# Supplementary Information (SI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 2024

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
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data_ihep_101
_database_code_depnum_ccdc_archive 'CCDC 2358409'
loop_
_audit_author_name
_audit_author_address
'Kong-Qiu Hu'
;Institute of High Energy Physics
China
;
_audit_update_record             
;
2024-05-27 deposited with the CCDC.	2024-08-05 downloaded from the CCDC.
;
_audit_creation_date             2024-05-27
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'C75 H80 N8 O37 U5, 3(C3 H7 N O), 2(C2 H8 N), 2(H), 0.5[]'
_chemical_formula_sum            'C124 H203 N25 O52 U5'
_chemical_formula_weight         4066.25
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
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                   45.847(6)
_cell_length_b                   29.165(4)
_cell_length_c                   14.8586(17)
_cell_angle_alpha                90
_cell_angle_beta                 107.195(4)
_cell_angle_gamma                90
_cell_volume                     18980(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9946
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      20.806
_cell_measurement_theta_min      2.657
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    4.325
_exptl_absorpt_correction_T_max  0.7446
_exptl_absorpt_correction_T_min  0.5333
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1075 before and 0.0894 after correction.
The Ratio of minimum to maximum transmission is 0.7162.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'yellowish yellow'
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.423
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             7992
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0945
_diffrn_reflns_av_unetI/netI     0.0675
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            30250
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        17.225
_diffrn_reflns_theta_max         17.225
_diffrn_reflns_theta_min         2.685
_diffrn_ambient_temperature      170.00
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4561
_reflns_number_total             5725
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.184
_refine_diff_density_min         -0.689
_refine_diff_density_rms         0.107
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     697
_refine_ls_number_reflns         5725
_refine_ls_number_restraints     985
_refine_ls_R_factor_all          0.0641
_refine_ls_R_factor_gt           0.0483
_refine_ls_restrained_S_all      0.986
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0667P)²+259.1652P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1199
_refine_ls_wR_factor_ref         0.1271
_refine_special_details          SQUEEZE
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 U1-O8
 1.75 with sigma of 0.01
 U2-O10
 1.75 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C38) \\sim Ueq, Uanis(C43) \\sim Ueq, Uanis(C44) \\sim Ueq, Uanis(O14)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O13) \\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(C41)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O6) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(O1) \\sim
Ueq, Uanis(O15) \\sim Ueq, Uanis(O5) \\sim Ueq, Uanis(O12) \\sim Ueq, Uanis(O3)
\\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C31) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C1) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C4) \\sim
Ueq, Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C8)
\\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C11) \\sim Ueq,
Uanis(C13) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C15)
\\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C19) \\sim Ueq,
Uanis(C18) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C22)
\\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C25) \\sim Ueq,
Uanis(C26) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C29)
\\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C32) \\sim Ueq,
Uanis(C33) \\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C36)
\\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(C38) \\sim Ueq, Uanis(C42) \\sim Ueq,
Uanis(C41) \\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C43)
\\sim Ueq, Uanis(C44) \\sim Ueq, Uanis(C45) \\sim Ueq, Uanis(C46) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: N6(0.5) O14(0.5) H(0.5) HA(0.5) C42(0.5) H42A(0.5) H42B(0.5)
 H42C(0.5) C43(0.5) H43A(0.5) H43B(0.5) H43C(0.5) C44(0.5) H44(0.5)
6.a Rotating group:
 O15(H,HA)
6.b Secondary CH2 refined with riding coordinates:
 N7(H7A,H7B), C10(H10A,H10B), C14(H14A,H14B), C33(H33A,H33B)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C9(H9), C15(H15), C20(H20), C22(H22), C26(H26), C30(H30),
 C32(H32), C36(H36), C40(H40), C44(H44)
6.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C13(H13A,H13B,H13C), C12(H12A,H12B,H12C), C19(H19A,H19B,
 H19C), C31(H31A,H31B,H31C), C35(H35A,H35B,H35C), C37(H37A,H37B,H37C), C38(H38A,
 H38B,H38C), C42(H42A,H42B,H42C), C41(H41A,H41B,H41C), C39(H39A,H39B,H39C),
 C43(H43A,H43B,H43C), C45(H45A,H45B,H45C), C46(H46A,H46B,H46C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.78550(2) 0.71940(3) 0.81071(5) 0.0552(4) Uani 1 1 d D . . . .
C1 C 0.8738(4) 0.5260(6) 0.9900(12) 0.027(4) Uani 1 1 d . U . . .
N1 N 0.8038(3) 0.6659(5) 0.7021(9) 0.043(4) Uani 1 1 d . . . . .
O1 O 0.7420(3) 0.7555(4) 0.8177(7) 0.057(3) Uani 1 1 d . U . . .
O3 O 0.8715(3) 0.6923(4) 1.0423(8) 0.064(4) Uani 1 1 d . U . . .
U3 U 0.500000 0.88368(4) -0.250000 0.0572(5) Uani 1 2 d S T P . .
C3 C 0.8743(4) 0.6092(6) 1.0184(11) 0.036(4) Uani 1 1 d . U . . .
H3 H 0.886556 0.604128 1.081359 0.043 Uiso 1 1 calc R U . . .
N3 N 0.5283(3) 0.9538(5) -0.1725(9) 0.039(4) Uani 1 1 d . . . . .
U2 U 0.62116(2) 0.93196(2) 0.44295(4) 0.0327(3) Uani 1 1 d D . . . .
C2 C 0.8666(4) 0.5712(6) 0.9559(11) 0.030(4) Uani 1 1 d . U . . .
N2 N 0.7394(4) 0.6980(5) 0.6653(9) 0.051(4) Uani 1 1 d . . . . .
O2 O 0.8360(3) 0.7030(4) 0.8700(7) 0.051(3) Uani 1 1 d . . . . .
O004 O 0.8883(2) 0.5167(3) 1.0758(7) 0.028(3) Uani 1 1 d . . . . .
N4 N 0.7791(4) 0.5142(6) 0.8661(12) 0.075(5) Uani 1 1 d . . . . .
C4 C 0.8489(4) 0.5804(6) 0.8634(11) 0.031(4) Uani 1 1 d . U . . .
H4 H 0.843333 0.555660 0.820259 0.037 Uiso 1 1 calc R U . . .
O4 O 0.7263(3) 0.8322(5) 0.8794(8) 0.074(4) Uani 1 1 d . U . . .
O005 O 0.5944(2) 0.9540(4) 0.2770(6) 0.033(3) Uani 1 1 d . . . . .
N5 N 0.8076(4) 0.7995(6) 1.0912(13) 0.084(6) Uani 1 1 d . . . . .
C5 C 0.8391(4) 0.6249(6) 0.8317(11) 0.037(4) Uani 1 1 d . U . . .
O5 O 0.5402(3) 0.8651(4) -0.1289(8) 0.065(4) Uani 1 1 d . U . . .
O006 O 0.8660(2) 0.4906(4) 0.9335(7) 0.035(3) Uani 1 1 d . . . . .
N6 N 0.6352(8) 0.7317(11) 0.384(2) 0.054(8) Uani 0.5 1 d . . P . .
C6 C 0.8454(4) 0.6612(6) 0.8963(12) 0.039(4) Uani 1 1 d . U . . .
O6 O 0.5584(3) 0.7984(5) -0.0038(9) 0.077(4) Uani 1 1 d . U . . .
O7 O 0.7946(3) 0.7665(4) 0.7510(9) 0.072(4) Uani 1 1 d . . . . .
N7 N 0.8810(3) 0.4643(5) 0.7732(9) 0.055(4) Uani 1 1 d . . . . .
H7A H 0.887512 0.490032 0.750186 0.065 Uiso 1 1 calc R U . . .
H7B H 0.878095 0.471830 0.829407 0.065 Uiso 1 1 calc R U . . .
C7 C 0.8645(4) 0.6528(6) 0.9909(12) 0.045(5) Uani 1 1 d . U . . .
O8 O 0.7758(3) 0.6700(3) 0.8654(8) 0.061(4) Uani 1 1 d D . . . .
C8 C 0.8907(5) 0.6846(7) 1.1374(12) 0.080(7) Uani 1 1 d . U . . .
H8A H 0.910333 0.671841 1.135857 0.120 Uiso 1 1 calc R U . . .
H8B H 0.880638 0.662948 1.169052 0.120 Uiso 1 1 calc R U . . .
H8C H 0.894138 0.713703 1.171779 0.120 Uiso 1 1 calc R U . . .
O009 O 0.6032(3) 0.8806(4) 0.3077(7) 0.043(3) Uani 1 1 d . . . . .
O9 O 0.6559(3) 0.9427(4) 0.4191(7) 0.045(3) Uani 1 1 d . . . . .
C9 C 0.8214(4) 0.6306(6) 0.7349(11) 0.038(5) Uani 1 1 d . U . . .
H9 H 0.822625 0.607212 0.691734 0.046 Uiso 1 1 calc R U . . .
O00B O 0.6482(2) 0.9031(4) 0.5950(7) 0.045(3) Uani 1 1 d . . . . .
O00D O 0.6401(3) 0.8531(4) 0.4854(7) 0.044(3) Uani 1 1 d . . . . .
O10 O 0.58577(19) 0.9244(3) 0.4670(7) 0.036(3) Uani 1 1 d D . . . .
C10 C 0.7907(4) 0.6718(6) 0.5974(11) 0.048(4) Uani 1 1 d . U . . .
H10A H 0.788322 0.704902 0.582430 0.058 Uiso 1 1 calc R U . . .
H10B H 0.805061 0.658912 0.565785 0.058 Uiso 1 1 calc R U . . .
O11 O 0.4773(3) 0.8851(4) -0.1748(8) 0.066(4) Uani 1 1 d . . . . .
C11 C 0.7605(4) 0.6488(6) 0.5598(12) 0.047(4) Uani 1 1 d . U . . .
C13 C 0.7441(4) 0.6741(7) 0.4645(11) 0.056(5) Uani 1 1 d . U . . .
H13A H 0.757105 0.672782 0.422711 0.084 Uiso 1 1 calc R U . . .
H13B H 0.740509 0.706231 0.477546 0.084 Uiso 1 1 calc R U . . .
H13C H 0.724570 0.659110 0.434054 0.084 Uiso 1 1 calc R U . . .
O13 O 0.7836(4) 0.4791(7) 0.7316(12) 0.132(7) Uani 1 1 d . U . . .
C12 C 0.7634(4) 0.5969(6) 0.5377(11) 0.058(5) Uani 1 1 d . U . . .
H12A H 0.743526 0.585370 0.499456 0.087 Uiso 1 1 calc R U . . .
H12B H 0.770076 0.579659 0.596818 0.087 Uiso 1 1 calc R U . . .
H12C H 0.778389 0.593259 0.502976 0.087 Uiso 1 1 calc R U . . .
O12 O 0.8008(3) 0.7570(5) 0.9609(9) 0.083(4) Uani 1 1 d . U . . .
C14 C 0.7406(4) 0.6524(6) 0.6258(11) 0.042(4) Uani 1 1 d . U . . .
H14A H 0.719524 0.642999 0.590711 0.050 Uiso 1 1 calc R U . . .
H14B H 0.748298 0.630456 0.678235 0.050 Uiso 1 1 calc R U . . .
O14 O 0.6609(6) 0.6701(9) 0.4460(18) 0.075(8) Uani 0.5 1 d . U P . .
C15 C 0.7150(5) 0.7217(6) 0.6311(12) 0.051(5) Uani 1 1 d . U . . .
H15 H 0.700101 0.709202 0.577940 0.062 Uiso 1 1 calc R U . . .
O15 O 0.500000 0.8014(8) -0.250000 0.103(7) Uani 1 2 d S TU P . .
H H 0.519529 0.758475 -0.176353 0.154 Uiso 0.5 1 d R U P . .
HA H 0.480479 0.758475 -0.323660 0.154 Uiso 0.5 1 d R U P . .
C16 C 0.7079(4) 0.7652(6) 0.6650(11) 0.039(4) Uani 1 1 d . U . . .
C17 C 0.7215(4) 0.7798(6) 0.7567(12) 0.043(5) Uani 1 1 d . U . . .
C19 C 0.7144(6) 0.8718(8) 0.9189(14) 0.097(8) Uani 1 1 d . U . . .
H19A H 0.714533 0.898972 0.880224 0.145 Uiso 1 1 calc R U . . .
H19B H 0.727292 0.877375 0.983452 0.145 Uiso 1 1 calc R U . . .
H19C H 0.693471 0.865388 0.919322 0.145 Uiso 1 1 calc R U . . .
C18 C 0.7122(4) 0.8204(7) 0.7877(13) 0.056(5) Uani 1 1 d . U . . .
C20 C 0.6917(4) 0.8486(7) 0.7250(12) 0.056(5) Uani 1 1 d . U . . .
H20 H 0.687536 0.878408 0.744201 0.067 Uiso 1 1 calc R U . . .
C21 C 0.6769(4) 0.8335(6) 0.6330(12) 0.041(4) Uani 1 1 d . U . . .
C22 C 0.6851(4) 0.7918(6) 0.6059(11) 0.034(4) Uani 1 1 d . U . . .
H22 H 0.674811 0.780665 0.544578 0.040 Uiso 1 1 calc R U . . .
C23 C 0.6545(4) 0.8646(7) 0.5700(13) 0.037(4) Uani 1 1 d . U . . .
C24 C 0.5924(4) 0.9113(6) 0.2499(12) 0.028(4) Uani 1 1 d . U . . .
C25 C 0.5773(4) 0.9009(6) 0.1499(11) 0.032(4) Uani 1 1 d . U . . .
C26 C 0.5663(3) 0.9342(6) 0.0853(11) 0.032(4) Uani 1 1 d . U . . .
H26 H 0.567573 0.965303 0.104859 0.039 Uiso 1 1 calc R U . . .
C27 C 0.5527(4) 0.9229(6) -0.0141(11) 0.036(4) Uani 1 1 d . U . . .
C28 C 0.5503(4) 0.8779(7) -0.0379(12) 0.047(5) Uani 1 1 d . U . . .
C29 C 0.5615(4) 0.8424(7) 0.0312(13) 0.056(5) Uani 1 1 d . U . . .
C30 C 0.5747(4) 0.8552(6) 0.1234(12) 0.041(4) Uani 1 1 d . U . . .
H30 H 0.582206 0.832277 0.169833 0.049 Uiso 1 1 calc R U . . .
C31 C 0.5740(5) 0.7625(7) 0.0585(13) 0.094(8) Uani 1 1 d . U . . .
H31A H 0.595966 0.764738 0.067412 0.140 Uiso 1 1 calc R U . . .
H31B H 0.566517 0.732621 0.030991 0.140 Uiso 1 1 calc R U . . .
H31C H 0.570005 0.765693 0.119500 0.140 Uiso 1 1 calc R U . . .
C32 C 0.5462(4) 0.9574(6) -0.0853(12) 0.043(5) Uani 1 1 d . U . . .
H32 H 0.555910 0.986228 -0.067895 0.052 Uiso 1 1 calc R U . . .
C33 C 0.5279(4) 0.9950(6) -0.2318(12) 0.050(5) Uani 1 1 d . U . . .
H33A H 0.529751 0.984729 -0.293398 0.060 Uiso 1 1 calc R U . . .
H33B H 0.546153 1.013733 -0.201309 0.060 Uiso 1 1 calc R U . . .
C34 C 0.500000 1.0256(9) -0.250000 0.045(6) Uani 1 2 d S TU P . .
C35 C 0.5014(4) 1.0550(6) -0.1649(10) 0.044(5) Uani 1 1 d . U . . .
H35A H 0.518296 1.076898 -0.154970 0.066 Uiso 1 1 calc R U . . .
H35B H 0.504750 1.035427 -0.109187 0.066 Uiso 1 1 calc R U . . .
H35C H 0.482163 1.071713 -0.175560 0.066 Uiso 1 1 calc R U . . .
C36 C 0.7916(6) 0.7844(8) 1.0085(16) 0.080(7) Uani 1 1 d . U . . .
H36 H 0.771388 0.795605 0.983442 0.095 Uiso 1 1 calc R U . . .
C37 C 0.7972(5) 0.8355(8) 1.1373(14) 0.090(7) Uani 1 1 d . U . . .
H37A H 0.808476 0.863592 1.133187 0.135 Uiso 1 1 calc R U . . .
H37B H 0.800622 0.827389 1.203577 0.135 Uiso 1 1 calc R U . . .
H37C H 0.775373 0.840453 1.107037 0.135 Uiso 1 1 calc R U . . .
C38 C 0.8361(6) 0.7771(10) 1.1371(19) 0.140(10) Uani 1 1 d . U . . .
H38A H 0.852407 0.790794 1.115590 0.210 Uiso 1 1 calc R U . . .
H38B H 0.834439 0.744368 1.121363 0.210 Uiso 1 1 calc R U . . .
H38C H 0.840892 0.780849 1.205422 0.210 Uiso 1 1 calc R U . . .
C42 C 0.6171(9) 0.7328(14) 0.439(3) 0.063(11) Uani 0.5 1 d . U P . .
H42A H 0.596303 0.740724 0.401710 0.094 Uiso 0.5 1 calc R U P . .
H42B H 0.624677 0.755798 0.488662 0.094 Uiso 0.5 1 calc R U P . .
H42C H 0.617070 0.702581 0.468064 0.094 Uiso 0.5 1 calc R U P . .
C41 C 0.7873(5) 0.5187(8) 0.9656(14) 0.088(7) Uani 1 1 d . U . . .
H41A H 0.800801 0.545226 0.985200 0.132 Uiso 1 1 calc R U . . .
H41B H 0.797961 0.490891 0.995083 0.132 Uiso 1 1 calc R U . . .
H41C H 0.768871 0.523010 0.985062 0.132 Uiso 1 1 calc R U . . .
C40 C 0.7898(6) 0.4828(9) 0.8229(19) 0.099(8) Uani 1 1 d . U . . .
H40 H 0.803226 0.460704 0.860541 0.119 Uiso 1 1 calc R U . . .
C39 C 0.7598(5) 0.5520(8) 0.8072(16) 0.099(8) Uani 1 1 d . U . . .
H39A H 0.755445 0.544622 0.740193 0.148 Uiso 1 1 calc R U . . .
H39B H 0.770856 0.581147 0.820559 0.148 Uiso 1 1 calc R U . . .
H39C H 0.740514 0.554667 0.822875 0.148 Uiso 1 1 calc R U . . .
C43 C 0.6294(8) 0.7622(11) 0.318(2) 0.036(8) Uani 0.5 1 d . U P . .
H43A H 0.648251 0.770021 0.302795 0.054 Uiso 0.5 1 calc R U P . .
H43B H 0.621189 0.789807 0.339175 0.054 Uiso 0.5 1 calc R U P . .
H43C H 0.614398 0.750073 0.261448 0.054 Uiso 0.5 1 calc R U P . .
C44 C 0.6551(9) 0.7007(14) 0.385(3) 0.056(9) Uani 0.5 1 d . U P . .
H44 H 0.665650 0.701120 0.338549 0.067 Uiso 0.5 1 calc R U P . .
C45 C 0.9048(4) 0.4303(7) 0.7898(12) 0.058(6) Uani 1 1 d . U . . .
H45A H 0.896231 0.400097 0.796366 0.087 Uiso 1 1 calc R U . . .
H45B H 0.920902 0.437795 0.847784 0.087 Uiso 1 1 calc R U . . .
H45C H 0.913289 0.429836 0.736664 0.087 Uiso 1 1 calc R U . . .
C46 C 0.8516(4) 0.4505(7) 0.7081(12) 0.063(6) Uani 1 1 d . U . . .
H46A H 0.852888 0.451335 0.643369 0.095 Uiso 1 1 calc R U . . .
H46B H 0.835684 0.471705 0.713874 0.095 Uiso 1 1 calc R U . . .
H46C H 0.846668 0.419372 0.723299 0.095 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 N1 2.559(14) . ?
U1 O1 2.284(12) . ?
U1 N2 2.612(15) . ?
U1 O2 2.273(12) . ?
U1 O7 1.750(13) . ?
U1 O8 1.774(8) . ?
U1 O12 2.399(13) . ?
C1 U2 2.905(17) 4_646 ?
C1 C2 1.41(2) . ?
C1 O004 1.280(17) . ?
C1 O006 1.313(18) . ?
N1 C9 1.309(19) . ?
N1 C10 1.504(19) . ?
O1 C17 1.306(18) . ?
O3 C7 1.366(19) . ?
O3 C8 1.444(19) . ?
U3 N3 2.512(14) . ?
U3 N3 2.512(14) 2_654 ?
U3 O5 2.229(12) . ?
U3 O5 2.229(12) 2_654 ?
U3 O11 1.737(13) . ?
U3 O11 1.737(13) 2_654 ?
U3 O15 2.40(2) . ?
C3 H3 0.9500 . ?
C3 C2 1.42(2) . ?
C3 C7 1.37(2) . ?
N3 C32 1.317(18) . ?
N3 C33 1.49(2) . ?
U2 O004 2.509(10) 4_656 ?
U2 O005 2.491(9) . ?
U2 O006 2.450(10) 4_656 ?
U2 O009 2.446(10) . ?
U2 O9 1.760(12) . ?
U2 O00B 2.385(10) . ?
U2 O00D 2.475(10) . ?
U2 O10 1.776(8) . ?
U2 C23 2.838(18) . ?
U2 C24 2.845(17) . ?
C2 C4 1.40(2) . ?
N2 C14 1.46(2) . ?
N2 C15 1.29(2) . ?
O2 C6 1.314(18) . ?
N4 C41 1.42(2) . ?
N4 C40 1.30(3) . ?
N4 C39 1.52(2) . ?
C4 H4 0.9500 . ?
C4 C5 1.41(2) . ?
O4 C19 1.47(2) . ?
O4 C18 1.369(19) . ?
O005 C24 1.305(18) . ?
N5 C36 1.31(2) . ?
N5 C37 1.41(2) . ?
N5 C38 1.44(3) . ?
C5 C6 1.40(2) . ?
C5 C9 1.44(2) . ?
O5 C28 1.346(19) . ?
N6 C42 1.33(4) . ?
N6 C43 1.29(4) . ?
N6 C44 1.28(4) . ?
C6 C7 1.44(2) . ?
O6 C29 1.38(2) . ?
O6 C31 1.44(2) . ?
N7 H7A 0.9100 . ?
N7 H7B 0.9100 . ?
N7 C45 1.44(2) . ?
N7 C46 1.46(2) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
O009 C24 1.236(17) . ?
C9 H9 0.9500 . ?
O00B C23 1.244(18) . ?
O00D C23 1.280(18) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C10 C11 1.49(2) . ?
C11 C13 1.58(2) . ?
C11 C12 1.56(2) . ?
C11 C14 1.53(2) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
O13 C40 1.31(2) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
O12 C36 1.22(2) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
O14 C44 1.25(4) . ?
C15 H15 0.9500 . ?
C15 C16 1.44(2) . ?
C16 C17 1.39(2) . ?
C16 C22 1.39(2) . ?
C17 C18 1.38(2) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C18 C20 1.38(2) . ?
C20 H20 0.9500 . ?
C20 C21 1.41(2) . ?
C21 C22 1.37(2) . ?
C21 C23 1.48(2) . ?
C22 H22 0.9500 . ?
C24 C25 1.47(2) . ?
C25 C26 1.35(2) . ?
C25 C30 1.38(2) . ?
C26 H26 0.9500 . ?
C26 C27 1.46(2) . ?
C27 C28 1.36(2) . ?
C27 C32 1.43(2) . ?
C28 C29 1.44(2) . ?
C29 C30 1.38(2) . ?
C30 H30 0.9500 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32 0.9500 . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C33 C34 1.52(2) . ?
C34 C35 1.51(2) . ?
C34 C35 1.51(2) 2_654 ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36 0.9500 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C40 H40 0.9500 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44 0.9500 . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 U1 N2 70.6(5) . . ?
O1 U1 N1 139.7(4) . . ?
O1 U1 N2 69.1(4) . . ?
O1 U1 O12 76.5(4) . . ?
O2 U1 N1 68.2(4) . . ?
O2 U1 O1 152.0(4) . . ?
O2 U1 N2 138.9(4) . . ?
O2 U1 O12 75.6(4) . . ?
O7 U1 N1 89.3(5) . . ?
O7 U1 O1 90.2(5) . . ?
O7 U1 N2 91.4(5) . . ?
O7 U1 O2 89.6(5) . . ?
O7 U1 O8 176.9(5) . . ?
O7 U1 O12 93.7(6) . . ?
O8 U1 N1 88.1(5) . . ?
O8 U1 O1 90.7(5) . . ?
O8 U1 N2 86.2(5) . . ?
O8 U1 O2 91.0(5) . . ?
O8 U1 O12 89.4(5) . . ?
O12 U1 N1 143.7(5) . . ?
O12 U1 N2 145.3(5) . . ?
C2 C1 U2 171.3(12) . 4_646 ?
O004 C1 U2 59.5(8) . 4_646 ?
O004 C1 C2 123.5(16) . . ?
O004 C1 O006 115.6(15) . . ?
O006 C1 U2 56.9(8) . 4_646 ?
O006 C1 C2 120.9(15) . . ?
C9 N1 U1 121.7(11) . . ?
C9 N1 C10 119.4(14) . . ?
C10 N1 U1 118.5(10) . . ?
C17 O1 U1 132.7(11) . . ?
C7 O3 C8 113.0(14) . . ?
N3 U3 N3 71.0(6) 2_654 . ?
O5 U3 N3 68.6(4) . . ?
O5 U3 N3 139.5(4) . 2_654 ?
O5 U3 N3 139.5(4) 2_654 . ?
O5 U3 N3 68.6(4) 2_654 2_654 ?
O5 U3 O5 151.9(6) 2_654 . ?
O5 U3 O15 75.9(3) 2_654 . ?
O5 U3 O15 75.9(3) . . ?
O11 U3 N3 90.7(5) 2_654 2_654 ?
O11 U3 N3 90.7(5) . . ?
O11 U3 N3 87.1(5) 2_654 . ?
O11 U3 N3 87.1(5) . 2_654 ?
O11 U3 O5 90.8(5) 2_654 . ?
O11 U3 O5 90.9(5) . 2_654 ?
O11 U3 O5 89.8(5) 2_654 2_654 ?
O11 U3 O5 89.8(5) . . ?
O11 U3 O11 177.3(9) 2_654 . ?
O11 U3 O15 91.4(4) . . ?
O11 U3 O15 91.4(4) 2_654 . ?
O15 U3 N3 144.5(3) . 2_654 ?
O15 U3 N3 144.5(3) . . ?
C2 C3 H3 118.9 . . ?
C7 C3 H3 118.9 . . ?
C7 C3 C2 122.2(15) . . ?
C32 N3 U3 127.1(12) . . ?
C32 N3 C33 114.4(14) . . ?
C33 N3 U3 118.1(10) . . ?
O004 U2 C1 26.1(3) 4_656 4_656 ?
O004 U2 C23 142.8(4) 4_656 . ?
O004 U2 C24 94.8(4) 4_656 . ?
O005 U2 C1 93.5(4) . 4_656 ?
O005 U2 O004 67.5(3) . 4_656 ?
O005 U2 C23 147.9(5) . . ?
O005 U2 C24 27.3(4) . . ?
O006 U2 C1 26.7(4) 4_656 4_656 ?
O006 U2 O004 52.5(3) 4_656 4_656 ?
O006 U2 O005 120.0(3) 4_656 . ?
O006 U2 O00D 118.0(3) 4_656 . ?
O006 U2 C23 91.3(5) 4_656 . ?
O006 U2 C24 147.2(4) 4_656 . ?
O009 U2 C1 146.4(4) . 4_656 ?
O009 U2 O004 120.4(3) . 4_656 ?
O009 U2 O005 52.9(3) . . ?
O009 U2 O006 172.4(4) . 4_656 ?
O009 U2 O00D 69.4(3) . . ?
O009 U2 C23 96.1(5) . . ?
O009 U2 C24 25.6(4) . . ?
O9 U2 C1 85.2(5) . 4_656 ?
O9 U2 O004 86.5(4) . 4_656 ?
O9 U2 O005 88.0(4) . . ?
O9 U2 O006 89.7(4) . 4_656 ?
O9 U2 O009 92.8(4) . . ?
O9 U2 O00B 90.3(4) . . ?
O9 U2 O00D 86.9(5) . . ?
O9 U2 O10 176.9(5) . . ?
O9 U2 C23 85.1(5) . . ?
O9 U2 C24 90.7(5) . . ?
O00B U2 C1 92.4(4) . 4_656 ?
O00B U2 O004 118.5(4) . 4_656 ?
O00B U2 O005 173.7(4) . . ?
O00B U2 O006 66.0(4) . 4_656 ?
O00B U2 O009 121.1(4) . . ?
O00B U2 O00D 52.1(4) . . ?
O00B U2 C23 25.7(4) . . ?
O00B U2 C24 146.7(5) . . ?
O00D U2 C1 143.6(4) . 4_656 ?
O00D U2 O004 168.5(3) . 4_656 ?
O00D U2 O005 121.7(3) . . ?
O00D U2 C23 26.8(4) . . ?
O00D U2 C24 94.8(4) . . ?
O10 U2 C1 91.9(5) . 4_656 ?
O10 U2 O004 90.4(4) . 4_656 ?
O10 U2 O005 91.2(4) . . ?
O10 U2 O006 88.1(4) . 4_656 ?
O10 U2 O009 89.1(4) . . ?
O10 U2 O00B 90.9(4) . . ?
O10 U2 O00D 96.0(4) . . ?
O10 U2 C23 97.1(5) . . ?
O10 U2 C24 89.9(5) . . ?
C23 U2 C1 117.0(5) . 4_656 ?
C23 U2 C24 121.4(5) . . ?
C24 U2 C1 120.8(5) . 4_656 ?
C1 C2 C3 120.3(14) . . ?
C1 C2 C4 122.5(15) . . ?
C4 C2 C3 116.8(15) . . ?
C14 N2 U1 115.7(10) . . ?
C15 N2 U1 126.5(13) . . ?
C15 N2 C14 117.4(16) . . ?
C6 O2 U1 121.1(11) . . ?
C1 O004 U2 94.5(9) . 4_646 ?
C41 N4 C39 117.5(19) . . ?
C40 N4 C41 124(2) . . ?
C40 N4 C39 118(2) . . ?
C2 C4 H4 118.6 . . ?
C2 C4 C5 122.8(15) . . ?
C5 C4 H4 118.6 . . ?
C18 O4 C19 118.1(14) . . ?
C24 O005 U2 91.6(9) . . ?
C36 N5 C37 122(2) . . ?
C36 N5 C38 118(2) . . ?
C37 N5 C38 120(2) . . ?
C6 C5 C4 119.0(15) . . ?
C6 C5 C9 122.7(16) . . ?
C9 C5 C4 118.2(15) . . ?
C28 O5 U3 134.5(11) . . ?
C1 O006 U2 96.4(9) . 4_646 ?
C42 N6 C43 115(4) . . ?
C42 N6 C44 125(4) . . ?
C44 N6 C43 119(4) . . ?
O2 C6 C5 121.0(15) . . ?
O2 C6 C7 119.9(15) . . ?
C5 C6 C7 118.9(16) . . ?
C29 O6 C31 117.3(14) . . ?
H7A N7 H7B 107.5 . . ?
C45 N7 H7A 108.5 . . ?
C45 N7 H7B 108.5 . . ?
C45 N7 C46 115.2(15) . . ?
C46 N7 H7A 108.5 . . ?
C46 N7 H7B 108.5 . . ?
O3 C7 C3 127.8(15) . . ?
O3 C7 C6 112.2(15) . . ?
C3 C7 C6 120.0(16) . . ?
O3 C8 H8A 109.5 . . ?
O3 C8 H8B 109.5 . . ?
O3 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C24 O009 U2 95.5(10) . . ?
N1 C9 C5 124.6(16) . . ?
N1 C9 H9 117.7 . . ?
C5 C9 H9 117.7 . . ?
C23 O00B U2 97.9(10) . . ?
C23 O00D U2 92.6(10) . . ?
N1 C10 H10A 109.1 . . ?
N1 C10 H10B 109.1 . . ?
H10A C10 H10B 107.9 . . ?
C11 C10 N1 112.3(15) . . ?
C11 C10 H10A 109.1 . . ?
C11 C10 H10B 109.1 . . ?
C10 C11 C13 105.6(15) . . ?
C10 C11 C12 112.8(16) . . ?
C10 C11 C14 113.2(14) . . ?
C12 C11 C13 108.2(13) . . ?
C14 C11 C13 109.1(15) . . ?
C14 C11 C12 107.8(15) . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C36 O12 U1 141.4(15) . . ?
N2 C14 C11 114.8(15) . . ?
N2 C14 H14A 108.6 . . ?
N2 C14 H14B 108.6 . . ?
C11 C14 H14A 108.6 . . ?
C11 C14 H14B 108.6 . . ?
H14A C14 H14B 107.5 . . ?
N2 C15 H15 116.7 . . ?
N2 C15 C16 126.6(18) . . ?
C16 C15 H15 116.7 . . ?
C17 C16 C15 122.2(16) . . ?
C22 C16 C15 118.5(16) . . ?
C22 C16 C17 119.1(16) . . ?
O1 C17 C16 122.5(16) . . ?
O1 C17 C18 117.7(16) . . ?
C18 C17 C16 119.8(17) . . ?
O4 C19 H19A 109.5 . . ?
O4 C19 H19B 109.5 . . ?
O4 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
O4 C18 C17 116.4(16) . . ?
O4 C18 C20 123.3(17) . . ?
C17 C18 C20 120.1(17) . . ?
C18 C20 H20 119.9 . . ?
C18 C20 C21 120.3(17) . . ?
C21 C20 H20 119.9 . . ?
C20 C21 C23 117.9(16) . . ?
C22 C21 C20 118.1(16) . . ?
C22 C21 C23 124.0(16) . . ?
C16 C22 H22 118.9 . . ?
C21 C22 C16 122.1(16) . . ?
C21 C22 H22 118.9 . . ?
O00B C23 U2 56.4(9) . . ?
O00B C23 O00D 115.6(16) . . ?
O00B C23 C21 123.0(16) . . ?
O00D C23 U2 60.6(9) . . ?
O00D C23 C21 121.4(16) . . ?
C21 C23 U2 169.3(13) . . ?
O005 C24 U2 61.1(8) . . ?
O005 C24 C25 118.5(15) . . ?
O009 C24 U2 58.8(8) . . ?
O009 C24 O005 119.9(15) . . ?
O009 C24 C25 121.6(16) . . ?
C25 C24 U2 179.3(14) . . ?
C26 C25 C24 122.2(16) . . ?
C26 C25 C30 120.4(15) . . ?
C30 C25 C24 117.4(15) . . ?
C25 C26 H26 119.5 . . ?
C25 C26 C27 120.9(16) . . ?
C27 C26 H26 119.5 . . ?
C28 C27 C26 117.3(16) . . ?
C28 C27 C32 120.5(16) . . ?
C32 C27 C26 121.6(16) . . ?
O5 C28 C29 117.5(16) . . ?
C27 C28 O5 120.4(17) . . ?
C27 C28 C29 121.7(17) . . ?
O6 C29 C28 115.1(16) . . ?
C30 C29 O6 126.6(17) . . ?
C30 C29 C28 118.3(17) . . ?
C25 C30 H30 119.3 . . ?
C29 C30 C25 121.4(17) . . ?
C29 C30 H30 119.3 . . ?
O6 C31 H31A 109.5 . . ?
O6 C31 H31B 109.5 . . ?
O6 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
N3 C32 C27 127.2(17) . . ?
N3 C32 H32 116.4 . . ?
C27 C32 H32 116.4 . . ?
N3 C33 H33A 108.2 . . ?
N3 C33 H33B 108.2 . . ?
N3 C33 C34 116.3(15) . . ?
H33A C33 H33B 107.4 . . ?
C34 C33 H33A 108.2 . . ?
C34 C33 H33B 108.2 . . ?
C33 C34 C33 108(2) 2_654 . ?
C35 C34 C33 111.0(9) 2_654 2_654 ?
C35 C34 C33 107.9(10) 2_654 . ?
C35 C34 C33 107.9(10) . 2_654 ?
C35 C34 C33 111.0(9) . . ?
C35 C34 C35 111(2) 2_654 . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
N5 C36 H36 117.6 . . ?
O12 C36 N5 125(2) . . ?
O12 C36 H36 117.6 . . ?
N5 C37 H37A 109.5 . . ?
N5 C37 H37B 109.5 . . ?
N5 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
N5 C38 H38A 109.5 . . ?
N5 C38 H38B 109.5 . . ?
N5 C38 H38C 109.5 . . ?
H38A C38 H38B 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
N6 C42 H42A 109.5 . . ?
N6 C42 H42B 109.5 . . ?
N6 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
N4 C41 H41A 109.5 . . ?
N4 C41 H41B 109.5 . . ?
N4 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
N4 C40 O13 125(3) . . ?
N4 C40 H40 117.4 . . ?
O13 C40 H40 117.4 . . ?
N4 C39 H39A 109.5 . . ?
N4 C39 H39B 109.5 . . ?
N4 C39 H39C 109.5 . . ?
H39A C39 H39B 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
N6 C43 H43A 109.5 . . ?
N6 C43 H43B 109.5 . . ?
N6 C43 H43C 109.5 . . ?
H43A C43 H43B 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
N6 C44 H44 119.5 . . ?
O14 C44 N6 121(4) . . ?
O14 C44 H44 119.5 . . ?
N7 C45 H45A 109.5 . . ?
N7 C45 H45B 109.5 . . ?
N7 C45 H45C 109.5 . . ?
H45A C45 H45B 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
N7 C46 H46A 109.5 . . ?
N7 C46 H46B 109.5 . . ?
N7 C46 H46C 109.5 . . ?
H46A C46 H46B 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
U1 N1 C9 C5 -18(2) . . . . ?
U1 N1 C10 C11 -82.1(16) . . . . ?
U1 O1 C17 C16 49(3) . . . . ?
U1 O1 C17 C18 -134.3(16) . . . . ?
U1 N2 C14 C11 -81.1(15) . . . . ?
U1 N2 C15 C16 0(3) . . . . ?
U1 O2 C6 C5 61(2) . . . . ?
U1 O2 C6 C7 -123.8(15) . . . . ?
U1 O12 C36 N5 -176.8(16) . . . . ?
C1 C2 C4 C5 173.5(16) . . . . ?
N1 C10 C11 C13 157.0(14) . . . . ?
N1 C10 C11 C12 -85.0(18) . . . . ?
N1 C10 C11 C14 38(2) . . . . ?
O1 C17 C18 O4 3(3) . . . . ?
O1 C17 C18 C20 176.7(18) . . . . ?
U3 N3 C32 C27 -3(3) . . . . ?
U3 N3 C33 C34 82.2(15) . . . . ?
U3 O5 C28 C27 -50(3) . . . . ?
U3 O5 C28 C29 136.8(15) . . . . ?
C3 C2 C4 C5 0(2) . . . . ?
N3 C33 C34 C33 -40.9(11) . . . 2_654 ?
N3 C33 C34 C35 -161.1(14) . . . 2_654 ?
N3 C33 C34 C35 77(2) . . . . ?
U2 O005 C24 O009 -0.7(16) . . . . ?
U2 O005 C24 C25 179.4(13) . . . . ?
U2 O009 C24 O005 0.7(16) . . . . ?
U2 O009 C24 C25 -179.4(14) . . . . ?
U2 O00B C23 O00D -13.2(17) . . . . ?
U2 O00B C23 C21 167.2(15) . . . . ?
U2 O00D C23 O00B 12.6(16) . . . . ?
U2 O00D C23 C21 -167.8(15) . . . . ?
C2 C1 O004 U2 170.3(14) . . . 4_646 ?
C2 C1 O006 U2 -170.0(14) . . . 4_646 ?
C2 C3 C7 O3 -176.4(17) . . . . ?
C2 C3 C7 C6 1(3) . . . . ?
C2 C4 C5 C6 -4(3) . . . . ?
C2 C4 C5 C9 179.1(15) . . . . ?
N2 C15 C16 C17 -22(3) . . . . ?
N2 C15 C16 C22 162.2(18) . . . . ?
O2 C6 C7 O3 -2(2) . . . . ?
O2 C6 C7 C3 179.9(17) . . . . ?
O004 C1 C2 C3 -3(2) . . . . ?
O004 C1 C2 C4 -175.4(15) . . . . ?
O004 C1 O006 U2 10.4(14) . . . 4_646 ?
C4 C5 C6 O2 -178.5(16) . . . . ?
C4 C5 C6 C7 7(3) . . . . ?
C4 C5 C9 N1 159.8(17) . . . . ?
O4 C18 C20 C21 -177.2(18) . . . . ?
O005 C24 C25 C26 2(2) . . . . ?
O005 C24 C25 C30 -178.3(15) . . . . ?
C5 C6 C7 O3 172.8(16) . . . . ?
C5 C6 C7 C3 -5(3) . . . . ?
O5 C28 C29 O6 -5(3) . . . . ?
O5 C28 C29 C30 173.6(17) . . . . ?
O006 C1 C2 C3 177.9(15) . . . . ?
O006 C1 C2 C4 5(2) . . . . ?
O006 C1 O004 U2 -10.1(14) . . . 4_646 ?
C6 C5 C9 N1 -17(3) . . . . ?
O6 C29 C30 C25 178.3(18) . . . . ?
C7 C3 C2 C1 -172.0(17) . . . . ?
C7 C3 C2 C4 1(3) . . . . ?
C8 O3 C7 C3 -2(3) . . . . ?
C8 O3 C7 C6 180.0(16) . . . . ?
O009 C24 C25 C26 -177.6(16) . . . . ?
O009 C24 C25 C30 2(2) . . . . ?
C9 N1 C10 C11 90(2) . . . . ?
C9 C5 C6 O2 -2(3) . . . . ?
C9 C5 C6 C7 -177.1(17) . . . . ?
C10 N1 C9 C5 169.8(16) . . . . ?
C10 C11 C14 N2 45(2) . . . . ?
C13 C11 C14 N2 -71.9(19) . . . . ?
C12 C11 C14 N2 170.8(14) . . . . ?
C14 N2 C15 C16 173.9(17) . . . . ?
C15 N2 C14 C11 104.8(19) . . . . ?
C15 C16 C17 O1 1(3) . . . . ?
C15 C16 C17 C18 -175.1(19) . . . . ?
C15 C16 C22 C21 179.8(17) . . . . ?
C16 C17 C18 O4 179.0(17) . . . . ?
C16 C17 C18 C20 -7(3) . . . . ?
C17 C16 C22 C21 4(3) . . . . ?
C17 C18 C20 C21 9(3) . . . . ?
C19 O4 C18 C17 -172.2(19) . . . . ?
C19 O4 C18 C20 14(3) . . . . ?
C18 C20 C21 C22 -5(3) . . . . ?
C18 C20 C21 C23 178.1(18) . . . . ?
C20 C21 C22 C16 -2(3) . . . . ?
C20 C21 C23 U2 83(7) . . . . ?
C20 C21 C23 O00B 0(3) . . . . ?
C20 C21 C23 O00D -179.7(16) . . . . ?
C22 C16 C17 O1 176.5(17) . . . . ?
C22 C16 C17 C18 0(3) . . . . ?
C22 C21 C23 U2 -94(7) . . . . ?
C22 C21 C23 O00B -177.3(18) . . . . ?
C22 C21 C23 O00D 3(3) . . . . ?
C23 C21 C22 C16 175.0(17) . . . . ?
C24 C25 C26 C27 177.1(15) . . . . ?
C24 C25 C30 C29 -178.4(17) . . . . ?
C25 C26 C27 C28 3(2) . . . . ?
C25 C26 C27 C32 -168.3(16) . . . . ?
C26 C25 C30 C29 1(3) . . . . ?
C26 C27 C28 O5 -174.7(15) . . . . ?
C26 C27 C28 C29 -2(3) . . . . ?
C26 C27 C32 N3 -163.9(16) . . . . ?
C27 C28 C29 O6 -178.0(18) . . . . ?
C27 C28 C29 C30 0(3) . . . . ?
C28 C27 C32 N3 25(3) . . . . ?
C28 C29 C30 C25 0(3) . . . . ?
C30 C25 C26 C27 -2(3) . . . . ?
C31 O6 C29 C28 169.2(18) . . . . ?
C31 O6 C29 C30 -9(3) . . . . ?
C32 N3 C33 C34 -103.6(17) . . . . ?
C32 C27 C28 O5 -4(3) . . . . ?
C32 C27 C28 C29 169.3(17) . . . . ?
C33 N3 C32 C27 -176.1(17) . . . . ?
C37 N5 C36 O12 172(2) . . . . ?
C38 N5 C36 O12 -11(4) . . . . ?
C42 N6 C44 O14 -6(6) . . . . ?
C41 N4 C40 O13 -177(2) . . . . ?
C39 N4 C40 O13 -5(4) . . . . ?
C43 N6 C44 O14 -178(3) . . . . ?

_platon_squeeze_details          ?
_platon_squeeze_special_details  
;
A solvent mask was calculated and 1912 electrons were 
found in a volume of 8920Å³ in 1 void per unit cell. 
This is consistent with the presence of 
12[C3H7ON] per Asymmetric Unit 
which account for 1920 electrons 
per unit cell.
;
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 -0.004 4460 956 '24 C3H7ON'
2 0.500 0.500 0.552 4460 956 '24 C3H7ON'

_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'

# start Validation Reply Form

_vrf_THETM01_ihep_101            
;
PROBLEM:  The value of sine(theta_max)/wavelength is less than 0.550
            Calculated sin(theta_max)/wavelength =    0.4166
RESPONSE: A full set of data was collected, however the very high
 angle data was dominated by noise [I/sigma(I) < 1.0] and was 
omitted. This arbitrary theta limit is inappropriate for highly 
disordered structures. It would rule out all macromolecular 
structures. A limit on data / parameter ratio's that properly takes
 into account the number of restraints / constraints and the 
redundancy of the measurements would be more appropriate. 
We are confident the structural characterization is valid.
;
# end Validation Reply Form

# start Validation Reply Form

_vrf_PLAT342_ihep_101            
;
PROBLEM:   Low Bond Precision on  C-C Bonds ...............    0.0229 Ang. 
RESPONSE: This alert is generated because of the disorder structure.
;
# end Validation Reply Form

# start Validation Reply Form
_vrf_PLAT910_ihep_101            
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         21 Note   
RESPONSE: Theta min = 2.657 deg. The theta value of the missing
 reflections are less than 2.657 deg. And therefore reflections were excluded.
;
# end Validation Reply Form


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

data_IHEP_102
_database_code_depnum_ccdc_archive 'CCDC 2358410'
loop_
_audit_author_name
_audit_author_address
'Kong-Qiu Hu'
;Institute of High Energy Physics
China
;
_audit_update_record             
;
2024-05-27 deposited with the CCDC.	2024-08-05 downloaded from the CCDC.
;
_audit_creation_date             2024-05-27
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C26 H30 N4 O14 U2'
_chemical_formula_sum            'C26 H30 N4 O14 U2'
_chemical_formula_weight         1098.60
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   17.9735(15)
_cell_length_b                   14.9023(13)
_cell_length_c                   12.2543(9)
_cell_angle_alpha                90
_cell_angle_beta                 96.152(3)
_cell_angle_gamma                90
_cell_volume                     3263.4(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9959
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      27.46
_cell_measurement_theta_min      2.73
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    9.984
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4981
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1273 before and 0.0823 after correction.
The Ratio of minimum to maximum transmission is 0.6681.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.236
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       rhombohedral
_exptl_crystal_F_000             2040
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0870
_diffrn_reflns_av_unetI/netI     0.0283
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            57937
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        20.813
_diffrn_reflns_theta_max         20.813
_diffrn_reflns_theta_min         2.524
_diffrn_ambient_temperature      170.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2814
_reflns_number_total             3407
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.389
_refine_diff_density_min         -0.697
_refine_diff_density_rms         0.120
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     421
_refine_ls_number_reflns         3407
_refine_ls_number_restraints     420
_refine_ls_R_factor_all          0.0421
_refine_ls_R_factor_gt           0.0290
_refine_ls_restrained_S_all      0.995
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0212P)²+35.2187P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0632
_refine_ls_wR_factor_ref         0.0702
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 U2-O3
 1.75 with sigma of 0.01
3. Rigid bond restraints
 U2, O14
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.005
 U2, O11
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.005
4. Uiso/Uaniso restraints and constraints
U2 \\sim O14: within 2A with sigma of 0.007 and sigma for terminal atoms of
0.001 within 2A
U2 \\sim O11: within 2A with sigma of 0.007 and sigma for terminal atoms of
0.001 within 2A
Uanis(C25) \\sim Ueq, Uanis(N4) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C26)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O12) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C11(H11A,H11B)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C9(H9), C12(H12), C14(H14), C21(H21), C24(H24), C17(H17)
6.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C19(H19A,H19B,H19C), C22(H22A,H22B,H22C), C23(H23A,H23B,
 H23C), C26(H26A,H26B,H26C), C25(H25A,H25B,H25C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.51096(2) 0.35178(2) 0.72010(3) 0.02637(14) Uani 1 1 d . . . . .
C1 C 0.8480(6) 0.3164(9) 0.7157(10) 0.059(4) Uani 1 1 d . . . . .
H1A H 0.848346 0.295117 0.640114 0.089 Uiso 1 1 calc R U . . .
H1B H 0.872902 0.272147 0.766416 0.089 Uiso 1 1 calc R U . . .
H1C H 0.874652 0.373752 0.724489 0.089 Uiso 1 1 calc R U . . .
O1 O 0.5105(4) 0.4705(5) 0.7216(6) 0.0469(19) Uani 1 1 d . . . . .
N1 N 0.5306(4) 0.3707(5) 0.9303(6) 0.0285(19) Uani 1 1 d . . . . .
U2 U 0.02036(2) 0.54053(3) 0.71852(4) 0.04646(16) Uani 1 1 d D U . . .
C2 C 0.7616(5) 0.3561(7) 0.8413(8) 0.032(2) Uani 1 1 d . . . . .
O2 O 0.5067(3) 0.2329(4) 0.7271(6) 0.0356(16) Uani 1 1 d . . . . .
N2 N 0.3891(4) 0.3463(6) 0.8094(6) 0.0331(19) Uani 1 1 d . . . . .
O3 O 0.0335(4) 0.6442(5) 0.6622(7) 0.067(2) Uani 1 1 d D . . . .
C3 C 0.8168(6) 0.3764(6) 0.9234(8) 0.034(2) Uani 1 1 d . . . . .
H3 H 0.867626 0.371858 0.909522 0.041 Uiso 1 1 calc R U . . .
N3 N 0.6416(5) 0.3682(6) 0.4236(7) 0.039(2) Uani 1 1 d . . . . .
N4 N -0.0914(8) 0.6788(10) 0.9543(12) 0.100(4) Uani 1 1 d . U . . .
O4 O 0.0073(4) 0.4336(6) 0.7754(8) 0.074(3) Uani 1 1 d . . . . .
C4 C 0.8000(5) 0.4037(7) 1.0274(8) 0.035(2) Uani 1 1 d . . . . .
O6 O 0.4119(4) 0.3521(6) 0.5885(5) 0.049(2) Uani 1 1 d . . . . .
C6 C 0.7256(5) 0.4080(7) 1.0479(8) 0.032(2) Uani 1 1 d . . . . .
H6 H 0.713640 0.426027 1.118244 0.038 Uiso 1 1 calc R U . . .
O5 O 0.6335(3) 0.3419(5) 0.7813(5) 0.0362(17) Uani 1 1 d . . . . .
C5 C 0.8604(6) 0.4253(8) 1.1170(9) 0.042(3) Uani 1 1 d . . . . .
O7 O 0.3621(4) 0.3920(5) 0.3848(6) 0.051(2) Uani 1 1 d . . . . .
C7 C 0.6672(5) 0.3858(6) 0.9652(8) 0.029(2) Uani 1 1 d . . . . .
O9 O 0.8471(4) 0.4600(6) 1.2051(6) 0.052(2) Uani 1 1 d . . . . .
C9 C 0.5905(5) 0.3844(7) 0.9943(8) 0.032(2) Uani 1 1 d . . . . .
H9 H 0.584470 0.394908 1.069304 0.038 Uiso 1 1 calc R U . . .
O8 O 0.7733(3) 0.3281(5) 0.7391(5) 0.0435(19) Uani 1 1 d . . . . .
C8 C 0.6853(5) 0.3614(6) 0.8600(8) 0.025(2) Uani 1 1 d . . . . .
O10 O 0.9273(4) 0.4086(6) 1.1010(6) 0.061(2) Uani 1 1 d . . . . .
C10 C 0.4604(5) 0.3780(8) 0.9850(8) 0.039(3) Uani 1 1 d . . . . .
H10A H 0.470009 0.358938 1.062580 0.047 Uiso 1 1 calc R U . . .
H10B H 0.442923 0.441041 0.983257 0.047 Uiso 1 1 calc R U . . .
O11 O 0.0880(4) 0.4774(6) 0.4047(7) 0.059(2) Uani 1 1 d . . . . .
C11 C 0.4024(5) 0.3195(8) 0.9256(8) 0.040(3) Uani 1 1 d . . . . .
H11A H 0.419226 0.256173 0.930588 0.048 Uiso 1 1 calc R U . . .
H11B H 0.355281 0.324217 0.960208 0.048 Uiso 1 1 calc R U . . .
O12 O 0.0757(4) 0.4728(6) 0.5819(7) 0.064(2) Uani 1 1 d . U . . .
C12 C 0.3205(5) 0.3607(7) 0.7673(8) 0.033(2) Uani 1 1 d . . . . .
H12 H 0.282904 0.357389 0.816070 0.039 Uiso 1 1 calc R U . . .
O13 O 0.5683(4) 0.3447(6) 0.5567(6) 0.053(2) Uani 1 1 d . . . . .
C13 C 0.2957(5) 0.3811(7) 0.6545(8) 0.032(2) Uani 1 1 d . . . . .
O14 O -0.0782(5) 0.5987(9) 0.8121(9) 0.104(4) Uani 1 1 d . U . . .
C14 C 0.2203(5) 0.4079(7) 0.6304(9) 0.036(2) Uani 1 1 d . . . . .
H14 H 0.188761 0.410444 0.687833 0.043 Uiso 1 1 calc R U . . .
C15 C 0.1914(5) 0.4307(7) 0.5241(9) 0.038(2) Uani 1 1 d . . . . .
C16 C 0.1132(6) 0.4631(8) 0.5021(11) 0.048(3) Uani 1 1 d . . . . .
C18 C 0.3114(6) 0.3986(7) 0.4600(8) 0.036(2) Uani 1 1 d . . . . .
C19 C 0.3348(7) 0.4095(9) 0.2730(9) 0.065(4) Uani 1 1 d . . . . .
H19A H 0.374576 0.397946 0.226012 0.097 Uiso 1 1 calc R U . . .
H19B H 0.319066 0.472395 0.265300 0.097 Uiso 1 1 calc R U . . .
H19C H 0.292033 0.370351 0.250982 0.097 Uiso 1 1 calc R U . . .
C20 C 0.3425(5) 0.3775(7) 0.5700(8) 0.031(2) Uani 1 1 d . . . . .
C21 C 0.5774(6) 0.3677(8) 0.4602(9) 0.049(3) Uani 1 1 d . . . . .
H21 H 0.534852 0.385441 0.412368 0.059 Uiso 1 1 calc R U . . .
C22 C 0.7082(6) 0.3470(8) 0.4926(10) 0.055(3) Uani 1 1 d . . . . .
H22A H 0.736370 0.301154 0.457128 0.083 Uiso 1 1 calc R U . . .
H22B H 0.694997 0.324211 0.563001 0.083 Uiso 1 1 calc R U . . .
H22C H 0.738889 0.401136 0.505039 0.083 Uiso 1 1 calc R U . . .
C23 C 0.6475(8) 0.3890(9) 0.3099(9) 0.066(4) Uani 1 1 d . . . . .
H23A H 0.662397 0.334990 0.272012 0.099 Uiso 1 1 calc R U . . .
H23B H 0.685205 0.435964 0.305096 0.099 Uiso 1 1 calc R U . . .
H23C H 0.599016 0.410082 0.275206 0.099 Uiso 1 1 calc R U . . .
C24 C -0.0945(10) 0.6131(14) 0.9022(17) 0.109(4) Uani 1 1 d . U . . .
H24 H -0.113256 0.562521 0.937681 0.131 Uiso 1 1 calc R U . . .
C26 C -0.1145(9) 0.7005(11) 1.0656(13) 0.100(4) Uani 1 1 d . U . . .
H26A H -0.150305 0.750309 1.059178 0.150 Uiso 1 1 calc R U . . .
H26B H -0.070339 0.717663 1.115112 0.150 Uiso 1 1 calc R U . . .
H26C H -0.137948 0.647669 1.095035 0.150 Uiso 1 1 calc R U . . .
C25 C -0.0456(11) 0.7526(14) 0.9061(17) 0.136(6) Uani 1 1 d . U . . .
H25A H -0.040507 0.738959 0.828978 0.204 Uiso 1 1 calc R U . . .
H25B H 0.004155 0.755738 0.947338 0.204 Uiso 1 1 calc R U . . .
H25C H -0.071083 0.810362 0.910929 0.204 Uiso 1 1 calc R U . . .
C17 C 0.2384(6) 0.4246(7) 0.4403(9) 0.037(2) Uani 1 1 d . . . . .
H17 H 0.218730 0.438986 0.367313 0.044 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 1.770(7) . ?
U1 N1 2.577(7) . ?
U1 O2 1.776(6) . ?
U1 N2 2.553(7) . ?
U1 O6 2.270(6) . ?
U1 O5 2.254(6) . ?
U1 O13 2.351(7) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C1 O8 1.414(12) . ?
N1 C9 1.279(12) . ?
N1 C10 1.495(12) . ?
U2 O3 1.719(7) . ?
U2 O4 1.765(8) . ?
U2 C5 2.827(11) 3_667 ?
U2 O9 2.465(7) 3_667 ?
U2 O10 2.431(7) 3_667 ?
U2 O11 2.349(7) 3_566 ?
U2 O12 2.274(8) . ?
U2 O14 2.374(10) . ?
C2 C3 1.368(13) . ?
C2 O8 1.357(11) . ?
C2 C8 1.417(13) . ?
N2 C11 1.474(12) . ?
N2 C12 1.302(12) . ?
C3 H3 0.9500 . ?
C3 C4 1.402(14) . ?
N3 C21 1.282(13) . ?
N3 C22 1.424(14) . ?
N3 C23 1.443(13) . ?
N4 C24 1.17(2) . ?
N4 C26 1.502(19) . ?
N4 C25 1.53(2) . ?
C4 C6 1.388(14) . ?
C4 C5 1.494(15) . ?
O6 C20 1.301(11) . ?
C6 H6 0.9500 . ?
C6 C7 1.417(13) . ?
O5 C8 1.299(11) . ?
C5 O9 1.243(12) . ?
C5 O10 1.264(12) . ?
O7 C18 1.368(12) . ?
O7 C19 1.429(12) . ?
C7 C9 1.460(14) . ?
C7 C8 1.410(13) . ?
C9 H9 0.9500 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C10 C11 1.488(14) . ?
O11 C16 1.248(14) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
O12 C16 1.254(14) . ?
C12 H12 0.9500 . ?
C12 C13 1.438(14) . ?
O13 C21 1.258(12) . ?
C13 C14 1.414(13) . ?
C13 C20 1.403(14) . ?
O14 C24 1.193(19) . ?
C14 H14 0.9500 . ?
C14 C15 1.392(14) . ?
C15 C16 1.483(15) . ?
C15 C17 1.400(15) . ?
C18 C20 1.437(14) . ?
C18 C17 1.366(14) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C21 H21 0.9500 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24 0.9500 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C17 H17 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 U1 N1 83.1(3) . . ?
O1 U1 O2 175.4(3) . . ?
O1 U1 N2 91.3(3) . . ?
O1 U1 O6 90.1(3) . . ?
O1 U1 O5 93.8(3) . . ?
O1 U1 O13 93.3(3) . . ?
O2 U1 N1 93.6(3) . . ?
O2 U1 N2 84.5(3) . . ?
O2 U1 O6 90.1(3) . . ?
O2 U1 O5 88.0(3) . . ?
O2 U1 O13 91.2(3) . . ?
N2 U1 N1 66.9(2) . . ?
O6 U1 N1 136.3(2) . . ?
O6 U1 N2 70.2(2) . . ?
O6 U1 O13 77.1(2) . . ?
O5 U1 N1 69.5(2) . . ?
O5 U1 N2 135.1(2) . . ?
O5 U1 O6 154.2(2) . . ?
O5 U1 O13 77.2(2) . . ?
O13 U1 N1 146.1(2) . . ?
O13 U1 N2 147.0(2) . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O8 C1 H1A 109.5 . . ?
O8 C1 H1B 109.5 . . ?
O8 C1 H1C 109.5 . . ?
C9 N1 U1 130.3(6) . . ?
C9 N1 C10 114.1(8) . . ?
C10 N1 U1 115.1(5) . . ?
O3 U2 O4 179.5(5) . . ?
O3 U2 C5 89.9(3) . 3_667 ?
O3 U2 O9 89.2(3) . 3_667 ?
O3 U2 O10 91.6(3) . 3_667 ?
O3 U2 O11 89.1(3) . 3_566 ?
O3 U2 O12 90.8(4) . . ?
O3 U2 O14 90.4(4) . . ?
O4 U2 C5 90.2(3) . 3_667 ?
O4 U2 O9 90.6(3) . 3_667 ?
O4 U2 O10 88.7(4) . 3_667 ?
O4 U2 O11 90.9(3) . 3_566 ?
O4 U2 O12 88.7(4) . . ?
O4 U2 O14 90.1(5) . . ?
O9 U2 C5 26.0(3) 3_667 3_667 ?
O10 U2 C5 26.5(3) 3_667 3_667 ?
O10 U2 O9 52.5(2) 3_667 3_667 ?
O11 U2 C5 172.9(3) 3_566 3_667 ?
O11 U2 O9 160.9(3) 3_566 3_667 ?
O11 U2 O10 146.5(3) 3_566 3_667 ?
O11 U2 O14 75.0(3) 3_566 . ?
O12 U2 C5 104.3(3) . 3_667 ?
O12 U2 O9 78.3(2) . 3_667 ?
O12 U2 O10 130.6(2) . 3_667 ?
O12 U2 O11 82.8(3) . 3_566 ?
O12 U2 O14 157.8(3) . . ?
O14 U2 C5 97.9(3) . 3_667 ?
O14 U2 O9 124.0(3) . 3_667 ?
O14 U2 O10 71.5(3) . 3_667 ?
C3 C2 C8 120.4(9) . . ?
O8 C2 C3 125.1(9) . . ?
O8 C2 C8 114.5(8) . . ?
C11 N2 U1 111.3(5) . . ?
C12 N2 U1 130.1(6) . . ?
C12 N2 C11 118.5(8) . . ?
C2 C3 H3 119.2 . . ?
C2 C3 C4 121.6(9) . . ?
C4 C3 H3 119.2 . . ?
C21 N3 C22 121.4(9) . . ?
C21 N3 C23 120.1(11) . . ?
C22 N3 C23 118.5(9) . . ?
C24 N4 C26 132.4(18) . . ?
C24 N4 C25 112.8(17) . . ?
C26 N4 C25 114.2(15) . . ?
C3 C4 C5 121.4(9) . . ?
C6 C4 C3 118.9(9) . . ?
C6 C4 C5 119.7(9) . . ?
C20 O6 U1 142.1(6) . . ?
C4 C6 H6 119.5 . . ?
C4 C6 C7 120.9(9) . . ?
C7 C6 H6 119.5 . . ?
C8 O5 U1 146.0(6) . . ?
C4 C5 U2 176.9(8) . 3_667 ?
O9 C5 U2 60.5(5) . 3_667 ?
O9 C5 C4 122.4(9) . . ?
O9 C5 O10 119.5(10) . . ?
O10 C5 U2 59.0(5) . 3_667 ?
O10 C5 C4 118.1(10) . . ?
C18 O7 C19 116.6(9) . . ?
C6 C7 C9 118.3(9) . . ?
C8 C7 C6 119.2(9) . . ?
C8 C7 C9 122.4(9) . . ?
C5 O9 U2 93.5(6) . 3_667 ?
N1 C9 C7 127.4(9) . . ?
N1 C9 H9 116.3 . . ?
C7 C9 H9 116.3 . . ?
C2 O8 C1 118.0(8) . . ?
O5 C8 C2 119.8(8) . . ?
O5 C8 C7 121.2(8) . . ?
C7 C8 C2 119.0(9) . . ?
C5 O10 U2 94.5(6) . 3_667 ?
N1 C10 H10A 110.0 . . ?
N1 C10 H10B 110.0 . . ?
H10A C10 H10B 108.4 . . ?
C11 C10 N1 108.6(8) . . ?
C11 C10 H10A 110.0 . . ?
C11 C10 H10B 110.0 . . ?
C16 O11 U2 141.9(8) . 3_566 ?
N2 C11 C10 110.2(8) . . ?
N2 C11 H11A 109.6 . . ?
N2 C11 H11B 109.6 . . ?
C10 C11 H11A 109.6 . . ?
C10 C11 H11B 109.6 . . ?
H11A C11 H11B 108.1 . . ?
C16 O12 U2 159.9(9) . . ?
N2 C12 H12 116.6 . . ?
N2 C12 C13 126.7(9) . . ?
C13 C12 H12 116.6 . . ?
C21 O13 U1 154.3(8) . . ?
C14 C13 C12 116.8(9) . . ?
C20 C13 C12 123.6(9) . . ?
C20 C13 C14 119.6(9) . . ?
C24 O14 U2 141.6(12) . . ?
C13 C14 H14 119.4 . . ?
C15 C14 C13 121.1(10) . . ?
C15 C14 H14 119.4 . . ?
C14 C15 C16 120.1(10) . . ?
C14 C15 C17 118.5(9) . . ?
C17 C15 C16 121.4(10) . . ?
O11 C16 O12 123.7(10) . . ?
O11 C16 C15 118.0(11) . . ?
O12 C16 C15 118.2(10) . . ?
O7 C18 C20 113.4(8) . . ?
C17 C18 O7 126.8(9) . . ?
C17 C18 C20 119.8(9) . . ?
O7 C19 H19A 109.5 . . ?
O7 C19 H19B 109.5 . . ?
O7 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
O6 C20 C13 121.5(9) . . ?
O6 C20 C18 119.7(9) . . ?
C13 C20 C18 118.7(9) . . ?
N3 C21 H21 118.6 . . ?
O13 C21 N3 122.9(11) . . ?
O13 C21 H21 118.6 . . ?
N3 C22 H22A 109.5 . . ?
N3 C22 H22B 109.5 . . ?
N3 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
N3 C23 H23A 109.5 . . ?
N3 C23 H23B 109.5 . . ?
N3 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
N4 C24 O14 131(2) . . ?
N4 C24 H24 114.5 . . ?
O14 C24 H24 114.5 . . ?
N4 C26 H26A 109.5 . . ?
N4 C26 H26B 109.5 . . ?
N4 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
N4 C25 H25A 109.5 . . ?
N4 C25 H25B 109.5 . . ?
N4 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C15 C17 H17 118.9 . . ?
C18 C17 C15 122.1(10) . . ?
C18 C17 H17 118.9 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
U1 N1 C9 C7 -5.6(15) . . . . ?
U1 N1 C10 C11 35.2(10) . . . . ?
U1 N2 C11 C10 53.2(10) . . . . ?
U1 N2 C12 C13 2.3(16) . . . . ?
U1 O6 C20 C13 -30.8(17) . . . . ?
U1 O6 C20 C18 152.1(8) . . . . ?
U1 O5 C8 C2 -164.0(8) . . . . ?
U1 O5 C8 C7 17.6(17) . . . . ?
U1 O13 C21 N3 146.0(13) . . . . ?
N1 C10 C11 N2 -58.5(11) . . . . ?
U2 O11 C16 O12 -39(2) 3_566 . . . ?
U2 O11 C16 C15 139.6(10) 3_566 . . . ?
U2 O12 C16 O11 -83(2) . . . . ?
U2 O12 C16 C15 99(2) . . . . ?
U2 O14 C24 N4 98(3) . . . . ?
C2 C3 C4 C6 1.6(16) . . . . ?
C2 C3 C4 C5 179.7(10) . . . . ?
N2 C12 C13 C14 -170.4(10) . . . . ?
N2 C12 C13 C20 8.2(17) . . . . ?
C3 C2 O8 C1 1.8(16) . . . . ?
C3 C2 C8 O5 -180.0(9) . . . . ?
C3 C2 C8 C7 -1.5(15) . . . . ?
C3 C4 C6 C7 -0.4(15) . . . . ?
C3 C4 C5 O9 170.9(11) . . . . ?
C3 C4 C5 O10 -8.0(17) . . . . ?
C4 C6 C7 C9 175.0(9) . . . . ?
C4 C6 C7 C8 -1.8(15) . . . . ?
C4 C5 O9 U2 178.7(10) . . . 3_667 ?
C4 C5 O10 U2 -178.7(9) . . . 3_667 ?
C6 C4 C5 O9 -11.0(17) . . . . ?
C6 C4 C5 O10 170.1(10) . . . . ?
C6 C7 C9 N1 176.0(10) . . . . ?
C6 C7 C8 C2 2.7(14) . . . . ?
C6 C7 C8 O5 -178.9(9) . . . . ?
C5 C4 C6 C7 -178.5(10) . . . . ?
O7 C18 C20 O6 -2.2(14) . . . . ?
O7 C18 C20 C13 -179.4(9) . . . . ?
O7 C18 C17 C15 -178.8(10) . . . . ?
O9 C5 O10 U2 2.4(12) . . . 3_667 ?
C9 N1 C10 C11 -151.9(9) . . . . ?
C9 C7 C8 C2 -174.0(9) . . . . ?
C9 C7 C8 O5 4.5(15) . . . . ?
O8 C2 C3 C4 -179.0(10) . . . . ?
O8 C2 C8 O5 -1.5(14) . . . . ?
O8 C2 C8 C7 177.0(8) . . . . ?
C8 C2 C3 C4 -0.7(16) . . . . ?
C8 C2 O8 C1 -176.6(10) . . . . ?
C8 C7 C9 N1 -7.3(16) . . . . ?
O10 C5 O9 U2 -2.4(12) . . . 3_667 ?
C10 N1 C9 C7 -177.2(10) . . . . ?
C11 N2 C12 C13 -175.3(10) . . . . ?
C12 N2 C11 C10 -128.7(10) . . . . ?
C12 C13 C14 C15 178.7(9) . . . . ?
C12 C13 C20 O6 2.4(16) . . . . ?
C12 C13 C20 C18 179.5(10) . . . . ?
C13 C14 C15 C16 -176.9(10) . . . . ?
C13 C14 C15 C17 1.4(15) . . . . ?
C14 C13 C20 O6 -179.1(10) . . . . ?
C14 C13 C20 C18 -2.0(14) . . . . ?
C14 C15 C16 O11 -175.5(10) . . . . ?
C14 C15 C16 O12 3.0(16) . . . . ?
C14 C15 C17 C18 -1.2(16) . . . . ?
C16 C15 C17 C18 177.1(10) . . . . ?
C19 O7 C18 C20 178.3(10) . . . . ?
C19 O7 C18 C17 -3.5(16) . . . . ?
C20 C13 C14 C15 0.1(15) . . . . ?
C20 C18 C17 C15 -0.7(16) . . . . ?
C22 N3 C21 O13 -3.4(18) . . . . ?
C23 N3 C21 O13 175.4(11) . . . . ?
C26 N4 C24 O14 176.8(17) . . . . ?
C25 N4 C24 O14 -13(3) . . . . ?
C17 C15 C16 O11 6.2(16) . . . . ?
C17 C15 C16 O12 -175.3(10) . . . . ?
C17 C18 C20 O6 179.5(10) . . . . ?
C17 C18 C20 C13 2.3(15) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'

# start Validation Reply Form

_vrf_THETM01_IHEP_102            
;
PROBLEM:  The value of sine(theta_max)/wavelength is less than 0.550
            Calculated sin(theta_max)/wavelength =    0.4999
RESPONSE: A full set of data was collected, however the very high
 angle data was dominated by noise [I/sigma(I) < 1.0] and was 
omitted. This arbitrary theta limit is inappropriate for highly 
disordered structures. It would rule out all macromolecular 
structures. A limit on data / parameter ratio's that properly takes
 into account the number of restraints / constraints and the 
redundancy of the measurements would be more appropriate. 
We are confident the structural characterization is valid.
;
# end Validation Reply Form
