# Supplementary Information (SI) for RSC Advances.
# This journal is © The Royal Society of Chemistry 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. 
# 
#######################################################################

data_hbpu
_database_code_depnum_ccdc_archive 'CCDC 2329479'
loop_
_audit_author_name
_audit_author_address
'Naveen Kulkarni'
;Amrita Vishwa Vidyapeetham
India
;
_audit_update_record             
;
2024-01-29 deposited with the CCDC.	2024-10-10 downloaded from the CCDC.
;

_vrf_PLAT241_hbpu                
;
PROBLEM: High   'MainMol' Ueq as Compared to Neighbors of       O1_3 Check
RESPONSE:
All the atoms of the acetate residue vibrates near perpendicular to the 
molecular plane. It does not warrant disorder modelling.

Excerpt from shelxl lst file.
Principal mean square atomic displacements U;
0.2200   0.0442   0.0268   O1_3;
0.1224   0.0569   0.0255   O2_3;
0.1104   0.0289   0.0149   C1_3;
0.2065   0.0705   0.0394   C2_3;
;

_vrf_PLAT420_hbpu                
;
PROBLEM: D-H Bond Without Acceptor  O8       --H8B      .     Please Check
RESPONSE:
Both hydrogens(H8A & H8B) bonded to O8 were found from difference Fourier.
Initially refined with the following DFIX cards.

  DFIX 0.95 O7 H7A O7 H7B O8 H8A O8 H8B;
  DFIX 1.4 H7A H7B H8A H8B;

Hydrogen H8A forms a hydrogen bond with O2 but H8B do not have an acceptor.
Hence H8B position was fixed, in such a way that it forms interaction with 
O3_#.

d(O8-H8B) = 0.97(2)A;
d(H8B...O3_#) = 2.816(7)A;
d(O8...O3_#) = 3.55(2)A;
angle(O8-H8B...O3_#) = 133.1(12)deg;

#: x, -y+1/2, z-1/2;

U(iso) value of hydrogen atoms blow up, when refined freely.
Hence fixed at 1.5 times to that of the parent atom.

Hydrogen atom positions were defined less precisely than other heavy atoms
in x-ray studies. Consider hydrogen locations with pinch of salt in hand.
;

_vrf_PLAT971_hbpu                
;
PROBLEM: Check Calcd Resid. Dens.  0.94Ang From U1              2.62 eA-3
RESPONSE:
There is no chemically sensible species corresponding to this residual density
peak. A similar trend was observed around both the heavy atoms U1 and U2. We
ascribe this to absorption effects.

Please compare the following alerts.

971_ALERT_2_C Check Calcd Resid. Dens.  0.98Ang From U2              2.26 eA-3;
971_ALERT_2_C Check Calcd Resid. Dens.  0.87Ang From U1              2.10 eA-3;
971_ALERT_2_C Check Calcd Resid. Dens.  1.05Ang From U2              1.95 eA-3;
971_ALERT_2_C Check Calcd Resid. Dens.  0.93Ang From U1              1.83 eA-3;
971_ALERT_2_C Check Calcd Resid. Dens.  0.83Ang From U2              1.63 eA-3;
971_ALERT_2_C Check Calcd Resid. Dens.  1.02Ang From U1              1.54 eA-3;
972_ALERT_2_C Check Calcd Resid. Dens.  0.57Ang From U1             -1.69 eA-3;
;

_vrf_PLAT973_hbpu                
;
PROBLEM: Check Calcd Positive Resid. Density on        U2       1.63 eA-3

RESPONSE: 
This is not due to incorrect atom type assignment. Full-matrix 
least squares refinement was converged and no damping(DAMP) was employed
in refinement cycles.

_refine_ls_shift/su_max           0.001 
_refine_ls_shift/su_mean          0.000 
;

_audit_creation_method           SHELXL-2019/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C18 H26 N8 O18 U4, 2(C7 H8 N4), 2(H2 O)'
_chemical_formula_sum            'C32 H46 N16 O20 U4'
_chemical_formula_weight         1926.97

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           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                   12.2065(13)
_cell_length_b                   15.7058(16)
_cell_length_c                   14.4096(15)
_cell_angle_alpha                90
_cell_angle_beta                 104.927(4)
_cell_angle_gamma                90
_cell_volume                     2669.3(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    300(2)
_cell_measurement_reflns_used    9928
_cell_measurement_theta_min      2.16
_cell_measurement_theta_max      25.60

_exptl_crystal_description       tabular
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    2.397
_exptl_crystal_F_000             1756
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.290
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.070
_exptl_absorpt_coefficient_mu    12.180
_shelx_estimated_absorpt_T_min   0.126
_shelx_estimated_absorpt_T_max   0.483
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.2952
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   SADABS-2016/2
_diffrn_ambient_temperature      300(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            48435
_diffrn_reflns_av_unetI/netI     0.0720
_diffrn_reflns_av_R_equivalents  0.0872
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.159
_diffrn_reflns_theta_max         28.322
_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
_reflns_number_total             6653
_reflns_number_gt                4679
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0341P)²+21.0671P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6653
_refine_ls_number_parameters     334
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0870
_refine_ls_R_factor_gt           0.0509
_refine_ls_wR_factor_ref         0.1048
_refine_ls_wR_factor_gt          0.0934
_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
U1 U 0.60634(3) 0.30904(2) 0.62024(3) 0.03158(11) Uani 1 1 d . . . . .
U2 U 0.63487(3) 0.55976(2) 0.52468(2) 0.02401(10) Uani 1 1 d . . . . .
O1 O 0.5578(5) 0.4319(4) 0.5416(5) 0.0351(15) Uani 1 1 d . . . . .
O2 O 0.6586(7) 0.2665(5) 0.5263(6) 0.060(2) Uani 1 1 d . . . . .
O3 O 0.5582(7) 0.3432(4) 0.7198(5) 0.0487(19) Uani 1 1 d . . . . .
O4 O 0.6284(6) 0.5941(5) 0.6417(4) 0.0408(17) Uani 1 1 d . . . . .
O5 O 0.6554(6) 0.5319(4) 0.4096(4) 0.0406(17) Uani 1 1 d . . . . .
O6 O 0.5824(5) 0.6993(4) 0.4667(5) 0.0389(17) Uani 1 1 d . . . . .
O7 O 0.8072(6) 0.6540(5) 0.5545(5) 0.0369(16) Uani 1 1 d D . . . .
H7A H 0.835(10) 0.669(7) 0.501(6) 0.09(4) Uiso 1 1 d D . . . .
H7B H 0.789(16) 0.710(3) 0.569(11) 0.17(8) Uiso 1 1 d D . . . .
O8 O 0.7763(19) 0.1259(13) 0.4335(15) 0.237(10) Uani 1 1 d . . . . .
H8A H 0.743855 0.182502 0.434961 0.356 Uiso 1 1 d . U . . .
H8B H 0.707769 0.102096 0.392644 0.356 Uiso 1 1 d . U . . .
N1_1 N 0.5306(7) 0.1574(5) 0.6399(5) 0.0349(19) Uani 1 1 d . . . . .
N2_1 N 0.5385(6) 0.1156(4) 0.7236(5) 0.0266(17) Uani 1 1 d . . . . .
N3_1 N 0.7188(6) 0.1626(5) 0.8135(5) 0.0276(17) Uani 1 1 d . . . . .
N4_1 N 0.7484(7) 0.2138(5) 0.7486(6) 0.041(2) Uani 1 1 d . . . . .
C1_1 C 0.4892(8) 0.0374(6) 0.7086(7) 0.038(2) Uani 1 1 d . . . . .
H1_1 H 0.485811 -0.002679 0.755234 0.045 Uiso 1 1 calc R U . . .
C2_1 C 0.4461(9) 0.0294(7) 0.6126(8) 0.045(3) Uani 1 1 d . . . . .
H2_1 H 0.406570 -0.016782 0.579866 0.054 Uiso 1 1 calc R U . . .
C3_1 C 0.4735(9) 0.1047(7) 0.5732(7) 0.047(3) Uani 1 1 d . . . . .
H3_1 H 0.453942 0.116606 0.507784 0.056 Uiso 1 1 calc R U . . .
C4_1 C 0.8587(9) 0.2052(7) 0.7638(8) 0.049(3) Uani 1 1 d . . . . .
H4_1 H 0.902531 0.233238 0.729297 0.059 Uiso 1 1 calc R U . . .
C5_1 C 0.9013(9) 0.1479(7) 0.8393(8) 0.051(3) Uani 1 1 d . . . . .
H5_1 H 0.976109 0.130693 0.863534 0.062 Uiso 1 1 calc R U . . .
C6_1 C 0.8102(8) 0.1236(6) 0.8687(7) 0.038(2) Uani 1 1 d . . . . .
H6_1 H 0.810606 0.086093 0.918774 0.046 Uiso 1 1 calc R U . . .
C7_1 C 0.6000(7) 0.1541(6) 0.8130(6) 0.028(2) Uani 1 1 d . . . . .
H7A_1 H 0.593038 0.118845 0.866467 0.033 Uiso 1 1 calc R U . . .
H7B_1 H 0.568377 0.209659 0.819901 0.033 Uiso 1 1 calc R U . . .
N1_2 N 0.7676(9) 0.8090(7) 0.6319(7) 0.060(3) Uani 1 1 d . . . . .
N2_2 N 0.7370(7) 0.8326(6) 0.7130(6) 0.047(2) Uani 1 1 d . . . . .
N3_2 N 0.8132(8) 0.7258(7) 0.8313(6) 0.050(2) Uani 1 1 d . . . . .
N4_2 N 0.8839(8) 0.7655(7) 0.9080(7) 0.056(3) Uani 1 1 d . . . . .
C1_2 C 0.7350(10) 0.9168(8) 0.7199(9) 0.059(3) Uani 1 1 d . . . . .
H1_2 H 0.716878 0.946805 0.769555 0.070 Uiso 1 1 calc R U . . .
C2_2 C 0.7631(11) 0.9522(8) 0.6438(9) 0.060(3) Uani 1 1 d . . . . .
H2_2 H 0.766786 1.009622 0.629024 0.073 Uiso 1 1 calc R U . . .
C3_2 C 0.7849(11) 0.8826(9) 0.5936(9) 0.060(3) Uani 1 1 d . . . . .
H3_2 H 0.809456 0.886841 0.537797 0.072 Uiso 1 1 calc R U . . .
C4_2 C 0.9686(11) 0.7112(9) 0.9401(8) 0.062(4) Uani 1 1 d . . . . .
H4_2 H 1.029272 0.720801 0.993188 0.074 Uiso 1 1 calc R U . . .
C5_2 C 0.9546(13) 0.6384(10) 0.8840(10) 0.079(4) Uani 1 1 d . . . . .
H5_2 H 1.002480 0.591442 0.890709 0.094 Uiso 1 1 calc R U . . .
C6_2 C 0.8542(12) 0.6514(10) 0.8164(10) 0.076(4) Uani 1 1 d . . . . .
H6_2 H 0.820518 0.613520 0.767814 0.091 Uiso 1 1 calc R U . . .
C7_2 C 0.7131(10) 0.7682(8) 0.7752(8) 0.057(3) Uani 1 1 d . . . . .
H7A_2 H 0.663024 0.726218 0.736727 0.068 Uiso 1 1 calc R U . . .
H7B_2 H 0.673339 0.793966 0.818340 0.068 Uiso 1 1 calc R U . . .
O1_3 O 0.7774(7) 0.3816(6) 0.6857(8) 0.097(4) Uani 1 1 d . . . . .
O2_3 O 0.8042(7) 0.4794(5) 0.5896(7) 0.068(3) Uani 1 1 d . . . . .
C1_3 C 0.8410(8) 0.4289(7) 0.6546(9) 0.051(3) Uani 1 1 d . . . . .
C2_3 C 0.9652(11) 0.4272(10) 0.7023(13) 0.105(6) Uani 1 1 d . . . . .
H2A_3 H 1.007043 0.426389 0.654363 0.158 Uiso 1 1 calc R U . . .
H2B_3 H 0.982854 0.377167 0.741636 0.158 Uiso 1 1 calc R U . . .
H2C_3 H 0.985331 0.476964 0.741720 0.158 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 O3 1.768(7) . ?
U1 O2 1.769(7) . ?
U1 O1 2.240(6) . ?
U1 O6 2.326(6) 3_666 ?
U1 O1_3 2.353(8) . ?
U1 N1_1 2.596(8) . ?
U1 N4_1 2.648(8) . ?
U1 U2 3.7561(5) 3_666 ?
U2 O4 1.791(6) . ?
U2 O5 1.794(6) . ?
U2 O1 2.257(6) . ?
U2 O1 2.303(6) 3_666 ?
U2 O6 2.374(6) . ?
U2 O2_3 2.396(7) . ?
U2 O7 2.517(6) . ?
U2 U2 3.6965(7) 3_666 ?
O7 H7A 0.94(2) . ?
O7 H7B 0.95(2) . ?
O8 H8A 0.97(2) . ?
O8 H8B 0.966(19) . ?
N1_1 C3_1 1.322(12) . ?
N1_1 N2_1 1.355(10) . ?
N2_1 C1_1 1.360(11) . ?
N2_1 C7_1 1.445(11) . ?
N3_1 C6_1 1.340(11) . ?
N3_1 N4_1 1.352(10) . ?
N3_1 C7_1 1.455(11) . ?
N4_1 C4_1 1.313(12) . ?
C1_1 C2_1 1.353(14) . ?
C1_1 H1_1 0.9300 . ?
C2_1 C3_1 1.389(14) . ?
C2_1 H2_1 0.9300 . ?
C3_1 H3_1 0.9300 . ?
C4_1 C5_1 1.404(15) . ?
C4_1 H4_1 0.9300 . ?
C5_1 C6_1 1.344(14) . ?
C5_1 H5_1 0.9300 . ?
C6_1 H6_1 0.9300 . ?
C7_1 H7A_1 0.9700 . ?
C7_1 H7B_1 0.9700 . ?
N1_2 C3_2 1.321(15) . ?
N1_2 N2_2 1.366(12) . ?
N2_2 C1_2 1.326(14) . ?
N2_2 C7_2 1.429(15) . ?
N3_2 C6_2 1.311(16) . ?
N3_2 N4_2 1.365(12) . ?
N3_2 C7_2 1.443(14) . ?
N4_2 C4_2 1.328(15) . ?
C1_2 C2_2 1.351(17) . ?
C1_2 H1_2 0.9300 . ?
C2_2 C3_2 1.375(16) . ?
C2_2 H2_2 0.9300 . ?
C3_2 H3_2 0.9300 . ?
C4_2 C5_2 1.385(17) . ?
C4_2 H4_2 0.9300 . ?
C5_2 C6_2 1.371(18) . ?
C5_2 H5_2 0.9300 . ?
C6_2 H6_2 0.9300 . ?
C7_2 H7A_2 0.9700 . ?
C7_2 H7B_2 0.9700 . ?
O1_3 C1_3 1.238(13) . ?
O2_3 C1_3 1.221(12) . ?
C1_3 C2_3 1.495(16) . ?
C2_3 H2A_3 0.9600 . ?
C2_3 H2B_3 0.9600 . ?
C2_3 H2C_3 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 U1 O2 175.0(3) . . ?
O3 U1 O1 92.8(3) . . ?
O2 U1 O1 92.2(3) . . ?
O3 U1 O6 87.9(3) . 3_666 ?
O2 U1 O6 94.0(3) . 3_666 ?
O1 U1 O6 71.3(2) . 3_666 ?
O3 U1 O1_3 88.5(4) . . ?
O2 U1 O1_3 91.8(4) . . ?
O1 U1 O1_3 83.0(3) . . ?
O6 U1 O1_3 153.8(3) 3_666 . ?
O3 U1 N1_1 89.3(3) . . ?
O2 U1 N1_1 86.9(3) . . ?
O1 U1 N1_1 142.2(2) . . ?
O6 U1 N1_1 71.1(2) 3_666 . ?
O1_3 U1 N1_1 134.8(3) . . ?
O3 U1 N4_1 84.2(3) . . ?
O2 U1 N4_1 91.2(3) . . ?
O1 U1 N4_1 151.7(2) . . ?
O6 U1 N4_1 136.4(2) 3_666 . ?
O1_3 U1 N4_1 68.9(3) . . ?
N1_1 U1 N4_1 66.0(2) . . ?
O3 U1 U2 84.7(2) . 3_666 ?
O2 U1 U2 99.6(2) . 3_666 ?
O1 U1 U2 34.77(15) . 3_666 ?
O6 U1 U2 37.38(15) 3_666 3_666 ?
O1_3 U1 U2 116.4(2) . 3_666 ?
N1_1 U1 U2 108.27(17) . 3_666 ?
N4_1 U1 U2 167.61(19) . 3_666 ?
O4 U2 O5 173.7(3) . . ?
O4 U2 O1 92.6(3) . . ?
O5 U2 O1 92.5(3) . . ?
O4 U2 O1 94.9(3) . 3_666 ?
O5 U2 O1 90.1(3) . 3_666 ?
O1 U2 O1 71.7(2) . 3_666 ?
O4 U2 O6 88.8(3) . . ?
O5 U2 O6 89.4(3) . . ?
O1 U2 O6 141.0(2) . . ?
O1 U2 O6 69.4(2) 3_666 . ?
O4 U2 O2_3 91.9(3) . . ?
O5 U2 O2_3 85.5(3) . . ?
O1 U2 O2_3 80.3(3) . . ?
O1 U2 O2_3 151.4(3) 3_666 . ?
O6 U2 O2_3 138.7(2) . . ?
O4 U2 O7 84.2(3) . . ?
O5 U2 O7 89.5(3) . . ?
O1 U2 O7 149.1(2) . . ?
O1 U2 O7 139.2(2) 3_666 . ?
O6 U2 O7 69.8(2) . . ?
O2_3 U2 O7 69.2(3) . . ?
O4 U2 U2 94.7(2) . 3_666 ?
O5 U2 U2 91.6(2) . 3_666 ?
O1 U2 U2 36.25(15) . 3_666 ?
O1 U2 U2 35.41(14) 3_666 3_666 ?
O6 U2 U2 104.77(15) . 3_666 ?
O2_3 U2 U2 116.3(2) . 3_666 ?
O7 U2 U2 174.47(17) . 3_666 ?
O4 U2 U1 98.0(2) . 3_666 ?
O5 U2 U1 84.0(2) . 3_666 ?
O1 U2 U1 105.02(15) . 3_666 ?
O1 U2 U1 33.68(14) 3_666 3_666 ?
O6 U2 U1 36.50(15) . 3_666 ?
O2_3 U2 U1 168.4(2) . 3_666 ?
O7 U2 U1 105.86(16) . 3_666 ?
U2 U2 U1 68.887(13) 3_666 3_666 ?
U1 O1 U2 139.3(3) . . ?
U1 O1 U2 111.6(2) . 3_666 ?
U2 O1 U2 108.3(2) . 3_666 ?
U1 O6 U2 106.1(2) 3_666 . ?
U2 O7 H7A 118(8) . . ?
U2 O7 H7B 111(10) . . ?
H7A O7 H7B 96(3) . . ?
H8A O8 H8B 94.2(19) . . ?
C3_1 N1_1 N2_1 104.3(7) . . ?
C3_1 N1_1 U1 129.1(6) . . ?
N2_1 N1_1 U1 126.5(5) . . ?
N1_1 N2_1 C1_1 111.6(7) . . ?
N1_1 N2_1 C7_1 119.6(7) . . ?
C1_1 N2_1 C7_1 128.7(8) . . ?
C6_1 N3_1 N4_1 110.6(8) . . ?
C6_1 N3_1 C7_1 129.7(8) . . ?
N4_1 N3_1 C7_1 119.7(7) . . ?
C4_1 N4_1 N3_1 105.6(8) . . ?
C4_1 N4_1 U1 129.3(7) . . ?
N3_1 N4_1 U1 125.1(5) . . ?
C2_1 C1_1 N2_1 106.6(9) . . ?
C2_1 C1_1 H1_1 126.7 . . ?
N2_1 C1_1 H1_1 126.7 . . ?
C1_1 C2_1 C3_1 105.5(9) . . ?
C1_1 C2_1 H2_1 127.2 . . ?
C3_1 C2_1 H2_1 127.2 . . ?
N1_1 C3_1 C2_1 111.9(9) . . ?
N1_1 C3_1 H3_1 124.0 . . ?
C2_1 C3_1 H3_1 124.0 . . ?
N4_1 C4_1 C5_1 110.8(10) . . ?
N4_1 C4_1 H4_1 124.6 . . ?
C5_1 C4_1 H4_1 124.6 . . ?
C6_1 C5_1 C4_1 104.8(9) . . ?
C6_1 C5_1 H5_1 127.6 . . ?
C4_1 C5_1 H5_1 127.6 . . ?
N3_1 C6_1 C5_1 108.2(9) . . ?
N3_1 C6_1 H6_1 125.9 . . ?
C5_1 C6_1 H6_1 125.9 . . ?
N2_1 C7_1 N3_1 109.4(7) . . ?
N2_1 C7_1 H7A_1 109.8 . . ?
N3_1 C7_1 H7A_1 109.8 . . ?
N2_1 C7_1 H7B_1 109.8 . . ?
N3_1 C7_1 H7B_1 109.8 . . ?
H7A_1 C7_1 H7B_1 108.3 . . ?
C3_2 N1_2 N2_2 103.2(10) . . ?
C1_2 N2_2 N1_2 110.4(10) . . ?
C1_2 N2_2 C7_2 130.3(10) . . ?
N1_2 N2_2 C7_2 119.3(10) . . ?
C6_2 N3_2 N4_2 110.6(10) . . ?
C6_2 N3_2 C7_2 128.6(11) . . ?
N4_2 N3_2 C7_2 120.7(10) . . ?
C4_2 N4_2 N3_2 105.2(10) . . ?
N2_2 C1_2 C2_2 109.7(11) . . ?
N2_2 C1_2 H1_2 125.2 . . ?
C2_2 C1_2 H1_2 125.2 . . ?
C1_2 C2_2 C3_2 102.9(11) . . ?
C1_2 C2_2 H2_2 128.6 . . ?
C3_2 C2_2 H2_2 128.6 . . ?
N1_2 C3_2 C2_2 113.7(11) . . ?
N1_2 C3_2 H3_2 123.1 . . ?
C2_2 C3_2 H3_2 123.1 . . ?
N4_2 C4_2 C5_2 111.1(11) . . ?
N4_2 C4_2 H4_2 124.5 . . ?
C5_2 C4_2 H4_2 124.5 . . ?
C6_2 C5_2 C4_2 104.2(13) . . ?
C6_2 C5_2 H5_2 127.9 . . ?
C4_2 C5_2 H5_2 127.9 . . ?
N3_2 C6_2 C5_2 109.0(12) . . ?
N3_2 C6_2 H6_2 125.5 . . ?
C5_2 C6_2 H6_2 125.5 . . ?
N2_2 C7_2 N3_2 113.4(10) . . ?
N2_2 C7_2 H7A_2 108.9 . . ?
N3_2 C7_2 H7A_2 108.9 . . ?
N2_2 C7_2 H7B_2 108.9 . . ?
N3_2 C7_2 H7B_2 108.9 . . ?
H7A_2 C7_2 H7B_2 107.7 . . ?
C1_3 O1_3 U1 136.0(8) . . ?
C1_3 O2_3 U2 138.7(8) . . ?
O2_3 C1_3 O1_3 121.7(10) . . ?
O2_3 C1_3 C2_3 119.6(11) . . ?
O1_3 C1_3 C2_3 118.6(11) . . ?
C1_3 C2_3 H2A_3 109.5 . . ?
C1_3 C2_3 H2B_3 109.5 . . ?
H2A_3 C2_3 H2B_3 109.5 . . ?
C1_3 C2_3 H2C_3 109.5 . . ?
H2A_3 C2_3 H2C_3 109.5 . . ?
H2B_3 C2_3 H2C_3 109.5 . . ?

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
C3_1 N1_1 N2_1 C1_1 1.4(11) . . . . ?
U1 N1_1 N2_1 C1_1 179.5(6) . . . . ?
C3_1 N1_1 N2_1 C7_1 178.0(8) . . . . ?
U1 N1_1 N2_1 C7_1 -3.9(11) . . . . ?
C6_1 N3_1 N4_1 C4_1 0.6(11) . . . . ?
C7_1 N3_1 N4_1 C4_1 -177.0(8) . . . . ?
C6_1 N3_1 N4_1 U1 -179.4(6) . . . . ?
C7_1 N3_1 N4_1 U1 3.0(11) . . . . ?
N1_1 N2_1 C1_1 C2_1 -1.4(11) . . . . ?
C7_1 N2_1 C1_1 C2_1 -177.6(9) . . . . ?
N2_1 C1_1 C2_1 C3_1 0.7(12) . . . . ?
N2_1 N1_1 C3_1 C2_1 -0.9(12) . . . . ?
U1 N1_1 C3_1 C2_1 -178.9(7) . . . . ?
C1_1 C2_1 C3_1 N1_1 0.1(13) . . . . ?
N3_1 N4_1 C4_1 C5_1 0.0(12) . . . . ?
U1 N4_1 C4_1 C5_1 -180.0(7) . . . . ?
N4_1 C4_1 C5_1 C6_1 -0.6(14) . . . . ?
N4_1 N3_1 C6_1 C5_1 -1.0(12) . . . . ?
C7_1 N3_1 C6_1 C5_1 176.3(9) . . . . ?
C4_1 C5_1 C6_1 N3_1 0.9(12) . . . . ?
N1_1 N2_1 C7_1 N3_1 -63.9(10) . . . . ?
C1_1 N2_1 C7_1 N3_1 112.0(10) . . . . ?
C6_1 N3_1 C7_1 N2_1 -113.4(10) . . . . ?
N4_1 N3_1 C7_1 N2_1 63.7(10) . . . . ?
C3_2 N1_2 N2_2 C1_2 1.0(13) . . . . ?
C3_2 N1_2 N2_2 C7_2 -179.0(10) . . . . ?
C6_2 N3_2 N4_2 C4_2 -1.1(14) . . . . ?
C7_2 N3_2 N4_2 C4_2 -177.2(10) . . . . ?
N1_2 N2_2 C1_2 C2_2 0.4(13) . . . . ?
C7_2 N2_2 C1_2 C2_2 -179.5(11) . . . . ?
N2_2 C1_2 C2_2 C3_2 -1.7(13) . . . . ?
N2_2 N1_2 C3_2 C2_2 -2.2(14) . . . . ?
C1_2 C2_2 C3_2 N1_2 2.5(15) . . . . ?
N3_2 N4_2 C4_2 C5_2 1.3(14) . . . . ?
N4_2 C4_2 C5_2 C6_2 -1.1(16) . . . . ?
N4_2 N3_2 C6_2 C5_2 0.4(16) . . . . ?
C7_2 N3_2 C6_2 C5_2 176.2(12) . . . . ?
C4_2 C5_2 C6_2 N3_2 0.4(17) . . . . ?
C1_2 N2_2 C7_2 N3_2 -105.8(13) . . . . ?
N1_2 N2_2 C7_2 N3_2 74.2(13) . . . . ?
C6_2 N3_2 C7_2 N2_2 -100.6(15) . . . . ?
N4_2 N3_2 C7_2 N2_2 74.8(13) . . . . ?
U2 O2_3 C1_3 O1_3 28(2) . . . . ?
U2 O2_3 C1_3 C2_3 -148.3(11) . . . . ?
U1 O1_3 C1_3 O2_3 35(2) . . . . ?
U1 O1_3 C1_3 C2_3 -148.9(11) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O7 H7B N1_2 0.95(2) 1.85(4) 2.772(12) 165(14) . yes
O8 H8A O2 0.97(2) 2.295(8) 3.12(3) 141.6(14) . yes
O8 H8B O3 0.966(19) 2.816(7) 3.55(2) 133.1(12) 4_565 yes

_refine_diff_density_max         2.257
_refine_diff_density_min         -1.390
_refine_diff_density_rms         0.238

