# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# 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_compound1
_database_code_depnum_ccdc_archive 'CCDC 1984900'
loop_
_audit_author_name
_audit_author_address
'Bradley E. Cowie'
;The University of Edinburgh
United Kingdom
;
_audit_update_record             
;
2020-02-18 deposited with the CCDC.	2020-06-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        '[{(py)U(OH)2U(O2C6H4)(py)}(LA)]'
_chemical_name_common            'Compound 1.3THF'
_chemical_melting_point          ?
_chemical_formula_moiety         'C74 H64 N10 O4 U2, 3(C4 H8 O)'
_chemical_formula_sum            'C86 H88 N10 O7 U2'
_chemical_formula_weight         1849.72

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      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                   16.9463(3)
_cell_length_b                   24.3235(4)
_cell_length_c                   17.9675(3)
_cell_angle_alpha                90
_cell_angle_beta                 98.7581(15)
_cell_angle_gamma                90
_cell_volume                     7319.77(19)
_cell_formula_units_Z            4
_cell_measurement_temperature    120.0(1)
_cell_measurement_reflns_used    15123
_cell_measurement_theta_min      3.0260
_cell_measurement_theta_max      25.2880

_exptl_crystal_description       plate
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.678
_exptl_crystal_F_000             3656
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.191
_exptl_crystal_size_mid          0.058
_exptl_crystal_size_min          0.034
_exptl_absorpt_coefficient_mu    4.485
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.91925
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
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      120.0(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_measurement_device_type  'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_method       'phi and omega scans'
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1042
_diffrn_reflns_number            74194
_diffrn_reflns_av_unetI/netI     0.0481
_diffrn_reflns_av_R_equivalents  0.0856
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.791
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -45.00  53.00   1.00   45.00    --  -16.31  77.00-120.00   98
  2  ω    -25.00  24.00   1.00   45.00    --  -16.31 -99.00   0.00   49
  3  ω    -89.00  22.00   1.00   45.00    --  -16.31 -19.00-180.00  111
  4  ω    -25.00  24.00   1.00   45.00    --  -16.31 -99.00  30.00   49
  5  ω    -55.00  30.00   1.00   45.00    --  -16.31  95.00-165.75   85
  6  ω      0.00  86.00   1.00   45.00    --   18.03  57.00-180.00   86
  7  ω    -11.00  87.00   1.00   45.00    --   18.03  77.00   0.00   98
  8  ω      0.00  86.00   1.00   45.00    --   18.03  57.00 150.00   86
  9  ω    -20.00  90.00   1.00   45.00    --   18.03  19.00 -30.00  110
 10  ω      0.00  86.00   1.00   45.00    --   18.03  57.00  30.00   86
 11  ω    -91.00 -34.00   1.00   45.00    --  -16.31-179.00-120.00   57
 12  ω      6.00  82.00   1.00   45.00    --   18.03-139.00 107.28   76
;
_reflns_number_total             7484
_reflns_number_gt                6009
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       '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-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_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 THF within the asymmetric unit was positionally disordered over
two positions. As a result, it was split into two parts and refined with an 
occupancy ratio of 0.73:0.27. In addition, the thermal parameters of the 
carbon atoms were restrained to be similar to one another through the use 
of the SIMU command. C(10) was also positionally disordered over two positions,
and was split into two parts and refined with a 0.69:0.31 ratio. The thermal
parameters of C(10) and C(10A) were restrained to be similar to one another
through the use of the SIMU command.   
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0176P)²+30.2950P] 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         7484
_refine_ls_number_parameters     510
_refine_ls_number_restraints     36
_refine_ls_R_factor_all          0.0514
_refine_ls_R_factor_gt           0.0336
_refine_ls_wR_factor_ref         0.0615
_refine_ls_wR_factor_gt          0.0570
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_restrained_S_all      1.033
_refine_ls_shift/su_max          0.019
_refine_ls_shift/su_mean         0.001

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
C59 C 0.4594(3) 0.2234(2) 0.5446(2) 0.0282(11) Uani 1 1 d . . . . .
H59 H 0.466258 0.260908 0.538109 0.034 Uiso 1 1 calc R U . . .
O10 O 0.2724(2) 0.71826(15) 0.6654(2) 0.0449(10) Uani 1 1 d . . . . .
C30 C 0.3538(3) 0.22205(19) 0.0242(2) 0.0191(9) Uani 1 1 d . . . . .
H30 H 0.309077 0.210446 -0.008615 0.023 Uiso 1 1 calc R U . . .
C7 C 0.4809(3) 0.3984(2) 0.3467(3) 0.0316(12) Uani 1 1 d . . . . .
H7A H 0.490854 0.366122 0.317896 0.038 Uiso 1 1 calc R U . . .
H7B H 0.432907 0.415940 0.321195 0.038 Uiso 1 1 calc R U . . .
N7 N 0.4528(2) 0.19093(15) 0.48409(19) 0.0183(8) Uani 1 1 d . . . . .
C19 C 0.2353(3) 0.0268(2) 0.3050(3) 0.0271(12) Uani 1 1 d . . . . .
H19 H 0.214974 -0.008673 0.298803 0.032 Uiso 1 1 calc R U . . .
N5 N 0.3888(2) 0.18750(14) 0.07312(19) 0.0159(8) Uani 1 1 d . . . . .
C15 C 0.2835(3) 0.2232(2) 0.3691(2) 0.0199(9) Uani 1 1 d . . . . .
H15 H 0.232501 0.212240 0.375995 0.024 Uiso 1 1 calc R U . . .
C27 C 0.3305(2) 0.10647(17) 0.1274(2) 0.0156(9) Uani 1 1 d . . . . .
N6 N 0.4498(2) 0.29477(14) 0.06316(19) 0.0152(8) Uani 1 1 d . . . . .
C63 C 0.4413(3) 0.13713(19) 0.4948(3) 0.0224(11) Uani 1 1 d . . . . .
H63 H 0.436055 0.114014 0.453144 0.027 Uiso 1 1 calc R U . . .
N4 N 0.3267(2) 0.18904(14) 0.33784(19) 0.0161(8) Uani 1 1 d . . . . .
C22 C 0.3055(3) 0.05043(18) 0.1193(3) 0.0195(10) Uani 1 1 d . . . . .
C18 C 0.2336(3) 0.0540(2) 0.3706(3) 0.0271(12) Uani 1 1 d . . . . .
H18 H 0.211660 0.036942 0.409021 0.033 Uiso 1 1 calc R U . . .
C14 C 0.3093(3) 0.2760(2) 0.3934(2) 0.0201(9) Uani 1 1 d . . . . .
N3 N 0.3854(2) 0.29526(14) 0.38720(19) 0.0151(8) Uani 1 1 d . . . . .
C33 C 0.4019(3) 0.36155(19) -0.0198(3) 0.0259(11) Uani 1 1 d . . . . .
H33 H 0.397501 0.394961 -0.045209 0.031 Uiso 1 1 calc R U . . .
C31 C 0.3806(2) 0.27693(19) 0.0186(2) 0.0171(9) Uani 1 1 d . . . . .
C32 C 0.3503(3) 0.3175(2) -0.0325(3) 0.0269(11) Uani 1 1 d . . . . .
H32 H 0.304389 0.315418 -0.068068 0.032 Uiso 1 1 calc R U . . .
C29 C 0.2965(2) 0.10819(18) 0.2545(2) 0.0172(10) Uani 1 1 d . . . . .
C34 C 0.4623(3) 0.34631(17) 0.0388(2) 0.0167(10) Uani 1 1 d . . . . .
C100 C 0.1993(3) 0.7262(2) 0.6910(3) 0.0412(14) Uani 1 1 d . . . . .
H10G H 0.159820 0.739989 0.650490 0.049 Uiso 1 1 calc R U . . .
H10H H 0.205210 0.752676 0.731808 0.049 Uiso 1 1 calc R U . . .
C25 C 0.3664(3) 0.10298(19) 0.0016(3) 0.0214(10) Uani 1 1 d . . . . .
H25 H 0.386010 0.120039 -0.038157 0.026 Uiso 1 1 calc R U . . .
C9 C 0.4572(3) 0.43107(19) 0.4751(3) 0.0310(11) Uani 1 1 d . U . . .
H9AA H 0.508759 0.448629 0.488421 0.037 Uiso 0.693(8) 1 calc R U P A 1
H9AB H 0.438837 0.419720 0.521304 0.037 Uiso 0.693(8) 1 calc R U P A 1
H9BC H 0.410918 0.452206 0.453006 0.037 Uiso 0.307(8) 1 calc R U P A 2
H9BD H 0.504022 0.454277 0.477502 0.037 Uiso 0.307(8) 1 calc R U P A 2
C61 C 0.4453(3) 0.1484(2) 0.6263(3) 0.0363(14) Uani 1 1 d . . . . .
H61 H 0.443563 0.134256 0.674166 0.044 Uiso 1 1 calc R U . . .
C20 C 0.2684(3) 0.05278(18) 0.2453(3) 0.0196(10) Uani 1 1 d . . . . .
C11 C 0.3913(3) 0.34564(18) 0.4199(2) 0.0179(10) Uani 1 1 d . . . . .
C23 C 0.3119(3) 0.02195(19) 0.0508(3) 0.0263(11) Uani 1 1 d . . . . .
H23 H 0.295482 -0.014498 0.045158 0.032 Uiso 1 1 calc R U . . .
C103 C 0.2887(3) 0.6616(2) 0.6616(3) 0.0449(15) Uani 1 1 d . . . . .
H10I H 0.345772 0.654855 0.670235 0.054 Uiso 1 1 calc R U . . .
H10J H 0.266386 0.646747 0.612817 0.054 Uiso 1 1 calc R U . . .
C16 C 0.2956(3) 0.13506(18) 0.3257(2) 0.0185(10) Uani 1 1 d . . . . .
C24 C 0.3417(3) 0.0476(2) -0.0058(3) 0.0265(11) Uani 1 1 d . . . . .
H24 H 0.345888 0.028487 -0.049916 0.032 Uiso 1 1 calc R U . . .
C17 C 0.2645(3) 0.10770(19) 0.3814(3) 0.0239(11) Uani 1 1 d . . . . .
H17 H 0.263854 0.125007 0.427502 0.029 Uiso 1 1 calc R U . . .
C6 C 0.4664(3) 0.38000(18) 0.4265(2) 0.0196(10) Uani 1 1 d . . . . .
C26 C 0.3621(3) 0.13222(18) 0.0661(2) 0.0180(10) Uani 1 1 d . . . . .
C10 C 0.3964(4) 0.4736(3) 0.4328(4) 0.0316(13) Uani 0.693(8) 1 d . U P A 1
H10A H 0.421715 0.493714 0.397050 0.047 Uiso 0.693(8) 1 calc R U P A 1
H10B H 0.379617 0.498598 0.468651 0.047 Uiso 0.693(8) 1 calc R U P A 1
H10C H 0.350823 0.454354 0.407029 0.047 Uiso 0.693(8) 1 calc R U P A 1
C8 C 0.5511(3) 0.4383(2) 0.3479(3) 0.0423(15) Uani 1 1 d . . . . .
H8A H 0.536724 0.473519 0.365806 0.063 Uiso 1 1 calc R U . . .
H8B H 0.563989 0.442021 0.297968 0.063 Uiso 1 1 calc R U . . .
H8C H 0.596653 0.424236 0.380799 0.063 Uiso 1 1 calc R U . . .
U1 U 0.47789(2) 0.22455(2) 0.34968(2) 0.01276(5) Uani 1 1 d . . . . .
C21 C 0.2738(3) 0.02508(19) 0.1778(3) 0.0249(11) Uani 1 1 d . . . . .
H21 H 0.255895 -0.011028 0.171964 0.030 Uiso 1 1 calc R U . . .
C28 C 0.3252(3) 0.13405(18) 0.1945(2) 0.0167(10) Uani 1 1 d . . . . .
H28 H 0.341141 0.170619 0.199458 0.020 Uiso 1 1 calc R U . . .
C62 C 0.4366(3) 0.1139(2) 0.5649(3) 0.0263(11) Uani 1 1 d . . . . .
H62 H 0.428029 0.076454 0.569942 0.032 Uiso 1 1 calc R U . . .
C12 C 0.3208(3) 0.3584(2) 0.4469(3) 0.0376(14) Uani 1 1 d . . . . .
H12 H 0.310281 0.390645 0.471491 0.045 Uiso 1 1 calc R U . . .
C60 C 0.4564(3) 0.2041(2) 0.6167(3) 0.0334(13) Uani 1 1 d . . . . .
H60 H 0.461876 0.227942 0.657620 0.040 Uiso 1 1 calc R U . . .
C13 C 0.2693(3) 0.3147(2) 0.4306(3) 0.0400(14) Uani 1 1 d . . . . .
H13 H 0.217879 0.311646 0.442307 0.048 Uiso 1 1 calc R U . . .
C102 C 0.2509(5) 0.6372(3) 0.7207(4) 0.076(2) Uani 1 1 d . . . . .
H10K H 0.284428 0.640873 0.769266 0.091 Uiso 1 1 calc R U . . .
H10L H 0.239878 0.598506 0.710823 0.091 Uiso 1 1 calc R U . . .
C101 C 0.1729(5) 0.6700(3) 0.7186(4) 0.083(3) Uani 1 1 d . . . . .
H10M H 0.156883 0.672678 0.768048 0.100 Uiso 1 1 calc R U . . .
H10N H 0.129669 0.654157 0.683509 0.100 Uiso 1 1 calc R U . . .
O1 O 0.48105(17) 0.13937(12) 0.32062(16) 0.0168(7) Uani 1 1 d . . . . .
C64 C 0.4900(3) 0.09131(17) 0.2864(2) 0.0162(9) Uani 1 1 d . . . . .
C66 C 0.4887(3) -0.00790(18) 0.2857(3) 0.0255(11) Uani 1 1 d . . . . .
H66 H 0.480664 -0.040993 0.309331 0.031 Uiso 1 1 calc R U . . .
C65 C 0.4784(3) 0.04137(19) 0.3213(3) 0.0232(11) Uani 1 1 d . . . . .
H65 H 0.463598 0.041204 0.369076 0.028 Uiso 1 1 calc R U . . .
O3 O 0.5717(2) 0.24879(13) 0.27355(17) 0.0150(7) Uani 1 1 d . . . . .
O20 O 0.500000 0.3080(3) 0.750000 0.075(2) Uani 1 2 d S T P . .
C200 C 0.5612(10) 0.3428(7) 0.7280(9) 0.085(5) Uani 0.729(19) 1 d . U P B 1
H20A H 0.574280 0.330771 0.679856 0.102 Uiso 0.729(19) 1 calc R U P B 1
H20B H 0.609041 0.340573 0.765081 0.102 Uiso 0.729(19) 1 calc R U P B 1
C201 C 0.5323(8) 0.3981(4) 0.7223(8) 0.074(4) Uani 0.729(19) 1 d . U P B 1
H20C H 0.508294 0.406854 0.671167 0.089 Uiso 0.729(19) 1 calc R U P B 1
H20D H 0.574862 0.424158 0.738560 0.089 Uiso 0.729(19) 1 calc R U P B 1
H3 H 0.610(3) 0.2526(19) 0.286(3) 0.007(14) Uiso 1 1 d . . . . .
C10A C 0.4456(10) 0.4096(7) 0.5644(9) 0.038(5) Uani 0.307(8) 1 d . . P A 2
H10D H 0.398264 0.387643 0.561734 0.056 Uiso 0.307(8) 1 calc R U P A 2
H10E H 0.441085 0.441151 0.595673 0.056 Uiso 0.307(8) 1 calc R U P A 2
H10F H 0.491184 0.388235 0.585546 0.056 Uiso 0.307(8) 1 calc R U P A 2
C2 C 0.560(3) 0.339(2) 0.770(3) 0.101(11) Uani 0.271(19) 1 d . U P B 2
H2A H 0.590244 0.342476 0.728018 0.121 Uiso 0.271(19) 1 calc R U P B 2
H2B H 0.595090 0.321949 0.811189 0.121 Uiso 0.271(19) 1 calc R U P B 2
C1 C 0.541(2) 0.3929(15) 0.792(2) 0.102(12) Uani 0.271(19) 1 d . U P B 2
H1A H 0.582003 0.420100 0.790328 0.123 Uiso 0.271(19) 1 calc R U P B 2
H1B H 0.520835 0.394092 0.840366 0.123 Uiso 0.271(19) 1 calc R U P B 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
C59 N7 1.335(6) . ?
C59 C60 1.386(6) . ?
O10 C100 1.399(6) . ?
O10 C103 1.410(6) . ?
C30 N5 1.293(5) . ?
C30 C31 1.419(6) . ?
C7 C8 1.532(6) . ?
C7 C6 1.556(6) . ?
N7 C63 1.341(6) . ?
N7 U1 2.645(3) . ?
C19 C18 1.355(7) . ?
C19 C20 1.431(6) . ?
N5 C26 1.419(5) . ?
N5 U1 2.624(3) 2_655 ?
C15 N4 1.292(5) . ?
C15 C14 1.405(6) . ?
C27 C28 1.394(6) . ?
C27 C22 1.429(6) . ?
C27 C26 1.438(6) . ?
N6 C34 1.355(5) . ?
N6 C31 1.385(5) . ?
N6 U1 2.508(3) 2_655 ?
C63 C62 1.392(6) . ?
N4 C16 1.419(5) . ?
N4 U1 2.681(4) . ?
C22 C21 1.395(6) . ?
C22 C23 1.431(6) . ?
C18 C17 1.410(6) . ?
C14 C13 1.389(6) . ?
C14 N3 1.393(5) . ?
N3 C11 1.356(5) . ?
N3 U1 2.488(3) . ?
C33 C32 1.379(6) . ?
C33 C34 1.402(6) . ?
C31 C32 1.392(6) . ?
C29 C28 1.397(6) . ?
C29 C20 1.430(6) . ?
C29 C16 1.439(6) . ?
C34 C6 1.513(6) 2_655 ?
C100 C101 1.544(9) . ?
C25 C26 1.372(6) . ?
C25 C24 1.412(6) . ?
C9 C6 1.540(6) . ?
C9 C10 1.570(8) . ?
C9 C10A 1.727(18) . ?
C61 C62 1.377(7) . ?
C61 C60 1.381(7) . ?
C20 C21 1.402(6) . ?
C11 C12 1.391(6) . ?
C11 C6 1.513(6) . ?
C23 C24 1.355(6) . ?
C103 C102 1.448(8) . ?
C16 C17 1.373(6) . ?
U1 O1 2.139(3) . ?
U1 O3 2.322(3) 2_655 ?
U1 O3 2.325(3) . ?
U1 U1 3.7696(3) 2_655 ?
C12 C13 1.379(7) . ?
C102 C101 1.540(10) . ?
O1 C64 1.340(5) . ?
C64 C65 1.394(6) . ?
C64 C64 1.402(8) 2_655 ?
C66 C65 1.382(6) . ?
C66 C66 1.392(9) 2_655 ?
O20 C2 1.28(5) 2_656 ?
O20 C2 1.28(5) . ?
O20 C200 1.438(16) . ?
O20 C200 1.438(16) 2_656 ?
C200 C201 1.431(18) . ?
C201 C201 1.59(2) 2_656 ?
C2 C1 1.42(6) . ?
C1 C1 1.89(8) 2_656 ?

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
N7 C59 C60 123.4(5) . . ?
C100 O10 C103 109.9(4) . . ?
N5 C30 C31 122.7(4) . . ?
C8 C7 C6 113.6(4) . . ?
C59 N7 C63 117.1(4) . . ?
C59 N7 U1 123.8(3) . . ?
C63 N7 U1 118.7(3) . . ?
C18 C19 C20 120.0(4) . . ?
C30 N5 C26 116.6(4) . . ?
C30 N5 U1 113.9(3) . 2_655 ?
C26 N5 U1 127.6(3) . 2_655 ?
N4 C15 C14 123.5(4) . . ?
C28 C27 C22 119.3(4) . . ?
C28 C27 C26 122.2(4) . . ?
C22 C27 C26 118.5(4) . . ?
C34 N6 C31 105.3(4) . . ?
C34 N6 U1 138.3(3) . 2_655 ?
C31 N6 U1 116.0(3) . 2_655 ?
N7 C63 C62 123.7(4) . . ?
C15 N4 C16 116.1(4) . . ?
C15 N4 U1 110.9(3) . . ?
C16 N4 U1 129.7(3) . . ?
C21 C22 C27 119.2(4) . . ?
C21 C22 C23 121.5(4) . . ?
C27 C22 C23 119.3(4) . . ?
C19 C18 C17 121.0(4) . . ?
C13 C14 N3 109.7(4) . . ?
C13 C14 C15 128.1(4) . . ?
N3 C14 C15 122.1(4) . . ?
C11 N3 C14 106.1(4) . . ?
C11 N3 U1 137.3(3) . . ?
C14 N3 U1 114.7(3) . . ?
C32 C33 C34 106.9(4) . . ?
N6 C31 C32 110.7(4) . . ?
N6 C31 C30 120.4(4) . . ?
C32 C31 C30 128.6(4) . . ?
C33 C32 C31 106.3(4) . . ?
C28 C29 C20 118.9(4) . . ?
C28 C29 C16 122.2(4) . . ?
C20 C29 C16 118.8(4) . . ?
N6 C34 C33 110.8(4) . . ?
N6 C34 C6 121.5(4) . 2_655 ?
C33 C34 C6 127.7(4) . 2_655 ?
O10 C100 C101 107.4(5) . . ?
C26 C25 C24 121.4(4) . . ?
C6 C9 C10 111.9(5) . . ?
C6 C9 C10A 108.6(6) . . ?
C62 C61 C60 119.8(5) . . ?
C21 C20 C29 119.2(4) . . ?
C21 C20 C19 121.4(4) . . ?
C29 C20 C19 119.4(4) . . ?
N3 C11 C12 110.1(4) . . ?
N3 C11 C6 122.6(4) . . ?
C12 C11 C6 127.3(4) . . ?
C24 C23 C22 120.6(4) . . ?
O10 C103 C102 104.7(5) . . ?
C17 C16 N4 120.7(4) . . ?
C17 C16 C29 119.1(4) . . ?
N4 C16 C29 120.2(4) . . ?
C23 C24 C25 120.5(4) . . ?
C16 C17 C18 121.6(4) . . ?
C11 C6 C34 110.1(4) . 2_655 ?
C11 C6 C9 109.4(4) . . ?
C34 C6 C9 110.3(4) 2_655 . ?
C11 C6 C7 109.7(4) . . ?
C34 C6 C7 107.9(4) 2_655 . ?
C9 C6 C7 109.5(4) . . ?
C25 C26 N5 120.6(4) . . ?
C25 C26 C27 119.7(4) . . ?
N5 C26 C27 119.7(4) . . ?
O1 U1 O3 91.83(11) . 2_655 ?
O1 U1 O3 93.28(11) . . ?
O3 U1 O3 63.58(15) 2_655 . ?
O1 U1 N3 140.88(11) . . ?
O3 U1 N3 86.07(11) 2_655 . ?
O3 U1 N3 119.95(11) . . ?
O1 U1 N6 141.64(11) . 2_655 ?
O3 U1 N6 119.62(11) 2_655 2_655 ?
O3 U1 N6 83.21(11) . 2_655 ?
N3 U1 N6 68.16(11) . 2_655 ?
O1 U1 N5 75.22(11) . 2_655 ?
O3 U1 N5 138.49(11) 2_655 2_655 ?
O3 U1 N5 77.74(11) . 2_655 ?
N3 U1 N5 128.41(11) . 2_655 ?
N6 U1 N5 66.68(11) 2_655 2_655 ?
O1 U1 N7 86.38(11) . . ?
O3 U1 N7 149.79(11) 2_655 . ?
O3 U1 N7 146.62(11) . . ?
N3 U1 N7 76.75(11) . . ?
N6 U1 N7 76.80(11) 2_655 . ?
N5 U1 N7 69.90(11) 2_655 . ?
O1 U1 N4 74.20(11) . . ?
O3 U1 N4 78.67(11) 2_655 . ?
O3 U1 N4 139.95(11) . . ?
N3 U1 N4 67.08(11) . . ?
N6 U1 N4 129.74(10) 2_655 . ?
N5 U1 N4 131.80(11) 2_655 . ?
N7 U1 N4 71.83(11) . . ?
O1 U1 U1 75.65(8) . 2_655 ?
O3 U1 U1 35.81(8) 2_655 2_655 ?
O3 U1 U1 35.75(8) . 2_655 ?
N3 U1 U1 118.82(8) . 2_655 ?
N6 U1 U1 116.39(8) 2_655 2_655 ?
N5 U1 U1 102.87(7) 2_655 2_655 ?
N7 U1 U1 161.91(8) . 2_655 ?
N4 U1 U1 104.50(7) . 2_655 ?
C22 C21 C20 121.5(4) . . ?
C27 C28 C29 121.7(4) . . ?
C61 C62 C63 117.7(5) . . ?
C13 C12 C11 107.6(4) . . ?
C61 C60 C59 118.3(5) . . ?
C12 C13 C14 106.6(4) . . ?
C103 C102 C101 104.1(5) . . ?
C102 C101 C100 100.2(5) . . ?
C64 O1 U1 165.0(3) . . ?
O1 C64 C65 121.4(4) . . ?
O1 C64 C64 119.2(2) . 2_655 ?
C65 C64 C64 119.4(3) . 2_655 ?
C65 C66 C66 119.9(3) . 2_655 ?
C66 C65 C64 120.7(4) . . ?
U1 O3 U1 108.43(14) 2_655 . ?
C2 O20 C2 107(4) 2_656 . ?
C200 O20 C200 108.1(12) . 2_656 ?
O20 C200 C201 108.7(10) . . ?
C200 C201 C201 102.4(7) . 2_656 ?
O20 C2 C1 114(4) . . ?
C2 C1 C1 87(3) . 2_656 ?

_refine_diff_density_max         0.959
_refine_diff_density_min         -0.775
_refine_diff_density_rms         0.124


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

data_compound6
_database_code_depnum_ccdc_archive 'CCDC 1984906'
loop_
_audit_author_name
_audit_author_address
'Bradley E. Cowie'
;The University of Edinburgh
United Kingdom
;
_audit_update_record             
;
2020-02-18 deposited with the CCDC.	2020-06-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        '[{(py)U(Cl)2U(O2C6H4)(py)}(LA)]'
_chemical_name_common            'Compound 6.solvent'
_chemical_melting_point          ?
_chemical_formula_moiety         'C74 H62 Cl2 N10 O2 U2'
_chemical_formula_sum            'C74 H62 Cl2 N10 O2 U2'
_chemical_formula_weight         1670.29

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_H-M_alt        '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_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, z'

_cell_length_a                   14.0058(3)
_cell_length_b                   21.7361(5)
_cell_length_c                   14.7736(3)
_cell_angle_alpha                90
_cell_angle_beta                 105.395(2)
_cell_angle_gamma                90
_cell_volume                     4336.17(17)
_cell_formula_units_Z            2
_cell_measurement_temperature    120.0(1)
_cell_measurement_reflns_used    11270
_cell_measurement_theta_min      3.4130
_cell_measurement_theta_max      26.7980

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.279
_exptl_crystal_F_000             1620
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.346
_exptl_crystal_size_mid          0.138
_exptl_crystal_size_min          0.095
_exptl_absorpt_coefficient_mu    3.833
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.793
_exptl_absorpt_correction_T_max  0.928
_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      120.0(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Eos
_diffrn_detector_area_resol_mean 16.1042
_diffrn_reflns_number            47380
_diffrn_reflns_av_unetI/netI     0.0602
_diffrn_reflns_av_R_equivalents  0.0670
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.857
_diffrn_reflns_theta_max         26.372
_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             9110
_reflns_number_gt                6549
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       '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-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_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  21.00   1.00   55.00    --  -17.88 -99.00 150.00   46
  2  ω    -87.00   1.00   1.00   55.00    --  -17.88 -37.00  30.00   88
  3  ω    -85.00  -1.00   1.00   55.00    --  -17.88 -57.00   0.00   84
  4  ω    -35.00  49.00   1.00   55.00    --  -17.88  57.00-150.00   84
  5  ω    -48.00  36.00   1.00   55.00    --   19.60 -57.00  60.00   84
  6  ω    -48.00  36.00   1.00   55.00    --   19.60 -57.00-120.00   84
  7  ω    -35.00  32.00   1.00   55.00    --  -17.88  57.00   0.00   67
;
_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) is positionally disordered over two positions, so it is split into two
parts and refined in a 0.53:0.47 ratio. A molecule of pyridine that is 
coordinated to uranium is positionally disordered over two positions, so it 
is split into two parts and refined in a 0.84:0.16 ratio, and the thermal 
ellipsoids are restrained to be similar to one another through the use
of the SIMU command. Furthermore, the geometry of N(5), C(59), C(60), C(61), 
C(62) and C(63) is constrained using AFIX 66. Finally, the lattice solvent
exhibited unresolvable disorder and was removed using a solvent mask
(393.3 electrons per cell = ~5 molecules of pyridine).,Solvent Mask
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0369P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9110
_refine_ls_number_parameters     471
_refine_ls_number_restraints     120
_refine_ls_R_factor_all          0.0632
_refine_ls_R_factor_gt           0.0382
_refine_ls_wR_factor_ref         0.0814
_refine_ls_wR_factor_gt          0.0746
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_restrained_S_all      1.018
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.47537(2) 0.34588(2) 0.75403(2) 0.02654(6) Uani 1 1 d . . . . .
Cl1 Cl 0.36273(12) 0.250000 0.80373(11) 0.0277(4) Uani 1 2 d S T P A .
Cl2 Cl 0.44265(13) 0.250000 0.62201(11) 0.0319(4) Uani 1 2 d S T P A .
O1 O 0.6115(2) 0.31165(14) 0.8331(2) 0.0295(8) Uani 1 1 d . . . . .
N4 N 0.4769(3) 0.36813(17) 0.9269(3) 0.0277(9) Uani 1 1 d . . . . .
N2 N 0.3916(3) 0.39732(18) 0.6076(3) 0.0327(10) Uani 1 1 d . . . . .
N1 N 0.5957(3) 0.36815(18) 0.6511(3) 0.0348(10) Uani 1 1 d . . . . .
N5 N 0.538(3) 0.4562(18) 0.804(3) 0.032(3) Uani 0.16(3) 1 d G U P A 1
C63 C 0.636(3) 0.4575(18) 0.857(3) 0.037(2) Uani 0.16(3) 1 d G U P A 1
H63 H 0.667022 0.421458 0.883186 0.045 Uiso 0.16(3) 1 calc R U P A 1
C62 C 0.688(3) 0.513(3) 0.870(3) 0.039(2) Uani 0.16(3) 1 d G U P A 1
H62 H 0.753835 0.513564 0.904589 0.046 Uiso 0.16(3) 1 calc R U P A 1
C61 C 0.642(5) 0.5665(19) 0.830(3) 0.041(2) Uani 0.16(3) 1 d G U P A 1
H61 H 0.676462 0.603448 0.838529 0.050 Uiso 0.16(3) 1 calc R U P A 1
C60 C 0.543(4) 0.5652(17) 0.778(3) 0.0441(19) Uani 0.16(3) 1 d G U P A 1
H60 H 0.512275 0.601227 0.751064 0.053 Uiso 0.16(3) 1 calc R U P A 1
C59 C 0.491(3) 0.510(2) 0.765(3) 0.046(2) Uani 0.16(3) 1 d G U P A 1
H59 H 0.425460 0.509121 0.729660 0.055 Uiso 0.16(3) 1 calc R U P A 1
N3 N 0.3241(3) 0.39810(17) 0.7654(3) 0.0299(9) Uani 1 1 d . . . . .
C57 C 0.7021(5) 0.250000 0.6719(4) 0.0279(16) Uani 1 2 d S T P . .
H57 H 0.633444 0.249999 0.649845 0.034 Uiso 1 2 calc R U P . .
C28 C 0.5518(5) 0.250000 1.0144(4) 0.0251(15) Uani 1 2 d S T P . .
H28 H 0.496366 0.249999 0.963171 0.030 Uiso 1 2 calc R U P . .
C56 C 0.7508(4) 0.3067(2) 0.6876(3) 0.0313(12) Uani 1 1 d . . . . .
C1 C 0.5534(4) 0.3976(2) 0.5742(4) 0.0412(14) Uani 1 1 d . . . . .
H1 H 0.592276 0.409846 0.535252 0.049 Uiso 1 1 calc R U . . .
C15 C 0.3967(4) 0.3946(2) 0.9350(3) 0.0293(11) Uani 1 1 d . . . . .
H15 H 0.391938 0.405137 0.994643 0.035 Uiso 1 1 calc R U . . .
C16 C 0.5551(4) 0.3645(2) 1.0110(3) 0.0291(11) Uani 1 1 d . . . . .
C29 C 0.5913(4) 0.3065(2) 1.0509(3) 0.0275(11) Uani 1 1 d . . . . .
C11 C 0.2365(3) 0.4160(2) 0.7071(3) 0.0303(11) Uani 1 1 d . . . . .
C64 C 0.6953(3) 0.2817(2) 0.8817(3) 0.0288(11) Uani 1 1 d . . . . .
C5 C 0.3007(4) 0.4187(2) 0.5637(3) 0.0353(12) Uani 1 1 d . . . . .
C14 C 0.3164(4) 0.4081(2) 0.8572(3) 0.0314(12) Uani 1 1 d . . . . .
C55 C 0.7016(4) 0.3642(2) 0.6747(3) 0.0314(12) Uani 1 1 d . . . . .
C17 C 0.5983(4) 0.4178(2) 1.0526(3) 0.0382(13) Uani 1 1 d . . . . .
H17 H 0.575851 0.455459 1.025079 0.046 Uiso 1 1 calc R U . . .
C7 C 0.1767(4) 0.3404(3) 0.5789(4) 0.0426(13) Uani 1 1 d . . . . .
H7AA H 0.154388 0.336617 0.511121 0.051 Uiso 0.468(11) 1 calc R U P B 1
H7AB H 0.233955 0.313894 0.600066 0.051 Uiso 0.468(11) 1 calc R U P B 1
H7BC H 0.227626 0.312949 0.614233 0.051 Uiso 0.532(11) 1 calc R U P B 2
H7BD H 0.117633 0.333687 0.600061 0.051 Uiso 0.532(11) 1 calc R U P B 2
C2 C 0.4513(4) 0.4118(2) 0.5469(3) 0.0378(13) Uani 1 1 d . . . . .
C6 C 0.2124(4) 0.4091(2) 0.6025(3) 0.0368(12) Uani 1 1 d . . . . .
C21 C 0.7091(5) 0.250000 1.1743(4) 0.0386(19) Uani 1 2 d S T P . .
H21 H 0.760175 0.250000 1.229413 0.046 Uiso 1 2 calc R U P . .
C54 C 0.7549(4) 0.4174(3) 0.6864(4) 0.0412(13) Uani 1 1 d . . . . .
H54 H 0.721849 0.454893 0.677174 0.049 Uiso 1 1 calc R U . . .
C13 C 0.2237(4) 0.4319(2) 0.8547(4) 0.0386(13) Uani 1 1 d . . . . .
H13 H 0.199917 0.442343 0.905712 0.046 Uiso 1 1 calc R U . . .
C65 C 0.7791(4) 0.3133(3) 0.9297(4) 0.0410(13) Uani 1 1 d . . . . .
H65 H 0.778713 0.356098 0.930627 0.049 Uiso 1 1 calc R U . . .
C18 C 0.6755(4) 0.4167(3) 1.1357(4) 0.0476(15) Uani 1 1 d . . . . .
H18 H 0.701943 0.453514 1.163471 0.057 Uiso 1 1 calc R U . . .
C12 C 0.1737(4) 0.4368(2) 0.7599(4) 0.0386(13) Uani 1 1 d . . . . .
H12 H 0.109515 0.451448 0.735978 0.046 Uiso 1 1 calc R U . . .
C20 C 0.6724(4) 0.3057(2) 1.1348(3) 0.0324(12) Uani 1 1 d . . . . .
C51 C 0.8568(4) 0.3063(2) 0.7139(3) 0.0351(12) Uani 1 1 d . . . . .
C19 C 0.7116(4) 0.3627(2) 1.1756(3) 0.0399(14) Uani 1 1 d . . . . .
H19 H 0.762833 0.362770 1.230545 0.048 Uiso 1 1 calc R U . . .
C9 C 0.1288(4) 0.4540(3) 0.5553(4) 0.0561(17) Uani 1 1 d . . . . .
H9A H 0.111753 0.447107 0.488006 0.067 Uiso 1 1 calc R U . . .
H9B H 0.070761 0.444273 0.576619 0.067 Uiso 1 1 calc R U . . .
C66 C 0.8632(4) 0.2817(2) 0.9762(4) 0.0448(14) Uani 1 1 d . . . . .
H66 H 0.919877 0.303075 1.007451 0.054 Uiso 1 1 calc R U . . .
C50 C 0.9073(6) 0.250000 0.7263(5) 0.0404(19) Uani 1 2 d S T P . .
H50 H 0.976186 0.250001 0.743251 0.048 Uiso 1 2 calc R U P . .
C52 C 0.9085(4) 0.3634(3) 0.7260(4) 0.0459(15) Uani 1 1 d . . . . .
H52 H 0.977327 0.363544 0.743803 0.055 Uiso 1 1 calc R U . . .
C4 C 0.3017(4) 0.4450(3) 0.4773(4) 0.0521(17) Uani 1 1 d . . . . .
H4 H 0.247821 0.461929 0.433530 0.063 Uiso 1 1 calc R U . . .
C10 C 0.1524(5) 0.5221(3) 0.5736(5) 0.074(2) Uani 1 1 d . . . . .
H10A H 0.177746 0.528820 0.639889 0.111 Uiso 1 1 calc R U . . .
H10B H 0.093239 0.545900 0.550339 0.111 Uiso 1 1 calc R U . . .
H10C H 0.201137 0.534408 0.542165 0.111 Uiso 1 1 calc R U . . .
C53 C 0.8599(4) 0.4166(3) 0.7123(4) 0.0495(15) Uani 1 1 d . . . . .
H53 H 0.894956 0.453391 0.719703 0.059 Uiso 1 1 calc R U . . .
C3 C 0.3956(4) 0.4412(3) 0.4692(4) 0.0553(18) Uani 1 1 d . . . . .
H3 H 0.418064 0.456024 0.419538 0.066 Uiso 1 1 calc R U . . .
C8 C 0.0973(8) 0.3162(5) 0.6181(9) 0.048(4) Uani 0.468(11) 1 d . . P B 1
H8A H 0.120970 0.314006 0.685297 0.071 Uiso 0.468(11) 1 calc R U P B 1
H8B H 0.078639 0.275806 0.593377 0.071 Uiso 0.468(11) 1 calc R U P B 1
H8C H 0.040906 0.342987 0.601220 0.071 Uiso 0.468(11) 1 calc R U P B 1
C8A C 0.1550(11) 0.3241(6) 0.4799(8) 0.083(5) Uani 0.532(11) 1 d . . P B 2
H8AA H 0.104714 0.351084 0.443957 0.125 Uiso 0.532(11) 1 calc R U P B 2
H8AB H 0.131928 0.282388 0.471447 0.125 Uiso 0.532(11) 1 calc R U P B 2
H8AC H 0.213942 0.328182 0.458902 0.125 Uiso 0.532(11) 1 calc R U P B 2
N5A N 0.5369(6) 0.4576(4) 0.7830(8) 0.0322(17) Uani 0.84(3) 1 d . U P A 2
C63A C 0.6263(7) 0.4706(5) 0.8368(7) 0.0351(17) Uani 0.84(3) 1 d . U P A 2
H63A H 0.665547 0.438035 0.866244 0.042 Uiso 0.84(3) 1 calc R U P A 2
C62A C 0.6652(8) 0.5293(5) 0.8522(7) 0.0394(17) Uani 0.84(3) 1 d . U P A 2
H62A H 0.729059 0.535946 0.889790 0.047 Uiso 0.84(3) 1 calc R U P A 2
C61A C 0.6068(11) 0.5773(4) 0.8104(8) 0.0425(17) Uani 0.84(3) 1 d . U P A 2
H61A H 0.630898 0.617399 0.818074 0.051 Uiso 0.84(3) 1 calc R U P A 2
C60A C 0.5140(10) 0.5659(4) 0.7579(8) 0.0473(16) Uani 0.84(3) 1 d . U P A 2
H60A H 0.473353 0.598605 0.731084 0.057 Uiso 0.84(3) 1 calc R U P A 2
C59A C 0.4788(7) 0.5076(5) 0.7437(8) 0.0456(16) Uani 0.84(3) 1 d . U P A 2
H59A H 0.414685 0.500989 0.706841 0.055 Uiso 0.84(3) 1 calc R U P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 O1 2.091(3) . ?
U1 N2 2.441(4) . ?
U1 N3 2.448(4) . ?
U1 N5A 2.574(7) . ?
U1 N5 2.59(4) . ?
U1 N4 2.594(4) . ?
U1 N1 2.598(4) . ?
U1 Cl2 2.8077(10) . ?
U1 Cl1 2.8260(11) . ?
O1 C64 1.367(5) . ?
N4 C15 1.296(6) . ?
N4 C16 1.424(6) . ?
N2 C5 1.349(6) . ?
N2 C2 1.414(6) . ?
N1 C1 1.301(6) . ?
N1 C55 1.433(6) . ?
N5 C63 1.3900 . ?
N5 C59 1.3900 . ?
C63 C62 1.3900 . ?
C63 H63 0.9300 . ?
C62 C61 1.3900 . ?
C62 H62 0.9300 . ?
C61 C60 1.3900 . ?
C61 H61 0.9300 . ?
C60 C59 1.3900 . ?
C60 H60 0.9300 . ?
C59 H59 0.9300 . ?
N3 C11 1.356(6) . ?
N3 C14 1.407(6) . ?
C57 C56 1.398(6) . ?
C57 C56 1.398(6) 4_565 ?
C57 H57 0.9300 . ?
C28 C29 1.395(5) 4_565 ?
C28 C29 1.395(5) . ?
C28 H28 0.9300 . ?
C56 C55 1.415(7) . ?
C56 C51 1.431(6) . ?
C1 C2 1.414(7) . ?
C1 H1 0.9300 . ?
C15 C14 1.409(7) . ?
C15 H15 0.9300 . ?
C16 C17 1.375(6) . ?
C16 C29 1.426(6) . ?
C29 C20 1.442(6) . ?
C11 C12 1.397(7) . ?
C11 C6 1.500(7) . ?
C64 C64 1.378(9) 4_565 ?
C64 C65 1.382(6) . ?
C5 C4 1.402(7) . ?
C5 C6 1.509(7) . ?
C14 C13 1.388(7) . ?
C55 C54 1.362(7) . ?
C17 C18 1.404(7) . ?
C17 H17 0.9300 . ?
C7 C8A 1.457(12) . ?
C7 C8 1.481(11) . ?
C7 C6 1.584(7) . ?
C7 H7AA 0.9700 . ?
C7 H7AB 0.9700 . ?
C7 H7BC 0.9700 . ?
C7 H7BD 0.9700 . ?
C2 C3 1.363(7) . ?
C6 C9 1.542(7) . ?
C21 C20 1.383(6) . ?
C21 C20 1.383(6) 4_565 ?
C21 H21 0.9300 . ?
C54 C53 1.418(7) . ?
C54 H54 0.9300 . ?
C13 C12 1.393(7) . ?
C13 H13 0.9300 . ?
C65 C66 1.381(7) . ?
C65 H65 0.9300 . ?
C18 C19 1.351(7) . ?
C18 H18 0.9300 . ?
C12 H12 0.9300 . ?
C20 C19 1.422(6) . ?
C51 C50 1.401(6) . ?
C51 C52 1.425(7) . ?
C19 H19 0.9300 . ?
C9 C10 1.524(8) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C66 C66 1.376(10) 4_565 ?
C66 H66 0.9300 . ?
C50 H50 0.9300 . ?
C52 C53 1.328(7) . ?
C52 H52 0.9300 . ?
C4 C3 1.353(7) . ?
C4 H4 0.9300 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C53 H53 0.9300 . ?
C3 H3 0.9300 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C8A H8AA 0.9600 . ?
C8A H8AB 0.9600 . ?
C8A H8AC 0.9600 . ?
N5A C63A 1.323(7) . ?
N5A C59A 1.389(8) . ?
C63A C62A 1.383(8) . ?
C63A H63A 0.9300 . ?
C62A C61A 1.368(9) . ?
C62A H62A 0.9300 . ?
C61A C60A 1.349(9) . ?
C61A H61A 0.9300 . ?
C60A C59A 1.356(10) . ?
C60A H60A 0.9300 . ?
C59A H59A 0.9300 . ?

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 N2 144.16(13) . . ?
O1 U1 N3 143.54(12) . . ?
N2 U1 N3 68.10(13) . . ?
O1 U1 N5A 91.6(2) . . ?
N2 U1 N5A 77.1(3) . . ?
N3 U1 N5A 79.0(2) . . ?
O1 U1 N5 88.9(10) . . ?
N2 U1 N5 82.9(9) . . ?
N3 U1 N5 77.5(12) . . ?
O1 U1 N4 75.42(12) . . ?
N2 U1 N4 131.57(13) . . ?
N3 U1 N4 68.12(12) . . ?
N5A U1 N4 75.2(3) . . ?
N5 U1 N4 68.3(11) . . ?
O1 U1 N1 75.88(12) . . ?
N2 U1 N1 68.28(13) . . ?
N3 U1 N1 131.41(12) . . ?
N5A U1 N1 71.4(2) . . ?
N5 U1 N1 76.9(13) . . ?
N4 U1 N1 134.79(13) . . ?
O1 U1 Cl2 94.61(9) . . ?
N2 U1 Cl2 76.88(9) . . ?
N3 U1 Cl2 114.02(10) . . ?
N5A U1 Cl2 143.3(2) . . ?
N5 U1 Cl2 150.0(12) . . ?
N4 U1 Cl2 141.22(9) . . ?
N1 U1 Cl2 75.12(9) . . ?
O1 U1 Cl1 94.68(9) . . ?
N2 U1 Cl1 113.44(10) . . ?
N3 U1 Cl1 76.78(9) . . ?
N5A U1 Cl1 146.9(2) . . ?
N5 U1 Cl1 140.9(12) . . ?
N4 U1 Cl1 74.99(9) . . ?
N1 U1 Cl1 141.55(9) . . ?
Cl2 U1 Cl1 68.51(4) . . ?
U1 Cl1 U1 95.03(5) . 4_565 ?
U1 Cl2 U1 95.86(5) 4_565 . ?
C64 O1 U1 172.4(3) . . ?
C15 N4 C16 115.4(4) . . ?
C15 N4 U1 113.1(3) . . ?
C16 N4 U1 130.7(3) . . ?
C5 N2 C2 105.0(4) . . ?
C5 N2 U1 139.0(3) . . ?
C2 N2 U1 116.0(3) . . ?
C1 N1 C55 116.4(4) . . ?
C1 N1 U1 112.8(3) . . ?
C55 N1 U1 129.5(3) . . ?
C63 N5 C59 120.0 . . ?
C63 N5 U1 113(2) . . ?
C59 N5 U1 125(2) . . ?
N5 C63 C62 120.0 . . ?
N5 C63 H63 120.0 . . ?
C62 C63 H63 120.0 . . ?
C61 C62 C63 120.0 . . ?
C61 C62 H62 120.0 . . ?
C63 C62 H62 120.0 . . ?
C62 C61 C60 120.0 . . ?
C62 C61 H61 120.0 . . ?
C60 C61 H61 120.0 . . ?
C61 C60 C59 120.0 . . ?
C61 C60 H60 120.0 . . ?
C59 C60 H60 120.0 . . ?
C60 C59 N5 120.0 . . ?
C60 C59 H59 120.0 . . ?
N5 C59 H59 120.0 . . ?
C11 N3 C14 106.2(4) . . ?
C11 N3 U1 138.1(3) . . ?
C14 N3 U1 115.3(3) . . ?
C56 C57 C56 123.7(6) . 4_565 ?
C56 C57 H57 118.2 . . ?
C56 C57 H57 118.2 4_565 . ?
C29 C28 C29 123.4(6) 4_565 . ?
C29 C28 H28 118.3 4_565 . ?
C29 C28 H28 118.3 . . ?
C57 C56 C55 123.9(5) . . ?
C57 C56 C51 117.7(5) . . ?
C55 C56 C51 118.3(5) . . ?
N1 C1 C2 123.2(5) . . ?
N1 C1 H1 118.4 . . ?
C2 C1 H1 118.4 . . ?
N4 C15 C14 122.8(4) . . ?
N4 C15 H15 118.6 . . ?
C14 C15 H15 118.6 . . ?
C17 C16 N4 119.2(4) . . ?
C17 C16 C29 119.6(4) . . ?
N4 C16 C29 121.2(4) . . ?
C28 C29 C16 123.8(4) . . ?
C28 C29 C20 117.6(5) . . ?
C16 C29 C20 118.6(4) . . ?
N3 C11 C12 109.7(4) . . ?
N3 C11 C6 122.9(4) . . ?
C12 C11 C6 127.3(5) . . ?
O1 C64 C64 118.4(2) . 4_565 ?
O1 C64 C65 121.7(4) . . ?
C64 C64 C65 119.8(3) 4_565 . ?
N2 C5 C4 110.0(5) . . ?
N2 C5 C6 122.3(4) . . ?
C4 C5 C6 127.6(5) . . ?
C13 C14 N3 110.0(4) . . ?
C13 C14 C15 129.7(5) . . ?
N3 C14 C15 120.3(4) . . ?
C54 C55 C56 120.1(5) . . ?
C54 C55 N1 118.5(5) . . ?
C56 C55 N1 121.4(4) . . ?
C16 C17 C18 121.4(5) . . ?
C16 C17 H17 119.3 . . ?
C18 C17 H17 119.3 . . ?
C8A C7 C6 114.8(7) . . ?
C8 C7 C6 118.4(6) . . ?
C8 C7 H7AA 107.7 . . ?
C6 C7 H7AA 107.7 . . ?
C8 C7 H7AB 107.7 . . ?
C6 C7 H7AB 107.7 . . ?
H7AA C7 H7AB 107.1 . . ?
C8A C7 H7BC 108.6 . . ?
C6 C7 H7BC 108.6 . . ?
C8A C7 H7BD 108.6 . . ?
C6 C7 H7BD 108.6 . . ?
H7BC C7 H7BD 107.5 . . ?
C3 C2 C1 130.7(5) . . ?
C3 C2 N2 109.6(5) . . ?
C1 C2 N2 119.6(4) . . ?
C11 C6 C5 113.3(4) . . ?
C11 C6 C9 109.8(4) . . ?
C5 C6 C9 110.0(4) . . ?
C11 C6 C7 107.0(4) . . ?
C5 C6 C7 106.8(4) . . ?
C9 C6 C7 109.9(4) . . ?
C20 C21 C20 122.3(6) . 4_565 ?
C20 C21 H21 118.8 . . ?
C20 C21 H21 118.8 4_565 . ?
C55 C54 C53 121.2(5) . . ?
C55 C54 H54 119.4 . . ?
C53 C54 H54 119.4 . . ?
C14 C13 C12 105.9(5) . . ?
C14 C13 H13 127.1 . . ?
C12 C13 H13 127.1 . . ?
C66 C65 C64 120.3(5) . . ?
C66 C65 H65 119.9 . . ?
C64 C65 H65 119.9 . . ?
C19 C18 C17 120.6(5) . . ?
C19 C18 H18 119.7 . . ?
C17 C18 H18 119.7 . . ?
C13 C12 C11 108.2(5) . . ?
C13 C12 H12 125.9 . . ?
C11 C12 H12 125.9 . . ?
C21 C20 C19 121.7(5) . . ?
C21 C20 C29 119.5(5) . . ?
C19 C20 C29 118.7(5) . . ?
C50 C51 C52 121.5(5) . . ?
C50 C51 C56 119.5(5) . . ?
C52 C51 C56 119.0(5) . . ?
C18 C19 C20 121.0(5) . . ?
C18 C19 H19 119.5 . . ?
C20 C19 H19 119.5 . . ?
C10 C9 C6 115.5(5) . . ?
C10 C9 H9A 108.4 . . ?
C6 C9 H9A 108.4 . . ?
C10 C9 H9B 108.4 . . ?
C6 C9 H9B 108.4 . . ?
H9A C9 H9B 107.5 . . ?
C66 C66 C65 119.9(3) 4_565 . ?
C66 C66 H66 120.0 4_565 . ?
C65 C66 H66 120.0 . . ?
C51 C50 C51 121.7(7) . 4_565 ?
C51 C50 H50 119.1 . . ?
C51 C50 H50 119.1 4_565 . ?
C53 C52 C51 121.1(5) . . ?
C53 C52 H52 119.5 . . ?
C51 C52 H52 119.5 . . ?
C3 C4 C5 107.5(5) . . ?
C3 C4 H4 126.2 . . ?
C5 C4 H4 126.2 . . ?
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 . . ?
C52 C53 C54 120.3(6) . . ?
C52 C53 H53 119.9 . . ?
C54 C53 H53 119.9 . . ?
C4 C3 C2 107.8(5) . . ?
C4 C3 H3 126.1 . . ?
C2 C3 H3 126.1 . . ?
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 . . ?
C7 C8A H8AA 109.5 . . ?
C7 C8A H8AB 109.5 . . ?
H8AA C8A H8AB 109.5 . . ?
C7 C8A H8AC 109.5 . . ?
H8AA C8A H8AC 109.5 . . ?
H8AB C8A H8AC 109.5 . . ?
C63A N5A C59A 116.1(6) . . ?
C63A N5A U1 121.5(5) . . ?
C59A N5A U1 122.4(5) . . ?
N5A C63A C62A 124.4(6) . . ?
N5A C63A H63A 117.8 . . ?
C62A C63A H63A 117.8 . . ?
C61A C62A C63A 117.9(6) . . ?
C61A C62A H62A 121.1 . . ?
C63A C62A H62A 121.1 . . ?
C60A C61A C62A 119.3(7) . . ?
C60A C61A H61A 120.4 . . ?
C62A C61A H61A 120.4 . . ?
C61A C60A C59A 121.0(7) . . ?
C61A C60A H60A 119.5 . . ?
C59A C60A H60A 119.5 . . ?
C60A C59A N5A 121.3(7) . . ?
C60A C59A H59A 119.4 . . ?
N5A C59A H59A 119.4 . . ?

_refine_diff_density_max         1.658
_refine_diff_density_min         -0.925
_refine_diff_density_rms         0.114



# start Validation Reply Form
_vrf_PLAT910_compound6           
;
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 19.3, indicating that there are 
no issues with the data collected.
;
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Pyridine/hexanes'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_compound8
_database_code_depnum_ccdc_archive 'CCDC 1984907'
loop_
_audit_author_name
_audit_author_address
'Bradley E. Cowie'
;The University of Edinburgh
United Kingdom
;
_audit_update_record             
;
2020-02-18 deposited with the CCDC.	2020-06-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        '[{(py)ClUOUCl(py)}(LA)]'
_chemical_name_common            'Compound 8.solvent'
_chemical_melting_point          ?
_chemical_formula_moiety         'C68 H58 Cl2 N10 O U2, solvent'
_chemical_formula_sum            'C68 H58 Cl2 N10 O U2'
_chemical_formula_weight         1578.20

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'
Cl Cl 0.1484 0.1585 '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                   12.2163(5)
_cell_length_b                   13.1548(5)
_cell_length_c                   21.1659(10)
_cell_angle_alpha                77.753(4)
_cell_angle_beta                 76.263(4)
_cell_angle_gamma                72.589(4)
_cell_volume                     3116.0(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    10380
_cell_measurement_theta_min      3.2170
_cell_measurement_theta_max      25.1670

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.682
_exptl_crystal_F_000             1524
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.124
_exptl_crystal_size_mid          0.085
_exptl_crystal_size_min          0.037
_exptl_absorpt_coefficient_mu    5.327
_shelx_estimated_absorpt_T_min   0.833
_shelx_estimated_absorpt_T_max   0.941
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.833
_exptl_absorpt_correction_T_max  0.941
_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   ?
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Eos
_diffrn_detector_area_resol_mean 8.0521
_diffrn_reflns_number            60766
_diffrn_reflns_av_unetI/netI     0.0927
_diffrn_reflns_av_R_equivalents  0.1020
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.926
_diffrn_reflns_theta_max         25.349
_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             11386
_reflns_number_gt                8593
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .
_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   37.50    --  -22.87 -99.00-180.00   47
  2  ω    -55.00  51.00   1.00   37.50    --  -22.87  37.00 150.00  106
  3  ω   -105.00 -32.00   1.00   37.50    --  -22.87 179.00 -30.00   73
  4  ω    -25.00  22.00   1.00   37.50    --  -22.87 -99.00 -60.00   47
  5  ω     34.00 104.00   1.00   37.50    --   24.12 179.00-120.00   70
  6  ω    -46.00  48.00   1.00   37.50    --   24.12 -57.00-120.00   94
  7  ω    -46.00  48.00   1.00   37.50    --   24.12 -57.00-150.00   94
  8  ω      0.00  95.00   1.00   37.50    --   24.12  57.00   0.00   95
  9  ω    -25.00  22.00   1.00   37.50    --  -22.87 -99.00  30.00   47
 10  ω   -103.00 -34.00   1.00   37.50    --  -22.87-179.00-120.00   69
 11  ω    -93.00   1.00   1.00   37.50    --  -22.87 -57.00-150.00   94
 12  ω    -25.00  69.00   1.00   37.50    --   24.12 -99.00 -60.00   94
 13  ω      0.00  95.00   1.00   37.50    --   24.12  57.00  90.00   95
 14  ω     -8.00  98.00   1.00   37.50    --   24.12  37.00-150.00  106
 15  ω    -25.00  69.00   1.00   37.50    --   24.12 -99.00  60.00   94
;
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       '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 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_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.

Residual lattice electron density (presumably from highly disordered lattice 
solvent) was modelled using the solvent mask feature of Olex2 
(81.1 electrons/cell). In addition, the SIMU command was used on carbon atoms
C(31)-C(34) (a pyrrolic ring) because the thermal ellipsoid of C(31) was
non-positive definite, and the SIMU command was used on carbon atoms C(9) and 
C(10) due to a failed Hirshfield test.,Solvent Mask
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0386P)²+17.3410P] 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         11386
_refine_ls_number_parameters     752
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.0858
_refine_ls_R_factor_gt           0.0590
_refine_ls_wR_factor_ref         0.1241
_refine_ls_wR_factor_gt          0.1139
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_restrained_S_all      1.053
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U2 U 0.45728(3) 0.43842(3) 0.81421(2) 0.02239(11) Uani 1 1 d . . . . .
U1 U 0.73735(3) 0.57075(3) 0.70608(2) 0.02189(11) Uani 1 1 d . . . . .
Cl2 Cl 0.5665(2) 0.24317(19) 0.78225(13) 0.0292(6) Uani 1 1 d . . . . .
Cl1 Cl 0.9180(2) 0.6321(2) 0.63051(14) 0.0394(7) Uani 1 1 d . . . . .
O1 O 0.5930(5) 0.5089(4) 0.7630(3) 0.0154(13) Uani 1 1 d . . . . .
N1 N 0.6477(7) 0.6290(6) 0.6030(4) 0.0256(19) Uani 1 1 d . . . . .
N4 N 0.8787(6) 0.4332(6) 0.7726(4) 0.0212(18) Uani 1 1 d . . . . .
N9 N 0.8276(7) 0.4061(6) 0.6417(4) 0.0264(19) Uani 1 1 d . . . . .
N3 N 0.7747(7) 0.6504(6) 0.7899(4) 0.0258(19) Uani 1 1 d . . . . .
C44 C 0.2606(8) 0.4753(8) 0.7201(5) 0.026(2) Uani 1 1 d . . . . .
H44 H 0.215876 0.461562 0.694507 0.031 Uiso 1 1 calc R U . . .
N5 N 0.3667(6) 0.4188(6) 0.7187(4) 0.0217(18) Uani 1 1 d . . . . .
N7 N 0.3807(6) 0.5333(6) 0.9104(4) 0.0209(18) Uani 1 1 d . . . . .
C40 C 0.2080(9) 0.6631(8) 0.8267(5) 0.029(2) Uani 1 1 d . . . . .
N10 N 0.2873(7) 0.3444(7) 0.8777(4) 0.029(2) Uani 1 1 d . . . . .
N6 N 0.2772(6) 0.5779(6) 0.7972(4) 0.0221(18) Uani 1 1 d . . . . .
N8 N 0.5366(6) 0.3276(6) 0.9212(4) 0.0173(17) Uani 1 1 d . . . . .
C59 C 0.9113(8) 0.3990(8) 0.5872(5) 0.028(2) Uani 1 1 d . . . . .
H59 H 0.942420 0.457333 0.568477 0.033 Uiso 1 1 calc R U . . .
C14 C 0.8375(10) 0.5759(8) 0.8332(5) 0.034(3) Uani 1 1 d . . . . .
C57 C 0.5432(8) 0.4555(7) 0.6105(4) 0.020(2) Uani 1 1 d . . . . .
H57 H 0.515386 0.501013 0.642232 0.024 Uiso 1 1 calc R U . . .
C49 C 0.5412(8) 0.2983(7) 0.5691(5) 0.023(2) Uani 1 1 d . . . . .
C56 C 0.6282(8) 0.4790(8) 0.5562(5) 0.025(2) Uani 1 1 d . . . . .
C68 C 0.1946(9) 0.3920(9) 0.9201(5) 0.035(3) Uani 1 1 d . . . . .
H68 H 0.193664 0.457402 0.930676 0.042 Uiso 1 1 calc R U . . .
C55 C 0.6759(8) 0.5695(8) 0.5500(5) 0.029(2) Uani 1 1 d . . . . .
C63 C 0.7847(9) 0.3221(8) 0.6675(5) 0.030(2) Uani 1 1 d . . . . .
H63 H 0.727363 0.326494 0.705392 0.036 Uiso 1 1 calc R U . . .
C31 C 0.3975(8) 0.4704(8) 0.9710(5) 0.0282(13) Uani 1 1 d . U . . .
C43 C 0.2112(8) 0.5562(8) 0.7587(5) 0.026(2) Uani 1 1 d . . . . .
N2 N 0.6402(7) 0.7626(7) 0.6944(5) 0.038(2) Uani 1 1 d . . . . .
C45 C 0.4114(8) 0.3447(8) 0.6720(5) 0.023(2) Uani 1 1 d . . . . .
C42 C 0.1011(9) 0.6276(9) 0.7664(6) 0.042(3) Uani 1 1 d . . . . .
H42 H 0.039931 0.629831 0.746542 0.050 Uiso 1 1 calc R U . . .
C46 C 0.3678(8) 0.2602(8) 0.6767(5) 0.025(2) Uani 1 1 d . . . . .
H46 H 0.308980 0.247635 0.712016 0.030 Uiso 1 1 calc R U . . .
C50 C 0.6252(9) 0.3229(8) 0.5138(5) 0.031(3) Uani 1 1 d . . . . .
H50 H 0.652118 0.278517 0.481426 0.038 Uiso 1 1 calc R U . . .
C28 C 0.7738(8) 0.2705(7) 0.8538(4) 0.017(2) Uani 1 1 d . . . . .
H28 H 0.733139 0.342764 0.852770 0.020 Uiso 1 1 calc R U . . .
C1 C 0.6045(8) 0.7329(8) 0.5918(5) 0.032(3) Uani 1 1 d . . . . .
H1 H 0.576751 0.762973 0.552828 0.039 Uiso 1 1 calc R U . . .
C2 C 0.5978(9) 0.8020(8) 0.6359(5) 0.033(3) Uani 1 1 d . . . . .
C32 C 0.3246(8) 0.5229(8) 1.0212(5) 0.0288(13) Uani 1 1 d . U . . .
H32 H 0.319195 0.497859 1.066028 0.035 Uiso 1 1 calc R U . . .
C41 C 0.0990(9) 0.6948(9) 0.8088(6) 0.042(3) Uani 1 1 d . . . . .
H41 H 0.036347 0.750871 0.822858 0.050 Uiso 1 1 calc R U . . .
C24 C 0.6341(10) 0.0333(8) 0.9843(5) 0.034(3) Uani 1 1 d . . . . .
H24 H 0.605018 -0.017523 1.016102 0.040 Uiso 1 1 calc R U . . .
C30 C 0.4770(8) 0.3684(7) 0.9743(5) 0.022(2) Uani 1 1 d . . . . .
H30 H 0.487722 0.328588 1.015289 0.027 Uiso 1 1 calc R U . . .
C5 C 0.6366(9) 0.8530(8) 0.7186(6) 0.039(3) Uani 1 1 d . . . . .
C54 C 0.7522(9) 0.5915(9) 0.4942(5) 0.035(3) Uani 1 1 d . . . . .
H54 H 0.780163 0.651917 0.488460 0.042 Uiso 1 1 calc R U . . .
C16 C 0.9356(8) 0.3210(8) 0.7688(5) 0.025(2) Uani 1 1 d . . . . .
C11 C 0.7457(8) 0.7447(8) 0.8124(6) 0.033(3) Uani 1 1 d . . . . .
C48 C 0.4953(9) 0.2084(7) 0.5763(5) 0.027(2) Uani 1 1 d . . . . .
H48 H 0.523414 0.161782 0.545173 0.032 Uiso 1 1 calc R U . . .
C58 C 0.4996(8) 0.3675(7) 0.6185(5) 0.018(2) Uani 1 1 d . . . . .
C3 C 0.5639(10) 0.9145(8) 0.6274(6) 0.041(3) Uani 1 1 d . . . . .
H3 H 0.531317 0.960172 0.592761 0.049 Uiso 1 1 calc R U . . .
C15 C 0.8866(10) 0.4711(8) 0.8228(6) 0.038(3) Uani 1 1 d . . . . .
H15 H 0.928241 0.424088 0.853609 0.046 Uiso 1 1 calc R U . . .
C23 C 0.7413(10) 0.0039(8) 0.9477(6) 0.034(3) Uani 1 1 d . . . . .
H23 H 0.784440 -0.067812 0.952925 0.041 Uiso 1 1 calc R U . . .
C36 C 0.3589(9) 0.7543(8) 0.8264(5) 0.035(3) Uani 1 1 d . . . . .
H36A H 0.386062 0.789014 0.853498 0.042 Uiso 1 1 calc R U . . .
H36B H 0.422481 0.693759 0.812834 0.042 Uiso 1 1 calc R U . . .
C17 C 1.0370(9) 0.2910(9) 0.7258(5) 0.035(3) Uani 1 1 d . . . . .
H17 H 1.070221 0.342921 0.697658 0.042 Uiso 1 1 calc R U . . .
C37 C 0.3302(11) 0.8326(9) 0.7664(6) 0.053(3) Uani 1 1 d . . . . .
H37A H 0.304732 0.798665 0.738716 0.080 Uiso 1 1 calc R U . . .
H37B H 0.398339 0.855423 0.742786 0.080 Uiso 1 1 calc R U . . .
H37C H 0.269046 0.894116 0.779321 0.080 Uiso 1 1 calc R U . . .
C62 C 0.8224(10) 0.2269(9) 0.6400(6) 0.043(3) Uani 1 1 d . . . . .
H62 H 0.789814 0.169433 0.658557 0.052 Uiso 1 1 calc R U . . .
C27 C 0.7239(8) 0.1924(7) 0.8949(4) 0.019(2) Uani 1 1 d . . . . .
C35 C 0.2548(8) 0.7106(8) 0.8689(5) 0.029(2) Uani 1 1 d . . . . .
C26 C 0.6074(8) 0.2199(7) 0.9316(5) 0.024(2) Uani 1 1 d . . . . .
C34 C 0.2970(8) 0.6246(8) 0.9244(5) 0.0288(13) Uani 1 1 d . U . . .
C39 C 0.1939(11) 0.8794(9) 0.9315(7) 0.055(4) Uani 1 1 d . . . . .
H39A H 0.235910 0.835590 0.965028 0.082 Uiso 1 1 calc R U . . .
H39B H 0.125902 0.929456 0.951146 0.082 Uiso 1 1 calc R U . . .
H39C H 0.243234 0.918281 0.899845 0.082 Uiso 1 1 calc R U . . .
C21 C 0.8969(9) 0.0542(8) 0.8592(5) 0.032(3) Uani 1 1 d . . . . .
H21 H 0.938943 -0.017834 0.862058 0.038 Uiso 1 1 calc R U . . .
C13 C 0.8472(14) 0.6270(10) 0.8827(6) 0.068(5) Uani 1 1 d . . . . .
H13 H 0.886202 0.595251 0.917596 0.082 Uiso 1 1 calc R U . . .
C33 C 0.2609(8) 0.6196(8) 0.9923(5) 0.0290(13) Uani 1 1 d . U . . .
H33 H 0.204243 0.671863 1.014185 0.035 Uiso 1 1 calc R U . . .
C52 C 0.7526(9) 0.4382(10) 0.4503(5) 0.038(3) Uani 1 1 d . . . . .
H52 H 0.780813 0.394518 0.417622 0.045 Uiso 1 1 calc R U . . .
C64 C 0.2849(10) 0.2520(9) 0.8634(6) 0.042(3) Uani 1 1 d . . . . .
H64 H 0.348001 0.217009 0.834441 0.050 Uiso 1 1 calc R U . . .
C47 C 0.4096(9) 0.1901(8) 0.6290(5) 0.029(2) Uani 1 1 d . . . . .
H47 H 0.378955 0.131639 0.633323 0.034 Uiso 1 1 calc R U . . .
C65 C 0.1945(11) 0.2054(9) 0.8889(6) 0.046(3) Uani 1 1 d . . . . .
H65 H 0.196480 0.140990 0.876562 0.055 Uiso 1 1 calc R U . . .
C4 C 0.5871(10) 0.9441(9) 0.6783(6) 0.044(3) Uani 1 1 d . . . . .
H4 H 0.572365 1.014702 0.685515 0.053 Uiso 1 1 calc R U . . .
C60 C 0.9514(10) 0.3067(10) 0.5591(5) 0.041(3) Uani 1 1 d . . . . .
H60 H 1.009214 0.303194 0.521480 0.049 Uiso 1 1 calc R U . . .
C22 C 0.7896(8) 0.0826(7) 0.9006(5) 0.024(2) Uani 1 1 d . . . . .
C12 C 0.7873(13) 0.7342(11) 0.8690(6) 0.059(4) Uani 1 1 d . . . . .
H12 H 0.777158 0.788435 0.893436 0.071 Uiso 1 1 calc R U . . .
C20 C 0.9437(8) 0.1314(8) 0.8133(5) 0.027(2) Uani 1 1 d . . . . .
C51 C 0.6685(8) 0.4121(8) 0.5066(5) 0.026(2) Uani 1 1 d . . . . .
C25 C 0.5654(9) 0.1407(8) 0.9748(5) 0.028(2) Uani 1 1 d . . . . .
H25 H 0.489456 0.158160 0.998520 0.034 Uiso 1 1 calc R U . . .
C19 C 1.0488(9) 0.1046(10) 0.7661(6) 0.041(3) Uani 1 1 d . . . . .
H19 H 1.088389 0.032517 0.764546 0.049 Uiso 1 1 calc R U . . .
C29 C 0.8835(8) 0.2428(8) 0.8141(5) 0.026(2) Uani 1 1 d . . . . .
C61 C 0.9076(11) 0.2207(10) 0.5855(7) 0.055(4) Uani 1 1 d . . . . .
H61 H 0.935671 0.157981 0.566529 0.066 Uiso 1 1 calc R U . . .
C38 C 0.1560(9) 0.8062(8) 0.8967(5) 0.035(3) Uani 1 1 d . . . . .
H38A H 0.119900 0.851066 0.860535 0.042 Uiso 1 1 calc R U . . .
H38B H 0.096813 0.776550 0.927649 0.042 Uiso 1 1 calc R U . . .
C6 C 0.6804(11) 0.8504(10) 0.7815(7) 0.058(4) Uani 1 1 d . . . . .
C66 C 0.1018(10) 0.2531(10) 0.9323(6) 0.043(3) Uani 1 1 d . . . . .
H66 H 0.040167 0.221856 0.950523 0.052 Uiso 1 1 calc R U . . .
C67 C 0.1018(10) 0.3497(10) 0.9485(6) 0.043(3) Uani 1 1 d . . . . .
H67 H 0.040079 0.385036 0.977990 0.052 Uiso 1 1 calc R U . . .
C10 C 0.8548(11) 0.9039(11) 0.7159(7) 0.065(4) Uani 1 1 d . U . . .
H10A H 0.880023 0.827406 0.716142 0.098 Uiso 1 1 calc R U . . .
H10B H 0.916522 0.928118 0.723729 0.098 Uiso 1 1 calc R U . . .
H10C H 0.835458 0.939358 0.673892 0.098 Uiso 1 1 calc R U . . .
C18 C 1.0913(9) 0.1812(9) 0.7241(6) 0.039(3) Uani 1 1 d . . . . .
H18 H 1.158502 0.161072 0.693030 0.047 Uiso 1 1 calc R U . . .
C8 C 0.4827(13) 0.9822(11) 0.8283(8) 0.076(5) Uani 1 1 d . . . . .
H8A H 0.516407 1.042272 0.812970 0.114 Uiso 1 1 calc R U . . .
H8B H 0.426407 0.994461 0.868052 0.114 Uiso 1 1 calc R U . . .
H8C H 0.444859 0.974571 0.795356 0.114 Uiso 1 1 calc R U . . .
C9 C 0.7451(13) 0.9315(11) 0.7710(7) 0.069(4) Uani 1 1 d . U . . .
H9A H 0.768962 0.932074 0.811498 0.082 Uiso 1 1 calc R U . . .
H9B H 0.695836 1.002408 0.758089 0.082 Uiso 1 1 calc R U . . .
C7 C 0.5695(12) 0.8893(13) 0.8408(7) 0.074(5) Uani 1 1 d . . . . .
H7A H 0.532377 0.830613 0.856785 0.089 Uiso 1 1 calc R U . . .
H7B H 0.601479 0.897372 0.876634 0.089 Uiso 1 1 calc R U . . .
C53 C 0.7902(10) 0.5255(10) 0.4450(5) 0.039(3) Uani 1 1 d . . . . .
H53 H 0.843055 0.543071 0.407612 0.047 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U2 O1 2.103(6) . ?
U2 N6 2.453(7) . ?
U2 N7 2.461(7) . ?
U2 N5 2.613(7) . ?
U2 N8 2.643(7) . ?
U2 Cl2 2.663(2) . ?
U2 N10 2.675(8) . ?
U1 O1 2.158(6) . ?
U1 N3 2.432(8) . ?
U1 N2 2.433(8) . ?
U1 N4 2.539(7) . ?
U1 N1 2.544(8) . ?
U1 N9 2.622(7) . ?
U1 Cl1 2.630(3) . ?
N1 C1 1.301(12) . ?
N1 C55 1.421(13) . ?
N4 C15 1.298(12) . ?
N4 C16 1.442(12) . ?
N9 C63 1.322(13) . ?
N9 C59 1.346(12) . ?
N3 C11 1.341(11) . ?
N3 C14 1.375(13) . ?
C44 N5 1.284(11) . ?
C44 C43 1.384(13) . ?
N5 C45 1.435(11) . ?
N7 C34 1.359(11) . ?
N7 C31 1.394(13) . ?
C40 N6 1.357(11) . ?
C40 C41 1.389(13) . ?
C40 C35 1.487(13) . ?
N10 C64 1.324(13) . ?
N10 C68 1.345(12) . ?
N6 C43 1.394(12) . ?
N8 C30 1.310(11) . ?
N8 C26 1.424(11) . ?
C59 C60 1.371(14) . ?
C14 C15 1.372(14) . ?
C14 C13 1.403(15) . ?
C57 C58 1.377(12) . ?
C57 C56 1.404(13) . ?
C49 C50 1.413(14) . ?
C49 C48 1.420(13) . ?
C49 C58 1.434(12) . ?
C56 C51 1.416(13) . ?
C56 C55 1.444(14) . ?
C68 C67 1.367(15) . ?
C55 C54 1.357(14) . ?
C63 C62 1.399(13) . ?
C31 C32 1.376(13) . ?
C31 C30 1.400(13) . ?
C43 C42 1.387(13) . ?
N2 C5 1.377(12) . ?
N2 C2 1.392(13) . ?
C45 C46 1.346(13) . ?
C45 C58 1.417(13) . ?
C42 C41 1.379(14) . ?
C46 C47 1.414(13) . ?
C50 C51 1.392(14) . ?
C28 C27 1.388(13) . ?
C28 C29 1.392(13) . ?
C1 C2 1.410(14) . ?
C2 C3 1.396(14) . ?
C32 C33 1.378(14) . ?
C24 C23 1.344(14) . ?
C24 C25 1.411(13) . ?
C5 C4 1.380(15) . ?
C5 C6 1.539(16) . ?
C54 C53 1.403(14) . ?
C16 C17 1.357(13) . ?
C16 C29 1.438(14) . ?
C11 C12 1.375(16) . ?
C11 C6 1.482(16) . ?
C48 C47 1.372(14) . ?
C3 C4 1.336(15) . ?
C23 C22 1.436(15) . ?
C36 C37 1.495(15) . ?
C36 C35 1.559(15) . ?
C17 C18 1.402(14) . ?
C62 C61 1.356(17) . ?
C27 C22 1.423(12) . ?
C27 C26 1.429(13) . ?
C35 C34 1.516(14) . ?
C35 C38 1.565(12) . ?
C26 C25 1.372(14) . ?
C34 C33 1.394(14) . ?
C39 C38 1.554(14) . ?
C21 C22 1.388(14) . ?
C21 C20 1.403(15) . ?
C13 C12 1.384(17) . ?
C52 C53 1.334(15) . ?
C52 C51 1.431(14) . ?
C64 C65 1.367(16) . ?
C65 C66 1.358(15) . ?
C60 C61 1.353(17) . ?
C20 C19 1.428(14) . ?
C20 C29 1.431(13) . ?
C19 C18 1.337(16) . ?
C6 C9 1.460(18) . ?
C6 C7 1.650(19) . ?
C66 C67 1.385(16) . ?
C10 C9 1.561(18) . ?
C8 C7 1.382(18) . ?

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 U2 N6 104.9(2) . . ?
O1 U2 N7 102.1(2) . . ?
N6 U2 N7 70.7(2) . . ?
O1 U2 N5 102.3(2) . . ?
N6 U2 N5 65.7(2) . . ?
N7 U2 N5 134.1(2) . . ?
O1 U2 N8 102.8(2) . . ?
N6 U2 N8 132.8(2) . . ?
N7 U2 N8 66.5(2) . . ?
N5 U2 N8 141.7(2) . . ?
O1 U2 Cl2 95.07(15) . . ?
N6 U2 Cl2 137.38(18) . . ?
N7 U2 Cl2 141.20(19) . . ?
N5 U2 Cl2 73.50(17) . . ?
N8 U2 Cl2 75.88(16) . . ?
O1 U2 N10 178.6(2) . . ?
N6 U2 N10 76.0(3) . . ?
N7 U2 N10 79.2(2) . . ?
N5 U2 N10 77.0(2) . . ?
N8 U2 N10 77.2(2) . . ?
Cl2 U2 N10 83.53(18) . . ?
O1 U1 N3 99.1(2) . . ?
O1 U1 N2 99.3(3) . . ?
N3 U1 N2 70.2(3) . . ?
O1 U1 N4 91.5(2) . . ?
N3 U1 N4 69.1(3) . . ?
N2 U1 N4 139.1(3) . . ?
O1 U1 N1 93.0(2) . . ?
N3 U1 N1 139.5(3) . . ?
N2 U1 N1 69.7(3) . . ?
N4 U1 N1 149.4(2) . . ?
O1 U1 N9 93.9(2) . . ?
N3 U1 N9 140.7(2) . . ?
N2 U1 N9 143.5(3) . . ?
N4 U1 N9 73.7(2) . . ?
N1 U1 N9 75.8(2) . . ?
O1 U1 Cl1 174.90(16) . . ?
N3 U1 Cl1 85.4(2) . . ?
N2 U1 Cl1 84.5(2) . . ?
N4 U1 Cl1 87.80(19) . . ?
N1 U1 Cl1 85.07(19) . . ?
N9 U1 Cl1 81.1(2) . . ?
U2 O1 U1 175.4(3) . . ?
C1 N1 C55 118.7(9) . . ?
C1 N1 U1 111.9(7) . . ?
C55 N1 U1 125.5(6) . . ?
C15 N4 C16 117.4(8) . . ?
C15 N4 U1 110.9(6) . . ?
C16 N4 U1 131.1(6) . . ?
C63 N9 C59 118.5(9) . . ?
C63 N9 U1 114.3(7) . . ?
C59 N9 U1 127.2(7) . . ?
C11 N3 C14 106.1(8) . . ?
C11 N3 U1 140.5(7) . . ?
C14 N3 U1 113.1(6) . . ?
N5 C44 C43 121.5(9) . . ?
C44 N5 C45 116.2(8) . . ?
C44 N5 U2 113.4(6) . . ?
C45 N5 U2 129.7(6) . . ?
C34 N7 C31 106.0(8) . . ?
C34 N7 U2 135.2(6) . . ?
C31 N7 U2 115.8(6) . . ?
N6 C40 C41 110.1(9) . . ?
N6 C40 C35 120.1(8) . . ?
C41 C40 C35 129.8(9) . . ?
C64 N10 C68 116.3(10) . . ?
C64 N10 U2 120.5(7) . . ?
C68 N10 U2 122.9(7) . . ?
C40 N6 C43 106.4(8) . . ?
C40 N6 U2 136.0(6) . . ?
C43 N6 U2 115.8(6) . . ?
C30 N8 C26 115.9(8) . . ?
C30 N8 U2 112.2(6) . . ?
C26 N8 U2 129.2(5) . . ?
N9 C59 C60 120.8(10) . . ?
C15 C14 N3 121.5(9) . . ?
C15 C14 C13 129.0(11) . . ?
N3 C14 C13 109.4(10) . . ?
C58 C57 C56 122.3(9) . . ?
C50 C49 C48 121.8(9) . . ?
C50 C49 C58 118.9(8) . . ?
C48 C49 C58 119.3(9) . . ?
C57 C56 C51 119.2(9) . . ?
C57 C56 C55 121.4(9) . . ?
C51 C56 C55 119.4(10) . . ?
N10 C68 C67 123.7(10) . . ?
C54 C55 N1 121.7(9) . . ?
C54 C55 C56 118.2(10) . . ?
N1 C55 C56 120.0(9) . . ?
N9 C63 C62 122.4(10) . . ?
C32 C31 N7 109.9(9) . . ?
C32 C31 C30 129.3(10) . . ?
N7 C31 C30 120.8(8) . . ?
C44 C43 C42 131.1(9) . . ?
C44 C43 N6 119.9(8) . . ?
C42 C43 N6 109.0(9) . . ?
C5 N2 C2 104.9(9) . . ?
C5 N2 U1 139.3(7) . . ?
C2 N2 U1 113.4(6) . . ?
C46 C45 C58 121.1(9) . . ?
C46 C45 N5 121.9(9) . . ?
C58 C45 N5 116.9(8) . . ?
C41 C42 C43 107.3(9) . . ?
C45 C46 C47 121.3(9) . . ?
C51 C50 C49 121.5(9) . . ?
C27 C28 C29 121.3(8) . . ?
N1 C1 C2 123.0(10) . . ?
N2 C2 C3 109.5(10) . . ?
N2 C2 C1 121.4(9) . . ?
C3 C2 C1 128.7(11) . . ?
C31 C32 C33 107.0(10) . . ?
C42 C41 C40 107.2(9) . . ?
C23 C24 C25 120.6(10) . . ?
N8 C30 C31 121.8(9) . . ?
N2 C5 C4 109.5(10) . . ?
N2 C5 C6 124.3(10) . . ?
C4 C5 C6 126.2(10) . . ?
C55 C54 C53 121.8(10) . . ?
C17 C16 C29 121.6(9) . . ?
C17 C16 N4 120.9(9) . . ?
C29 C16 N4 117.4(8) . . ?
N3 C11 C12 111.6(10) . . ?
N3 C11 C6 126.6(10) . . ?
C12 C11 C6 121.7(10) . . ?
C47 C48 C49 120.2(9) . . ?
C57 C58 C45 122.9(9) . . ?
C57 C58 C49 118.9(9) . . ?
C45 C58 C49 118.2(8) . . ?
C4 C3 C2 107.0(10) . . ?
N4 C15 C14 124.2(10) . . ?
C24 C23 C22 120.3(9) . . ?
C37 C36 C35 114.3(9) . . ?
C16 C17 C18 119.5(11) . . ?
C61 C62 C63 118.3(11) . . ?
C28 C27 C22 119.5(9) . . ?
C28 C27 C26 121.4(8) . . ?
C22 C27 C26 119.1(9) . . ?
C40 C35 C34 109.4(8) . . ?
C40 C35 C36 109.0(8) . . ?
C34 C35 C36 109.5(8) . . ?
C40 C35 C38 108.8(8) . . ?
C34 C35 C38 110.9(8) . . ?
C36 C35 C38 109.2(9) . . ?
C25 C26 N8 121.4(9) . . ?
C25 C26 C27 118.9(9) . . ?
N8 C26 C27 119.7(8) . . ?
N7 C34 C33 109.7(9) . . ?
N7 C34 C35 120.0(8) . . ?
C33 C34 C35 130.3(9) . . ?
C22 C21 C20 121.7(9) . . ?
C12 C13 C14 106.2(12) . . ?
C32 C33 C34 107.5(9) . . ?
C53 C52 C51 119.7(10) . . ?
N10 C64 C65 123.4(11) . . ?
C48 C47 C46 119.9(9) . . ?
C66 C65 C64 120.0(11) . . ?
C3 C4 C5 109.0(10) . . ?
C61 C60 C59 120.7(10) . . ?
C21 C22 C27 119.1(10) . . ?
C21 C22 C23 121.9(9) . . ?
C27 C22 C23 119.0(9) . . ?
C11 C12 C13 106.6(10) . . ?
C21 C20 C19 123.4(9) . . ?
C21 C20 C29 118.2(9) . . ?
C19 C20 C29 118.4(10) . . ?
C50 C51 C56 119.2(9) . . ?
C50 C51 C52 121.8(9) . . ?
C56 C51 C52 119.0(9) . . ?
C26 C25 C24 121.8(9) . . ?
C18 C19 C20 121.2(10) . . ?
C28 C29 C20 119.4(9) . . ?
C28 C29 C16 122.8(8) . . ?
C20 C29 C16 117.5(9) . . ?
C60 C61 C62 119.2(11) . . ?
C39 C38 C35 116.4(9) . . ?
C9 C6 C11 111.1(10) . . ?
C9 C6 C5 110.3(12) . . ?
C11 C6 C5 117.5(9) . . ?
C9 C6 C7 103.2(11) . . ?
C11 C6 C7 103.1(12) . . ?
C5 C6 C7 110.5(10) . . ?
C65 C66 C67 118.0(11) . . ?
C68 C67 C66 118.5(10) . . ?
C19 C18 C17 121.7(10) . . ?
C6 C9 C10 108.8(12) . . ?
C8 C7 C6 120.0(14) . . ?
C52 C53 C54 121.8(11) . . ?

_refine_diff_density_max         4.186
_refine_diff_density_min         -2.058
_refine_diff_density_rms         0.181



# start Validation Reply Form
_vrf_PLAT910_compound8           
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         18 Note  
RESPONSE: This has been noted, but is not serious. The independent 
reflections/parameters ratio is equal to 15, indicating that there are 
no issues with the data collected.
;
# end Validation Reply Form



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

data_compound5A
_database_code_depnum_ccdc_archive 'CCDC 1984905'
loop_
_audit_author_name
_audit_author_address
'Bradley E. Cowie'
;The University of Edinburgh
United Kingdom
;
_audit_update_record             
;
2020-02-18 deposited with the CCDC.	2020-06-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        '[{(py)U(u-F)(u-OBcat)U(u-O2C6H4)(py)}(LA)]'
_chemical_name_common            'Compound 5A.3dme'
_chemical_melting_point          ?
_chemical_formula_moiety         'C80 H66 B F N10 O5 U2, 3(C4 H10 O2)'
_chemical_formula_sum            'C92 H96 B F N10 O11 U2'
_chemical_formula_weight         2023.65

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'
F F 0.0171 0.0103 '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                   14.6146(3)
_cell_length_b                   16.3896(4)
_cell_length_c                   18.1536(4)
_cell_angle_alpha                77.518(2)
_cell_angle_beta                 78.699(2)
_cell_angle_gamma                82.007(2)
_cell_volume                     4141.91(17)
_cell_formula_units_Z            2
_cell_measurement_temperature    120.01(10)
_cell_measurement_reflns_used    33672
_cell_measurement_theta_min      3.4990
_cell_measurement_theta_max      32.3000

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.623
_exptl_crystal_F_000             2008
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.612
_exptl_crystal_size_mid          0.154
_exptl_crystal_size_min          0.066
_exptl_absorpt_coefficient_mu    3.975
_shelx_estimated_absorpt_T_min   0.201
_shelx_estimated_absorpt_T_max   1.000
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_correction_T_min  0.201
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      120.01(10)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Atlas
_diffrn_detector_area_resol_mean 5.1574
_diffrn_reflns_number            105405
_diffrn_reflns_av_unetI/netI     0.0582
_diffrn_reflns_av_R_equivalents  0.0478
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         2.802
_diffrn_reflns_theta_max         32.951
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.926
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.926
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.926
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             28789
_reflns_number_gt                21060
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -78.00 -29.00   1.00   10.00    --  -17.68 133.00 -61.61   49
  2  ω    -92.00  14.00   1.00   10.00    --  -17.68 -77.00-150.00  106
  3  ω    -54.00  42.00   1.00   10.00    --   19.09 -38.00-120.00   96
  4  ω      3.00  75.00   1.00   10.00    --   19.09-127.00 116.48   72
  5  ω    -18.00  98.00   1.00   10.00    --   19.09  19.00  60.00  116
  6  ω    -12.00  93.00   1.00   10.00    --   19.09  77.00-180.00  105
  7  ω     -3.00  92.00   1.00   10.00    --   19.09  38.00 120.00   95
  8  ω    -55.00  50.00   1.00   10.00    --   19.09 -77.00   0.00  105
  9  ω    -76.00 -27.00   1.00   10.00    --  -17.68 130.00 124.61   49
;

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

_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_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.

All three molecules of lattice 1,2-dme were positionally disordered over 
two positions. The molecule of 1,2-dme with carbons C(100)-C(103) and 
oxygens O(10) and O(11) was split into two parts and refined with an occupancy
ratio of 0.8:0.2. The thermal parameters of the part with the highest occupancy
were refined anisotropically, whereas the thermal parameters of the lower
occpancy part were refined using ISOR due to the presence of non-positive 
definite thermal ellipsoids when refined anisotropically. Furthermore, 
the thermal ellipsoids of the carbon atoms were refined to be similar to one
another using the SIMU command. The molecule of 1,2-dme with carbons C(200)-C(203) 
and oxygens O(20) and O(21) was split into two parts and refined with an 
occupancy ratio of 0.62:0.38. The thermal parameters of atoms O(20) and O(20A), 
O(21) and O(21A), and C(200) and C(1F) were restrained to be similar to one 
another through the use of the SIMU command. The molecule of 1,2-dme with carbons 
C(300)-C(303) and oxygens O(30) and O(31) were split into two parts and 
refined in a 0.75:0.25 ratio. In addition, the thermal parameters of the carbons 
C(300), C(301), C(302), C(1B), C(1K) and C(1L), and oxygens O(30), O(30A), O(31) 
and O(31A) were restrained to be similar to one another using the SIMU
command. The C(1B)-O(31A), C(1A)-O(31A), C(1L)-O(30A) and C(1K)-O(30A) bond 
lengths of one of the disordered molecules of 1,2-dme were restrained to be 
similar to one another using the SADI command. The C(202)-C(201), C(1E)-C(1C), 
C(201)-O(20), C(1E)-O(20A), O(20)-C(200), O(20A)-C(1F), C(301)-O(30), C(102)-O(11), 
O(10)-C(101), C(101)-C(102), C(1A)-O(31A), O(31A)-C(1B), C(1B)-C(1K), C(1K)-O(30A), 
O(30A)-C(1L), C(1I)-C(1H), C(1J)-O(10A), O(10A)-C(1H), C(1H)-C(1I), C(1I)-O(11A) 
and O(11A)-C(1G) bond lengths of the disordered molecules of 1,2-dme were
restrained to ~1.4 Angstroms using the DANG command. Finally, the thermal 
parameters of C(1A) and C(303), and O(10) and O(11) were contrained to be equal
to each other, respectively, using the EADP command due to unstable refinement
without it.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0269P)²+6.2134P] 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         28789
_refine_ls_number_parameters     1194
_refine_ls_number_restraints     174
_refine_ls_R_factor_all          0.0701
_refine_ls_R_factor_gt           0.0407
_refine_ls_wR_factor_ref         0.0838
_refine_ls_wR_factor_gt          0.0746
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_restrained_S_all      1.046
_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 0.26867(2) 0.66954(2) 0.83198(2) 0.01878(3) Uani 1 1 d . . . . .
U2 U 0.26004(2) 0.84360(2) 0.65248(2) 0.01791(3) Uani 1 1 d . . . . .
F1 F 0.31546(13) 0.79897(12) 0.77071(11) 0.0218(4) Uani 1 1 d . . . . .
O1 O 0.34976(16) 0.61592(15) 0.74165(14) 0.0236(5) Uani 1 1 d . . . . .
O2 O 0.34418(16) 0.73938(14) 0.61659(14) 0.0226(5) Uani 1 1 d . . . . .
O3 O 0.16429(16) 0.75791(14) 0.75154(13) 0.0207(5) Uani 1 1 d . . . . .
O4 O 0.0091(2) 0.7224(2) 0.7347(2) 0.0550(9) Uani 1 1 d . . . . .
O5 O 0.0055(3) 0.8117(2) 0.8142(2) 0.0627(10) Uani 1 1 d . . . . .
N1 N 0.4427(2) 0.65095(18) 0.86131(17) 0.0239(6) Uani 1 1 d . . . . .
N2 N 0.2815(2) 0.70827(18) 0.95464(17) 0.0237(6) Uani 1 1 d . . . . .
N3 N 0.1166(2) 0.66870(17) 0.91896(16) 0.0225(6) Uani 1 1 d . . . . .
N4 N 0.1607(2) 0.56525(18) 0.80924(18) 0.0242(6) Uani 1 1 d . . . . .
N5 N 0.1597(2) 0.78861(19) 0.57314(16) 0.0236(6) Uani 1 1 d . . . . .
N6 N 0.10969(19) 0.93138(18) 0.64393(16) 0.0225(6) Uani 1 1 d . . . . .
N7 N 0.2641(2) 0.98179(17) 0.68382(16) 0.0220(6) Uani 1 1 d . . . . .
N8 N 0.42814(19) 0.88580(17) 0.63027(16) 0.0208(6) Uani 1 1 d . . . . .
N9 N 0.2945(2) 0.52418(18) 0.92196(18) 0.0276(7) Uani 1 1 d . . . . .
N10 N 0.2887(2) 0.92999(19) 0.51235(17) 0.0263(6) Uani 1 1 d . . . . .
C1 C 0.4458(3) 0.6554(2) 0.9313(2) 0.0297(8) Uani 1 1 d . . . . .
H1 H 0.501992 0.639057 0.949650 0.036 Uiso 1 1 calc R U . . .
C2 C 0.3662(3) 0.6842(2) 0.9804(2) 0.0291(8) Uani 1 1 d . . . . .
C3 C 0.3565(3) 0.6923(3) 1.0566(2) 0.0398(10) Uani 1 1 d . . . . .
H3 H 0.402989 0.679604 1.086915 0.048 Uiso 1 1 calc R U . . .
C4 C 0.2635(3) 0.7230(3) 1.0784(2) 0.0408(10) Uani 1 1 d . . . . .
H4 H 0.235798 0.734944 1.126117 0.049 Uiso 1 1 calc R U . . .
C5 C 0.2198(3) 0.7326(2) 1.0145(2) 0.0283(8) Uani 1 1 d . . . . .
C6 C 0.1223(3) 0.7701(2) 1.0027(2) 0.0289(8) Uani 1 1 d . . . . .
C7 C 0.1333(3) 0.8482(2) 0.9367(2) 0.0307(8) Uani 1 1 d . . . . .
H7A H 0.165990 0.829954 0.890275 0.037 Uiso 1 1 calc R U . . .
H7B H 0.071423 0.873687 0.927744 0.037 Uiso 1 1 calc R U . . .
C8 C 0.1867(3) 0.9148(3) 0.9528(3) 0.0452(11) Uani 1 1 d . . . . .
H8A H 0.149353 0.940589 0.992998 0.068 Uiso 1 1 calc R U . . .
H8B H 0.199519 0.956750 0.907284 0.068 Uiso 1 1 calc R U . . .
H8C H 0.244710 0.888646 0.968336 0.068 Uiso 1 1 calc R U . . .
C9 C 0.0641(3) 0.7963(3) 1.0759(2) 0.0414(10) Uani 1 1 d . . . . .
H9A H 0.050071 0.746049 1.113780 0.050 Uiso 1 1 calc R U . . .
H9B H 0.101781 0.827355 1.096372 0.050 Uiso 1 1 calc R U . . .
C10 C -0.0285(3) 0.8505(3) 1.0638(3) 0.0491(12) Uani 1 1 d . . . . .
H10A H -0.016041 0.907557 1.042438 0.074 Uiso 1 1 calc R U . . .
H10B H -0.069997 0.848250 1.112122 0.074 Uiso 1 1 calc R U . . .
H10C H -0.057239 0.829457 1.029425 0.074 Uiso 1 1 calc R U . . .
C11 C 0.0752(3) 0.7051(2) 0.9797(2) 0.0272(8) Uani 1 1 d . . . . .
C12 C -0.0086(3) 0.6704(3) 1.0142(2) 0.0376(10) Uani 1 1 d . . . . .
H12 H -0.049554 0.684407 1.056807 0.045 Uiso 1 1 calc R U . . .
C13 C -0.0192(3) 0.6112(3) 0.9732(3) 0.0395(10) Uani 1 1 d . . . . .
H13 H -0.068614 0.578042 0.982835 0.047 Uiso 1 1 calc R U . . .
C14 C 0.0581(2) 0.6108(2) 0.9147(2) 0.0264(8) Uani 1 1 d . . . . .
C15 C 0.0837(3) 0.5591(2) 0.8599(2) 0.0285(8) Uani 1 1 d . . . . .
H15 H 0.044466 0.519152 0.859753 0.034 Uiso 1 1 calc R U . . .
C16 C 0.1839(3) 0.5034(2) 0.7622(2) 0.0274(8) Uani 1 1 d . . . . .
C17 C 0.1908(3) 0.4198(2) 0.7944(3) 0.0352(9) Uani 1 1 d . . . . .
H17 H 0.178996 0.403016 0.847367 0.042 Uiso 1 1 calc R U . . .
C18 C 0.2156(3) 0.3581(3) 0.7476(3) 0.0448(11) Uani 1 1 d . . . . .
H18 H 0.219524 0.301517 0.770623 0.054 Uiso 1 1 calc R U . . .
C19 C 0.2336(3) 0.3798(3) 0.6712(3) 0.0424(11) Uani 1 1 d . . . . .
H19 H 0.250502 0.338251 0.641945 0.051 Uiso 1 1 calc R U . . .
C20 C 0.2271(3) 0.4665(2) 0.6338(3) 0.0343(9) Uani 1 1 d . . . . .
C21 C 0.2407(3) 0.4917(3) 0.5544(3) 0.0375(10) Uani 1 1 d . . . . .
H21 H 0.258763 0.451069 0.524265 0.045 Uiso 1 1 calc R U . . .
C22 C 0.2281(3) 0.5754(3) 0.5187(2) 0.0340(9) Uani 1 1 d . . . . .
C23 C 0.2366(3) 0.6009(3) 0.4369(3) 0.0444(11) Uani 1 1 d . . . . .
H23 H 0.254515 0.560840 0.406165 0.053 Uiso 1 1 calc R U . . .
C24 C 0.2191(3) 0.6821(3) 0.4044(3) 0.0479(12) Uani 1 1 d . . . . .
H24 H 0.223742 0.697163 0.351467 0.058 Uiso 1 1 calc R U . . .
C25 C 0.1934(3) 0.7451(3) 0.4497(2) 0.0381(10) Uani 1 1 d . . . . .
H25 H 0.182254 0.800891 0.425760 0.046 Uiso 1 1 calc R U . . .
C26 C 0.1848(3) 0.7253(3) 0.5277(2) 0.0290(8) Uani 1 1 d . . . . .
C27 C 0.2014(2) 0.6383(2) 0.5650(2) 0.0285(8) Uani 1 1 d . . . . .
C28 C 0.1879(2) 0.6140(2) 0.6451(2) 0.0251(7) Uani 1 1 d . . . . .
H28 H 0.169955 0.654757 0.675158 0.030 Uiso 1 1 calc R U . . .
C29 C 0.2011(2) 0.5296(2) 0.6803(2) 0.0280(8) Uani 1 1 d . . . . .
C30 C 0.0827(3) 0.8373(2) 0.5642(2) 0.0293(8) Uani 1 1 d . . . . .
H30 H 0.044774 0.825248 0.533137 0.035 Uiso 1 1 calc R U . . .
C31 C 0.0542(3) 0.9076(2) 0.5997(2) 0.0284(8) Uani 1 1 d . . . . .
C32 C -0.0242(3) 0.9658(3) 0.5928(3) 0.0425(11) Uani 1 1 d . . . . .
H32 H -0.072063 0.963895 0.566413 0.051 Uiso 1 1 calc R U . . .
C33 C -0.0173(3) 1.0267(3) 0.6325(2) 0.0396(10) Uani 1 1 d . . . . .
H33 H -0.059745 1.073770 0.637839 0.048 Uiso 1 1 calc R U . . .
C34 C 0.0652(3) 1.0048(2) 0.6634(2) 0.0282(8) Uani 1 1 d . . . . .
C35 C 0.0975(3) 1.0487(2) 0.7173(2) 0.0281(8) Uani 1 1 d . . . . .
C36 C 0.0595(3) 1.0044(3) 0.8007(2) 0.0366(9) Uani 1 1 d . . . . .
H36A H 0.084200 0.945675 0.807035 0.044 Uiso 1 1 calc R U . . .
H36B H 0.084402 1.028894 0.835780 0.044 Uiso 1 1 calc R U . . .
C37 C -0.0463(3) 1.0086(3) 0.8245(3) 0.0469(11) Uani 1 1 d . . . . .
H37A H -0.071627 1.066118 0.823146 0.070 Uiso 1 1 calc R U . . .
H37B H -0.061652 0.976875 0.875483 0.070 Uiso 1 1 calc R U . . .
H37C H -0.072500 0.985660 0.789821 0.070 Uiso 1 1 calc R U . . .
C38 C 0.0570(3) 1.1425(2) 0.7045(3) 0.0400(10) Uani 1 1 d . . . . .
H38A H -0.010763 1.145096 0.710960 0.048 Uiso 1 1 calc R U . . .
H38B H 0.071623 1.167694 0.743947 0.048 Uiso 1 1 calc R U . . .
C39 C 0.0928(4) 1.1946(3) 0.6270(3) 0.0529(13) Uani 1 1 d . . . . .
H39A H 0.159486 1.194915 0.620785 0.079 Uiso 1 1 calc R U . . .
H39B H 0.063354 1.251137 0.623729 0.079 Uiso 1 1 calc R U . . .
H39C H 0.078097 1.170825 0.587311 0.079 Uiso 1 1 calc R U . . .
C40 C 0.2027(3) 1.0436(2) 0.7108(2) 0.0250(7) Uani 1 1 d . . . . .
C41 C 0.2513(3) 1.0978(2) 0.7361(2) 0.0342(9) Uani 1 1 d . . . . .
H41 H 0.224916 1.144225 0.757466 0.041 Uiso 1 1 calc R U . . .
C42 C 0.3464(3) 1.0690(2) 0.7232(2) 0.0341(9) Uani 1 1 d . . . . .
H42 H 0.395400 1.092176 0.734414 0.041 Uiso 1 1 calc R U . . .
C43 C 0.3532(3) 0.9982(2) 0.6900(2) 0.0245(7) Uani 1 1 d . . . . .
C44 C 0.4338(2) 0.9500(2) 0.6599(2) 0.0242(7) Uani 1 1 d . . . . .
H44 H 0.492677 0.964426 0.661355 0.029 Uiso 1 1 calc R U . . .
C45 C 0.5127(2) 0.8459(2) 0.5933(2) 0.0232(7) Uani 1 1 d . . . . .
C46 C 0.5471(3) 0.8765(2) 0.5178(2) 0.0274(8) Uani 1 1 d . . . . .
H46 H 0.516115 0.924201 0.491865 0.033 Uiso 1 1 calc R U . . .
C47 C 0.6288(3) 0.8368(2) 0.4786(2) 0.0298(8) Uani 1 1 d . . . . .
H47 H 0.651479 0.859404 0.427754 0.036 Uiso 1 1 calc R U . . .
C48 C 0.6742(3) 0.7661(2) 0.5147(2) 0.0301(8) Uani 1 1 d . . . . .
H48 H 0.727660 0.740500 0.488321 0.036 Uiso 1 1 calc R U . . .
C49 C 0.6407(2) 0.7306(2) 0.5929(2) 0.0265(8) Uani 1 1 d . . . . .
C50 C 0.6840(3) 0.6560(2) 0.6299(2) 0.0304(8) Uani 1 1 d . . . . .
H50 H 0.738961 0.631439 0.604468 0.036 Uiso 1 1 calc R U . . .
C51 C 0.6473(3) 0.6174(2) 0.7038(2) 0.0286(8) Uani 1 1 d . . . . .
C52 C 0.6902(3) 0.5390(3) 0.7401(2) 0.0349(9) Uani 1 1 d . . . . .
H52 H 0.744822 0.514003 0.714639 0.042 Uiso 1 1 calc R U . . .
C53 C 0.6517(3) 0.5009(3) 0.8111(3) 0.0386(10) Uani 1 1 d . . . . .
H53 H 0.680318 0.450031 0.834106 0.046 Uiso 1 1 calc R U . . .
C54 C 0.5684(3) 0.5377(3) 0.8507(2) 0.0340(9) Uani 1 1 d . . . . .
H54 H 0.541936 0.509495 0.898604 0.041 Uiso 1 1 calc R U . . .
C55 C 0.5257(2) 0.6142(2) 0.8199(2) 0.0258(7) Uani 1 1 d . . . . .
C56 C 0.5643(2) 0.6566(2) 0.7447(2) 0.0238(7) Uani 1 1 d . . . . .
C57 C 0.5237(2) 0.7342(2) 0.7096(2) 0.0230(7) Uani 1 1 d . . . . .
H57 H 0.472768 0.761888 0.736959 0.028 Uiso 1 1 calc R U . . .
C58 C 0.5586(2) 0.7709(2) 0.6337(2) 0.0231(7) Uani 1 1 d . . . . .
C59 C 0.3447(3) 0.4601(2) 0.8923(2) 0.0345(9) Uani 1 1 d . . . . .
H59 H 0.373457 0.470953 0.841165 0.041 Uiso 1 1 calc R U . . .
C60 C 0.3559(3) 0.3794(3) 0.9334(3) 0.0423(11) Uani 1 1 d . . . . .
H60 H 0.391443 0.336819 0.910677 0.051 Uiso 1 1 calc R U . . .
C61 C 0.3132(3) 0.3632(3) 1.0088(3) 0.0445(11) Uani 1 1 d . . . . .
H61 H 0.318940 0.309152 1.037839 0.053 Uiso 1 1 calc R U . . .
C62 C 0.2615(3) 0.4281(3) 1.0414(3) 0.0402(10) Uani 1 1 d . . . . .
H62 H 0.231646 0.418235 1.092234 0.048 Uiso 1 1 calc R U . . .
C63 C 0.2556(3) 0.5074(2) 0.9966(2) 0.0324(9) Uani 1 1 d . . . . .
H63 H 0.223131 0.551411 1.018922 0.039 Uiso 1 1 calc R U . . .
C64 C 0.2544(2) 1.0113(2) 0.4934(2) 0.0279(8) Uani 1 1 d . . . . .
H64 H 0.223244 1.038071 0.532898 0.034 Uiso 1 1 calc R U . . .
C65 C 0.2625(3) 1.0570(3) 0.4202(2) 0.0341(9) Uani 1 1 d . . . . .
H65 H 0.237402 1.112804 0.410276 0.041 Uiso 1 1 calc R U . . .
C66 C 0.3092(3) 1.0176(3) 0.3614(2) 0.0377(10) Uani 1 1 d . . . . .
H66 H 0.315677 1.046623 0.310900 0.045 Uiso 1 1 calc R U . . .
C67 C 0.3458(3) 0.9352(3) 0.3782(2) 0.0370(10) Uani 1 1 d . . . . .
H67 H 0.377589 0.907602 0.339477 0.044 Uiso 1 1 calc R U . . .
C68 C 0.3344(3) 0.8942(3) 0.4539(2) 0.0318(8) Uani 1 1 d . . . . .
H68 H 0.359991 0.838682 0.464979 0.038 Uiso 1 1 calc R U . . .
C69 C 0.4029(2) 0.6032(2) 0.6739(2) 0.0229(7) Uani 1 1 d . . . . .
C70 C 0.4616(3) 0.5297(2) 0.6681(2) 0.0286(8) Uani 1 1 d . . . . .
H70 H 0.463468 0.486757 0.710797 0.034 Uiso 1 1 calc R U . . .
C71 C 0.5178(3) 0.5201(2) 0.5983(2) 0.0333(9) Uani 1 1 d . . . . .
H71 H 0.557232 0.470956 0.594704 0.040 Uiso 1 1 calc R U . . .
C72 C 0.5151(3) 0.5837(2) 0.5345(2) 0.0310(8) Uani 1 1 d . . . . .
H72 H 0.552648 0.577337 0.488071 0.037 Uiso 1 1 calc R U . . .
C73 C 0.4560(2) 0.6569(2) 0.5401(2) 0.0266(8) Uani 1 1 d . . . . .
H73 H 0.454022 0.699458 0.497036 0.032 Uiso 1 1 calc R U . . .
C74 C 0.4000(2) 0.6674(2) 0.6090(2) 0.0219(7) Uani 1 1 d . . . . .
C75 C -0.0781(4) 0.7431(4) 0.7603(3) 0.0586(14) Uani 1 1 d . . . . .
C76 C -0.1575(4) 0.7182(4) 0.7437(4) 0.0734(18) Uani 1 1 d . . . . .
H76 H -0.154717 0.680778 0.711251 0.088 Uiso 1 1 calc R U . . .
C77 C -0.2473(5) 0.7566(4) 0.7822(4) 0.081(2) Uani 1 1 d . . . . .
H77 H -0.303817 0.745332 0.772273 0.097 Uiso 1 1 calc R U . . .
C78 C -0.2474(4) 0.8050(4) 0.8290(4) 0.0734(18) Uani 1 1 d . . . . .
H78 H -0.305089 0.826881 0.852741 0.088 Uiso 1 1 calc R U . . .
C79 C -0.1671(4) 0.8267(4) 0.8465(3) 0.0637(15) Uani 1 1 d . . . . .
H79 H -0.170152 0.860456 0.882243 0.076 Uiso 1 1 calc R U . . .
C80 C -0.0829(3) 0.7965(3) 0.8089(3) 0.0488(12) Uani 1 1 d . . . . .
B1 B 0.0677(4) 0.7627(4) 0.7652(3) 0.0503(14) Uani 1 1 d . . . . .
O10 O 0.3733(5) 0.1763(6) 0.9560(5) 0.113(2) Uani 0.795(7) 1 d D . P A 1
O11 O 0.4667(4) 0.1202(6) 1.0872(4) 0.113(2) Uani 0.795(7) 1 d D . P A 1
C100 C 0.2980(8) 0.1682(9) 0.9212(7) 0.107(4) Uani 0.795(7) 1 d . U P A 1
H10D H 0.316099 0.181094 0.866572 0.161 Uiso 0.795(7) 1 calc R U P A 1
H10E H 0.245159 0.206340 0.936692 0.161 Uiso 0.795(7) 1 calc R U P A 1
H10F H 0.281159 0.111659 0.936714 0.161 Uiso 0.795(7) 1 calc R U P A 1
C101 C 0.4387(5) 0.1127(5) 0.9645(4) 0.070(2) Uani 0.795(7) 1 d D U P A 1
H10G H 0.472911 0.106721 0.914193 0.084 Uiso 0.795(7) 1 calc R U P A 1
H10H H 0.408106 0.061895 0.986326 0.084 Uiso 0.795(7) 1 calc R U P A 1
C102 C 0.5055(5) 0.1182(5) 1.0117(4) 0.0627(19) Uani 0.795(7) 1 d D U P A 1
H10I H 0.552628 0.070341 1.010399 0.075 Uiso 0.795(7) 1 calc R U P A 1
H10J H 0.536956 0.168502 0.989944 0.075 Uiso 0.795(7) 1 calc R U P A 1
C103 C 0.5333(6) 0.1156(7) 1.1357(5) 0.083(3) Uani 0.795(7) 1 d . U P A 1
H10K H 0.575080 0.158241 1.113996 0.125 Uiso 0.795(7) 1 calc R U P A 1
H10L H 0.568544 0.061319 1.140451 0.125 Uiso 0.795(7) 1 calc R U P A 1
H10M H 0.501318 0.124185 1.185308 0.125 Uiso 0.795(7) 1 calc R U P A 1
O20 O 0.8921(4) 0.4265(4) 0.7199(5) 0.078(2) Uani 0.684(10) 1 d D U P B 1
O21 O 0.9121(16) 0.5646(17) 0.5820(15) 0.087(6) Uani 0.623(19) 1 d . U P B 1
C200 C 0.9089(7) 0.4385(7) 0.7958(6) 0.065(3) Uani 0.684(10) 1 d D U P B 1
H20A H 0.910835 0.497228 0.794166 0.098 Uiso 0.684(10) 1 calc R U P B 1
H20B H 0.967587 0.408290 0.806222 0.098 Uiso 0.684(10) 1 calc R U P B 1
H20C H 0.859077 0.417810 0.835413 0.098 Uiso 0.684(10) 1 calc R U P B 1
C201 C 0.9625(8) 0.4328(7) 0.6611(8) 0.078(3) Uani 0.684(10) 1 d D U P B 1
H20D H 0.946467 0.408407 0.621715 0.093 Uiso 0.684(10) 1 calc R U P B 1
H20E H 1.017414 0.399242 0.677897 0.093 Uiso 0.684(10) 1 calc R U P B 1
C202 C 0.9889(7) 0.5210(9) 0.6250(10) 0.080(3) Uani 0.623(19) 1 d D U P B 1
H20F H 0.994465 0.550915 0.664294 0.096 Uiso 0.623(19) 1 calc R U P B 1
H20G H 1.048486 0.518534 0.590382 0.096 Uiso 0.623(19) 1 calc R U P B 1
C203 C 0.9409(18) 0.6418(19) 0.5332(14) 0.111(8) Uani 0.623(19) 1 d . U P B 1
H20H H 0.993848 0.629347 0.495318 0.166 Uiso 0.623(19) 1 calc R U P B 1
H20I H 0.957958 0.676661 0.563538 0.166 Uiso 0.623(19) 1 calc R U P B 1
H20J H 0.890081 0.670681 0.508323 0.166 Uiso 0.623(19) 1 calc R U P B 1
O20A O 0.9306(11) 0.4812(9) 0.7314(11) 0.085(4) Uani 0.316(10) 1 d D U P B 2
O21A O 0.917(3) 0.580(2) 0.597(2) 0.058(5) Uani 0.377(19) 1 d . U P B 2
C1C C 0.9805(15) 0.5046(14) 0.5818(16) 0.084(4) Uani 0.377(19) 1 d D U P B 2
H1CA H 1.041537 0.518022 0.552888 0.101 Uiso 0.377(19) 1 calc R U P B 2
H1CB H 0.953186 0.469246 0.557170 0.101 Uiso 0.377(19) 1 calc R U P B 2
C1D C 0.940(3) 0.655(3) 0.5601(17) 0.061(5) Uani 0.377(19) 1 d . U P B 2
H1DA H 0.985236 0.648581 0.514700 0.091 Uiso 0.377(19) 1 calc R U P B 2
H1DB H 0.967688 0.679855 0.592499 0.091 Uiso 0.377(19) 1 calc R U P B 2
H1DC H 0.885695 0.689409 0.546065 0.091 Uiso 0.377(19) 1 calc R U P B 2
C1E C 0.9828(19) 0.469(2) 0.664(2) 0.082(4) Uani 0.316(10) 1 d D U P B 2
H1EA H 0.982987 0.408740 0.667209 0.099 Uiso 0.316(10) 1 calc R U P B 2
H1EB H 1.045675 0.475950 0.669784 0.099 Uiso 0.316(10) 1 calc R U P B 2
C1F C 0.911(2) 0.385(2) 0.7637(18) 0.109(8) Uani 0.316(10) 1 d D U P B 2
H1FA H 0.947531 0.350676 0.729553 0.163 Uiso 0.316(10) 1 calc R U P B 2
H1FB H 0.845634 0.379757 0.767262 0.163 Uiso 0.316(10) 1 calc R U P B 2
H1FC H 0.928298 0.366953 0.813464 0.163 Uiso 0.316(10) 1 calc R U P B 2
O30 O 0.4643(5) 0.7767(5) 0.3053(4) 0.0562(19) Uani 0.748(8) 1 d D U P C 1
O31 O 0.3828(4) 0.8948(4) 0.1921(3) 0.0620(17) Uani 0.748(8) 1 d . U P C 1
C300 C 0.5361(12) 0.7199(13) 0.3265(15) 0.069(5) Uani 0.748(8) 1 d . U P C 1
H30A H 0.581971 0.712833 0.281958 0.103 Uiso 0.748(8) 1 calc R U P C 1
H30B H 0.512519 0.666995 0.350553 0.103 Uiso 0.748(8) 1 calc R U P C 1
H30C H 0.564599 0.739679 0.361770 0.103 Uiso 0.748(8) 1 calc R U P C 1
C301 C 0.4309(7) 0.7547(7) 0.2451(6) 0.076(3) Uani 0.748(8) 1 d D U P C 1
H30D H 0.411802 0.698257 0.260577 0.092 Uiso 0.748(8) 1 calc R U P C 1
H30E H 0.480090 0.756137 0.200520 0.092 Uiso 0.748(8) 1 calc R U P C 1
C302 C 0.3486(7) 0.8163(6) 0.2258(6) 0.077(3) Uani 0.748(8) 1 d . U P C 1
H30F H 0.318155 0.797596 0.190420 0.093 Uiso 0.748(8) 1 calc R U P C 1
H30G H 0.303221 0.821089 0.271861 0.093 Uiso 0.748(8) 1 calc R U P C 1
C303 C 0.3102(6) 0.9567(7) 0.1677(5) 0.080(3) Uani 0.748(8) 1 d . . P C 1
H30H H 0.281552 0.937401 0.132167 0.120 Uiso 0.748(8) 1 calc R U P C 1
H30I H 0.336547 1.008289 0.143122 0.120 Uiso 0.748(8) 1 calc R U P C 1
H30J H 0.263868 0.965967 0.211232 0.120 Uiso 0.748(8) 1 calc R U P C 1
C1A C 0.2671(19) 0.9390(16) 0.1942(16) 0.080(3) Uani 0.252(8) 1 d D . P C 2
H1AA H 0.270443 0.943320 0.140146 0.120 Uiso 0.252(8) 1 calc R U P C 2
H1AB H 0.290627 0.987260 0.203077 0.120 Uiso 0.252(8) 1 calc R U P C 2
H1AC H 0.203073 0.936516 0.219395 0.120 Uiso 0.252(8) 1 calc R U P C 2
O31A O 0.3212(11) 0.8662(12) 0.2232(9) 0.064(4) Uani 0.252(8) 1 d D U P C 2
C1B C 0.4076(13) 0.8420(18) 0.1807(15) 0.073(4) Uani 0.252(8) 1 d D U P C 2
H1BA H 0.445571 0.888764 0.167903 0.088 Uiso 0.252(8) 1 calc R U P C 2
H1BB H 0.396620 0.830629 0.133054 0.088 Uiso 0.252(8) 1 calc R U P C 2
C1K C 0.459(2) 0.7710(18) 0.2175(16) 0.073(4) Uani 0.252(8) 1 d D U P C 2
H1KA H 0.419143 0.725764 0.237221 0.088 Uiso 0.252(8) 1 calc R U P C 2
H1KB H 0.511095 0.751987 0.180903 0.088 Uiso 0.252(8) 1 calc R U P C 2
O30A O 0.4932(15) 0.7908(17) 0.2778(12) 0.051(4) Uani 0.252(8) 1 d D U P C 2
C1L C 0.554(3) 0.731(3) 0.318(4) 0.045(7) Uani 0.252(8) 1 d D U P C 2
H1LA H 0.614723 0.727388 0.286470 0.067 Uiso 0.252(8) 1 calc R U P C 2
H1LB H 0.529537 0.677633 0.330003 0.067 Uiso 0.252(8) 1 calc R U P C 2
H1LC H 0.558535 0.748367 0.364134 0.067 Uiso 0.252(8) 1 calc R U P C 2
C1G C 0.514(3) 0.070(2) 1.1539(15) 0.075(8) Uiso 0.205(7) 1 d D U P A 2
H1GA H 0.579644 0.076727 1.139757 0.113 Uiso 0.205(7) 1 calc R U P A 2
H1GB H 0.504916 0.017712 1.188577 0.113 Uiso 0.205(7) 1 calc R U P A 2
H1GC H 0.482585 0.115469 1.178308 0.113 Uiso 0.205(7) 1 calc R U P A 2
O11A O 0.4765(12) 0.0718(10) 1.0883(10) 0.044(5) Uiso 0.205(7) 1 d D . P A 2
C1H C 0.374(2) 0.0971(12) 1.0078(16) 0.064(4) Uiso 0.205(7) 1 d D U P A 2
H1HA H 0.411626 0.062107 0.974151 0.077 Uiso 0.205(7) 1 calc R U P A 2
H1HB H 0.322461 0.068281 1.040853 0.077 Uiso 0.205(7) 1 calc R U P A 2
C1I C 0.425(2) 0.1357(14) 1.0460(18) 0.077(4) Uiso 0.205(7) 1 d D U P A 2
H1IA H 0.466556 0.172335 1.009364 0.093 Uiso 0.205(7) 1 calc R U P A 2
H1IB H 0.383216 0.168781 1.079349 0.093 Uiso 0.205(7) 1 calc R U P A 2
O10A O 0.3474(14) 0.1775(11) 0.9716(12) 0.045(5) Uiso 0.205(7) 1 d D . P A 2
C1J C 0.270(3) 0.154(4) 0.949(3) 0.116(12) Uiso 0.205(7) 1 d D U P A 2
H1JA H 0.239978 0.202207 0.919197 0.174 Uiso 0.205(7) 1 calc R U P A 2
H1JB H 0.226460 0.132749 0.993728 0.174 Uiso 0.205(7) 1 calc R U P A 2
H1JC H 0.290700 0.111428 0.919017 0.174 Uiso 0.205(7) 1 calc R U P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 O1 2.106(2) . ?
U1 F1 2.3000(18) . ?
U1 O3 2.429(2) . ?
U1 N3 2.461(3) . ?
U1 N2 2.491(3) . ?
U1 N9 2.607(3) . ?
U1 N4 2.625(3) . ?
U1 N1 2.662(3) . ?
U1 U2 3.84902(19) . ?
U2 O2 2.106(2) . ?
U2 O3 2.373(2) . ?
U2 F1 2.3741(19) . ?
U2 N7 2.463(3) . ?
U2 N6 2.466(3) . ?
U2 N8 2.577(3) . ?
U2 N5 2.607(3) . ?
U2 N10 2.616(3) . ?
O1 C69 1.360(4) . ?
O2 C74 1.355(4) . ?
O3 B1 1.379(7) . ?
O4 C75 1.293(6) . ?
O4 B1 1.407(7) . ?
O5 C80 1.375(6) . ?
O5 B1 1.431(7) . ?
N1 C1 1.298(5) . ?
N1 C55 1.427(5) . ?
N2 C5 1.362(5) . ?
N2 C2 1.385(5) . ?
N3 C11 1.364(5) . ?
N3 C14 1.385(4) . ?
N4 C15 1.307(5) . ?
N4 C16 1.426(5) . ?
N5 C30 1.302(5) . ?
N5 C26 1.427(5) . ?
N6 C34 1.368(5) . ?
N6 C31 1.390(5) . ?
N7 C40 1.364(4) . ?
N7 C43 1.396(4) . ?
N8 C44 1.300(4) . ?
N8 C45 1.430(4) . ?
N9 C59 1.344(5) . ?
N9 C63 1.348(5) . ?
N10 C68 1.340(5) . ?
N10 C64 1.353(5) . ?
C1 C2 1.412(6) . ?
C2 C3 1.396(5) . ?
C3 C4 1.394(6) . ?
C4 C5 1.401(5) . ?
C5 C6 1.509(5) . ?
C6 C11 1.514(5) . ?
C6 C9 1.542(5) . ?
C6 C7 1.555(5) . ?
C7 C8 1.533(5) . ?
C9 C10 1.538(6) . ?
C11 C12 1.398(5) . ?
C12 C13 1.387(6) . ?
C13 C14 1.391(5) . ?
C14 C15 1.406(5) . ?
C16 C17 1.367(5) . ?
C16 C29 1.438(6) . ?
C17 C18 1.422(6) . ?
C18 C19 1.338(7) . ?
C19 C20 1.435(6) . ?
C20 C21 1.394(6) . ?
C20 C29 1.437(5) . ?
C21 C22 1.387(6) . ?
C22 C27 1.434(5) . ?
C22 C23 1.438(6) . ?
C23 C24 1.345(7) . ?
C24 C25 1.423(6) . ?
C25 C26 1.368(5) . ?
C26 C27 1.450(6) . ?
C27 C28 1.404(5) . ?
C28 C29 1.398(5) . ?
C30 C31 1.414(6) . ?
C31 C32 1.392(5) . ?
C32 C33 1.375(6) . ?
C33 C34 1.398(5) . ?
C34 C35 1.510(5) . ?
C35 C40 1.510(5) . ?
C35 C38 1.553(5) . ?
C35 C36 1.562(5) . ?
C36 C37 1.517(6) . ?
C38 C39 1.517(6) . ?
C40 C41 1.409(5) . ?
C41 C42 1.394(6) . ?
C42 C43 1.402(5) . ?
C43 C44 1.410(5) . ?
C45 C46 1.373(5) . ?
C45 C58 1.441(5) . ?
C46 C47 1.416(5) . ?
C47 C48 1.357(5) . ?
C48 C49 1.429(5) . ?
C49 C50 1.394(5) . ?
C49 C58 1.438(5) . ?
C50 C51 1.391(5) . ?
C51 C52 1.432(5) . ?
C51 C56 1.439(5) . ?
C52 C53 1.354(6) . ?
C53 C54 1.415(6) . ?
C54 C55 1.375(5) . ?
C55 C56 1.435(5) . ?
C56 C57 1.402(5) . ?
C57 C58 1.403(5) . ?
C59 C60 1.377(6) . ?
C60 C61 1.375(7) . ?
C61 C62 1.387(6) . ?
C62 C63 1.378(5) . ?
C64 C65 1.370(5) . ?
C65 C66 1.382(6) . ?
C66 C67 1.375(6) . ?
C67 C68 1.382(6) . ?
C69 C70 1.390(5) . ?
C69 C74 1.402(5) . ?
C70 C71 1.394(5) . ?
C71 C72 1.383(6) . ?
C72 C73 1.388(5) . ?
C73 C74 1.385(5) . ?
C75 C80 1.356(7) . ?
C75 C76 1.387(7) . ?
C76 C77 1.485(9) . ?
C77 C78 1.282(8) . ?
C78 C79 1.385(8) . ?
C79 C80 1.369(7) . ?
O10 C101 1.317(7) . ?
O10 C100 1.406(10) . ?
O11 C102 1.383(7) . ?
O11 C103 1.419(9) . ?
C101 C102 1.443(7) . ?
O20 C201 1.327(15) . ?
O20 C200 1.503(13) . ?
O21 C203 1.44(4) . ?
O21 C202 1.50(3) . ?
C201 C202 1.520(19) . ?
O20A C1E 1.35(4) . ?
O20A C1F 1.60(3) . ?
O21A C1D 1.31(5) . ?
O21A C1C 1.49(4) . ?
C1C C1E 1.49(5) . ?
O30 C300 1.359(12) . ?
O30 C301 1.412(9) . ?
O31 C302 1.414(11) . ?
O31 C303 1.428(10) . ?
C301 C302 1.504(14) . ?
C1A O31A 1.399(8) . ?
O31A C1B 1.399(8) . ?
C1B C1K 1.408(10) . ?
C1K O30A 1.402(8) . ?
O30A C1L 1.402(8) . ?
C1G O11A 1.397(10) . ?
O11A C1I 1.381(10) . ?
C1H O10A 1.378(10) . ?
C1H C1I 1.405(7) . ?
O10A C1J 1.400(10) . ?

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 F1 89.79(8) . . ?
O1 U1 O3 93.87(9) . . ?
F1 U1 O3 63.88(7) . . ?
O1 U1 N3 143.29(9) . . ?
F1 U1 N3 116.65(8) . . ?
O3 U1 N3 77.61(9) . . ?
O1 U1 N2 141.32(9) . . ?
F1 U1 N2 87.60(8) . . ?
O3 U1 N2 119.05(9) . . ?
N3 U1 N2 69.05(10) . . ?
O1 U1 N9 87.74(10) . . ?
F1 U1 N9 151.49(8) . . ?
O3 U1 N9 144.62(9) . . ?
N3 U1 N9 80.17(10) . . ?
N2 U1 N9 76.92(10) . . ?
O1 U1 N4 76.24(9) . . ?
F1 U1 N4 136.28(8) . . ?
O3 U1 N4 75.81(8) . . ?
N3 U1 N4 67.05(10) . . ?
N2 U1 N4 128.46(10) . . ?
N9 U1 N4 70.29(9) . . ?
O1 U1 N1 75.96(9) . . ?
F1 U1 N1 80.07(8) . . ?
O3 U1 N1 142.71(8) . . ?
N3 U1 N1 130.65(9) . . ?
N2 U1 N1 65.58(10) . . ?
N9 U1 N1 71.78(9) . . ?
N4 U1 N1 133.25(9) . . ?
O1 U1 U2 75.25(7) . . ?
F1 U1 U2 35.20(5) . . ?
O3 U1 U2 36.24(5) . . ?
N3 U1 U2 111.18(6) . . ?
N2 U1 U2 119.05(6) . . ?
N9 U1 U2 162.53(7) . . ?
N4 U1 U2 101.19(6) . . ?
N1 U1 U2 107.05(6) . . ?
O2 U2 O3 92.93(9) . . ?
O2 U2 F1 87.09(8) . . ?
O3 U2 F1 63.67(7) . . ?
O2 U2 N7 143.93(9) . . ?
O3 U2 N7 111.27(9) . . ?
F1 U2 N7 80.77(8) . . ?
O2 U2 N6 143.82(9) . . ?
O3 U2 N6 82.16(9) . . ?
F1 U2 N6 121.25(8) . . ?
N7 U2 N6 68.61(10) . . ?
O2 U2 N8 76.39(9) . . ?
O3 U2 N8 135.75(8) . . ?
F1 U2 N8 72.88(8) . . ?
N7 U2 N8 67.59(9) . . ?
N6 U2 N8 130.30(9) . . ?
O2 U2 N5 75.58(9) . . ?
O3 U2 N5 79.24(8) . . ?
F1 U2 N5 138.13(8) . . ?
N7 U2 N5 133.43(9) . . ?
N6 U2 N5 68.28(10) . . ?
N8 U2 N5 135.73(9) . . ?
O2 U2 N10 90.31(10) . . ?
O3 U2 N10 149.32(8) . . ?
F1 U2 N10 147.00(8) . . ?
N7 U2 N10 82.20(9) . . ?
N6 U2 N10 77.40(9) . . ?
N8 U2 N10 74.54(9) . . ?
N5 U2 N10 72.07(9) . . ?
O2 U2 U1 73.12(7) . . ?
O3 U2 U1 37.23(6) . . ?
F1 U2 U1 33.94(4) . . ?
N7 U2 U1 110.29(6) . . ?
N6 U2 U1 116.86(7) . . ?
N8 U2 U1 99.55(6) . . ?
N5 U2 U1 104.19(6) . . ?
N10 U2 U1 163.37(7) . . ?
U1 F1 U2 110.86(7) . . ?
C69 O1 U1 164.6(2) . . ?
C74 O2 U2 168.1(2) . . ?
B1 O3 U2 126.8(3) . . ?
B1 O3 U1 126.4(3) . . ?
U2 O3 U1 106.53(9) . . ?
C75 O4 B1 110.6(5) . . ?
C80 O5 B1 104.8(4) . . ?
C1 N1 C55 116.2(3) . . ?
C1 N1 U1 113.1(2) . . ?
C55 N1 U1 128.0(2) . . ?
C5 N2 C2 105.9(3) . . ?
C5 N2 U1 135.5(2) . . ?
C2 N2 U1 116.8(2) . . ?
C11 N3 C14 106.5(3) . . ?
C11 N3 U1 136.3(2) . . ?
C14 N3 U1 116.7(2) . . ?
C15 N4 C16 117.0(3) . . ?
C15 N4 U1 112.8(2) . . ?
C16 N4 U1 128.5(2) . . ?
C30 N5 C26 116.8(3) . . ?
C30 N5 U2 112.4(2) . . ?
C26 N5 U2 129.5(2) . . ?
C34 N6 C31 105.8(3) . . ?
C34 N6 U2 139.0(2) . . ?
C31 N6 U2 114.8(2) . . ?
C40 N7 C43 106.2(3) . . ?
C40 N7 U2 138.5(2) . . ?
C43 N7 U2 114.0(2) . . ?
C44 N8 C45 118.3(3) . . ?
C44 N8 U2 113.3(2) . . ?
C45 N8 U2 128.3(2) . . ?
C59 N9 C63 117.1(3) . . ?
C59 N9 U1 119.0(3) . . ?
C63 N9 U1 123.7(3) . . ?
C68 N10 C64 115.8(3) . . ?
C68 N10 U2 121.3(3) . . ?
C64 N10 U2 122.7(3) . . ?
N1 C1 C2 121.9(3) . . ?
N2 C2 C3 110.2(4) . . ?
N2 C2 C1 120.2(3) . . ?
C3 C2 C1 129.6(4) . . ?
C4 C3 C2 106.6(4) . . ?
C3 C4 C5 106.6(4) . . ?
N2 C5 C4 110.6(4) . . ?
N2 C5 C6 119.2(3) . . ?
C4 C5 C6 130.0(4) . . ?
C5 C6 C11 108.0(3) . . ?
C5 C6 C9 111.6(3) . . ?
C11 C6 C9 109.9(3) . . ?
C5 C6 C7 107.0(3) . . ?
C11 C6 C7 110.2(3) . . ?
C9 C6 C7 110.0(3) . . ?
C8 C7 C6 113.7(3) . . ?
C10 C9 C6 114.3(4) . . ?
N3 C11 C12 109.8(3) . . ?
N3 C11 C6 120.7(3) . . ?
C12 C11 C6 129.5(4) . . ?
C13 C12 C11 107.1(4) . . ?
C12 C13 C14 106.9(4) . . ?
N3 C14 C13 109.6(3) . . ?
N3 C14 C15 120.6(3) . . ?
C13 C14 C15 129.6(4) . . ?
N4 C15 C14 122.4(3) . . ?
C17 C16 N4 120.6(4) . . ?
C17 C16 C29 119.8(4) . . ?
N4 C16 C29 119.5(3) . . ?
C16 C17 C18 120.7(4) . . ?
C19 C18 C17 121.3(4) . . ?
C18 C19 C20 120.7(4) . . ?
C21 C20 C19 122.6(4) . . ?
C21 C20 C29 118.8(4) . . ?
C19 C20 C29 118.6(4) . . ?
C22 C21 C20 122.3(4) . . ?
C21 C22 C27 119.0(4) . . ?
C21 C22 C23 122.3(4) . . ?
C27 C22 C23 118.7(4) . . ?
C24 C23 C22 120.8(4) . . ?
C23 C24 C25 121.0(4) . . ?
C26 C25 C24 121.2(4) . . ?
C25 C26 N5 121.3(4) . . ?
C25 C26 C27 119.4(4) . . ?
N5 C26 C27 119.4(3) . . ?
C28 C27 C22 119.5(4) . . ?
C28 C27 C26 121.6(3) . . ?
C22 C27 C26 118.9(4) . . ?
C29 C28 C27 120.9(3) . . ?
C28 C29 C20 119.5(4) . . ?
C28 C29 C16 121.6(3) . . ?
C20 C29 C16 118.8(3) . . ?
N5 C30 C31 122.9(3) . . ?
N6 C31 C32 109.9(4) . . ?
N6 C31 C30 121.5(3) . . ?
C32 C31 C30 128.5(4) . . ?
C33 C32 C31 107.0(4) . . ?
C32 C33 C34 107.4(4) . . ?
N6 C34 C33 110.0(4) . . ?
N6 C34 C35 123.3(3) . . ?
C33 C34 C35 126.3(4) . . ?
C40 C35 C34 114.6(3) . . ?
C40 C35 C38 109.1(3) . . ?
C34 C35 C38 109.8(3) . . ?
C40 C35 C36 106.2(3) . . ?
C34 C35 C36 107.5(3) . . ?
C38 C35 C36 109.5(3) . . ?
C37 C36 C35 116.6(4) . . ?
C39 C38 C35 115.1(4) . . ?
N7 C40 C41 110.1(3) . . ?
N7 C40 C35 124.3(3) . . ?
C41 C40 C35 125.5(3) . . ?
C42 C41 C40 107.4(3) . . ?
C41 C42 C43 106.3(3) . . ?
N7 C43 C42 110.1(3) . . ?
N7 C43 C44 120.4(3) . . ?
C42 C43 C44 129.4(3) . . ?
N8 C44 C43 121.8(3) . . ?
C46 C45 N8 119.9(3) . . ?
C46 C45 C58 119.9(3) . . ?
N8 C45 C58 120.1(3) . . ?
C45 C46 C47 121.4(3) . . ?
C48 C47 C46 120.4(4) . . ?
C47 C48 C49 120.7(4) . . ?
C50 C49 C48 121.4(4) . . ?
C50 C49 C58 119.0(3) . . ?
C48 C49 C58 119.5(3) . . ?
C51 C50 C49 121.7(4) . . ?
C50 C51 C52 121.2(4) . . ?
C50 C51 C56 119.6(3) . . ?
C52 C51 C56 119.2(4) . . ?
C53 C52 C51 120.5(4) . . ?
C52 C53 C54 120.6(4) . . ?
C55 C54 C53 121.5(4) . . ?
C54 C55 N1 120.7(3) . . ?
C54 C55 C56 119.5(4) . . ?
N1 C55 C56 119.9(3) . . ?
C57 C56 C55 122.4(3) . . ?
C57 C56 C51 118.9(3) . . ?
C55 C56 C51 118.6(3) . . ?
C56 C57 C58 121.1(3) . . ?
C57 C58 C49 119.5(3) . . ?
C57 C58 C45 122.4(3) . . ?
C49 C58 C45 118.0(3) . . ?
N9 C59 C60 123.6(4) . . ?
C61 C60 C59 118.3(4) . . ?
C60 C61 C62 119.6(4) . . ?
C63 C62 C61 118.3(4) . . ?
N9 C63 C62 123.1(4) . . ?
N10 C64 C65 124.5(4) . . ?
C64 C65 C66 118.0(4) . . ?
C67 C66 C65 119.4(4) . . ?
C66 C67 C68 118.5(4) . . ?
N10 C68 C67 123.8(4) . . ?
O1 C69 C70 121.7(3) . . ?
O1 C69 C74 118.7(3) . . ?
C70 C69 C74 119.5(3) . . ?
C69 C70 C71 120.2(4) . . ?
C72 C71 C70 120.1(4) . . ?
C71 C72 C73 119.8(4) . . ?
C74 C73 C72 120.7(4) . . ?
O2 C74 C73 121.9(3) . . ?
O2 C74 C69 118.5(3) . . ?
C73 C74 C69 119.6(3) . . ?
O4 C75 C80 108.8(5) . . ?
O4 C75 C76 128.8(6) . . ?
C80 C75 C76 122.5(6) . . ?
C75 C76 C77 114.2(6) . . ?
C78 C77 C76 120.6(6) . . ?
C77 C78 C79 124.1(7) . . ?
C80 C79 C78 117.1(6) . . ?
C75 C80 C79 121.5(5) . . ?
C75 C80 O5 110.6(5) . . ?
C79 C80 O5 127.9(5) . . ?
O3 B1 O4 128.5(5) . . ?
O3 B1 O5 126.2(5) . . ?
O4 B1 O5 105.3(5) . . ?
C101 O10 C100 118.5(10) . . ?
C102 O11 C103 114.3(7) . . ?
O10 C101 C102 116.3(7) . . ?
O11 C102 C101 114.3(6) . . ?
C201 O20 C200 118.6(8) . . ?
C203 O21 C202 110.2(18) . . ?
O20 C201 C202 116.4(11) . . ?
O21 C202 C201 106.9(14) . . ?
C1E O20A C1F 96(2) . . ?
C1D O21A C1C 119(3) . . ?
O21A C1C C1E 95(3) . . ?
O20A C1E C1C 136(2) . . ?
C300 O30 C301 110.0(15) . . ?
C302 O31 C303 111.9(8) . . ?
O30 C301 C302 108.6(8) . . ?
O31 C302 C301 107.7(8) . . ?
C1B O31A C1A 120(2) . . ?
O31A C1B C1K 115(3) . . ?
O30A C1K C1B 110(2) . . ?
C1L O30A C1K 120(4) . . ?
C1I O11A C1G 130(2) . . ?
O10A C1H C1I 85.5(17) . . ?
O11A C1I C1H 106.7(19) . . ?
C1H O10A C1J 94(3) . . ?

_refine_diff_density_max         1.820
_refine_diff_density_min         -1.282
_refine_diff_density_rms         0.143



# start Validation Reply Form
_vrf_PLAT411_compound5A          
;
PROBLEM: Short Inter H...H Contact  H78      ..H1IB     .       1.51 Ang.  
RESPONSE: Both H(78) and H(1IB) are generated in calculated positions, 
however, H(1IB) belongs to a highly disordered molecule of lattice
1,2-dme that has been split into two parts. This has been left as is because 
the disordered molecule of lattice solvent was modelled to the best of our
abilities.
;
_vrf_PLAT230_compound5A          
;
PROBLEM: Hirshfeld Test Diff for    O3       --B1       .        9.3 s.u.  
RESPONSE: This has been investigated and the following observations have
been made: (1) there is no residual electron density in close proximity to
O(3) or B(1), indicating that electron density hasn't been missed in 
assigning the identity of these atoms, and (2) R1 increases when O(3) and B(1)
are changed to different elements. As a result, we are satisfied with our 
assignments and this alert has been noted but is not serious.
;
_vrf_PLAT910_compound5A          
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         20 Note  
RESPONSE: This has been noted, but is not serious. The independent 
reflections/parameters ratio is equal to 24.1, indicating that there are 
no issues with the data collected.
;
_vrf_PLAT973_compound5A          
;
PROBLEM: Check Calcd Positive Resid. Density on        U1       1.94 eA-3  
RESPONSE: The positive residual electron density on U(1) is caused by 
uranium being such a heavy metal, and is often seen with 3rd row 
transition metals and f-block elements due to their strong scattering 
properties.
;
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: 1,2-dimethoxyethane'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_compound2
_database_code_depnum_ccdc_archive 'CCDC 1984901'
loop_
_audit_author_name
_audit_author_address
'Bradley E. Cowie'
;The University of Edinburgh
United Kingdom
;
_audit_update_record             
;
2020-02-18 deposited with the CCDC.	2020-06-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        '[{(py)U(OMe)1.69(OH)0.31U(O2C6H4)(py)}(LA)]'
_chemical_name_common            'Compound 2.C6H6'
_chemical_melting_point          ?
_chemical_formula_moiety         'C75.69 H67.06 N10 O4 U2, C6 H6'
_chemical_formula_sum            'C81.69 H73.06 N10 O4 U2'
_chemical_formula_weight         1734.84

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   10.6363(6)
_cell_length_b                   14.9997(8)
_cell_length_c                   21.8493(12)
_cell_angle_alpha                90.546(4)
_cell_angle_beta                 102.195(5)
_cell_angle_gamma                94.113(5)
_cell_volume                     3397.3(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    7933
_cell_measurement_theta_min      3.2610
_cell_measurement_theta_max      23.2020

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.696
_exptl_crystal_F_000             1698
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.062
_exptl_crystal_size_min          0.036
_exptl_absorpt_coefficient_mu    4.822
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   Analytical
_exptl_absorpt_correction_T_min  0.965
_exptl_absorpt_correction_T_max  0.988
_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   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Eos
_diffrn_detector_area_resol_mean 8.0521
_diffrn_reflns_number            66944
_diffrn_reflns_av_unetI/netI     0.1039
_diffrn_reflns_av_R_equivalents  0.1173
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         2.862
_diffrn_reflns_theta_max         25.350
_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             12421
_reflns_number_gt                8941
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -87.00 -32.00   1.00   30.00    --  -16.53 179.00 120.00   55
  2  ω    -25.00  20.00   1.00   30.00    --  -16.53 -99.00 -30.00   45
  3  ω    -25.00  20.00   1.00   30.00    --  -16.53 -99.00 120.00   45
  4  ω    -25.00  20.00   1.00   30.00    --  -16.53 -99.00 150.00   45
  5  ω    -25.00  20.00   1.00   30.00    --  -16.53 -99.00 -90.00   45
  6  ω    -34.00  52.00   1.00   30.00    --  -16.53  37.00  90.00   86
  7  ω    -25.00  55.00   1.00   30.00    --   18.25 -99.00 150.00   80
  8  ω    -47.00  33.00   1.00   30.00    --   18.25 -57.00-120.00   80
  9  ω    -51.00  88.00   1.00   30.00    --   18.25   0.00  90.00  139
 10  ω    -34.00  52.00   1.00   30.00    --  -16.53  37.00   0.00   86
 11  ω    -25.00  20.00   1.00   30.00    --  -16.53 -99.00  60.00   45
 12  ω      3.00  84.00   1.00   30.00    --   18.25  57.00 -90.00   81
 13  ω      3.00  72.00   1.00   30.00    --   18.25  57.00 120.00   69
 14  ω    -25.00  55.00   1.00   30.00    --   18.25 -99.00   0.00   80
;

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

_computing_data_collection       '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 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_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 lattice benzene was positionally disordered over two positions. 
As a result, it was split into two parts and refined with an occupancy ratio 
of 0.58:0.42. In addition, the thermal parameters of the carbon atoms were 
restrained to be similar to one another through the use of the SIMU command.
C(8) was also positionally disordered over two positions,
and was split into two parts and refined with a 0.58:0.42 ratio. The thermal
parameters of C(8) and C(8A) were restrained to be similar to one another
through the use of the SIMU command, and the C(7)-C(8) and C(7)-C(8A) 
distances were restrained to be similar to one another using the SADI 
command. The thermal ellipsoids of the carbon atoms of the 
bridging catecholate ligand (C(69)-C(74)) were restrained using the RIGU
command, and the thermal ellipsoids of the carbon atoms of one of the 
anthracenyl ligand linkers (C(45)-C(58)) were restrained using the RIGU 
command. Finally, one of the 
bridging methoxy ligands possesses full occupancy (C(75)) whereas the other 
only possesses partial occupancy (C(76)). C(76) was refined freely with an
occupancy of 0.69, and the remainder of the 0.31 occupancy bound to O(4) 
is attributed to a hydrogen atom (based on a 1H NMR spectrum indicating that
there is one methoxy and one hydroxy ligand bridging the two U centres). 
However, the hydrogen atom with 0.31 occupancy was not located in the 
difference map.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     'w=1/[σ²(Fo²)] 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         12421
_refine_ls_number_parameters     932
_refine_ls_number_restraints     349
_refine_ls_R_factor_all          0.0856
_refine_ls_R_factor_gt           0.0520
_refine_ls_wR_factor_ref         0.0700
_refine_ls_wR_factor_gt          0.0629
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_restrained_S_all      1.007
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.46569(3) 0.61284(2) 0.21963(2) 0.01565(8) Uani 1 1 d . . . . .
U2 U 0.62937(2) 0.78062(2) 0.34662(2) 0.01344(8) Uani 1 1 d . . . . .
O1 O 0.4117(4) 0.7355(3) 0.1793(2) 0.0178(12) Uani 1 1 d . . . . .
O4 O 0.6686(4) 0.6676(3) 0.2774(2) 0.0160(11) Uani 1 1 d . . . . .
O2 O 0.5367(4) 0.8538(3) 0.2701(2) 0.0188(12) Uani 1 1 d . . . . .
O3 O 0.4729(4) 0.6596(3) 0.3237(2) 0.0187(12) Uani 1 1 d . . . . .
C28 C 0.2425(6) 0.7995(5) 0.2747(3) 0.0164(18) Uani 1 1 d . . . . .
H28 H 0.290407 0.756033 0.296687 0.020 Uiso 1 1 calc R U . . .
N10 N 0.7119(5) 0.9313(4) 0.4096(3) 0.0215(15) Uani 1 1 d . . . . .
N7 N 0.6243(5) 0.7436(4) 0.4564(3) 0.0158(14) Uani 1 1 d . . . . .
N6 N 0.8434(5) 0.7457(4) 0.4075(3) 0.0158(14) Uani 1 1 d . . . . .
C45 C 0.8143(6) 0.9232(5) 0.2577(3) 0.0182(15) Uani 1 1 d . . . . .
C43 C 0.9474(6) 0.7722(5) 0.3807(3) 0.0182(18) Uani 1 1 d . . . . .
N8 N 0.4382(5) 0.8482(4) 0.3843(3) 0.0175(14) Uani 1 1 d . . . . .
N2 N 0.5835(5) 0.4835(4) 0.1976(3) 0.0248(16) Uani 1 1 d . . . . .
C64 C 0.6887(7) 1.0091(5) 0.3820(4) 0.027(2) Uani 1 1 d . . . . .
H64 H 0.638173 1.008371 0.341616 0.032 Uiso 1 1 calc R U . . .
C34 C 0.6907(6) 0.6977(5) 0.5034(3) 0.0183(17) Uani 1 1 d . . . . .
C27 C 0.2615(6) 0.8861(5) 0.2982(3) 0.0158(17) Uani 1 1 d . . . . .
C26 C 0.3558(6) 0.9125(4) 0.3540(3) 0.0140(17) Uani 1 1 d . . . . .
N3 N 0.3681(5) 0.4734(4) 0.2544(3) 0.0203(15) Uani 1 1 d . . . . .
N9 N 0.3252(5) 0.5373(4) 0.1159(3) 0.0230(15) Uani 1 1 d . . . . .
C31 C 0.5247(6) 0.7782(5) 0.4796(3) 0.0191(18) Uani 1 1 d . . . . .
N1 N 0.5942(5) 0.6407(4) 0.1289(3) 0.0235(16) Uani 1 1 d . . . . .
N5 N 0.8180(5) 0.8536(3) 0.3021(3) 0.0162(14) Uani 1 1 d . . . . .
C30 C 0.4370(7) 0.8319(5) 0.4425(4) 0.0228(19) Uani 1 1 d . . . . .
H30 H 0.375331 0.856814 0.460426 0.027 Uiso 1 1 calc R U . . .
C42 C 1.0585(7) 0.7348(5) 0.4124(4) 0.025(2) Uani 1 1 d . . . . .
H42 H 1.140333 0.742406 0.403543 0.031 Uiso 1 1 calc R U . . .
N4 N 0.2188(5) 0.6190(4) 0.2220(3) 0.0181(14) Uani 1 1 d . . . . .
C74 C 0.4710(6) 0.8850(5) 0.2148(3) 0.0159(15) Uani 1 1 d . . . . .
C68 C 0.7837(7) 0.9341(6) 0.4671(4) 0.037(2) Uani 1 1 d . . . . .
H68 H 0.800668 0.880565 0.487256 0.044 Uiso 1 1 calc R U . . .
C58 C 0.7560(6) 0.9039(5) 0.1929(3) 0.0176(14) Uani 1 1 d . . . . .
C1 C 0.6436(7) 0.5680(6) 0.1134(4) 0.030(2) Uani 1 1 d . . . . .
H1 H 0.680018 0.568797 0.078294 0.036 Uiso 1 1 calc R U . . .
C49 C 0.7456(6) 0.9762(5) 0.1498(4) 0.0243(15) Uani 1 1 d . . . . .
C40 C 0.8911(6) 0.6933(5) 0.4560(3) 0.0177(17) Uani 1 1 d . . . . .
C20 C 0.0800(6) 0.8410(5) 0.1863(3) 0.0192(18) Uani 1 1 d . . . . .
C21 C 0.0998(6) 0.9286(5) 0.2102(4) 0.023(2) Uani 1 1 d . . . . .
H21 H 0.052059 0.972090 0.188146 0.028 Uiso 1 1 calc R U . . .
C11 C 0.4073(8) 0.3901(5) 0.2706(3) 0.0243(19) Uani 1 1 d . . . . .
C15 C 0.1653(7) 0.5439(5) 0.2365(3) 0.025(2) Uani 1 1 d . . . . .
H15 H 0.076891 0.538732 0.234579 0.030 Uiso 1 1 calc R U . . .
C41 C 1.0234(7) 0.6849(5) 0.4590(3) 0.0248(19) Uani 1 1 d . . . . .
H41 H 1.077203 0.651431 0.487584 0.030 Uiso 1 1 calc R U . . .
C75 C 0.4003(8) 0.6193(5) 0.3656(4) 0.045(3) Uani 1 1 d . . . . .
H75A H 0.312267 0.634196 0.353724 0.067 Uiso 1 1 calc R U . . .
H75B H 0.436321 0.641047 0.407556 0.067 Uiso 1 1 calc R U . . .
H75C H 0.403360 0.555547 0.363659 0.067 Uiso 1 1 calc R U . . .
C57 C 0.7064(6) 0.8181(5) 0.1709(3) 0.0204(16) Uani 1 1 d . . . . .
H57 H 0.714648 0.771352 0.198742 0.025 Uiso 1 1 calc R U . . .
C36 C 0.7677(7) 0.5530(5) 0.4727(3) 0.0232(19) Uani 1 1 d . . . . .
H36A H 0.714694 0.557687 0.431022 0.028 Uiso 1 1 calc R U . . .
H36B H 0.844129 0.524162 0.468132 0.028 Uiso 1 1 calc R U . . .
C55 C 0.5903(6) 0.7127(5) 0.0858(4) 0.0217(16) Uani 1 1 d . . . . .
C5 C 0.5966(7) 0.3992(5) 0.2195(4) 0.032(2) Uani 1 1 d . . . . .
C39 C 0.9516(7) 0.7338(5) 0.5967(4) 0.039(2) Uani 1 1 d . . . . .
H39A H 1.006821 0.723912 0.636483 0.059 Uiso 1 1 calc R U . . .
H39B H 0.882607 0.768400 0.602795 0.059 Uiso 1 1 calc R U . . .
H39C H 1.000571 0.765488 0.570448 0.059 Uiso 1 1 calc R U . . .
C3 C 0.6955(8) 0.4097(6) 0.1372(4) 0.048(3) Uani 1 1 d . . . . .
H3 H 0.740131 0.397156 0.106216 0.058 Uiso 1 1 calc R U . . .
C13 C 0.1968(8) 0.3856(5) 0.2723(4) 0.039(2) Uani 1 1 d . . . . .
H13 H 0.113975 0.366156 0.276348 0.047 Uiso 1 1 calc R U . . .
C29 C 0.1539(6) 0.7742(5) 0.2192(3) 0.0179(18) Uani 1 1 d . . . . .
C46 C 0.8618(6) 1.0079(5) 0.2761(4) 0.0243(17) Uani 1 1 d . . . . .
H46 H 0.901696 1.019905 0.317800 0.029 Uiso 1 1 calc R U . . .
C71 C 0.3372(7) 0.9443(5) 0.1014(4) 0.0274(18) Uani 1 1 d . . . . .
H71 H 0.293020 0.963867 0.063130 0.033 Uiso 1 1 calc R U . . .
C61 C 0.1602(7) 0.4635(6) 0.0100(4) 0.032(2) Uani 1 1 d . . . . .
H61 H 0.103519 0.438770 -0.025446 0.038 Uiso 1 1 calc R U . . .
C56 C 0.6444(6) 0.7999(5) 0.1079(3) 0.0191(14) Uani 1 1 d . . . . .
C70 C 0.3383(7) 0.8549(5) 0.1127(3) 0.0249(18) Uani 1 1 d . . . . .
H70 H 0.292863 0.813972 0.082341 0.030 Uiso 1 1 calc R U . . .
C69 C 0.4055(6) 0.8245(5) 0.1685(3) 0.0159(15) Uani 1 1 d . . . . .
C16 C 0.1347(6) 0.6849(5) 0.1940(4) 0.0230(19) Uani 1 1 d . . . . .
C2 C 0.6439(7) 0.4891(5) 0.1479(4) 0.031(2) Uani 1 1 d . . . . .
C51 C 0.6376(7) 0.8710(5) 0.0657(4) 0.0288(17) Uani 1 1 d . . . . .
C24 C 0.2891(7) 1.0636(5) 0.3455(4) 0.025(2) Uani 1 1 d . . . . .
H24 H 0.298400 1.121832 0.361696 0.030 Uiso 1 1 calc R U . . .
C38 C 0.8958(6) 0.6439(5) 0.5654(3) 0.0252(19) Uani 1 1 d . . . . .
H38A H 0.845167 0.613223 0.591980 0.030 Uiso 1 1 calc R U . . .
H38B H 0.966648 0.607748 0.562717 0.030 Uiso 1 1 calc R U . . .
C33 C 0.6362(7) 0.6997(5) 0.5554(4) 0.031(2) Uani 1 1 d . . . . .
H33 H 0.664897 0.672076 0.593182 0.038 Uiso 1 1 calc R U . . .
C6 C 0.5456(8) 0.3673(5) 0.2749(4) 0.037(2) Uani 1 1 d . . . . .
C35 C 0.8110(7) 0.6496(5) 0.4998(3) 0.0219(19) Uani 1 1 d . . . . .
C50 C 0.6883(7) 0.9568(5) 0.0873(4) 0.0311(18) Uani 1 1 d . . . . .
H50 H 0.683672 1.002722 0.058800 0.037 Uiso 1 1 calc R U . . .
C44 C 0.9313(7) 0.8311(5) 0.3308(3) 0.0204(18) Uani 1 1 d . . . . .
H44 H 1.004001 0.855116 0.317650 0.025 Uiso 1 1 calc R U . . .
C23 C 0.2041(7) 1.0425(5) 0.2915(4) 0.026(2) Uani 1 1 d . . . . .
H23 H 0.155358 1.086608 0.270907 0.031 Uiso 1 1 calc R U . . .
C25 C 0.3649(6) 0.9971(5) 0.3780(4) 0.0235(19) Uani 1 1 d . . . . .
H25 H 0.421248 1.011943 0.415984 0.028 Uiso 1 1 calc R U . . .
C67 C 0.8352(7) 1.0140(6) 0.4988(4) 0.039(2) Uani 1 1 d . . . . .
H67 H 0.884186 1.013727 0.539447 0.047 Uiso 1 1 calc R U . . .
C7 C 0.6265(8) 0.4159(6) 0.3340(4) 0.053(3) Uani 1 1 d D U . . .
H7A H 0.582980 0.405667 0.368386 0.064 Uiso 1 1 calc R U . A 2
H7B H 0.631146 0.479619 0.326808 0.064 Uiso 1 1 calc R U . A 2
C22 C 0.1873(6) 0.9541(5) 0.2652(4) 0.0199(18) Uani 1 1 d . . . . .
C32 C 0.5306(7) 0.7507(5) 0.5406(4) 0.031(2) Uani 1 1 d . . . . .
H32 H 0.474936 0.763958 0.566478 0.037 Uiso 1 1 calc R U . . .
C62 C 0.2227(7) 0.4093(6) 0.0536(4) 0.035(2) Uani 1 1 d . . . . .
H62 H 0.209909 0.347432 0.048675 0.042 Uiso 1 1 calc R U . . .
C48 C 0.7958(7) 1.0633(5) 0.1725(4) 0.0321(18) Uani 1 1 d . . . . .
H48 H 0.789648 1.110497 0.144946 0.038 Uiso 1 1 calc R U . . .
C14 C 0.2375(8) 0.4699(5) 0.2550(4) 0.0252(19) Uani 1 1 d . . . . .
C12 C 0.3034(8) 0.3367(5) 0.2823(3) 0.034(2) Uani 1 1 d . . . . .
H12 H 0.305529 0.277639 0.294775 0.041 Uiso 1 1 calc R U . . .
C73 C 0.4686(6) 0.9752(5) 0.2031(3) 0.0204(17) Uani 1 1 d . . . . .
H73 H 0.512578 1.016438 0.233572 0.025 Uiso 1 1 calc R U . . .
C72 C 0.4017(6) 1.0052(5) 0.1466(3) 0.0235(17) Uani 1 1 d . . . . .
H72 H 0.400333 1.066124 0.139364 0.028 Uiso 1 1 calc R U . . .
C19 C -0.0151(7) 0.8152(5) 0.1308(4) 0.030(2) Uani 1 1 d . . . . .
H19 H -0.063364 0.858257 0.108621 0.036 Uiso 1 1 calc R U . . .
C59 C 0.2626(7) 0.5888(5) 0.0719(4) 0.025(2) Uani 1 1 d . . . . .
H59 H 0.274909 0.650577 0.077795 0.030 Uiso 1 1 calc R U . . .
C52 C 0.5743(7) 0.8532(6) 0.0020(4) 0.040(2) Uani 1 1 d . . . . .
H52 H 0.566787 0.899511 -0.026301 0.048 Uiso 1 1 calc R U . . .
C54 C 0.5325(7) 0.6991(6) 0.0236(4) 0.0344(19) Uani 1 1 d . . . . .
H54 H 0.498201 0.642111 0.009070 0.041 Uiso 1 1 calc R U . . .
C65 C 0.7358(8) 1.0893(5) 0.4102(4) 0.039(2) Uani 1 1 d . . . . .
H65 H 0.715945 1.141969 0.389346 0.046 Uiso 1 1 calc R U . . .
C4 C 0.6664(8) 0.3527(5) 0.1828(4) 0.040(2) Uani 1 1 d . . . . .
H4 H 0.688861 0.294106 0.188226 0.048 Uiso 1 1 calc R U . . .
C63 C 0.3063(7) 0.4485(6) 0.1059(4) 0.036(2) Uani 1 1 d . . . . .
H63 H 0.351261 0.411560 0.135358 0.044 Uiso 1 1 calc R U . . .
C53 C 0.5246(8) 0.7692(6) -0.0179(4) 0.040(2) Uani 1 1 d . . . . .
H53 H 0.484942 0.758590 -0.059771 0.048 Uiso 1 1 calc R U . . .
C60 C 0.1802(7) 0.5543(6) 0.0178(4) 0.033(2) Uani 1 1 d . . . . .
H60 H 0.139369 0.591952 -0.012409 0.039 Uiso 1 1 calc R U . . .
C17 C 0.0410(6) 0.6643(5) 0.1423(4) 0.027(2) Uani 1 1 d . . . . .
H17 H 0.026293 0.605433 0.127193 0.032 Uiso 1 1 calc R U . . .
C18 C -0.0348(7) 0.7302(6) 0.1107(4) 0.030(2) Uani 1 1 d . . . . .
H18 H -0.099126 0.714137 0.075649 0.036 Uiso 1 1 calc R U . . .
C47 C 0.8516(7) 1.0786(5) 0.2328(4) 0.0305(18) Uani 1 1 d . . . . .
H47 H 0.884295 1.136102 0.246664 0.037 Uiso 1 1 calc R U . . .
C10 C 0.4765(10) 0.2076(5) 0.2287(4) 0.069(3) Uani 1 1 d . . . . .
H10A H 0.418057 0.243252 0.201591 0.103 Uiso 1 1 calc R U . . .
H10B H 0.428439 0.159678 0.244413 0.103 Uiso 1 1 calc R U . . .
H10C H 0.534195 0.183274 0.205678 0.103 Uiso 1 1 calc R U . . .
C202 C 1.1192(13) 1.1508(10) 0.1199(9) 0.047(3) Uani 0.58(3) 1 d G U P B 1
H202 H 1.192785 1.128051 0.143401 0.057 Uiso 0.58(3) 1 calc R U P B 1
C201 C 1.0597(12) 1.1111(11) 0.0623(9) 0.051(3) Uani 0.58(3) 1 d G U P B 1
H201 H 1.093454 1.061904 0.047299 0.061 Uiso 0.58(3) 1 calc R U P B 1
C200 C 0.9496(15) 1.1451(12) 0.0271(5) 0.049(3) Uani 0.58(3) 1 d G U P B 1
H200 H 0.909803 1.118540 -0.011394 0.058 Uiso 0.58(3) 1 calc R U P B 1
C205 C 0.8991(13) 1.2186(11) 0.0495(8) 0.043(3) Uani 0.58(3) 1 d G U P B 1
H205 H 0.825481 1.241324 0.026016 0.052 Uiso 0.58(3) 1 calc R U P B 1
C204 C 0.9586(14) 1.2583(9) 0.1071(8) 0.043(3) Uani 0.58(3) 1 d G U P B 1
H204 H 0.924810 1.307471 0.122119 0.052 Uiso 0.58(3) 1 calc R U P B 1
C203 C 1.0686(16) 1.2243(10) 0.1423(5) 0.048(3) Uani 0.58(3) 1 d G U P B 1
H203 H 1.108461 1.250836 0.180812 0.058 Uiso 0.58(3) 1 calc R U P B 1
C37 C 0.6933(8) 0.4925(5) 0.5101(4) 0.044(2) Uani 1 1 d . . . . .
H37A H 0.749699 0.477565 0.548435 0.066 Uiso 1 1 calc R U . . .
H37B H 0.660262 0.438807 0.486070 0.066 Uiso 1 1 calc R U . . .
H37C H 0.622981 0.522873 0.519509 0.066 Uiso 1 1 calc R U . . .
C66 C 0.8121(8) 1.0929(6) 0.4689(5) 0.042(3) Uani 1 1 d . . . . .
H66 H 0.847302 1.147303 0.488138 0.050 Uiso 1 1 calc R U . . .
C9 C 0.5540(10) 0.2656(5) 0.2834(4) 0.059(3) Uani 1 1 d . . . . .
H9A H 0.643795 0.252606 0.289718 0.071 Uiso 1 1 calc R U . . .
H9B H 0.524068 0.249108 0.320968 0.071 Uiso 1 1 calc R U . . .
C8 C 0.7655(14) 0.386(2) 0.3535(12) 0.059(4) Uani 0.58(4) 1 d D U P C 2
H8A H 0.762106 0.324099 0.364467 0.088 Uiso 0.58(4) 1 calc R U P C 2
H8B H 0.812044 0.421538 0.388920 0.088 Uiso 0.58(4) 1 calc R U P C 2
H8C H 0.808409 0.393568 0.319216 0.088 Uiso 0.58(4) 1 calc R U P C 2
C76 C 0.7928(10) 0.6336(7) 0.2727(5) 0.036(4) Uani 0.687(15) 1 d . . P . .
H76A H 0.777557 0.580918 0.246106 0.055 Uiso 0.687(15) 1 calc R U P . .
H76B H 0.839016 0.619242 0.313642 0.055 Uiso 0.687(15) 1 calc R U P . .
H76C H 0.842883 0.678560 0.255286 0.055 Uiso 0.687(15) 1 calc R U P . .
C8A C 0.7740(10) 0.422(3) 0.3376(16) 0.059(4) Uani 0.42(4) 1 d D U P C 3
H8AA H 0.802172 0.363570 0.334099 0.088 Uiso 0.42(4) 1 calc R U P C 3
H8AB H 0.817814 0.449819 0.376934 0.088 Uiso 0.42(4) 1 calc R U P C 3
H8AC H 0.793275 0.457956 0.303962 0.088 Uiso 0.42(4) 1 calc R U P C 3
C102 C 1.1371(14) 1.1667(15) 0.0973(13) 0.051(3) Uani 0.42(3) 1 d G U P B 2
H102 H 1.218803 1.145426 0.107308 0.061 Uiso 0.42(3) 1 calc R U P B 2
C101 C 1.0525(18) 1.1387(17) 0.0418(11) 0.050(3) Uani 0.42(3) 1 d G U P B 2
H101 H 1.077655 1.098788 0.014620 0.060 Uiso 0.42(3) 1 calc R U P B 2
C100 C 0.9305(18) 1.1704(17) 0.0268(7) 0.049(3) Uani 0.42(3) 1 d G U P B 2
H100 H 0.873873 1.151748 -0.010345 0.059 Uiso 0.42(3) 1 calc R U P B 2
C105 C 0.8929(15) 1.2301(15) 0.0674(12) 0.044(3) Uani 0.42(3) 1 d G U P B 2
H105 H 0.811236 1.251347 0.057378 0.052 Uiso 0.42(3) 1 calc R U P B 2
C104 C 0.977(2) 1.2581(15) 0.1229(10) 0.045(3) Uani 0.42(3) 1 d G U P B 2
H104 H 0.952381 1.297987 0.150066 0.054 Uiso 0.42(3) 1 calc R U P B 2
C103 C 1.100(2) 1.2263(14) 0.1379(7) 0.047(3) Uani 0.42(3) 1 d G U P B 2
H103 H 1.156165 1.245028 0.175031 0.057 Uiso 0.42(3) 1 calc R U P B 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 O1 2.112(4) . ?
U1 O4 2.345(4) . ?
U1 O3 2.358(5) . ?
U1 N3 2.466(6) . ?
U1 N2 2.480(5) . ?
U1 N9 2.633(6) . ?
U1 N4 2.646(5) . ?
U1 N1 2.656(6) . ?
U1 U2 3.7763(5) . ?
U2 O2 2.113(4) . ?
U2 O3 2.347(4) . ?
U2 O4 2.379(4) . ?
U2 N6 2.476(5) . ?
U2 N7 2.478(6) . ?
U2 N5 2.589(6) . ?
U2 N8 2.614(5) . ?
U2 N10 2.630(6) . ?
O1 C69 1.362(7) . ?
O4 C76 1.472(11) . ?
O2 C74 1.368(7) . ?
O3 C75 1.429(9) . ?
C28 C27 1.377(9) . ?
C28 C29 1.400(9) . ?
N10 C68 1.324(9) . ?
N10 C64 1.334(9) . ?
N7 C34 1.344(8) . ?
N7 C31 1.396(8) . ?
N6 C40 1.357(8) . ?
N6 C43 1.393(8) . ?
C45 C46 1.357(9) . ?
C45 N5 1.428(8) . ?
C45 C58 1.438(9) . ?
C43 C42 1.395(9) . ?
C43 C44 1.400(9) . ?
N8 C30 1.299(8) . ?
N8 C26 1.423(8) . ?
N2 C5 1.363(9) . ?
N2 C2 1.374(9) . ?
C64 C65 1.360(10) . ?
C34 C33 1.381(9) . ?
C34 C35 1.529(9) . ?
C27 C26 1.438(9) . ?
C27 C22 1.439(9) . ?
C26 C25 1.358(9) . ?
N3 C11 1.371(8) . ?
N3 C14 1.389(9) . ?
N9 C59 1.335(8) . ?
N9 C63 1.341(9) . ?
C31 C32 1.390(10) . ?
C31 C30 1.405(9) . ?
N1 C1 1.314(8) . ?
N1 C55 1.437(9) . ?
N5 C44 1.305(8) . ?
C42 C41 1.369(10) . ?
N4 C15 1.298(8) . ?
N4 C16 1.434(8) . ?
C74 C73 1.381(9) . ?
C74 C69 1.388(9) . ?
C68 C67 1.394(10) . ?
C58 C57 1.397(9) . ?
C58 C49 1.437(9) . ?
C1 C2 1.409(10) . ?
C49 C50 1.392(10) . ?
C49 C48 1.419(10) . ?
C40 C41 1.410(9) . ?
C40 C35 1.532(10) . ?
C20 C21 1.395(9) . ?
C20 C29 1.423(9) . ?
C20 C19 1.435(9) . ?
C21 C22 1.387(9) . ?
C11 C12 1.388(10) . ?
C11 C6 1.518(10) . ?
C15 C14 1.409(9) . ?
C57 C56 1.410(9) . ?
C36 C37 1.518(10) . ?
C36 C35 1.560(9) . ?
C55 C54 1.375(10) . ?
C55 C56 1.427(10) . ?
C5 C4 1.412(10) . ?
C5 C6 1.498(11) . ?
C39 C38 1.528(9) . ?
C3 C2 1.384(9) . ?
C3 C4 1.388(11) . ?
C13 C12 1.375(10) . ?
C13 C14 1.388(10) . ?
C29 C16 1.428(9) . ?
C46 C47 1.422(10) . ?
C71 C70 1.367(9) . ?
C71 C72 1.374(9) . ?
C61 C62 1.355(10) . ?
C61 C60 1.367(10) . ?
C56 C51 1.413(10) . ?
C70 C69 1.375(9) . ?
C16 C17 1.357(9) . ?
C51 C50 1.396(10) . ?
C51 C52 1.427(10) . ?
C24 C23 1.345(9) . ?
C24 C25 1.427(9) . ?
C38 C35 1.531(9) . ?
C33 C32 1.388(9) . ?
C6 C7 1.537(10) . ?
C6 C9 1.544(10) . ?
C23 C22 1.425(9) . ?
C67 C66 1.370(11) . ?
C7 C8 1.550(10) . ?
C7 C8A 1.550(10) . ?
C62 C63 1.387(10) . ?
C48 C47 1.337(10) . ?
C73 C72 1.384(9) . ?
C19 C18 1.331(10) . ?
C59 C60 1.385(9) . ?
C52 C53 1.361(11) . ?
C54 C53 1.392(10) . ?
C65 C66 1.365(11) . ?
C17 C18 1.412(9) . ?
C10 C9 1.525(11) . ?
C202 C201 1.3900 . ?
C202 C203 1.3900 . ?
C201 C200 1.3900 . ?
C200 C205 1.3900 . ?
C205 C204 1.3900 . ?
C204 C203 1.3900 . ?
C102 C101 1.3900 . ?
C102 C103 1.3900 . ?
C101 C100 1.3900 . ?
C100 C105 1.3900 . ?
C105 C104 1.3900 . ?
C104 C103 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
O1 U1 O4 96.40(16) . . ?
O1 U1 O3 95.55(16) . . ?
O4 U1 O3 64.11(15) . . ?
O1 U1 N3 140.23(17) . . ?
O4 U1 N3 117.45(17) . . ?
O3 U1 N3 82.42(17) . . ?
O1 U1 N2 138.8(2) . . ?
O4 U1 N2 83.65(17) . . ?
O3 U1 N2 120.45(18) . . ?
N3 U1 N2 69.6(2) . . ?
O1 U1 N9 85.89(18) . . ?
O4 U1 N9 148.91(16) . . ?
O3 U1 N9 146.74(16) . . ?
N3 U1 N9 75.75(19) . . ?
N2 U1 N9 74.79(18) . . ?
O1 U1 N4 74.42(17) . . ?
O4 U1 N4 139.40(15) . . ?
O3 U1 N4 77.30(16) . . ?
N3 U1 N4 66.36(18) . . ?
N2 U1 N4 129.23(18) . . ?
N9 U1 N4 71.10(17) . . ?
O1 U1 N1 73.22(17) . . ?
O4 U1 N1 78.92(16) . . ?
O3 U1 N1 140.09(16) . . ?
N3 U1 N1 130.53(18) . . ?
N2 U1 N1 66.36(19) . . ?
N9 U1 N1 72.06(18) . . ?
N4 U1 N1 131.95(17) . . ?
O1 U1 U2 77.74(12) . . ?
O4 U1 U2 37.24(10) . . ?
O3 U1 U2 36.53(11) . . ?
N3 U1 U2 116.48(13) . . ?
N2 U1 U2 118.83(13) . . ?
N9 U1 U2 163.58(13) . . ?
N4 U1 U2 102.80(12) . . ?
N1 U1 U2 103.88(12) . . ?
O2 U2 O3 92.64(17) . . ?
O2 U2 O4 90.85(16) . . ?
O3 U2 O4 63.75(15) . . ?
O2 U2 N6 143.39(18) . . ?
O3 U2 N6 115.92(17) . . ?
O4 U2 N6 82.77(16) . . ?
O2 U2 N7 142.51(16) . . ?
O3 U2 N7 83.10(17) . . ?
O4 U2 N7 119.46(16) . . ?
N6 U2 N7 67.69(18) . . ?
O2 U2 N5 76.21(17) . . ?
O3 U2 N5 139.03(16) . . ?
O4 U2 N5 76.94(16) . . ?
N6 U2 N5 67.23(18) . . ?
N7 U2 N5 128.84(17) . . ?
O2 U2 N8 74.97(17) . . ?
O3 U2 N8 79.83(16) . . ?
O4 U2 N8 140.35(16) . . ?
N6 U2 N8 129.76(18) . . ?
N7 U2 N8 67.60(17) . . ?
N5 U2 N8 131.99(17) . . ?
O2 U2 N10 89.76(18) . . ?
O3 U2 N10 148.32(16) . . ?
O4 U2 N10 147.84(16) . . ?
N6 U2 N10 77.77(17) . . ?
N7 U2 N10 76.04(18) . . ?
N5 U2 N10 72.01(17) . . ?
N8 U2 N10 70.32(17) . . ?
O2 U2 U1 72.90(13) . . ?
O3 U2 U1 36.72(11) . . ?
O4 U2 U1 36.61(10) . . ?
N6 U2 U1 116.35(12) . . ?
N7 U2 U1 117.71(12) . . ?
N5 U2 U1 103.16(12) . . ?
N8 U2 U1 103.95(12) . . ?
N10 U2 U1 162.66(13) . . ?
C69 O1 U1 162.4(4) . . ?
C76 O4 U1 125.6(5) . . ?
C76 O4 U2 128.2(5) . . ?
U1 O4 U2 106.15(16) . . ?
C74 O2 U2 168.6(4) . . ?
C75 O3 U2 126.7(4) . . ?
C75 O3 U1 126.5(4) . . ?
U2 O3 U1 106.76(18) . . ?
C27 C28 C29 122.6(6) . . ?
C68 N10 C64 117.4(7) . . ?
C68 N10 U2 122.8(5) . . ?
C64 N10 U2 119.6(5) . . ?
C34 N7 C31 105.9(6) . . ?
C34 N7 U2 138.9(4) . . ?
C31 N7 U2 115.3(4) . . ?
C40 N6 C43 105.8(5) . . ?
C40 N6 U2 137.7(5) . . ?
C43 N6 U2 115.2(4) . . ?
C46 C45 N5 121.0(7) . . ?
C46 C45 C58 119.5(7) . . ?
N5 C45 C58 119.5(6) . . ?
N6 C43 C42 110.1(6) . . ?
N6 C43 C44 120.1(6) . . ?
C42 C43 C44 129.7(7) . . ?
C30 N8 C26 117.8(6) . . ?
C30 N8 U2 113.0(4) . . ?
C26 N8 U2 127.9(4) . . ?
C5 N2 C2 106.2(6) . . ?
C5 N2 U1 135.8(5) . . ?
C2 N2 U1 117.7(5) . . ?
N10 C64 C65 122.9(8) . . ?
N7 C34 C33 111.1(6) . . ?
N7 C34 C35 124.4(6) . . ?
C33 C34 C35 124.5(6) . . ?
C28 C27 C26 122.5(6) . . ?
C28 C27 C22 119.5(6) . . ?
C26 C27 C22 118.0(6) . . ?
C25 C26 N8 120.4(6) . . ?
C25 C26 C27 120.5(6) . . ?
N8 C26 C27 119.0(6) . . ?
C11 N3 C14 106.1(6) . . ?
C11 N3 U1 136.3(5) . . ?
C14 N3 U1 117.4(4) . . ?
C59 N9 C63 117.3(7) . . ?
C59 N9 U1 119.1(5) . . ?
C63 N9 U1 123.5(5) . . ?
C32 C31 N7 109.5(6) . . ?
C32 C31 C30 129.5(7) . . ?
N7 C31 C30 121.0(7) . . ?
C1 N1 C55 116.1(6) . . ?
C1 N1 U1 112.3(5) . . ?
C55 N1 U1 129.6(4) . . ?
C44 N5 C45 117.4(6) . . ?
C44 N5 U2 113.8(5) . . ?
C45 N5 U2 128.1(4) . . ?
N8 C30 C31 123.0(7) . . ?
C41 C42 C43 106.5(7) . . ?
C15 N4 C16 117.3(6) . . ?
C15 N4 U1 113.7(4) . . ?
C16 N4 U1 126.8(4) . . ?
O2 C74 C73 122.0(6) . . ?
O2 C74 C69 119.4(6) . . ?
C73 C74 C69 118.6(7) . . ?
N10 C68 C67 122.8(8) . . ?
C57 C58 C49 119.0(7) . . ?
C57 C58 C45 122.3(7) . . ?
C49 C58 C45 118.6(7) . . ?
N1 C1 C2 122.9(7) . . ?
C50 C49 C48 123.0(7) . . ?
C50 C49 C58 118.1(7) . . ?
C48 C49 C58 118.8(7) . . ?
N6 C40 C41 109.8(6) . . ?
N6 C40 C35 124.4(6) . . ?
C41 C40 C35 125.8(6) . . ?
C21 C20 C29 118.8(7) . . ?
C21 C20 C19 122.3(7) . . ?
C29 C20 C19 118.8(7) . . ?
C22 C21 C20 123.2(7) . . ?
N3 C11 C12 109.1(7) . . ?
N3 C11 C6 122.0(7) . . ?
C12 C11 C6 129.0(7) . . ?
N4 C15 C14 121.8(7) . . ?
C42 C41 C40 107.7(6) . . ?
C58 C57 C56 122.4(7) . . ?
C37 C36 C35 116.8(6) . . ?
C54 C55 C56 119.5(7) . . ?
C54 C55 N1 120.7(7) . . ?
C56 C55 N1 119.8(7) . . ?
N2 C5 C4 108.7(8) . . ?
N2 C5 C6 122.6(7) . . ?
C4 C5 C6 128.6(7) . . ?
C2 C3 C4 105.1(8) . . ?
C12 C13 C14 106.2(8) . . ?
C28 C29 C20 118.3(6) . . ?
C28 C29 C16 123.1(6) . . ?
C20 C29 C16 118.6(7) . . ?
C45 C46 C47 121.2(8) . . ?
C70 C71 C72 119.9(7) . . ?
C62 C61 C60 120.2(7) . . ?
C57 C56 C51 118.0(7) . . ?
C57 C56 C55 122.3(7) . . ?
C51 C56 C55 119.7(7) . . ?
C71 C70 C69 120.9(7) . . ?
O1 C69 C70 121.5(6) . . ?
O1 C69 C74 118.4(6) . . ?
C70 C69 C74 120.0(7) . . ?
C17 C16 C29 119.7(7) . . ?
C17 C16 N4 120.8(7) . . ?
C29 C16 N4 119.5(6) . . ?
N2 C2 C3 111.7(8) . . ?
N2 C2 C1 120.2(7) . . ?
C3 C2 C1 128.1(8) . . ?
C50 C51 C56 119.9(7) . . ?
C50 C51 C52 121.7(8) . . ?
C56 C51 C52 118.3(8) . . ?
C23 C24 C25 120.4(7) . . ?
C39 C38 C35 115.0(6) . . ?
C34 C33 C32 107.1(7) . . ?
C5 C6 C11 111.7(6) . . ?
C5 C6 C7 108.5(8) . . ?
C11 C6 C7 106.6(6) . . ?
C5 C6 C9 112.0(7) . . ?
C11 C6 C9 109.4(8) . . ?
C7 C6 C9 108.4(7) . . ?
C34 C35 C38 109.8(6) . . ?
C34 C35 C40 113.8(6) . . ?
C38 C35 C40 109.5(6) . . ?
C34 C35 C36 108.6(6) . . ?
C38 C35 C36 109.0(6) . . ?
C40 C35 C36 106.1(6) . . ?
C49 C50 C51 122.5(7) . . ?
N5 C44 C43 122.3(7) . . ?
C24 C23 C22 121.4(7) . . ?
C26 C25 C24 120.7(7) . . ?
C66 C67 C68 118.7(8) . . ?
C6 C7 C8 114.0(9) . . ?
C6 C7 C8A 114.6(12) . . ?
C21 C22 C23 123.7(7) . . ?
C21 C22 C27 117.6(6) . . ?
C23 C22 C27 118.7(7) . . ?
C33 C32 C31 106.3(7) . . ?
C61 C62 C63 118.3(8) . . ?
C47 C48 C49 120.9(8) . . ?
C13 C14 N3 110.0(7) . . ?
C13 C14 C15 129.4(8) . . ?
N3 C14 C15 120.5(7) . . ?
C13 C12 C11 108.6(7) . . ?
C74 C73 C72 121.0(7) . . ?
C71 C72 C73 119.5(7) . . ?
C18 C19 C20 120.7(7) . . ?
N9 C59 C60 122.8(7) . . ?
C53 C52 C51 120.7(8) . . ?
C55 C54 C53 121.0(8) . . ?
C64 C65 C66 120.2(8) . . ?
C3 C4 C5 108.2(7) . . ?
N9 C63 C62 123.0(8) . . ?
C52 C53 C54 120.9(8) . . ?
C61 C60 C59 118.4(8) . . ?
C16 C17 C18 121.5(7) . . ?
C19 C18 C17 120.6(7) . . ?
C48 C47 C46 120.8(8) . . ?
C201 C202 C203 120.0 . . ?
C202 C201 C200 120.0 . . ?
C205 C200 C201 120.0 . . ?
C204 C205 C200 120.0 . . ?
C205 C204 C203 120.0 . . ?
C204 C203 C202 120.0 . . ?
C65 C66 C67 118.0(8) . . ?
C10 C9 C6 114.8(7) . . ?
C101 C102 C103 120.0 . . ?
C102 C101 C100 120.0 . . ?
C105 C100 C101 120.0 . . ?
C100 C105 C104 120.0 . . ?
C105 C104 C103 120.0 . . ?
C104 C103 C102 120.0 . . ?

_refine_diff_density_max         1.601
_refine_diff_density_min         -0.942
_refine_diff_density_rms         0.167


# start Validation Reply Form
_vrf_PLAT973_compound2           
;
PROBLEM: Check Calcd Positive Resid. Density on        U2       2.27 eA-3  
RESPONSE: This is attributed to the scattering power of a heavy metal such
as uranium. The data was analysed for twinning, however there didn't 
appear to be any.
;
_vrf_PLAT910_compound2           
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         20 Note  
RESPONSE: This has been noted, but is not serious. The independent 
reflections/parameters ratio is equal to 13.3, indicating that there are 
no issues with the data collected.
;
# end Validation Reply Form
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Benzene/hexanes'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_compound3
_database_code_depnum_ccdc_archive 'CCDC 1984902'
loop_
_audit_author_name
_audit_author_address
'Bradley E. Cowie'
;The University of Edinburgh
United Kingdom
;
_audit_update_record             
;
2020-02-18 deposited with the CCDC.	2020-06-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        '[{(py)U(S2)U(O2C6H4)(py)}(LA)]'
_chemical_name_common            'Compound 3.5py'
_chemical_melting_point          ?
_chemical_formula_moiety         'C74 H63 N10 O2 S2 U2, 5(C5 H5 N)'
_chemical_formula_sum            'C99 H88 N15 O2 S2 U2'
_chemical_formula_weight         2060.02

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   13.7332(2)
_cell_length_b                   17.5327(3)
_cell_length_c                   18.0598(3)
_cell_angle_alpha                77.6190(10)
_cell_angle_beta                 85.4690(10)
_cell_angle_gamma                88.9250(10)
_cell_volume                     4234.03(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(1)
_cell_measurement_reflns_used    43178
_cell_measurement_theta_min      3.2090
_cell_measurement_theta_max      27.7370

_exptl_crystal_description       block
_exptl_crystal_colour            'translucent orange'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.616
_exptl_crystal_F_000             2038
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.266
_exptl_crystal_size_mid          0.101
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    3.922
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.88725
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.54a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      120(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_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            142230
_diffrn_reflns_av_unetI/netI     0.1665
_diffrn_reflns_av_R_equivalents  0.0937
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.808
_diffrn_reflns_theta_max         29.395
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.923
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.923
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.923
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             58720
_reflns_number_gt                33537
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -35.00  54.00   1.00   25.00    --  -15.66  37.00-180.00   89
  2  ω    -42.00  52.00   1.00   25.00    --  -15.66  77.00 -30.00   94
  3  ω    -35.00  54.00   1.00   25.00    --  -15.66  37.00 -90.00   89
  4  ω    -83.00  11.00   1.00   25.00    --  -15.66 -77.00-150.00   94
  5  ω    -60.00  16.00   1.00   25.00    --  -15.66 109.00 -54.10   76
  6  ω      1.00  85.00   1.00   25.00    --   17.38  57.00  90.00   84
  7  ω     34.00  90.00   1.00   25.00    --   17.38 179.00   0.00   56
  8  ω     -9.00  85.00   1.00   25.00    --   17.38  77.00 120.00   94
  9  ω    -88.00 -34.00   1.00   25.00    --  -15.66-179.00 -30.00   54
 10  ω    -25.00  23.00   1.00   25.00    --  -15.66 -99.00 -30.00   48
 11  ω     -2.00  87.00   1.00   25.00    --   17.38  37.00 -30.00   89
 12  ω      3.00  77.00   1.00   25.00    --   17.38-135.00 134.17   74
 13  ω    -25.00  56.00   1.00   25.00    --   17.38 -99.00 -60.00   81
 14  ω    -25.00  56.00   1.00   25.00    --   17.38 -99.00-180.00   81
 15  ω    -69.00   4.00   1.00   25.00    --  -15.66 124.00 132.87   73
 16  ω    -64.00  11.00   1.00   25.00    --  -15.66 115.00 177.32   75
 17  ω    -65.00  10.00   1.00   25.00    --  -15.66 117.00 -26.25   75
 18  ω    -16.00  62.00   1.00   25.00    --   17.38-109.00  -2.05   78
 19  ω     34.00  90.00   1.00   25.00    --   17.38 179.00-180.00   56
 20  ω      1.00  85.00   1.00   25.00    --   17.38  57.00  30.00   84
 21  ω    -25.00  23.00   1.00   25.00    --  -15.66 -99.00-120.00   48
 22  ω    -68.00   5.00   1.00   25.00    --  -15.66 123.00  90.84   73
 23  ω    -52.00  87.00   1.00   25.00    --   17.38   0.00-180.00  139
 24  ω    -52.00  24.00   1.00   25.00    --   17.38   0.00-150.00   76
 25  ω     -2.00  87.00   1.00   25.00    --   17.38  37.00-120.00   89
;
_oxdiff_twin_items               2
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
_oxdiff_twin_reflns_isolated
_oxdiff_twin_reflns_overlapped
_twin_individual_twin_lattice_type
_twin_individual_twin_matrix_11
_twin_individual_twin_matrix_12
_twin_individual_twin_matrix_13
_twin_individual_twin_matrix_21
_twin_individual_twin_matrix_22
_twin_individual_twin_matrix_23
_twin_individual_twin_matrix_31
_twin_individual_twin_matrix_32
_twin_individual_twin_matrix_33
1 0.7098 38249 147316 ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000
0.0000 1.0000
2 0.2902 38340 147316 nmt -1.0003 -0.0001 0.0007 -0.1223 0.0328 0.9670 -0.1251
1.0340 -0.0334
_oxdiff_twin_integration_method  simultaneous
_twin_special_details            
;
Component 2 rotated by 179.9034° 
 around [0.00 0.71 0.71] (reciprocal) or [-0.09 0.73 0.68] (direct)
;

_reflns_special_details          
;
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       'CrysAlisPro 1.171.40.54a (Rigaku OD, 2019)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.54a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.54a (Rigaku OD, 2019)'
_computing_structure_solution    'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_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.

Refined as a 2-component twin with component 1 being equal to 78% 
(BASF = 0.2209(2)) using SADABS.

The thermal ellipsoids of the carbon atoms of one of the U-coordinated 
pyridine ligands (N10, C70, C71, C72, C73, C74) were restrained using the 
RIGU command. Furthermore, two of the lattice pyridine molecules (C886, C887,
C888/N888 and C997, C998, C999/N999) reside on special positions. Therefore,
one carbon atom per pyridine molecule (C888 and C999) was assigned as both a
carbon atom and a nitrogen atom with 50% occupancy. The positional and 
thermal parameters of the N/C refined atoms were fixed using the EXYZ and 
EADP commands, respectively.,Twin
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0121P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         58720
_refine_ls_number_parameters     1086
_refine_ls_number_restraints     21
_refine_ls_R_factor_all          0.0861
_refine_ls_R_factor_gt           0.0385
_refine_ls_wR_factor_ref         0.0511
_refine_ls_wR_factor_gt          0.0481
_refine_ls_goodness_of_fit_ref   0.765
_refine_ls_restrained_S_all      0.765
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.10646(2) 0.26746(2) 0.18438(2) 0.01216(6) Uani 1 1 d . . . . .
U2 U 0.38847(2) 0.17802(2) 0.27007(2) 0.01208(6) Uani 1 1 d . . . . .
S1 S 0.28893(8) 0.21408(7) 0.13866(7) 0.0151(3) Uani 1 1 d . . . . .
S2 S 0.21444(9) 0.13038(7) 0.22473(7) 0.0156(3) Uani 1 1 d . . . . .
O1 O 0.1531(2) 0.32470(18) 0.26594(18) 0.0153(8) Uani 1 1 d . . . . .
O2 O 0.3238(2) 0.26479(18) 0.32288(18) 0.0167(8) Uani 1 1 d . . . . .
N1 N 0.1677(3) 0.3989(2) 0.1025(2) 0.0130(10) Uani 1 1 d . . . . .
N2 N 0.0920(2) 0.2761(2) 0.0467(2) 0.0112(9) Uani 1 1 d . . . . .
N3 N -0.0094(3) 0.1704(2) 0.1619(2) 0.0135(10) Uani 1 1 d . . . . .
N4 N -0.0039(3) 0.2106(2) 0.3050(2) 0.0145(10) Uani 1 1 d . . . . .
N5 N 0.4930(3) 0.2991(2) 0.2113(2) 0.0136(10) Uani 1 1 d . . . . .
N6 N 0.5179(2) 0.1504(2) 0.1763(2) 0.0112(9) Uani 1 1 d . . . . .
N7 N 0.4173(2) 0.0365(2) 0.2810(2) 0.0113(9) Uani 1 1 d . . . . .
N8 N 0.3230(3) 0.0980(2) 0.3995(2) 0.0124(10) Uani 1 1 d . . . . .
N9 N -0.0476(3) 0.3525(2) 0.1665(2) 0.0188(11) Uani 1 1 d . . . . .
N10 N 0.5352(3) 0.1624(2) 0.3522(2) 0.0174(11) Uani 1 1 d . . . . .
C1 C 0.1574(3) 0.4066(3) 0.0311(3) 0.0156(13) Uani 1 1 d . . . . .
H1 H 0.173220 0.454302 -0.001206 0.019 Uiso 1 1 calc R U . . .
C2 C 0.1232(3) 0.3463(3) -0.0007(3) 0.0151(12) Uani 1 1 d . . . . .
C3 C 0.1135(3) 0.3437(3) -0.0760(3) 0.0201(14) Uani 1 1 d . . . . .
H3 H 0.129621 0.383123 -0.118368 0.024 Uiso 1 1 calc R U . . .
C4 C 0.0753(3) 0.2710(3) -0.0760(3) 0.0190(13) Uani 1 1 d . . . . .
H4 H 0.061101 0.252277 -0.118309 0.023 Uiso 1 1 calc R U . . .
C5 C 0.0624(3) 0.2316(3) -0.0003(3) 0.0116(12) Uani 1 1 d . . . . .
C6 C 0.0270(3) 0.1482(3) 0.0289(3) 0.0117(12) Uani 1 1 d . . . . .
C7 C 0.1183(3) 0.0935(3) 0.0414(3) 0.0191(14) Uani 1 1 d . . . . .
H7A H 0.155477 0.108960 0.079225 0.023 Uiso 1 1 calc R U . . .
H7B H 0.095731 0.040523 0.062022 0.023 Uiso 1 1 calc R U . . .
C8 C 0.1863(3) 0.0933(3) -0.0291(3) 0.0250(14) Uani 1 1 d . . . . .
H8A H 0.153816 0.069801 -0.063760 0.038 Uiso 1 1 calc R U . . .
H8B H 0.244119 0.063912 -0.014862 0.038 Uiso 1 1 calc R U . . .
H8C H 0.203958 0.145971 -0.053246 0.038 Uiso 1 1 calc R U . . .
C9 C -0.0324(3) 0.1230(3) -0.0305(3) 0.0183(13) Uani 1 1 d . . . . .
H9A H 0.008969 0.128106 -0.077345 0.022 Uiso 1 1 calc R U . . .
H9B H -0.048070 0.068059 -0.012778 0.022 Uiso 1 1 calc R U . . .
C10 C -0.1273(3) 0.1674(3) -0.0487(3) 0.0255(15) Uani 1 1 d . . . . .
H10A H -0.170361 0.161409 -0.003341 0.038 Uiso 1 1 calc R U . . .
H10B H -0.157932 0.146980 -0.086288 0.038 Uiso 1 1 calc R U . . .
H10C H -0.113090 0.221786 -0.067961 0.038 Uiso 1 1 calc R U . . .
C11 C -0.0318(3) 0.1364(3) 0.1050(3) 0.0137(12) Uani 1 1 d . . . . .
C12 C -0.1092(3) 0.0841(3) 0.1307(3) 0.0219(14) Uani 1 1 d . . . . .
H12 H -0.137210 0.052944 0.102442 0.026 Uiso 1 1 calc R U . . .
C13 C -0.1366(3) 0.0869(3) 0.2050(3) 0.0222(14) Uani 1 1 d . . . . .
H13 H -0.186696 0.058892 0.236261 0.027 Uiso 1 1 calc R U . . .
C14 C -0.0741(3) 0.1399(3) 0.2239(3) 0.0160(13) Uani 1 1 d . . . . .
C15 C -0.0704(3) 0.1636(3) 0.2927(3) 0.0169(14) Uani 1 1 d . . . . .
H15 H -0.117752 0.144918 0.331781 0.020 Uiso 1 1 calc R U . . .
C16 C -0.0185(4) 0.2367(3) 0.3745(3) 0.0170(14) Uani 1 1 d . . . . .
C17 C -0.1025(3) 0.2775(3) 0.3875(3) 0.0212(15) Uani 1 1 d . . . . .
H17 H -0.147919 0.286992 0.351021 0.025 Uiso 1 1 calc R U . . .
C18 C -0.1208(4) 0.3052(3) 0.4550(3) 0.0234(14) Uani 1 1 d . . . . .
H18 H -0.177324 0.333620 0.462160 0.028 Uiso 1 1 calc R U . . .
C19 C -0.0566(4) 0.2908(3) 0.5096(3) 0.0244(14) Uani 1 1 d . . . . .
H19 H -0.069930 0.308641 0.554208 0.029 Uiso 1 1 calc R U . . .
C20 C 0.0312(4) 0.2485(3) 0.4992(3) 0.0179(14) Uani 1 1 d . . . . .
C21 C 0.0981(4) 0.2329(3) 0.5544(3) 0.0210(14) Uani 1 1 d . . . . .
H21 H 0.084382 0.250341 0.599298 0.025 Uiso 1 1 calc R U . . .
C22 C 0.1852(4) 0.1923(3) 0.5453(3) 0.0190(14) Uani 1 1 d . . . . .
C23 C 0.2519(4) 0.1773(3) 0.6028(3) 0.0240(15) Uani 1 1 d . . . . .
H23 H 0.237697 0.193888 0.648022 0.029 Uiso 1 1 calc R U . . .
C24 C 0.3369(4) 0.1385(3) 0.5915(3) 0.0242(15) Uani 1 1 d . . . . .
H24 H 0.380920 0.129242 0.629080 0.029 Uiso 1 1 calc R U . . .
C25 C 0.3585(4) 0.1126(3) 0.5244(3) 0.0195(15) Uani 1 1 d . . . . .
H25 H 0.416789 0.086021 0.518207 0.023 Uiso 1 1 calc R U . . .
C26 C 0.2966(4) 0.1251(3) 0.4675(3) 0.0142(13) Uani 1 1 d . . . . .
C27 C 0.2057(3) 0.1653(3) 0.4765(3) 0.0123(13) Uani 1 1 d . . . . .
C28 C 0.1375(3) 0.1785(3) 0.4220(3) 0.0154(13) Uani 1 1 d . . . . .
H28 H 0.149471 0.158484 0.378487 0.018 Uiso 1 1 calc R U . . .
C29 C 0.0515(4) 0.2210(3) 0.4307(3) 0.0148(13) Uani 1 1 d . . . . .
C30 C 0.3398(3) 0.0227(3) 0.4079(3) 0.0193(14) Uani 1 1 d . . . . .
H30 H 0.322976 -0.009683 0.454947 0.023 Uiso 1 1 calc R U . . .
C31 C 0.3818(3) -0.0108(3) 0.3496(3) 0.0147(12) Uani 1 1 d . . . . .
C32 C 0.3976(3) -0.0892(3) 0.3485(3) 0.0197(14) Uani 1 1 d . . . . .
H32 H 0.380872 -0.131903 0.387538 0.024 Uiso 1 1 calc R U . . .
C33 C 0.4428(3) -0.0906(3) 0.2782(3) 0.0188(13) Uani 1 1 d . . . . .
H33 H 0.461903 -0.135147 0.260635 0.023 Uiso 1 1 calc R U . . .
C34 C 0.4550(3) -0.0137(3) 0.2378(3) 0.0129(12) Uani 1 1 d . . . . .
C35 C 0.4982(3) 0.0125(3) 0.1571(3) 0.0120(12) Uani 1 1 d . . . . .
C36 C 0.4146(3) 0.0250(3) 0.1020(3) 0.0148(13) Uani 1 1 d . . . . .
H36A H 0.369843 0.063964 0.115915 0.018 Uiso 1 1 calc R U . . .
H36B H 0.442857 0.045826 0.050872 0.018 Uiso 1 1 calc R U . . .
C37 C 0.3565(3) -0.0483(3) 0.1014(3) 0.0242(14) Uani 1 1 d . . . . .
H37A H 0.395941 -0.082189 0.076024 0.036 Uiso 1 1 calc R U . . .
H37B H 0.298706 -0.033817 0.075073 0.036 Uiso 1 1 calc R U . . .
H37C H 0.338445 -0.074956 0.152735 0.036 Uiso 1 1 calc R U . . .
C38 C 0.5704(3) -0.0501(3) 0.1372(3) 0.0168(13) Uani 1 1 d . . . . .
H38A H 0.534739 -0.098405 0.142217 0.020 Uiso 1 1 calc R U . . .
H38B H 0.594320 -0.033621 0.084271 0.020 Uiso 1 1 calc R U . . .
C39 C 0.6584(3) -0.0670(3) 0.1852(3) 0.0272(15) Uani 1 1 d . . . . .
H39A H 0.700113 -0.022033 0.174757 0.041 Uiso 1 1 calc R U . . .
H39B H 0.694073 -0.110777 0.172826 0.041 Uiso 1 1 calc R U . . .
H39C H 0.636172 -0.078790 0.238155 0.041 Uiso 1 1 calc R U . . .
C40 C 0.5506(3) 0.0907(3) 0.1439(3) 0.0130(12) Uani 1 1 d . . . . .
C41 C 0.6330(3) 0.1141(3) 0.0935(3) 0.0187(13) Uani 1 1 d . . . . .
H41 H 0.668197 0.083673 0.064391 0.022 Uiso 1 1 calc R U . . .
C42 C 0.6521(3) 0.1901(3) 0.0953(3) 0.0220(14) Uani 1 1 d . . . . .
H42 H 0.702853 0.220819 0.067834 0.026 Uiso 1 1 calc R U . . .
C43 C 0.5815(3) 0.2127(3) 0.1457(3) 0.0151(12) Uani 1 1 d . . . . .
C44 C 0.5671(3) 0.2845(3) 0.1665(3) 0.0164(14) Uani 1 1 d . . . . .
H44 H 0.612565 0.323846 0.147556 0.020 Uiso 1 1 calc R U . . .
C45 C 0.4970(4) 0.3699(3) 0.2365(3) 0.0146(13) Uani 1 1 d . . . . .
C46 C 0.5751(4) 0.3836(3) 0.2749(3) 0.0165(14) Uani 1 1 d . . . . .
H46 H 0.624233 0.346250 0.283349 0.020 Uiso 1 1 calc R U . . .
C47 C 0.5826(4) 0.4529(3) 0.3017(3) 0.0214(14) Uani 1 1 d . . . . .
H47 H 0.636356 0.460763 0.327424 0.026 Uiso 1 1 calc R U . . .
C48 C 0.5118(4) 0.5081(3) 0.2903(3) 0.0242(15) Uani 1 1 d . . . . .
H48 H 0.516977 0.553245 0.308985 0.029 Uiso 1 1 calc R U . . .
C49 C 0.4299(4) 0.4979(3) 0.2502(3) 0.0168(14) Uani 1 1 d . . . . .
C50 C 0.3579(4) 0.5549(3) 0.2360(3) 0.0212(14) Uani 1 1 d . . . . .
H50 H 0.363672 0.600363 0.254012 0.025 Uiso 1 1 calc R U . . .
C51 C 0.2782(4) 0.5467(3) 0.1960(3) 0.0158(13) Uani 1 1 d . . . . .
C52 C 0.2068(4) 0.6072(3) 0.1801(3) 0.0272(15) Uani 1 1 d . . . . .
H52 H 0.213466 0.653281 0.196910 0.033 Uiso 1 1 calc R U . . .
C53 C 0.1301(4) 0.5981(3) 0.1409(3) 0.0291(16) Uani 1 1 d . . . . .
H53 H 0.084283 0.637901 0.130653 0.035 Uiso 1 1 calc R U . . .
C54 C 0.1186(4) 0.5285(3) 0.1152(3) 0.0212(15) Uani 1 1 d . . . . .
H54 H 0.064618 0.523216 0.088742 0.025 Uiso 1 1 calc R U . . .
C55 C 0.1841(4) 0.4691(3) 0.1279(3) 0.0187(14) Uani 1 1 d . . . . .
C56 C 0.2681(4) 0.4760(3) 0.1687(3) 0.0131(13) Uani 1 1 d . . . . .
C57 C 0.3421(3) 0.4195(3) 0.1811(3) 0.0147(13) Uani 1 1 d . . . . .
H57 H 0.337934 0.374932 0.161269 0.018 Uiso 1 1 calc R U . . .
C58 C 0.4218(3) 0.4278(3) 0.2220(3) 0.0127(13) Uani 1 1 d . . . . .
C59 C -0.1082(4) 0.3498(3) 0.1130(3) 0.0215(15) Uani 1 1 d . . . . .
H59 H -0.092328 0.316438 0.080185 0.026 Uiso 1 1 calc R U . . .
C60 C -0.1927(4) 0.3931(3) 0.1030(3) 0.0249(16) Uani 1 1 d . . . . .
H60 H -0.232234 0.389326 0.064471 0.030 Uiso 1 1 calc R U . . .
C61 C -0.2169(4) 0.4424(3) 0.1521(3) 0.0226(14) Uani 1 1 d . . . . .
H61 H -0.273997 0.471823 0.147483 0.027 Uiso 1 1 calc R U . . .
C62 C -0.1568(3) 0.4475(3) 0.2070(3) 0.0218(14) Uani 1 1 d . . . . .
H62 H -0.171824 0.480521 0.240360 0.026 Uiso 1 1 calc R U . . .
C63 C -0.0737(4) 0.4030(3) 0.2123(3) 0.0223(14) Uani 1 1 d . . . . .
H63 H -0.032470 0.407570 0.249548 0.027 Uiso 1 1 calc R U . . .
C64 C 0.1893(4) 0.3536(3) 0.3231(3) 0.0155(12) Uani 1 1 d . . . . .
C65 C 0.1433(3) 0.4127(3) 0.3515(3) 0.0199(13) Uani 1 1 d . . . . .
H65 H 0.086446 0.434531 0.331089 0.024 Uiso 1 1 calc R U . . .
C66 C 0.1799(4) 0.4403(3) 0.4098(3) 0.0280(14) Uani 1 1 d . . . . .
H66 H 0.147441 0.479662 0.429216 0.034 Uiso 1 1 calc R U . . .
C67 C 0.2647(4) 0.4089(3) 0.4387(3) 0.0267(14) Uani 1 1 d . . . . .
H67 H 0.290069 0.427126 0.477912 0.032 Uiso 1 1 calc R U . . .
C68 C 0.3126(4) 0.3505(3) 0.4100(3) 0.0214(14) Uani 1 1 d . . . . .
H68 H 0.369888 0.329659 0.430286 0.026 Uiso 1 1 calc R U . . .
C69 C 0.2770(3) 0.3220(3) 0.3513(3) 0.0142(12) Uani 1 1 d . . . . .
C70 C 0.6021(3) 0.1079(3) 0.3504(3) 0.0183(14) Uani 1 1 d . . . . .
H70 H 0.593689 0.072567 0.319624 0.022 Uiso 1 1 calc R U . . .
C71 C 0.6844(3) 0.0997(3) 0.3915(3) 0.0198(13) Uani 1 1 d . . . . .
H71 H 0.729599 0.060092 0.388488 0.024 Uiso 1 1 calc R U . . .
C72 C 0.6966(4) 0.1515(3) 0.4365(3) 0.0232(13) Uani 1 1 d . . . . .
H72 H 0.751801 0.148616 0.463696 0.028 Uiso 1 1 calc R U . . .
C73 C 0.6277(3) 0.2077(3) 0.4415(3) 0.0208(13) Uani 1 1 d . . . . .
H73 H 0.634008 0.242609 0.472971 0.025 Uiso 1 1 calc R U . . .
C74 C 0.5480(4) 0.2112(3) 0.3981(3) 0.0200(14) Uani 1 1 d . . . . .
H74 H 0.501102 0.249603 0.401255 0.024 Uiso 1 1 calc R U . . .
N0AA N 0.0141(3) -0.1851(3) 0.2480(3) 0.0345(13) Uani 1 1 d . . . . .
C0AA C 0.1019(5) -0.2107(3) 0.2706(3) 0.0368(17) Uani 1 1 d . . . . .
H0AA H 0.112841 -0.264279 0.281318 0.044 Uiso 1 1 calc R U . . .
C1AA C 0.1764(4) -0.1632(3) 0.2790(3) 0.0351(16) Uani 1 1 d . . . . .
H1AA H 0.235822 -0.183966 0.295230 0.042 Uiso 1 1 calc R U . . .
C102 C 0.1610(4) -0.0845(3) 0.2630(3) 0.0343(16) Uani 1 1 d . . . . .
H102 H 0.210268 -0.050506 0.267695 0.041 Uiso 1 1 calc R U . . .
C103 C 0.0716(4) -0.0559(3) 0.2398(3) 0.0304(15) Uani 1 1 d . . . . .
H103 H 0.059449 -0.002471 0.228148 0.036 Uiso 1 1 calc R U . . .
C104 C 0.0014(4) -0.1081(3) 0.2345(3) 0.0311(15) Uani 1 1 d . . . . .
H104 H -0.059407 -0.088467 0.220501 0.037 Uiso 1 1 calc R U . . .
N999 N 0.5495(9) 0.4429(4) -0.0219(5) 0.102(3) Uani 0.5 1 d . . P A 1
H999 H 0.580369 0.405392 -0.037299 0.122 Uiso 0.5 1 calc R U P A 1
C999 C 0.5495(9) 0.4429(4) -0.0219(5) 0.102(3) Uani 0.5 1 d . . P A 2
H99A H 0.582885 0.402339 -0.038555 0.122 Uiso 0.5 1 calc R U P A 2
C998 C 0.5959(6) 0.4853(5) 0.0194(4) 0.063(2) Uani 1 1 d . . . . .
H998 H 0.659759 0.474526 0.032295 0.076 Uiso 0.5 1 calc R U P A 1
H99B H 0.659759 0.474526 0.032295 0.076 Uiso 0.5 1 calc R U P A 2
C997 C 0.4547(9) 0.4581(6) -0.0397(5) 0.086(3) Uani 1 1 d . . . . .
H997 H 0.425616 0.426787 -0.067303 0.103 Uiso 0.5 1 calc R U P A 1
H99C H 0.425616 0.426787 -0.067303 0.103 Uiso 0.5 1 calc R U P A 2
N888 N 0.0935(5) -0.0219(4) 0.5204(5) 0.076(2) Uani 0.5 1 d . . P B 1
H888 H 0.151671 -0.035220 0.532731 0.092 Uiso 0.5 1 calc R U P B 1
C888 C 0.0935(5) -0.0219(4) 0.5204(5) 0.076(2) Uani 0.5 1 d . . P B 2
H88A H 0.156403 -0.036300 0.533732 0.092 Uiso 0.5 1 calc R U P B 2
C887 C 0.0582(8) -0.0379(5) 0.4574(5) 0.074(3) Uani 1 1 d . . . . .
H887 H 0.097648 -0.064711 0.427259 0.089 Uiso 0.5 1 calc R U P B 1
H88B H 0.097648 -0.064711 0.427259 0.089 Uiso 0.5 1 calc R U P B 2
C886 C 0.0321(8) 0.0161(5) 0.5633(5) 0.074(3) Uani 1 1 d . . . . .
H886 H 0.052765 0.027387 0.607535 0.089 Uiso 0.5 1 calc R U P B 1
H88C H 0.052765 0.027387 0.607535 0.089 Uiso 0.5 1 calc R U P B 2
N13 N -0.2004(5) 0.5226(3) 0.3898(3) 0.0538(17) Uani 1 1 d . . . . .
C300 C -0.1044(5) 0.5198(4) 0.3812(4) 0.0450(18) Uani 1 1 d . . . . .
H300 H -0.072530 0.477232 0.409233 0.054 Uiso 1 1 calc R U . . .
C301 C -0.0501(4) 0.5756(4) 0.3338(4) 0.0416(18) Uani 1 1 d . . . . .
H301 H 0.017552 0.571246 0.329311 0.050 Uiso 1 1 calc R U . . .
C302 C -0.0952(6) 0.6383(4) 0.2928(4) 0.052(2) Uani 1 1 d . . . . .
H302 H -0.058853 0.677588 0.260059 0.062 Uiso 1 1 calc R U . . .
C303 C -0.1935(7) 0.6429(4) 0.3002(4) 0.063(3) Uani 1 1 d . . . . .
H303 H -0.226568 0.685023 0.272631 0.076 Uiso 1 1 calc R U . . .
C304 C -0.2435(5) 0.5831(6) 0.3500(5) 0.063(3) Uani 1 1 d . . . . .
H304 H -0.311291 0.586031 0.355583 0.076 Uiso 1 1 calc R U . . .
N14 N 0.6162(3) 0.3083(3) 0.6372(3) 0.0336(13) Uani 1 1 d . . . . .
C400 C 0.6640(4) 0.3620(4) 0.5842(4) 0.0355(17) Uani 1 1 d . . . . .
H400 H 0.728845 0.371471 0.590707 0.043 Uiso 1 1 calc R U . . .
C401 C 0.6245(4) 0.4043(3) 0.5206(3) 0.0356(16) Uani 1 1 d . . . . .
H401 H 0.661743 0.441007 0.485378 0.043 Uiso 1 1 calc R U . . .
C402 C 0.5293(4) 0.3914(3) 0.5101(3) 0.0332(16) Uani 1 1 d . . . . .
H402 H 0.500324 0.419475 0.467743 0.040 Uiso 1 1 calc R U . . .
C403 C 0.4770(4) 0.3363(3) 0.5631(3) 0.0259(14) Uani 1 1 d . . . . .
H403 H 0.412270 0.325765 0.557280 0.031 Uiso 1 1 calc R U . . .
C404 C 0.5232(4) 0.2972(3) 0.6247(3) 0.0273(14) Uani 1 1 d . . . . .
H404 H 0.487226 0.260248 0.660501 0.033 Uiso 1 1 calc R U . . .
N15 N 0.4303(4) 0.2806(3) -0.1914(3) 0.0464(15) Uani 1 1 d . . . . .
C500 C 0.5185(4) 0.2642(3) -0.1665(4) 0.0333(16) Uani 1 1 d . . . . .
H500 H 0.570950 0.266280 -0.202752 0.040 Uiso 1 1 calc R U . . .
C501 C 0.5381(4) 0.2444(3) -0.0916(4) 0.0332(16) Uani 1 1 d . . . . .
H501 H 0.601510 0.233742 -0.077779 0.040 Uiso 1 1 calc R U . . .
C502 C 0.4611(4) 0.2407(3) -0.0375(3) 0.0326(16) Uani 1 1 d . . . . .
H502 H 0.471214 0.226938 0.014024 0.039 Uiso 1 1 calc R U . . .
C503 C 0.3690(4) 0.2576(3) -0.0609(3) 0.0346(16) Uani 1 1 d . . . . .
H503 H 0.315321 0.255761 -0.025759 0.041 Uiso 1 1 calc R U . . .
C504 C 0.3582(4) 0.2771(4) -0.1368(4) 0.0473(18) Uani 1 1 d . . . . .
H504 H 0.295508 0.289004 -0.151875 0.057 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 O1 2.096(3) . ?
U1 N3 2.469(4) . ?
U1 N2 2.482(4) . ?
U1 N9 2.566(4) . ?
U1 N1 2.572(4) . ?
U1 N4 2.576(4) . ?
U1 S1 2.7846(12) . ?
U1 S2 2.7914(13) . ?
U2 O2 2.109(3) . ?
U2 N6 2.472(4) . ?
U2 N7 2.473(4) . ?
U2 N8 2.559(4) . ?
U2 N10 2.571(4) . ?
U2 N5 2.570(4) . ?
U2 S1 2.7816(13) . ?
U2 S2 2.7852(12) . ?
S1 S2 2.1079(15) . ?
O1 C64 1.373(5) . ?
O2 C69 1.352(5) . ?
N1 C1 1.288(6) . ?
N1 C55 1.429(6) . ?
N2 C5 1.358(5) . ?
N2 C2 1.393(5) . ?
N3 C11 1.351(5) . ?
N3 C14 1.390(5) . ?
N4 C15 1.304(5) . ?
N4 C16 1.424(6) . ?
N5 C44 1.306(5) . ?
N5 C45 1.414(6) . ?
N6 C40 1.358(5) . ?
N6 C43 1.401(5) . ?
N7 C34 1.366(5) . ?
N7 C31 1.392(6) . ?
N8 C30 1.315(6) . ?
N8 C26 1.428(6) . ?
N9 C59 1.332(6) . ?
N9 C63 1.362(6) . ?
N10 C70 1.317(5) . ?
N10 C74 1.337(6) . ?
C1 C2 1.410(6) . ?
C2 C3 1.387(6) . ?
C3 C4 1.387(6) . ?
C4 C5 1.393(6) . ?
C5 C6 1.518(6) . ?
C6 C11 1.514(6) . ?
C6 C9 1.538(6) . ?
C6 C7 1.566(6) . ?
C7 C8 1.519(6) . ?
C9 C10 1.527(5) . ?
C11 C12 1.401(6) . ?
C12 C13 1.376(6) . ?
C13 C14 1.389(6) . ?
C14 C15 1.397(6) . ?
C16 C17 1.376(6) . ?
C16 C29 1.433(6) . ?
C17 C18 1.410(7) . ?
C18 C19 1.354(6) . ?
C19 C20 1.425(6) . ?
C20 C21 1.391(6) . ?
C20 C29 1.427(7) . ?
C21 C22 1.398(6) . ?
C22 C23 1.418(6) . ?
C22 C27 1.428(7) . ?
C23 C24 1.364(6) . ?
C24 C25 1.392(7) . ?
C25 C26 1.364(6) . ?
C26 C27 1.438(6) . ?
C27 C28 1.391(6) . ?
C28 C29 1.400(6) . ?
C30 C31 1.394(6) . ?
C31 C32 1.391(6) . ?
C32 C33 1.374(6) . ?
C33 C34 1.396(6) . ?
C34 C35 1.506(6) . ?
C35 C40 1.525(6) . ?
C35 C38 1.545(6) . ?
C35 C36 1.559(6) . ?
C36 C37 1.528(6) . ?
C38 C39 1.531(5) . ?
C40 C41 1.405(6) . ?
C41 C42 1.371(6) . ?
C42 C43 1.388(6) . ?
C43 C44 1.394(6) . ?
C45 C46 1.373(6) . ?
C45 C58 1.433(6) . ?
C46 C47 1.410(7) . ?
C47 C48 1.354(6) . ?
C48 C49 1.420(6) . ?
C49 C50 1.391(6) . ?
C49 C58 1.437(7) . ?
C50 C51 1.384(6) . ?
C51 C52 1.430(6) . ?
C51 C56 1.443(6) . ?
C52 C53 1.345(6) . ?
C53 C54 1.410(7) . ?
C54 C55 1.357(6) . ?
C55 C56 1.438(6) . ?
C56 C57 1.403(6) . ?
C57 C58 1.395(6) . ?
C59 C60 1.377(6) . ?
C60 C61 1.383(7) . ?
C61 C62 1.358(6) . ?
C62 C63 1.368(6) . ?
C64 C65 1.375(6) . ?
C64 C69 1.402(5) . ?
C65 C66 1.380(6) . ?
C66 C67 1.372(6) . ?
C67 C68 1.378(6) . ?
C68 C69 1.388(6) . ?
C70 C71 1.390(6) . ?
C71 C72 1.363(7) . ?
C72 C73 1.365(6) . ?
C73 C74 1.388(6) . ?
N0AA C104 1.331(6) . ?
N0AA C0AA 1.342(6) . ?
C0AA C1AA 1.370(7) . ?
C1AA C102 1.363(7) . ?
C102 C103 1.380(6) . ?
C103 C104 1.364(6) . ?
N999 C998 1.359(10) . ?
N999 C997 1.373(10) . ?
C999 C998 1.359(10) . ?
C999 C997 1.373(10) . ?
C998 C997 1.302(10) 2_665 ?
N888 C887 1.357(9) . ?
N888 C886 1.362(9) . ?
C888 C887 1.357(9) . ?
C888 C886 1.362(9) . ?
C887 C886 1.346(10) 2_556 ?
N13 C304 1.308(8) . ?
N13 C300 1.316(7) . ?
C300 C301 1.347(7) . ?
C301 C302 1.355(8) . ?
C302 C303 1.349(8) . ?
C303 C304 1.380(9) . ?
N14 C400 1.331(7) . ?
N14 C404 1.340(6) . ?
C400 C401 1.372(7) . ?
C401 C402 1.366(6) . ?
C402 C403 1.373(7) . ?
C403 C404 1.370(6) . ?
N15 C500 1.331(6) . ?
N15 C504 1.334(7) . ?
C500 C501 1.369(7) . ?
C501 C502 1.375(7) . ?
C502 C503 1.373(6) . ?
C503 C504 1.359(7) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 U1 N3 144.37(12) . . ?
O1 U1 N2 145.26(12) . . ?
N3 U1 N2 68.14(12) . . ?
O1 U1 N9 92.32(13) . . ?
N3 U1 N9 80.16(12) . . ?
N2 U1 N9 80.48(13) . . ?
O1 U1 N1 77.68(12) . . ?
N3 U1 N1 132.11(13) . . ?
N2 U1 N1 67.60(12) . . ?
N9 U1 N1 75.46(12) . . ?
O1 U1 N4 76.23(12) . . ?
N3 U1 N4 68.13(12) . . ?
N2 U1 N4 133.50(12) . . ?
N9 U1 N4 77.30(12) . . ?
N1 U1 N4 141.11(12) . . ?
O1 U1 S1 97.27(8) . . ?
N3 U1 S1 104.37(9) . . ?
N2 U1 S1 78.16(8) . . ?
N9 U1 S1 154.47(10) . . ?
N1 U1 S1 83.54(9) . . ?
N4 U1 S1 127.96(9) . . ?
O1 U1 S2 97.69(9) . . ?
N3 U1 S2 79.44(9) . . ?
N2 U1 S2 102.13(9) . . ?
N9 U1 S2 156.68(9) . . ?
N1 U1 S2 127.23(8) . . ?
N4 U1 S2 84.68(9) . . ?
S1 U1 S2 44.42(3) . . ?
O2 U2 N6 145.00(12) . . ?
O2 U2 N7 145.74(12) . . ?
N6 U2 N7 67.49(12) . . ?
O2 U2 N8 77.85(12) . . ?
N6 U2 N8 131.64(12) . . ?
N7 U2 N8 67.98(12) . . ?
O2 U2 N10 92.68(13) . . ?
N6 U2 N10 80.40(12) . . ?
N7 U2 N10 81.38(12) . . ?
N8 U2 N10 75.26(12) . . ?
O2 U2 N5 77.00(12) . . ?
N6 U2 N5 68.02(12) . . ?
N7 U2 N5 132.78(12) . . ?
N8 U2 N5 140.86(12) . . ?
N10 U2 N5 76.48(12) . . ?
O2 U2 S1 97.04(9) . . ?
N6 U2 S1 80.08(8) . . ?
N7 U2 S1 101.05(9) . . ?
N8 U2 S1 126.49(8) . . ?
N10 U2 S1 157.62(9) . . ?
N5 U2 S1 86.11(9) . . ?
O2 U2 S2 95.32(8) . . ?
N6 U2 S2 105.77(8) . . ?
N7 U2 S2 78.23(8) . . ?
N8 U2 S2 82.52(9) . . ?
N10 U2 S2 154.21(9) . . ?
N5 U2 S2 129.24(9) . . ?
S1 U2 S2 44.50(3) . . ?
S2 S1 U2 67.84(5) . . ?
S2 S1 U1 67.96(5) . . ?
U2 S1 U1 105.12(4) . . ?
S1 S2 U2 67.66(4) . . ?
S1 S2 U1 67.62(4) . . ?
U2 S2 U1 104.84(4) . . ?
C64 O1 U1 172.8(3) . . ?
C69 O2 U2 174.7(3) . . ?
C1 N1 C55 116.3(4) . . ?
C1 N1 U1 114.0(3) . . ?
C55 N1 U1 127.1(3) . . ?
C5 N2 C2 105.5(4) . . ?
C5 N2 U1 139.3(3) . . ?
C2 N2 U1 115.2(3) . . ?
C11 N3 C14 106.3(4) . . ?
C11 N3 U1 138.9(3) . . ?
C14 N3 U1 114.8(3) . . ?
C15 N4 C16 115.7(4) . . ?
C15 N4 U1 112.7(3) . . ?
C16 N4 U1 129.5(3) . . ?
C44 N5 C45 116.2(4) . . ?
C44 N5 U2 113.2(3) . . ?
C45 N5 U2 128.0(3) . . ?
C40 N6 C43 105.6(4) . . ?
C40 N6 U2 139.6(3) . . ?
C43 N6 U2 114.8(3) . . ?
C34 N7 C31 105.4(4) . . ?
C34 N7 U2 139.4(3) . . ?
C31 N7 U2 115.1(3) . . ?
C30 N8 C26 116.1(4) . . ?
C30 N8 U2 113.5(3) . . ?
C26 N8 U2 128.0(3) . . ?
C59 N9 C63 115.3(5) . . ?
C59 N9 U1 122.9(4) . . ?
C63 N9 U1 121.8(3) . . ?
C70 N10 C74 116.6(5) . . ?
C70 N10 U2 122.6(4) . . ?
C74 N10 U2 120.8(3) . . ?
N1 C1 C2 123.3(5) . . ?
C3 C2 N2 110.0(4) . . ?
C3 C2 C1 130.3(5) . . ?
N2 C2 C1 119.8(5) . . ?
C2 C3 C4 106.9(5) . . ?
C3 C4 C5 106.7(5) . . ?
N2 C5 C4 110.9(4) . . ?
N2 C5 C6 122.4(4) . . ?
C4 C5 C6 126.6(4) . . ?
C11 C6 C5 113.1(4) . . ?
C11 C6 C9 110.5(4) . . ?
C5 C6 C9 110.0(4) . . ?
C11 C6 C7 106.3(4) . . ?
C5 C6 C7 108.4(4) . . ?
C9 C6 C7 108.3(4) . . ?
C8 C7 C6 115.5(4) . . ?
C10 C9 C6 116.6(4) . . ?
N3 C11 C12 109.5(4) . . ?
N3 C11 C6 123.5(4) . . ?
C12 C11 C6 126.8(4) . . ?
C13 C12 C11 108.1(4) . . ?
C12 C13 C14 106.0(4) . . ?
C13 C14 N3 110.1(4) . . ?
C13 C14 C15 129.2(5) . . ?
N3 C14 C15 120.7(4) . . ?
N4 C15 C14 123.4(5) . . ?
C17 C16 N4 118.6(5) . . ?
C17 C16 C29 119.9(5) . . ?
N4 C16 C29 121.5(5) . . ?
C16 C17 C18 121.2(5) . . ?
C19 C18 C17 120.5(5) . . ?
C18 C19 C20 120.6(5) . . ?
C21 C20 C19 121.6(5) . . ?
C21 C20 C29 118.8(5) . . ?
C19 C20 C29 119.6(5) . . ?
C20 C21 C22 122.7(5) . . ?
C21 C22 C23 121.3(5) . . ?
C21 C22 C27 118.4(5) . . ?
C23 C22 C27 120.3(5) . . ?
C24 C23 C22 119.8(5) . . ?
C23 C24 C25 120.6(5) . . ?
C26 C25 C24 121.9(5) . . ?
C25 C26 N8 119.5(5) . . ?
C25 C26 C27 119.9(5) . . ?
N8 C26 C27 120.6(5) . . ?
C28 C27 C22 119.2(5) . . ?
C28 C27 C26 123.4(5) . . ?
C22 C27 C26 117.5(5) . . ?
C27 C28 C29 122.2(5) . . ?
C28 C29 C20 118.7(5) . . ?
C28 C29 C16 123.0(5) . . ?
C20 C29 C16 118.2(5) . . ?
N8 C30 C31 123.0(5) . . ?
C32 C31 N7 110.6(4) . . ?
C32 C31 C30 129.3(5) . . ?
N7 C31 C30 120.1(5) . . ?
C33 C32 C31 106.1(5) . . ?
C32 C33 C34 108.1(4) . . ?
N7 C34 C33 109.8(4) . . ?
N7 C34 C35 123.5(4) . . ?
C33 C34 C35 126.5(4) . . ?
C34 C35 C40 112.5(4) . . ?
C34 C35 C38 109.6(4) . . ?
C40 C35 C38 109.4(4) . . ?
C34 C35 C36 109.4(4) . . ?
C40 C35 C36 105.9(4) . . ?
C38 C35 C36 109.9(4) . . ?
C37 C36 C35 114.9(4) . . ?
C39 C38 C35 115.9(4) . . ?
N6 C40 C41 110.2(4) . . ?
N6 C40 C35 123.3(4) . . ?
C41 C40 C35 126.4(4) . . ?
C42 C41 C40 107.3(4) . . ?
C41 C42 C43 107.1(5) . . ?
C42 C43 C44 129.9(5) . . ?
C42 C43 N6 109.8(4) . . ?
C44 C43 N6 120.3(4) . . ?
N5 C44 C43 123.3(5) . . ?
C46 C45 N5 119.2(5) . . ?
C46 C45 C58 119.5(5) . . ?
N5 C45 C58 121.2(5) . . ?
C45 C46 C47 121.6(5) . . ?
C48 C47 C46 120.3(5) . . ?
C47 C48 C49 120.8(5) . . ?
C50 C49 C48 121.6(5) . . ?
C50 C49 C58 119.0(5) . . ?
C48 C49 C58 119.4(5) . . ?
C51 C50 C49 122.6(5) . . ?
C50 C51 C52 121.5(5) . . ?
C50 C51 C56 119.0(5) . . ?
C52 C51 C56 119.4(5) . . ?
C53 C52 C51 120.5(5) . . ?
C52 C53 C54 120.5(5) . . ?
C55 C54 C53 122.0(5) . . ?
C54 C55 N1 119.8(5) . . ?
C54 C55 C56 120.0(5) . . ?
N1 C55 C56 120.2(5) . . ?
C57 C56 C55 124.0(5) . . ?
C57 C56 C51 118.3(5) . . ?
C55 C56 C51 117.6(5) . . ?
C58 C57 C56 122.2(5) . . ?
C57 C58 C45 123.0(5) . . ?
C57 C58 C49 118.7(5) . . ?
C45 C58 C49 118.3(5) . . ?
N9 C59 C60 124.5(5) . . ?
C59 C60 C61 117.9(5) . . ?
C62 C61 C60 119.6(5) . . ?
C61 C62 C63 118.5(5) . . ?
N9 C63 C62 124.2(5) . . ?
O1 C64 C65 121.9(5) . . ?
O1 C64 C69 118.0(5) . . ?
C65 C64 C69 120.2(5) . . ?
C64 C65 C66 121.2(5) . . ?
C67 C66 C65 119.1(5) . . ?
C66 C67 C68 120.4(5) . . ?
C67 C68 C69 121.4(5) . . ?
O2 C69 C68 121.5(5) . . ?
O2 C69 C64 120.7(5) . . ?
C68 C69 C64 117.8(5) . . ?
N10 C70 C71 124.2(5) . . ?
C72 C71 C70 117.8(5) . . ?
C73 C72 C71 119.8(5) . . ?
C72 C73 C74 118.1(5) . . ?
N10 C74 C73 123.4(5) . . ?
C104 N0AA C0AA 115.5(5) . . ?
N0AA C0AA C1AA 124.5(5) . . ?
C102 C1AA C0AA 118.1(6) . . ?
C1AA C102 C103 119.2(5) . . ?
C104 C103 C102 118.2(5) . . ?
N0AA C104 C103 124.5(5) . . ?
C998 N999 C997 122.1(8) . . ?
C998 C999 C997 122.1(8) . . ?
C997 C998 N999 115.6(8) 2_665 . ?
C997 C998 C999 115.6(8) 2_665 . ?
C998 C997 N999 122.3(9) 2_665 . ?
C998 C997 C999 122.3(9) 2_665 . ?
C887 N888 C886 116.4(8) . . ?
C887 C888 C886 116.4(8) . . ?
C886 C887 N888 122.4(9) 2_556 . ?
C886 C887 C888 122.4(9) 2_556 . ?
C887 C886 N888 121.2(9) 2_556 . ?
C887 C886 C888 121.2(9) 2_556 . ?
C304 N13 C300 117.3(6) . . ?
N13 C300 C301 123.1(6) . . ?
C300 C301 C302 119.3(6) . . ?
C303 C302 C301 119.0(7) . . ?
C302 C303 C304 117.9(7) . . ?
N13 C304 C303 123.3(6) . . ?
C400 N14 C404 114.9(5) . . ?
N14 C400 C401 124.7(5) . . ?
C402 C401 C400 118.5(6) . . ?
C401 C402 C403 119.0(6) . . ?
C404 C403 C402 118.0(5) . . ?
N14 C404 C403 125.0(5) . . ?
C500 N15 C504 114.7(5) . . ?
N15 C500 C501 125.1(5) . . ?
C500 C501 C502 118.0(6) . . ?
C503 C502 C501 118.7(5) . . ?
C504 C503 C502 118.3(5) . . ?
N15 C504 C503 125.3(6) . . ?

_refine_diff_density_max         2.757
_refine_diff_density_min         -1.815
_refine_diff_density_rms         0.152


# start Validation Reply Form
_vrf_PLAT331_compound3           
;
PROBLEM: Small Aver Phenyl C-C Dist C997      -C998_b   .       1.34 Ang.  
RESPONSE: This molecule of lattice pyridine possessed large thermal motion,
giving rise to shorter than usual C-C distances. However, attempts to 
model the positional disorder of this molecule of pyridine resulted in 
unstable refinement. Therefore, this molecule of lattice solvent was left
as was.
;
_vrf_PLAT910_compound3           
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         21 Note  
RESPONSE: This has been noted, but is not serious. The independent 
reflections/parameters ratio is equal to 54, indicating that there are 
no issues with the data collected.
;
# end Validation Reply Form
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Pyridine/hexanes'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_compound4
_database_code_depnum_ccdc_archive 'CCDC 1984903'
loop_
_audit_author_name
_audit_author_address
'Bradley E. Cowie'
;The University of Edinburgh
United Kingdom
;
_audit_update_record             
;
2020-02-18 deposited with the CCDC.	2020-06-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        '[{(py)U(u-Se2)U(u-O2C6H4)(py)}(LA)]'
_chemical_name_common            'Compound 4.2CH2Cl2'
_chemical_melting_point          ?
_chemical_formula_moiety         'C74 H62 N10 O2 Se2 U2, 2(C H2 Cl2)'
_chemical_formula_sum            'C76 H66 Cl4 N10 O2 Se2 U2'
_chemical_formula_weight         1927.16

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

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

_cell_length_a                   10.9153(2)
_cell_length_b                   19.1212(4)
_cell_length_c                   34.2194(6)
_cell_angle_alpha                90
_cell_angle_beta                 92.935(2)
_cell_angle_gamma                90
_cell_volume                     7132.7(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    34327
_cell_measurement_theta_min      3.1080
_cell_measurement_theta_max      27.1310

_exptl_crystal_description       block
_exptl_crystal_colour            'clear pale yellow'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.795
_exptl_crystal_F_000             3712
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.148
_exptl_crystal_size_mid          0.078
_exptl_crystal_size_min          0.063
_exptl_absorpt_coefficient_mu    5.760
_shelx_estimated_absorpt_T_min   0.999
_shelx_estimated_absorpt_T_max   1.000
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.999
_exptl_absorpt_correction_T_max  1.000
_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   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 8.0521
_diffrn_reflns_number            133959
_diffrn_reflns_av_unetI/netI     0.0475
_diffrn_reflns_av_R_equivalents  0.0851
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_theta_min         2.834
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_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  23.00   1.00   30.00    --  -14.31 -99.00  30.00   48
  2  ω    -80.00   1.00   1.00   30.00    --  -14.31 -57.00   0.00   81
  3  ω    -85.00 -34.00   1.00   30.00    --  -14.31-179.00   0.00   51
  4  ω    -80.00   1.00   1.00   30.00    --  -14.31 -57.00 -90.00   81
  5  ω    -25.00  23.00   1.00   30.00    --  -14.31 -99.00 150.00   48
  6  ω     -1.00  85.00   1.00   30.00    --   16.03  37.00   0.00   86
  7  ω     -1.00  85.00   1.00   30.00    --   16.03  37.00 -60.00   86
  8  ω     34.00  86.00   1.00   30.00    --   16.03 179.00-150.00   52
  9  ω    -52.00  34.00   1.00   30.00    --   16.03 -37.00-180.00   86
 10  ω    -29.00  51.00   1.00   30.00    --  -14.31  57.00 -30.00   80
 11  ω    -32.00  54.00   1.00   30.00    --  -14.31  37.00 -60.00   86
 12  ω    -29.00  51.00   1.00   30.00    --  -14.31  57.00  30.00   80
 13  ω     -2.00  50.00   1.00   30.00    --   16.03-126.00 178.68   52
;
_reflns_number_total             13030
_reflns_number_gt                10932
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       '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 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_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 coordinated to U(2) (N(10), C(70), C(71), C(72), 
C(73), C(74)) was positionally disordered over two positions. As a result, 
it was split into two parts and refined with an occupancy ratio of 
0.58:0.42. In addition, the thermal parameters of the 
carbon and nitrogen atoms were restrained to be similar to one another, 
respectively, through the use of the SIMU command. In addition, residual 
lattice electron density (presumably from highly disordered lattice solvent) 
was modelled using the solvent mask feature of Olex2 (84.6 electrons/cell).,Solvent Mask
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0214P)²+39.6362P] 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         13030
_refine_ls_number_parameters     900
_refine_ls_number_restraints     132
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_gt           0.0424
_refine_ls_wR_factor_ref         0.0787
_refine_ls_wR_factor_gt          0.0749
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_restrained_S_all      1.060
_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 0.64703(2) 0.64738(2) 0.69080(2) 0.01411(6) Uani 1 1 d . . . . .
U2 U 0.64267(2) 0.81560(2) 0.59697(2) 0.01530(6) Uani 1 1 d . . . . .
Se2 Se 0.58381(6) 0.79481(3) 0.67856(2) 0.01889(14) Uani 1 1 d . . . . .
Se1 Se 0.78998(5) 0.76809(3) 0.66602(2) 0.01945(14) Uani 1 1 d . . . . .
Cl3 Cl 0.6611(3) 0.27185(13) 0.60065(10) 0.0813(9) Uani 1 1 d . . . . .
Cl4 Cl 0.4284(2) 0.33971(15) 0.58426(11) 0.0984(12) Uani 1 1 d . . . . .
Cl2 Cl 0.1168(2) 0.94802(15) 0.71687(10) 0.0864(9) Uani 1 1 d . . . . .
O2 O 0.5913(4) 0.7155(2) 0.57651(12) 0.0177(9) Uani 1 1 d . . . . .
O1 O 0.5854(3) 0.6160(2) 0.63413(11) 0.0165(9) Uani 1 1 d . . . . .
Cl1 Cl 0.2086(3) 0.81281(19) 0.69446(15) 0.1299(15) Uani 1 1 d . . . . .
N2 N 0.8194(4) 0.6493(3) 0.74011(15) 0.0185(11) Uani 1 1 d . . . . .
N3 N 0.5818(4) 0.6835(3) 0.75642(15) 0.0184(11) Uani 1 1 d . . . . .
N8 N 0.4095(4) 0.8244(3) 0.58833(15) 0.0193(12) Uani 1 1 d . . . . .
N4 N 0.4139(4) 0.6382(3) 0.69675(15) 0.0186(12) Uani 1 1 d . . . . .
N7 N 0.5650(5) 0.9327(3) 0.61601(15) 0.0185(12) Uani 1 1 d . . . . .
N5 N 0.8323(4) 0.7746(3) 0.56249(15) 0.0198(12) Uani 1 1 d . . . . .
N6 N 0.8078(5) 0.9042(3) 0.60118(15) 0.0224(12) Uani 1 1 d . . . . .
N1 N 0.8338(5) 0.5796(3) 0.66664(15) 0.0200(12) Uani 1 1 d . . . . .
N10 N 0.6109(12) 0.8628(7) 0.5262(3) 0.023(3) Uani 0.58(2) 1 d G U P A 1
C74 C 0.6017(15) 0.8212(5) 0.4929(5) 0.025(3) Uani 0.58(2) 1 d G U P A 1
H74 H 0.598217 0.772749 0.495245 0.029 Uiso 0.58(2) 1 calc R U P A 1
C73 C 0.5975(13) 0.8519(7) 0.4560(4) 0.035(2) Uani 0.58(2) 1 d G U P A 1
H73 H 0.591313 0.824013 0.433723 0.042 Uiso 0.58(2) 1 calc R U P A 1
C72 C 0.6027(12) 0.9242(7) 0.4525(3) 0.044(2) Uani 0.58(2) 1 d G U P A 1
H72 H 0.599907 0.944761 0.427813 0.053 Uiso 0.58(2) 1 calc R U P A 1
C71 C 0.6120(17) 0.9658(5) 0.4858(4) 0.044(3) Uani 0.58(2) 1 d G U P A 1
H71 H 0.615406 1.014244 0.483426 0.052 Uiso 0.58(2) 1 calc R U P A 1
C70 C 0.6161(15) 0.9351(6) 0.5227(3) 0.040(3) Uani 0.58(2) 1 d G U P A 1
H70 H 0.622311 0.962981 0.544948 0.048 Uiso 0.58(2) 1 calc R U P A 1
N9 N 0.6081(4) 0.5222(3) 0.71403(15) 0.0198(12) Uani 1 1 d . . . . .
C5 C 0.8501(6) 0.6762(3) 0.77576(18) 0.0204(14) Uani 1 1 d . . . . .
C16 C 0.3291(5) 0.5998(3) 0.67223(18) 0.0167(13) Uani 1 1 d . . . . .
C11 C 0.6323(6) 0.7092(3) 0.79086(17) 0.0189(14) Uani 1 1 d . . . . .
C69 C 0.5456(5) 0.6515(3) 0.56818(17) 0.0163(13) Uani 1 1 d . . . . .
C28 C 0.3187(5) 0.6931(3) 0.62140(18) 0.0181(14) Uani 1 1 d . . . . .
H28 H 0.369137 0.721476 0.637387 0.022 Uiso 1 1 calc R U . . .
C56 C 0.8418(5) 0.5557(3) 0.59541(19) 0.0192(14) Uani 1 1 d . . . . .
C2 C 0.9232(6) 0.6142(3) 0.72897(18) 0.0201(14) Uani 1 1 d . . . . .
C40 C 0.8319(6) 0.9675(3) 0.61742(19) 0.0242(15) Uani 1 1 d . . . . .
C57 C 0.8374(5) 0.6257(3) 0.58485(19) 0.0212(14) Uani 1 1 d . . . . .
H57 H 0.832638 0.659357 0.604356 0.025 Uiso 1 1 calc R U . . .
C58 C 0.8397(5) 0.6474(3) 0.54615(18) 0.0196(14) Uani 1 1 d . . . . .
C64 C 0.5405(5) 0.6012(3) 0.59721(18) 0.0155(13) Uani 1 1 d . . . . .
C26 C 0.3225(5) 0.7801(3) 0.56698(19) 0.0220(15) Uani 1 1 d . . . . .
C14 C 0.4564(6) 0.6821(3) 0.76079(18) 0.0195(14) Uani 1 1 d . . . . .
C34 C 0.6090(6) 0.9918(3) 0.63328(17) 0.0195(14) Uani 1 1 d . . . . .
C45 C 0.8413(6) 0.7197(4) 0.53448(18) 0.0225(15) Uani 1 1 d . . . . .
C1 C 0.9248(6) 0.5784(3) 0.69325(19) 0.0228(15) Uani 1 1 d . . . . .
H1 H 0.994056 0.552308 0.688134 0.027 Uiso 1 1 calc R U . . .
C15 C 0.3762(6) 0.6564(3) 0.73102(19) 0.0199(14) Uani 1 1 d . . . . .
H15 H 0.293362 0.652142 0.735705 0.024 Uiso 1 1 calc R U . . .
C30 C 0.3650(6) 0.8803(3) 0.60394(18) 0.0218(15) Uani 1 1 d . . . . .
H30 H 0.280283 0.884894 0.604637 0.026 Uiso 1 1 calc R U . . .
C27 C 0.2806(5) 0.7169(3) 0.58393(19) 0.0187(14) Uani 1 1 d . . . . .
C44 C 0.9220(6) 0.8183(3) 0.56569(19) 0.0242(15) Uani 1 1 d . . . . .
H44 H 0.993860 0.807407 0.553527 0.029 Uiso 1 1 calc R U . . .
C31 C 0.4390(6) 0.9335(3) 0.61959(18) 0.0191(14) Uani 1 1 d . . . . .
C65 C 0.4848(5) 0.5371(3) 0.58880(19) 0.0213(14) Uani 1 1 d . . . . .
H65 H 0.480245 0.503605 0.608376 0.026 Uiso 1 1 calc R U . . .
C29 C 0.2829(5) 0.6281(3) 0.63525(18) 0.0187(14) Uani 1 1 d . . . . .
C55 C 0.8442(6) 0.5314(3) 0.63539(19) 0.0223(15) Uani 1 1 d . . . . .
C63 C 0.5964(6) 0.4705(3) 0.6880(2) 0.0241(15) Uani 1 1 d . . . . .
H63 H 0.610829 0.480582 0.662004 0.029 Uiso 1 1 calc R U . . .
C59 C 0.5875(6) 0.5057(3) 0.75167(19) 0.0245(15) Uani 1 1 d . . . . .
H59 H 0.596205 0.540334 0.770684 0.029 Uiso 1 1 calc R U . . .
C46 C 0.8498(6) 0.7374(4) 0.49633(19) 0.0265(16) Uani 1 1 d . . . . .
H46 H 0.852605 0.784308 0.489318 0.032 Uiso 1 1 calc R U . . .
C43 C 0.9174(6) 0.8811(4) 0.5864(2) 0.0272(16) Uani 1 1 d . . . . .
C33 C 0.5121(6) 1.0308(3) 0.64823(19) 0.0259(16) Uani 1 1 d . . . . .
H33 H 0.518634 1.073351 0.661386 0.031 Uiso 1 1 calc R U . . .
C3 C 1.0174(6) 0.6196(4) 0.7574(2) 0.0292(17) Uani 1 1 d . . . . .
H3 H 1.095597 0.600529 0.756638 0.035 Uiso 1 1 calc R U . . .
C6 C 0.7673(6) 0.7258(3) 0.79724(18) 0.0206(14) Uani 1 1 d . . . . .
C7 C 0.7860(6) 0.8017(3) 0.78210(19) 0.0254(15) Uani 1 1 d . . . . .
H7A H 0.758200 0.803220 0.754736 0.030 Uiso 1 1 calc R U . . .
H7B H 0.733196 0.832504 0.796192 0.030 Uiso 1 1 calc R U . . .
C12 C 0.5409(6) 0.7237(3) 0.81672(18) 0.0226(15) Uani 1 1 d . . . . .
H12 H 0.552482 0.741242 0.841983 0.027 Uiso 1 1 calc R U . . .
C68 C 0.4976(6) 0.6362(3) 0.53057(18) 0.0235(15) Uani 1 1 d . . . . .
H68 H 0.501760 0.669496 0.510886 0.028 Uiso 1 1 calc R U . . .
C13 C 0.4300(6) 0.7069(3) 0.79779(19) 0.0235(15) Uani 1 1 d . . . . .
H13 H 0.352720 0.711369 0.807749 0.028 Uiso 1 1 calc R U . . .
C32 C 0.4055(6) 0.9936(3) 0.63952(18) 0.0241(15) Uani 1 1 d . . . . .
H32 H 0.326615 1.006263 0.645756 0.029 Uiso 1 1 calc R U . . .
C54 C 0.8595(6) 0.4619(3) 0.6438(2) 0.0259(16) Uani 1 1 d . . . . .
H54 H 0.863011 0.447356 0.669734 0.031 Uiso 1 1 calc R U . . .
C51 C 0.8499(6) 0.5040(4) 0.5652(2) 0.0244(15) Uani 1 1 d . . . . .
C35 C 0.7415(6) 1.0150(3) 0.6365(2) 0.0241(15) Uani 1 1 d . . . . .
C62 C 0.5642(6) 0.4036(4) 0.6972(2) 0.0298(17) Uani 1 1 d . . . . .
H62 H 0.557249 0.369244 0.677915 0.036 Uiso 1 1 calc R U . . .
C52 C 0.8646(6) 0.4319(4) 0.5758(2) 0.0306(17) Uani 1 1 d . . . . .
H52 H 0.870488 0.398322 0.556288 0.037 Uiso 1 1 calc R U . . .
C37 C 0.7745(7) 0.9600(4) 0.7048(2) 0.0357(19) Uani 1 1 d . . . . .
H37A H 0.690416 0.945722 0.705823 0.054 Uiso 1 1 calc R U . . .
H37B H 0.807432 0.969733 0.730739 0.054 Uiso 1 1 calc R U . . .
H37C H 0.821032 0.923247 0.693474 0.054 Uiso 1 1 calc R U . . .
C53 C 0.8702(6) 0.4119(4) 0.6139(2) 0.0315(17) Uani 1 1 d . . . . .
H53 H 0.881036 0.364937 0.620314 0.038 Uiso 1 1 calc R U . . .
C17 C 0.2932(6) 0.5349(3) 0.68361(19) 0.0221(15) Uani 1 1 d . . . . .
H17 H 0.322781 0.517448 0.707645 0.027 Uiso 1 1 calc R U . . .
C66 C 0.4360(6) 0.5229(3) 0.55136(19) 0.0215(14) Uani 1 1 d . . . . .
H66 H 0.398083 0.480153 0.545920 0.026 Uiso 1 1 calc R U . . .
C9 C 0.8040(6) 0.7248(4) 0.84181(18) 0.0275(16) Uani 1 1 d . . . . .
H9A H 0.889504 0.738181 0.845386 0.033 Uiso 1 1 calc R U . . .
H9B H 0.755791 0.759738 0.854659 0.033 Uiso 1 1 calc R U . . .
C21 C 0.1576(5) 0.6111(3) 0.5755(2) 0.0231(15) Uani 1 1 d . . . . .
H21 H 0.100811 0.584613 0.560742 0.028 Uiso 1 1 calc R U . . .
C47 C 0.8545(6) 0.6852(4) 0.4669(2) 0.0331(17) Uani 1 1 d . . . . .
H47 H 0.859644 0.698465 0.440911 0.040 Uiso 1 1 calc R U . . .
C4 C 0.9714(6) 0.6594(4) 0.7874(2) 0.0301(17) Uani 1 1 d . . . . .
H4 H 1.013076 0.672335 0.810688 0.036 Uiso 1 1 calc R U . . .
C20 C 0.1993(5) 0.5861(3) 0.61166(18) 0.0211(15) Uani 1 1 d . . . . .
C25 C 0.2844(6) 0.7992(4) 0.53014(19) 0.0269(16) Uani 1 1 d . . . . .
H25 H 0.313791 0.840336 0.519561 0.032 Uiso 1 1 calc R U . . .
C67 C 0.4442(6) 0.5724(3) 0.52229(19) 0.0239(15) Uani 1 1 d . . . . .
H67 H 0.413490 0.562561 0.497032 0.029 Uiso 1 1 calc R U . . .
C22 C 0.1964(5) 0.6738(3) 0.56029(18) 0.0199(14) Uani 1 1 d . . . . .
C60 C 0.5544(6) 0.4397(4) 0.7627(2) 0.0286(16) Uani 1 1 d . . . . .
H60 H 0.539961 0.430190 0.788693 0.034 Uiso 1 1 calc R U . . .
C23 C 0.1579(6) 0.6966(4) 0.52196(19) 0.0259(16) Uani 1 1 d . . . . .
H23 H 0.103217 0.669502 0.506744 0.031 Uiso 1 1 calc R U . . .
C42 C 1.0075(6) 0.9317(4) 0.5934(2) 0.040(2) Uani 1 1 d . . . . .
H42 H 1.088219 0.929566 0.586010 0.048 Uiso 1 1 calc R U . . .
C38 C 0.7491(7) 1.0902(4) 0.6174(2) 0.0354(18) Uani 1 1 d . . . . .
H38A H 0.691474 1.120880 0.629593 0.042 Uiso 1 1 calc R U . . .
H38B H 0.830774 1.108955 0.622870 0.042 Uiso 1 1 calc R U . . .
C24 C 0.2001(6) 0.7572(4) 0.50751(19) 0.0273(16) Uani 1 1 d . . . . .
H24 H 0.173699 0.771587 0.482509 0.033 Uiso 1 1 calc R U . . .
C19 C 0.1667(5) 0.5183(3) 0.62535(19) 0.0218(15) Uani 1 1 d . . . . .
H19 H 0.112925 0.490709 0.610081 0.026 Uiso 1 1 calc R U . . .
C18 C 0.2125(6) 0.4937(4) 0.6599(2) 0.0277(16) Uani 1 1 d . . . . .
H18 H 0.190736 0.449316 0.668193 0.033 Uiso 1 1 calc R U . . .
C61 C 0.5427(6) 0.3881(4) 0.7352(2) 0.0302(17) Uani 1 1 d . . . . .
H61 H 0.520298 0.343085 0.742215 0.036 Uiso 1 1 calc R U . . .
C49 C 0.8464(6) 0.5954(4) 0.5161(2) 0.0264(16) Uani 1 1 d . . . . .
C36 C 0.7817(7) 1.0247(4) 0.6801(2) 0.0344(18) Uani 1 1 d . . . . .
H36A H 0.865545 1.041577 0.681784 0.041 Uiso 1 1 calc R U . . .
H36B H 0.730613 1.060495 0.691037 0.041 Uiso 1 1 calc R U . . .
C48 C 0.8516(6) 0.6163(4) 0.4762(2) 0.0326(18) Uani 1 1 d . . . . .
H48 H 0.852957 0.582768 0.456521 0.039 Uiso 1 1 calc R U . . .
C41 C 0.9545(7) 0.9853(4) 0.6132(2) 0.040(2) Uani 1 1 d . . . . .
H41 H 0.993275 1.026013 0.622194 0.049 Uiso 1 1 calc R U . . .
C10 C 0.7864(7) 0.6542(4) 0.8621(2) 0.0362(18) Uani 1 1 d . . . . .
H10A H 0.700596 0.642904 0.861560 0.054 Uiso 1 1 calc R U . . .
H10B H 0.817847 0.657074 0.888791 0.054 Uiso 1 1 calc R U . . .
H10C H 0.829631 0.618479 0.848740 0.054 Uiso 1 1 calc R U . . .
C50 C 0.8507(6) 0.5252(4) 0.5266(2) 0.0293(17) Uani 1 1 d . . . . .
H50 H 0.854159 0.491529 0.507135 0.035 Uiso 1 1 calc R U . . .
C39 C 0.7215(8) 1.0909(4) 0.5733(2) 0.043(2) Uani 1 1 d . . . . .
H39A H 0.778962 1.061336 0.560867 0.065 Uiso 1 1 calc R U . . .
H39B H 0.728494 1.137834 0.563662 0.065 Uiso 1 1 calc R U . . .
H39C H 0.639728 1.074052 0.567591 0.065 Uiso 1 1 calc R U . . .
C8 C 0.9141(7) 0.8308(4) 0.7856(2) 0.041(2) Uani 1 1 d . . . . .
H8A H 0.940613 0.834035 0.812720 0.062 Uiso 1 1 calc R U . . .
H8B H 0.915023 0.876498 0.773970 0.062 Uiso 1 1 calc R U . . .
H8C H 0.968471 0.800519 0.772318 0.062 Uiso 1 1 calc R U . . .
C200 C 0.5870(9) 0.3426(6) 0.5809(3) 0.081(4) Uani 1 1 d . . . . .
H20A H 0.605510 0.346263 0.553574 0.097 Uiso 1 1 calc R U . . .
H20B H 0.618209 0.384371 0.594096 0.097 Uiso 1 1 calc R U . . .
C100 C 0.0833(9) 0.8685(5) 0.6927(3) 0.068(3) Uani 1 1 d . . . . .
H10D H 0.015425 0.845833 0.704859 0.082 Uiso 1 1 calc R U . . .
H10E H 0.058308 0.877905 0.665633 0.082 Uiso 1 1 calc R U . . .
N10A N 0.6227(18) 0.8693(11) 0.5280(5) 0.026(4) Uani 0.42(2) 1 d G U P A 2
C74A C 0.576(2) 0.8260(9) 0.4983(7) 0.028(3) Uani 0.42(2) 1 d G U P A 2
H74A H 0.543171 0.782682 0.504266 0.033 Uiso 0.42(2) 1 calc R U P A 2
C73A C 0.5780(18) 0.8476(10) 0.4595(6) 0.036(3) Uani 0.42(2) 1 d G U P A 2
H73A H 0.546666 0.818587 0.439572 0.043 Uiso 0.42(2) 1 calc R U P A 2
C72A C 0.6269(17) 0.9124(10) 0.4505(4) 0.041(3) Uani 0.42(2) 1 d G U P A 2
H72A H 0.628314 0.926762 0.424588 0.049 Uiso 0.42(2) 1 calc R U P A 2
C71A C 0.674(2) 0.9557(8) 0.4803(5) 0.043(3) Uani 0.42(2) 1 d G U P A 2
H71A H 0.706466 0.999032 0.474298 0.052 Uiso 0.42(2) 1 calc R U P A 2
C70A C 0.672(2) 0.9342(10) 0.5191(4) 0.041(3) Uani 0.42(2) 1 d G U P A 2
H70A H 0.702971 0.963129 0.538993 0.049 Uiso 0.42(2) 1 calc R U P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 O1 2.107(4) . ?
U1 N2 2.463(5) . ?
U1 N3 2.488(5) . ?
U1 N9 2.564(5) . ?
U1 N4 2.569(5) . ?
U1 N1 2.587(5) . ?
U1 Se2 2.9273(6) . ?
U1 Se1 2.9354(7) . ?
U2 O2 2.104(4) . ?
U2 N6 2.472(5) . ?
U2 N7 2.493(5) . ?
U2 N8 2.553(5) . ?
U2 N5 2.558(5) . ?
U2 N10A 2.572(15) . ?
U2 N10 2.591(11) . ?
U2 Se2 2.9239(7) . ?
U2 Se1 2.9333(6) . ?
Se2 Se1 2.3682(9) . ?
Cl3 C200 1.698(11) . ?
Cl4 C200 1.742(10) . ?
Cl2 C100 1.760(10) . ?
O2 C69 1.346(7) . ?
O1 C64 1.362(7) . ?
Cl1 C100 1.731(10) . ?
N2 C5 1.350(8) . ?
N2 C2 1.387(8) . ?
N3 C11 1.366(7) . ?
N3 C14 1.384(8) . ?
N8 C30 1.300(8) . ?
N8 C26 1.443(8) . ?
N4 C15 1.310(8) . ?
N4 C16 1.422(7) . ?
N7 C34 1.353(8) . ?
N7 C31 1.387(8) . ?
N5 C44 1.287(8) . ?
N5 C45 1.428(8) . ?
N6 C40 1.353(8) . ?
N6 C43 1.395(8) . ?
N1 C1 1.313(8) . ?
N1 C55 1.420(8) . ?
N10 C74 1.3900 . ?
N10 C70 1.3900 . ?
C74 C73 1.3900 . ?
C73 C72 1.3900 . ?
C72 C71 1.3900 . ?
C71 C70 1.3900 . ?
N9 C63 1.333(8) . ?
N9 C59 1.356(8) . ?
C5 C4 1.400(9) . ?
C5 C6 1.524(9) . ?
C16 C17 1.363(9) . ?
C16 C29 1.444(9) . ?
C11 C12 1.394(9) . ?
C11 C6 1.513(9) . ?
C69 C64 1.386(8) . ?
C69 C68 1.396(8) . ?
C28 C29 1.394(9) . ?
C28 C27 1.403(9) . ?
C56 C57 1.388(9) . ?
C56 C51 1.436(9) . ?
C56 C55 1.444(9) . ?
C2 C3 1.382(9) . ?
C2 C1 1.402(9) . ?
C40 C41 1.395(10) . ?
C40 C35 1.513(9) . ?
C57 C58 1.389(9) . ?
C58 C49 1.435(9) . ?
C58 C45 1.440(9) . ?
C64 C65 1.391(8) . ?
C26 C25 1.357(9) . ?
C26 C27 1.427(9) . ?
C14 C13 1.396(9) . ?
C14 C15 1.398(9) . ?
C34 C33 1.412(9) . ?
C34 C35 1.512(9) . ?
C45 C46 1.356(9) . ?
C30 C31 1.389(9) . ?
C27 C22 1.449(8) . ?
C44 C43 1.396(9) . ?
C31 C32 1.395(9) . ?
C65 C66 1.389(9) . ?
C29 C20 1.433(8) . ?
C55 C54 1.368(9) . ?
C63 C62 1.369(9) . ?
C59 C60 1.370(9) . ?
C46 C47 1.420(10) . ?
C43 C42 1.391(10) . ?
C33 C32 1.383(9) . ?
C3 C4 1.393(10) . ?
C6 C9 1.557(8) . ?
C6 C7 1.558(9) . ?
C7 C8 1.504(9) . ?
C12 C13 1.381(9) . ?
C68 C67 1.376(9) . ?
C54 C53 1.409(9) . ?
C51 C50 1.382(10) . ?
C51 C52 1.432(9) . ?
C35 C36 1.544(9) . ?
C35 C38 1.585(9) . ?
C62 C61 1.366(9) . ?
C52 C53 1.357(10) . ?
C37 C36 1.501(10) . ?
C17 C18 1.407(9) . ?
C66 C67 1.379(9) . ?
C9 C10 1.534(10) . ?
C21 C22 1.381(9) . ?
C21 C20 1.382(9) . ?
C47 C48 1.354(10) . ?
C20 C19 1.429(9) . ?
C25 C24 1.421(9) . ?
C22 C23 1.425(9) . ?
C60 C61 1.365(10) . ?
C23 C24 1.349(9) . ?
C42 C41 1.374(10) . ?
C38 C39 1.523(10) . ?
C19 C18 1.345(9) . ?
C49 C50 1.390(10) . ?
C49 C48 1.428(10) . ?
N10A C74A 1.3900 . ?
N10A C70A 1.3900 . ?
C74A C73A 1.3900 . ?
C73A C72A 1.3900 . ?
C72A C71A 1.3900 . ?
C71A C70A 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
O1 U1 N2 146.25(16) . . ?
O1 U1 N3 144.81(16) . . ?
N2 U1 N3 67.76(16) . . ?
O1 U1 N9 88.25(16) . . ?
N2 U1 N9 86.25(16) . . ?
N3 U1 N9 85.42(17) . . ?
O1 U1 N4 77.46(15) . . ?
N2 U1 N4 132.22(16) . . ?
N3 U1 N4 67.49(16) . . ?
N9 U1 N4 74.41(16) . . ?
O1 U1 N1 77.45(15) . . ?
N2 U1 N1 68.87(16) . . ?
N3 U1 N1 133.97(16) . . ?
N9 U1 N1 77.11(16) . . ?
N4 U1 N1 142.27(16) . . ?
O1 U1 Se2 94.62(11) . . ?
N2 U1 Se2 104.47(12) . . ?
N3 U1 Se2 77.60(12) . . ?
N9 U1 Se2 154.38(11) . . ?
N4 U1 Se2 81.37(11) . . ?
N1 U1 Se2 128.37(11) . . ?
O1 U1 Se1 96.15(11) . . ?
N2 U1 Se1 77.72(12) . . ?
N3 U1 Se1 102.89(12) . . ?
N9 U1 Se1 157.28(11) . . ?
N4 U1 Se1 128.30(11) . . ?
N1 U1 Se1 82.10(11) . . ?
Se2 U1 Se1 47.649(18) . . ?
O2 U2 N6 145.45(17) . . ?
O2 U2 N7 144.65(16) . . ?
N6 U2 N7 68.05(17) . . ?
O2 U2 N8 76.97(16) . . ?
N6 U2 N8 132.93(17) . . ?
N7 U2 N8 67.69(16) . . ?
O2 U2 N5 77.06(16) . . ?
N6 U2 N5 68.40(17) . . ?
N7 U2 N5 133.62(17) . . ?
N8 U2 N5 142.42(16) . . ?
O2 U2 N10A 92.8(5) . . ?
N6 U2 N10A 78.9(5) . . ?
N7 U2 N10A 82.3(5) . . ?
N8 U2 N10A 80.2(4) . . ?
N5 U2 N10A 74.4(4) . . ?
O2 U2 N10 89.1(3) . . ?
N6 U2 N10 83.0(3) . . ?
N7 U2 N10 84.3(3) . . ?
N8 U2 N10 77.5(3) . . ?
N5 U2 N10 75.4(3) . . ?
O2 U2 Se2 97.26(11) . . ?
N6 U2 Se2 103.45(12) . . ?
N7 U2 Se2 77.19(12) . . ?
N8 U2 Se2 81.55(11) . . ?
N5 U2 Se2 128.43(11) . . ?
N10A U2 Se2 156.6(4) . . ?
N10 U2 Se2 156.1(3) . . ?
O2 U2 Se1 96.43(11) . . ?
N6 U2 Se1 78.30(12) . . ?
N7 U2 Se1 104.33(11) . . ?
N8 U2 Se1 128.02(11) . . ?
N5 U2 Se1 81.58(11) . . ?
N10A U2 Se1 151.6(4) . . ?
N10 U2 Se1 154.5(3) . . ?
Se2 U2 Se1 47.697(18) . . ?
Se1 Se2 U2 66.36(2) . . ?
Se1 Se2 U1 66.36(2) . . ?
U2 Se2 U1 101.877(19) . . ?
Se2 Se1 U2 65.94(2) . . ?
Se2 Se1 U1 66.00(2) . . ?
U2 Se1 U1 101.457(19) . . ?
C69 O2 U2 170.6(4) . . ?
C64 O1 U1 175.0(4) . . ?
C5 N2 C2 105.3(5) . . ?
C5 N2 U1 140.4(4) . . ?
C2 N2 U1 114.3(4) . . ?
C11 N3 C14 105.7(5) . . ?
C11 N3 U1 139.2(4) . . ?
C14 N3 U1 115.0(4) . . ?
C30 N8 C26 116.1(5) . . ?
C30 N8 U2 113.5(4) . . ?
C26 N8 U2 130.3(4) . . ?
C15 N4 C16 116.2(5) . . ?
C15 N4 U1 114.2(4) . . ?
C16 N4 U1 127.3(4) . . ?
C34 N7 C31 106.5(5) . . ?
C34 N7 U2 138.3(4) . . ?
C31 N7 U2 112.6(4) . . ?
C44 N5 C45 117.1(5) . . ?
C44 N5 U2 113.1(4) . . ?
C45 N5 U2 128.3(4) . . ?
C40 N6 C43 106.3(5) . . ?
C40 N6 U2 139.8(4) . . ?
C43 N6 U2 113.5(4) . . ?
C1 N1 C55 115.1(5) . . ?
C1 N1 U1 111.6(4) . . ?
C55 N1 U1 131.3(4) . . ?
C74 N10 C70 120.0 . . ?
C74 N10 U2 124.6(6) . . ?
C70 N10 U2 115.1(7) . . ?
N10 C74 C73 120.0 . . ?
C72 C73 C74 120.0 . . ?
C71 C72 C73 120.0 . . ?
C70 C71 C72 120.0 . . ?
C71 C70 N10 120.0 . . ?
C63 N9 C59 116.6(5) . . ?
C63 N9 U1 119.7(4) . . ?
C59 N9 U1 123.4(4) . . ?
N2 C5 C4 110.9(6) . . ?
N2 C5 C6 123.2(5) . . ?
C4 C5 C6 125.5(6) . . ?
C17 C16 N4 119.3(6) . . ?
C17 C16 C29 119.9(6) . . ?
N4 C16 C29 120.7(5) . . ?
N3 C11 C12 110.4(5) . . ?
N3 C11 C6 123.1(5) . . ?
C12 C11 C6 126.2(6) . . ?
O2 C69 C64 120.5(5) . . ?
O2 C69 C68 120.2(6) . . ?
C64 C69 C68 119.2(6) . . ?
C29 C28 C27 121.6(6) . . ?
C57 C56 C51 118.7(6) . . ?
C57 C56 C55 123.8(6) . . ?
C51 C56 C55 117.5(6) . . ?
C3 C2 N2 111.0(6) . . ?
C3 C2 C1 127.5(6) . . ?
N2 C2 C1 121.5(5) . . ?
N6 C40 C41 110.1(6) . . ?
N6 C40 C35 126.6(6) . . ?
C41 C40 C35 123.2(6) . . ?
C56 C57 C58 122.3(6) . . ?
C57 C58 C49 118.7(6) . . ?
C57 C58 C45 123.5(6) . . ?
C49 C58 C45 117.7(6) . . ?
O1 C64 C69 119.6(5) . . ?
O1 C64 C65 120.6(6) . . ?
C69 C64 C65 119.8(6) . . ?
C25 C26 C27 121.0(6) . . ?
C25 C26 N8 118.4(6) . . ?
C27 C26 N8 120.5(6) . . ?
N3 C14 C13 110.0(5) . . ?
N3 C14 C15 120.9(6) . . ?
C13 C14 C15 129.0(6) . . ?
N7 C34 C33 110.1(6) . . ?
N7 C34 C35 126.4(6) . . ?
C33 C34 C35 123.4(6) . . ?
C46 C45 N5 118.3(6) . . ?
C46 C45 C58 120.5(6) . . ?
N5 C45 C58 121.2(6) . . ?
N1 C1 C2 123.6(6) . . ?
N4 C15 C14 122.2(6) . . ?
N8 C30 C31 122.5(6) . . ?
C28 C27 C26 124.0(6) . . ?
C28 C27 C22 118.4(6) . . ?
C26 C27 C22 117.5(6) . . ?
N5 C44 C43 123.6(6) . . ?
N7 C31 C30 121.2(6) . . ?
N7 C31 C32 109.7(6) . . ?
C30 C31 C32 129.1(6) . . ?
C66 C65 C64 120.4(6) . . ?
C28 C29 C20 119.4(6) . . ?
C28 C29 C16 122.8(5) . . ?
C20 C29 C16 117.9(6) . . ?
C54 C55 N1 119.1(6) . . ?
C54 C55 C56 120.4(6) . . ?
N1 C55 C56 120.5(6) . . ?
N9 C63 C62 123.8(6) . . ?
N9 C59 C60 122.3(6) . . ?
C45 C46 C47 121.0(7) . . ?
C42 C43 N6 109.2(6) . . ?
C42 C43 C44 129.9(7) . . ?
N6 C43 C44 120.7(6) . . ?
C32 C33 C34 106.7(6) . . ?
C2 C3 C4 106.1(6) . . ?
C11 C6 C5 113.4(5) . . ?
C11 C6 C9 109.8(5) . . ?
C5 C6 C9 109.6(5) . . ?
C11 C6 C7 106.9(5) . . ?
C5 C6 C7 109.1(5) . . ?
C9 C6 C7 107.8(5) . . ?
C8 C7 C6 117.1(6) . . ?
C13 C12 C11 107.1(6) . . ?
C67 C68 C69 120.8(6) . . ?
C12 C13 C14 106.7(6) . . ?
C33 C32 C31 106.9(6) . . ?
C55 C54 C53 121.4(7) . . ?
C50 C51 C52 121.2(6) . . ?
C50 C51 C56 119.2(6) . . ?
C52 C51 C56 119.5(6) . . ?
C34 C35 C40 115.8(5) . . ?
C34 C35 C36 109.2(6) . . ?
C40 C35 C36 109.3(5) . . ?
C34 C35 C38 107.8(5) . . ?
C40 C35 C38 108.5(6) . . ?
C36 C35 C38 105.8(5) . . ?
C61 C62 C63 118.7(7) . . ?
C53 C52 C51 120.8(6) . . ?
C52 C53 C54 120.3(7) . . ?
C16 C17 C18 121.7(6) . . ?
C67 C66 C65 119.6(6) . . ?
C10 C9 C6 115.0(5) . . ?
C22 C21 C20 123.0(6) . . ?
C48 C47 C46 121.0(7) . . ?
C3 C4 C5 106.7(6) . . ?
C21 C20 C19 122.1(6) . . ?
C21 C20 C29 118.7(6) . . ?
C19 C20 C29 119.1(6) . . ?
C26 C25 C24 120.9(6) . . ?
C68 C67 C66 120.2(6) . . ?
C21 C22 C23 122.1(6) . . ?
C21 C22 C27 118.7(6) . . ?
C23 C22 C27 119.2(6) . . ?
C61 C60 C59 119.5(7) . . ?
C24 C23 C22 120.7(6) . . ?
C41 C42 C43 107.0(7) . . ?
C39 C38 C35 113.9(6) . . ?
C23 C24 C25 120.6(6) . . ?
C18 C19 C20 121.2(6) . . ?
C19 C18 C17 120.3(6) . . ?
C60 C61 C62 119.0(7) . . ?
C50 C49 C48 121.1(7) . . ?
C50 C49 C58 119.0(6) . . ?
C48 C49 C58 119.8(7) . . ?
C37 C36 C35 115.1(6) . . ?
C47 C48 C49 119.9(7) . . ?
C42 C41 C40 107.4(6) . . ?
C51 C50 C49 122.0(6) . . ?
Cl3 C200 Cl4 113.8(5) . . ?
Cl1 C100 Cl2 111.8(6) . . ?
C74A N10A C70A 120.0 . . ?
C74A N10A U2 116.4(10) . . ?
C70A N10A U2 122.9(10) . . ?
C73A C74A N10A 120.0 . . ?
C74A C73A C72A 120.0 . . ?
C71A C72A C73A 120.0 . . ?
C72A C71A C70A 120.0 . . ?
C71A C70A N10A 120.0 . . ?

_refine_diff_density_max         1.571
_refine_diff_density_min         -1.739
_refine_diff_density_rms         0.143


