 H 0.744147 -0.099058 0.552363 0.046 Uiso 1 1 calc R U . . .
C25 C 0.6415(2) 0.0206(2) 0.49370(17) 0.0328(7) Uani 1 1 d . . . . .
H25 H 0.593429 -0.005139 0.494334 0.039 Uiso 1 1 calc R U . . .
C26 C 0.6234(2) 0.1132(2) 0.45906(14) 0.0243(6) Uani 1 1 d . . . . .
C27 C 0.6969(2) 0.1537(2) 0.45810(14) 0.0226(6) Uani 1 1 d . . . . .
C28 C 0.6797(2) 0.2487(2) 0.42605(14) 0.0223(6) Uani 1 1 d . . . . .
H28 H 0.618463 0.287308 0.405783 0.027 Uiso 1 1 calc R U . . .
C29 C 0.7522(2) 0.2872(2) 0.42370(14) 0.0222(5) Uani 1 1 d . . . . .
C30 C 0.4573(2) 0.1889(2) 0.46001(15) 0.0264(6) Uani 1 1 d . . . . .
H30 H 0.466572 0.169090 0.507850 0.032 Uiso 1 1 calc R U . . .
C31 C 0.3623(2) 0.2379(2) 0.42964(16) 0.0300(7) Uani 1 1 d . . . . .
C32 C 0.2758(3) 0.2648(3) 0.46143(18) 0.0491(10) Uani 1 1 d . . . . .
H32 H 0.268151 0.257115 0.508456 0.059 Uiso 1 1 calc R U . . .
C33 C 0.2028(2) 0.3056(3) 0.40910(19) 0.0465(10) Uani 1 1 d . . . . .
H33 H 0.136807 0.331181 0.414421 0.056 Uiso 1 1 calc R U . . .
C34 C 0.2470(2) 0.3010(2) 0.34703(16) 0.0271(6) Uani 1 1 d . . . . .
C35 C 0.1959(2) 0.3359(2) 0.27582(15) 0.0245(6) Uani 1 1 d . . . . .
C36 C 0.0921(2) 0.3330(2) 0.28243(17) 0.0312(7) Uani 1 1 d . . . . .
H36A H 0.057313 0.374942 0.309971 0.037 Uiso 1 1 calc R U . . .
H36B H 0.059551 0.357972 0.236776 0.037 Uiso 1 1 calc R U . . .
C37 C 0.0843(3) 0.2364(3) 0.3144(2) 0.0414(8) Uani 1 1 d . . . . .
H37A H 0.117967 0.193966 0.287570 0.062 Uiso 1 1 calc R U . . .
H37B H 0.017400 0.242192 0.314972 0.062 Uiso 1 1 calc R U . . .
H37C H 0.112778 0.212165 0.360724 0.062 Uiso 1 1 calc R U . . .
C38 C 0.1894(2) 0.4398(2) 0.24437(18) 0.0320(7) Uani 1 1 d . . . . .
H38A H 0.152925 0.477328 0.274238 0.038 Uiso 1 1 calc R U . . .
H38B H 0.254303 0.441886 0.244092 0.038 Uiso 1 1 calc R U . . .
C39 C 0.1424(3) 0.4853(3) 0.1714(2) 0.0523(10) Uani 1 1 d . . . . .
H39A H 0.175722 0.447183 0.141638 0.078 Uiso 1 1 calc R U . . .
H39B H 0.146271 0.547120 0.154819 0.078 Uiso 1 1 calc R U . . .
H39C H 0.075736 0.490224 0.171768 0.078 Uiso 1 1 calc R U . . .
C40 C 0.2494(2) 0.2793(2) 0.22720(15) 0.0232(6) Uani 1 1 d . . . . .
C41 C 0.2087(2) 0.2506(2) 0.17867(17) 0.0306(7) Uani 1 1 d . . . . .
H41 H 0.143907 0.257509 0.173518 0.037 Uiso 1 1 calc R U . . .
C42 C 0.2827(2) 0.2101(2) 0.14011(17) 0.0300(7) Uani 1 1 d . . . . .
H42 H 0.277897 0.184481 0.104290 0.036 Uiso 1 1 calc R U . . .
C43 C 0.3664(2) 0.2157(2) 0.16618(15) 0.0238(6) Uani 1 1 d . . . . .
C44 C 0.4605(2) 0.1897(2) 0.14295(15) 0.0238(6) Uani 1 1 d . . . . .
H44 H 0.473113 0.163841 0.105602 0.029 Uiso 1 1 calc R U . . .
C45 C 0.6198(2) 0.1828(2) 0.14015(15) 0.0248(6) Uani 1 1 d . . . . .
C46 C 0.6733(2) 0.0949(2) 0.13360(17) 0.0315(7) Uani 1 1 d . . . . .
H46 H 0.653079 0.044303 0.152850 0.038 Uiso 1 1 calc R U . . .
C47 C 0.7597(2) 0.0806(3) 0.09757(19) 0.0379(8) Uani 1 1 d . . . . .
H47 H 0.795282 0.020535 0.093459 0.046 Uiso 1 1 calc R U . . .
C48 C 0.7908(2) 0.1528(3) 0.06921(17) 0.0358(8) Uani 1 1 d . . . . .
H48 H 0.847790 0.141730 0.046155 0.043 Uiso 1 1 calc R U . . .
C49 C 0.7371(2) 0.2460(2) 0.07421(15) 0.0285(6) Uani 1 1 d . . . . .
C50 C 0.7632(2) 0.3236(3) 0.04189(16) 0.0317(7) Uani 1 1 d . . . . .
H50 H 0.820188 0.313977 0.018858 0.038 Uiso 1 1 calc R U . . .
C51 C 0.7066(2) 0.4152(2) 0.04296(15) 0.0296(7) Uani 1 1 d . . . . .
C52 C 0.7268(3) 0.4963(3) 0.00383(17) 0.0409(8) Uani 1 1 d . . . . .
H52 H 0.781286 0.488743 -0.021894 0.049 Uiso 1 1 calc R U . . .
C53 C 0.6670(3) 0.5841(3) 0.00400(19) 0.0451(9) Uani 1 1 d . . . . .
H53 H 0.678868 0.636236 -0.023857 0.054 Uiso 1 1 calc R U . . .
C54 C 0.5867(3) 0.5978(3) 0.04584(17) 0.0372(8) Uani 1 1 d . . . . .
H54 H 0.547858 0.658826 0.046120 0.045 Uiso 1 1 calc R U . . .
C55 C 0.5652(2) 0.5227(2) 0.08595(15) 0.0269(6) Uani 1 1 d . . . . .
C56 C 0.6222(2) 0.4289(2) 0.08230(14) 0.0252(6) Uani 1 1 d . . . . .
C57 C 0.5956(2) 0.3519(2) 0.11493(14) 0.0235(6) Uani 1 1 d . . . . .
H57 H 0.540357 0.361184 0.139938 0.028 Uiso 1 1 calc R U . . .
C58 C 0.6502(2) 0.2611(2) 0.11087(14) 0.0240(6) Uani 1 1 d . . . . .
C59 C 0.7418(2) 0.4942(2) 0.19736(17) 0.0318(7) Uani 1 1 d . . . . .
H59 H 0.710881 0.558516 0.192227 0.038 Uiso 1 1 calc R U . . .
C60 C 0.8327(2) 0.4633(3) 0.17297(19) 0.0383(8) Uani 1 1 d . . . . .
H60 H 0.862572 0.506133 0.152213 0.046 Uiso 1 1 calc R U . . .
C61 C 0.8788(2) 0.3685(3) 0.17966(18) 0.0367(8) Uani 1 1 d . . . . .
H61 H 0.939783 0.346314 0.162940 0.044 Uiso 1 1 calc R U . . .
C62 C 0.8330(2) 0.3069(2) 0.21161(17) 0.0318(7) Uani 1 1 d . . . . .
H62 H 0.862701 0.242367 0.216967 0.038 Uiso 1 1 calc R U . . .
C63 C 0.7422(2) 0.3423(2) 0.23558(15) 0.0264(6) Uani 1 1 d . . . . .
H63 H 0.711950 0.300413 0.257642 0.032 Uiso 1 1 calc R U . . .
C64 C 0.5538(2) -0.0160(2) 0.33381(18) 0.0342(7) Uani 1 1 d . . . . .
H64 H 0.614381 -0.010820 0.336253 0.041 Uiso 1 1 calc R U . . .
C65 C 0.5486(3) -0.1047(2) 0.34407(19) 0.0385(8) Uani 1 1 d . . . . .
H65 H 0.604936 -0.157600 0.352040 0.046 Uiso 1 1 calc R U . . .
C66 C 0.4600(3) -0.1142(2) 0.34243(18) 0.0392(8) Uani 1 1 d . . . . .
H66 H 0.455005 -0.173216 0.348897 0.047 Uiso 1 1 calc R U . . .
C67 C 0.3790(3) -0.0345(3) 0.3310(2) 0.0419(8) Uani 1 1 d . . . . .
H67 H 0.317764 -0.038833 0.330832 0.050 Uiso 1 1 calc R U . . .
C68 C 0.3888(2) 0.0519(2) 0.31994(18) 0.0340(7) Uani 1 1 d . . . . .
H68 H 0.332963 0.105341 0.311632 0.041 Uiso 1 1 calc R U . . .
O6 O 0.76237(16) -0.00087(17) 0.34212(15) 0.0428(6) Uani 1 1 d D . . . .
O7 O 0.81269(16) 0.10775(16) 0.26787(14) 0.0395(6) Uani 1 1 d D . . . .
C75 C 0.8573(2) -0.0539(2) 0.3226(2) 0.0377(8) Uani 1 1 d D . . . .
C76 C 0.8995(2) 0.0247(2) 0.29223(17) 0.0330(7) Uani 1 1 d D . . . .
C77 C 0.9114(3) -0.1258(3) 0.3888(2) 0.0504(10) Uani 1 1 d D . . . .
H77A H 0.912176 -0.093663 0.423101 0.076 Uiso 1 1 calc R U . . .
H77B H 0.976678 -0.158379 0.379235 0.076 Uiso 1 1 calc R U . . .
H77C H 0.879313 -0.170346 0.405455 0.076 Uiso 1 1 calc R U . . .
C78 C 0.8432(4) -0.1050(3) 0.2724(3) 0.0674(14) Uani 1 1 d D . . . .
H78A H 0.811231 -0.148146 0.294201 0.101 Uiso 1 1 calc R U . . .
H78B H 0.905032 -0.139416 0.258491 0.101 Uiso 1 1 calc R U . . .
H78C H 0.804227 -0.060115 0.232666 0.101 Uiso 1 1 calc R U . . .
C79 C 0.9556(3) 0.0443(3) 0.3442(2) 0.0478(9) Uani 1 1 d D . . . .
H79A H 0.972194 0.098798 0.322629 0.072 Uiso 1 1 calc R U . . .
H79B H 1.013664 -0.009213 0.360548 0.072 Uiso 1 1 calc R U . . .
H79C H 0.916490 0.055726 0.382260 0.072 Uiso 1 1 calc R U . . .
C80 C 0.9599(3) 0.0116(4) 0.2303(2) 0.0576(12) Uani 1 1 d D . . . .
H80A H 0.921116 0.008840 0.194256 0.086 Uiso 1 1 calc R U . . .
H80B H 1.014663 -0.046060 0.243644 0.086 Uiso 1 1 calc R U . . .
H80C H 0.982115 0.063743 0.213868 0.086 Uiso 1 1 calc R U . . .
B2 B 0.7365(2) 0.0914(2) 0.30227(17) 0.0243(6) Uani 1 1 d D . . . .
O4 O 0.4392(3) 0.7897(2) 0.1989(2) 0.0613(12) Uani 0.792(4) 1 d D . P B 1
O5 O 0.5760(3) 0.7448(2) 0.14084(17) 0.0560(11) Uani 0.792(4) 1 d D . P B 1
C69 C 0.4234(5) 0.8630(3) 0.1321(3) 0.0681(17) Uani 0.792(4) 1 d D . P B 1
C70 C 0.5279(5) 0.8476(3) 0.1139(3) 0.0661(16) Uani 0.792(4) 1 d D . P B 1
C71 C 0.3554(7) 0.8495(5) 0.0878(5) 0.114(4) Uani 0.792(4) 1 d D . P B 1
H71A H 0.343857 0.896194 0.044109 0.170 Uiso 0.792(4) 1 calc R U P B 1
H71B H 0.382581 0.787683 0.080633 0.170 Uiso 0.792(4) 1 calc R U P B 1
H71C H 0.295337 0.855801 0.109633 0.170 Uiso 0.792(4) 1 calc R U P B 1
C72 C 0.3730(7) 0.9584(4) 0.1491(4) 0.108(3) Uani 0.792(4) 1 d D . P B 1
H72A H 0.416261 0.968645 0.178047 0.162 Uiso 0.792(4) 1 calc R U P B 1
H72B H 0.356011 1.008481 0.107097 0.162 Uiso 0.792(4) 1 calc R U P B 1
H72C H 0.315514 0.957455 0.172710 0.162 Uiso 0.792(4) 1 calc R U P B 1
C73 C 0.5368(9) 0.8661(5) 0.0333(3) 0.135(5) Uani 0.792(4) 1 d D . P B 1
H73A H 0.506805 0.932325 0.011374 0.203 Uiso 0.792(4) 1 calc R U P B 1
H73B H 0.603910 0.845590 0.023416 0.203 Uiso 0.792(4) 1 calc R U P B 1
H73C H 0.504995 0.831653 0.016033 0.203 Uiso 0.792(4) 1 calc R U P B 1
C74 C 0.5821(7) 0.8958(5) 0.1416(4) 0.097(3) Uani 0.792(4) 1 d D . P B 1
H74A H 0.551078 0.962899 0.124219 0.146 Uiso 0.792(4) 1 calc R U P B 1
H74B H 0.582906 0.878391 0.191041 0.146 Uiso 0.792(4) 1 calc R U P B 1
H74C H 0.647301 0.877324 0.127345 0.146 Uiso 0.792(4) 1 calc R U P B 1
B1 B 0.5224(3) 0.7166(3) 0.1936(2) 0.0327(8) Uiso 0.792(4) 1 d D . P B 1
O4A O 0.5371(11) 0.7899(8) 0.2093(8) 0.080(6) Uiso 0.208(4) 1 d D . P B 2
O5A O 0.4661(9) 0.7470(7) 0.1328(5) 0.047(3) Uiso 0.208(4) 1 d D . P B 2
C69A C 0.461770 0.875220 0.163820 0.125 Uiso 0.2079 1 d D . P B 2
C70A C 0.478010 0.839240 0.099990 0.140 Uiso 0.2079 1 d D . P B 2
C71A C 0.364380 0.892790 0.194650 0.191 Uiso 0.2079 1 d D . P B 2
H71D H 0.317226 0.947486 0.164957 0.286 Uiso 0.208(4) 1 calc R U P B 2
H71E H 0.345373 0.838971 0.199455 0.286 Uiso 0.208(4) 1 calc R U P B 2
H71F H 0.368555 0.903095 0.239161 0.286 Uiso 0.208(4) 1 calc R U P B 2
C72A C 0.496390 0.956230 0.160650 0.067 Uiso 0.2079 1 d D . P B 2
H72D H 0.451120 1.013516 0.132095 0.101 Uiso 0.208(4) 1 calc R U P B 2
H72E H 0.501263 0.962742 0.206320 0.101 Uiso 0.208(4) 1 calc R U P B 2
H72F H 0.558751 0.943826 0.141524 0.101 Uiso 0.208(4) 1 calc R U P B 2
C73A C 0.407070 0.880960 0.037010 0.047 Uiso 0.2079 1 d D . P B 2
H73D H 0.409717 0.941330 0.012280 0.070 Uiso 0.208(4) 1 calc R U P B 2
H73E H 0.424054 0.839417 0.007507 0.070 Uiso 0.208(4) 1 calc R U P B 2
H73F H 0.342682 0.888454 0.051508 0.070 Uiso 0.208(4) 1 calc R U P B 2
C74A C 0.578820 0.839540 0.077640 0.086 Uiso 0.2079 1 d D . P B 2
H74D H 0.575544 0.903317 0.057479 0.129 Uiso 0.208(4) 1 calc R U P B 2
H74E H 0.624015 0.811614 0.117158 0.129 Uiso 0.208(4) 1 calc R U P B 2
H74F H 0.599768 0.803876 0.044344 0.129 Uiso 0.208(4) 1 calc R U P B 2
B1A B 0.5224(3) 0.7166(3) 0.1936(2) 0.0327(8) Uiso 0.208(4) 1 d D . P B 2
C103 C 0.8597(6) 0.9115(6) -0.0197(5) 0.094(5) Uani 0.440(6) 1 d G . P C 1
H103 H 0.840144 0.975530 -0.022478 0.112 Uiso 0.440(6) 1 calc R U P C 1
C102 C 0.8156(5) 0.8553(8) 0.0244(4) 0.105(6) Uani 0.440(6) 1 d G . P C 1
H102 H 0.766433 0.881744 0.051055 0.126 Uiso 0.440(6) 1 calc R U P C 1
C101 C 0.8448(6) 0.7597(7) 0.0286(4) 0.107(6) Uani 0.440(6) 1 d G . P C 1
H101 H 0.815272 0.722066 0.058109 0.129 Uiso 0.440(6) 1 calc R U P C 1
C100 C 0.9182(6) 0.7202(6) -0.0112(5) 0.095(7) Uani 0.440(6) 1 d DG . P C 1
C105 C 0.9624(5) 0.7764(7) -0.0553(4) 0.067(4) Uani 0.440(6) 1 d G . P C 1
H105 H 1.011535 0.749958 -0.081903 0.081 Uiso 0.440(6) 1 calc R U P C 1
C104 C 0.9331(6) 0.8720(7) -0.0595(4) 0.074(5) Uani 0.440(6) 1 d G . P C 1
H104 H 0.962697 0.909636 -0.088958 0.089 Uiso 0.440(6) 1 calc R U P C 1
C106 C 0.9543(15) 0.6154(11) -0.0084(10) 0.117(7) Uani 0.440(6) 1 d D . P C 1
H10D H 1.004937 0.602522 -0.039602 0.175 Uiso 0.440(6) 1 calc R U P C 1
H10E H 0.978889 0.578501 0.037691 0.175 Uiso 0.440(6) 1 calc R U P C 1
H10F H 0.901739 0.599337 -0.021440 0.175 Uiso 0.440(6) 1 calc R U P C 1
C115 C 0.9105(6) 0.8561(11) -0.0576(5) 0.117(8) Uani 0.560(6) 1 d G . P C 2
H115 H 0.883439 0.844693 -0.093790 0.141 Uiso 0.560(6) 1 calc R U P C 2
C114 C 0.9148(6) 0.9449(9) -0.0637(5) 0.123(6) Uani 0.560(6) 1 d G . P C 2
H114 H 0.890647 0.992893 -0.104038 0.148 Uiso 0.560(6) 1 calc R U P C 2
C113 C 0.9553(7) 0.9619(8) -0.0096(8) 0.148(8) Uani 0.560(6) 1 d G . P C 2
H113 H 0.958185 1.021302 -0.013666 0.178 Uiso 0.560(6) 1 calc R U P C 2
C112 C 0.9914(6) 0.8901(12) 0.0507(6) 0.133(7) Uani 0.560(6) 1 d G . P C 2
H112 H 1.018515 0.901514 0.086955 0.159 Uiso 0.560(6) 1 calc R U P C 2
C111 C 0.9871(6) 0.8013(10) 0.0569(4) 0.119(6) Uani 0.560(6) 1 d G . P C 2
H111 H 1.011307 0.753314 0.097204 0.143 Uiso 0.560(6) 1 calc R U P C 2
C110 C 0.9467(7) 0.7843(8) 0.0027(6) 0.131(6) Uani 0.560(6) 1 d DG . P C 2
C116 C 0.9509(15) 0.6867(14) 0.0018(12) 0.174(12) Uani 0.560(6) 1 d D . P C 2
H11A H 0.918767 0.690705 -0.040023 0.261 Uiso 0.560(6) 1 calc R U P C 2
H11B H 1.017315 0.646033 0.004258 0.261 Uiso 0.560(6) 1 calc R U P C 2
H11C H 0.919375 0.661675 0.040729 0.261 Uiso 0.560(6) 1 calc R U P C 2
C120 C 0.8949(4) -0.3717(5) 0.3632(3) 0.057(3) Uani 0.564(10) 1 d DG . P D 1
C121 C 0.9467(3) -0.3721(5) 0.3042(4) 0.056(2) Uani 0.564(10) 1 d G . P D 1
H121 H 1.013923 -0.391745 0.307697 0.067 Uiso 0.564(10) 1 calc R U P D 1
C122 C 0.8980(5) -0.3430(7) 0.2398(3) 0.109(6) Uani 0.564(10) 1 d G . P D 1
H122 H 0.932692 -0.343259 0.200280 0.131 Uiso 0.564(10) 1 calc R U P D 1
C123 C 0.7976(5) -0.3136(7) 0.2345(3) 0.086(3) Uani 0.564(10) 1 d G . P D 1
H123 H 0.764997 -0.294155 0.191460 0.103 Uiso 0.564(10) 1 calc R U P D 1
C124 C 0.7458(3) -0.3132(6) 0.2936(4) 0.060(3) Uani 0.564(10) 1 d G . P D 1
H124 H 0.678531 -0.293536 0.290058 0.072 Uiso 0.564(10) 1 calc R U P D 1
C125 C 0.7944(4) -0.3423(5) 0.3580(3) 0.055(2) Uani 0.564(10) 1 d G . P D 1
H125 H 0.759760 -0.342022 0.397476 0.066 Uiso 0.564(10) 1 calc R U P D 1
C126 C 0.9503(8) -0.4023(7) 0.4302(6) 0.087(4) Uani 0.564(10) 1 d D . P D 1
H12A H 0.906327 -0.398793 0.466639 0.130 Uiso 0.564(10) 1 calc R U P D 1
H12B H 0.994090 -0.466118 0.437477 0.130 Uiso 0.564(10) 1 calc R U P D 1
H12C H 0.986321 -0.361816 0.430116 0.130 Uiso 0.564(10) 1 calc R U P D 1
C130 C 0.8803(9) -0.3543(7) 0.2881(6) 0.086(4) Uani 0.436(10) 1 d G . P D 2
C135 C 0.7814(10) -0.3292(7) 0.2747(5) 0.101(5) Uani 0.436(10) 1 d G . P D 2
H135 H 0.756383 -0.313747 0.229639 0.122 Uiso 0.436(10) 1 calc R U P D 2
C134 C 0.7198(6) -0.3272(8) 0.3287(6) 0.094(5) Uani 0.436(10) 1 d G . P D 2
H134 H 0.653570 -0.310419 0.319694 0.113 Uiso 0.436(10) 1 calc R U P D 2
C133 C 0.7571(7) -0.3503(6) 0.3960(6) 0.083(4) Uani 0.436(10) 1 d G . P D 2
H133 H 0.715853 -0.348948 0.432146 0.100 Uiso 0.436(10) 1 calc R U P D 2
C132 C 0.8560(7) -0.3754(6) 0.4095(6) 0.063(3) Uani 0.436(10) 1 d G . P D 2
H132 H 0.880949 -0.390806 0.454546 0.075 Uiso 0.436(10) 1 calc R U P D 2
C131 C 0.9176(6) -0.3774(7) 0.3555(7) 0.089(5) Uani 0.436(10) 1 d G . P D 2
H131 H 0.983765 -0.394134 0.364492 0.107 Uiso 0.436(10) 1 calc R U P D 2
C136 C 0.909(2) -0.3446(18) 0.2296(14) 0.200(13) Uani 0.436(10) 1 d . . P D 2
H13A H 0.937237 -0.405331 0.220720 0.301 Uiso 0.436(10) 1 calc R U P D 2
H13B H 0.957182 -0.315351 0.225624 0.301 Uiso 0.436(10) 1 calc R U P D 2
H13C H 0.855867 -0.305634 0.196721 0.301 Uiso 0.436(10) 1 calc R U P D 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 O3 2.1386(19) . ?
U1 O1 2.162(2) . ?
U1 N3 2.441(2) . ?
U1 N2 2.449(2) . ?
U1 N4 2.587(2) . ?
U1 N1 2.589(2) . ?
U1 N9 2.611(2) . ?
U2 O3 2.1123(19) . ?
U2 O2 2.1723(19) . ?
U2 N7 2.477(2) . ?
U2 N6 2.506(2) . ?
U2 N8 2.565(2) . ?
U2 N5 2.582(2) . ?
U2 N10 2.664(2) . ?
O1 B1A 1.332(4) . ?
O1 B1 1.332(4) . ?
O2 B2 1.341(4) . ?
N1 C1 1.306(4) . ?
N1 C55 1.421(4) . ?
N2 C5 1.354(4) . ?
N2 C2 1.393(4) . ?
N3 C11 1.351(4) . ?
N3 C14 1.394(4) . ?
N4 C15 1.310(4) . ?
N4 C16 1.436(4) . ?
N5 C44 1.305(4) . ?
N5 C45 1.422(4) . ?
N6 C40 1.356(4) . ?
N6 C43 1.386(4) . ?
N7 C34 1.363(4) . ?
N7 C31 1.388(4) . ?
N8 C30 1.298(4) . ?
N8 C26 1.429(3) . ?
N9 C63 1.342(4) . ?
N9 C59 1.345(4) . ?
N10 C64 1.343(4) . ?
N10 C68 1.347(4) . ?
C1 C2 1.406(5) . ?
C2 C3 1.396(5) . ?
C3 C4 1.378(5) . ?
C4 C5 1.414(5) . ?
C5 C6 1.513(5) . ?
C6 C11 1.515(4) . ?
C6 C9 1.553(5) . ?
C6 C7 1.559(5) . ?
C7 C8A 1.420(19) . ?
C7 C8 1.420(8) . ?
C9 C10 1.519(7) . ?
C11 C12 1.409(4) . ?
C12 C13 1.383(5) . ?
C13 C14 1.393(4) . ?
C14 C15 1.397(4) . ?
C16 C17 1.365(4) . ?
C16 C29 1.430(4) . ?
C17 C18 1.417(4) . ?
C18 C19 1.354(5) . ?
C19 C20 1.430(4) . ?
C20 C21 1.389(4) . ?
C20 C29 1.442(4) . ?
C21 C22 1.391(4) . ?
C22 C23 1.426(4) . ?
C22 C27 1.439(4) . ?
C23 C24 1.356(5) . ?
C24 C25 1.422(4) . ?
C25 C26 1.369(4) . ?
C26 C27 1.434(4) . ?
C27 C28 1.394(4) . ?
C28 C29 1.395(4) . ?
C30 C31 1.412(4) . ?
C31 C32 1.388(5) . ?
C32 C33 1.388(5) . ?
C33 C34 1.395(5) . ?
C34 C35 1.518(4) . ?
C35 C40 1.512(4) . ?
C35 C36 1.547(4) . ?
C35 C38 1.555(4) . ?
C36 C37 1.525(5) . ?
C38 C39 1.525(5) . ?
C40 C41 1.410(4) . ?
C41 C42 1.384(5) . ?
C42 C43 1.399(4) . ?
C43 C44 1.405(4) . ?
C45 C46 1.368(4) . ?
C45 C58 1.429(4) . ?
C46 C47 1.420(5) . ?
C47 C48 1.349(5) . ?
C48 C49 1.430(5) . ?
C49 C50 1.393(5) . ?
C49 C58 1.434(4) . ?
C50 C51 1.394(5) . ?
C51 C52 1.430(5) . ?
C51 C56 1.434(4) . ?
C52 C53 1.353(6) . ?
C53 C54 1.416(5) . ?
C54 C55 1.371(4) . ?
C55 C56 1.439(4) . ?
C56 C57 1.391(4) . ?
C57 C58 1.394(4) . ?
C59 C60 1.379(5) . ?
C60 C61 1.376(5) . ?
C61 C62 1.378(5) . ?
C62 C63 1.383(4) . ?
C64 C65 1.381(5) . ?
C65 C66 1.369(5) . ?
C66 C67 1.369(5) . ?
C67 C68 1.371(5) . ?
O6 B2 1.382(4) . ?
O6 C75 1.459(4) . ?
O7 B2 1.363(4) . ?
O7 C76 1.458(4) . ?
C75 C78 1.508(5) . ?
C75 C77 1.529(5) . ?
C75 C76 1.546(5) . ?
C76 C79 1.512(5) . ?
C76 C80 1.523(5) . ?
O4 B1 1.382(5) . ?
O4 C69 1.484(6) . ?
O5 B1 1.373(5) . ?
O5 C70 1.473(6) . ?
C69 C71 1.472(8) . ?
C69 C70 1.522(8) . ?
C69 C72 1.546(8) . ?
C70 C74 1.484(8) . ?
C70 C73 1.581(7) . ?
O4A B1A 1.357(12) . ?
O4A C69A 1.503(12) . ?
O5A B1A 1.381(10) . ?
O5A C70A 1.492(10) . ?
C69A C71A 1.5083 . ?
C69A C72A 1.5132 . ?
C69A C70A 1.5155 . ?
C70A C73A 1.5216 . ?
C70A C74A 1.5394 . ?
C103 C102 1.3900 . ?
C103 C104 1.3900 . ?
C102 C101 1.3900 . ?
C101 C100 1.3900 . ?
C100 C105 1.3900 . ?
C100 C106 1.528(15) . ?
C105 C104 1.3900 . ?
C115 C114 1.3900 . ?
C115 C110 1.3900 . ?
C114 C113 1.3900 . ?
C113 C112 1.3900 . ?
C112 C111 1.3900 . ?
C111 C110 1.3900 . ?
C110 C116 1.516(16) . ?
C120 C121 1.3900 . ?
C120 C125 1.3900 . ?
C120 C126 1.478(10) . ?
C121 C122 1.3900 . ?
C122 C123 1.3900 . ?
C123 C124 1.3900 . ?
C124 C125 1.3900 . ?
C130 C136 1.23(3) . ?
C130 C135 1.3900 . ?
C130 C131 1.3900 . ?
C135 C134 1.3900 . ?
C134 C133 1.3900 . ?
C133 C132 1.3900 . ?
C132 C131 1.3900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 U1 O1 169.05(8) . . ?
O3 U1 N3 107.90(8) . . ?
O1 U1 N3 83.00(8) . . ?
O3 U1 N2 97.13(8) . . ?
O1 U1 N2 85.35(8) . . ?
N3 U1 N2 70.93(8) . . ?
O3 U1 N4 95.89(7) . . ?
O1 U1 N4 88.99(8) . . ?
N3 U1 N4 68.52(8) . . ?
N2 U1 N4 139.44(8) . . ?
O3 U1 N1 90.19(7) . . ?
O1 U1 N1 80.77(8) . . ?
N3 U1 N1 137.13(8) . . ?
N2 U1 N1 68.42(8) . . ?
N4 U1 N1 149.67(8) . . ?
O3 U1 N9 92.31(8) . . ?
O1 U1 N9 79.78(8) . . ?
N3 U1 N9 137.37(8) . . ?
N2 U1 N9 144.69(8) . . ?
N4 U1 N9 72.46(8) . . ?
N1 U1 N9 77.64(8) . . ?
O3 U2 O2 96.51(7) . . ?
O3 U2 N7 95.30(8) . . ?
O2 U2 N7 144.53(8) . . ?
O3 U2 N6 106.28(7) . . ?
O2 U2 N6 137.90(8) . . ?
N7 U2 N6 68.65(8) . . ?
O3 U2 N8 96.73(7) . . ?
O2 U2 N8 77.87(7) . . ?
N7 U2 N8 67.59(8) . . ?
N6 U2 N8 131.87(7) . . ?
O3 U2 N5 104.19(7) . . ?
O2 U2 N5 74.40(7) . . ?
N7 U2 N5 134.01(7) . . ?
N6 U2 N5 66.02(7) . . ?
N8 U2 N5 146.78(8) . . ?
O3 U2 N10 173.80(8) . . ?
O2 U2 N10 85.41(8) . . ?
N7 U2 N10 79.87(8) . . ?
N6 U2 N10 75.72(7) . . ?
N8 U2 N10 77.87(8) . . ?
N5 U2 N10 82.00(8) . . ?
B1A O1 U1 145.7(2) . . ?
B1 O1 U1 145.7(2) . . ?
B2 O2 U2 166.9(2) . . ?
U2 O3 U1 176.15(10) . . ?
C1 N1 C55 118.1(3) . . ?
C1 N1 U1 112.7(2) . . ?
C55 N1 U1 126.60(18) . . ?
C5 N2 C2 106.6(3) . . ?
C5 N2 U1 138.2(2) . . ?
C2 N2 U1 114.9(2) . . ?
C11 N3 C14 105.7(2) . . ?
C11 N3 U1 137.2(2) . . ?
C14 N3 U1 111.67(18) . . ?
C15 N4 C16 113.8(2) . . ?
C15 N4 U1 109.09(18) . . ?
C16 N4 U1 135.31(18) . . ?
C44 N5 C45 116.1(2) . . ?
C44 N5 U2 113.88(19) . . ?
C45 N5 U2 129.37(17) . . ?
C40 N6 C43 105.7(2) . . ?
C40 N6 U2 137.19(19) . . ?
C43 N6 U2 113.84(17) . . ?
C34 N7 C31 105.8(2) . . ?
C34 N7 U2 139.1(2) . . ?
C31 N7 U2 114.85(18) . . ?
C30 N8 C26 116.8(2) . . ?
C30 N8 U2 114.61(18) . . ?
C26 N8 U2 128.31(18) . . ?
C63 N9 C59 117.8(3) . . ?
C63 N9 U1 121.42(19) . . ?
C59 N9 U1 120.7(2) . . ?
C64 N10 C68 116.5(3) . . ?
C64 N10 U2 120.9(2) . . ?
C68 N10 U2 122.6(2) . . ?
N1 C1 C2 122.4(3) . . ?
N2 C2 C3 109.6(3) . . ?
N2 C2 C1 121.3(3) . . ?
C3 C2 C1 128.6(3) . . ?
C4 C3 C2 106.9(3) . . ?
C3 C4 C5 107.2(3) . . ?
N2 C5 C4 109.7(3) . . ?
N2 C5 C6 124.9(3) . . ?
C4 C5 C6 125.4(3) . . ?
C5 C6 C11 114.1(3) . . ?
C5 C6 C9 109.2(3) . . ?
C11 C6 C9 108.8(3) . . ?
C5 C6 C7 106.7(3) . . ?
C11 C6 C7 108.2(3) . . ?
C9 C6 C7 109.8(3) . . ?
C8A C7 C6 120.7(6) . . ?
C8 C7 C6 119.7(5) . . ?
C10 C9 C6 115.1(3) . . ?
N3 C11 C12 110.6(3) . . ?
N3 C11 C6 122.4(3) . . ?
C12 C11 C6 126.7(3) . . ?
C13 C12 C11 106.9(3) . . ?
C12 C13 C14 106.5(3) . . ?
C13 C14 N3 110.3(3) . . ?
C13 C14 C15 128.9(3) . . ?
N3 C14 C15 120.8(3) . . ?
N4 C15 C14 123.3(3) . . ?
C17 C16 C29 120.5(3) . . ?
C17 C16 N4 121.6(3) . . ?
C29 C16 N4 117.7(2) . . ?
C16 C17 C18 120.6(3) . . ?
C19 C18 C17 121.0(3) . . ?
C18 C19 C20 120.7(3) . . ?
C21 C20 C19 122.8(3) . . ?
C21 C20 C29 118.6(3) . . ?
C19 C20 C29 118.6(3) . . ?
C20 C21 C22 122.5(3) . . ?
C21 C22 C23 122.7(3) . . ?
C21 C22 C27 118.6(3) . . ?
C23 C22 C27 118.7(3) . . ?
C24 C23 C22 120.8(3) . . ?
C23 C24 C25 120.8(3) . . ?
C26 C25 C24 120.7(3) . . ?
C25 C26 N8 121.2(3) . . ?
C25 C26 C27 120.1(3) . . ?
N8 C26 C27 118.8(3) . . ?
C28 C27 C26 121.7(3) . . ?
C28 C27 C22 119.4(3) . . ?
C26 C27 C22 118.9(3) . . ?
C27 C28 C29 121.5(3) . . ?
C28 C29 C16 122.3(3) . . ?
C28 C29 C20 119.3(3) . . ?
C16 C29 C20 118.4(3) . . ?
N8 C30 C31 121.8(3) . . ?
N7 C31 C32 110.4(3) . . ?
N7 C31 C30 120.6(3) . . ?
C32 C31 C30 129.0(3) . . ?
C33 C32 C31 106.4(3) . . ?
C32 C33 C34 107.3(3) . . ?
N7 C34 C33 110.2(3) . . ?
N7 C34 C35 123.6(3) . . ?
C33 C34 C35 126.2(3) . . ?
C40 C35 C34 112.7(2) . . ?
C40 C35 C36 109.9(2) . . ?
C34 C35 C36 109.3(2) . . ?
C40 C35 C38 107.7(2) . . ?
C34 C35 C38 108.2(2) . . ?
C36 C35 C38 108.9(2) . . ?
C37 C36 C35 116.2(3) . . ?
C39 C38 C35 115.2(3) . . ?
N6 C40 C41 110.2(3) . . ?
N6 C40 C35 122.3(2) . . ?
C41 C40 C35 127.1(3) . . ?
C42 C41 C40 107.4(3) . . ?
C41 C42 C43 105.7(3) . . ?
N6 C43 C42 110.9(3) . . ?
N6 C43 C44 119.9(2) . . ?
C42 C43 C44 129.1(3) . . ?
N5 C44 C43 121.2(3) . . ?
C46 C45 N5 122.3(3) . . ?
C46 C45 C58 120.4(3) . . ?
N5 C45 C58 117.2(3) . . ?
C45 C46 C47 120.4(3) . . ?
C48 C47 C46 121.0(3) . . ?
C47 C48 C49 120.8(3) . . ?
C50 C49 C48 122.6(3) . . ?
C50 C49 C58 118.7(3) . . ?
C48 C49 C58 118.6(3) . . ?
C49 C50 C51 122.2(3) . . ?
C50 C51 C52 122.7(3) . . ?
C50 C51 C56 118.6(3) . . ?
C52 C51 C56 118.7(3) . . ?
C53 C52 C51 120.4(3) . . ?
C52 C53 C54 121.1(3) . . ?
C55 C54 C53 121.0(3) . . ?
C54 C55 N1 121.7(3) . . ?
C54 C55 C56 119.2(3) . . ?
N1 C55 C56 119.0(3) . . ?
C57 C56 C51 119.6(3) . . ?
C57 C56 C55 121.2(3) . . ?
C51 C56 C55 119.1(3) . . ?
C56 C57 C58 121.3(3) . . ?
C57 C58 C45 121.6(3) . . ?
C57 C58 C49 119.5(3) . . ?
C45 C58 C49 118.8(3) . . ?
N9 C59 C60 122.5(3) . . ?
C61 C60 C59 119.3(3) . . ?
C60 C61 C62 118.8(3) . . ?
C61 C62 C63 119.0(3) . . ?
N9 C63 C62 122.6(3) . . ?
N10 C64 C65 122.8(3) . . ?
C66 C65 C64 119.6(3) . . ?
C67 C66 C65 118.3(3) . . ?
C66 C67 C68 119.5(3) . . ?
N10 C68 C67 123.3(3) . . ?
B2 O6 C75 107.8(3) . . ?
B2 O7 C76 108.5(2) . . ?
O6 C75 C78 108.5(3) . . ?
O6 C75 C77 106.5(3) . . ?
C78 C75 C77 109.5(3) . . ?
O6 C75 C76 102.1(2) . . ?
C78 C75 C76 115.0(4) . . ?
C77 C75 C76 114.5(3) . . ?
O7 C76 C79 107.9(3) . . ?
O7 C76 C80 107.4(3) . . ?
C79 C76 C80 109.2(3) . . ?
O7 C76 C75 102.5(2) . . ?
C79 C76 C75 114.6(3) . . ?
C80 C76 C75 114.6(3) . . ?
O2 B2 O7 125.2(3) . . ?
O2 B2 O6 123.4(3) . . ?
O7 B2 O6 111.4(3) . . ?
B1 O4 C69 106.0(4) . . ?
B1 O5 C70 106.0(4) . . ?
C71 C69 O4 107.8(5) . . ?
C71 C69 C70 121.1(7) . . ?
O4 C69 C70 100.0(4) . . ?
C71 C69 C72 108.1(6) . . ?
O4 C69 C72 105.7(5) . . ?
C70 C69 C72 112.6(6) . . ?
O5 C70 C74 109.0(5) . . ?
O5 C70 C69 103.0(4) . . ?
C74 C70 C69 119.1(6) . . ?
O5 C70 C73 104.0(5) . . ?
C74 C70 C73 109.8(6) . . ?
C69 C70 C73 110.7(6) . . ?
O1 B1 O5 122.1(3) . . ?
O1 B1 O4 125.9(3) . . ?
O5 B1 O4 111.9(3) . . ?
B1A O4A C69A 103.6(8) . . ?
B1A O5A C70A 101.9(7) . . ?
O4A C69A C71A 110.6(7) . . ?
O4A C69A C72A 105.1(5) . . ?
C71A C69A C72A 110.3 . . ?
O4A C69A C70A 95.3(6) . . ?
C71A C69A C70A 118.9 . . ?
C72A C69A C70A 114.7 . . ?
O5A C70A C69A 96.3(4) . . ?
O5A C70A C73A 103.5(4) . . ?
C69A C70A C73A 123.6 . . ?
O5A C70A C74A 118.7(5) . . ?
C69A C70A C74A 105.7 . . ?
C73A C70A C74A 109.4 . . ?
O1 B1A O4A 124.6(6) . . ?
O1 B1A O5A 124.2(5) . . ?
O4A B1A O5A 110.9(7) . . ?
C102 C103 C104 120.0 . . ?
C101 C102 C103 120.0 . . ?
C100 C101 C102 120.0 . . ?
C101 C100 C105 120.0 . . ?
C101 C100 C106 122.5(10) . . ?
C105 C100 C106 117.5(10) . . ?
C100 C105 C104 120.0 . . ?
C105 C104 C103 120.0 . . ?
C114 C115 C110 120.0 . . ?
C115 C114 C113 120.0 . . ?
C112 C113 C114 120.0 . . ?
C111 C112 C113 120.0 . . ?
C112 C111 C110 120.0 . . ?
C111 C110 C115 120.0 . . ?
C111 C110 C116 123.0(12) . . ?
C115 C110 C116 116.6(13) . . ?
C121 C120 C125 120.0 . . ?
C121 C120 C126 117.7(6) . . ?
C125 C120 C126 122.3(6) . . ?
C120 C121 C122 120.0 . . ?
C123 C122 C121 120.0 . . ?
C124 C123 C122 120.0 . . ?
C123 C124 C125 120.0 . . ?
C124 C125 C120 120.0 . . ?
C136 C130 C135 101.4(19) . . ?
C136 C130 C131 138.5(19) . . ?
C135 C130 C131 120.0 . . ?
C130 C135 C134 120.0 . . ?
C133 C134 C135 120.0 . . ?
C134 C133 C132 120.0 . . ?
C131 C132 C133 120.0 . . ?
C132 C131 C130 120.0 . . ?

_refine_diff_density_max         2.234
_refine_diff_density_min         -1.517
_refine_diff_density_rms         0.096

# start Validation Reply Form
_vrf_PLAT201_2_2toluene          
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) .......          1 Report
RESPONSE: The OBpin ligand was positionally disordered over two positions, 
so was split into two parts and refined in a 0.79:0.21 ratio. Attempts
to refine the minor component anisotropically resulted in unstable
refinement, therefore it was left as isotropic. 
;
_vrf_PLAT220_2_2toluene          
;
PROBLEM: Non-Solvent Resd 1  C   Ueq(max)/Ueq(min) Range         8.6 Ratio 
RESPONSE: The OBpin ligand was positionally disordered over two positions, 
so was split into two parts and refined in a 0.79:0.21 ratio. We have 
modelled both components to the best of our ability. 
;
_vrf_PLAT250_2_2toluene          
;
PROBLEM: Large U3/U1 Ratio for Average U(i,j) Tensor ....        4.1 Note  
RESPONSE: This problem has likely arised from the large U(i,j) values for
the lattice toluene molecules. It has been noted, but is not serious.
;
####################################################################### 
# 
# 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_3_THF
_database_code_depnum_ccdc_archive 'CCDC 1812762'
_audit_update_record             
;
2017-12-20 deposited with the CCDC.
2018-03-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        '[{(py){cat(py)BO)UOUOBcat(py)}(LA)]'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C85 H71 B2 N11 O7 U2, C4 H8 O'
_chemical_formula_sum            'C89 H79 B2 N11 O8 U2'
_chemical_formula_weight         1928.36

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 0.0020 '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'
B B 0.0010 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -9.6770 9.6650 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   14.8167(3)
_cell_length_b                   15.0681(3)
_cell_length_c                   18.9308(4)
_cell_angle_alpha                68.5930(10)
_cell_angle_beta                 79.0720(10)
_cell_angle_gamma                86.2280(10)
_cell_volume                     3863.52(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9840
_cell_measurement_theta_min      3.01
_cell_measurement_theta_max      28.02

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.658
_exptl_crystal_F_000             1896
_exptl_transmission_factor_min   0.3817
_exptl_transmission_factor_max   0.4311
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.160
_exptl_absorpt_coefficient_mu    4.253
_shelx_estimated_absorpt_T_min   0.469
_shelx_estimated_absorpt_T_max   0.549
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3817
_exptl_absorpt_correction_T_max  0.4311
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_special_details           
;
 The following wavelength and cell were deduced by SADABS from the
 direction cosines etc. They are given here for emergency use only:
 CELL 0.71093   14.844   15.094   18.962   68.604   79.102   86.214
;
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radition_source          'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            88345
_diffrn_reflns_av_unetI/netI     0.0459
_diffrn_reflns_av_R_equivalents  0.0501
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.993
_diffrn_reflns_theta_max         28.345
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             18474
_reflns_number_gt                14137
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
The thermal parameters of C(92) of the lattice THF molecule was attempted to 
be split into two parts and treated for positional disorder, however this 
resulted in unstable refinement of the THF molecule. As a result, the thermal 
parameters of the THF carbon atoms were restrained to be similar to one another 
using the SIMU command. 
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0259P)²+4.7880P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         18474
_refine_ls_number_parameters     1009
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0519
_refine_ls_R_factor_gt           0.0298
_refine_ls_wR_factor_ref         0.0649
_refine_ls_wR_factor_gt          0.0586
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_restrained_S_all      1.014
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
N8 N 0.3478(2) 0.1650(2) 0.31082(17) 0.0202(7) Uani 1 1 d . . . . .
C26 C 0.3690(3) 0.2027(3) 0.3637(2) 0.0210(8) Uani 1 1 d . . . . .
C32 C 0.4260(3) -0.0306(3) 0.2397(3) 0.0362(11) Uani 1 1 d . . . . .
H32 H 0.459872 -0.077555 0.273299 0.043 Uiso 1 1 calc R U . . .
C33 C 0.4113(3) -0.0268(3) 0.1688(3) 0.0377(11) Uani 1 1 d . . . . .
H33 H 0.433834 -0.070531 0.144004 0.045 Uiso 1 1 calc R U . . .
C23 C 0.4143(3) 0.3028(3) 0.4524(2) 0.0319(10) Uani 1 1 d . . . . .
H23 H 0.430909 0.338512 0.480265 0.038 Uiso 1 1 calc R U . . .
C83 C 0.3437(3) 0.7160(4) 0.3028(3) 0.0502(13) Uani 1 1 d . . . . .
H83 H 0.321885 0.769708 0.315823 0.060 Uiso 1 1 calc R U . . .
C67 C 0.6251(3) 0.2083(4) 0.1141(3) 0.0444(12) Uani 1 1 d . . . . .
H67 H 0.658101 0.164443 0.093367 0.053 Uiso 1 1 calc R U . . .
C82 C 0.2814(3) 0.6527(4) 0.3016(3) 0.0532(14) Uani 1 1 d . . . . .
H82 H 0.217066 0.661783 0.313583 0.064 Uiso 1 1 calc R U . . .
C65 C 0.6221(3) 0.3242(3) 0.1676(3) 0.0415(11) Uani 1 1 d . . . . .
H65 H 0.652966 0.364400 0.184122 0.050 Uiso 1 1 calc R U . . .
C68 C 0.5310(3) 0.2134(3) 0.1207(2) 0.0325(10) Uani 1 1 d . . . . .
H68 H 0.500648 0.174998 0.102201 0.039 Uiso 1 1 calc R U . . .
C9 C -0.0455(4) -0.1288(3) 0.2712(3) 0.0464(13) Uani 1 1 d . . . . .
H9A H -0.041259 -0.176032 0.322993 0.056 Uiso 1 1 calc R U . . .
H9B H -0.111452 -0.120870 0.267297 0.056 Uiso 1 1 calc R U . . .
C66 C 0.6708(3) 0.2643(4) 0.1365(3) 0.0444(12) Uani 1 1 d . . . . .
H66 H 0.735969 0.261969 0.130675 0.053 Uiso 1 1 calc R U . . .
C10 C 0.0028(5) -0.1699(3) 0.2109(3) 0.0668(18) Uani 1 1 d . . . . .
H10A H -0.026103 -0.230700 0.219884 0.100 Uiso 1 1 calc R U . . .
H10B H -0.002555 -0.125060 0.159223 0.100 Uiso 1 1 calc R U . . .
H10C H 0.067839 -0.180379 0.215077 0.100 Uiso 1 1 calc R U . . .
O10 O 0.3735(2) 0.1608(3) 0.7138(2) 0.0525(9) Uani 1 1 d . . . . .
C90 C 0.3302(5) 0.2333(6) 0.6618(4) 0.0933(13) Uani 1 1 d . U . . .
H90A H 0.295354 0.205608 0.635039 0.112 Uiso 1 1 calc R U . . .
H90B H 0.377018 0.277478 0.622516 0.112 Uiso 1 1 calc R U . . .
C91 C 0.2690(5) 0.2848(6) 0.7010(4) 0.0949(13) Uani 1 1 d . U . . .
H91A H 0.205681 0.283687 0.691453 0.114 Uiso 1 1 calc R U . . .
H91B H 0.289118 0.351982 0.683388 0.114 Uiso 1 1 calc R U . . .
C92 C 0.2727(6) 0.2363(6) 0.7819(4) 0.0951(13) Uani 1 1 d . U . . .
H92A H 0.210089 0.217636 0.811864 0.114 Uiso 1 1 calc R U . . .
H92B H 0.299635 0.278730 0.801926 0.114 Uiso 1 1 calc R U . . .
C93 C 0.3301(5) 0.1514(6) 0.7886(4) 0.0939(13) Uani 1 1 d . U . . .
H93A H 0.376343 0.147308 0.821231 0.113 Uiso 1 1 calc R U . . .
H93B H 0.291723 0.093037 0.812312 0.113 Uiso 1 1 calc R U . . .
C76 C -0.3697(3) 0.0123(4) 0.4444(3) 0.0472(13) Uani 1 1 d . . . . .
H76 H -0.405860 -0.019593 0.493577 0.057 Uiso 1 1 calc R U . . .
C71 C -0.2887(3) 0.3495(4) 0.4880(3) 0.0461(12) Uani 1 1 d . . . . .
H71 H -0.262614 0.319834 0.533108 0.055 Uiso 1 1 calc R U . . .
C77 C -0.3651(3) -0.0216(4) 0.3858(3) 0.0521(14) Uani 1 1 d . . . . .
H77 H -0.399767 -0.076124 0.393209 0.063 Uiso 1 1 calc R U . . .
C72 C -0.3494(4) 0.4269(4) 0.4807(4) 0.0613(16) Uani 1 1 d . . . . .
H72 H -0.364174 0.450089 0.521845 0.074 Uiso 1 1 calc R U . . .
U2 U 0.29811(2) 0.26661(2) 0.18202(2) 0.01625(4) Uani 1 1 d . . . . .
U1 U 0.01045(2) 0.23185(2) 0.26196(2) 0.01596(4) Uani 1 1 d . . . . .
B1 B -0.2162(3) 0.2399(3) 0.3437(3) 0.0259(10) Uani 1 1 d . . . . .
C27 C 0.2964(3) 0.2459(3) 0.4026(2) 0.0205(8) Uani 1 1 d . . . . .
N4 N 0.0174(2) 0.2023(2) 0.40457(17) 0.0186(6) Uani 1 1 d . . . . .
N2 N -0.0205(2) 0.1413(2) 0.18320(17) 0.0216(7) Uani 1 1 d . . . . .
N6 N 0.3377(2) 0.2616(2) 0.05021(17) 0.0184(6) Uani 1 1 d . . . . .
O3 O 0.15792(16) 0.24732(18) 0.22002(14) 0.0203(5) Uani 1 1 d . . . . .
O1 O -0.13170(17) 0.24129(18) 0.29540(14) 0.0222(6) Uani 1 1 d . . . . .
N10 N 0.4803(2) 0.2716(2) 0.15280(18) 0.0238(7) Uani 1 1 d . . . . .
O2 O 0.32093(18) 0.37505(17) 0.23069(15) 0.0239(6) Uani 1 1 d . . . . .
O5 O -0.21292(18) 0.2456(2) 0.42013(16) 0.0310(7) Uani 1 1 d . . . . .
O6 O 0.42458(18) 0.48407(19) 0.24385(16) 0.0283(6) Uani 1 1 d . . . . .
N1 N -0.0255(2) 0.3425(2) 0.12880(17) 0.0200(7) Uani 1 1 d . . . . .
C25 C 0.4576(3) 0.2062(3) 0.3746(2) 0.0270(9) Uani 1 1 d . . . . .
H25 H 0.504911 0.175194 0.350798 0.032 Uiso 1 1 calc R U . . .
O4 O -0.27993(18) 0.31830(19) 0.30860(17) 0.0302(7) Uani 1 1 d . . . . .
C1 C -0.0617(2) 0.2952(3) 0.0951(2) 0.0223(8) Uani 1 1 d . . . . .
H1 H -0.090964 0.329761 0.052627 0.027 Uiso 1 1 calc R U . . .
C69 C -0.3080(3) 0.3627(3) 0.3601(3) 0.0345(10) Uani 1 1 d . . . . .
N5 N 0.3044(2) 0.4313(2) 0.07164(17) 0.0190(6) Uani 1 1 d . . . . .
N9 N -0.0025(2) 0.3982(2) 0.27774(17) 0.0193(7) Uani 1 1 d . . . . .
C28 C 0.2051(2) 0.2363(2) 0.4003(2) 0.0191(8) Uani 1 1 d . . . . .
H28 H 0.189728 0.199587 0.372774 0.023 Uiso 1 1 calc R U . . .
C16 C 0.0390(2) 0.2640(3) 0.4406(2) 0.0193(8) Uani 1 1 d . . . . .
C44 C 0.3557(3) 0.4317(3) 0.0078(2) 0.0227(8) Uani 1 1 d . . . . .
H44 H 0.379056 0.490369 -0.030438 0.027 Uiso 1 1 calc R U . . .
C60 C -0.1002(3) 0.5169(3) 0.3085(2) 0.0321(10) Uani 1 1 d . . . . .
H60 H -0.160590 0.540740 0.317471 0.038 Uiso 1 1 calc R U . . .
C29 C 0.1345(2) 0.2790(3) 0.4374(2) 0.0192(8) Uani 1 1 d . . . . .
N11 N -0.2677(2) 0.1394(2) 0.3617(2) 0.0288(8) Uani 1 1 d . . . . .
C59 C -0.0858(3) 0.4372(3) 0.2892(2) 0.0258(9) Uani 1 1 d . . . . .
H59 H -0.137468 0.407760 0.283641 0.031 Uiso 1 1 calc R U . . .
N3 N -0.0156(2) 0.0653(2) 0.34650(17) 0.0197(6) Uani 1 1 d . . . . .
C51 C -0.0019(3) 0.5991(3) 0.1035(2) 0.0238(8) Uani 1 1 d . . . . .
C58 C 0.1841(2) 0.5436(2) 0.0903(2) 0.0185(7) Uani 1 1 d . . . . .
C14 C -0.0580(2) 0.0611(3) 0.4195(2) 0.0193(8) Uani 1 1 d . . . . .
B2 B 0.3367(3) 0.4486(3) 0.2484(3) 0.0245(10) Uani 1 1 d . . . . .
C49 C 0.1585(3) 0.6346(3) 0.0958(2) 0.0214(8) Uani 1 1 d . . . . .
C20 C 0.1591(3) 0.3388(3) 0.4760(2) 0.0240(8) Uani 1 1 d . . . . .
C24 C 0.4801(3) 0.2550(3) 0.4204(2) 0.0338(10) Uani 1 1 d . . . . .
H24 H 0.541452 0.254232 0.428650 0.041 Uiso 1 1 calc R U . . .
C21 C 0.2514(3) 0.3468(3) 0.4787(2) 0.0282(9) Uani 1 1 d . . . . .
H21 H 0.267550 0.385187 0.504633 0.034 Uiso 1 1 calc R U . . .
C43 C 0.3769(3) 0.3457(3) -0.0053(2) 0.0213(8) Uani 1 1 d . . . . .
C40 C 0.3626(2) 0.1927(3) 0.0199(2) 0.0210(8) Uani 1 1 d . . . . .
C15 C -0.0363(2) 0.1298(3) 0.4481(2) 0.0203(8) Uani 1 1 d . . . . .
H15 H -0.061064 0.123452 0.499807 0.024 Uiso 1 1 calc R U . . .
N7 N 0.3387(2) 0.1008(2) 0.19044(18) 0.0205(7) Uani 1 1 d . . . . .
C42 C 0.4271(3) 0.3286(3) -0.0688(2) 0.0280(9) Uani 1 1 d . . . . .
H42 H 0.460259 0.374016 -0.114163 0.034 Uiso 1 1 calc R U . . .
C61 C -0.0264(3) 0.5615(3) 0.3145(2) 0.0350(10) Uani 1 1 d . . . . .
H61 H -0.034522 0.617396 0.327089 0.042 Uiso 1 1 calc R U . . .
C54 C -0.1371(3) 0.4709(3) 0.1131(2) 0.0282(9) Uani 1 1 d . . . . .
H54 H -0.183740 0.427834 0.117592 0.034 Uiso 1 1 calc R U . . .
C7 C 0.0982(3) -0.0341(3) 0.2555(2) 0.0407(12) Uani 1 1 d . . . . .
H7A H 0.123915 -0.049786 0.209275 0.049 Uiso 1 1 calc R U . . .
H7B H 0.119797 0.030774 0.245971 0.049 Uiso 1 1 calc R U . . .
C19 C 0.0872(3) 0.3836(3) 0.5123(2) 0.0296(9) Uani 1 1 d . . . . .
H19 H 0.102210 0.425157 0.536003 0.035 Uiso 1 1 calc R U . . .
C62 C 0.0600(3) 0.5244(3) 0.3021(2) 0.0309(9) Uani 1 1 d . . . . .
H62 H 0.112361 0.554510 0.305771 0.037 Uiso 1 1 calc R U . . .
C37 C 0.3132(4) -0.0679(3) 0.0420(3) 0.0486(13) Uani 1 1 d . . . . .
H37A H 0.340116 -0.101568 0.007519 0.073 Uiso 1 1 calc R U . . .
H37B H 0.322995 -0.105087 0.094548 0.073 Uiso 1 1 calc R U . . .
H37C H 0.247098 -0.059679 0.041653 0.073 Uiso 1 1 calc R U . . .
C8 C 0.1367(4) -0.1042(4) 0.3240(3) 0.0595(16) Uani 1 1 d . . . . .
H8A H 0.203936 -0.100269 0.312913 0.089 Uiso 1 1 calc R U . . .
H8B H 0.113331 -0.088301 0.369943 0.089 Uiso 1 1 calc R U . . .
H8C H 0.117459 -0.169042 0.333165 0.089 Uiso 1 1 calc R U . . .
C53 C -0.1610(3) 0.5656(3) 0.1073(2) 0.0328(10) Uani 1 1 d . . . . .
H53 H -0.222667 0.586440 0.105093 0.039 Uiso 1 1 calc R U . . .
C55 C -0.0480(3) 0.4404(3) 0.1123(2) 0.0213(8) Uani 1 1 d . . . . .
C41 C 0.4190(3) 0.2313(3) -0.0524(2) 0.0267(9) Uani 1 1 d . . . . .
H41 H 0.446733 0.197288 -0.084435 0.032 Uiso 1 1 calc R U . . .
C78 C -0.3096(4) 0.0245(4) 0.3157(3) 0.0523(14) Uani 1 1 d . . . . .
H78 H -0.304835 0.000913 0.274977 0.063 Uiso 1 1 calc R U . . .
C52 C -0.0958(3) 0.6268(3) 0.1049(2) 0.0305(9) Uani 1 1 d . . . . .
H52 H -0.113261 0.688906 0.104194 0.037 Uiso 1 1 calc R U . . .
C56 C 0.0237(2) 0.5053(2) 0.1029(2) 0.0188(8) Uani 1 1 d . . . . .
C85 C 0.4711(3) 0.6254(3) 0.2658(3) 0.0344(10) Uani 1 1 d . . . . .
H85 H 0.535401 0.616127 0.253834 0.041 Uiso 1 1 calc R U . . .
C75 C -0.3203(3) 0.0942(3) 0.4307(3) 0.0362(10) Uani 1 1 d . . . . .
H75 H -0.323898 0.118637 0.470806 0.043 Uiso 1 1 calc R U . . .
C5 C -0.0373(3) 0.0486(3) 0.1958(2) 0.0283(9) Uani 1 1 d . . . . .
C6 C -0.0079(3) -0.0325(3) 0.2649(2) 0.0320(10) Uani 1 1 d . . . . .
C46 C 0.3446(3) 0.5833(3) 0.0758(2) 0.0258(9) Uani 1 1 d . . . . .
H46 H 0.407991 0.567748 0.067673 0.031 Uiso 1 1 calc R U . . .
C45 C 0.2801(3) 0.5213(2) 0.0788(2) 0.0203(8) Uani 1 1 d . . . . .
C57 C 0.1162(2) 0.4806(3) 0.0944(2) 0.0191(8) Uani 1 1 d . . . . .
H57 H 0.133534 0.420051 0.091456 0.023 Uiso 1 1 calc R U . . .
C2 C -0.0589(3) 0.1949(3) 0.1197(2) 0.0232(8) Uani 1 1 d . . . . .
C22 C 0.3207(3) 0.3005(3) 0.4449(2) 0.0259(9) Uani 1 1 d . . . . .
C3 C -0.1003(3) 0.1352(3) 0.0932(2) 0.0344(10) Uani 1 1 d . . . . .
H3 H -0.131463 0.154335 0.050503 0.041 Uiso 1 1 calc R U . . .
C31 C 0.3810(3) 0.0484(3) 0.2525(2) 0.0261(9) Uani 1 1 d . . . . .
C50 C 0.0657(3) 0.6601(3) 0.1012(2) 0.0238(8) Uani 1 1 d . . . . .
H50 H 0.048441 0.720976 0.103450 0.029 Uiso 1 1 calc R U . . .
C80 C 0.4088(3) 0.5635(3) 0.2644(2) 0.0264(9) Uani 1 1 d . . . . .
C39 C 0.1771(3) 0.1422(4) 0.0035(3) 0.0447(12) Uani 1 1 d . . . . .
H39A H 0.109965 0.143037 0.017353 0.067 Uiso 1 1 calc R U . . .
H39B H 0.200001 0.207608 -0.024459 0.067 Uiso 1 1 calc R U . . .
H39C H 0.194745 0.104367 -0.029450 0.067 Uiso 1 1 calc R U . . .
C64 C 0.5281(3) 0.3272(3) 0.1755(2) 0.0307(9) Uani 1 1 d . . . . .
H64 H 0.495186 0.369767 0.197639 0.037 Uiso 1 1 calc R U . . .
O7 O 0.26905(19) 0.5049(2) 0.27474(18) 0.0361(7) Uani 1 1 d . . . . .
C38 C 0.2181(3) 0.0987(3) 0.0757(2) 0.0272(9) Uani 1 1 d . . . . .
H38A H 0.192697 0.033563 0.104058 0.033 Uiso 1 1 calc R U . . .
H38B H 0.197941 0.136547 0.109036 0.033 Uiso 1 1 calc R U . . .
C63 C 0.0699(3) 0.4428(3) 0.2841(2) 0.0231(8) Uani 1 1 d . . . . .
H63 H 0.129651 0.417269 0.275976 0.028 Uiso 1 1 calc R U . . .
C48 C 0.2285(3) 0.6961(3) 0.0941(2) 0.0274(9) Uani 1 1 d . . . . .
H48 H 0.211949 0.755510 0.099583 0.033 Uiso 1 1 calc R U . . .
C35 C 0.3243(3) 0.0925(3) 0.0630(2) 0.0238(8) Uani 1 1 d . . . . .
C34 C 0.3569(3) 0.0538(3) 0.1400(2) 0.0249(8) Uani 1 1 d . . . . .
C79 C -0.2612(3) 0.1043(3) 0.3050(3) 0.0370(10) Uani 1 1 d . . . . .
H79 H -0.222614 0.135311 0.256885 0.044 Uiso 1 1 calc R U . . .
C70 C -0.2692(3) 0.3189(3) 0.4265(3) 0.0348(10) Uani 1 1 d . . . . .
C36 C 0.3589(3) 0.0297(3) 0.0147(2) 0.0328(10) Uani 1 1 d . . . . .
H36A H 0.350149 0.065238 -0.039024 0.039 Uiso 1 1 calc R U . . .
H36B H 0.425811 0.019970 0.013709 0.039 Uiso 1 1 calc R U . . .
C84 C 0.4360(3) 0.7030(3) 0.2856(3) 0.0388(11) Uani 1 1 d . . . . .
H84 H 0.477219 0.747601 0.287221 0.047 Uiso 1 1 calc R U . . .
C47 C 0.3177(3) 0.6715(3) 0.0849(2) 0.0296(9) Uani 1 1 d . . . . .
H47 H 0.363165 0.713392 0.084515 0.036 Uiso 1 1 calc R U . . .
C17 C -0.0267(3) 0.3077(3) 0.4776(2) 0.0253(8) Uani 1 1 d . . . . .
H17 H -0.089817 0.297684 0.479113 0.030 Uiso 1 1 calc R U . . .
C13 C -0.1149(2) -0.0193(3) 0.4556(2) 0.0217(8) Uani 1 1 d . . . . .
H13 H -0.151068 -0.038613 0.505832 0.026 Uiso 1 1 calc R U . . .
C18 C -0.0020(3) 0.3678(3) 0.5136(2) 0.0298(9) Uani 1 1 d . . . . .
H18 H -0.048858 0.397482 0.539096 0.036 Uiso 1 1 calc R U . . .
C74 C -0.3673(3) 0.4383(3) 0.3537(3) 0.0469(13) Uani 1 1 d . . . . .
H74 H -0.393532 0.468242 0.308731 0.056 Uiso 1 1 calc R U . . .
C12 C -0.1079(3) -0.0652(3) 0.4032(2) 0.0254(9) Uani 1 1 d . . . . .
H12 H -0.138988 -0.121909 0.410637 0.030 Uiso 1 1 calc R U . . .
C73 C -0.3875(4) 0.4696(4) 0.4166(4) 0.0604(17) Uani 1 1 d . . . . .
H73 H -0.428454 0.521385 0.414181 0.072 Uiso 1 1 calc R U . . .
C30 C 0.3847(3) 0.0835(3) 0.3112(2) 0.0257(9) Uani 1 1 d . . . . .
H30 H 0.415069 0.046940 0.352464 0.031 Uiso 1 1 calc R U . . .
C4 C -0.0871(3) 0.0434(3) 0.1408(2) 0.0385(11) Uani 1 1 d . . . . .
H4 H -0.107578 -0.013095 0.137437 0.046 Uiso 1 1 calc R U . . .
C11 C -0.0465(3) -0.0122(3) 0.3374(2) 0.0234(8) Uani 1 1 d . . . . .
C81 C 0.3161(3) 0.5759(3) 0.2823(3) 0.0327(10) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N8 C30 1.309(5) . ?
N8 C26 1.409(5) . ?
N8 U2 2.577(3) . ?
C26 C25 1.373(5) . ?
C26 C27 1.443(5) . ?
C32 C33 1.382(6) . ?
C32 C31 1.401(5) . ?
C32 H32 0.9500 . ?
C33 C34 1.406(5) . ?
C33 H33 0.9500 . ?
C23 C24 1.356(6) . ?
C23 C22 1.424(5) . ?
C23 H23 0.9500 . ?
C83 C84 1.362(6) . ?
C83 C82 1.379(6) . ?
C83 H83 0.9500 . ?
C67 C66 1.342(7) . ?
C67 C68 1.376(6) . ?
C67 H67 0.9500 . ?
C82 C81 1.377(6) . ?
C82 H82 0.9500 . ?
C65 C66 1.350(6) . ?
C65 C64 1.372(6) . ?
C65 H65 0.9500 . ?
C68 N10 1.352(5) . ?
C68 H68 0.9500 . ?
C9 C10 1.531(6) . ?
C9 C6 1.546(6) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C66 H66 0.9500 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
O10 C90 1.392(8) . ?
O10 C93 1.400(7) . ?
C90 C91 1.431(9) . ?
C90 H90A 0.9900 . ?
C90 H90B 0.9900 . ?
C91 C92 1.446(9) . ?
C91 H91A 0.9900 . ?
C91 H91B 0.9900 . ?
C92 C93 1.468(9) . ?
C92 H92A 0.9900 . ?
C92 H92B 0.9900 . ?
C93 H93A 0.9900 . ?
C93 H93B 0.9900 . ?
C76 C77 1.370(7) . ?
C76 C75 1.392(6) . ?
C76 H76 0.9500 . ?
C71 C70 1.377(6) . ?
C71 C72 1.406(7) . ?
C71 H71 0.9500 . ?
C77 C78 1.381(7) . ?
C77 H77 0.9500 . ?
C72 C73 1.358(8) . ?
C72 H72 0.9500 . ?
U2 O3 2.068(2) . ?
U2 O2 2.219(2) . ?
U2 N6 2.481(3) . ?
U2 N7 2.486(3) . ?
U2 N5 2.589(3) . ?
U2 N10 2.652(3) . ?
U1 O1 2.092(2) . ?
U1 O3 2.176(2) . ?
U1 N3 2.443(3) . ?
U1 N2 2.474(3) . ?
U1 N4 2.592(3) . ?
U1 N1 2.597(3) . ?
U1 N9 2.621(3) . ?
B1 O1 1.400(5) . ?
B1 O5 1.491(5) . ?
B1 O4 1.499(5) . ?
B1 N11 1.633(6) . ?
C27 C28 1.380(5) . ?
C27 C22 1.440(5) . ?
N4 C15 1.309(5) . ?
N4 C16 1.420(4) . ?
N2 C5 1.359(5) . ?
N2 C2 1.383(5) . ?
N6 C40 1.359(4) . ?
N6 C43 1.392(4) . ?
N10 C64 1.358(5) . ?
O2 B2 1.315(5) . ?
O5 C70 1.367(5) . ?
O6 C80 1.380(4) . ?
O6 B2 1.415(5) . ?
N1 C1 1.308(5) . ?
N1 C55 1.422(5) . ?
C25 C24 1.419(6) . ?
C25 H25 0.9500 . ?
O4 C69 1.362(5) . ?
C1 C2 1.411(5) . ?
C1 H1 0.9500 . ?
C69 C74 1.375(6) . ?
C69 C70 1.403(6) . ?
N5 C44 1.298(5) . ?
N5 C45 1.428(4) . ?
N9 C59 1.345(5) . ?
N9 C63 1.349(5) . ?
C28 C29 1.402(5) . ?
C28 H28 0.9500 . ?
C16 C17 1.365(5) . ?
C16 C29 1.434(5) . ?
C44 C43 1.412(5) . ?
C44 H44 0.9500 . ?
C60 C61 1.364(6) . ?
C60 C59 1.371(5) . ?
C60 H60 0.9500 . ?
C29 C20 1.449(5) . ?
N11 C79 1.345(5) . ?
N11 C75 1.346(5) . ?
C59 H59 0.9500 . ?
N3 C11 1.362(5) . ?
N3 C14 1.385(5) . ?
C51 C50 1.388(5) . ?
C51 C52 1.425(5) . ?
C51 C56 1.442(5) . ?
C58 C57 1.401(5) . ?
C58 C49 1.434(5) . ?
C58 C45 1.434(5) . ?
C14 C13 1.399(5) . ?
C14 C15 1.410(5) . ?
B2 O7 1.408(5) . ?
C49 C50 1.397(5) . ?
C49 C48 1.424(5) . ?
C20 C21 1.393(5) . ?
C20 C19 1.425(5) . ?
C24 H24 0.9500 . ?
C21 C22 1.390(5) . ?
C21 H21 0.9500 . ?
C43 C42 1.389(5) . ?
C40 C41 1.400(5) . ?
C40 C35 1.518(5) . ?
C15 H15 0.9500 . ?
N7 C34 1.363(5) . ?
N7 C31 1.391(5) . ?
C42 C41 1.392(5) . ?
C42 H42 0.9500 . ?
C61 C62 1.377(6) . ?
C61 H61 0.9500 . ?
C54 C55 1.369(5) . ?
C54 C53 1.417(6) . ?
C54 H54 0.9500 . ?
C7 C8 1.524(6) . ?
C7 C6 1.547(6) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C19 C18 1.353(6) . ?
C19 H19 0.9500 . ?
C62 C63 1.382(5) . ?
C62 H62 0.9500 . ?
C37 C36 1.527(6) . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C53 C52 1.362(6) . ?
C53 H53 0.9500 . ?
C55 C56 1.433(5) . ?
C41 H41 0.9500 . ?
C78 C79 1.372(6) . ?
C78 H78 0.9500 . ?
C52 H52 0.9500 . ?
C56 C57 1.391(5) . ?
C85 C80 1.366(5) . ?
C85 C84 1.393(6) . ?
C85 H85 0.9500 . ?
C75 H75 0.9500 . ?
C5 C4 1.412(6) . ?
C5 C6 1.541(6) . ?
C6 C11 1.511(5) . ?
C46 C45 1.361(5) . ?
C46 C47 1.423(5) . ?
C46 H46 0.9500 . ?
C57 H57 0.9500 . ?
C2 C3 1.399(5) . ?
C3 C4 1.373(6) . ?
C3 H3 0.9500 . ?
C31 C30 1.405(5) . ?
C50 H50 0.9500 . ?
C80 C81 1.369(6) . ?
C39 C38 1.510(6) . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C64 H64 0.9500 . ?
O7 C81 1.378(5) . ?
C38 C35 1.549(5) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C63 H63 0.9500 . ?
C48 C47 1.345(6) . ?
C48 H48 0.9500 . ?
C35 C34 1.519(5) . ?
C35 C36 1.545(5) . ?
C79 H79 0.9500 . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C84 H84 0.9500 . ?
C47 H47 0.9500 . ?
C17 C18 1.418(5) . ?
C17 H17 0.9500 . ?
C13 C12 1.386(5) . ?
C13 H13 0.9500 . ?
C18 H18 0.9500 . ?
C74 C73 1.409(7) . ?
C74 H74 0.9500 . ?
C12 C11 1.399(5) . ?
C12 H12 0.9500 . ?
C73 H73 0.9500 . ?
C30 H30 0.9500 . ?
C4 H4 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C30 N8 C26 118.0(3) . . ?
C30 N8 U2 113.5(2) . . ?
C26 N8 U2 124.0(2) . . ?
C25 C26 N8 121.9(3) . . ?
C25 C26 C27 119.3(3) . . ?
N8 C26 C27 118.6(3) . . ?
C33 C32 C31 106.5(4) . . ?
C33 C32 H32 126.7 . . ?
C31 C32 H32 126.7 . . ?
C32 C33 C34 107.3(4) . . ?
C32 C33 H33 126.3 . . ?
C34 C33 H33 126.3 . . ?
C24 C23 C22 121.2(4) . . ?
C24 C23 H23 119.4 . . ?
C22 C23 H23 119.4 . . ?
C84 C83 C82 121.3(4) . . ?
C84 C83 H83 119.3 . . ?
C82 C83 H83 119.3 . . ?
C66 C67 C68 120.8(4) . . ?
C66 C67 H67 119.6 . . ?
C68 C67 H67 119.6 . . ?
C81 C82 C83 117.4(4) . . ?
C81 C82 H82 121.3 . . ?
C83 C82 H82 121.3 . . ?
C66 C65 C64 120.2(4) . . ?
C66 C65 H65 119.9 . . ?
C64 C65 H65 119.9 . . ?
N10 C68 C67 122.0(4) . . ?
N10 C68 H68 119.0 . . ?
C67 C68 H68 119.0 . . ?
C10 C9 C6 115.9(4) . . ?
C10 C9 H9A 108.3 . . ?
C6 C9 H9A 108.3 . . ?
C10 C9 H9B 108.3 . . ?
C6 C9 H9B 108.3 . . ?
H9A C9 H9B 107.4 . . ?
C67 C66 C65 118.4(4) . . ?
C67 C66 H66 120.8 . . ?
C65 C66 H66 120.8 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C90 O10 C93 108.4(5) . . ?
O10 C90 C91 110.5(6) . . ?
O10 C90 H90A 109.6 . . ?
C91 C90 H90A 109.6 . . ?
O10 C90 H90B 109.6 . . ?
C91 C90 H90B 109.6 . . ?
H90A C90 H90B 108.1 . . ?
C90 C91 C92 105.3(7) . . ?
C90 C91 H91A 110.7 . . ?
C92 C91 H91A 110.7 . . ?
C90 C91 H91B 110.7 . . ?
C92 C91 H91B 110.7 . . ?
H91A C91 H91B 108.8 . . ?
C91 C92 C93 107.3(6) . . ?
C91 C92 H92A 110.2 . . ?
C93 C92 H92A 110.2 . . ?
C91 C92 H92B 110.2 . . ?
C93 C92 H92B 110.2 . . ?
H92A C92 H92B 108.5 . . ?
O10 C93 C92 106.8(6) . . ?
O10 C93 H93A 110.4 . . ?
C92 C93 H93A 110.4 . . ?
O10 C93 H93B 110.4 . . ?
C92 C93 H93B 110.4 . . ?
H93A C93 H93B 108.6 . . ?
C77 C76 C75 118.8(5) . . ?
C77 C76 H76 120.6 . . ?
C75 C76 H76 120.6 . . ?
C70 C71 C72 116.6(5) . . ?
C70 C71 H71 121.7 . . ?
C72 C71 H71 121.7 . . ?
C76 C77 C78 119.2(5) . . ?
C76 C77 H77 120.4 . . ?
C78 C77 H77 120.4 . . ?
C73 C72 C71 122.2(5) . . ?
C73 C72 H72 118.9 . . ?
C71 C72 H72 118.9 . . ?
O3 U2 O2 99.15(10) . . ?
O3 U2 N6 109.19(10) . . ?
O2 U2 N6 132.73(9) . . ?
O3 U2 N7 98.18(10) . . ?
O2 U2 N7 142.14(10) . . ?
N6 U2 N7 70.58(10) . . ?
O3 U2 N8 97.06(10) . . ?
O2 U2 N8 77.24(10) . . ?
N6 U2 N8 132.87(9) . . ?
N7 U2 N8 67.38(10) . . ?
O3 U2 N5 101.32(9) . . ?
O2 U2 N5 72.83(9) . . ?
N6 U2 N5 65.17(9) . . ?
N7 U2 N5 135.36(10) . . ?
N8 U2 N5 146.88(10) . . ?
O3 U2 N10 171.63(10) . . ?
O2 U2 N10 80.71(10) . . ?
N6 U2 N10 76.31(9) . . ?
N7 U2 N10 77.44(10) . . ?
N8 U2 N10 74.70(9) . . ?
N5 U2 N10 86.68(9) . . ?
O1 U1 O3 170.65(10) . . ?
O1 U1 N3 82.90(10) . . ?
O3 U1 N3 106.19(9) . . ?
O1 U1 N2 88.21(10) . . ?
O3 U1 N2 96.61(10) . . ?
N3 U1 N2 72.05(10) . . ?
O1 U1 N4 85.11(9) . . ?
O3 U1 N4 96.34(9) . . ?
N3 U1 N4 66.82(10) . . ?
N2 U1 N4 138.82(9) . . ?
O1 U1 N1 82.32(9) . . ?
O3 U1 N1 92.08(9) . . ?
N3 U1 N1 137.28(10) . . ?
N2 U1 N1 67.64(10) . . ?
N4 U1 N1 150.27(9) . . ?
O1 U1 N9 78.92(9) . . ?
O3 U1 N9 92.66(9) . . ?
N3 U1 N9 136.68(10) . . ?
N2 U1 N9 145.11(9) . . ?
N4 U1 N9 72.68(9) . . ?
N1 U1 N9 78.50(9) . . ?
O1 B1 O5 116.6(3) . . ?
O1 B1 O4 113.8(3) . . ?
O5 B1 O4 104.7(3) . . ?
O1 B1 N11 107.9(3) . . ?
O5 B1 N11 106.1(3) . . ?
O4 B1 N11 106.9(3) . . ?
C28 C27 C22 119.6(3) . . ?
C28 C27 C26 121.9(3) . . ?
C22 C27 C26 118.6(3) . . ?
C15 N4 C16 116.3(3) . . ?
C15 N4 U1 107.9(2) . . ?
C16 N4 U1 131.5(2) . . ?
C5 N2 C2 106.1(3) . . ?
C5 N2 U1 135.9(2) . . ?
C2 N2 U1 114.2(2) . . ?
C40 N6 C43 105.7(3) . . ?
C40 N6 U2 135.6(2) . . ?
C43 N6 U2 113.8(2) . . ?
U2 O3 U1 177.55(13) . . ?
B1 O1 U1 158.8(3) . . ?
C68 N10 C64 116.1(3) . . ?
C68 N10 U2 122.3(3) . . ?
C64 N10 U2 121.4(3) . . ?
B2 O2 U2 171.1(3) . . ?
C70 O5 B1 106.8(3) . . ?
C80 O6 B2 105.9(3) . . ?
C1 N1 C55 118.9(3) . . ?
C1 N1 U1 111.8(2) . . ?
C55 N1 U1 122.4(2) . . ?
C26 C25 C24 121.5(4) . . ?
C26 C25 H25 119.2 . . ?
C24 C25 H25 119.2 . . ?
C69 O4 B1 107.1(3) . . ?
N1 C1 C2 122.4(3) . . ?
N1 C1 H1 118.8 . . ?
C2 C1 H1 118.8 . . ?
O4 C69 C74 128.4(5) . . ?
O4 C69 C70 110.5(4) . . ?
C74 C69 C70 121.1(5) . . ?
C44 N5 C45 117.5(3) . . ?
C44 N5 U2 113.1(2) . . ?
C45 N5 U2 127.1(2) . . ?
C59 N9 C63 116.9(3) . . ?
C59 N9 U1 119.7(2) . . ?
C63 N9 U1 122.9(2) . . ?
C27 C28 C29 122.0(3) . . ?
C27 C28 H28 119.0 . . ?
C29 C28 H28 119.0 . . ?
C17 C16 N4 122.8(3) . . ?
C17 C16 C29 120.1(3) . . ?
N4 C16 C29 117.1(3) . . ?
N5 C44 C43 120.4(3) . . ?
N5 C44 H44 119.8 . . ?
C43 C44 H44 119.8 . . ?
C61 C60 C59 118.9(4) . . ?
C61 C60 H60 120.6 . . ?
C59 C60 H60 120.6 . . ?
C28 C29 C16 122.8(3) . . ?
C28 C29 C20 118.5(3) . . ?
C16 C29 C20 118.7(3) . . ?
C79 N11 C75 119.6(4) . . ?
C79 N11 B1 119.0(3) . . ?
C75 N11 B1 121.2(4) . . ?
N9 C59 C60 123.6(4) . . ?
N9 C59 H59 118.2 . . ?
C60 C59 H59 118.2 . . ?
C11 N3 C14 105.7(3) . . ?
C11 N3 U1 133.5(2) . . ?
C14 N3 U1 109.4(2) . . ?
C50 C51 C52 122.0(4) . . ?
C50 C51 C56 119.2(3) . . ?
C52 C51 C56 118.8(4) . . ?
C57 C58 C49 119.9(3) . . ?
C57 C58 C45 122.1(3) . . ?
C49 C58 C45 118.0(3) . . ?
N3 C14 C13 110.4(3) . . ?
N3 C14 C15 119.6(3) . . ?
C13 C14 C15 129.9(3) . . ?
O2 B2 O7 125.5(4) . . ?
O2 B2 O6 125.5(4) . . ?
O7 B2 O6 109.0(3) . . ?
C50 C49 C48 122.6(3) . . ?
C50 C49 C58 118.5(3) . . ?
C48 C49 C58 118.8(3) . . ?
C21 C20 C19 122.8(4) . . ?
C21 C20 C29 118.8(3) . . ?
C19 C20 C29 118.4(3) . . ?
C23 C24 C25 120.2(4) . . ?
C23 C24 H24 119.9 . . ?
C25 C24 H24 119.9 . . ?
C22 C21 C20 122.3(4) . . ?
C22 C21 H21 118.9 . . ?
C20 C21 H21 118.9 . . ?
C42 C43 N6 110.7(3) . . ?
C42 C43 C44 130.8(4) . . ?
N6 C43 C44 118.3(3) . . ?
N6 C40 C41 110.2(3) . . ?
N6 C40 C35 119.5(3) . . ?
C41 C40 C35 130.1(3) . . ?
N4 C15 C14 121.1(3) . . ?
N4 C15 H15 119.4 . . ?
C14 C15 H15 119.4 . . ?
C34 N7 C31 105.9(3) . . ?
C34 N7 U2 136.0(2) . . ?
C31 N7 U2 114.6(2) . . ?
C43 C42 C41 105.9(3) . . ?
C43 C42 H42 127.0 . . ?
C41 C42 H42 127.0 . . ?
C60 C61 C62 119.0(4) . . ?
C60 C61 H61 120.5 . . ?
C62 C61 H61 120.5 . . ?
C55 C54 C53 121.2(4) . . ?
C55 C54 H54 119.4 . . ?
C53 C54 H54 119.4 . . ?
C8 C7 C6 115.2(4) . . ?
C8 C7 H7A 108.5 . . ?
C6 C7 H7A 108.5 . . ?
C8 C7 H7B 108.5 . . ?
C6 C7 H7B 108.5 . . ?
H7A C7 H7B 107.5 . . ?
C18 C19 C20 120.9(4) . . ?
C18 C19 H19 119.5 . . ?
C20 C19 H19 119.5 . . ?
C61 C62 C63 119.3(4) . . ?
C61 C62 H62 120.3 . . ?
C63 C62 H62 120.3 . . ?
C36 C37 H37A 109.5 . . ?
C36 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C36 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C52 C53 C54 120.2(4) . . ?
C52 C53 H53 119.9 . . ?
C54 C53 H53 119.9 . . ?
C54 C55 N1 121.1(3) . . ?
C54 C55 C56 120.2(3) . . ?
N1 C55 C56 118.4(3) . . ?
C42 C41 C40 107.4(3) . . ?
C42 C41 H41 126.3 . . ?
C40 C41 H41 126.3 . . ?
C79 C78 C77 120.0(5) . . ?
C79 C78 H78 120.0 . . ?
C77 C78 H78 120.0 . . ?
C53 C52 C51 121.0(4) . . ?
C53 C52 H52 119.5 . . ?
C51 C52 H52 119.5 . . ?
C57 C56 C55 122.5(3) . . ?
C57 C56 C51 119.2(3) . . ?
C55 C56 C51 118.3(3) . . ?
C80 C85 C84 116.9(4) . . ?
C80 C85 H85 121.5 . . ?
C84 C85 H85 121.5 . . ?
N11 C75 C76 121.4(5) . . ?
N11 C75 H75 119.3 . . ?
C76 C75 H75 119.3 . . ?
N2 C5 C4 109.9(4) . . ?
N2 C5 C6 120.9(3) . . ?
C4 C5 C6 129.1(4) . . ?
C11 C6 C5 108.3(3) . . ?
C11 C6 C9 109.7(3) . . ?
C5 C6 C9 110.0(4) . . ?
C11 C6 C7 108.0(3) . . ?
C5 C6 C7 109.5(3) . . ?
C9 C6 C7 111.2(4) . . ?
C45 C46 C47 120.3(4) . . ?
C45 C46 H46 119.8 . . ?
C47 C46 H46 119.8 . . ?
C46 C45 N5 121.9(3) . . ?
C46 C45 C58 120.9(3) . . ?
N5 C45 C58 117.2(3) . . ?
C56 C57 C58 121.0(3) . . ?
C56 C57 H57 119.5 . . ?
C58 C57 H57 119.5 . . ?
N2 C2 C3 110.2(3) . . ?
N2 C2 C1 121.0(3) . . ?
C3 C2 C1 128.5(4) . . ?
C21 C22 C23 122.5(4) . . ?
C21 C22 C27 118.7(3) . . ?
C23 C22 C27 118.8(4) . . ?
C4 C3 C2 106.6(4) . . ?
C4 C3 H3 126.7 . . ?
C2 C3 H3 126.7 . . ?
N7 C31 C32 110.1(3) . . ?
N7 C31 C30 120.5(3) . . ?
C32 C31 C30 128.8(4) . . ?
C51 C50 C49 122.0(3) . . ?
C51 C50 H50 119.0 . . ?
C49 C50 H50 119.0 . . ?
C85 C80 C81 121.9(4) . . ?
C85 C80 O6 128.8(4) . . ?
C81 C80 O6 109.3(3) . . ?
C38 C39 H39A 109.5 . . ?
C38 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C38 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
N10 C64 C65 122.4(4) . . ?
N10 C64 H64 118.8 . . ?
C65 C64 H64 118.8 . . ?
C81 O7 B2 105.7(3) . . ?
C39 C38 C35 115.5(3) . . ?
C39 C38 H38A 108.4 . . ?
C35 C38 H38A 108.4 . . ?
C39 C38 H38B 108.4 . . ?
C35 C38 H38B 108.4 . . ?
H38A C38 H38B 107.5 . . ?
N9 C63 C62 122.2(4) . . ?
N9 C63 H63 118.9 . . ?
C62 C63 H63 118.9 . . ?
C47 C48 C49 121.2(4) . . ?
C47 C48 H48 119.4 . . ?
C49 C48 H48 119.4 . . ?
C40 C35 C34 108.0(3) . . ?
C40 C35 C36 109.3(3) . . ?
C34 C35 C36 110.8(3) . . ?
C40 C35 C38 108.0(3) . . ?
C34 C35 C38 110.2(3) . . ?
C36 C35 C38 110.4(3) . . ?
N7 C34 C33 110.2(3) . . ?
N7 C34 C35 121.1(3) . . ?
C33 C34 C35 128.7(3) . . ?
N11 C79 C78 120.9(5) . . ?
N11 C79 H79 119.5 . . ?
C78 C79 H79 119.5 . . ?
O5 C70 C71 127.5(4) . . ?
O5 C70 C69 110.9(4) . . ?
C71 C70 C69 121.6(4) . . ?
C37 C36 C35 116.2(4) . . ?
C37 C36 H36A 108.2 . . ?
C35 C36 H36A 108.2 . . ?
C37 C36 H36B 108.2 . . ?
C35 C36 H36B 108.2 . . ?
H36A C36 H36B 107.4 . . ?
C83 C84 C85 121.3(4) . . ?
C83 C84 H84 119.3 . . ?
C85 C84 H84 119.3 . . ?
C48 C47 C46 120.6(4) . . ?
C48 C47 H47 119.7 . . ?
C46 C47 H47 119.7 . . ?
C16 C17 C18 120.9(4) . . ?
C16 C17 H17 119.6 . . ?
C18 C17 H17 119.6 . . ?
C12 C13 C14 106.2(3) . . ?
C12 C13 H13 126.9 . . ?
C14 C13 H13 126.9 . . ?
C19 C18 C17 121.0(4) . . ?
C19 C18 H18 119.5 . . ?
C17 C18 H18 119.5 . . ?
C69 C74 C73 117.4(5) . . ?
C69 C74 H74 121.3 . . ?
C73 C74 H74 121.3 . . ?
C13 C12 C11 107.2(3) . . ?
C13 C12 H12 126.4 . . ?
C11 C12 H12 126.4 . . ?
C72 C73 C74 121.1(5) . . ?
C72 C73 H73 119.4 . . ?
C74 C73 H73 119.4 . . ?
N8 C30 C31 122.2(3) . . ?
N8 C30 H30 118.9 . . ?
C31 C30 H30 118.9 . . ?
C3 C4 C5 107.2(4) . . ?
C3 C4 H4 126.4 . . ?
C5 C4 H4 126.4 . . ?
N3 C11 C12 110.5(3) . . ?
N3 C11 C6 119.1(3) . . ?
C12 C11 C6 130.2(3) . . ?
C80 C81 C82 121.2(4) . . ?
C80 C81 O7 110.1(3) . . ?
C82 C81 O7 128.7(4) . . ?

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
C30 N8 C26 C25 46.4(5) . . . . ?
U2 N8 C26 C25 -108.2(4) . . . . ?
C30 N8 C26 C27 -138.8(4) . . . . ?
U2 N8 C26 C27 66.5(4) . . . . ?
C31 C32 C33 C34 -0.6(5) . . . . ?
C84 C83 C82 C81 -0.1(9) . . . . ?
C66 C67 C68 N10 -2.9(8) . . . . ?
C68 C67 C66 C65 1.7(8) . . . . ?
C64 C65 C66 C67 -0.2(8) . . . . ?
C93 O10 C90 C91 10.8(9) . . . . ?
O10 C90 C91 C92 -3.2(10) . . . . ?
C90 C91 C92 C93 -5.2(10) . . . . ?
C90 O10 C93 C92 -13.7(8) . . . . ?
C91 C92 C93 O10 11.7(9) . . . . ?
C75 C76 C77 C78 2.1(7) . . . . ?
C70 C71 C72 C73 0.3(8) . . . . ?
C25 C26 C27 C28 -173.2(4) . . . . ?
N8 C26 C27 C28 11.9(5) . . . . ?
C25 C26 C27 C22 6.7(5) . . . . ?
N8 C26 C27 C22 -168.2(3) . . . . ?
O5 B1 O1 U1 16.1(9) . . . . ?
O4 B1 O1 U1 138.3(6) . . . . ?
N11 B1 O1 U1 -103.2(7) . . . . ?
C67 C68 N10 C64 2.4(6) . . . . ?
C67 C68 N10 U2 -172.1(3) . . . . ?
O1 B1 O5 C70 127.1(4) . . . . ?
O4 B1 O5 C70 0.3(4) . . . . ?
N11 B1 O5 C70 -112.7(3) . . . . ?
N8 C26 C25 C24 171.8(4) . . . . ?
C27 C26 C25 C24 -2.8(6) . . . . ?
O1 B1 O4 C69 -128.1(4) . . . . ?
O5 B1 O4 C69 0.4(4) . . . . ?
N11 B1 O4 C69 112.8(3) . . . . ?
C55 N1 C1 C2 -166.5(3) . . . . ?
U1 N1 C1 C2 -14.9(4) . . . . ?
B1 O4 C69 C74 -179.5(4) . . . . ?
B1 O4 C69 C70 -0.9(4) . . . . ?
C22 C27 C28 C29 0.8(5) . . . . ?
C26 C27 C28 C29 -179.3(3) . . . . ?
C15 N4 C16 C17 -55.7(5) . . . . ?
U1 N4 C16 C17 97.9(4) . . . . ?
C15 N4 C16 C29 123.9(3) . . . . ?
U1 N4 C16 C29 -82.4(4) . . . . ?
C45 N5 C44 C43 -175.5(3) . . . . ?
U2 N5 C44 C43 20.4(4) . . . . ?
C27 C28 C29 C16 -175.1(3) . . . . ?
C27 C28 C29 C20 3.0(5) . . . . ?
C17 C16 C29 C28 -180.0(3) . . . . ?
N4 C16 C29 C28 0.4(5) . . . . ?
C17 C16 C29 C20 1.9(5) . . . . ?
N4 C16 C29 C20 -177.8(3) . . . . ?
O1 B1 N11 C79 -38.6(5) . . . . ?
O5 B1 N11 C79 -164.3(3) . . . . ?
O4 B1 N11 C79 84.3(4) . . . . ?
O1 B1 N11 C75 145.2(4) . . . . ?
O5 B1 N11 C75 19.4(5) . . . . ?
O4 B1 N11 C75 -92.0(4) . . . . ?
C63 N9 C59 C60 -1.6(6) . . . . ?
U1 N9 C59 C60 170.7(3) . . . . ?
C61 C60 C59 N9 1.9(6) . . . . ?
C11 N3 C14 C13 0.2(4) . . . . ?
U1 N3 C14 C13 149.1(2) . . . . ?
C11 N3 C14 C15 176.8(3) . . . . ?
U1 N3 C14 C15 -34.2(4) . . . . ?
C80 O6 B2 O2 177.4(4) . . . . ?
C80 O6 B2 O7 -2.4(4) . . . . ?
C57 C58 C49 C50 -3.3(5) . . . . ?
C45 C58 C49 C50 175.3(3) . . . . ?
C57 C58 C49 C48 177.8(3) . . . . ?
C45 C58 C49 C48 -3.6(5) . . . . ?
C28 C29 C20 C21 -3.8(5) . . . . ?
C16 C29 C20 C21 174.4(3) . . . . ?
C28 C29 C20 C19 178.8(3) . . . . ?
C16 C29 C20 C19 -2.9(5) . . . . ?
C22 C23 C24 C25 3.9(7) . . . . ?
C26 C25 C24 C23 -2.5(6) . . . . ?
C19 C20 C21 C22 178.1(4) . . . . ?
C29 C20 C21 C22 0.9(6) . . . . ?
C40 N6 C43 C42 -1.2(4) . . . . ?
U2 N6 C43 C42 158.0(2) . . . . ?
C40 N6 C43 C44 174.5(3) . . . . ?
U2 N6 C43 C44 -26.3(4) . . . . ?
N5 C44 C43 C42 177.9(4) . . . . ?
N5 C44 C43 N6 3.2(5) . . . . ?
C43 N6 C40 C41 1.9(4) . . . . ?
U2 N6 C40 C41 -150.4(3) . . . . ?
C43 N6 C40 C35 -174.8(3) . . . . ?
U2 N6 C40 C35 32.9(5) . . . . ?
C16 N4 C15 C14 -176.4(3) . . . . ?
U1 N4 C15 C14 24.0(4) . . . . ?
N3 C14 C15 N4 5.7(5) . . . . ?
C13 C14 C15 N4 -178.4(3) . . . . ?
N6 C43 C42 C41 0.0(4) . . . . ?
C44 C43 C42 C41 -175.0(4) . . . . ?
C59 C60 C61 C62 -0.8(6) . . . . ?
C21 C20 C19 C18 -174.6(4) . . . . ?
C29 C20 C19 C18 2.7(6) . . . . ?
C60 C61 C62 C63 -0.3(6) . . . . ?
C55 C54 C53 C52 -3.5(6) . . . . ?
C53 C54 C55 N1 171.1(4) . . . . ?
C53 C54 C55 C56 -2.1(6) . . . . ?
C1 N1 C55 C54 47.2(5) . . . . ?
U1 N1 C55 C54 -101.3(4) . . . . ?
C1 N1 C55 C56 -139.4(3) . . . . ?
U1 N1 C55 C56 72.1(4) . . . . ?
C43 C42 C41 C40 1.2(4) . . . . ?
N6 C40 C41 C42 -2.0(4) . . . . ?
C35 C40 C41 C42 174.2(4) . . . . ?
C76 C77 C78 C79 -1.3(8) . . . . ?
C54 C53 C52 C51 3.8(6) . . . . ?
C50 C51 C52 C53 -179.8(4) . . . . ?
C56 C51 C52 C53 1.4(6) . . . . ?
C54 C55 C56 C57 -173.9(4) . . . . ?
N1 C55 C56 C57 12.7(5) . . . . ?
C54 C55 C56 C51 7.2(5) . . . . ?
N1 C55 C56 C51 -166.3(3) . . . . ?
C50 C51 C56 C57 -4.6(5) . . . . ?
C52 C51 C56 C57 174.2(3) . . . . ?
C50 C51 C56 C55 174.4(3) . . . . ?
C52 C51 C56 C55 -6.7(5) . . . . ?
C79 N11 C75 C76 -1.0(6) . . . . ?
B1 N11 C75 C76 175.2(4) . . . . ?
C77 C76 C75 N11 -1.0(7) . . . . ?
C2 N2 C5 C4 -0.6(5) . . . . ?
U1 N2 C5 C4 155.2(3) . . . . ?
C2 N2 C5 C6 -177.3(4) . . . . ?
U1 N2 C5 C6 -21.5(6) . . . . ?
N2 C5 C6 C11 53.2(5) . . . . ?
C4 C5 C6 C11 -122.8(5) . . . . ?
N2 C5 C6 C9 173.1(4) . . . . ?
C4 C5 C6 C9 -2.9(6) . . . . ?
N2 C5 C6 C7 -64.4(5) . . . . ?
C4 C5 C6 C7 119.6(5) . . . . ?
C10 C9 C6 C11 -167.1(4) . . . . ?
C10 C9 C6 C5 73.8(6) . . . . ?
C10 C9 C6 C7 -47.7(6) . . . . ?
C8 C7 C6 C11 56.1(5) . . . . ?
C8 C7 C6 C5 173.8(4) . . . . ?
C8 C7 C6 C9 -64.4(5) . . . . ?
C47 C46 C45 N5 -178.6(3) . . . . ?
C47 C46 C45 C58 0.6(6) . . . . ?
C44 N5 C45 C46 -61.3(5) . . . . ?
U2 N5 C45 C46 100.2(4) . . . . ?
C44 N5 C45 C58 119.4(4) . . . . ?
U2 N5 C45 C58 -79.1(4) . . . . ?
C57 C58 C45 C46 -179.3(3) . . . . ?
C49 C58 C45 C46 2.2(5) . . . . ?
C57 C58 C45 N5 0.0(5) . . . . ?
C49 C58 C45 N5 -178.6(3) . . . . ?
C55 C56 C57 C58 -175.9(3) . . . . ?
C51 C56 C57 C58 3.1(5) . . . . ?
C49 C58 C57 C56 0.9(5) . . . . ?
C45 C58 C57 C56 -177.7(3) . . . . ?
C5 N2 C2 C3 0.4(4) . . . . ?
U1 N2 C2 C3 -161.3(3) . . . . ?
C5 N2 C2 C1 173.9(3) . . . . ?
U1 N2 C2 C1 12.1(4) . . . . ?
N1 C1 C2 N2 2.7(6) . . . . ?
N1 C1 C2 C3 174.8(4) . . . . ?
C20 C21 C22 C23 -175.3(4) . . . . ?
C20 C21 C22 C27 2.9(6) . . . . ?
C24 C23 C22 C21 178.4(4) . . . . ?
C24 C23 C22 C27 0.1(6) . . . . ?
C28 C27 C22 C21 -3.7(5) . . . . ?
C26 C27 C22 C21 176.3(3) . . . . ?
C28 C27 C22 C23 174.6(4) . . . . ?
C26 C27 C22 C23 -5.3(5) . . . . ?
N2 C2 C3 C4 -0.1(5) . . . . ?
C1 C2 C3 C4 -172.9(4) . . . . ?
C34 N7 C31 C32 0.4(5) . . . . ?
U2 N7 C31 C32 -161.8(3) . . . . ?
C34 N7 C31 C30 172.5(4) . . . . ?
U2 N7 C31 C30 10.2(5) . . . . ?
C33 C32 C31 N7 0.1(5) . . . . ?
C33 C32 C31 C30 -171.0(4) . . . . ?
C52 C51 C50 C49 -176.6(4) . . . . ?
C56 C51 C50 C49 2.2(6) . . . . ?
C48 C49 C50 C51 -179.4(4) . . . . ?
C58 C49 C50 C51 1.7(5) . . . . ?
C84 C85 C80 C81 -0.7(7) . . . . ?
C84 C85 C80 O6 177.1(4) . . . . ?
B2 O6 C80 C85 -176.8(4) . . . . ?
B2 O6 C80 C81 1.2(4) . . . . ?
C68 N10 C64 C65 -0.9(6) . . . . ?
U2 N10 C64 C65 173.6(3) . . . . ?
C66 C65 C64 N10 -0.1(7) . . . . ?
O2 B2 O7 C81 -177.1(4) . . . . ?
O6 B2 O7 C81 2.7(4) . . . . ?
C59 N9 C63 C62 0.4(5) . . . . ?
U1 N9 C63 C62 -171.7(3) . . . . ?
C61 C62 C63 N9 0.5(6) . . . . ?
C50 C49 C48 C47 -176.6(4) . . . . ?
C58 C49 C48 C47 2.2(6) . . . . ?
N6 C40 C35 C34 -62.3(4) . . . . ?
C41 C40 C35 C34 121.8(4) . . . . ?
N6 C40 C35 C36 177.1(3) . . . . ?
C41 C40 C35 C36 1.2(5) . . . . ?
N6 C40 C35 C38 56.9(4) . . . . ?
C41 C40 C35 C38 -119.0(4) . . . . ?
C39 C38 C35 C40 58.4(4) . . . . ?
C39 C38 C35 C34 176.2(3) . . . . ?
C39 C38 C35 C36 -61.1(5) . . . . ?
C31 N7 C34 C33 -0.8(5) . . . . ?
U2 N7 C34 C33 155.6(3) . . . . ?
C31 N7 C34 C35 -177.7(3) . . . . ?
U2 N7 C34 C35 -21.2(6) . . . . ?
C32 C33 C34 N7 0.9(5) . . . . ?
C32 C33 C34 C35 177.4(4) . . . . ?
C40 C35 C34 N7 56.8(5) . . . . ?
C36 C35 C34 N7 176.5(3) . . . . ?
C38 C35 C34 N7 -61.1(5) . . . . ?
C40 C35 C34 C33 -119.4(5) . . . . ?
C36 C35 C34 C33 0.3(6) . . . . ?
C38 C35 C34 C33 122.8(5) . . . . ?
C75 N11 C79 C78 1.8(6) . . . . ?
B1 N11 C79 C78 -174.5(4) . . . . ?
C77 C78 C79 N11 -0.7(7) . . . . ?
B1 O5 C70 C71 178.8(4) . . . . ?
B1 O5 C70 C69 -0.8(4) . . . . ?
C72 C71 C70 O5 -179.8(4) . . . . ?
C72 C71 C70 C69 -0.2(7) . . . . ?
O4 C69 C70 O5 1.2(5) . . . . ?
C74 C69 C70 O5 179.8(4) . . . . ?
O4 C69 C70 C71 -178.5(4) . . . . ?
C74 C69 C70 C71 0.2(7) . . . . ?
C40 C35 C36 C37 -169.0(4) . . . . ?
C34 C35 C36 C37 72.1(5) . . . . ?
C38 C35 C36 C37 -50.3(5) . . . . ?
C82 C83 C84 C85 0.3(8) . . . . ?
C80 C85 C84 C83 0.0(7) . . . . ?
C49 C48 C47 C46 0.6(6) . . . . ?
C45 C46 C47 C48 -2.1(6) . . . . ?
N4 C16 C17 C18 179.2(3) . . . . ?
C29 C16 C17 C18 -0.4(6) . . . . ?
N3 C14 C13 C12 -0.5(4) . . . . ?
C15 C14 C13 C12 -176.7(4) . . . . ?
C20 C19 C18 C17 -1.2(6) . . . . ?
C16 C17 C18 C19 0.1(6) . . . . ?
O4 C69 C74 C73 178.2(4) . . . . ?
C70 C69 C74 C73 -0.2(7) . . . . ?
C14 C13 C12 C11 0.6(4) . . . . ?
C71 C72 C73 C74 -0.4(9) . . . . ?
C69 C74 C73 C72 0.4(8) . . . . ?
C26 N8 C30 C31 -168.6(4) . . . . ?
U2 N8 C30 C31 -11.4(5) . . . . ?
N7 C31 C30 N8 1.2(6) . . . . ?
C32 C31 C30 N8 171.5(4) . . . . ?
C2 C3 C4 C5 -0.2(5) . . . . ?
N2 C5 C4 C3 0.5(5) . . . . ?
C6 C5 C4 C3 176.8(4) . . . . ?
C14 N3 C11 C12 0.2(4) . . . . ?
U1 N3 C11 C12 -137.7(3) . . . . ?
C14 N3 C11 C6 -175.8(3) . . . . ?
U1 N3 C11 C6 46.2(5) . . . . ?
C13 C12 C11 N3 -0.5(4) . . . . ?
C13 C12 C11 C6 174.9(4) . . . . ?
C5 C6 C11 N3 -65.6(5) . . . . ?
C9 C6 C11 N3 174.3(4) . . . . ?
C7 C6 C11 N3 52.9(4) . . . . ?
C5 C6 C11 C12 119.2(4) . . . . ?
C9 C6 C11 C12 -0.9(6) . . . . ?
C7 C6 C11 C12 -122.2(4) . . . . ?
C85 C80 C81 C82 1.0(7) . . . . ?
O6 C80 C81 C82 -177.2(4) . . . . ?
C85 C80 C81 O7 178.7(4) . . . . ?
O6 C80 C81 O7 0.6(5) . . . . ?
C83 C82 C81 C80 -0.6(8) . . . . ?
C83 C82 C81 O7 -177.9(5) . . . . ?
B2 O7 C81 C80 -2.0(5) . . . . ?
B2 O7 C81 C82 175.5(5) . . . . ?

_refine_diff_density_max         1.102
_refine_diff_density_min         -1.069
_refine_diff_density_rms         0.117


# start Validation Reply Form
_vrf_PLAT910_3_THF               
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         24 Note  
RESPONSE: This has been noted, but is not serious. The independent 
reflections/parameters ratio is equal to 18.3, indicating that there are 
no issues with the data collected.
;
####################################################################### 
# 
# 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_5THF_THF
_database_code_depnum_ccdc_archive 'CCDC 1812764'
_audit_update_record             
;
2017-12-20 deposited with the CCDC.
2018-03-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 [{HPh2SiO(THF)UOU(THF)OSiPh2H}(LA)]
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C94 H94 N8 O5 Si2 U2, C4 H8 O'
_chemical_formula_sum            'C98 H102 N8 O7 Si2 U2'
_chemical_formula_weight         2036.12

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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_space_group_IT_number           15
_symmetry_space_group_name_H-M   C2/c
_space_group_name_Hall           '-C 2yc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   22.5124(2)
_cell_length_b                   19.8405(2)
_cell_length_c                   20.1410(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 110.2830(10)
_cell_angle_gamma                90.00
_cell_volume                     8438.29(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    22958
_cell_measurement_theta_min      3.0660
_cell_measurement_theta_max      28.693

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.603
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4056
_exptl_absorpt_coefficient_mu    3.925
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.3404
_exptl_absorpt_correction_T_max  0.7442
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.42b (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_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.
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 16.1042
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            88911
_diffrn_reflns_av_R_equivalents  0.0598
_diffrn_reflns_av_sigmaI/netI    0.0306
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.82
_diffrn_reflns_theta_max         26.37
_reflns_number_total             8628
_reflns_number_gt                7290
_reflns_threshold_expression     >2σ(I)
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -25.00  22.00   1.00   30.00    --  -18.53 -99.00 120.00   47
  2  ω    -25.00  22.00   1.00   30.00    --  -18.53 -99.00 -60.00   47
  3  ω    -25.00  22.00   1.00   30.00    --  -18.53 -99.00-180.00   47
  4  ω    -93.00 -34.00   1.00   30.00    --  -18.53-179.00 -30.00   59
  5  ω    -93.00 -34.00   1.00   30.00    --  -18.53-179.00-180.00   59
  6  ω    -25.00  22.00   1.00   30.00    --  -18.53 -99.00  30.00   47
  7  ω     -2.00  91.00   1.00   30.00    --   20.25  38.00 -90.00   93
  8  ω    -48.00  39.00   1.00   30.00    --   20.25 -57.00   0.00   87
  9  ω      2.00  89.00   1.00   30.00    --   20.25  57.00 -90.00   87
 10  ω    -48.00  39.00   1.00   30.00    --   20.25 -57.00 120.00   87
 11  ω    -67.00  12.00   1.00   30.00    --  -18.53 114.00-133.62   79
 12  ω      2.00  89.00   1.00   30.00    --   20.25  57.00 150.00   87
 13  ω    -48.00  39.00   1.00   30.00    --   20.25 -57.00 150.00   87
 14  ω     -2.00  42.00   1.00   30.00    --   20.25-126.00 160.91   44
 15  ω    -18.00  93.00   1.00   30.00    --   20.25  19.00 120.00  111
;

_computing_data_collection       'CrysAlisPro 1.171.38.42b (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.42b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.42b (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.

The THF lattice solvent was positionally disordered over two 
positions, so it's thermal parameters were split into two parts (A and B) 
and refined anisotropically in a 31:69 ratio (Part A:Part B). In addition, 
the thermal parameters of the THF molecule were restrained to be similar to 
one another through the use of the SIMU and DELU commands.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0195P)²+30.4918P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8628
_refine_ls_number_parameters     586
_refine_ls_number_restraints     132
_refine_ls_R_factor_all          0.0378
_refine_ls_R_factor_gt           0.0267
_refine_ls_wR_factor_ref         0.0574
_refine_ls_wR_factor_gt          0.0538
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_restrained_S_all      1.040
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.506351(6) 0.241329(6) 0.646554(6) 0.01630(4) Uani 1 1 d . . .
Si1 Si 0.49518(5) 0.26559(6) 0.46243(5) 0.0253(2) Uani 1 1 d . . .
O3 O 0.5000 0.23380(16) 0.7500 0.0202(7) Uani 1 2 d S . .
O1 O 0.49928(11) 0.23453(12) 0.53827(12) 0.0241(5) Uani 1 1 d . . .
O4 O 0.47988(13) 0.11669(13) 0.61334(15) 0.0344(6) Uani 1 1 d . . .
N1 N 0.38361(12) 0.24410(14) 0.58818(14) 0.0192(6) Uani 1 1 d . . .
N3 N 0.59492(13) 0.31647(14) 0.65192(15) 0.0212(6) Uani 1 1 d . . .
N4 N 0.61510(13) 0.17970(14) 0.67478(15) 0.0209(6) Uani 1 1 d . . .
N2 N 0.46636(13) 0.35670(14) 0.62065(14) 0.0183(6) Uani 1 1 d . . .
C11 C 0.60129(16) 0.38267(17) 0.63992(18) 0.0229(8) Uani 1 1 d . . .
C29 C 0.65384(16) 0.10111(17) 0.77393(19) 0.0215(7) Uani 1 1 d . . .
C55 C 0.34383(15) 0.18791(17) 0.55983(18) 0.0207(7) Uani 1 1 d . . .
C57 C 0.35504(15) 0.14924(17) 0.68017(18) 0.0200(7) Uani 1 1 d . . .
H57 H 0.3753 0.1905 0.6989 0.024 Uiso 1 1 calc R . .
C16 C 0.63715(16) 0.11365(17) 0.69890(19) 0.0230(8) Uani 1 1 d . . .
C1 C 0.36504(17) 0.30269(18) 0.55871(19) 0.0211(7) Uani 1 1 d . . .
C5 C 0.49193(16) 0.41810(16) 0.61847(18) 0.0203(7) Uani 1 1 d . . .
C4 C 0.44756(17) 0.46021(18) 0.5701(2) 0.0272(8) Uani 1 1 d . . .
H4 H 0.4542 0.5054 0.5589 0.033 Uiso 1 1 calc R . .
C2 C 0.40430(16) 0.35987(17) 0.57321(18) 0.0217(7) Uani 1 1 d . . .
C15 C 0.65284(17) 0.21457(19) 0.65137(19) 0.0241(8) Uani 1 1 d . . .
C14 C 0.64283(16) 0.28337(18) 0.63654(18) 0.0236(8) Uani 1 1 d . . .
C54 C 0.31714(16) 0.17785(19) 0.48819(19) 0.0259(8) Uani 1 1 d . . .
H54 H 0.3213 0.2116 0.4566 0.031 Uiso 1 1 calc R . .
C3 C 0.39241(18) 0.42338(18) 0.5420(2) 0.0289(9) Uani 1 1 d . . .
H3 H 0.3538 0.4385 0.5079 0.035 Uiso 1 1 calc R . .
C49 C 0.31689(17) 0.03775(18) 0.6986(2) 0.0263(8) Uani 1 1 d . . .
C7 C 0.57496(16) 0.42217(18) 0.74159(18) 0.0237(8) Uani 1 1 d . . .
H7A H 0.5527 0.4573 0.7589 0.028 Uiso 1 1 calc R . .
H7B H 0.5576 0.3779 0.7485 0.028 Uiso 1 1 calc R . .
C6 C 0.56081(17) 0.43318(17) 0.66107(19) 0.0227(8) Uani 1 1 d . . .
C12 C 0.65213(18) 0.3930(2) 0.6159(2) 0.0325(9) Uani 1 1 d . . .
H12 H 0.6657 0.4348 0.6031 0.039 Uiso 1 1 calc R . .
C56 C 0.33490(16) 0.13838(17) 0.60740(19) 0.0225(8) Uani 1 1 d . . .
C53 C 0.28349(17) 0.1181(2) 0.4606(2) 0.0313(9) Uani 1 1 d . . .
H53 H 0.2648 0.1127 0.4108 0.038 Uiso 1 1 calc R . .
C64 C 0.37142(18) 0.3147(2) 0.3896(2) 0.0298(9) Uani 1 1 d . . .
H64 H 0.3868 0.3549 0.4154 0.036 Uiso 1 1 calc R . .
C63 C 0.41245(17) 0.26068(19) 0.39709(18) 0.0264(8) Uani 1 1 d . . .
C13 C 0.67872(18) 0.3300(2) 0.6144(2) 0.0342(9) Uani 1 1 d . . .
H13 H 0.7143 0.3205 0.6010 0.041 Uiso 1 1 calc R . .
C51 C 0.30239(16) 0.07682(18) 0.5790(2) 0.0251(8) Uani 1 1 d . . .
C17 C 0.64642(18) 0.06528(19) 0.6557(2) 0.0296(9) Uani 1 1 d . . .
H17 H 0.6347 0.0737 0.6063 0.036 Uiso 1 1 calc R . .
C50 C 0.29504(17) 0.02808(18) 0.6253(2) 0.0292(9) Uani 1 1 d . . .
H50 H 0.2745 -0.0131 0.6065 0.035 Uiso 1 1 calc R . .
C52 C 0.27738(18) 0.06817(19) 0.5038(2) 0.0296(9) Uani 1 1 d . . .
H52 H 0.2565 0.0274 0.4842 0.036 Uiso 1 1 calc R . .
C9 C 0.57794(18) 0.50593(18) 0.6470(2) 0.0299(9) Uani 1 1 d . . .
H9A H 0.6245 0.5111 0.6670 0.036 Uiso 1 1 calc R . .
H9B H 0.5647 0.5128 0.5952 0.036 Uiso 1 1 calc R . .
C62 C 0.4871(2) 0.0615(2) 0.6618(3) 0.0529(13) Uani 1 1 d . . .
H62A H 0.4525 0.0614 0.6815 0.063 Uiso 1 1 calc R . .
H62B H 0.5281 0.0646 0.7014 0.063 Uiso 1 1 calc R . .
C59 C 0.4622(2) 0.0913(2) 0.5422(2) 0.0451(12) Uani 1 1 d . . .
H59B H 0.4980 0.0961 0.5247 0.054 Uiso 1 1 calc R . .
H59A H 0.4258 0.1171 0.5105 0.054 Uiso 1 1 calc R . .
C69 C 0.54794(18) 0.2167(2) 0.4252(2) 0.0336(9) Uani 1 1 d . . .
C8 C 0.64515(18) 0.4243(2) 0.7859(2) 0.0347(9) Uani 1 1 d . . .
H8A H 0.6506 0.4170 0.8358 0.052 Uiso 1 1 calc R . .
H8B H 0.6626 0.4684 0.7805 0.052 Uiso 1 1 calc R . .
H8C H 0.6675 0.3889 0.7700 0.052 Uiso 1 1 calc R . .
C10 C 0.5478(2) 0.56092(19) 0.6780(2) 0.0377(10) Uani 1 1 d . . .
H10B H 0.5610 0.6053 0.6669 0.057 Uiso 1 1 calc R . .
H10A H 0.5614 0.5555 0.7295 0.057 Uiso 1 1 calc R . .
H10C H 0.5015 0.5573 0.6576 0.057 Uiso 1 1 calc R . .
C18 C 0.6736(2) 0.0022(2) 0.6838(2) 0.0374(10) Uani 1 1 d . . .
H18 H 0.6787 -0.0315 0.6527 0.045 Uiso 1 1 calc R . .
C68 C 0.3882(2) 0.2033(2) 0.3571(2) 0.0356(10) Uani 1 1 d . . .
H68 H 0.4151 0.1656 0.3604 0.043 Uiso 1 1 calc R . .
C66 C 0.2856(2) 0.2537(2) 0.3079(2) 0.0459(12) Uani 1 1 d . . .
H66 H 0.2423 0.2509 0.2786 0.055 Uiso 1 1 calc R . .
C60 C 0.4450(2) 0.0194(2) 0.5430(3) 0.0460(12) Uani 1 1 d . . .
H60B H 0.4553 -0.0062 0.5061 0.055 Uiso 1 1 calc R . .
H60A H 0.3993 0.0143 0.5349 0.055 Uiso 1 1 calc R . .
C67 C 0.3254(2) 0.2000(2) 0.3126(2) 0.0438(11) Uani 1 1 d . . .
H67 H 0.3100 0.1606 0.2854 0.053 Uiso 1 1 calc R . .
C74 C 0.5940(2) 0.1734(2) 0.4664(2) 0.0383(10) Uani 1 1 d . . .
H74 H 0.5987 0.1675 0.5148 0.046 Uiso 1 1 calc R . .
C70 C 0.5433(2) 0.2244(3) 0.3550(2) 0.0564(14) Uani 1 1 d . . .
H70 H 0.5121 0.2539 0.3253 0.068 Uiso 1 1 calc R . .
C19 C 0.69221(19) -0.01061(19) 0.7538(2) 0.0348(10) Uani 1 1 d . . .
H19 H 0.7117 -0.0525 0.7716 0.042 Uiso 1 1 calc R . .
C73 C 0.6338(2) 0.1380(3) 0.4388(3) 0.0515(12) Uani 1 1 d . . .
H73 H 0.6647 0.1078 0.4680 0.062 Uiso 1 1 calc R . .
C61 C 0.4844(3) -0.0046(3) 0.6156(3) 0.0703(17) Uani 1 1 d . . .
H61B H 0.5272 -0.0186 0.6177 0.084 Uiso 1 1 calc R . .
H61A H 0.4637 -0.0425 0.6312 0.084 Uiso 1 1 calc R . .
C65 C 0.3088(2) 0.3116(2) 0.3455(2) 0.0416(11) Uani 1 1 d . . .
H65 H 0.2818 0.3493 0.3413 0.050 Uiso 1 1 calc R . .
C72 C 0.6279(2) 0.1470(3) 0.3694(3) 0.0614(15) Uani 1 1 d . . .
H72 H 0.6550 0.1234 0.3504 0.074 Uiso 1 1 calc R . .
C71 C 0.5828(3) 0.1901(3) 0.3274(3) 0.0680(17) Uani 1 1 d . . .
H71 H 0.5788 0.1964 0.2793 0.082 Uiso 1 1 calc R . .
O10A O 0.2867(9) 0.6816(12) 0.6198(10) 0.116(4) Uani 0.308(10) 1 d PDU A 2
C93A C 0.3526(11) 0.6311(16) 0.5707(12) 0.096(4) Uani 0.308(10) 1 d PDU A 2
H93B H 0.3618 0.6067 0.5325 0.115 Uiso 0.308(10) 1 calc PR A 2
H93A H 0.3854 0.6657 0.5916 0.115 Uiso 0.308(10) 1 calc PR A 2
C92A C 0.3436(13) 0.5844(11) 0.6254(14) 0.100(4) Uani 0.308(10) 1 d PDU A 2
H92B H 0.3824 0.5592 0.6524 0.120 Uiso 0.308(10) 1 calc PR A 2
H92A H 0.3072 0.5534 0.6061 0.120 Uiso 0.308(10) 1 calc PR A 2
C94A C 0.2859(14) 0.6599(17) 0.5466(12) 0.101(4) Uani 0.308(10) 1 d PDU A 2
H94A H 0.2532 0.6254 0.5247 0.121 Uiso 0.308(10) 1 calc PR A 2
H94B H 0.2807 0.6986 0.5139 0.121 Uiso 0.308(10) 1 calc PR A 2
C91A C 0.3295(11) 0.6463(13) 0.6678(10) 0.093(4) Uani 0.308(10) 1 d PDU A 2
H91B H 0.3132 0.6304 0.7049 0.111 Uiso 0.308(10) 1 calc PR A 2
H91A H 0.3683 0.6733 0.6904 0.111 Uiso 0.308(10) 1 calc PR A 2
O10B O 0.2593(4) 0.6406(6) 0.5972(5) 0.116(4) Uani 0.692(10) 1 d PDU A 1
C93B C 0.3317(6) 0.6154(7) 0.5551(5) 0.095(3) Uani 0.692(10) 1 d PDU A 1
H93D H 0.3018 0.5785 0.5326 0.114 Uiso 0.692(10) 1 calc PR A 1
H93C H 0.3614 0.6224 0.5292 0.114 Uiso 0.692(10) 1 calc PR A 1
C92B C 0.3657(5) 0.6033(7) 0.6329(6) 0.089(3) Uani 0.692(10) 1 d PDU A 1
H92D H 0.3953 0.6401 0.6562 0.107 Uiso 0.692(10) 1 calc PR A 1
H92C H 0.3874 0.5591 0.6431 0.107 Uiso 0.692(10) 1 calc PR A 1
C94B C 0.2974(6) 0.6804(7) 0.5615(7) 0.094(4) Uani 0.692(10) 1 d PDU A 1
H94D H 0.3254 0.7148 0.5924 0.113 Uiso 0.692(10) 1 calc PR A 1
H94C H 0.2714 0.7000 0.5154 0.113 Uiso 0.692(10) 1 calc PR A 1
C91B C 0.3019(5) 0.6051(7) 0.6498(6) 0.095(3) Uani 0.692(10) 1 d PDU A 1
H91D H 0.2863 0.5587 0.6515 0.114 Uiso 0.692(10) 1 calc PR A 1
H91C H 0.3091 0.6270 0.6960 0.114 Uiso 0.692(10) 1 calc PR A 1
H80 H 0.5147(16) 0.3314(17) 0.4712(18) 0.023(9) Uiso 1 1 d . . .
H1 H 0.3240(17) 0.3070(16) 0.5281(18) 0.016(9) Uiso 1 1 d . . .
H15 H 0.6911(17) 0.1953(17) 0.6467(18) 0.022(9) Uiso 1 1 d . . .


_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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 2.135(2) . ?
U1 O3 2.1425(3) . ?
U1 N2 2.449(3) . ?
U1 N3 2.462(3) . ?
U1 O4 2.577(3) . ?
U1 N1 2.602(3) . ?
U1 N4 2.617(3) . ?
Si1 O1 1.620(2) . ?
Si1 C63 1.874(4) . ?
Si1 C69 1.879(4) . ?
Si1 H80 1.37(3) . ?
O3 U1 2.1425(3) 2_656 ?
O4 C59 1.438(5) . ?
O4 C62 1.438(5) . ?
N1 C1 1.306(4) . ?
N1 C55 1.420(4) . ?
N3 C11 1.352(4) . ?
N3 C14 1.386(4) . ?
N4 C15 1.304(4) . ?
N4 C16 1.426(4) . ?
N2 C5 1.355(4) . ?
N2 C2 1.394(4) . ?
C11 C12 1.404(5) . ?
C11 C6 1.512(5) . ?
C29 C57 1.391(5) 2_656 ?
C29 C49 1.438(5) 2_656 ?
C29 C16 1.447(5) . ?
C55 C54 1.372(5) . ?
C55 C56 1.434(5) . ?
C57 C29 1.391(5) 2_656 ?
C57 C56 1.393(5) . ?
C57 H57 0.9500 . ?
C16 C17 1.360(5) . ?
C1 C2 1.405(5) . ?
C1 H1 0.92(3) . ?
C5 C4 1.403(5) . ?
C5 C6 1.519(5) . ?
C4 C3 1.382(5) . ?
C4 H4 0.9500 . ?
C2 C3 1.392(5) . ?
C15 C14 1.399(5) . ?
C15 H15 0.98(4) . ?
C14 C13 1.399(5) . ?
C54 C53 1.413(5) . ?
C54 H54 0.9500 . ?
C3 H3 0.9500 . ?
C49 C50 1.398(5) . ?
C49 C19 1.420(5) 2_656 ?
C49 C29 1.438(5) 2_656 ?
C7 C8 1.522(5) . ?
C7 C6 1.556(5) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C6 C9 1.545(5) . ?
C12 C13 1.390(5) . ?
C12 H12 0.9500 . ?
C56 C51 1.437(5) . ?
C53 C52 1.356(5) . ?
C53 H53 0.9500 . ?
C64 C65 1.383(6) . ?
C64 C63 1.388(5) . ?
C64 H64 0.9500 . ?
C63 C68 1.393(5) . ?
C13 H13 0.9500 . ?
C51 C50 1.393(5) . ?
C51 C52 1.430(5) . ?
C17 C18 1.422(5) . ?
C17 H17 0.9500 . ?
C50 H50 0.9500 . ?
C52 H52 0.9500 . ?
C9 C10 1.528(5) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C62 C61 1.597(7) . ?
C62 H62A 0.9900 . ?
C62 H62B 0.9900 . ?
C59 C60 1.481(6) . ?
C59 H59B 0.9900 . ?
C59 H59A 0.9900 . ?
C69 C74 1.380(5) . ?
C69 C70 1.389(6) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10C 0.9800 . ?
C18 C19 1.349(6) . ?
C18 H18 0.9500 . ?
C68 C67 1.387(6) . ?
C68 H68 0.9500 . ?
C66 C65 1.374(6) . ?
C66 C67 1.375(6) . ?
C66 H66 0.9500 . ?
C60 C61 1.501(7) . ?
C60 H60B 0.9900 . ?
C60 H60A 0.9900 . ?
C67 H67 0.9500 . ?
C74 C73 1.396(6) . ?
C74 H74 0.9500 . ?
C70 C71 1.382(6) . ?
C70 H70 0.9500 . ?
C19 C49 1.420(5) 2_656 ?
C19 H19 0.9500 . ?
C73 C72 1.369(7) . ?
C73 H73 0.9500 . ?
C61 H61B 0.9900 . ?
C61 H61A 0.9900 . ?
C65 H65 0.9500 . ?
C72 C71 1.371(7) . ?
C72 H72 0.9500 . ?
C71 H71 0.9500 . ?
O10A C91A 1.308(15) . ?
O10A C94A 1.531(19) . ?
C93A C92A 1.506(19) . ?
C93A C94A 1.52(2) . ?
C93A H93B 0.9900 . ?
C93A H93A 0.9900 . ?
C92A C91A 1.589(19) . ?
C92A H92B 0.9900 . ?
C92A H92A 0.9900 . ?
C94A H94A 0.9900 . ?
C94A H94B 0.9900 . ?
C91A H91B 0.9900 . ?
C91A H91A 0.9900 . ?
O10B C91B 1.355(9) . ?
O10B C94B 1.517(14) . ?
C93B C92B 1.506(13) . ?
C93B C94B 1.531(14) . ?
C93B H93D 0.9900 . ?
C93B H93C 0.9900 . ?
C92B C91B 1.585(12) . ?
C92B H92D 0.9900 . ?
C92B H92C 0.9900 . ?
C94B H94D 0.9900 . ?
C94B H94C 0.9900 . ?
C91B H91D 0.9900 . ?
C91B H91C 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 O3 169.23(9) . . ?
O1 U1 N2 87.11(9) . . ?
O3 U1 N2 97.41(10) . . ?
O1 U1 N3 81.70(9) . . ?
O3 U1 N3 109.00(8) . . ?
N2 U1 N3 71.07(9) . . ?
O1 U1 O4 75.26(9) . . ?
O3 U1 O4 95.63(10) . . ?
N2 U1 O4 143.78(9) . . ?
N3 U1 O4 134.70(9) . . ?
O1 U1 N1 81.27(9) . . ?
O3 U1 N1 91.29(6) . . ?
N2 U1 N1 68.25(9) . . ?
N3 U1 N1 136.41(9) . . ?
O4 U1 N1 77.83(8) . . ?
O1 U1 N4 85.72(9) . . ?
O3 U1 N4 97.41(7) . . ?
N2 U1 N4 136.91(9) . . ?
N3 U1 N4 65.85(9) . . ?
O4 U1 N4 73.91(9) . . ?
N1 U1 N4 151.08(8) . . ?
O1 Si1 C63 111.12(15) . . ?
O1 Si1 C69 110.04(16) . . ?
C63 Si1 C69 107.75(17) . . ?
O1 Si1 H80 109.3(14) . . ?
C63 Si1 H80 109.6(14) . . ?
C69 Si1 H80 108.9(15) . . ?
U1 O3 U1 172.00(17) . 2_656 ?
Si1 O1 U1 154.01(15) . . ?
C59 O4 C62 109.7(3) . . ?
C59 O4 U1 123.6(2) . . ?
C62 O4 U1 126.3(3) . . ?
C1 N1 C55 117.3(3) . . ?
C1 N1 U1 110.3(2) . . ?
C55 N1 U1 126.0(2) . . ?
C11 N3 C14 106.3(3) . . ?
C11 N3 U1 135.6(2) . . ?
C14 N3 U1 112.6(2) . . ?
C15 N4 C16 114.7(3) . . ?
C15 N4 U1 110.6(2) . . ?
C16 N4 U1 133.8(2) . . ?
C5 N2 C2 105.9(3) . . ?
C5 N2 U1 135.9(2) . . ?
C2 N2 U1 113.3(2) . . ?
N3 C11 C12 110.7(3) . . ?
N3 C11 C6 118.8(3) . . ?
C12 C11 C6 130.1(3) . . ?
C57 C29 C49 119.8(3) 2_656 2_656 ?
C57 C29 C16 122.1(3) 2_656 . ?
C49 C29 C16 118.1(3) 2_656 . ?
C54 C55 N1 121.5(3) . . ?
C54 C55 C56 119.4(3) . . ?
N1 C55 C56 119.0(3) . . ?
C29 C57 C56 121.6(3) 2_656 . ?
C29 C57 H57 119.2 2_656 . ?
C56 C57 H57 119.2 . . ?
C17 C16 N4 122.9(3) . . ?
C17 C16 C29 120.4(3) . . ?
N4 C16 C29 116.6(3) . . ?
N1 C1 C2 123.0(3) . . ?
N1 C1 H1 118(2) . . ?
C2 C1 H1 118(2) . . ?
N2 C5 C4 110.5(3) . . ?
N2 C5 C6 121.4(3) . . ?
C4 C5 C6 128.0(3) . . ?
C3 C4 C5 107.0(3) . . ?
C3 C4 H4 126.5 . . ?
C5 C4 H4 126.5 . . ?
C3 C2 N2 109.9(3) . . ?
C3 C2 C1 128.9(3) . . ?
N2 C2 C1 121.0(3) . . ?
N4 C15 C14 121.2(3) . . ?
N4 C15 H15 122(2) . . ?
C14 C15 H15 116(2) . . ?
N3 C14 C15 119.7(3) . . ?
N3 C14 C13 109.8(3) . . ?
C15 C14 C13 130.2(3) . . ?
C55 C54 C53 121.0(3) . . ?
C55 C54 H54 119.5 . . ?
C53 C54 H54 119.5 . . ?
C4 C3 C2 106.8(3) . . ?
C4 C3 H3 126.6 . . ?
C2 C3 H3 126.6 . . ?
C50 C49 C19 122.7(3) . 2_656 ?
C50 C49 C29 118.2(3) . 2_656 ?
C19 C49 C29 119.0(3) 2_656 2_656 ?
C8 C7 C6 113.8(3) . . ?
C8 C7 H7A 108.8 . . ?
C6 C7 H7A 108.8 . . ?
C8 C7 H7B 108.8 . . ?
C6 C7 H7B 108.8 . . ?
H7A C7 H7B 107.7 . . ?
C11 C6 C5 107.9(3) . . ?
C11 C6 C9 110.8(3) . . ?
C5 C6 C9 110.6(3) . . ?
C11 C6 C7 106.0(3) . . ?
C5 C6 C7 111.2(3) . . ?
C9 C6 C7 110.4(3) . . ?
C13 C12 C11 106.6(3) . . ?
C13 C12 H12 126.7 . . ?
C11 C12 H12 126.7 . . ?
C57 C56 C55 121.8(3) . . ?
C57 C56 C51 119.1(3) . . ?
C55 C56 C51 119.1(3) . . ?
C52 C53 C54 121.4(4) . . ?
C52 C53 H53 119.3 . . ?
C54 C53 H53 119.3 . . ?
C65 C64 C63 121.8(4) . . ?
C65 C64 H64 119.1 . . ?
C63 C64 H64 119.1 . . ?
C64 C63 C68 117.1(3) . . ?
C64 C63 Si1 119.9(3) . . ?
C68 C63 Si1 123.0(3) . . ?
C12 C13 C14 106.7(3) . . ?
C12 C13 H13 126.7 . . ?
C14 C13 H13 126.7 . . ?
C50 C51 C52 122.1(3) . . ?
C50 C51 C56 119.0(3) . . ?
C52 C51 C56 118.9(3) . . ?
C16 C17 C18 120.4(4) . . ?
C16 C17 H17 119.8 . . ?
C18 C17 H17 119.8 . . ?
C51 C50 C49 122.2(3) . . ?
C51 C50 H50 118.9 . . ?
C49 C50 H50 118.9 . . ?
C53 C52 C51 120.1(3) . . ?
C53 C52 H52 120.0 . . ?
C51 C52 H52 120.0 . . ?
C10 C9 C6 114.7(3) . . ?
C10 C9 H9A 108.6 . . ?
C6 C9 H9A 108.6 . . ?
C10 C9 H9B 108.6 . . ?
C6 C9 H9B 108.6 . . ?
H9A C9 H9B 107.6 . . ?
O4 C62 C61 104.9(4) . . ?
O4 C62 H62A 110.8 . . ?
C61 C62 H62A 110.8 . . ?
O4 C62 H62B 110.8 . . ?
C61 C62 H62B 110.8 . . ?
H62A C62 H62B 108.9 . . ?
O4 C59 C60 108.1(4) . . ?
O4 C59 H59B 110.1 . . ?
C60 C59 H59B 110.1 . . ?
O4 C59 H59A 110.1 . . ?
C60 C59 H59A 110.1 . . ?
H59B C59 H59A 108.4 . . ?
C74 C69 C70 117.1(4) . . ?
C74 C69 Si1 121.9(3) . . ?
C70 C69 Si1 121.0(3) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C9 C10 H10B 109.5 . . ?
C9 C10 H10A 109.5 . . ?
H10B C10 H10A 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
C19 C18 C17 121.1(4) . . ?
C19 C18 H18 119.4 . . ?
C17 C18 H18 119.4 . . ?
C67 C68 C63 121.3(4) . . ?
C67 C68 H68 119.3 . . ?
C63 C68 H68 119.3 . . ?
C65 C66 C67 119.7(4) . . ?
C65 C66 H66 120.1 . . ?
C67 C66 H66 120.1 . . ?
C59 C60 C61 104.3(4) . . ?
C59 C60 H60B 110.9 . . ?
C61 C60 H60B 110.9 . . ?
C59 C60 H60A 110.9 . . ?
C61 C60 H60A 110.9 . . ?
H60B C60 H60A 108.9 . . ?
C66 C67 C68 120.1(4) . . ?
C66 C67 H67 119.9 . . ?
C68 C67 H67 119.9 . . ?
C69 C74 C73 121.8(4) . . ?
C69 C74 H74 119.1 . . ?
C73 C74 H74 119.1 . . ?
C71 C70 C69 121.6(4) . . ?
C71 C70 H70 119.2 . . ?
C69 C70 H70 119.2 . . ?
C18 C19 C49 120.9(4) . 2_656 ?
C18 C19 H19 119.6 . . ?
C49 C19 H19 119.6 2_656 . ?
C72 C73 C74 119.4(4) . . ?
C72 C73 H73 120.3 . . ?
C74 C73 H73 120.3 . . ?
C60 C61 C62 101.5(4) . . ?
C60 C61 H61B 111.5 . . ?
C62 C61 H61B 111.5 . . ?
C60 C61 H61A 111.5 . . ?
C62 C61 H61A 111.5 . . ?
H61B C61 H61A 109.3 . . ?
C66 C65 C64 119.9(4) . . ?
C66 C65 H65 120.1 . . ?
C64 C65 H65 120.1 . . ?
C73 C72 C71 120.1(5) . . ?
C73 C72 H72 120.0 . . ?
C71 C72 H72 120.0 . . ?
C72 C71 C70 120.0(5) . . ?
C72 C71 H71 120.0 . . ?
C70 C71 H71 120.0 . . ?
C91A O10A C94A 108.7(14) . . ?
C92A C93A C94A 95.6(18) . . ?
C92A C93A H93B 112.6 . . ?
C94A C93A H93B 112.6 . . ?
C92A C93A H93A 112.6 . . ?
C94A C93A H93A 112.6 . . ?
H93B C93A H93A 110.1 . . ?
C93A C92A C91A 91.2(16) . . ?
C93A C92A H92B 113.4 . . ?
C91A C92A H92B 113.4 . . ?
C93A C92A H92A 113.4 . . ?
C91A C92A H92A 113.4 . . ?
H92B C92A H92A 110.7 . . ?
C93A C94A O10A 96.7(17) . . ?
C93A C94A H94A 112.4 . . ?
O10A C94A H94A 112.4 . . ?
C93A C94A H94B 112.4 . . ?
O10A C94A H94B 112.4 . . ?
H94A C94A H94B 110.0 . . ?
O10A C91A C92A 104.5(16) . . ?
O10A C91A H91B 110.9 . . ?
C92A C91A H91B 110.9 . . ?
O10A C91A H91A 110.9 . . ?
C92A C91A H91A 110.9 . . ?
H91B C91A H91A 108.9 . . ?
C91B O10B C94B 106.0(7) . . ?
C92B C93B C94B 97.8(10) . . ?
C92B C93B H93D 112.2 . . ?
C94B C93B H93D 112.2 . . ?
C92B C93B H93C 112.2 . . ?
C94B C93B H93C 112.2 . . ?
H93D C93B H93C 109.8 . . ?
C93B C92B C91B 92.8(9) . . ?
C93B C92B H92D 113.1 . . ?
C91B C92B H92D 113.1 . . ?
C93B C92B H92C 113.1 . . ?
C91B C92B H92C 113.1 . . ?
H92D C92B H92C 110.5 . . ?
O10B C94B C93B 89.3(10) . . ?
O10B C94B H94D 113.8 . . ?
C93B C94B H94D 113.8 . . ?
O10B C94B H94C 113.8 . . ?
C93B C94B H94C 113.8 . . ?
H94D C94B H94C 111.0 . . ?
O10B C91B C92B 107.1(7) . . ?
O10B C91B H91D 110.3 . . ?
C92B C91B H91D 110.3 . . ?
O10B C91B H91C 110.3 . . ?
C92B C91B H91C 110.3 . . ?
H91D C91B H91C 108.6 . . ?

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
C63 Si1 O1 U1 -104.3(3) . . . . ?
C69 Si1 O1 U1 136.5(3) . . . . ?
O3 U1 O1 Si1 136.5(4) . . . . ?
N2 U1 O1 Si1 21.3(3) . . . . ?
N3 U1 O1 Si1 -50.0(3) . . . . ?
O4 U1 O1 Si1 169.3(4) . . . . ?
N1 U1 O1 Si1 89.7(3) . . . . ?
N4 U1 O1 Si1 -116.2(3) . . . . ?
O1 U1 O4 C59 -9.0(3) . . . . ?
O3 U1 O4 C59 165.2(3) . . . . ?
N2 U1 O4 C59 54.5(3) . . . . ?
N3 U1 O4 C59 -70.9(3) . . . . ?
N1 U1 O4 C59 75.1(3) . . . . ?
N4 U1 O4 C59 -98.7(3) . . . . ?
O1 U1 O4 C62 163.5(3) . . . . ?
O3 U1 O4 C62 -22.3(3) . . . . ?
N2 U1 O4 C62 -133.0(3) . . . . ?
N3 U1 O4 C62 101.6(3) . . . . ?
N1 U1 O4 C62 -112.4(3) . . . . ?
N4 U1 O4 C62 73.8(3) . . . . ?
O1 U1 N1 C1 -74.1(2) . . . . ?
O3 U1 N1 C1 113.7(2) . . . . ?
N2 U1 N1 C1 16.3(2) . . . . ?
N3 U1 N1 C1 -6.0(3) . . . . ?
O4 U1 N1 C1 -150.8(2) . . . . ?
N4 U1 N1 C1 -138.4(2) . . . . ?
O1 U1 N1 C55 76.7(3) . . . . ?
O3 U1 N1 C55 -95.5(3) . . . . ?
N2 U1 N1 C55 167.0(3) . . . . ?
N3 U1 N1 C55 144.8(2) . . . . ?
O4 U1 N1 C55 0.0(3) . . . . ?
N4 U1 N1 C55 12.4(4) . . . . ?
O1 U1 N3 C11 86.4(3) . . . . ?
O3 U1 N3 C11 -94.8(3) . . . . ?
N2 U1 N3 C11 -3.4(3) . . . . ?
O4 U1 N3 C11 146.0(3) . . . . ?
N1 U1 N3 C11 18.5(4) . . . . ?
N4 U1 N3 C11 175.4(4) . . . . ?
O1 U1 N3 C14 -63.0(2) . . . . ?
O3 U1 N3 C14 115.7(2) . . . . ?
N2 U1 N3 C14 -152.8(2) . . . . ?
O4 U1 N3 C14 -3.4(3) . . . . ?
N1 U1 N3 C14 -131.0(2) . . . . ?
N4 U1 N3 C14 26.0(2) . . . . ?
O1 U1 N4 C15 58.9(2) . . . . ?
O3 U1 N4 C15 -131.5(2) . . . . ?
N2 U1 N4 C15 -22.3(3) . . . . ?
N3 U1 N4 C15 -23.9(2) . . . . ?
O4 U1 N4 C15 134.8(2) . . . . ?
N1 U1 N4 C15 122.1(2) . . . . ?
O1 U1 N4 C16 -109.1(3) . . . . ?
O3 U1 N4 C16 60.5(3) . . . . ?
N2 U1 N4 C16 169.7(3) . . . . ?
N3 U1 N4 C16 168.1(3) . . . . ?
O4 U1 N4 C16 -33.2(3) . . . . ?
N1 U1 N4 C16 -45.9(4) . . . . ?
O1 U1 N2 C5 -85.2(3) . . . . ?
O3 U1 N2 C5 104.6(3) . . . . ?
N3 U1 N2 C5 -3.0(3) . . . . ?
O4 U1 N2 C5 -145.2(3) . . . . ?
N1 U1 N2 C5 -167.0(3) . . . . ?
N4 U1 N2 C5 -4.6(4) . . . . ?
O1 U1 N2 C2 65.6(2) . . . . ?
O3 U1 N2 C2 -104.6(2) . . . . ?
N3 U1 N2 C2 147.8(2) . . . . ?
O4 U1 N2 C2 5.6(3) . . . . ?
N1 U1 N2 C2 -16.2(2) . . . . ?
N4 U1 N2 C2 146.2(2) . . . . ?
C14 N3 C11 C12 0.9(4) . . . . ?
U1 N3 C11 C12 -149.8(3) . . . . ?
C14 N3 C11 C6 -172.2(3) . . . . ?
U1 N3 C11 C6 37.1(5) . . . . ?
C1 N1 C55 C54 44.3(5) . . . . ?
U1 N1 C55 C54 -104.7(3) . . . . ?
C1 N1 C55 C56 -139.8(3) . . . . ?
U1 N1 C55 C56 71.2(4) . . . . ?
C15 N4 C16 C17 -62.9(5) . . . . ?
U1 N4 C16 C17 104.7(4) . . . . ?
C15 N4 C16 C29 112.9(4) . . . . ?
U1 N4 C16 C29 -79.4(4) . . . . ?
C57 C29 C16 C17 -179.9(3) 2_656 . . . ?
C49 C29 C16 C17 3.0(5) 2_656 . . . ?
C57 C29 C16 N4 4.2(5) 2_656 . . . ?
C49 C29 C16 N4 -172.9(3) 2_656 . . . ?
C55 N1 C1 C2 -168.9(3) . . . . ?
U1 N1 C1 C2 -15.3(4) . . . . ?
C2 N2 C5 C4 -0.5(4) . . . . ?
U1 N2 C5 C4 151.7(3) . . . . ?
C2 N2 C5 C6 -177.1(3) . . . . ?
U1 N2 C5 C6 -24.9(5) . . . . ?
N2 C5 C4 C3 0.6(4) . . . . ?
C6 C5 C4 C3 176.9(3) . . . . ?
C5 N2 C2 C3 0.3(4) . . . . ?
U1 N2 C2 C3 -159.1(2) . . . . ?
C5 N2 C2 C1 175.7(3) . . . . ?
U1 N2 C2 C1 16.4(4) . . . . ?
N1 C1 C2 C3 174.7(4) . . . . ?
N1 C1 C2 N2 0.2(5) . . . . ?
C16 N4 C15 C14 -169.7(3) . . . . ?
U1 N4 C15 C14 19.8(4) . . . . ?
C11 N3 C14 C15 173.0(3) . . . . ?
U1 N3 C14 C15 -28.7(4) . . . . ?
C11 N3 C14 C13 -0.4(4) . . . . ?
U1 N3 C14 C13 157.9(2) . . . . ?
N4 C15 C14 N3 4.9(5) . . . . ?
N4 C15 C14 C13 176.8(4) . . . . ?
N1 C55 C54 C53 172.9(3) . . . . ?
C56 C55 C54 C53 -2.9(5) . . . . ?
C5 C4 C3 C2 -0.4(4) . . . . ?
N2 C2 C3 C4 0.1(4) . . . . ?
C1 C2 C3 C4 -174.9(4) . . . . ?
N3 C11 C6 C5 -62.2(4) . . . . ?
C12 C11 C6 C5 126.3(4) . . . . ?
N3 C11 C6 C9 176.7(3) . . . . ?
C12 C11 C6 C9 5.1(5) . . . . ?
N3 C11 C6 C7 57.0(4) . . . . ?
C12 C11 C6 C7 -114.6(4) . . . . ?
N2 C5 C6 C11 57.0(4) . . . . ?
C4 C5 C6 C11 -119.0(4) . . . . ?
N2 C5 C6 C9 178.3(3) . . . . ?
C4 C5 C6 C9 2.3(5) . . . . ?
N2 C5 C6 C7 -58.8(4) . . . . ?
C4 C5 C6 C7 125.2(4) . . . . ?
C8 C7 C6 C11 52.8(4) . . . . ?
C8 C7 C6 C5 169.8(3) . . . . ?
C8 C7 C6 C9 -67.2(4) . . . . ?
N3 C11 C12 C13 -1.1(4) . . . . ?
C6 C11 C12 C13 171.0(4) . . . . ?
C29 C57 C56 C55 179.9(3) 2_656 . . . ?
C29 C57 C56 C51 2.0(5) 2_656 . . . ?
C54 C55 C56 C57 -173.0(3) . . . . ?
N1 C55 C56 C57 11.1(5) . . . . ?
C54 C55 C56 C51 4.9(5) . . . . ?
N1 C55 C56 C51 -171.0(3) . . . . ?
C55 C54 C53 C52 -1.2(6) . . . . ?
C65 C64 C63 C68 1.3(6) . . . . ?
C65 C64 C63 Si1 -175.6(3) . . . . ?
O1 Si1 C63 C64 92.5(3) . . . . ?
C69 Si1 C63 C64 -146.9(3) . . . . ?
O1 Si1 C63 C68 -84.2(3) . . . . ?
C69 Si1 C63 C68 36.4(4) . . . . ?
C11 C12 C13 C14 0.8(4) . . . . ?
N3 C14 C13 C12 -0.3(4) . . . . ?
C15 C14 C13 C12 -172.8(4) . . . . ?
C57 C56 C51 C50 -3.6(5) . . . . ?
C55 C56 C51 C50 178.5(3) . . . . ?
C57 C56 C51 C52 175.1(3) . . . . ?
C55 C56 C51 C52 -2.8(5) . . . . ?
N4 C16 C17 C18 174.6(3) . . . . ?
C29 C16 C17 C18 -1.1(6) . . . . ?
C52 C51 C50 C49 -177.0(4) . . . . ?
C56 C51 C50 C49 1.6(6) . . . . ?
C19 C49 C50 C51 177.8(4) 2_656 . . . ?
C29 C49 C50 C51 1.8(5) 2_656 . . . ?
C54 C53 C52 C51 3.3(6) . . . . ?
C50 C51 C52 C53 177.4(4) . . . . ?
C56 C51 C52 C53 -1.2(5) . . . . ?
C11 C6 C9 C10 -170.1(3) . . . . ?
C5 C6 C9 C10 70.3(4) . . . . ?
C7 C6 C9 C10 -53.1(4) . . . . ?
C59 O4 C62 C61 10.0(4) . . . . ?
U1 O4 C62 C61 -163.3(3) . . . . ?
C62 O4 C59 C60 11.5(4) . . . . ?
U1 O4 C59 C60 -174.9(2) . . . . ?
O1 Si1 C69 C74 -15.0(4) . . . . ?
C63 Si1 C69 C74 -136.3(4) . . . . ?
O1 Si1 C69 C70 166.8(4) . . . . ?
C63 Si1 C69 C70 45.5(4) . . . . ?
C16 C17 C18 C19 -1.6(6) . . . . ?
C64 C63 C68 C67 -1.0(6) . . . . ?
Si1 C63 C68 C67 175.8(3) . . . . ?
O4 C59 C60 C61 -29.4(5) . . . . ?
C65 C66 C67 C68 2.2(7) . . . . ?
C63 C68 C67 C66 -0.7(7) . . . . ?
C70 C69 C74 C73 -0.7(7) . . . . ?
Si1 C69 C74 C73 -179.0(4) . . . . ?
C74 C69 C70 C71 0.1(8) . . . . ?
Si1 C69 C70 C71 178.3(5) . . . . ?
C17 C18 C19 C49 2.3(6) . . . 2_656 ?
C69 C74 C73 C72 1.0(8) . . . . ?
C59 C60 C61 C62 33.4(5) . . . . ?
O4 C62 C61 C60 -27.0(5) . . . . ?
C67 C66 C65 C64 -1.9(7) . . . . ?
C63 C64 C65 C66 0.1(6) . . . . ?
C74 C73 C72 C71 -0.6(8) . . . . ?
C73 C72 C71 C70 -0.1(9) . . . . ?
C69 C70 C71 C72 0.3(9) . . . . ?
C94A C93A C92A C91A -61(3) . . . . ?
C92A C93A C94A O10A 54(3) . . . . ?
C91A O10A C94A C93A -22(3) . . . . ?
C94A O10A C91A C92A -17(3) . . . . ?
C93A C92A C91A O10A 50(2) . . . . ?
C94B C93B C92B C91B 55.3(15) . . . . ?
C91B O10B C94B C93B 50.5(13) . . . . ?
C92B C93B C94B O10B -65.7(14) . . . . ?
C94B O10B C91B C92B -18.0(14) . . . . ?
C93B C92B C91B O10B -23.3(15) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        26.37
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.257
_refine_diff_density_min         -0.576
_refine_diff_density_rms         0.095

# start Validation Reply Form
_vrf_PLAT411_5THF_THF            
;
PROBLEM: Short Inter H...H Contact H73      ..H94A      .       1.95 Ang.  
RESPONSE: This has been noted and is not serious.
;
####################################################################### 
# 
# 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_5py_py
_database_code_depnum_ccdc_archive 'CCDC 1812765'
_audit_update_record             
;
2017-12-20 deposited with the CCDC.
2018-03-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        '[{HPh2SiO(py)UOU(py)OSiPh2H}(LA)]'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C92 H80 N10 O3 Si2 U2, C5 H5 N'
_chemical_formula_sum            'C97 H85 N11 O3 Si2 U2'
_chemical_formula_weight         1985.00

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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   23.8381(5)
_cell_length_b                   17.7807(2)
_cell_length_c                   21.4711(4)
_cell_angle_alpha                90
_cell_angle_beta                 114.099(2)
_cell_angle_gamma                90
_cell_volume                     8307.5(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    19902
_cell_measurement_theta_min      3.3510
_cell_measurement_theta_max      26.7760

_exptl_crystal_description       block
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.587
_exptl_crystal_F_000             3920
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.198
_exptl_crystal_size_mid          0.085
_exptl_crystal_size_min          0.062
_exptl_absorpt_coefficient_mu    3.982
_shelx_estimated_absorpt_T_min   0.506
_shelx_estimated_absorpt_T_max   0.790
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.850
_exptl_absorpt_correction_T_max  0.947
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Eos
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 16.1042
_diffrn_reflns_number            125163
_diffrn_reflns_av_unetI/netI     0.0353
_diffrn_reflns_av_R_equivalents  0.0977
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         2.958
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             8502
_reflns_number_gt                7300
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_refine_special_details          
;
Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.

A molecule of pyridine within the asymmetric unit was refined with
0.5 occupancy, leaving one molecule of pyridine per molecule of 
[{Ph2HSiOU(py)OU(py)OSiHPh2}(LA)].
;

_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8502
_refine_ls_number_parameters     540
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0406
_refine_ls_R_factor_gt           0.0302
_refine_ls_wR_factor_ref         0.0994
_refine_ls_wR_factor_gt          0.0907
_refine_ls_goodness_of_fit_ref   0.766
_refine_ls_restrained_S_all      0.766
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.40543(2) 0.46455(2) 0.73521(2) 0.01359(7) Uani 1 1 d . . . . .
Si1 Si 0.24860(6) 0.42793(7) 0.71019(6) 0.0203(3) Uani 1 1 d . . . . .
O3 O 0.500000 0.4717(2) 0.750000 0.0154(9) Uani 1 2 d S T P . .
O1 O 0.31371(15) 0.47084(15) 0.72901(17) 0.0212(7) Uani 1 1 d . . . . .
N6 N 0.59165(15) 0.33813(19) 0.71750(16) 0.0164(7) Uani 1 1 d . . . . .
N1 N 0.36183(18) 0.52931(18) 0.61648(19) 0.0188(8) Uani 1 1 d . . . . .
N5 N 0.56710(17) 0.46786(18) 0.63572(18) 0.0164(7) Uani 1 1 d . . . . .
N2 N 0.35487(17) 0.37606(19) 0.64096(17) 0.0187(7) Uani 1 1 d . . . . .
N9 N 0.38930(17) 0.6085(2) 0.75424(18) 0.0216(8) Uani 1 1 d . . . . .
C40 C 0.60517(19) 0.2665(2) 0.7404(2) 0.0167(8) Uani 1 1 d . . . . .
C35 C 0.6245(2) 0.2442(2) 0.8149(2) 0.0196(9) Uani 1 1 d . . . . .
C44 C 0.56765(19) 0.4024(2) 0.6095(2) 0.0195(9) Uani 1 1 d . . . . .
H44 H 0.561652 0.399357 0.563028 0.023 Uiso 1 1 calc R U . . .
C45 C 0.5680(2) 0.5340(2) 0.5990(2) 0.0204(9) Uani 1 1 d . . . . .
C56 C 0.42244(19) 0.6239(2) 0.5893(2) 0.0180(8) Uani 1 1 d . . . . .
C55 C 0.3672(2) 0.6044(2) 0.5966(2) 0.0208(9) Uani 1 1 d . . . . .
C1 C 0.3185(2) 0.4890(3) 0.5728(2) 0.0224(9) Uani 1 1 d . . . . .
H1A H 0.290462 0.511943 0.532009 0.027 Uiso 1 1 calc R U . . .
C59 C 0.3421(2) 0.6373(3) 0.7633(3) 0.0299(11) Uani 1 1 d . . . . .
H59 H 0.313842 0.604149 0.770112 0.036 Uiso 1 1 calc R U . . .
C43 C 0.57686(19) 0.3355(2) 0.6477(2) 0.0170(8) Uani 1 1 d . . . . .
C57 C 0.46837(19) 0.5708(2) 0.5987(2) 0.0172(8) Uani 1 1 d . . . . .
H57 H 0.463752 0.521326 0.612702 0.021 Uiso 1 1 calc R U . . .
C5 C 0.33623(19) 0.3037(2) 0.6365(2) 0.0182(8) Uani 1 1 d . . . . .
C58 C 0.5206(2) 0.5884(2) 0.5883(2) 0.0179(9) Uani 1 1 d . . . . .
C36 C 0.5659(2) 0.2345(2) 0.8286(2) 0.0211(9) Uani 1 1 d . . . . .
H36A H 0.542515 0.282308 0.817300 0.025 Uiso 1 1 calc R U . . .
H36B H 0.539674 0.195403 0.797414 0.025 Uiso 1 1 calc R U . . .
C4 C 0.2818(2) 0.2926(2) 0.5767(2) 0.0241(10) Uani 1 1 d . . . . .
H4 H 0.259802 0.246916 0.561722 0.029 Uiso 1 1 calc R U . . .
C54 C 0.3225(2) 0.6573(3) 0.5858(2) 0.0268(10) Uani 1 1 d . . . . .
H54 H 0.285569 0.643903 0.589897 0.032 Uiso 1 1 calc R U . . .
C42 C 0.5808(2) 0.2617(2) 0.6279(2) 0.0220(9) Uani 1 1 d . . . . .
H42 H 0.573153 0.244822 0.583150 0.026 Uiso 1 1 calc R U . . .
C39 C 0.7170(2) 0.1641(3) 0.8153(2) 0.0275(10) Uani 1 1 d . . . . .
H39A H 0.705888 0.169488 0.766284 0.041 Uiso 1 1 calc R U . . .
H39B H 0.737286 0.115544 0.830987 0.041 Uiso 1 1 calc R U . . .
H39C H 0.745011 0.204808 0.839946 0.041 Uiso 1 1 calc R U . . .
C46 C 0.6144(2) 0.5498(3) 0.5790(2) 0.0254(10) Uani 1 1 d . . . . .
H46 H 0.644255 0.512456 0.583223 0.030 Uiso 1 1 calc R U . . .
C63 C 0.4271(3) 0.6563(3) 0.7450(3) 0.0442(14) Uani 1 1 d . . . . .
H63 H 0.460908 0.636422 0.737765 0.053 Uiso 1 1 calc R U . . .
C2 C 0.3116(2) 0.4121(2) 0.5835(2) 0.0187(9) Uani 1 1 d . . . . .
C3 C 0.2673(2) 0.3616(3) 0.5446(2) 0.0251(10) Uani 1 1 d . . . . .
H3 H 0.233056 0.372292 0.503095 0.030 Uiso 1 1 calc R U . . .
C49 C 0.5275(2) 0.6632(2) 0.5658(2) 0.0224(9) Uani 1 1 d . . . . .
C41 C 0.5981(2) 0.2180(2) 0.6859(2) 0.0235(9) Uani 1 1 d . . . . .
H41 H 0.604060 0.165030 0.688564 0.028 Uiso 1 1 calc R U . . .
C51 C 0.4301(2) 0.6995(2) 0.5699(2) 0.0212(9) Uani 1 1 d . . . . .
C48 C 0.5781(2) 0.6763(3) 0.5476(2) 0.0275(10) Uani 1 1 d . . . . .
H48 H 0.583401 0.724813 0.532190 0.033 Uiso 1 1 calc R U . . .
C50 C 0.4821(2) 0.7166(2) 0.5583(2) 0.0231(10) Uani 1 1 d . . . . .
H50 H 0.486823 0.766217 0.544890 0.028 Uiso 1 1 calc R U . . .
C68 C 0.2575(2) 0.3872(3) 0.9033(3) 0.0343(12) Uani 1 1 d . . . . .
H68 H 0.284924 0.360943 0.942409 0.041 Uiso 1 1 calc R U . . .
C70 C 0.1855(2) 0.4739(3) 0.6362(3) 0.0301(11) Uani 1 1 d . . . . .
C69 C 0.2677(2) 0.3887(3) 0.8440(2) 0.0293(10) Uani 1 1 d . . . . .
H69 H 0.301821 0.362091 0.842808 0.035 Uiso 1 1 calc R U . . .
C65 C 0.1795(2) 0.4665(2) 0.7903(3) 0.0259(10) Uani 1 1 d . . . . .
H65 H 0.152918 0.495068 0.752261 0.031 Uiso 1 1 calc R U . . .
C38 C 0.6592(2) 0.1681(2) 0.8289(2) 0.0215(9) Uani 1 1 d . . . . .
H38A H 0.670586 0.154713 0.877350 0.026 Uiso 1 1 calc R U . . .
H38B H 0.630319 0.129087 0.800805 0.026 Uiso 1 1 calc R U . . .
C52 C 0.3831(2) 0.7533(3) 0.5613(2) 0.0293(11) Uani 1 1 d . . . . .
H52 H 0.388045 0.804026 0.550577 0.035 Uiso 1 1 calc R U . . .
C71 C 0.1830(3) 0.5512(3) 0.6270(3) 0.0400(13) Uani 1 1 d . . . . .
H71 H 0.213979 0.581697 0.659346 0.048 Uiso 1 1 calc R U . . .
C47 C 0.6182(2) 0.6216(3) 0.5518(2) 0.0286(10) Uani 1 1 d . . . . .
H47 H 0.649720 0.631029 0.536464 0.034 Uiso 1 1 calc R U . . .
C64 C 0.2296(2) 0.4279(2) 0.7868(2) 0.0227(9) Uani 1 1 d . . . . .
C60 C 0.3324(3) 0.7140(3) 0.7632(3) 0.0457(15) Uani 1 1 d . . . . .
H60 H 0.297881 0.732812 0.769576 0.055 Uiso 1 1 calc R U . . .
C53 C 0.3312(2) 0.7322(3) 0.5683(2) 0.0325(12) Uani 1 1 d . . . . .
H53 H 0.299959 0.768493 0.561425 0.039 Uiso 1 1 calc R U . . .
C61 C 0.3726(3) 0.7624(3) 0.7538(3) 0.0361(12) Uani 1 1 d . . . . .
H61 H 0.366629 0.815254 0.753486 0.043 Uiso 1 1 calc R U . . .
C66 C 0.1687(3) 0.4632(3) 0.8486(3) 0.0332(13) Uani 1 1 d . . . . .
H66 H 0.133997 0.488515 0.849671 0.040 Uiso 1 1 calc R U . . .
C37 C 0.5778(2) 0.2127(3) 0.9020(2) 0.0358(12) Uani 1 1 d . . . . .
H37A H 0.596194 0.162435 0.911984 0.054 Uiso 1 1 calc R U . . .
H37B H 0.538870 0.212577 0.907351 0.054 Uiso 1 1 calc R U . . .
H37C H 0.605946 0.249159 0.933718 0.054 Uiso 1 1 calc R U . . .
C67 C 0.2069(2) 0.4244(3) 0.9049(2) 0.0336(12) Uani 1 1 d . . . . .
H67 H 0.198883 0.422818 0.944726 0.040 Uiso 1 1 calc R U . . .
C74 C 0.0932(4) 0.4651(5) 0.5306(4) 0.073(3) Uani 1 1 d . . . . .
H74 H 0.062866 0.435237 0.496774 0.088 Uiso 1 1 calc R U . . .
C75 C 0.1394(3) 0.4317(4) 0.5869(3) 0.0504(16) Uani 1 1 d . . . . .
H75 H 0.139385 0.378575 0.591880 0.060 Uiso 1 1 calc R U . . .
C73 C 0.0922(4) 0.5428(5) 0.5247(4) 0.072(3) Uani 1 1 d . . . . .
H73 H 0.060259 0.566259 0.487127 0.087 Uiso 1 1 calc R U . . .
C62 C 0.4211(3) 0.7329(3) 0.7451(3) 0.0464(15) Uani 1 1 d . . . . .
H62 H 0.450552 0.764765 0.739190 0.056 Uiso 1 1 calc R U . . .
C72 C 0.1361(3) 0.5856(4) 0.5718(3) 0.0534(17) Uani 1 1 d . . . . .
H72 H 0.135065 0.638757 0.567170 0.064 Uiso 1 1 calc R U . . .
C103 C 0.5023(5) 1.0277(3) 0.7385(5) 0.037(4) Uani 0.5 1 d G . P A -1
H103 H 0.507462 1.067403 0.711624 0.045 Uiso 0.5 1 calc R U P A -1
C102 C 0.4892(4) 1.0440(3) 0.7944(5) 0.039(3) Uani 0.5 1 d G . P A -1
H102 H 0.485344 1.094745 0.805819 0.047 Uiso 0.5 1 calc R U P A -1
C101 C 0.4817(4) 0.9859(4) 0.8337(4) 0.040(3) Uani 0.5 1 d G . P A -1
H101 H 0.472713 0.996974 0.871911 0.048 Uiso 0.5 1 calc R U P A -1
C100 C 0.4873(5) 0.9116(3) 0.8170(5) 0.054(4) Uani 0.5 1 d G . P A -1
H100 H 0.482199 0.871860 0.843808 0.065 Uiso 0.5 1 calc R U P A -1
N100 N 0.5005(6) 0.8953(3) 0.7610(5) 0.052(3) Uani 0.5 1 d G . P A -1
C104 C 0.5080(6) 0.9534(4) 0.7218(5) 0.051(3) Uani 0.5 1 d G . P A -1
H104 H 0.516948 0.942287 0.683520 0.061 Uiso 0.5 1 calc R U P A -1
H80 H 0.248(2) 0.354(3) 0.692(3) 0.040(15) Uiso 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 O1 2.138(3) . ?
U1 O3 2.1482(3) . ?
U1 N2 2.456(3) . ?
U1 N6 2.456(3) 2_656 ?
U1 N5 2.575(3) 2_656 ?
U1 N1 2.596(4) . ?
U1 N9 2.644(4) . ?
Si1 O1 1.626(3) . ?
Si1 C70 1.872(5) . ?
Si1 C64 1.877(5) . ?
Si1 H80 1.37(5) . ?
N6 C40 1.356(5) . ?
N6 C43 1.393(5) . ?
N1 C1 1.292(6) . ?
N1 C55 1.424(5) . ?
N5 C44 1.295(5) . ?
N5 C45 1.421(5) . ?
N2 C5 1.351(5) . ?
N2 C2 1.398(5) . ?
N9 C63 1.311(7) . ?
N9 C59 1.320(6) . ?
C40 C41 1.406(6) . ?
C40 C35 1.525(6) . ?
C35 C5 1.513(6) 2_656 ?
C35 C38 1.551(6) . ?
C35 C36 1.552(6) . ?
C44 C43 1.411(6) . ?
C44 H44 0.9500 . ?
C45 C46 1.370(7) . ?
C45 C58 1.433(6) . ?
C56 C57 1.397(6) . ?
C56 C55 1.431(6) . ?
C56 C51 1.440(6) . ?
C55 C54 1.368(6) . ?
C1 C2 1.407(6) . ?
C1 H1A 0.9500 . ?
C59 C60 1.383(7) . ?
C59 H59 0.9500 . ?
C43 C42 1.394(6) . ?
C57 C58 1.388(6) . ?
C57 H57 0.9500 . ?
C5 C4 1.417(6) . ?
C58 C49 1.447(6) . ?
C36 C37 1.534(6) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C4 C3 1.379(6) . ?
C4 H4 0.9500 . ?
C54 C53 1.423(6) . ?
C54 H54 0.9500 . ?
C42 C41 1.382(6) . ?
C42 H42 0.9500 . ?
C39 C38 1.522(6) . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C46 C47 1.423(6) . ?
C46 H46 0.9500 . ?
C63 C62 1.371(8) . ?
C63 H63 0.9500 . ?
C2 C3 1.378(6) . ?
C3 H3 0.9500 . ?
C49 C50 1.399(6) . ?
C49 C48 1.430(6) . ?
C41 H41 0.9500 . ?
C51 C50 1.393(7) . ?
C51 C52 1.428(6) . ?
C48 C47 1.341(7) . ?
C48 H48 0.9500 . ?
C50 H50 0.9500 . ?
C68 C67 1.388(8) . ?
C68 C69 1.391(7) . ?
C68 H68 0.9500 . ?
C70 C71 1.387(7) . ?
C70 C75 1.394(8) . ?
C69 C64 1.381(7) . ?
C69 H69 0.9500 . ?
C65 C66 1.378(7) . ?
C65 C64 1.406(7) . ?
C65 H65 0.9500 . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C52 C53 1.358(7) . ?
C52 H52 0.9500 . ?
C71 C72 1.395(7) . ?
C71 H71 0.9500 . ?
C47 H47 0.9500 . ?
C60 C61 1.361(7) . ?
C60 H60 0.9500 . ?
C53 H53 0.9500 . ?
C61 C62 1.351(8) . ?
C61 H61 0.9500 . ?
C66 C67 1.367(8) . ?
C66 H66 0.9500 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C67 H67 0.9500 . ?
C74 C73 1.385(10) . ?
C74 C75 1.394(10) . ?
C74 H74 0.9500 . ?
C75 H75 0.9500 . ?
C73 C72 1.355(11) . ?
C73 H73 0.9500 . ?
C62 H62 0.9500 . ?
C72 H72 0.9500 . ?
C103 C102 1.3900 . ?
C103 C104 1.3900 . ?
C103 H103 0.9500 . ?
C102 C101 1.3900 . ?
C102 H102 0.9500 . ?
C101 C100 1.3900 . ?
C101 H101 0.9500 . ?
C100 N100 1.3900 . ?
C100 H100 0.9500 . ?
N100 C104 1.3900 . ?
C104 H104 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 U1 O3 172.19(12) . . ?
O1 U1 N2 80.62(12) . . ?
O3 U1 N2 106.97(11) . . ?
O1 U1 N6 85.94(11) . 2_656 ?
O3 U1 N6 98.17(12) . 2_656 ?
N2 U1 N6 71.08(11) . 2_656 ?
O1 U1 N5 82.53(12) . 2_656 ?
O3 U1 N5 92.82(8) . 2_656 ?
N2 U1 N5 136.47(11) . 2_656 ?
N6 U1 N5 67.92(10) 2_656 2_656 ?
O1 U1 N1 85.79(12) . . ?
O3 U1 N1 95.40(10) . . ?
N2 U1 N1 67.05(11) . . ?
N6 U1 N1 138.10(11) 2_656 . ?
N5 U1 N1 150.52(10) 2_656 . ?
O1 U1 N9 75.49(11) . . ?
O3 U1 N9 97.47(13) . . ?
N2 U1 N9 133.94(11) . . ?
N6 U1 N9 143.45(11) 2_656 . ?
N5 U1 N9 78.50(11) 2_656 . ?
N1 U1 N9 72.38(11) . . ?
O1 Si1 C70 111.1(2) . . ?
O1 Si1 C64 109.28(18) . . ?
C70 Si1 C64 110.3(2) . . ?
O1 Si1 H80 115(2) . . ?
C70 Si1 H80 105(2) . . ?
C64 Si1 H80 105(2) . . ?
U1 O3 U1 173.2(2) . 2_656 ?
Si1 O1 U1 147.05(18) . . ?
C40 N6 C43 106.0(3) . . ?
C40 N6 U1 138.4(3) . 2_656 ?
C43 N6 U1 115.3(3) . 2_656 ?
C1 N1 C55 116.4(4) . . ?
C1 N1 U1 110.4(3) . . ?
C55 N1 U1 131.5(3) . . ?
C44 N5 C45 119.9(4) . . ?
C44 N5 U1 113.8(3) . 2_656 ?
C45 N5 U1 124.1(3) . 2_656 ?
C5 N2 C2 105.7(3) . . ?
C5 N2 U1 134.8(3) . . ?
C2 N2 U1 111.7(3) . . ?
C63 N9 C59 116.7(4) . . ?
C63 N9 U1 116.9(3) . . ?
C59 N9 U1 125.7(3) . . ?
N6 C40 C41 110.2(4) . . ?
N6 C40 C35 123.3(4) . . ?
C41 C40 C35 126.5(4) . . ?
C5 C35 C40 112.3(3) 2_656 . ?
C5 C35 C38 110.2(3) 2_656 . ?
C40 C35 C38 109.8(3) . . ?
C5 C35 C36 107.3(3) 2_656 . ?
C40 C35 C36 108.5(3) . . ?
C38 C35 C36 108.4(3) . . ?
N5 C44 C43 122.1(4) . . ?
N5 C44 H44 118.9 . . ?
C43 C44 H44 118.9 . . ?
C46 C45 N5 122.7(4) . . ?
C46 C45 C58 119.7(4) . . ?
N5 C45 C58 117.3(4) . . ?
C57 C56 C55 121.4(4) . . ?
C57 C56 C51 119.3(4) . . ?
C55 C56 C51 119.3(4) . . ?
C54 C55 N1 122.4(4) . . ?
C54 C55 C56 120.2(4) . . ?
N1 C55 C56 117.4(4) . . ?
N1 C1 C2 122.2(4) . . ?
N1 C1 H1A 118.9 . . ?
C2 C1 H1A 118.9 . . ?
N9 C59 C60 122.2(5) . . ?
N9 C59 H59 118.9 . . ?
C60 C59 H59 118.9 . . ?
N6 C43 C42 110.0(3) . . ?
N6 C43 C44 120.5(4) . . ?
C42 C43 C44 129.0(4) . . ?
C58 C57 C56 121.7(4) . . ?
C58 C57 H57 119.2 . . ?
C56 C57 H57 119.2 . . ?
N2 C5 C4 110.5(4) . . ?
N2 C5 C35 121.6(4) . 2_656 ?
C4 C5 C35 127.4(4) . 2_656 ?
C57 C58 C45 121.4(4) . . ?
C57 C58 C49 119.6(4) . . ?
C45 C58 C49 119.0(4) . . ?
C37 C36 C35 114.8(4) . . ?
C37 C36 H36A 108.6 . . ?
C35 C36 H36A 108.6 . . ?
C37 C36 H36B 108.6 . . ?
C35 C36 H36B 108.6 . . ?
H36A C36 H36B 107.5 . . ?
C3 C4 C5 106.2(4) . . ?
C3 C4 H4 126.9 . . ?
C5 C4 H4 126.9 . . ?
C55 C54 C53 120.1(5) . . ?
C55 C54 H54 120.0 . . ?
C53 C54 H54 120.0 . . ?
C41 C42 C43 106.7(4) . . ?
C41 C42 H42 126.7 . . ?
C43 C42 H42 126.7 . . ?
C38 C39 H39A 109.5 . . ?
C38 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C38 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C45 C46 C47 120.5(4) . . ?
C45 C46 H46 119.7 . . ?
C47 C46 H46 119.7 . . ?
N9 C63 C62 124.5(5) . . ?
N9 C63 H63 117.7 . . ?
C62 C63 H63 117.7 . . ?
C3 C2 N2 110.1(4) . . ?
C3 C2 C1 130.2(4) . . ?
N2 C2 C1 119.8(4) . . ?
C2 C3 C4 107.6(4) . . ?
C2 C3 H3 126.2 . . ?
C4 C3 H3 126.2 . . ?
C50 C49 C48 124.0(4) . . ?
C50 C49 C58 118.2(4) . . ?
C48 C49 C58 117.7(4) . . ?
C42 C41 C40 107.1(4) . . ?
C42 C41 H41 126.4 . . ?
C40 C41 H41 126.4 . . ?
C50 C51 C52 122.7(4) . . ?
C50 C51 C56 118.8(4) . . ?
C52 C51 C56 118.5(4) . . ?
C47 C48 C49 121.4(4) . . ?
C47 C48 H48 119.3 . . ?
C49 C48 H48 119.3 . . ?
C51 C50 C49 122.4(4) . . ?
C51 C50 H50 118.8 . . ?
C49 C50 H50 118.8 . . ?
C67 C68 C69 119.5(5) . . ?
C67 C68 H68 120.3 . . ?
C69 C68 H68 120.3 . . ?
C71 C70 C75 116.8(5) . . ?
C71 C70 Si1 121.8(4) . . ?
C75 C70 Si1 121.4(4) . . ?
C64 C69 C68 121.7(5) . . ?
C64 C69 H69 119.2 . . ?
C68 C69 H69 119.2 . . ?
C66 C65 C64 120.3(5) . . ?
C66 C65 H65 119.8 . . ?
C64 C65 H65 119.8 . . ?
C39 C38 C35 117.1(4) . . ?
C39 C38 H38A 108.0 . . ?
C35 C38 H38A 108.0 . . ?
C39 C38 H38B 108.0 . . ?
C35 C38 H38B 108.0 . . ?
H38A C38 H38B 107.3 . . ?
C53 C52 C51 120.2(4) . . ?
C53 C52 H52 119.9 . . ?
C51 C52 H52 119.9 . . ?
C70 C71 C72 121.9(6) . . ?
C70 C71 H71 119.1 . . ?
C72 C71 H71 119.1 . . ?
C48 C47 C46 121.1(4) . . ?
C48 C47 H47 119.5 . . ?
C46 C47 H47 119.5 . . ?
C69 C64 C65 117.7(4) . . ?
C69 C64 Si1 118.2(4) . . ?
C65 C64 Si1 124.1(4) . . ?
C61 C60 C59 119.8(5) . . ?
C61 C60 H60 120.1 . . ?
C59 C60 H60 120.1 . . ?
C52 C53 C54 121.7(4) . . ?
C52 C53 H53 119.1 . . ?
C54 C53 H53 119.1 . . ?
C62 C61 C60 117.9(5) . . ?
C62 C61 H61 121.0 . . ?
C60 C61 H61 121.0 . . ?
C67 C66 C65 121.4(5) . . ?
C67 C66 H66 119.3 . . ?
C65 C66 H66 119.3 . . ?
C36 C37 H37A 109.5 . . ?
C36 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C36 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C66 C67 C68 119.4(5) . . ?
C66 C67 H67 120.3 . . ?
C68 C67 H67 120.3 . . ?
C73 C74 C75 118.8(7) . . ?
C73 C74 H74 120.6 . . ?
C75 C74 H74 120.6 . . ?
C74 C75 C70 121.9(7) . . ?
C74 C75 H75 119.1 . . ?
C70 C75 H75 119.1 . . ?
C72 C73 C74 120.9(6) . . ?
C72 C73 H73 119.6 . . ?
C74 C73 H73 119.6 . . ?
C61 C62 C63 118.8(5) . . ?
C61 C62 H62 120.6 . . ?
C63 C62 H62 120.6 . . ?
C73 C72 C71 119.7(6) . . ?
C73 C72 H72 120.1 . . ?
C71 C72 H72 120.1 . . ?
C102 C103 C104 120.0 . . ?
C102 C103 H103 120.0 . . ?
C104 C103 H103 120.0 . . ?
C101 C102 C103 120.0 . . ?
C101 C102 H102 120.0 . . ?
C103 C102 H102 120.0 . . ?
C100 C101 C102 120.0 . . ?
C100 C101 H101 120.0 . . ?
C102 C101 H101 120.0 . . ?
C101 C100 N100 120.0 . . ?
C101 C100 H100 120.0 . . ?
N100 C100 H100 120.0 . . ?
C104 N100 C100 120.0 . . ?
N100 C104 C103 120.0 . . ?
N100 C104 H104 120.0 . . ?
C103 C104 H104 120.0 . . ?

_refine_diff_density_max         0.863
_refine_diff_density_min         -0.733
_refine_diff_density_rms         0.098


# start Validation Reply Form
_vrf_PLAT410_5py_py              
;
PROBLEM: Short Intra H...H Contact H63      ..H63       .       1.72 Ang.  
RESPONSE: While a distance of 1.72 Angstroms is within the sum of the Van
der Waals radii, it is well outside of the sum of the covalent radii. 
Furthermore, H(63) is generated in a calculated position and symmetry 
generated, resulting in close approach. 
;
_vrf_PLAT910_5py_py              
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         12 Note  
RESPONSE: This has been noted, but is not serious. The independent 
reflections/parameters ratio is equal to 15.7, indicating that there are 
no issues with the data collected.
;
# end Validation Reply Form


####################################################################### 
# 
# 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_4_4THF_hexane
_database_code_depnum_ccdc_archive 'CCDC 1812763'
_audit_update_record             
;
2017-12-20 deposited with the CCDC.
2018-03-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 [{(py)UO(u-C6H4O2)U(py)}(LA)]
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C74 H62 N10 O3 U2, 4(C4 H8 O), C6 H14'
_chemical_formula_sum            'C96 H108 N10 O7 U2'
_chemical_formula_weight         1990.0461

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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 21/m'
_space_group_name_Hall           '-P 2yb'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, z'

_cell_length_a                   14.0792(3)
_cell_length_b                   21.2447(5)
_cell_length_c                   14.5359(3)
_cell_angle_alpha                90.000(2)
_cell_angle_beta                 105.081(2)
_cell_angle_gamma                90.000(2)
_cell_volume                     4198.07(16)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    24758
_cell_measurement_theta_min      3.0460
_cell_measurement_theta_max      27.8540

_exptl_crystal_description       block
_exptl_crystal_colour            'dark orange'
_exptl_crystal_size_max          0.331
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.105
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.595
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1976
_exptl_absorpt_coefficient_mu    3.918
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_correction_T_min  0.3579
_exptl_absorpt_correction_T_max  0.6953
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_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.
;
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 5.1574
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            86045
_diffrn_reflns_av_R_equivalents  0.0673
_diffrn_reflns_av_sigmaI/netI    0.0353
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.05
_diffrn_reflns_theta_max         26.38
_reflns_number_total             8803
_reflns_number_gt                7424
_reflns_threshold_expression     >2σ(I)
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -32.00  63.00   1.00   15.00    --   -9.43  38.00 150.00   95
  2  ω    -20.00  30.00   1.00   15.00    --   -9.43 -99.00  60.00   50
  3  ω    -20.00  30.00   1.00   15.00    --   -9.43 -99.00 -30.00   50
  4  ω    -52.00  -5.00   1.00   15.00    --   -9.43 103.00 -75.44   47
  5  ω    -32.00  63.00   1.00   15.00    --   -9.43  38.00-180.00   95
  6  ω     16.00  85.00   1.00   15.00    --   10.92-153.00  90.37   69
  7  ω    -59.00  38.00   1.00   15.00    --   10.92 -57.00   0.00   97
  8  ω    -62.00  33.00   1.00   15.00    --   10.92 -38.00 -90.00   95
  9  ω    -44.00  38.00   1.00   15.00    --   10.92 -57.00-150.00   82
 10  ω    -62.00 -28.00   1.00   15.00    --   10.92 -38.00  30.00   34
 11  ω      7.00  38.00   1.00   15.00    --   10.92 -57.00  30.00   31
 12  ω    -50.00   6.00   1.00   15.00    --   10.92 -38.00 -30.00   56
;
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.

C(8) was positionally disordered over two positions, so it?s thermal 
parameters were split into two parts with an occupancy set to 0.5 and refined 
anisotropically. As a result, H(8B) was positionally disordered, so it?s thermal 
parameters were also split into two parts and refined with an occupancy of 0.5. 
Also, three molecules of THF and one molecule of hexane were SQUEEZED 
from the lattice of 4?4THF?hexane through the use of the SQUEEZE routine 
due to unresolvable disorder.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0459P)²+11.3692P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8803
_refine_ls_number_parameters     451
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0540
_refine_ls_R_factor_gt           0.0403
_refine_ls_wR_factor_ref         0.0969
_refine_ls_wR_factor_gt          0.0914
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_restrained_S_all      1.050
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.979435(12) 0.156885(8) 0.256824(12) 0.02405(7) Uani 1 1 d . . .
C53 C 1.1812(5) 0.0795(4) 0.6341(5) 0.066(2) Uani 1 1 d . . .
H53 H 1.2089 0.0408 0.6613 0.079 Uiso 1 1 calc R . .
C54 C 1.0997(5) 0.0791(3) 0.5526(5) 0.0576(19) Uani 1 1 d . . .
H54 H 1.0737 0.0400 0.5256 0.069 Uiso 1 1 calc R . .
C28 C 1.1976(5) 0.2500 0.1678(5) 0.0295(16) Uani 1 2 d S . .
H28 H 1.1278 0.2500 0.1468 0.035 Uiso 1 2 calc SR . .
O30 O 0.6182(6) 0.7500 0.0895(6) 0.080(2) Uani 1 2 d S . .
C66 C 1.3718(4) 0.2175(3) 0.4786(4) 0.0445(14) Uani 1 1 d . . .
H66 H 1.4296 0.1952 0.5100 0.053 Uiso 1 1 calc R . .
C3 C 0.7214(5) 0.0738(4) 0.3580(5) 0.069(2) Uani 1 1 d . . .
H3 H 0.6976 0.0625 0.4112 0.083 Uiso 1 1 calc R . .
N5 N 1.0340(3) 0.0371(2) 0.2837(4) 0.0420(12) Uani 1 1 d . . .
C9 C 0.6282(4) 0.0474(3) 0.0572(5) 0.0573(19) Uani 1 1 d . . .
H9A H 0.6105 0.0531 -0.0128 0.069 Uiso 1 1 calc R . .
H9B H 0.5686 0.0563 0.0792 0.069 Uiso 1 1 calc R . .
C13 C 0.8870(5) 0.0611(4) -0.0371(6) 0.073(3) Uani 1 1 d . . .
H13 H 0.9086 0.0448 -0.0891 0.088 Uiso 1 1 calc R . .
N3 N 0.8871(3) 0.1078(2) 0.1034(3) 0.0338(10) Uani 1 1 d . . .
C57 C 1.0564(5) 0.2500 0.5162(5) 0.0316(16) Uani 1 2 d S . .
H57 H 0.9991 0.2500 0.4643 0.038 Uiso 1 2 calc SR . .
C10 C 0.6577(6) -0.0220(3) 0.0799(8) 0.101(4) Uani 1 1 d . . .
H10A H 0.6029 -0.0495 0.0486 0.152 Uiso 1 1 calc R . .
H10B H 0.6738 -0.0287 0.1490 0.152 Uiso 1 1 calc R . .
H10C H 0.7153 -0.0320 0.0566 0.152 Uiso 1 1 calc R . .
N2 N 0.8211(3) 0.1089(2) 0.2686(3) 0.0344(10) Uani 1 1 d . . .
O1 O 1.1210(2) 0.18606(15) 0.3382(2) 0.0257(7) Uani 1 1 d . . .
C301 C 0.7711(7) 0.7147(5) 0.0787(6) 0.092(3) Uani 1 1 d . . .
H30A H 0.8003 0.6978 0.0287 0.110 Uiso 1 1 calc R . .
H30B H 0.8078 0.6978 0.1414 0.110 Uiso 1 1 calc R . .
C56 C 1.0964(4) 0.1928(3) 0.5525(3) 0.0322(12) Uani 1 1 d . . .
N1 N 0.9775(3) 0.1322(2) 0.4292(3) 0.0342(10) Uani 1 1 d . . .
C52 C 1.2194(5) 0.1344(4) 0.6730(5) 0.0550(18) Uani 1 1 d . . .
H52 H 1.2742 0.1339 0.7274 0.066 Uiso 1 1 calc R . .
C6 C 0.7078(4) 0.0959(2) 0.1026(4) 0.0369(13) Uani 1 1 d . . .
C50 C 1.2192(6) 0.2500 0.6735(5) 0.043(2) Uani 1 2 d S . .
H50 H 1.2742 0.2500 0.7277 0.052 Uiso 1 2 calc SR . .
C19 C 1.4023(4) 0.1338(4) 0.2216(5) 0.0523(17) Uani 1 1 d . . .
H19 H 1.4721 0.1333 0.2405 0.063 Uiso 1 1 calc R . .
C65 C 1.2878(4) 0.1849(3) 0.4331(4) 0.0382(13) Uani 1 1 d . . .
H65 H 1.2878 0.1402 0.4347 0.046 Uiso 1 1 calc R . .
C18 C 1.3529(5) 0.0794(4) 0.2061(5) 0.061(2) Uani 1 1 d . . .
H18 H 1.3882 0.0408 0.2128 0.073 Uiso 1 1 calc R . .
C62 C 1.1600(5) -0.0388(3) 0.3404(5) 0.0534(17) Uani 1 1 d . . .
H62 H 1.2258 -0.0477 0.3746 0.064 Uiso 1 1 calc R . .
C12 C 0.7937(5) 0.0591(4) -0.0264(5) 0.071(3) Uani 1 1 d . . .
H12 H 0.7378 0.0418 -0.0706 0.085 Uiso 1 1 calc R . .
C4 C 0.6718(4) 0.0697(3) 0.2643(5) 0.057(2) Uani 1 1 d . . .
H4 H 0.6063 0.0550 0.2403 0.068 Uiso 1 1 calc R . .
C29 C 1.2460(4) 0.1928(3) 0.1823(3) 0.0308(12) Uani 1 1 d . . .
C51 C 1.1800(4) 0.1930(3) 0.6347(4) 0.0419(14) Uani 1 1 d . . .
N4 N 1.0913(3) 0.1321(2) 0.1449(3) 0.0311(10) Uani 1 1 d . . .
C20 C 1.3519(4) 0.1923(3) 0.2103(4) 0.0384(13) Uani 1 1 d . . .
C55 C 1.0584(4) 0.1335(3) 0.5126(4) 0.0371(13) Uani 1 1 d . . .
O3 O 0.9338(4) 0.2500 0.2272(4) 0.0394(13) Uani 1 2 d S . .
C17 C 1.2480(4) 0.0785(3) 0.1796(4) 0.0474(16) Uani 1 1 d . . .
H17 H 1.2141 0.0394 0.1694 0.057 Uiso 1 1 calc R . .
C21 C 1.4013(5) 0.2500 0.2238(6) 0.042(2) Uani 1 2 d S . .
H21 H 1.4712 0.2500 0.2428 0.050 Uiso 1 2 calc SR . .
C300 C 0.6643(7) 0.6992(4) 0.0581(6) 0.082(3) Uani 1 1 d . . .
H30C H 0.6365 0.6925 -0.0111 0.098 Uiso 1 1 calc R . .
H30D H 0.6546 0.6603 0.0921 0.098 Uiso 1 1 calc R . .
C15 C 1.0457(4) 0.1022(3) 0.0687(4) 0.0429(15) Uani 1 1 d . . .
H15 H 1.0834 0.0865 0.0282 0.052 Uiso 1 1 calc R . .
C63 C 1.1266(4) 0.0226(3) 0.3317(5) 0.0496(16) Uani 1 1 d . . .
H63 H 1.1701 0.0554 0.3604 0.059 Uiso 1 1 calc R . .
C11 C 0.7947(4) 0.0868(3) 0.0609(4) 0.0418(15) Uani 1 1 d . . .
C14 C 0.9445(4) 0.0917(3) 0.0426(4) 0.0455(16) Uani 1 1 d . . .
C59 C 0.9759(4) -0.0110(2) 0.2461(4) 0.0383(13) Uani 1 1 d . . .
H59 H 0.9094 -0.0020 0.2141 0.046 Uiso 1 1 calc R . .
C16 C 1.1961(4) 0.1332(3) 0.1687(4) 0.0347(12) Uani 1 1 d . . .
C5 C 0.7334(4) 0.0907(2) 0.2092(4) 0.0370(13) Uani 1 1 d . . .
C1 C 0.8964(4) 0.1081(3) 0.4394(4) 0.0464(16) Uani 1 1 d . . .
H1 H 0.8917 0.0971 0.5013 0.056 Uiso 1 1 calc R . .
C61 C 1.0989(5) -0.0863(3) 0.3001(5) 0.0572(18) Uani 1 1 d . . .
H61 H 1.1209 -0.1287 0.3062 0.069 Uiso 1 1 calc R . .
C64 C 1.2025(3) 0.2169(2) 0.3846(3) 0.0252(10) Uani 1 1 d . . .
C2 C 0.8145(4) 0.0979(3) 0.3603(4) 0.0445(15) Uani 1 1 d . . .
C60 C 1.0056(5) -0.0718(3) 0.2507(5) 0.061(2) Uani 1 1 d . . .
H60 H 0.9617 -0.1039 0.2199 0.073 Uiso 1 1 calc R . .
C7 C 0.6674(4) 0.1632(3) 0.0743(4) 0.0381(13) Uani 1 1 d D . .
C8A C 0.5816(8) 0.1807(6) 0.1056(9) 0.041(3) Uani 0.50 1 d P . .
H8A H 0.5963 0.1768 0.1750 0.061 Uiso 0.50 1 calc PR . .
H8B H 0.5268 0.1528 0.0759 0.061 Uiso 0.50 1 calc PR . .
H8C H 0.5636 0.2243 0.0870 0.061 Uiso 0.50 1 calc PR . .
C8B C 0.6257(11) 0.1736(7) -0.0257(9) 0.048(3) Uani 0.50 1 d P . .
H8F H 0.6750 0.1644 -0.0605 0.072 Uiso 0.50 1 calc PR . .
H8E H 0.6048 0.2176 -0.0364 0.072 Uiso 0.50 1 calc PR . .
H8D H 0.5687 0.1460 -0.0486 0.072 Uiso 0.50 1 calc PR . .
H7A H 0.721(3) 0.191(2) 0.102(4) 0.058 Uiso 1 1 d D . .
H7B H 0.625(9) 0.173(8) 0.115(8) 0.058 Uiso 0.50 1 d PD . .
H7C H 0.653(13) 0.165(8) 0.0054(11) 0.058 Uiso 0.50 1 d PD . .


_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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 O3 2.0900(17) . ?
U1 O1 2.128(3) . ?
U1 N2 2.497(4) . ?
U1 N3 2.498(4) . ?
U1 N1 2.567(4) . ?
U1 N4 2.595(4) . ?
U1 N5 2.657(4) . ?
U1 U1 3.9564(3) 4_565 ?
C53 C52 1.348(10) . ?
C53 C54 1.418(8) . ?
C53 H53 0.9500 . ?
C54 C55 1.356(8) . ?
C54 H54 0.9500 . ?
C28 C29 1.383(6) 4_565 ?
C28 C29 1.383(6) . ?
C28 H28 0.9500 . ?
O30 C300 1.396(9) 4_575 ?
O30 C300 1.396(9) . ?
C66 C66 1.381(12) 4_565 ?
C66 C65 1.382(8) . ?
C66 H66 0.9500 . ?
C3 C4 1.362(10) . ?
C3 C2 1.399(8) . ?
C3 H3 0.9500 . ?
N5 C59 1.335(7) . ?
N5 C63 1.344(7) . ?
C9 C6 1.539(8) . ?
C9 C10 1.545(9) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C13 C12 1.364(10) . ?
C13 C14 1.390(8) . ?
C13 H13 0.9500 . ?
N3 C11 1.363(7) . ?
N3 C14 1.387(7) . ?
C57 C56 1.385(6) 4_565 ?
C57 C56 1.385(6) . ?
C57 H57 0.9500 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
N2 C5 1.366(6) . ?
N2 C2 1.380(7) . ?
O1 C64 1.342(5) . ?
C301 C300 1.492(12) . ?
C301 C301 1.500(19) 4_575 ?
C301 H30A 0.9900 . ?
C301 H30B 0.9900 . ?
C56 C55 1.432(8) . ?
C56 C51 1.442(7) . ?
N1 C1 1.294(7) . ?
N1 C55 1.431(6) . ?
C52 C51 1.417(9) . ?
C52 H52 0.9500 . ?
C6 C5 1.502(8) . ?
C6 C11 1.512(8) . ?
C6 C7 1.554(7) . ?
C50 C51 1.388(7) 4_565 ?
C50 C51 1.388(7) . ?
C50 H50 0.9500 . ?
C19 C18 1.337(10) . ?
C19 C20 1.420(9) . ?
C19 H19 0.9500 . ?
C65 C64 1.400(7) . ?
C65 H65 0.9500 . ?
C18 C17 1.426(9) . ?
C18 H18 0.9500 . ?
C62 C61 1.356(9) . ?
C62 C63 1.380(8) . ?
C62 H62 0.9500 . ?
C12 C11 1.396(9) . ?
C12 H12 0.9500 . ?
C4 C5 1.398(9) . ?
C4 H4 0.9500 . ?
C29 C16 1.436(8) . ?
C29 C20 1.439(7) . ?
N4 C15 1.293(7) . ?
N4 C16 1.426(7) . ?
C20 C21 1.397(7) . ?
O3 U1 2.0900(17) 4_565 ?
C17 C16 1.360(8) . ?
C17 H17 0.9500 . ?
C21 C20 1.397(7) 4_565 ?
C21 H21 0.9500 . ?
C300 H30C 0.9900 . ?
C300 H30D 0.9900 . ?
C15 C14 1.394(8) . ?
C15 H15 0.9500 . ?
C63 H63 0.9500 . ?
C59 C60 1.355(9) . ?
C59 H59 0.9500 . ?
C1 C2 1.417(8) . ?
C1 H1 0.9500 . ?
C61 C60 1.359(9) . ?
C61 H61 0.9500 . ?
C64 C64 1.405(10) 4_565 ?
C60 H60 0.9500 . ?
C7 C8B 1.437(13) . ?
C7 C8A 1.444(12) . ?
C7 H7A 0.970(5) . ?
C7 H7B 0.970(5) . ?
C7 H7C 0.970(5) . ?
C8A H8A 0.9800 . ?
C8A H8B 0.9800 . ?
C8A H8C 0.9800 . ?
C8A H7B 0.61(11) . ?
C8B H8F 0.9800 . ?
C8B H8E 0.9800 . ?
C8B H8D 0.9800 . ?
C8B H7C 0.54(11) . ?

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
O3 U1 O1 91.85(16) . . ?
O3 U1 N2 99.66(17) . . ?
O1 U1 N2 143.53(13) . . ?
O3 U1 N3 98.65(17) . . ?
O1 U1 N3 144.33(14) . . ?
N2 U1 N3 67.96(15) . . ?
O3 U1 N1 108.27(19) . . ?
O1 U1 N1 76.27(13) . . ?
N2 U1 N1 67.27(14) . . ?
N3 U1 N1 130.63(15) . . ?
O3 U1 N4 105.50(19) . . ?
O1 U1 N4 76.97(13) . . ?
N2 U1 N4 131.18(14) . . ?
N3 U1 N4 67.38(14) . . ?
N1 U1 N4 137.10(14) . . ?
O3 U1 N5 176.67(18) . . ?
O1 U1 N5 90.23(13) . . ?
N2 U1 N5 80.14(14) . . ?
N3 U1 N5 78.18(14) . . ?
N1 U1 N5 74.76(16) . . ?
N4 U1 N5 72.45(15) . . ?
O3 U1 U1 18.82(13) . 4_565 ?
O1 U1 U1 73.07(9) . 4_565 ?
N2 U1 U1 114.07(10) . 4_565 ?
N3 U1 U1 114.66(10) . 4_565 ?
N1 U1 U1 101.78(10) . 4_565 ?
N4 U1 U1 101.70(10) . 4_565 ?
N5 U1 U1 163.24(10) . 4_565 ?
C52 C53 C54 120.3(6) . . ?
C52 C53 H53 119.9 . . ?
C54 C53 H53 119.9 . . ?
C55 C54 C53 121.2(7) . . ?
C55 C54 H54 119.4 . . ?
C53 C54 H54 119.4 . . ?
C29 C28 C29 123.1(7) 4_565 . ?
C29 C28 H28 118.5 4_565 . ?
C29 C28 H28 118.5 . . ?
C300 O30 C300 101.3(10) 4_575 . ?
C66 C66 C65 120.1(3) 4_565 . ?
C66 C66 H66 120.0 4_565 . ?
C65 C66 H66 120.0 . . ?
C4 C3 C2 106.3(6) . . ?
C4 C3 H3 126.8 . . ?
C2 C3 H3 126.8 . . ?
C59 N5 C63 116.4(5) . . ?
C59 N5 U1 123.4(3) . . ?
C63 N5 U1 120.0(4) . . ?
C6 C9 C10 115.0(5) . . ?
C6 C9 H9A 108.5 . . ?
C10 C9 H9A 108.5 . . ?
C6 C9 H9B 108.5 . . ?
C10 C9 H9B 108.5 . . ?
H9A C9 H9B 107.5 . . ?
C12 C13 C14 106.8(6) . . ?
C12 C13 H13 126.6 . . ?
C14 C13 H13 126.6 . . ?
C11 N3 C14 106.0(4) . . ?
C11 N3 U1 139.1(4) . . ?
C14 N3 U1 114.7(3) . . ?
C56 C57 C56 122.7(7) 4_565 . ?
C56 C57 H57 118.7 4_565 . ?
C56 C57 H57 118.7 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C5 N2 C2 106.6(5) . . ?
C5 N2 U1 138.5(4) . . ?
C2 N2 U1 114.9(3) . . ?
C64 O1 U1 167.7(3) . . ?
C300 C301 C301 102.8(5) . 4_575 ?
C300 C301 H30A 111.2 . . ?
C301 C301 H30A 111.2 4_575 . ?
C300 C301 H30B 111.2 . . ?
C301 C301 H30B 111.2 4_575 . ?
H30A C301 H30B 109.1 . . ?
C57 C56 C55 123.0(5) . . ?
C57 C56 C51 118.4(5) . . ?
C55 C56 C51 118.5(5) . . ?
C1 N1 C55 116.2(5) . . ?
C1 N1 U1 115.2(4) . . ?
C55 N1 U1 128.0(3) . . ?
C53 C52 C51 121.6(5) . . ?
C53 C52 H52 119.2 . . ?
C51 C52 H52 119.2 . . ?
C5 C6 C11 113.7(4) . . ?
C5 C6 C9 110.2(5) . . ?
C11 C6 C9 108.5(5) . . ?
C5 C6 C7 108.3(5) . . ?
C11 C6 C7 107.0(5) . . ?
C9 C6 C7 109.1(4) . . ?
C51 C50 C51 121.4(7) 4_565 . ?
C51 C50 H50 119.3 4_565 . ?
C51 C50 H50 119.3 . . ?
C18 C19 C20 121.0(5) . . ?
C18 C19 H19 119.5 . . ?
C20 C19 H19 119.5 . . ?
C66 C65 C64 120.8(5) . . ?
C66 C65 H65 119.6 . . ?
C64 C65 H65 119.6 . . ?
C19 C18 C17 120.9(6) . . ?
C19 C18 H18 119.5 . . ?
C17 C18 H18 119.5 . . ?
C61 C62 C63 120.1(6) . . ?
C61 C62 H62 120.0 . . ?
C63 C62 H62 120.0 . . ?
C13 C12 C11 107.9(5) . . ?
C13 C12 H12 126.0 . . ?
C11 C12 H12 126.0 . . ?
C3 C4 C5 108.6(5) . . ?
C3 C4 H4 125.7 . . ?
C5 C4 H4 125.7 . . ?
C28 C29 C16 123.3(5) . . ?
C28 C29 C20 118.8(5) . . ?
C16 C29 C20 117.8(5) . . ?
C50 C51 C52 122.2(5) . . ?
C50 C51 C56 119.5(6) . . ?
C52 C51 C56 118.3(6) . . ?
C15 N4 C16 117.9(4) . . ?
C15 N4 U1 112.9(4) . . ?
C16 N4 U1 127.1(3) . . ?
C21 C20 C19 122.4(5) . . ?
C21 C20 C29 118.4(5) . . ?
C19 C20 C29 119.2(6) . . ?
C54 C55 N1 120.4(5) . . ?
C54 C55 C56 120.2(5) . . ?
N1 C55 C56 119.5(5) . . ?
U1 O3 U1 142.4(3) 4_565 . ?
C16 C17 C18 120.5(6) . . ?
C16 C17 H17 119.8 . . ?
C18 C17 H17 119.8 . . ?
C20 C21 C20 122.5(7) 4_565 . ?
C20 C21 H21 118.7 4_565 . ?
C20 C21 H21 118.7 . . ?
O30 C300 C301 107.1(7) . . ?
O30 C300 H30C 110.3 . . ?
C301 C300 H30C 110.3 . . ?
O30 C300 H30D 110.3 . . ?
C301 C300 H30D 110.3 . . ?
H30C C300 H30D 108.6 . . ?
N4 C15 C14 123.9(5) . . ?
N4 C15 H15 118.1 . . ?
C14 C15 H15 118.1 . . ?
N5 C63 C62 121.7(6) . . ?
N5 C63 H63 119.1 . . ?
C62 C63 H63 119.1 . . ?
N3 C11 C12 109.5(5) . . ?
N3 C11 C6 123.6(5) . . ?
C12 C11 C6 126.9(5) . . ?
N3 C14 C13 109.7(5) . . ?
N3 C14 C15 120.7(5) . . ?
C13 C14 C15 129.4(6) . . ?
N5 C59 C60 124.2(5) . . ?
N5 C59 H59 117.9 . . ?
C60 C59 H59 117.9 . . ?
C17 C16 N4 120.3(5) . . ?
C17 C16 C29 120.5(5) . . ?
N4 C16 C29 119.1(5) . . ?
N2 C5 C4 108.8(5) . . ?
N2 C5 C6 124.5(5) . . ?
C4 C5 C6 126.6(5) . . ?
N1 C1 C2 121.6(5) . . ?
N1 C1 H1 119.2 . . ?
C2 C1 H1 119.2 . . ?
C62 C61 C60 118.5(6) . . ?
C62 C61 H61 120.8 . . ?
C60 C61 H61 120.8 . . ?
O1 C64 C65 121.7(5) . . ?
O1 C64 C64 119.3(3) . 4_565 ?
C65 C64 C64 119.1(3) . 4_565 ?
N2 C2 C3 109.7(5) . . ?
N2 C2 C1 120.8(5) . . ?
C3 C2 C1 129.5(6) . . ?
C59 C60 C61 119.1(6) . . ?
C59 C60 H60 120.5 . . ?
C61 C60 H60 120.5 . . ?
C8B C7 C8A 97.1(8) . . ?
C8B C7 C6 115.7(7) . . ?
C8A C7 C6 115.6(7) . . ?
C8B C7 H7A 114(4) . . ?
C8A C7 H7A 110(4) . . ?
C6 C7 H7A 105(4) . . ?
C8B C7 H7B 116(9) . . ?
C6 C7 H7B 106(10) . . ?
H7A C7 H7B 98(10) . . ?
C8A C7 H7C 110(10) . . ?
C6 C7 H7C 106(10) . . ?
H7A C7 H7C 110(10) . . ?
H7B C7 H7C 129(10) . . ?
C7 C8A H8A 109.5 . . ?
C7 C8A H8B 109.5 . . ?
H8A C8A H8B 109.5 . . ?
C7 C8A H8C 109.5 . . ?
H8A C8A H8C 109.5 . . ?
H8B C8A H8C 109.5 . . ?
H8A C8A H7B 79.0 . . ?
H8B C8A H7B 124.9 . . ?
H8C C8A H7B 118.6 . . ?
C7 C8B H8F 109.5 . . ?
C7 C8B H8E 109.5 . . ?
H8F C8B H8E 109.5 . . ?
C7 C8B H8D 109.5 . . ?
H8F C8B H8D 109.5 . . ?
H8E C8B H8D 109.5 . . ?
H8F C8B H7C 85.8 . . ?
H8E C8B H7C 125.1 . . ?
H8D C8B H7C 114.2 . . ?

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
C52 C53 C54 C55 -0.4(12) . . . . ?
O1 U1 N5 C59 -178.0(5) . . . . ?
N2 U1 N5 C59 37.4(5) . . . . ?
N3 U1 N5 C59 -32.0(5) . . . . ?
N1 U1 N5 C59 106.3(5) . . . . ?
N4 U1 N5 C59 -101.7(5) . . . . ?
U1 U1 N5 C59 -173.5(3) 4_565 . . . ?
O1 U1 N5 C63 -2.7(5) . . . . ?
N2 U1 N5 C63 -147.4(5) . . . . ?
N3 U1 N5 C63 143.3(5) . . . . ?
N1 U1 N5 C63 -78.4(5) . . . . ?
N4 U1 N5 C63 73.5(5) . . . . ?
U1 U1 N5 C63 1.7(8) 4_565 . . . ?
O3 U1 N3 C11 -80.9(6) . . . . ?
O1 U1 N3 C11 173.6(5) . . . . ?
N2 U1 N3 C11 16.1(5) . . . . ?
N1 U1 N3 C11 42.3(6) . . . . ?
N4 U1 N3 C11 175.8(6) . . . . ?
N5 U1 N3 C11 100.1(6) . . . . ?
U1 U1 N3 C11 -91.3(5) 4_565 . . . ?
O3 U1 N3 C14 105.4(4) . . . . ?
O1 U1 N3 C14 -0.1(5) . . . . ?
N2 U1 N3 C14 -157.6(4) . . . . ?
N1 U1 N3 C14 -131.3(4) . . . . ?
N4 U1 N3 C14 2.1(4) . . . . ?
N5 U1 N3 C14 -73.6(4) . . . . ?
U1 U1 N3 C14 95.0(4) 4_565 . . . ?
O3 U1 N2 C5 75.3(5) . . . . ?
O1 U1 N2 C5 -178.1(4) . . . . ?
N3 U1 N2 C5 -20.2(5) . . . . ?
N1 U1 N2 C5 -178.8(6) . . . . ?
N4 U1 N2 C5 -45.3(6) . . . . ?
N5 U1 N2 C5 -101.3(5) . . . . ?
U1 U1 N2 C5 88.0(5) 4_565 . . . ?
O3 U1 N2 C2 -102.5(4) . . . . ?
O1 U1 N2 C2 4.0(5) . . . . ?
N3 U1 N2 C2 162.0(4) . . . . ?
N1 U1 N2 C2 3.3(4) . . . . ?
N4 U1 N2 C2 136.8(4) . . . . ?
N5 U1 N2 C2 80.8(4) . . . . ?
U1 U1 N2 C2 -89.9(4) 4_565 . . . ?
O3 U1 O1 C64 -0.3(14) . . . . ?
N2 U1 O1 C64 -109.3(14) . . . . ?
N3 U1 O1 C64 107.3(14) . . . . ?
N1 U1 O1 C64 -108.6(14) . . . . ?
N4 U1 O1 C64 105.2(14) . . . . ?
N5 U1 O1 C64 177.1(14) . . . . ?
U1 U1 O1 C64 -1.5(14) 4_565 . . . ?
C56 C57 C56 C55 -176.9(4) 4_565 . . . ?
C56 C57 C56 C51 3.5(10) 4_565 . . . ?
O3 U1 N1 C1 92.0(5) . . . . ?
O1 U1 N1 C1 179.4(5) . . . . ?
N2 U1 N1 C1 -1.0(4) . . . . ?
N3 U1 N1 C1 -27.4(5) . . . . ?
N4 U1 N1 C1 -127.7(4) . . . . ?
N5 U1 N1 C1 -86.5(5) . . . . ?
U1 U1 N1 C1 110.4(4) 4_565 . . . ?
O3 U1 N1 C55 -97.5(5) . . . . ?
O1 U1 N1 C55 -10.1(4) . . . . ?
N2 U1 N1 C55 169.4(5) . . . . ?
N3 U1 N1 C55 143.0(4) . . . . ?
N4 U1 N1 C55 42.7(5) . . . . ?
N5 U1 N1 C55 83.9(5) . . . . ?
U1 U1 N1 C55 -79.2(4) 4_565 . . . ?
C54 C53 C52 C51 0.3(12) . . . . ?
C10 C9 C6 C5 -60.7(9) . . . . ?
C10 C9 C6 C11 64.3(9) . . . . ?
C10 C9 C6 C7 -179.5(7) . . . . ?
C66 C66 C65 C64 1.5(7) 4_565 . . . ?
C20 C19 C18 C17 -1.3(11) . . . . ?
C14 C13 C12 C11 -1.6(10) . . . . ?
C2 C3 C4 C5 0.3(9) . . . . ?
C29 C28 C29 C16 179.1(4) 4_565 . . . ?
C29 C28 C29 C20 -2.4(10) 4_565 . . . ?
C51 C50 C51 C52 179.6(5) 4_565 . . . ?
C51 C50 C51 C56 -0.1(11) 4_565 . . . ?
C53 C52 C51 C50 -179.3(7) . . . . ?
C53 C52 C51 C56 0.4(10) . . . . ?
C57 C56 C51 C50 -1.6(8) . . . . ?
C55 C56 C51 C50 178.8(6) . . . . ?
C57 C56 C51 C52 178.6(6) . . . . ?
C55 C56 C51 C52 -1.0(8) . . . . ?
O3 U1 N4 C15 -98.2(4) . . . . ?
O1 U1 N4 C15 173.5(4) . . . . ?
N2 U1 N4 C15 20.1(5) . . . . ?
N3 U1 N4 C15 -5.1(4) . . . . ?
N1 U1 N4 C15 120.9(4) . . . . ?
N5 U1 N4 C15 79.1(4) . . . . ?
U1 U1 N4 C15 -117.2(4) 4_565 . . . ?
O3 U1 N4 C16 98.7(4) . . . . ?
O1 U1 N4 C16 10.5(4) . . . . ?
N2 U1 N4 C16 -143.0(4) . . . . ?
N3 U1 N4 C16 -168.2(5) . . . . ?
N1 U1 N4 C16 -42.2(5) . . . . ?
N5 U1 N4 C16 -84.0(4) . . . . ?
U1 U1 N4 C16 79.8(4) 4_565 . . . ?
C18 C19 C20 C21 -178.4(7) . . . . ?
C18 C19 C20 C29 0.4(9) . . . . ?
C28 C29 C20 C21 1.4(8) . . . . ?
C16 C29 C20 C21 180.0(5) . . . . ?
C28 C29 C20 C19 -177.4(5) . . . . ?
C16 C29 C20 C19 1.1(7) . . . . ?
C53 C54 C55 N1 178.7(6) . . . . ?
C53 C54 C55 C56 -0.2(10) . . . . ?
C1 N1 C55 C54 65.9(8) . . . . ?
U1 N1 C55 C54 -104.4(6) . . . . ?
C1 N1 C55 C56 -115.2(6) . . . . ?
U1 N1 C55 C56 74.4(6) . . . . ?
C57 C56 C55 C54 -178.7(6) . . . . ?
C51 C56 C55 C54 0.9(8) . . . . ?
C57 C56 C55 N1 2.4(8) . . . . ?
C51 C56 C55 N1 -178.0(5) . . . . ?
O1 U1 O3 U1 -3.7(5) . . . 4_565 ?
N2 U1 O3 U1 141.5(5) . . . 4_565 ?
N3 U1 O3 U1 -149.5(5) . . . 4_565 ?
N1 U1 O3 U1 72.4(5) . . . 4_565 ?
N4 U1 O3 U1 -80.7(5) . . . 4_565 ?
C19 C18 C17 C16 0.6(11) . . . . ?
C19 C20 C21 C20 178.3(5) . . . 4_565 ?
C29 C20 C21 C20 -0.5(11) . . . 4_565 ?
C300 O30 C300 C301 42.3(10) 4_575 . . . ?
C301 C301 C300 O30 -25.9(7) 4_575 . . . ?
C16 N4 C15 C14 172.9(6) . . . . ?
U1 N4 C15 C14 8.2(8) . . . . ?
C59 N5 C63 C62 1.0(10) . . . . ?
U1 N5 C63 C62 -174.6(5) . . . . ?
C61 C62 C63 N5 -0.1(11) . . . . ?
C14 N3 C11 C12 -1.3(7) . . . . ?
U1 N3 C11 C12 -175.3(5) . . . . ?
C14 N3 C11 C6 -178.6(5) . . . . ?
U1 N3 C11 C6 7.4(9) . . . . ?
C13 C12 C11 N3 1.8(9) . . . . ?
C13 C12 C11 C6 179.0(6) . . . . ?
C5 C6 C11 N3 -36.9(7) . . . . ?
C9 C6 C11 N3 -159.8(5) . . . . ?
C7 C6 C11 N3 82.6(6) . . . . ?
C5 C6 C11 C12 146.3(7) . . . . ?
C9 C6 C11 C12 23.3(9) . . . . ?
C7 C6 C11 C12 -94.2(7) . . . . ?
C11 N3 C14 C13 0.3(7) . . . . ?
U1 N3 C14 C13 176.0(5) . . . . ?
C11 N3 C14 C15 -174.9(6) . . . . ?
U1 N3 C14 C15 0.8(7) . . . . ?
C12 C13 C14 N3 0.8(9) . . . . ?
C12 C13 C14 C15 175.5(7) . . . . ?
N4 C15 C14 N3 -6.6(10) . . . . ?
N4 C15 C14 C13 179.3(7) . . . . ?
C63 N5 C59 C60 -2.5(10) . . . . ?
U1 N5 C59 C60 172.9(5) . . . . ?
C18 C17 C16 N4 -178.1(6) . . . . ?
C18 C17 C16 C29 1.0(9) . . . . ?
C15 N4 C16 C17 -56.2(8) . . . . ?
U1 N4 C16 C17 106.1(5) . . . . ?
C15 N4 C16 C29 124.7(6) . . . . ?
U1 N4 C16 C29 -73.0(6) . . . . ?
C28 C29 C16 C17 176.7(6) . . . . ?
C20 C29 C16 C17 -1.8(8) . . . . ?
C28 C29 C16 N4 -4.2(8) . . . . ?
C20 C29 C16 N4 177.3(5) . . . . ?
C2 N2 C5 C4 1.3(6) . . . . ?
U1 N2 C5 C4 -176.7(4) . . . . ?
C2 N2 C5 C6 178.5(5) . . . . ?
U1 N2 C5 C6 0.5(8) . . . . ?
C3 C4 C5 N2 -1.0(8) . . . . ?
C3 C4 C5 C6 -178.1(6) . . . . ?
C11 C6 C5 N2 33.4(7) . . . . ?
C9 C6 C5 N2 155.4(5) . . . . ?
C7 C6 C5 N2 -85.3(6) . . . . ?
C11 C6 C5 C4 -149.9(6) . . . . ?
C9 C6 C5 C4 -27.9(8) . . . . ?
C7 C6 C5 C4 91.4(7) . . . . ?
C55 N1 C1 C2 -173.1(6) . . . . ?
U1 N1 C1 C2 -1.5(8) . . . . ?
C63 C62 C61 C60 0.7(11) . . . . ?
U1 O1 C64 C65 -178.3(11) . . . . ?
U1 O1 C64 C64 1.7(15) . . . 4_565 ?
C66 C65 C64 O1 178.5(5) . . . . ?
C66 C65 C64 C64 -1.5(7) . . . 4_565 ?
C5 N2 C2 C3 -1.2(7) . . . . ?
U1 N2 C2 C3 177.4(5) . . . . ?
C5 N2 C2 C1 175.8(6) . . . . ?
U1 N2 C2 C1 -5.6(7) . . . . ?
C4 C3 C2 N2 0.5(8) . . . . ?
C4 C3 C2 C1 -176.1(7) . . . . ?
N1 C1 C2 N2 5.0(10) . . . . ?
N1 C1 C2 C3 -178.7(7) . . . . ?
N5 C59 C60 C61 3.2(11) . . . . ?
C62 C61 C60 C59 -2.1(11) . . . . ?
C5 C6 C7 C8B -171.2(8) . . . . ?
C11 C6 C7 C8B 65.9(9) . . . . ?
C9 C6 C7 C8B -51.3(10) . . . . ?
C5 C6 C7 C8A -58.7(8) . . . . ?
C11 C6 C7 C8A 178.4(7) . . . . ?
C9 C6 C7 C8A 61.2(9) . . . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        26.38
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         1.900
_refine_diff_density_min         -1.021
_refine_diff_density_rms         0.119

# SQUEEZE RESULTS 
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
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
_platon_squeeze_void_content
1 -0.500 0.198 -0.500 1234 245 ' '
_platon_squeeze_details          
;
;
# start Validation Reply Form
_vrf_CHEMW03_4_4THF_hexane       
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as
RESPONSE: The ratio of given/expected molecular weights differ
due to the use of the SQUEEZE routine to remove 3 molecules of
THF and 1 molecule of hexane from the lattice.
;
_vrf_PLAT910_4_4THF_hexane       
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         17 Note  
RESPONSE: This has been noted, but is not serious. The independent 
reflections/parameters ratio is equal to 15.6, indicating that there are 
no issues with the data collected.
;
_vrf_PLAT990_4_4THF_hexane       
;
PROBLEM: Deprecated .res/.hkl Input Style SQUEEZE Job ...          ! Note 
RESPONSE: The SQUEEZE routine was run using SHELXL-97 (Sheldrick, 2008). 
;
