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

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

data_Compound_1
_database_code_depnum_ccdc_archive 'CCDC 1852697'
_audit_update_record             
;
2018-09-21 deposited with the CCDC.
2018-09-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         '(C5 H5 N I 1+)2, (Pu N6 O18 2-), (H2 O)2'
_chemical_formula_sum            'C10 H14 I2 N8 O20 Pu'
_exptl_crystal_recrystallization_method 'Evaporation from acidic aqueous media'
_chemical_melting_point          ?

_exptl_crystal_description       Prismatic
_exptl_crystal_colour            'Dark Green'
_diffrn_ambient_temperature      110(2)
_chemical_formula_weight         1062.09

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'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pu Pu -9.4100 4.3056 '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'
_chemical_absolute_configuration ?

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'

_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.
;

_cell_length_a                   8.7845(7)
_cell_length_b                   12.3118(10)
_cell_length_c                   12.6497(11)
_cell_angle_alpha                90
_cell_angle_beta                 96.4470(10)
_cell_angle_gamma                90
_cell_volume                     1359.45(19)
_cell_formula_units_Z            2
_cell_measurement_temperature    110(2)
_cell_measurement_reflns_used    6526
_cell_measurement_theta_min      4.633
_cell_measurement_theta_max      56.174
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.595
_exptl_crystal_F_000             980
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.075
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    4.795
_shelx_estimated_absorpt_T_min   0.646
_shelx_estimated_absorpt_T_max   0.796
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4626
_exptl_absorpt_correction_T_max  0.5633
_exptl_absorpt_process_details   'SADABS, Krause, et. al J. Appl. Cryst. 2015'
_exptl_absorpt_special_details   ?
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Microfocus Source'
_diffrn_source_type              Bruker
_diffrn_measurement_device_type  'Bruker Quazar'
_diffrn_measurement_method       'Omega Scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            16668
_diffrn_reflns_av_unetI/netI     0.0478
_diffrn_reflns_av_R_equivalents  0.0598
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.316
_diffrn_reflns_theta_max         28.354
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             3374
_reflns_number_gt                2579
_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       'APEX, Bruker-AXS'
_computing_cell_refinement       'SAINT, Bruker-AXS'
_computing_data_reduction        'SAINT, Bruker-AXS'
_computing_structure_solution    'SIR92 (Gualardi, 1994)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'WINGX (Farrugia, 2012)'
_computing_publication_material  'Crystal Maker (Palmer, 2009)'
_refine_special_details          
;

The final refinement features several B and C level alerts related to residual electron
density, the largest being 3.81eA-3. We have ruled out the possibility of twinning, residual solvent molecules, disorder and 
unidentified atoms. The issue is most likely caused by absorption owing to the presence of heavy atoms.



;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0367P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3374
_refine_ls_number_parameters     199
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0513
_refine_ls_R_factor_gt           0.0331
_refine_ls_wR_factor_ref         0.0754
_refine_ls_wR_factor_gt          0.0682
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_restrained_S_all      1.010
_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
C1 C 0.3156(6) 0.3511(5) 0.3328(5) 0.0322(13) Uani 1 1 d . . . . .
H1 H 0.3117 0.3313 0.2599 0.039 Uiso 1 1 calc R U . . .
C2 C 0.2579(7) 0.4498(5) 0.3599(5) 0.0317(13) Uani 1 1 d . . . . .
H2 H 0.2138 0.4985 0.3067 0.038 Uiso 1 1 calc R U . . .
C3 C 0.2657(6) 0.4761(4) 0.4655(5) 0.0254(12) Uani 1 1 d . . . . .
C4 C 0.3320(6) 0.4041(4) 0.5436(5) 0.0263(12) Uani 1 1 d . . . . .
H4 H 0.3394 0.4223 0.6170 0.032 Uiso 1 1 calc R U . . .
C5 C 0.3858(6) 0.3065(4) 0.5109(5) 0.0264(12) Uani 1 1 d . . . . .
H5 H 0.4296 0.2557 0.5620 0.032 Uiso 1 1 calc R U . . .
N1 N 0.9912(5) 0.8459(4) 0.6747(4) 0.0233(10) Uani 1 1 d . . . . .
N2 N 1.1375(5) 1.1640(3) 0.6489(3) 0.0211(9) Uani 1 1 d . . . . .
N3 N 1.3054(5) 0.9349(3) 0.4553(4) 0.0233(10) Uani 1 1 d . . . . .
N4 N 0.3768(5) 0.2829(4) 0.4072(4) 0.0266(10) Uani 1 1 d D . . . .
O1 O 1.0536(4) 0.9390(3) 0.6889(3) 0.0234(8) Uani 1 1 d . . . . .
O2 O 0.9546(4) 0.8197(3) 0.5770(3) 0.0227(8) Uani 1 1 d . . . . .
O3 O 0.9667(4) 0.7872(3) 0.7482(3) 0.0342(10) Uani 1 1 d . . . . .
O4 O 0.9923(4) 1.1510(3) 0.6279(3) 0.0203(8) Uani 1 1 d . . . . .
O5 O 1.2182(4) 1.0992(3) 0.6008(3) 0.0239(8) Uani 1 1 d . . . . .
O6 O 1.1921(4) 1.2342(3) 0.7090(3) 0.0296(9) Uani 1 1 d . . . . .
O7 O 1.2425(4) 0.8922(3) 0.5305(3) 0.0234(8) Uani 1 1 d . . . . .
O8 O 1.2288(4) 1.0077(3) 0.4018(3) 0.0213(7) Uani 1 1 d . . . . .
O9 O 1.4338(4) 0.9090(3) 0.4355(3) 0.0312(9) Uani 1 1 d . . . . .
OW1 O 0.4840(5) 0.1122(3) 0.2954(4) 0.0319(9) Uani 1 1 d D . . . .
I1 I 0.17798(5) 0.62341(3) 0.51266(4) 0.04201(13) Uani 1 1 d . . . . .
Pu1 Pu 1.0000 1.0000 0.5000 0.01625(8) Uani 1 2 d S . P . .
OWH1 H 0.560(5) 0.138(5) 0.269(5) 0.06(2) Uiso 1 1 d D . . . .
OWH2 H 0.526(7) 0.062(4) 0.333(5) 0.07(3) Uiso 1 1 d D . . . .
HN1 H 0.419(5) 0.225(3) 0.382(4) 0.021(14) Uiso 1 1 d 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
C1 N4 1.328(7) . ?
C1 C2 1.376(8) . ?
C1 H1 0.9500 . ?
C2 C3 1.369(8) . ?
C2 H2 0.9500 . ?
C3 C4 1.405(7) . ?
C3 I1 2.084(5) . ?
C4 C5 1.371(7) . ?
C4 H4 0.9500 . ?
C5 N4 1.337(7) . ?
C5 H5 0.9500 . ?
N1 O3 1.215(5) . ?
N1 O1 1.275(5) . ?
N1 O2 1.282(5) . ?
N2 O6 1.214(5) . ?
N2 O5 1.267(5) . ?
N2 O4 1.283(5) . ?
N3 O9 1.224(5) . ?
N3 O7 1.267(5) . ?
N3 O8 1.269(5) . ?
N4 HN1 0.881(19) . ?
O1 Pu1 2.499(4) . ?
O2 Pu1 2.474(3) . ?
O4 Pu1 2.471(3) . ?
O5 Pu1 2.499(4) . ?
O7 Pu1 2.502(3) . ?
O8 Pu1 2.480(3) . ?
OW1 OWH1 0.840(19) . ?
OW1 OWH2 0.84(2) . ?
Pu1 O4 2.471(3) 3_776 ?
Pu1 O2 2.474(3) 3_776 ?
Pu1 O8 2.480(3) 3_776 ?
Pu1 O1 2.499(4) 3_776 ?
Pu1 O5 2.499(4) 3_776 ?
Pu1 O7 2.502(3) 3_776 ?

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
N4 C1 C2 120.9(6) . . ?
N4 C1 H1 119.6 . . ?
C2 C1 H1 119.6 . . ?
C3 C2 C1 118.2(5) . . ?
C3 C2 H2 120.9 . . ?
C1 C2 H2 120.9 . . ?
C2 C3 C4 120.6(5) . . ?
C2 C3 I1 120.3(4) . . ?
C4 C3 I1 119.1(4) . . ?
C5 C4 C3 118.0(5) . . ?
C5 C4 H4 121.0 . . ?
C3 C4 H4 121.0 . . ?
N4 C5 C4 120.2(5) . . ?
N4 C5 H5 119.9 . . ?
C4 C5 H5 119.9 . . ?
O3 N1 O1 122.4(5) . . ?
O3 N1 O2 122.8(4) . . ?
O1 N1 O2 114.8(4) . . ?
O6 N2 O5 123.1(4) . . ?
O6 N2 O4 122.1(4) . . ?
O5 N2 O4 114.8(4) . . ?
O9 N3 O7 122.4(4) . . ?
O9 N3 O8 121.3(4) . . ?
O7 N3 O8 116.3(4) . . ?
C1 N4 C5 122.1(5) . . ?
C1 N4 HN1 115(4) . . ?
C5 N4 HN1 123(4) . . ?
N1 O1 Pu1 95.9(3) . . ?
N1 O2 Pu1 96.9(3) . . ?
N2 O4 Pu1 97.4(3) . . ?
N2 O5 Pu1 96.5(3) . . ?
N3 O7 Pu1 95.7(3) . . ?
N3 O8 Pu1 96.7(3) . . ?
OWH1 OW1 OWH2 101(3) . . ?
O4 Pu1 O4 180.00(15) 3_776 . ?
O4 Pu1 O2 113.56(11) 3_776 3_776 ?
O4 Pu1 O2 66.44(11) . 3_776 ?
O4 Pu1 O2 66.44(11) 3_776 . ?
O4 Pu1 O2 113.56(11) . . ?
O2 Pu1 O2 180.0 3_776 . ?
O4 Pu1 O8 67.52(11) 3_776 . ?
O4 Pu1 O8 112.48(11) . . ?
O2 Pu1 O8 65.99(11) 3_776 . ?
O2 Pu1 O8 114.01(11) . . ?
O4 Pu1 O8 112.48(11) 3_776 3_776 ?
O4 Pu1 O8 67.52(11) . 3_776 ?
O2 Pu1 O8 114.01(11) 3_776 3_776 ?
O2 Pu1 O8 65.99(11) . 3_776 ?
O8 Pu1 O8 180.00(15) . 3_776 ?
O4 Pu1 O1 112.59(11) 3_776 . ?
O4 Pu1 O1 67.41(11) . . ?
O2 Pu1 O1 128.67(12) 3_776 . ?
O2 Pu1 O1 51.33(12) . . ?
O8 Pu1 O1 114.47(11) . . ?
O8 Pu1 O1 65.53(11) 3_776 . ?
O4 Pu1 O1 67.41(11) 3_776 3_776 ?
O4 Pu1 O1 112.59(11) . 3_776 ?
O2 Pu1 O1 51.33(12) 3_776 3_776 ?
O2 Pu1 O1 128.67(12) . 3_776 ?
O8 Pu1 O1 65.53(11) . 3_776 ?
O8 Pu1 O1 114.47(11) 3_776 3_776 ?
O1 Pu1 O1 180.0 . 3_776 ?
O4 Pu1 O5 51.22(11) 3_776 3_776 ?
O4 Pu1 O5 128.78(11) . 3_776 ?
O2 Pu1 O5 112.72(12) 3_776 3_776 ?
O2 Pu1 O5 67.29(12) . 3_776 ?
O8 Pu1 O5 112.43(11) . 3_776 ?
O8 Pu1 O5 67.57(11) 3_776 3_776 ?
O1 Pu1 O5 113.10(12) . 3_776 ?
O1 Pu1 O5 66.90(12) 3_776 3_776 ?
O4 Pu1 O5 128.78(11) 3_776 . ?
O4 Pu1 O5 51.22(11) . . ?
O2 Pu1 O5 67.29(12) 3_776 . ?
O2 Pu1 O5 112.71(12) . . ?
O8 Pu1 O5 67.57(11) . . ?
O8 Pu1 O5 112.43(11) 3_776 . ?
O1 Pu1 O5 66.90(12) . . ?
O1 Pu1 O5 113.10(12) 3_776 . ?
O5 Pu1 O5 180.00(11) 3_776 . ?
O4 Pu1 O7 67.46(11) 3_776 . ?
O4 Pu1 O7 112.54(11) . . ?
O2 Pu1 O7 111.37(11) 3_776 . ?
O2 Pu1 O7 68.63(11) . . ?
O8 Pu1 O7 51.24(11) . . ?
O8 Pu1 O7 128.76(11) 3_776 . ?
O1 Pu1 O7 68.12(11) . . ?
O1 Pu1 O7 111.88(11) 3_776 . ?
O5 Pu1 O7 114.23(11) 3_776 . ?
O5 Pu1 O7 65.77(11) . . ?
O4 Pu1 O7 112.54(11) 3_776 3_776 ?
O4 Pu1 O7 67.46(11) . 3_776 ?
O2 Pu1 O7 68.63(11) 3_776 3_776 ?
O2 Pu1 O7 111.37(11) . 3_776 ?
O8 Pu1 O7 128.76(11) . 3_776 ?
O8 Pu1 O7 51.24(11) 3_776 3_776 ?
O1 Pu1 O7 111.88(11) . 3_776 ?
O1 Pu1 O7 68.12(11) 3_776 3_776 ?
O5 Pu1 O7 65.77(11) 3_776 3_776 ?
O5 Pu1 O7 114.23(11) . 3_776 ?
O7 Pu1 O7 180.0 . 3_776 ?

_refine_diff_density_max         3.813
_refine_diff_density_min         -0.906
_refine_diff_density_rms         0.194

####################################################################### 
# 
# 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_Compound_3
_database_code_depnum_ccdc_archive 'CCDC 1852699'
_audit_update_record             
;
2018-09-21 deposited with the CCDC.
2018-09-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         '(C5 H5 N I 1+)2, (Pu N2 O6 Cl3 2-)'
_chemical_formula_sum            'C10 H10 Cl4 I2 N4 O6 Pu'
_exptl_crystal_recrystallization_method 'Evaporation from acidic aqueous media'
_chemical_melting_point          ?

_exptl_crystal_description       Blade
_exptl_crystal_colour            Orange
_diffrn_ambient_temperature      298(2)
_chemical_formula_weight         919.82

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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'
Pu Pu -9.4100 4.3056 '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'
_chemical_absolute_configuration ?

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

_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.
;

_cell_length_a                   9.8096(8)
_cell_length_b                   10.1402(8)
_cell_length_c                   11.5033(9)
_cell_angle_alpha                73.4160(10)
_cell_angle_beta                 82.3640(10)
_cell_angle_gamma                87.1000(10)
_cell_volume                     1086.83(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    7821
_cell_measurement_theta_min      4.759
_cell_measurement_theta_max      54.312
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.811
_exptl_crystal_F_000             828
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.075
_exptl_crystal_size_min          0.025
_exptl_absorpt_coefficient_mu    6.398
_shelx_estimated_absorpt_T_min   0.567
_shelx_estimated_absorpt_T_max   0.856
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3610
_exptl_absorpt_correction_T_max  0.4912
_exptl_absorpt_process_details   'SADABS, Krause, et. al J. Appl. Cryst. 2015'
_exptl_absorpt_special_details   ?
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   Sealed-tube
_diffrn_source_type              Bruker
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'Omega and Phi Scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            12875
_diffrn_reflns_av_unetI/netI     0.0364
_diffrn_reflns_av_R_equivalents  0.0301
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.861
_diffrn_reflns_theta_max         27.182
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             4809
_reflns_number_gt                4134
_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       'APEX, Bruker-AXS'
_computing_cell_refinement       'SAINT, Bruker-AXS'
_computing_data_reduction        'SAINT, Bruker-AXS'
_computing_structure_solution    'SIR92 (Gualardi, 1994)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'WINGX (Farrugia, 2012)'
_computing_publication_material  'Crystal Maker (Palmer, 2009)'
_refine_special_details          
;
The final refinement features several A, B and C level alerts related to residual electron
density near the Pu metal center and the I atom. We have ruled out the possibility of twinning, 
residual solvent molecules and unidentified atoms. The issue is most likely caused by absorption 
owing to the presence of heavy atoms. 

;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0505P)²+3.4602P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4809
_refine_ls_number_parameters     252
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0440
_refine_ls_R_factor_gt           0.0360
_refine_ls_wR_factor_ref         0.0934
_refine_ls_wR_factor_gt          0.0876
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_restrained_S_all      1.044
_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
Pu1 Pu 0.74497(2) 0.23207(2) 0.25935(2) 0.02007(9) Uani 1 1 d . . . . .
Cl1 Cl 0.9569(2) 0.1840(2) 0.38202(18) 0.0441(5) Uani 1 1 d . . . . .
Cl2 Cl 0.50945(17) 0.20612(18) 0.18586(16) 0.0311(4) Uani 1 1 d . . . . .
Cl3 Cl 0.62121(17) 0.37688(17) 0.39662(15) 0.0283(4) Uani 1 1 d . . . . .
Cl4 Cl 0.89384(17) 0.16294(18) 0.08076(14) 0.0283(3) Uani 1 1 d . . . . .
O1 O 0.8891(5) 0.4342(6) 0.1846(5) 0.0426(13) Uani 1 1 d . . . . .
O2 O 0.7107(5) 0.4403(5) 0.0953(5) 0.0380(12) Uani 1 1 d . . . . .
O3 O 0.8519(7) 0.6110(6) 0.0342(5) 0.0536(16) Uani 1 1 d . . . . .
O4 O 0.6462(6) 0.0654(5) 0.4477(5) 0.0378(12) Uani 1 1 d . . . . .
O5 O 0.7365(5) -0.0204(5) 0.3042(4) 0.0345(12) Uani 1 1 d . . . . .
O6 O 0.6556(6) -0.1563(5) 0.4798(5) 0.0450(14) Uani 1 1 d . . . . .
N1 N 0.8174(5) 0.4975(5) 0.1044(5) 0.0200(11) Uani 1 1 d . . . . .
N2 N 0.6786(6) -0.0399(6) 0.4131(5) 0.0265(12) Uani 1 1 d . . . . .
I1 I -0.05238(4) 0.75002(4) 0.28551(4) 0.02751(12) Uani 1 1 d . . . . .
N3 N 0.3106(6) 0.4124(6) 0.3107(5) 0.0259(12) Uani 1 1 d D . . . .
C1 C 0.2682(7) 0.4561(7) 0.4090(6) 0.0273(14) Uani 1 1 d . . . . .
H1 H 0.3088 0.4210 0.4804 0.033 Uiso 1 1 calc R U . . .
C2 C 0.1644(7) 0.5528(7) 0.4042(6) 0.0267(14) Uani 1 1 d . . . . .
H2 H 0.1330 0.5830 0.4723 0.032 Uiso 1 1 calc R U . . .
C3 C 0.1068(6) 0.6050(7) 0.2951(6) 0.0242(13) Uani 1 1 d . . . . .
C4 C 0.1569(7) 0.5605(7) 0.1932(6) 0.0273(14) Uani 1 1 d . . . . .
H4 H 0.1219 0.5966 0.1192 0.033 Uiso 1 1 calc R U . . .
C5 C 0.2594(7) 0.4620(7) 0.2052(6) 0.0277(14) Uani 1 1 d . . . . .
H5 H 0.2934 0.4297 0.1388 0.033 Uiso 1 1 calc R U . . .
I2 I 0.54096(5) 0.72228(5) 0.18692(5) 0.04264(15) Uani 1 1 d . . . . .
N4 N 0.1796(6) 1.0546(6) 0.1965(6) 0.0313(13) Uani 1 1 d D . . . .
C6 C 0.2281(7) 0.9866(8) 0.3008(7) 0.0351(17) Uani 1 1 d . . . . .
H6 H 0.1908 1.0033 0.3740 0.042 Uiso 1 1 calc R U . . .
C7 C 0.3336(7) 0.8915(8) 0.2995(7) 0.0334(16) Uani 1 1 d . . . . .
H7 H 0.3689 0.8441 0.3712 0.040 Uiso 1 1 calc R U . . .
C8 C 0.3855(7) 0.8682(6) 0.1897(6) 0.0267(14) Uani 1 1 d . . . . .
C9 C 0.3335(7) 0.9404(7) 0.0817(6) 0.0285(15) Uani 1 1 d . . . . .
H9 H 0.3690 0.9258 0.0072 0.034 Uiso 1 1 calc R U . . .
C10 C 0.2278(7) 1.0342(8) 0.0888(7) 0.0314(15) Uani 1 1 d . . . . .
H10 H 0.1903 1.0830 0.0186 0.038 Uiso 1 1 calc R U . . .
HN1 H 0.385(4) 0.364(6) 0.308(7) 0.03(2) Uiso 1 1 d D . . . .
HN2 H 0.111(6) 1.111(7) 0.181(8) 0.06(3) Uiso 1 1 d 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
Pu1 O1 2.429(5) . ?
Pu1 O2 2.441(5) . ?
Pu1 O4 2.451(5) . ?
Pu1 O5 2.467(5) . ?
Pu1 Cl3 2.5995(15) . ?
Pu1 Cl4 2.6011(15) . ?
Pu1 Cl2 2.6133(16) . ?
Pu1 Cl1 2.6143(18) . ?
O1 N1 1.243(7) . ?
O2 N1 1.253(7) . ?
O3 N1 1.236(7) . ?
O4 N2 1.254(7) . ?
O5 N2 1.270(7) . ?
O6 N2 1.223(7) . ?
I1 C3 2.082(6) . ?
N3 C5 1.329(8) . ?
N3 C1 1.338(9) . ?
N3 HN1 0.86(2) . ?
C1 C2 1.373(9) . ?
C1 H1 0.9300 . ?
C2 C3 1.398(9) . ?
C2 H2 0.9300 . ?
C3 C4 1.395(9) . ?
C4 C5 1.372(9) . ?
C4 H4 0.9300 . ?
C5 H5 0.9300 . ?
I2 C8 2.074(6) . ?
N4 C10 1.336(9) . ?
N4 C6 1.337(9) . ?
N4 HN2 0.86(2) . ?
C6 C7 1.380(10) . ?
C6 H6 0.9300 . ?
C7 C8 1.377(10) . ?
C7 H7 0.9300 . ?
C8 C9 1.397(9) . ?
C9 C10 1.381(10) . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Pu1 O2 51.96(18) . . ?
O1 Pu1 O4 142.41(18) . . ?
O2 Pu1 O4 147.50(18) . . ?
O1 Pu1 O5 145.92(18) . . ?
O2 Pu1 O5 140.27(17) . . ?
O4 Pu1 O5 51.84(16) . . ?
O1 Pu1 Cl3 81.69(14) . . ?
O2 Pu1 Cl3 83.04(13) . . ?
O4 Pu1 Cl3 74.14(12) . . ?
O5 Pu1 Cl3 125.59(12) . . ?
O1 Pu1 Cl4 81.69(14) . . ?
O2 Pu1 Cl4 81.50(13) . . ?
O4 Pu1 Cl4 123.62(12) . . ?
O5 Pu1 Cl4 72.32(12) . . ?
Cl3 Pu1 Cl4 162.09(6) . . ?
O1 Pu1 Cl2 125.21(14) . . ?
O2 Pu1 Cl2 73.38(13) . . ?
O4 Pu1 Cl2 83.28(13) . . ?
O5 Pu1 Cl2 79.64(12) . . ?
Cl3 Pu1 Cl2 89.10(5) . . ?
Cl4 Pu1 Cl2 95.07(5) . . ?
O1 Pu1 Cl1 72.80(14) . . ?
O2 Pu1 Cl1 124.71(13) . . ?
O4 Pu1 Cl1 79.67(14) . . ?
O5 Pu1 Cl1 85.01(13) . . ?
Cl3 Pu1 Cl1 92.08(5) . . ?
Cl4 Pu1 Cl1 89.34(6) . . ?
Cl2 Pu1 Cl1 161.88(7) . . ?
N1 O1 Pu1 95.7(4) . . ?
N1 O2 Pu1 94.9(4) . . ?
N2 O4 Pu1 96.2(4) . . ?
N2 O5 Pu1 95.0(4) . . ?
O3 N1 O1 121.3(6) . . ?
O3 N1 O2 121.2(6) . . ?
O1 N1 O2 117.5(5) . . ?
O6 N2 O4 122.4(6) . . ?
O6 N2 O5 120.9(5) . . ?
O4 N2 O5 116.8(6) . . ?
C5 N3 C1 122.8(6) . . ?
C5 N3 HN1 115(5) . . ?
C1 N3 HN1 121(5) . . ?
N3 C1 C2 119.7(6) . . ?
N3 C1 H1 120.1 . . ?
C2 C1 H1 120.1 . . ?
C1 C2 C3 118.8(6) . . ?
C1 C2 H2 120.6 . . ?
C3 C2 H2 120.6 . . ?
C4 C3 C2 119.8(6) . . ?
C4 C3 I1 120.5(5) . . ?
C2 C3 I1 119.7(5) . . ?
C5 C4 C3 118.2(6) . . ?
C5 C4 H4 120.9 . . ?
C3 C4 H4 120.9 . . ?
N3 C5 C4 120.6(6) . . ?
N3 C5 H5 119.7 . . ?
C4 C5 H5 119.7 . . ?
C10 N4 C6 122.9(6) . . ?
C10 N4 HN2 104(6) . . ?
C6 N4 HN2 132(6) . . ?
N4 C6 C7 119.7(7) . . ?
N4 C6 H6 120.1 . . ?
C7 C6 H6 120.1 . . ?
C8 C7 C6 118.7(7) . . ?
C8 C7 H7 120.7 . . ?
C6 C7 H7 120.7 . . ?
C7 C8 C9 120.7(6) . . ?
C7 C8 I2 119.1(5) . . ?
C9 C8 I2 120.2(5) . . ?
C10 C9 C8 118.0(7) . . ?
C10 C9 H9 121.0 . . ?
C8 C9 H9 121.0 . . ?
N4 C10 C9 119.9(6) . . ?
N4 C10 H10 120.0 . . ?
C9 C10 H10 120.0 . . ?

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
Pu1 O1 N1 O3 -177.4(5) . . . . ?
Pu1 O1 N1 O2 0.8(6) . . . . ?
Pu1 O2 N1 O3 177.4(5) . . . . ?
Pu1 O2 N1 O1 -0.8(6) . . . . ?
Pu1 O4 N2 O6 177.0(6) . . . . ?
Pu1 O4 N2 O5 -3.3(6) . . . . ?
Pu1 O5 N2 O6 -177.0(6) . . . . ?
Pu1 O5 N2 O4 3.3(6) . . . . ?
C5 N3 C1 C2 2.3(11) . . . . ?
N3 C1 C2 C3 -1.0(10) . . . . ?
C1 C2 C3 C4 -1.2(10) . . . . ?
C1 C2 C3 I1 179.3(5) . . . . ?
C2 C3 C4 C5 2.2(10) . . . . ?
I1 C3 C4 C5 -178.3(5) . . . . ?
C1 N3 C5 C4 -1.2(11) . . . . ?
C3 C4 C5 N3 -1.0(10) . . . . ?
C10 N4 C6 C7 0.7(11) . . . . ?
N4 C6 C7 C8 -0.7(11) . . . . ?
C6 C7 C8 C9 0.7(11) . . . . ?
C6 C7 C8 I2 -178.6(5) . . . . ?
C7 C8 C9 C10 -0.8(10) . . . . ?
I2 C8 C9 C10 178.5(5) . . . . ?
C6 N4 C10 C9 -0.8(11) . . . . ?
C8 C9 C10 N4 0.8(10) . . . . ?

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
N3 HN1 Cl2 0.86(2) 2.58(5) 3.287(6) 140(6) .
N3 HN1 Cl3 0.86(2) 2.68(6) 3.298(6) 130(6) .
C1 H1 Cl3 0.93 2.95 3.470(7) 116.4 2_666
C4 H4 Cl4 0.93 2.85 3.644(7) 144.2 2_665
C5 H5 O2 0.93 2.64 3.289(9) 127.1 2_665
N4 HN2 Cl1 0.86(2) 2.85(8) 3.334(6) 117(7) 1_465
N4 HN2 Cl4 0.86(2) 2.52(5) 3.269(6) 146(8) 1_465
C6 H6 Cl1 0.93 2.87 3.438(8) 120.5 1_465
C7 H7 Cl3 0.93 2.97 3.832(7) 155.6 2_666
C7 H7 O4 0.93 2.49 3.095(9) 122.9 2_666
C9 H9 Cl2 0.93 3.00 3.895(7) 163.1 2_665
N3 HN1 Cl2 0.86(2) 2.58(5) 3.287(6) 140(6) .
N3 HN1 Cl3 0.86(2) 2.68(6) 3.298(6) 130(6) .
C1 H1 Cl3 0.93 2.95 3.470(7) 116.4 2_666
C4 H4 Cl4 0.93 2.85 3.644(7) 144.2 2_665
C5 H5 O2 0.93 2.64 3.289(9) 127.1 2_665
N4 HN2 Cl1 0.86(2) 2.85(8) 3.334(6) 117(7) 1_465
N4 HN2 Cl4 0.86(2) 2.52(5) 3.269(6) 146(8) 1_465
C6 H6 Cl1 0.93 2.87 3.438(8) 120.5 1_465
C7 H7 Cl3 0.93 2.97 3.832(7) 155.6 2_666
C7 H7 O4 0.93 2.49 3.095(9) 122.9 2_666
C9 H9 Cl2 0.93 3.00 3.895(7) 163.1 2_665

_refine_diff_density_max         3.844
_refine_diff_density_min         -1.374
_refine_diff_density_rms         0.221

####################################################################### 
# 
# 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_Compound_2
_database_code_depnum_ccdc_archive 'CCDC 1852698'
_audit_update_record             
;
2018-09-21 deposited with the CCDC.
2018-09-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         '(C5 H6 N 1+)2, (Pu N3 O9 Cl3 2-)'
_chemical_formula_sum            'C10 H12 Cl3 N5 O9 Pu'
_exptl_crystal_recrystallization_method 'Evaporation from acidic aqueous media'
_chemical_melting_point          ?

_exptl_crystal_description       Blade
_exptl_crystal_colour            'Dark Red'
_diffrn_ambient_temperature      110(2)
_chemical_formula_weight         694.60

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pu Pu -9.4100 4.3056 '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'
_chemical_absolute_configuration ?

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'

_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.
;

_cell_length_a                   17.2683(14)
_cell_length_b                   7.7622(6)
_cell_length_c                   15.1117(11)
_cell_angle_alpha                90
_cell_angle_beta                 97.598(2)
_cell_angle_gamma                90
_cell_volume                     2007.8(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    110(2)
_cell_measurement_reflns_used    9538
_cell_measurement_theta_min      5.763
_cell_measurement_theta_max      54.396
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.298
_exptl_crystal_F_000             1296
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.075
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    3.735
_shelx_estimated_absorpt_T_min   0.706
_shelx_estimated_absorpt_T_max   0.835
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.386178
_exptl_absorpt_correction_T_max  0.491251
_exptl_absorpt_process_details   'SADABS, Krause, et. al J. Appl. Cryst. 2015'
_exptl_absorpt_special_details   ?
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Microfocus Source'
_diffrn_source_type              Bruker
_diffrn_measurement_device_type  'Bruker Quazar'
_diffrn_measurement_method       'Omega Scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            4463
_diffrn_reflns_av_unetI/netI     0.0098
_diffrn_reflns_av_R_equivalents  0.0301
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.956
_diffrn_reflns_theta_max         27.265
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             4463
_reflns_number_gt                4188
_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       'APEX, Bruker-AXS'
_computing_cell_refinement       'SAINT, Bruker-AXS'
_computing_data_reduction        'SAINT, Bruker-AXS'
_computing_structure_solution    'SIR92 (Gualardi, 1994)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'WINGX (Farrugia, 2012)'
_computing_publication_material  'Crystal Maker (Palmer, 2009)'
_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)+(0.0214P)²+2.9740P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4463
_refine_ls_number_parameters     252
_refine_ls_number_restraints     13
_refine_ls_R_factor_all          0.0239
_refine_ls_R_factor_gt           0.0216
_refine_ls_wR_factor_ref         0.0529
_refine_ls_wR_factor_gt          0.0518
_refine_ls_goodness_of_fit_ref   1.183
_refine_ls_restrained_S_all      1.181
_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
C1 C 0.4187(3) 0.2053(8) 0.1022(3) 0.0707(13) Uani 1 1 d . . . . .
H1 H 0.4155 0.2186 0.1641 0.085 Uiso 1 1 calc R U . . .
C2 C 0.4785(3) 0.2733(7) 0.0664(4) 0.0693(12) Uani 1 1 d . . . . .
H2 H 0.5182 0.3347 0.1030 0.083 Uiso 1 1 calc R U . . .
C3 C 0.4827(3) 0.2546(7) -0.0222(4) 0.0698(13) Uani 1 1 d . . . . .
H3 H 0.5253 0.3032 -0.0473 0.084 Uiso 1 1 calc R U . . .
C4 C 0.4259(4) 0.1666(7) -0.0755(4) 0.0822(16) Uani 1 1 d . . . . .
H4A H 0.4285 0.1523 -0.1375 0.099 Uiso 1 1 calc R U . . .
C5 C 0.3648(3) 0.0992(7) -0.0363(4) 0.0827(16) Uani 1 1 d . . . . .
H5 H 0.3237 0.0389 -0.0712 0.099 Uiso 1 1 calc R U . . .
N5A N 0.0882(4) 0.2603(9) 0.1071(3) 0.076(2) Uani 0.581(6) 1 d G U P A 1
H5A H 0.1144 0.2545 0.1610 0.092 Uiso 0.581(6) 1 calc R U P A 1
C6A C 0.0098(4) 0.2137(11) 0.0931(4) 0.077(3) Uani 0.581(6) 1 d G . P A 1
H6A H -0.0154 0.1756 0.1417 0.092 Uiso 0.581(6) 1 calc R U P A 1
C7A C -0.0317(3) 0.2229(13) 0.0078(5) 0.093(4) Uani 0.581(6) 1 d G . P A 1
H7A H -0.0853 0.1910 -0.0017 0.111 Uiso 0.581(6) 1 calc R U P A 1
C8A C 0.0052(4) 0.2787(13) -0.0633(4) 0.098(4) Uani 0.581(6) 1 d G . P A 1
H8A H -0.0231 0.2849 -0.1216 0.118 Uiso 0.581(6) 1 calc R U P A 1
C9A C 0.0836(4) 0.3252(11) -0.0493(3) 0.068(2) Uani 0.581(6) 1 d G . P A 1
H9A H 0.1088 0.3634 -0.0980 0.082 Uiso 0.581(6) 1 calc R U P A 1
C10A C 0.1251(3) 0.3161(9) 0.0359(4) 0.0640(19) Uani 0.581(6) 1 d G . P A 1
H10A H 0.1787 0.3479 0.0455 0.077 Uiso 0.581(6) 1 calc R U P A 1
N5B N 0.0330(6) 0.2549(15) 0.1074(4) 0.076(2) Uani 0.419(6) 1 d G U P A 2
H6A1 H 0.0318 0.2460 0.1652 0.092 Uiso 0.419(6) 1 calc R U P A 2
C6B C -0.0359(4) 0.2446(16) 0.0486(7) 0.077(3) Uani 0.419(6) 1 d G . P A 2
H6B H -0.0843 0.2279 0.0709 0.092 Uiso 0.419(6) 1 calc R U P A 2
C7B C -0.0341(4) 0.2587(18) -0.0428(6) 0.093(4) Uani 0.419(6) 1 d G . P A 2
H7B H -0.0812 0.2517 -0.0829 0.111 Uiso 0.419(6) 1 calc R U P A 2
C8B C 0.0367(6) 0.283(2) -0.0754(4) 0.098(4) Uani 0.419(6) 1 d G . P A 2
H8B H 0.0380 0.2928 -0.1379 0.118 Uiso 0.419(6) 1 calc R U P A 2
C9B C 0.1056(4) 0.2934(17) -0.0166(6) 0.068(2) Uani 0.419(6) 1 d G . P A 2
H9B H 0.1540 0.3101 -0.0389 0.082 Uiso 0.419(6) 1 calc R U P A 2
C10B C 0.1038(4) 0.2793(14) 0.0748(5) 0.0640(19) Uani 0.419(6) 1 d G . P A 2
H10B H 0.1509 0.2864 0.1149 0.077 Uiso 0.419(6) 1 calc R U P A 2
Cl1 Cl 0.27872(7) 0.32517(13) 0.74912(8) 0.0638(3) Uani 1 1 d . . . . .
Cl2 Cl 0.09639(5) 0.55864(15) 0.75588(7) 0.0546(2) Uani 1 1 d . . . . .
Cl3 Cl 0.22263(6) 0.63288(15) 0.58479(6) 0.0576(2) Uani 1 1 d . . . . .
N1 N 0.38876(19) 0.8106(5) 0.7278(2) 0.0520(8) Uani 1 1 d . . . . .
N2 N 0.16083(19) 0.9650(4) 0.7852(2) 0.0540(8) Uani 1 1 d . . . . .
N3 N 0.2975(2) 0.5730(5) 0.9461(2) 0.0538(8) Uani 1 1 d . . . . .
N4 N 0.3641(2) 0.1194(6) 0.0508(4) 0.0758(12) Uani 1 1 d D . . . .
O1 O 0.33020(17) 0.8931(4) 0.7488(2) 0.0574(7) Uani 1 1 d . . . . .
O2 O 0.37857(17) 0.6493(4) 0.7207(2) 0.0589(7) Uani 1 1 d . . . . .
O3 O 0.44858(19) 0.8802(5) 0.7155(2) 0.0785(10) Uani 1 1 d . . . . .
O4 O 0.16789(17) 0.9088(4) 0.70787(19) 0.0554(7) Uani 1 1 d . . . . .
O5 O 0.19895(17) 0.8842(4) 0.84932(19) 0.0560(7) Uani 1 1 d . . . . .
O6 O 0.1201(2) 1.0872(5) 0.7960(3) 0.0853(11) Uani 1 1 d . . . . .
O7 O 0.22875(16) 0.5376(4) 0.91047(18) 0.0583(7) Uani 1 1 d . . . . .
O8 O 0.33722(16) 0.6600(4) 0.8957(2) 0.0616(8) Uani 1 1 d . . . . .
O9 O 0.3238(2) 0.5300(5) 1.0200(2) 0.0800(10) Uani 1 1 d . . . . .
Pu1 Pu 0.24266(2) 0.64896(2) 0.75991(2) 0.03707(5) Uani 1 1 d . . . . .
HN1 H 0.321(3) 0.103(10) 0.076(5) 0.15(3) Uiso 1 1 d 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
C1 N4 1.321(7) . ?
C1 C2 1.336(7) . ?
C1 H1 0.9500 . ?
C2 C3 1.359(7) . ?
C2 H2 0.9500 . ?
C3 C4 1.366(8) . ?
C3 H3 0.9500 . ?
C4 C5 1.381(9) . ?
C4 H4A 0.9500 . ?
C5 N4 1.326(8) . ?
C5 H5 0.9500 . ?
N5A C6A 1.3900 . ?
N5A C10A 1.3900 . ?
N5A H5A 0.8800 . ?
C6A C7A 1.3900 . ?
C6A H6A 0.9500 . ?
C7A C8A 1.3900 . ?
C7A H7A 0.9500 . ?
C8A C9A 1.3900 . ?
C8A H8A 0.9500 . ?
C9A C10A 1.3900 . ?
C9A H9A 0.9500 . ?
C10A H10A 0.9500 . ?
N5B C6B 1.3900 . ?
N5B C10B 1.3900 . ?
N5B H6A1 0.8800 . ?
C6B C7B 1.3900 . ?
C6B H6B 0.9500 . ?
C7B C8B 1.3900 . ?
C7B H7B 0.9500 . ?
C8B C9B 1.3900 . ?
C8B H8B 0.9500 . ?
C9B C10B 1.3900 . ?
C9B H9B 0.9500 . ?
C10B H10B 0.9500 . ?
Cl1 Pu1 2.5996(11) . ?
Cl2 Pu1 2.6142(9) . ?
Cl3 Pu1 2.6261(10) . ?
N1 O3 1.202(4) . ?
N1 O2 1.267(4) . ?
N1 O1 1.273(4) . ?
N2 O6 1.205(4) . ?
N2 O5 1.264(4) . ?
N2 O4 1.268(4) . ?
N3 O9 1.197(4) . ?
N3 O7 1.267(4) . ?
N3 O8 1.282(5) . ?
N4 HN1 0.88(2) . ?
O1 Pu1 2.444(3) . ?
O2 Pu1 2.496(3) . ?
O4 Pu1 2.467(3) . ?
O5 Pu1 2.449(3) . ?
O7 Pu1 2.475(3) . ?
O8 Pu1 2.449(3) . ?

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
N4 C1 C2 119.4(5) . . ?
N4 C1 H1 120.3 . . ?
C2 C1 H1 120.3 . . ?
C1 C2 C3 120.1(5) . . ?
C1 C2 H2 120.0 . . ?
C3 C2 H2 120.0 . . ?
C2 C3 C4 120.5(5) . . ?
C2 C3 H3 119.7 . . ?
C4 C3 H3 119.7 . . ?
C3 C4 C5 117.8(5) . . ?
C3 C4 H4A 121.1 . . ?
C5 C4 H4A 121.1 . . ?
N4 C5 C4 119.3(5) . . ?
N4 C5 H5 120.4 . . ?
C4 C5 H5 120.4 . . ?
C6A N5A C10A 120.0 . . ?
C6A N5A H5A 120.0 . . ?
C10A N5A H5A 120.0 . . ?
C7A C6A N5A 120.0 . . ?
C7A C6A H6A 120.0 . . ?
N5A C6A H6A 120.0 . . ?
C6A C7A C8A 120.0 . . ?
C6A C7A H7A 120.0 . . ?
C8A C7A H7A 120.0 . . ?
C7A C8A C9A 120.0 . . ?
C7A C8A H8A 120.0 . . ?
C9A C8A H8A 120.0 . . ?
C8A C9A C10A 120.0 . . ?
C8A C9A H9A 120.0 . . ?
C10A C9A H9A 120.0 . . ?
C9A C10A N5A 120.0 . . ?
C9A C10A H10A 120.0 . . ?
N5A C10A H10A 120.0 . . ?
C6B N5B C10B 120.0 . . ?
C6B N5B H6A1 120.0 . . ?
C10B N5B H6A1 120.0 . . ?
C7B C6B N5B 120.0 . . ?
C7B C6B H6B 120.0 . . ?
N5B C6B H6B 120.0 . . ?
C6B C7B C8B 120.0 . . ?
C6B C7B H7B 120.0 . . ?
C8B C7B H7B 120.0 . . ?
C7B C8B C9B 120.0 . . ?
C7B C8B H8B 120.0 . . ?
C9B C8B H8B 120.0 . . ?
C10B C9B C8B 120.0 . . ?
C10B C9B H9B 120.0 . . ?
C8B C9B H9B 120.0 . . ?
C9B C10B N5B 120.0 . . ?
C9B C10B H10B 120.0 . . ?
N5B C10B H10B 120.0 . . ?
O3 N1 O2 123.0(4) . . ?
O3 N1 O1 122.6(4) . . ?
O2 N1 O1 114.4(3) . . ?
O6 N2 O5 122.8(4) . . ?
O6 N2 O4 121.6(4) . . ?
O5 N2 O4 115.6(3) . . ?
O9 N3 O7 123.6(4) . . ?
O9 N3 O8 122.3(4) . . ?
O7 N3 O8 114.0(3) . . ?
C1 N4 C5 123.0(5) . . ?
C1 N4 HN1 113(5) . . ?
C5 N4 HN1 121(5) . . ?
N1 O1 Pu1 98.4(2) . . ?
N1 O2 Pu1 96.1(2) . . ?
N2 O4 Pu1 95.6(2) . . ?
N2 O5 Pu1 96.6(2) . . ?
N3 O7 Pu1 96.6(2) . . ?
N3 O8 Pu1 97.4(2) . . ?
O1 Pu1 O8 71.36(10) . . ?
O1 Pu1 O5 72.43(10) . . ?
O8 Pu1 O5 74.43(10) . . ?
O1 Pu1 O4 69.30(10) . . ?
O8 Pu1 O4 120.09(10) . . ?
O5 Pu1 O4 51.67(10) . . ?
O1 Pu1 O7 118.04(10) . . ?
O8 Pu1 O7 51.47(10) . . ?
O5 Pu1 O7 71.27(10) . . ?
O4 Pu1 O7 117.92(10) . . ?
O1 Pu1 O2 51.18(9) . . ?
O8 Pu1 O2 69.83(11) . . ?
O5 Pu1 O2 119.89(10) . . ?
O4 Pu1 O2 113.11(10) . . ?
O7 Pu1 O2 115.30(10) . . ?
O1 Pu1 Cl1 126.15(7) . . ?
O8 Pu1 Cl1 87.01(8) . . ?
O5 Pu1 Cl1 148.13(8) . . ?
O4 Pu1 Cl1 152.89(8) . . ?
O7 Pu1 Cl1 76.89(8) . . ?
O2 Pu1 Cl1 75.26(7) . . ?
O1 Pu1 Cl2 144.18(7) . . ?
O8 Pu1 Cl2 124.34(8) . . ?
O5 Pu1 Cl2 81.12(8) . . ?
O4 Pu1 Cl2 75.43(8) . . ?
O7 Pu1 Cl2 73.55(7) . . ?
O2 Pu1 Cl2 158.57(8) . . ?
Cl1 Pu1 Cl2 88.74(4) . . ?
O1 Pu1 Cl3 88.16(8) . . ?
O8 Pu1 Cl3 146.13(8) . . ?
O5 Pu1 Cl3 125.61(7) . . ?
O4 Pu1 Cl3 73.97(7) . . ?
O7 Pu1 Cl3 153.37(8) . . ?
O2 Pu1 Cl3 76.31(8) . . ?
Cl1 Pu1 Cl3 83.77(4) . . ?
Cl2 Pu1 Cl3 88.03(3) . . ?

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
N4 C1 C2 C3 0.4(8) . . . . ?
C1 C2 C3 C4 0.0(8) . . . . ?
C2 C3 C4 C5 0.4(8) . . . . ?
C3 C4 C5 N4 -1.1(8) . . . . ?
C10A N5A C6A C7A 0.0 . . . . ?
N5A C6A C7A C8A 0.0 . . . . ?
C6A C7A C8A C9A 0.0 . . . . ?
C7A C8A C9A C10A 0.0 . . . . ?
C8A C9A C10A N5A 0.0 . . . . ?
C6A N5A C10A C9A 0.0 . . . . ?
C10B N5B C6B C7B 0.0 . . . . ?
N5B C6B C7B C8B 0.0 . . . . ?
C6B C7B C8B C9B 0.0 . . . . ?
C7B C8B C9B C10B 0.0 . . . . ?
C8B C9B C10B N5B 0.0 . . . . ?
C6B N5B C10B C9B 0.0 . . . . ?
C2 C1 N4 C5 -1.2(9) . . . . ?
C4 C5 N4 C1 1.6(9) . . . . ?
O3 N1 O1 Pu1 -179.4(3) . . . . ?
O2 N1 O1 Pu1 0.7(4) . . . . ?
O3 N1 O2 Pu1 179.5(3) . . . . ?
O1 N1 O2 Pu1 -0.7(3) . . . . ?
O6 N2 O4 Pu1 -172.4(4) . . . . ?
O5 N2 O4 Pu1 7.4(3) . . . . ?
O6 N2 O5 Pu1 172.3(4) . . . . ?
O4 N2 O5 Pu1 -7.5(4) . . . . ?
O9 N3 O7 Pu1 -173.3(4) . . . . ?
O8 N3 O7 Pu1 6.8(4) . . . . ?
O9 N3 O8 Pu1 173.2(4) . . . . ?
O7 N3 O8 Pu1 -6.8(4) . . . . ?

_refine_diff_density_max         0.772
_refine_diff_density_min         -0.832
_refine_diff_density_rms         0.097

####################################################################### 
# 
# 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_Compound_4
_database_code_depnum_ccdc_archive 'CCDC 1852700'
_audit_update_record             
;
2018-09-21 deposited with the CCDC.
2018-09-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         '(C5 H5 N Cl 1+)2, (Pu O5 N Cl3 2-)'
_chemical_formula_sum            'C10 H10 Cl5 N3 O5 Pu'
_exptl_crystal_recrystallization_method 'Evaporation from acidic aqueous media'
_chemical_melting_point          ?

_exptl_crystal_description       Blade
_exptl_crystal_colour            Yellow
_diffrn_ambient_temperature      298(2)
_chemical_formula_weight         671.46

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0015 0.0009 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.0998 0.0984 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0030 0.0019 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0056 0.0036 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pu Pu -13.5905 6.9468 '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'
_chemical_absolute_configuration ?

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

_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.
;

_cell_length_a                   6.7493(5)
_cell_length_b                   10.8107(9)
_cell_length_c                   14.1715(11)
_cell_angle_alpha                73.657(2)
_cell_angle_beta                 81.412(2)
_cell_angle_gamma                75.206(2)
_cell_volume                     956.00(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    18087
_cell_measurement_theta_min      4.744
_cell_measurement_theta_max      44.168
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.333
_exptl_crystal_F_000             620
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.075
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    5.149
_shelx_estimated_absorpt_T_min   0.627
_shelx_estimated_absorpt_T_max   0.783
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5704
_exptl_absorpt_correction_T_max  0.7447
_exptl_absorpt_process_details   'SADABS, Krause, et. al J. Appl. Cryst. 2015'
_exptl_absorpt_special_details   ?
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           AgK\a
_diffrn_radiation_wavelength     0.56086
_diffrn_source                   'Microfocus '
_diffrn_source_type              Bruker
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'Omega and Phi Scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            18087
_diffrn_reflns_av_unetI/netI     0.0361
_diffrn_reflns_av_R_equivalents  0.0382
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.372
_diffrn_reflns_theta_max         22.097
_diffrn_reflns_theta_full        19.665
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             4740
_reflns_number_gt                4364
_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       'APEX, Bruker-AXS'
_computing_cell_refinement       'SAINT, Bruker-AXS'
_computing_data_reduction        'SAINT, Bruker-AXS'
_computing_structure_solution    'SIR92 (Gualardi, 1994)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'WINGX (Farrugia, 2012)'
_computing_publication_material  'Crystal Maker (Palmer, 2009)'
_refine_special_details          
;
The final refinement features several A and C level alerts related to residual electron
density. We have ruled out the possibility of twinning, residual solvent molecules and 
unidentified atoms. The issue is most likely caused by absorption owing to the presence 
of heavy atoms. 

;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+10.7047P] 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         4740
_refine_ls_number_parameters     217
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0716
_refine_ls_R_factor_gt           0.0646
_refine_ls_wR_factor_ref         0.1134
_refine_ls_wR_factor_gt          0.1114
_refine_ls_goodness_of_fit_ref   1.341
_refine_ls_restrained_S_all      1.341
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pu1 Pu 0.21349(6) 0.79570(3) 0.22740(3) 0.03320(11) Uani 1 1 d . . . . .
Cl1 Cl 0.3409(6) 0.6292(3) 0.1105(2) 0.0711(10) Uani 1 1 d . . . . .
Cl2 Cl 0.0932(7) 0.9125(3) 0.3756(2) 0.0826(12) Uani 1 1 d . . . . .
Cl3 Cl 0.2528(5) 0.5682(2) 0.37253(19) 0.0548(7) Uani 1 1 d . . . . .
O1 O 0.4668(13) 0.7971(8) 0.2347(6) 0.064(2) Uani 1 1 d . . . . .
O2 O -0.0419(12) 0.7963(8) 0.2188(6) 0.064(2) Uani 1 1 d . . . . .
O3 O 0.2397(16) 0.9245(8) 0.0509(6) 0.071(3) Uani 1 1 d . . . . .
O4 O 0.1481(15) 1.0449(7) 0.1530(6) 0.067(2) Uani 1 1 d . . . . .
O5 O 0.2160(18) 1.1359(9) -0.0017(6) 0.085(3) Uani 1 1 d . . . . .
N1 N 0.2001(16) 1.0381(9) 0.0653(7) 0.055(2) Uani 1 1 d . . . . .
Cl4 Cl 0.9146(6) 0.4059(4) 0.1000(2) 0.0842(11) Uani 1 1 d . . . . .
N2 N 0.8354(17) 0.3652(15) 0.4188(8) 0.077(3) Uani 1 1 d . . . . .
HN1 H 0.8196 0.3555 0.4816 0.092 Uiso 1 1 d R U . . .
C1 C 0.900(2) 0.2586(15) 0.3850(9) 0.070(4) Uani 1 1 d . . . . .
H1 H 0.9288 0.1752 0.4286 0.084 Uiso 1 1 calc R U . . .
C2 C 0.9254(19) 0.2717(11) 0.2873(8) 0.054(3) Uani 1 1 d . . . . .
H2 H 0.9717 0.1972 0.2627 0.065 Uiso 1 1 calc R U . . .
C3 C 0.8827(16) 0.3950(10) 0.2238(8) 0.048(2) Uani 1 1 d . . . . .
C4 C 0.816(2) 0.5047(12) 0.2589(12) 0.070(4) Uani 1 1 d . . . . .
H4 H 0.7871 0.5888 0.2164 0.083 Uiso 1 1 calc R U . . .
C5 C 0.793(2) 0.4867(17) 0.3604(14) 0.086(5) Uani 1 1 d . . . . .
H5 H 0.7486 0.5592 0.3874 0.103 Uiso 1 1 calc R U . . .
Cl5 Cl 0.4185(7) 0.1677(4) 0.4263(2) 0.0895(12) Uani 1 1 d . . . . .
N3 N 0.5648(14) 0.1898(9) 0.1093(7) 0.052(2) Uani 1 1 d . . . . .
HN2 H 0.5998 0.1950 0.0471 0.062 Uiso 1 1 d R U . . .
C6 C 0.4694(17) 0.2998(10) 0.1373(8) 0.050(3) Uani 1 1 d . . . . .
H6 H 0.4351 0.3795 0.0900 0.059 Uiso 1 1 calc R U . . .
C7 C 0.4218(17) 0.2956(10) 0.2353(8) 0.050(3) Uani 1 1 d . . . . .
H7 H 0.3573 0.3717 0.2559 0.060 Uiso 1 1 calc R U . . .
C8 C 0.4730(18) 0.1746(11) 0.3026(8) 0.051(3) Uani 1 1 d . . . . .
C9 C 0.569(2) 0.0621(11) 0.2730(9) 0.062(3) Uani 1 1 d . . . . .
H9 H 0.6027 -0.0191 0.3188 0.074 Uiso 1 1 calc R U . . .
C10 C 0.6138(19) 0.0725(10) 0.1742(10) 0.059(3) Uani 1 1 d . . . . .
H10 H 0.6785 -0.0023 0.1520 0.071 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
Pu1 O1 1.732(8) . ?
Pu1 O2 1.744(8) . ?
Pu1 O3 2.502(8) . ?
Pu1 O4 2.549(7) . ?
Pu1 Cl2 2.669(3) . ?
Pu1 Cl1 2.680(3) . ?
Pu1 Cl3 2.708(3) . ?
Pu1 N1 2.951(9) . ?
O3 N1 1.257(11) . ?
O4 N1 1.257(11) . ?
O5 N1 1.222(11) . ?
Cl4 C3 1.709(11) . ?
N2 C1 1.318(18) . ?
N2 C5 1.33(2) . ?
N2 HN1 0.8598 . ?
C1 C2 1.341(16) . ?
C1 H1 0.9300 . ?
C2 C3 1.370(14) . ?
C2 H2 0.9300 . ?
C3 C4 1.360(16) . ?
C4 C5 1.39(2) . ?
C4 H4 0.9300 . ?
C5 H5 0.9300 . ?
Cl5 C8 1.722(11) . ?
N3 C10 1.335(14) . ?
N3 C6 1.336(13) . ?
N3 HN2 0.8676 . ?
C6 C7 1.369(14) . ?
C6 H6 0.9300 . ?
C7 C8 1.380(14) . ?
C7 H7 0.9300 . ?
C8 C9 1.371(15) . ?
C9 C10 1.366(17) . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Pu1 O2 179.2(4) . . ?
O1 Pu1 O3 89.1(4) . . ?
O2 Pu1 O3 90.2(4) . . ?
O1 Pu1 O4 88.1(3) . . ?
O2 Pu1 O4 91.2(3) . . ?
O3 Pu1 O4 50.0(2) . . ?
O1 Pu1 Cl2 90.4(3) . . ?
O2 Pu1 Cl2 89.6(3) . . ?
O3 Pu1 Cl2 122.40(19) . . ?
O4 Pu1 Cl2 72.45(19) . . ?
O1 Pu1 Cl1 89.8(3) . . ?
O2 Pu1 Cl1 90.4(3) . . ?
O3 Pu1 Cl1 70.23(19) . . ?
O4 Pu1 Cl1 120.19(19) . . ?
Cl2 Pu1 Cl1 167.36(8) . . ?
O1 Pu1 Cl3 89.7(3) . . ?
O2 Pu1 Cl3 91.1(3) . . ?
O3 Pu1 Cl3 153.18(19) . . ?
O4 Pu1 Cl3 156.71(19) . . ?
Cl2 Pu1 Cl3 84.40(8) . . ?
Cl1 Pu1 Cl3 82.97(8) . . ?
O1 Pu1 N1 87.0(3) . . ?
O2 Pu1 N1 92.3(3) . . ?
O3 Pu1 N1 25.0(2) . . ?
O4 Pu1 N1 25.1(2) . . ?
Cl2 Pu1 N1 97.5(2) . . ?
Cl1 Pu1 N1 95.1(2) . . ?
Cl3 Pu1 N1 176.2(2) . . ?
N1 O3 Pu1 97.9(6) . . ?
N1 O4 Pu1 95.6(6) . . ?
O5 N1 O3 121.9(10) . . ?
O5 N1 O4 121.9(10) . . ?
O3 N1 O4 116.2(9) . . ?
O5 N1 Pu1 173.4(9) . . ?
O3 N1 Pu1 57.1(5) . . ?
O4 N1 Pu1 59.3(5) . . ?
C1 N2 C5 123.0(12) . . ?
C1 N2 HN1 118.5 . . ?
C5 N2 HN1 118.5 . . ?
N2 C1 C2 119.4(13) . . ?
N2 C1 H1 120.3 . . ?
C2 C1 H1 120.3 . . ?
C1 C2 C3 119.8(12) . . ?
C1 C2 H2 120.1 . . ?
C3 C2 H2 120.1 . . ?
C4 C3 C2 120.6(11) . . ?
C4 C3 Cl4 121.5(10) . . ?
C2 C3 Cl4 117.9(9) . . ?
C3 C4 C5 117.6(13) . . ?
C3 C4 H4 121.2 . . ?
C5 C4 H4 121.2 . . ?
N2 C5 C4 119.5(12) . . ?
N2 C5 H5 120.2 . . ?
C4 C5 H5 120.2 . . ?
C10 N3 C6 122.2(10) . . ?
C10 N3 HN2 118.7 . . ?
C6 N3 HN2 119.0 . . ?
N3 C6 C7 120.2(10) . . ?
N3 C6 H6 119.9 . . ?
C7 C6 H6 119.9 . . ?
C6 C7 C8 117.7(10) . . ?
C6 C7 H7 121.1 . . ?
C8 C7 H7 121.1 . . ?
C9 C8 C7 121.5(10) . . ?
C9 C8 Cl5 120.0(9) . . ?
C7 C8 Cl5 118.4(9) . . ?
C10 C9 C8 118.1(10) . . ?
C10 C9 H9 121.0 . . ?
C8 C9 H9 121.0 . . ?
N3 C10 C9 120.2(10) . . ?
N3 C10 H10 119.9 . . ?
C9 C10 H10 119.9 . . ?

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
Pu1 O3 N1 O5 172.3(10) . . . . ?
Pu1 O3 N1 O4 -6.0(11) . . . . ?
Pu1 O4 N1 O5 -172.4(10) . . . . ?
Pu1 O4 N1 O3 5.9(11) . . . . ?
C5 N2 C1 C2 0(2) . . . . ?
N2 C1 C2 C3 0(2) . . . . ?
C1 C2 C3 C4 0.4(19) . . . . ?
C1 C2 C3 Cl4 -179.3(10) . . . . ?
C2 C3 C4 C5 -0.2(19) . . . . ?
Cl4 C3 C4 C5 179.6(10) . . . . ?
C1 N2 C5 C4 0(2) . . . . ?
C3 C4 C5 N2 0(2) . . . . ?
C10 N3 C6 C7 1.3(17) . . . . ?
N3 C6 C7 C8 -1.0(17) . . . . ?
C6 C7 C8 C9 0.3(18) . . . . ?
C6 C7 C8 Cl5 178.9(9) . . . . ?
C7 C8 C9 C10 0.1(19) . . . . ?
Cl5 C8 C9 C10 -178.5(10) . . . . ?
C6 N3 C10 C9 -0.9(18) . . . . ?
C8 C9 C10 N3 0.1(19) . . . . ?

_refine_diff_density_max         2.114
_refine_diff_density_min         -3.800
_refine_diff_density_rms         0.198

