# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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_mh93ab
_database_code_depnum_ccdc_archive 'CCDC 1470117'
_audit_update_record             
;
2016-04-22 deposited with the CCDC.
2016-05-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C26 H26 N4 O6 U'
_chemical_formula_sum            'C26 H26 N4 O6 U'
_chemical_formula_weight         728.54

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'
U U -9.6767 9.6646 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   9.544(3)
_cell_length_b                   8.859(3)
_cell_length_c                   15.195(4)
_cell_angle_alpha                90
_cell_angle_beta                 91.73(3)
_cell_angle_gamma                90
_cell_volume                     1284.2(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    12183
_cell_measurement_theta_min      2.44
_cell_measurement_theta_max      27.24

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.884
_exptl_crystal_F_000             700
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_exptl_absorpt_coefficient_mu    6.368
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.688
_exptl_absorpt_correction_T_max  0.792
_exptl_absorpt_process_details   'Stoe, X-area ver. 1.54'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  IPDS2t
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            13554
_diffrn_reflns_av_unetI/netI     0.0430
_diffrn_reflns_av_R_equivalents  0.0668
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.487
_diffrn_reflns_theta_max         26.754
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             2714
_reflns_number_gt                1955
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Diamond 3.0'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_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)+(0.0450P)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         2714
_refine_ls_number_parameters     170
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0569
_refine_ls_R_factor_gt           0.0323
_refine_ls_wR_factor_ref         0.0774
_refine_ls_wR_factor_gt          0.0679
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_restrained_S_all      1.000
_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 0.0000 0.0000 0.5000 0.02034(10) Uani 1 2 d S . P . .
O1 O -0.0689(5) 0.0381(4) 0.6045(3) 0.0277(9) Uani 1 1 d . . . . .
O1M O -0.0452(5) -0.2679(4) 0.5256(3) 0.0258(8) Uani 1 1 d . . . . .
H1M H -0.0863 -0.3214 0.4771 0.039 Uiso 1 1 calc R U . . .
C1M C -0.0181(6) -0.3548(6) 0.6035(4) 0.0280(12) Uani 1 1 d . . . . .
H1MA H -0.0030 -0.4606 0.5875 0.042 Uiso 1 1 calc R U . . .
H1MB H -0.0986 -0.3478 0.6419 0.042 Uiso 1 1 calc R U . . .
H1MC H 0.0657 -0.3158 0.6346 0.042 Uiso 1 1 calc R U . . .
O2 O 0.2020(4) -0.0959(4) 0.5692(3) 0.0235(9) Uani 1 1 d . . . . .
N1 N 0.2307(5) 0.0515(5) 0.5662(3) 0.0224(10) Uani 1 1 d . . . . .
N2 N 0.2865(5) 0.3543(5) 0.5490(3) 0.0222(9) Uani 1 1 d . . . . .
C1 C 0.3423(6) 0.1033(6) 0.6059(4) 0.0207(11) Uani 1 1 d . . . . .
C11 C 0.4380(5) 0.0035(7) 0.6579(3) 0.0232(10) Uani 1 1 d . . . . .
C21 C 0.5786(6) -0.0122(6) 0.6394(3) 0.0239(10) Uani 1 1 d . . . . .
H21 H 0.6163 0.0411 0.5913 0.029 Uiso 1 1 calc R U . . .
C31 C 0.6650(6) -0.1057(6) 0.6910(4) 0.0275(12) Uani 1 1 d . . . . .
H31 H 0.7616 -0.1148 0.6786 0.033 Uiso 1 1 calc R U . . .
C41 C 0.6101(6) -0.1851(6) 0.7603(4) 0.0236(11) Uani 1 1 d . . . . .
H41 H 0.6693 -0.2481 0.7957 0.028 Uiso 1 1 calc R U . . .
C51 C 0.4688(6) -0.1732(6) 0.7782(4) 0.0251(12) Uani 1 1 d . . . . .
H51 H 0.4311 -0.2299 0.8250 0.030 Uiso 1 1 calc R U . . .
C61 C 0.3832(6) -0.0791(6) 0.7282(4) 0.0229(11) Uani 1 1 d . . . . .
H61 H 0.2869 -0.0700 0.7412 0.028 Uiso 1 1 calc R U . . .
C22 C 0.3702(6) 0.2691(6) 0.6024(4) 0.0220(11) Uani 1 1 d . . . . .
C32 C 0.4776(7) 0.3334(7) 0.6539(4) 0.0277(12) Uani 1 1 d . . . . .
H32 H 0.5364 0.2718 0.6904 0.033 Uiso 1 1 calc R U . . .
C42 C 0.4979(6) 0.4891(7) 0.6513(4) 0.0321(12) Uani 1 1 d . . . . .
H42 H 0.5700 0.5348 0.6866 0.039 Uiso 1 1 calc R U . . .
C52 C 0.4120(7) 0.5765(6) 0.5970(4) 0.0281(13) Uani 1 1 d . . . . .
H52 H 0.4235 0.6829 0.5941 0.034 Uiso 1 1 calc R U . . .
C62 C 0.3095(6) 0.5045(7) 0.5472(4) 0.0277(10) Uani 1 1 d . . . . .
H62 H 0.2513 0.5641 0.5092 0.033 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 1.769(4) 3_556 ?
U1 O1 1.769(4) . ?
U1 O2 2.329(4) 3_556 ?
U1 O2 2.329(4) . ?
U1 N1 2.436(5) 3_556 ?
U1 N1 2.436(5) . ?
U1 O1M 2.445(4) 3_556 ?
U1 O1M 2.445(4) . ?
O1M C1M 1.430(6) . ?
O1M H1M 0.9500 . ?
C1M H1MA 0.9800 . ?
C1M H1MB 0.9800 . ?
C1M H1MC 0.9800 . ?
O2 N1 1.335(6) . ?
N1 C1 1.293(7) . ?
N2 C62 1.349(8) . ?
N2 C22 1.352(7) . ?
C1 C11 1.482(8) . ?
C1 C22 1.494(7) . ?
C11 C21 1.387(7) . ?
C11 C61 1.407(7) . ?
C21 C31 1.393(8) . ?
C21 H21 0.9500 . ?
C31 C41 1.382(8) . ?
C31 H31 0.9500 . ?
C41 C51 1.388(8) . ?
C41 H41 0.9500 . ?
C51 C61 1.380(8) . ?
C51 H51 0.9500 . ?
C61 H61 0.9500 . ?
C22 C32 1.392(8) . ?
C32 C42 1.394(9) . ?
C32 H32 0.9500 . ?
C42 C52 1.383(9) . ?
C42 H42 0.9500 . ?
C52 C62 1.376(8) . ?
C52 H52 0.9500 . ?
C62 H62 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 O1 180.0 3_556 . ?
O1 U1 O2 89.42(17) 3_556 3_556 ?
O1 U1 O2 90.58(17) . 3_556 ?
O1 U1 O2 90.58(17) 3_556 . ?
O1 U1 O2 89.42(17) . . ?
O2 U1 O2 180.0 3_556 . ?
O1 U1 N1 87.11(18) 3_556 3_556 ?
O1 U1 N1 92.89(18) . 3_556 ?
O2 U1 N1 32.45(16) 3_556 3_556 ?
O2 U1 N1 147.55(16) . 3_556 ?
O1 U1 N1 92.89(18) 3_556 . ?
O1 U1 N1 87.11(18) . . ?
O2 U1 N1 147.55(16) 3_556 . ?
O2 U1 N1 32.45(16) . . ?
N1 U1 N1 180.0 3_556 . ?
O1 U1 O1M 88.31(15) 3_556 3_556 ?
O1 U1 O1M 91.69(15) . 3_556 ?
O2 U1 O1M 73.85(13) 3_556 3_556 ?
O2 U1 O1M 106.15(13) . 3_556 ?
N1 U1 O1M 106.12(15) 3_556 3_556 ?
N1 U1 O1M 73.88(15) . 3_556 ?
O1 U1 O1M 91.69(15) 3_556 . ?
O1 U1 O1M 88.31(15) . . ?
O2 U1 O1M 106.15(13) 3_556 . ?
O2 U1 O1M 73.85(13) . . ?
N1 U1 O1M 73.88(15) 3_556 . ?
N1 U1 O1M 106.12(15) . . ?
O1M U1 O1M 180.0 3_556 . ?
C1M O1M U1 128.8(3) . . ?
C1M O1M H1M 115.6 . . ?
U1 O1M H1M 115.6 . . ?
O1M C1M H1MA 109.5 . . ?
O1M C1M H1MB 109.5 . . ?
H1MA C1M H1MB 109.5 . . ?
O1M C1M H1MC 109.5 . . ?
H1MA C1M H1MC 109.5 . . ?
H1MB C1M H1MC 109.5 . . ?
N1 O2 U1 78.2(3) . . ?
C1 N1 O2 119.9(5) . . ?
C1 N1 U1 168.8(4) . . ?
O2 N1 U1 69.4(3) . . ?
C62 N2 C22 118.0(5) . . ?
N1 C1 C11 121.5(5) . . ?
N1 C1 C22 118.5(5) . . ?
C11 C1 C22 119.9(5) . . ?
C21 C11 C61 119.0(5) . . ?
C21 C11 C1 122.4(5) . . ?
C61 C11 C1 118.5(5) . . ?
C11 C21 C31 120.4(5) . . ?
C11 C21 H21 119.8 . . ?
C31 C21 H21 119.8 . . ?
C41 C31 C21 120.0(5) . . ?
C41 C31 H31 120.0 . . ?
C21 C31 H31 120.0 . . ?
C31 C41 C51 120.3(5) . . ?
C31 C41 H41 119.9 . . ?
C51 C41 H41 119.9 . . ?
C61 C51 C41 120.0(5) . . ?
C61 C51 H51 120.0 . . ?
C41 C51 H51 120.0 . . ?
C51 C61 C11 120.3(5) . . ?
C51 C61 H61 119.8 . . ?
C11 C61 H61 119.8 . . ?
N2 C22 C32 121.4(5) . . ?
N2 C22 C1 117.9(5) . . ?
C32 C22 C1 120.7(5) . . ?
C22 C32 C42 119.3(6) . . ?
C22 C32 H32 120.3 . . ?
C42 C32 H32 120.3 . . ?
C52 C42 C32 119.4(6) . . ?
C52 C42 H42 120.3 . . ?
C32 C42 H42 120.3 . . ?
C62 C52 C42 117.9(5) . . ?
C62 C52 H52 121.1 . . ?
C42 C52 H52 121.1 . . ?
N2 C62 C52 124.0(5) . . ?
N2 C62 H62 118.0 . . ?
C52 C62 H62 118.0 . . ?

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
O1M H1M N2 0.95 1.96 2.649(6) 127.4 3_556

_refine_diff_density_max         0.622
_refine_diff_density_min         -1.784
_refine_diff_density_rms         0.126

####################################################################### 
# 
# 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_shelxl
_database_code_depnum_ccdc_archive 'CCDC 1471435'
_audit_update_record             
;
2016-04-22 deposited with the CCDC.
2016-05-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C34 H52 N10 O22 U3'
_chemical_formula_weight         1666.94

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -4.3638 13.4090 '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                   8.5148(2)
_cell_length_b                   10.3208(2)
_cell_length_c                   14.4390(3)
_cell_angle_alpha                93.5290(10)
_cell_angle_beta                 100.2610(10)
_cell_angle_gamma                95.3940(10)
_cell_volume                     1239.09(5)
_cell_formula_units_Z            1
_cell_measurement_temperature    160(2)
_cell_measurement_reflns_used    28291
_cell_measurement_theta_min      6.64
_cell_measurement_theta_max      71.89

_exptl_crystal_description       parallelepiped
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.234
_exptl_crystal_F_000             778
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.10
_exptl_absorpt_coefficient_mu    28.045
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.059
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'CrystalClear, Rigaku MSC, 2005'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      160(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Rigaku R-AXIS SPIDER IPDS'
_diffrn_measurement_method       'θ scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            29005
_diffrn_reflns_av_unetI/netI     0.0668
_diffrn_reflns_av_R_equivalents  0.0927
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         6.645
_diffrn_reflns_theta_max         64.962
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.935
_diffrn_measured_fraction_theta_full 0.874
_diffrn_reflns_Laue_measured_fraction_max 0.935
_diffrn_reflns_Laue_measured_fraction_full 0.874
_diffrn_reflns_point_group_measured_fraction_max 0.935
_diffrn_reflns_point_group_measured_fraction_full 0.874
_reflns_number_total             3924
_reflns_number_gt                3740
_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       'CrystalClear, Rigaku MSC, 2005'
_computing_cell_refinement       'CrystalClear, Rigaku MSC, 2005'
_computing_data_reduction        'CrystalClear, Rigaku MSC, 2005'
_computing_structure_solution    'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    'Diamond ver.3.1'
_computing_publication_material  ?
_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)+(0.0596P)²+3.4544P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3924
_refine_ls_number_parameters     318
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0442
_refine_ls_R_factor_gt           0.0426
_refine_ls_wR_factor_ref         0.1087
_refine_ls_wR_factor_gt          0.1064
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_restrained_S_all      1.057
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.12082(3) 0.28668(3) 0.31697(2) 0.02107(13) Uani 1 1 d . . . . .
O1 O 0.0528(6) 0.0686(6) 0.3199(4) 0.0302(14) Uani 1 1 d . . . . .
N1 N 0.1618(8) 0.0947(8) 0.4005(4) 0.0273(17) Uani 1 1 d . . . . .
C1 C 0.1046(11) -0.1319(10) 0.4347(6) 0.036(2) Uani 1 1 d . . . . .
H1A H 0.0061 -0.1288 0.3883 0.050 Uiso 1 1 calc R U . . .
H1B H 0.0773 -0.1656 0.4924 0.050 Uiso 1 1 calc R U . . .
H1C H 0.1739 -0.1894 0.4085 0.050 Uiso 1 1 calc R U . . .
C2 C 0.1914(10) 0.0032(9) 0.4572(5) 0.026(2) Uani 1 1 d . . . . .
C3 C 0.3162(9) 0.0352(9) 0.5413(5) 0.0236(19) Uani 1 1 d . . . . .
C4 C 0.3644(10) -0.0577(10) 0.6028(6) 0.033(2) Uani 1 1 d . . . . .
H4 H 0.3123 -0.1443 0.5923 0.043 Uiso 1 1 calc R U . . .
C5 C 0.4881(10) -0.0250(11) 0.6792(6) 0.037(2) Uani 1 1 d . . . . .
H5 H 0.5208 -0.0878 0.7220 0.048 Uiso 1 1 calc R U . . .
C6 C 0.5630(10) 0.1016(10) 0.6919(6) 0.032(2) Uani 1 1 d . . . . .
H6 H 0.6507 0.1266 0.7424 0.041 Uiso 1 1 calc R U . . .
C7 C 0.5083(10) 0.1895(11) 0.6306(6) 0.036(2) Uani 1 1 d . . . . .
H7 H 0.5582 0.2767 0.6406 0.047 Uiso 1 1 calc R U . . .
N2 N 0.3880(8) 0.1593(8) 0.5570(5) 0.0298(18) Uani 1 1 d . . . . .
N3 N 0.1225(8) 0.5605(8) 0.2586(5) 0.0246(16) Uani 1 1 d . . . . .
O2 O 0.0373(7) 0.4631(6) 0.2100(4) 0.0312(15) Uani 1 1 d . . . . .
O3 O 0.1170(8) 0.6688(7) 0.2363(4) 0.0390(16) Uani 1 1 d . . . . .
O4 O 0.2146(7) 0.5330(7) 0.3305(4) 0.0402(17) Uani 1 1 d . . . . .
O5 O 0.3000(7) 0.3598(6) 0.4643(4) 0.0347(16) Uani 1 1 d . . . . .
C8 C 0.2786(17) 0.4563(12) 0.5340(7) 0.065(4) Uani 1 1 d . . . . .
H8A H 0.3827 0.5046 0.5618 0.091 Uiso 1 1 calc R U . . .
H8B H 0.2323 0.4143 0.5834 0.091 Uiso 1 1 calc R U . . .
H8C H 0.2062 0.5169 0.5048 0.091 Uiso 1 1 calc R U . . .
O6 O -0.0460(6) 0.2027(6) 0.1648(4) 0.0269(15) Uani 1 1 d . . . . .
C10 C 0.0173(10) 0.1257(11) 0.0958(6) 0.041(3) Uani 1 1 d . . . . .
H10A H -0.0679 0.0983 0.0411 0.057 Uiso 1 1 calc R U . . .
H10B H 0.0574 0.0484 0.1239 0.057 Uiso 1 1 calc R U . . .
H10C H 0.1053 0.1781 0.0756 0.057 Uiso 1 1 calc R U . . .
O7 O 0.2857(6) 0.2619(6) 0.2625(4) 0.0274(14) Uani 1 1 d . . . . .
O8 O -0.0426(6) 0.3174(6) 0.3710(4) 0.0291(14) Uani 1 1 d . . . . .
U2 U -0.5000 0.0000 0.0000 0.01863(14) Uani 1 2 d S . P . .
N11 N -0.4665(7) 0.2094(7) 0.0930(4) 0.0202(15) Uani 1 1 d . . . . .
O11 O -0.3580(6) 0.1317(6) 0.1328(4) 0.0223(14) Uani 1 1 d . . . . .
C11 C -0.3661(9) 0.3703(9) 0.2267(5) 0.029(2) Uani 1 1 d . . . . .
H11A H -0.3205 0.2961 0.2566 0.040 Uiso 1 1 calc R U . . .
H11B H -0.4280 0.4130 0.2685 0.040 Uiso 1 1 calc R U . . .
H11C H -0.2791 0.4329 0.2152 0.040 Uiso 1 1 calc R U . . .
C12 C -0.4734(8) 0.3231(8) 0.1353(5) 0.0217(19) Uani 1 1 d . . . . .
C13 C -0.5883(8) 0.4071(8) 0.0887(5) 0.0216(18) Uani 1 1 d . . . . .
C14 C -0.5848(10) 0.5364(9) 0.1232(6) 0.028(2) Uani 1 1 d . . . . .
H14 H -0.5114 0.5701 0.1788 0.037 Uiso 1 1 calc R U . . .
C15 C -0.6906(10) 0.6170(9) 0.0753(6) 0.030(2) Uani 1 1 d . . . . .
H15 H -0.6865 0.7064 0.0965 0.040 Uiso 1 1 calc R U . . .
C16 C -0.7990(9) 0.5653(9) -0.0019(6) 0.0267(19) Uani 1 1 d . . . . .
H16 H -0.8733 0.6174 -0.0348 0.035 Uiso 1 1 calc R U . . .
C17 C -0.7990(10) 0.4348(10) -0.0317(6) 0.030(2) Uani 1 1 d . . . . .
H17 H -0.8764 0.3985 -0.0849 0.039 Uiso 1 1 calc R U . . .
N12 N -0.6946(7) 0.3573(7) 0.0111(4) 0.0230(16) Uani 1 1 d . . . . .
O12 O -0.7013(7) 0.1278(6) -0.0801(4) 0.0310(14) Uani 1 1 d . . . . .
C18 C -0.7687(11) 0.1380(11) -0.1762(6) 0.042(3) Uani 1 1 d . . . . .
H18A H -0.8662 0.1824 -0.1801 0.058 Uiso 1 1 calc R U . . .
H18B H -0.7956 0.0505 -0.2088 0.058 Uiso 1 1 calc R U . . .
H18C H -0.6909 0.1882 -0.2062 0.058 Uiso 1 1 calc R U . . .
O13 O -0.3597(6) 0.0602(6) -0.0684(4) 0.0287(14) Uani 1 1 d . . . . .
H5O H 0.3149 0.2669 0.4808 0.040 Uiso 1 1 d . . . . .
H6O H -0.1541 0.1956 0.1485 0.098 Uiso 1 1 d . . . . .
H12O H -0.7038 0.2088 -0.0476 0.027 Uiso 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 O8 1.757(5) . ?
U1 O7 1.758(5) . ?
U1 O1 2.276(6) . ?
U1 N1 2.404(8) . ?
U1 O5 2.419(6) . ?
U1 O6 2.453(5) . ?
U1 O2 2.531(6) . ?
U1 O4 2.577(7) . ?
U1 N3 2.997(8) . ?
O1 N1 1.349(8) . ?
N1 C2 1.300(11) . ?
C1 C2 1.504(13) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C3 1.462(11) . ?
C3 N2 1.353(11) . ?
C3 C4 1.388(12) . ?
C4 C5 1.384(12) . ?
C4 H4 0.9500 . ?
C5 C6 1.385(14) . ?
C5 H5 0.9500 . ?
C6 C7 1.362(13) . ?
C6 H6 0.9500 . ?
C7 N2 1.337(11) . ?
C7 H7 0.9500 . ?
N3 O3 1.185(9) . ?
N3 O4 1.249(9) . ?
N3 O2 1.274(9) . ?
O5 C8 1.419(11) . ?
O5 H5O 1.0160 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
O6 C10 1.446(10) . ?
O6 H6O 0.9027 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
U2 O13 1.774(5) 2_455 ?
U2 O13 1.774(5) . ?
U2 O11 2.351(6) . ?
U2 O11 2.351(6) 2_455 ?
U2 O12 2.434(6) 2_455 ?
U2 O12 2.434(6) . ?
U2 N11 2.439(7) 2_455 ?
U2 N11 2.439(7) . ?
N11 C12 1.300(10) . ?
N11 O11 1.354(8) . ?
C11 C12 1.491(10) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 C13 1.469(11) . ?
C13 N12 1.350(10) . ?
C13 C14 1.391(12) . ?
C14 C15 1.403(12) . ?
C14 H14 0.9500 . ?
C15 C16 1.359(12) . ?
C15 H15 0.9500 . ?
C16 C17 1.389(13) . ?
C16 H16 0.9500 . ?
C17 N12 1.345(11) . ?
C17 H17 0.9500 . ?
O12 C18 1.418(10) . ?
O12 H12O 0.9373 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 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
O8 U1 O7 177.9(3) . . ?
O8 U1 O1 89.3(3) . . ?
O7 U1 O1 92.7(2) . . ?
O8 U1 N1 91.6(3) . . ?
O7 U1 N1 90.2(2) . . ?
O1 U1 N1 33.4(2) . . ?
O8 U1 O5 89.1(2) . . ?
O7 U1 O5 90.5(2) . . ?
O1 U1 O5 107.2(2) . . ?
N1 U1 O5 74.0(2) . . ?
O8 U1 O6 94.6(2) . . ?
O7 U1 O6 85.9(2) . . ?
O1 U1 O6 71.0(2) . . ?
N1 U1 O6 104.0(2) . . ?
O5 U1 O6 175.86(19) . . ?
O8 U1 O2 86.4(2) . . ?
O7 U1 O2 92.0(2) . . ?
O1 U1 O2 136.48(19) . . ?
N1 U1 O2 169.8(2) . . ?
O5 U1 O2 116.0(2) . . ?
O6 U1 O2 66.2(2) . . ?
O8 U1 O4 90.4(3) . . ?
O7 U1 O4 87.6(2) . . ?
O1 U1 O4 174.23(18) . . ?
N1 U1 O4 140.9(2) . . ?
O5 U1 O4 67.0(2) . . ?
O6 U1 O4 114.7(2) . . ?
O2 U1 O4 49.24(19) . . ?
O8 U1 N3 87.2(2) . . ?
O7 U1 N3 90.8(2) . . ?
O1 U1 N3 161.23(19) . . ?
N1 U1 N3 165.1(2) . . ?
O5 U1 N3 91.2(2) . . ?
O6 U1 N3 90.8(2) . . ?
O2 U1 N3 24.86(18) . . ?
O4 U1 N3 24.43(18) . . ?
N1 O1 U1 78.6(4) . . ?
C2 N1 O1 119.9(7) . . ?
C2 N1 U1 171.2(6) . . ?
O1 N1 U1 68.1(4) . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C2 C3 117.6(8) . . ?
N1 C2 C1 120.9(8) . . ?
C3 C2 C1 121.5(8) . . ?
N2 C3 C4 120.0(8) . . ?
N2 C3 C2 117.9(8) . . ?
C4 C3 C2 122.0(8) . . ?
C5 C4 C3 120.3(9) . . ?
C5 C4 H4 119.8 . . ?
C3 C4 H4 119.8 . . ?
C4 C5 C6 118.5(9) . . ?
C4 C5 H5 120.8 . . ?
C6 C5 H5 120.8 . . ?
C7 C6 C5 118.7(9) . . ?
C7 C6 H6 120.7 . . ?
C5 C6 H6 120.7 . . ?
N2 C7 C6 123.4(10) . . ?
N2 C7 H7 118.3 . . ?
C6 C7 H7 118.3 . . ?
C7 N2 C3 119.1(8) . . ?
O3 N3 O4 122.5(7) . . ?
O3 N3 O2 122.5(7) . . ?
O4 N3 O2 115.0(8) . . ?
O3 N3 U1 177.3(5) . . ?
O4 N3 U1 58.6(5) . . ?
O2 N3 U1 56.6(4) . . ?
N3 O2 U1 98.5(5) . . ?
N3 O4 U1 97.0(5) . . ?
C8 O5 U1 127.8(6) . . ?
C8 O5 H5O 120.7 . . ?
U1 O5 H5O 92.5 . . ?
O5 C8 H8A 109.5 . . ?
O5 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
O5 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C10 O6 U1 121.4(5) . . ?
C10 O6 H6O 109.0 . . ?
U1 O6 H6O 127.9 . . ?
O6 C10 H10A 109.5 . . ?
O6 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
O6 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
O13 U2 O13 180.0(2) 2_455 . ?
O13 U2 O11 89.8(2) 2_455 . ?
O13 U2 O11 90.2(2) . . ?
O13 U2 O11 90.2(2) 2_455 2_455 ?
O13 U2 O11 89.8(2) . 2_455 ?
O11 U2 O11 180.0 . 2_455 ?
O13 U2 O12 90.9(2) 2_455 2_455 ?
O13 U2 O12 89.1(2) . 2_455 ?
O11 U2 O12 73.23(19) . 2_455 ?
O11 U2 O12 106.77(19) 2_455 2_455 ?
O13 U2 O12 89.1(2) 2_455 . ?
O13 U2 O12 90.9(2) . . ?
O11 U2 O12 106.77(19) . . ?
O11 U2 O12 73.23(19) 2_455 . ?
O12 U2 O12 180.0 2_455 . ?
O13 U2 N11 90.8(2) 2_455 2_455 ?
O13 U2 N11 89.2(2) . 2_455 ?
O11 U2 N11 147.2(2) . 2_455 ?
O11 U2 N11 32.8(2) 2_455 2_455 ?
O12 U2 N11 74.0(2) 2_455 2_455 ?
O12 U2 N11 106.0(2) . 2_455 ?
O13 U2 N11 89.2(2) 2_455 . ?
O13 U2 N11 90.8(2) . . ?
O11 U2 N11 32.8(2) . . ?
O11 U2 N11 147.2(2) 2_455 . ?
O12 U2 N11 106.0(2) 2_455 . ?
O12 U2 N11 74.0(2) . . ?
N11 U2 N11 180.0 2_455 . ?
C12 N11 O11 119.1(6) . . ?
C12 N11 U2 170.2(5) . . ?
O11 N11 U2 70.1(4) . . ?
N11 O11 U2 77.2(4) . . ?
C12 C11 H11A 109.5 . . ?
C12 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C12 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N11 C12 C13 117.9(7) . . ?
N11 C12 C11 122.0(8) . . ?
C13 C12 C11 120.1(7) . . ?
N12 C13 C14 120.8(8) . . ?
N12 C13 C12 118.8(7) . . ?
C14 C13 C12 120.4(7) . . ?
C13 C14 C15 119.6(8) . . ?
C13 C14 H14 120.2 . . ?
C15 C14 H14 120.2 . . ?
C16 C15 C14 119.1(9) . . ?
C16 C15 H15 120.4 . . ?
C14 C15 H15 120.4 . . ?
C15 C16 C17 118.6(8) . . ?
C15 C16 H16 120.7 . . ?
C17 C16 H16 120.7 . . ?
N12 C17 C16 123.2(8) . . ?
N12 C17 H17 118.4 . . ?
C16 C17 H17 118.4 . . ?
C17 N12 C13 118.6(8) . . ?
C18 O12 U2 133.9(5) . . ?
C18 O12 H12O 107.3 . . ?
U2 O12 H12O 113.0 . . ?
O12 C18 H18A 109.5 . . ?
O12 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
O12 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?

_refine_diff_density_max         2.894
_refine_diff_density_min         -2.928
_refine_diff_density_rms         0.260

# start Validation Reply Form
_vrf_PLAT911_shelxl              
;
PROBLEM: Missing # FCF Refl Between THmin & STh/L=  0.588        253 Report
RESPONSE: This is probably due to reflections masked by the beam stop shadow
on the image plate. Even in this case, the data to parameters ratio during
refinement is more than ten.
;
_vrf_PLAT971_shelxl              
;
PROBLEM: Check Calcd Residual Density  0.86A From      O8       2.97 eA-3  
RESPONSE: This alert is probably due to systematic errors caused by the 
difficulties to define precisely the shape of crystals and thus to perform 
an accurate  numerical absorption correction. We have tried to determine
the shape of the crystal as accurate as possible and we present herein
the best refinement of all our attempts.
;
_vrf_PLAT972_shelxl              
;
PROBLEM: Check Calcd Residual Density  0.76A From      U2      -2.78 eA-3  
RESPONSE: See response to PLAT971.
;
# end Validation Reply Form

_shelxl_version_number           2014/6

####################################################################### 
# 
# 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_shelxl
_database_code_depnum_ccdc_archive 'CCDC 1471436'
_audit_update_record             
;
2016-04-22 deposited with the CCDC.
2016-05-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C16 H22 N4 O6 U'
_chemical_formula_weight         604.40

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                   7.5311(4)
_cell_length_b                   8.3134(5)
_cell_length_c                   9.0115(5)
_cell_angle_alpha                71.652(2)
_cell_angle_beta                 66.613(2)
_cell_angle_gamma                66.900(2)
_cell_volume                     467.80(5)
_cell_formula_units_Z            1
_cell_measurement_temperature    160(2)
_cell_measurement_reflns_used    9272
_cell_measurement_theta_min      3.09
_cell_measurement_theta_max      27.50

_exptl_crystal_description       parallelepiped
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.145
_exptl_crystal_F_000             286
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_exptl_absorpt_coefficient_mu    8.716
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.502
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'CrystalClear, Rigaku MSC, 2005'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      160(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Rigaku R-AXIS SPIDER IPDS'
_diffrn_measurement_method       'θ scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            8816
_diffrn_reflns_av_unetI/netI     0.0228
_diffrn_reflns_av_R_equivalents  0.0281
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         3.096
_diffrn_reflns_theta_max         26.998
_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             2041
_reflns_number_gt                2041
_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       'CrystalClear, Rigaku MSC, 2005'
_computing_cell_refinement       'CrystalClear, Rigaku MSC, 2005'
_computing_data_reduction        'CrystalClear, Rigaku MSC, 2005'
_computing_structure_solution    'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    'Diamond ver.3.1'
_computing_publication_material  ?
_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)+(0.0204P)²+0.0133P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2041
_refine_ls_number_parameters     168
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0135
_refine_ls_R_factor_gt           0.0135
_refine_ls_wR_factor_ref         0.0323
_refine_ls_wR_factor_gt          0.0323
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_restrained_S_all      1.058
_refine_ls_shift/su_max          0.000
_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 0.5000 0.5000 0.0000 0.01538(5) Uani 1 2 d S . P . .
O1 O 0.3480(3) 0.3718(2) 0.0151(2) 0.0225(3) Uani 1 1 d . . . . .
O2 O 0.2599(3) 0.6075(2) 0.2366(2) 0.0219(3) Uani 1 1 d . . . . .
N1 N 0.3867(3) 0.4574(3) 0.2997(2) 0.0182(4) Uani 1 1 d . . . . .
N2 N 0.6450(3) 0.1477(3) 0.4136(2) 0.0190(4) Uani 1 1 d . . . . .
C1 C 0.1786(4) 0.5275(4) 0.5726(3) 0.0230(5) Uani 1 1 d . . . . .
C2 C 0.3538(3) 0.4151(3) 0.4574(3) 0.0177(4) Uani 1 1 d . . . . .
C3 C 0.4926(3) 0.2482(3) 0.5216(3) 0.0171(4) Uani 1 1 d . . . . .
C4 C 0.4667(4) 0.1960(3) 0.6907(3) 0.0224(5) Uani 1 1 d . . . . .
C5 C 0.5963(4) 0.0367(4) 0.7478(3) 0.0281(6) Uani 1 1 d . . . . .
C6 C 0.7485(4) -0.0670(3) 0.6383(3) 0.0260(5) Uani 1 1 d . . . . .
C7 C 0.7679(4) -0.0051(3) 0.4718(3) 0.0217(5) Uani 1 1 d . . . . .
O3 O 0.2459(3) 0.7689(2) -0.0873(2) 0.0229(4) Uani 1 1 d . . . . .
C8 C 0.0339(4) 0.7846(5) -0.0294(4) 0.0348(7) Uani 1 1 d . . . . .
H3O H 0.271(6) 0.795(5) -0.169(5) 0.036(11) Uiso 1 1 d . . . . .
H1A H 0.222(5) 0.543(4) 0.655(4) 0.029(8) Uiso 1 1 d . . . . .
H1B H 0.077(5) 0.476(5) 0.627(4) 0.034(9) Uiso 1 1 d . . . . .
H1C H 0.126(5) 0.642(5) 0.516(4) 0.030(8) Uiso 1 1 d . . . . .
H4 H 0.373(5) 0.261(4) 0.763(4) 0.026(8) Uiso 1 1 d . . . . .
H5 H 0.580(5) 0.002(5) 0.864(5) 0.042(10) Uiso 1 1 d . . . . .
H6 H 0.843(5) -0.174(4) 0.669(4) 0.026(8) Uiso 1 1 d . . . . .
H7 H 0.870(5) -0.066(4) 0.390(4) 0.021(7) Uiso 1 1 d . . . . .
H8A H 0.013(5) 0.699(5) -0.062(4) 0.038(9) Uiso 1 1 d . . . . .
H8B H -0.045(7) 0.899(6) -0.073(5) 0.061(12) Uiso 1 1 d . . . . .
H8C H -0.012(7) 0.773(6) 0.091(6) 0.062(12) Uiso 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 O1 1.7911(18) . ?
U1 O1 1.7911(18) 2_665 ?
U1 O2 2.3423(16) . ?
U1 O2 2.3423(16) 2_665 ?
U1 N1 2.4398(19) . ?
U1 N1 2.4398(19) 2_665 ?
U1 O3 2.4514(17) 2_665 ?
U1 O3 2.4514(17) . ?
O2 N1 1.357(2) . ?
N1 C2 1.296(3) . ?
N2 C7 1.338(3) . ?
N2 C3 1.355(3) . ?
C1 C2 1.499(3) . ?
C1 H1A 0.98(4) . ?
C1 H1B 0.91(4) . ?
C1 H1C 0.94(3) . ?
C2 C3 1.480(3) . ?
C3 C4 1.401(3) . ?
C4 C5 1.388(4) . ?
C4 H4 0.88(3) . ?
C5 C6 1.376(4) . ?
C5 H5 0.97(4) . ?
C6 C7 1.392(3) . ?
C6 H6 0.94(3) . ?
C7 H7 0.93(3) . ?
O3 C8 1.434(3) . ?
O3 H3O 0.67(4) . ?
C8 H8A 0.93(4) . ?
C8 H8B 0.96(5) . ?
C8 H8C 0.99(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 U1 O1 180.0 . 2_665 ?
O1 U1 O2 89.76(7) . . ?
O1 U1 O2 90.23(7) 2_665 . ?
O1 U1 O2 90.24(7) . 2_665 ?
O1 U1 O2 89.77(7) 2_665 2_665 ?
O2 U1 O2 180.0 . 2_665 ?
O1 U1 N1 89.45(7) . . ?
O1 U1 N1 90.55(7) 2_665 . ?
O2 U1 N1 32.89(6) . . ?
O2 U1 N1 147.11(6) 2_665 . ?
O1 U1 N1 90.55(7) . 2_665 ?
O1 U1 N1 89.45(7) 2_665 2_665 ?
O2 U1 N1 147.11(6) . 2_665 ?
O2 U1 N1 32.89(6) 2_665 2_665 ?
N1 U1 N1 180.0 . 2_665 ?
O1 U1 O3 91.46(7) . 2_665 ?
O1 U1 O3 88.54(7) 2_665 2_665 ?
O2 U1 O3 107.71(6) . 2_665 ?
O2 U1 O3 72.28(6) 2_665 2_665 ?
N1 U1 O3 74.85(6) . 2_665 ?
N1 U1 O3 105.15(6) 2_665 2_665 ?
O1 U1 O3 88.54(7) . . ?
O1 U1 O3 91.46(7) 2_665 . ?
O2 U1 O3 72.29(6) . . ?
O2 U1 O3 107.71(6) 2_665 . ?
N1 U1 O3 105.15(6) . . ?
N1 U1 O3 74.85(6) 2_665 . ?
O3 U1 O3 180.0 2_665 . ?
N1 O2 U1 77.51(11) . . ?
C2 N1 O2 119.31(19) . . ?
C2 N1 U1 170.94(17) . . ?
O2 N1 U1 69.61(10) . . ?
C7 N2 C3 118.7(2) . . ?
C2 C1 H1A 110.8(18) . . ?
C2 C1 H1B 111(2) . . ?
H1A C1 H1B 108(3) . . ?
C2 C1 H1C 111(2) . . ?
H1A C1 H1C 106(3) . . ?
H1B C1 H1C 109(3) . . ?
N1 C2 C3 117.6(2) . . ?
N1 C2 C1 121.7(2) . . ?
C3 C2 C1 120.6(2) . . ?
N2 C3 C4 120.9(2) . . ?
N2 C3 C2 118.69(19) . . ?
C4 C3 C2 120.4(2) . . ?
C5 C4 C3 119.2(2) . . ?
C5 C4 H4 118(2) . . ?
C3 C4 H4 123(2) . . ?
C6 C5 C4 119.9(2) . . ?
C6 C5 H5 121(2) . . ?
C4 C5 H5 119(2) . . ?
C5 C6 C7 117.8(2) . . ?
C5 C6 H6 123.7(19) . . ?
C7 C6 H6 118.4(18) . . ?
N2 C7 C6 123.5(2) . . ?
N2 C7 H7 113.8(18) . . ?
C6 C7 H7 122.6(18) . . ?
C8 O3 U1 122.25(17) . . ?
C8 O3 H3O 106(3) . . ?
U1 O3 H3O 113(3) . . ?
O3 C8 H8A 110(2) . . ?
O3 C8 H8B 112(3) . . ?
H8A C8 H8B 107(3) . . ?
O3 C8 H8C 107(3) . . ?
H8A C8 H8C 112(3) . . ?
H8B C8 H8C 108(3) . . ?

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
O3 H3O N2 0.67(4) 1.99(4) 2.654(3) 176(4) 2_665

_refine_diff_density_max         1.256
_refine_diff_density_min         -0.647
_refine_diff_density_rms         0.096

_shelxl_version_number           2014/6

####################################################################### 
# 
# 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_shelxl
_database_code_depnum_ccdc_archive 'CCDC 1471437'
_audit_update_record             
;
2016-04-22 deposited with the CCDC.
2016-05-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 H22 N4 O12 U2'
_chemical_formula_weight         962.45

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -4.3638 13.4090 '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                   8.7891(3)
_cell_length_b                   11.1500(3)
_cell_length_c                   13.0540(4)
_cell_angle_alpha                90
_cell_angle_beta                 108.4480(10)
_cell_angle_gamma                90
_cell_volume                     1213.53(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    160(2)
_cell_measurement_reflns_used    7494
_cell_measurement_theta_min      6.63
_cell_measurement_theta_max      71.91

_exptl_crystal_description       parallelepiped
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.634
_exptl_crystal_F_000             876
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_exptl_absorpt_coefficient_mu    37.901
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.520
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'CrystalClear, Rigaku MSC, 2005'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      160(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Rigaku R-AXIS SPIDER IPDS'
_diffrn_measurement_method       'θ scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            9808
_diffrn_reflns_av_unetI/netI     0.1005
_diffrn_reflns_av_R_equivalents  0.0884
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         6.630
_diffrn_reflns_theta_max         64.997
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 0.935
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 0.935
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 0.935
_reflns_number_total             2049
_reflns_number_gt                1566
_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       'CrystalClear, Rigaku MSC, 2005'
_computing_cell_refinement       'CrystalClear, Rigaku MSC, 2005'
_computing_data_reduction        'CrystalClear, Rigaku MSC, 2005'
_computing_structure_solution    'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    'Diamond ver.3.1'
_computing_publication_material  ?
_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)+(0.0510P)²+7.5991P] 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         2049
_refine_ls_number_parameters     166
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0769
_refine_ls_R_factor_gt           0.0599
_refine_ls_wR_factor_ref         0.1455
_refine_ls_wR_factor_gt          0.1249
_refine_ls_goodness_of_fit_ref   1.146
_refine_ls_restrained_S_all      1.159
_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 0.65466(7) 0.15704(4) 0.01156(4) 0.0307(3) Uani 1 1 d . . . . .
N1 N 0.7471(17) 0.3780(11) 0.0695(10) 0.031(3) Uani 1 1 d . . . . .
N2 N 0.4840(16) 0.2856(12) 0.0998(11) 0.036(3) Uani 1 1 d . . . . .
O1 O 0.8818(12) 0.4277(9) 0.0559(10) 0.039(3) Uani 1 1 d . . . . .
H1O H 0.9369 0.3737 0.0398 0.051 Uiso 1 1 calc R U . . .
O2 O 0.5349(12) 0.2134(10) -0.1127(8) 0.042(3) Uani 1 1 d . . . . .
O3 O 0.7811(16) 0.1155(11) 0.1377(10) 0.061(4) Uani 1 1 d . . . . .
O4 O 0.8865(15) 0.2279(11) -0.0365(10) 0.055(4) Uani 1 1 d . . . . .
O5 O 0.8095(14) 0.0451(9) -0.0867(9) 0.040(3) Uani 1 1 d . . . . .
O6 O 0.5510(17) -0.0330(11) -0.0262(13) 0.087(5) Uani 1 1 d . U . . .
C1 C 0.7303(19) 0.5692(14) 0.1562(14) 0.041(5) Uani 1 1 d . . . . .
H1A H 0.8302 0.5872 0.1410 0.053 Uiso 1 1 calc R U . . .
H1B H 0.7491 0.5735 0.2343 0.053 Uiso 1 1 calc R U . . .
H1C H 0.6481 0.6278 0.1194 0.053 Uiso 1 1 calc R U . . .
C2 C 0.6758(19) 0.4482(13) 0.1174(12) 0.028(4) Uani 1 1 d . . . . .
C3 C 0.5266(18) 0.4012(14) 0.1314(11) 0.027(4) Uani 1 1 d . . . . .
C4 C 0.4305(18) 0.4733(15) 0.1726(12) 0.033(4) Uani 1 1 d . . . . .
H4 H 0.4622 0.5530 0.1954 0.043 Uiso 1 1 calc R U . . .
C5 C 0.288(2) 0.4273(15) 0.1799(12) 0.034(4) Uani 1 1 d . . . . .
H5 H 0.2197 0.4771 0.2048 0.044 Uiso 1 1 calc R U . . .
C6 C 0.245(2) 0.3112(15) 0.1517(13) 0.037(4) Uani 1 1 d . . . . .
H6 H 0.1488 0.2788 0.1585 0.048 Uiso 1 1 calc R U . . .
C7 C 0.3476(17) 0.2413(13) 0.1124(11) 0.023(3) Uani 1 1 d . U . . .
H7 H 0.3201 0.1599 0.0940 0.031 Uiso 1 1 calc R U . . .
C8 C 0.8987(19) 0.1314(15) -0.0870(13) 0.029(4) Uani 1 1 d . U . . .
C9 C 1.0137(18) 0.1338(13) -0.1528(13) 0.030(4) Uani 1 1 d . . . . .
H9A H 1.1218 0.1537 -0.1055 0.039 Uiso 1 1 calc R U . . .
H9B H 0.9784 0.1944 -0.2098 0.039 Uiso 1 1 calc R U . . .
H9C H 1.0152 0.0549 -0.1855 0.039 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 1.733(12) . ?
U1 O2 1.747(11) . ?
U1 O6 2.298(12) . ?
U1 O6 2.331(12) 3_655 ?
U1 O4 2.445(11) . ?
U1 O5 2.483(9) . ?
U1 N2 2.593(13) . ?
U1 N1 2.629(13) . ?
U1 C8 2.843(15) . ?
N1 C2 1.282(18) . ?
N1 O1 1.369(15) . ?
N2 C7 1.354(17) . ?
N2 C3 1.369(19) . ?
O1 H1O 0.8400 . ?
O4 C8 1.283(17) . ?
O5 C8 1.242(17) . ?
O6 O6 1.48(2) 3_655 ?
O6 U1 2.331(12) 3_655 ?
C1 C2 1.467(19) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C3 1.48(2) . ?
C3 C4 1.392(19) . ?
C4 C5 1.38(2) . ?
C4 H4 0.9500 . ?
C5 C6 1.37(2) . ?
C5 H5 0.9500 . ?
C6 C7 1.406(19) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C8 C9 1.520(19) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 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
O3 U1 O2 174.3(5) . . ?
O3 U1 O6 92.8(6) . . ?
O2 U1 O6 92.9(6) . . ?
O3 U1 O6 92.5(6) . 3_655 ?
O2 U1 O6 92.0(6) . 3_655 ?
O6 U1 O6 37.4(5) . 3_655 ?
O3 U1 O4 89.7(5) . . ?
O2 U1 O4 87.3(5) . . ?
O6 U1 O4 123.3(4) . . ?
O6 U1 O4 160.6(4) 3_655 . ?
O3 U1 O5 93.7(5) . . ?
O2 U1 O5 88.2(4) . . ?
O6 U1 O5 70.8(3) . . ?
O6 U1 O5 108.1(4) 3_655 . ?
O4 U1 O5 52.6(4) . . ?
O3 U1 N2 90.7(5) . . ?
O2 U1 N2 87.2(5) . . ?
O6 U1 N2 111.0(4) . . ?
O6 U1 N2 73.7(4) 3_655 . ?
O4 U1 N2 125.6(4) . . ?
O5 U1 N2 175.1(4) . . ?
O3 U1 N1 86.0(5) . . ?
O2 U1 N1 88.3(5) . . ?
O6 U1 N1 172.5(4) . . ?
O6 U1 N1 135.2(4) 3_655 . ?
O4 U1 N1 64.2(4) . . ?
O5 U1 N1 116.7(4) . . ?
N2 U1 N1 61.6(4) . . ?
O3 U1 C8 93.1(5) . . ?
O2 U1 C8 86.3(5) . . ?
O6 U1 C8 96.6(4) . . ?
O6 U1 C8 133.9(4) 3_655 . ?
O4 U1 C8 26.8(4) . . ?
O5 U1 C8 25.9(3) . . ?
N2 U1 C8 151.9(4) . . ?
N1 U1 C8 90.9(4) . . ?
C2 N1 O1 113.1(13) . . ?
C2 N1 U1 123.9(11) . . ?
O1 N1 U1 122.9(9) . . ?
C7 N2 C3 118.4(13) . . ?
C7 N2 U1 120.7(10) . . ?
C3 N2 U1 120.8(9) . . ?
N1 O1 H1O 109.5 . . ?
C8 O4 U1 94.2(10) . . ?
C8 O5 U1 93.5(8) . . ?
O6 O6 U1 72.5(9) 3_655 . ?
O6 O6 U1 70.1(9) 3_655 3_655 ?
U1 O6 U1 142.6(5) . 3_655 ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C2 C1 125.0(14) . . ?
N1 C2 C3 115.7(13) . . ?
C1 C2 C3 119.3(14) . . ?
N2 C3 C4 121.2(14) . . ?
N2 C3 C2 117.8(13) . . ?
C4 C3 C2 120.9(14) . . ?
C5 C4 C3 119.0(15) . . ?
C5 C4 H4 120.5 . . ?
C3 C4 H4 120.5 . . ?
C6 C5 C4 120.9(15) . . ?
C6 C5 H5 119.5 . . ?
C4 C5 H5 119.5 . . ?
C5 C6 C7 117.9(15) . . ?
C5 C6 H6 121.0 . . ?
C7 C6 H6 121.0 . . ?
N2 C7 C6 122.4(14) . . ?
N2 C7 H7 118.8 . . ?
C6 C7 H7 118.8 . . ?
O5 C8 O4 119.6(14) . . ?
O5 C8 C9 123.2(13) . . ?
O4 C8 C9 117.0(14) . . ?
O5 C8 U1 60.7(8) . . ?
O4 C8 U1 59.1(8) . . ?
C9 C8 U1 170.4(11) . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?

_refine_diff_density_max         3.089
_refine_diff_density_min         -3.122
_refine_diff_density_rms         0.378

# start Validation Reply Form
_vrf_PLAT973_shelxl              
;
PROBLEM: Check Calcd Positive Residual Density on      U1       4.61 eA-3  
RESPONSE: This alert is probably due to systematic errors caused by the 
difficulties to define precisely the shape of crystals and thus to perform 
an accurate  numerical absorption correction.  Due to the size (<0.1) and 
shape (very thin plates) of available crystals it was impossible to overcome 
these alerts although numerous attempts to define the shape as accurately as 
possible were undertaken. The best refinement given here was performed with 
data corrected only with empirical absorption method. Also attempts to account 
for unresolved twinning were not successful. 
;
_vrf_PLAT213_shelxl              
;
PROBLEM: Atom O5              has ADP max/min Ratio .....        4.1 prolat
RESPONSE: See response to PLAT973.
;
_vrf_PLAT971_shelxl              
;
PROBLEM: Check Calcd Residual Density  1.24A From      U1       2.58 eA-3  
RESPONSE: See response to PLAT973.
;
_vrf_PLAT972_shelxl              
;
PROBLEM: Check Calcd Residual Density  0.77A From      U1      -3.46 eA-3  
RESPONSE: See response to PLAT973.
;
# end Validation Reply Form

_shelxl_version_number           2014/6

