# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_p1

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
  
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_structural     (C4H7N2)((UO2)(AsO4))
_chemical_formula_moiety         'As O6 U, C4 N2'
_chemical_formula_sum            'C4 As N2 O6 U'
_chemical_formula_weight         485.01

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'
As As 0.0499 2.0058 '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'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P -1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.170(3)
_cell_length_b                   7.181(3)
_cell_length_c                   9.831(4)
_cell_angle_alpha                73.511(4)
_cell_angle_beta                 73.892(4)
_cell_angle_gamma                89.122(4)
_cell_volume                     465.2(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    176(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      27.59

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    3.463
_exptl_crystal_density_method    none
_exptl_crystal_F_000             422
_exptl_absorpt_coefficient_mu    20.980
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6810
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   ?

_exptl_special_details           
;  
;

_diffrn_ambient_temperature      176(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'BRUKER AXS Apex-2 CCD-4k'
_diffrn_measurement_method       'phi-omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            5568
_diffrn_reflns_av_R_equivalents  0.0471
_diffrn_reflns_av_sigmaI/netI    0.0615
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.25
_diffrn_reflns_theta_max         27.59
_reflns_number_total             2139
_reflns_number_gt                1848
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0252P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    none
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2139
_refine_ls_number_parameters     67
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0412
_refine_ls_R_factor_gt           0.0319
_refine_ls_wR_factor_ref         0.0659
_refine_ls_wR_factor_gt          0.0627
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_restrained_S_all      1.013
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.70629(4) 0.22113(4) 0.10114(3) 0.00632(9) Uani 1 1 d . . .
As1 As 0.75331(11) 0.74802(11) 0.00794(9) 0.00641(17) Uani 1 1 d . . .
O1 O 0.7821(7) 0.3105(7) -0.0970(6) 0.0104(12) Uiso 1 1 d . . .
O2 O 0.7333(7) 0.5249(7) 0.1270(6) 0.0085(11) Uiso 1 1 d . . .
O3 O 0.9814(8) 0.8092(7) -0.1053(6) 0.0104(12) Uiso 1 1 d . . .
O4 O 0.6145(7) 0.7486(7) -0.1067(6) 0.0093(11) Uiso 1 1 d . . .
O5 O 0.6255(7) 0.1392(7) 0.2994(6) 0.0085(11) Uiso 1 1 d . . .
O6 O 0.6803(8) 0.9069(8) 0.1031(6) 0.0104(12) Uiso 1 1 d . . .
N1 N 0.1290(9) 0.7181(9) 0.4727(7) 0.0107(14) Uiso 1 1 d . . .
N2 N -0.1445(9) 0.7199(9) 0.6309(7) 0.0104(14) Uiso 1 1 d . . .
C1 C 0.0355(12) 0.6606(12) 0.6152(9) 0.0133(17) Uiso 1 1 d . . .
C2 C 0.0048(12) 0.8160(12) 0.3927(9) 0.0135(18) Uiso 1 1 d . . .
C3 C -0.1687(12) 0.8164(12) 0.4949(9) 0.0171(19) Uiso 1 1 d . . .
C4 C 0.3366(13) 0.6944(13) 0.4077(10) 0.0189(19) 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 O5 1.793(5) . ?
U1 O1 1.793(5) . ?
U1 O3 2.257(5) 2_765 ?
U1 O6 2.261(5) 1_545 ?
U1 O2 2.283(5) . ?
U1 O4 2.294(5) 2_665 ?
As1 O6 1.663(5) . ?
As1 O2 1.675(5) . ?
As1 O3 1.685(5) . ?
As1 O4 1.697(5) . ?
O3 U1 2.257(5) 2_765 ?
O4 U1 2.294(5) 2_665 ?
O6 U1 2.261(5) 1_565 ?
N1 C1 1.320(10) . ?
N1 C2 1.400(10) . ?
N1 C4 1.476(11) . ?
N2 C1 1.334(10) . ?
N2 C3 1.378(10) . ?
C2 C3 1.365(11) . ?

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
O5 U1 O1 178.0(2) . . ?
O5 U1 O3 90.4(2) . 2_765 ?
O1 U1 O3 90.8(2) . 2_765 ?
O5 U1 O6 88.0(2) . 1_545 ?
O1 U1 O6 93.6(2) . 1_545 ?
O3 U1 O6 90.21(19) 2_765 1_545 ?
O5 U1 O2 85.7(2) . . ?
O1 U1 O2 92.7(2) . . ?
O3 U1 O2 87.64(18) 2_765 . ?
O6 U1 O2 173.36(18) 1_545 . ?
O5 U1 O4 87.4(2) . 2_665 ?
O1 U1 O4 91.3(2) . 2_665 ?
O3 U1 O4 177.72(19) 2_765 2_665 ?
O6 U1 O4 90.35(18) 1_545 2_665 ?
O2 U1 O4 91.56(18) . 2_665 ?
O6 As1 O2 108.9(3) . . ?
O6 As1 O3 111.5(3) . . ?
O2 As1 O3 111.9(3) . . ?
O6 As1 O4 110.8(3) . . ?
O2 As1 O4 108.9(2) . . ?
O3 As1 O4 104.7(3) . . ?
As1 O2 U1 132.3(3) . . ?
As1 O3 U1 140.4(3) . 2_765 ?
As1 O4 U1 137.3(3) . 2_665 ?
As1 O6 U1 145.2(3) . 1_565 ?
C1 N1 C2 109.7(7) . . ?
C1 N1 C4 125.3(7) . . ?
C2 N1 C4 124.9(7) . . ?
C1 N2 C3 110.4(7) . . ?
N1 C1 N2 107.5(7) . . ?
C3 C2 N1 106.1(7) . . ?
C2 C3 N2 106.3(7) . . ?

_diffrn_measured_fraction_theta_max 0.987
_diffrn_reflns_theta_full        27.59
_diffrn_measured_fraction_theta_full 0.987
_refine_diff_density_max         1.281
_refine_diff_density_min         -1.913
_refine_diff_density_rms         0.318


_database_code_depnum_ccdc_archive 'CCDC 984852'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_pnmax

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
  
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_structural     (C8H15N2)2((UO2)4(SeO3)5)
_chemical_formula_moiety         'O23 Se5 U4, 2(C8 N2)'
_chemical_formula_sum            'C16 N4 O23 Se5 U4'
_chemical_formula_weight         1963.12

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

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Pnma

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

_cell_length_a                   18.860(2)
_cell_length_b                   18.010(2)
_cell_length_c                   11.1408(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3784.3(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    174(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      27.54

_exptl_crystal_description       Prismatic
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    3.446
_exptl_crystal_density_method    none
_exptl_crystal_F_000             3384
_exptl_absorpt_coefficient_mu    21.960
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4216
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      174(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'BRUKER AXS Apex-2 CCD-4k'
_diffrn_measurement_method       'phi-omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            42673
_diffrn_reflns_av_R_equivalents  0.0898
_diffrn_reflns_av_sigmaI/netI    0.0465
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.12
_diffrn_reflns_theta_max         27.54
_reflns_number_total             4507
_reflns_number_gt                3631
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0153P)²+181.9279P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    none
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4507
_refine_ls_number_parameters     137
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0680
_refine_ls_R_factor_gt           0.0499
_refine_ls_wR_factor_ref         0.1103
_refine_ls_wR_factor_gt          0.1046
_refine_ls_goodness_of_fit_ref   1.149
_refine_ls_restrained_S_all      1.149
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.21103(3) 0.05424(3) 0.55188(4) 0.01664(12) Uani 1 1 d . . .
U2 U 0.18683(4) 0.2500 0.74116(6) 0.01520(16) Uani 1 2 d S . .
U3 U 0.16690(4) 0.2500 1.12141(6) 0.01513(16) Uani 1 2 d S . .
Se1 Se 0.20289(10) 0.2500 0.44329(15) 0.0159(4) Uani 1 2 d S . .
Se2 Se 0.31347(8) -0.05613(7) 0.73906(11) 0.0215(3) Uani 1 1 d . . .
Se3 Se 0.18335(8) 0.09048(7) 0.89505(11) 0.0196(3) Uani 1 1 d . . .
O1 O 0.1874(5) 0.1121(5) 0.7441(8) 0.0203(19) Uiso 1 1 d . . .
O2 O 0.1776(5) 0.1835(5) 0.5482(8) 0.0177(19) Uiso 1 1 d . . .
O3 O 0.1950(5) 0.1816(5) 0.9350(8) 0.019(2) Uiso 1 1 d . . .
O4 O 0.1429(7) 0.2500 0.3373(11) 0.018(3) Uiso 1 2 d S . .
O5 O 0.2615(5) 0.0501(5) 0.9218(8) 0.023(2) Uiso 1 1 d . . .
O6 O 0.2788(7) 0.2500 0.7240(13) 0.025(3) Uiso 1 2 d S . .
O7 O 0.0758(7) 0.2500 1.0872(12) 0.020(3) Uiso 1 2 d S . .
O8 O 0.2317(5) -0.0427(5) 0.6781(8) 0.023(2) Uiso 1 1 d . . .
O9 O 0.0951(7) 0.2500 0.7554(13) 0.026(3) Uiso 1 2 d S . .
O10 O 0.3021(5) 0.0777(6) 0.5622(9) 0.030(2) Uiso 1 1 d . . .
O11 O 0.2586(7) 0.2500 1.1618(12) 0.023(3) Uiso 1 2 d S . .
O12 O 0.3476(5) -0.1233(5) 0.6524(9) 0.024(2) Uiso 1 1 d . . .
O13 O 0.1220(5) 0.0260(6) 0.5394(9) 0.029(2) Uiso 1 1 d . . .
O14 O 0.2892(6) -0.1039(6) 0.8621(9) 0.030(2) Uiso 1 1 d . . .
N1 N 0.0787(11) -0.1475(12) 0.7002(19) 0.073(6) Uiso 1 1 d . . .
N2 N 0.0585(12) -0.1440(12) 0.507(2) 0.081(6) Uiso 1 1 d . . .
C1 C 0.1086(13) -0.1435(13) 0.587(2) 0.066(6) Uiso 1 1 d . . .
C2 C 0.0057(14) 0.1518(15) 0.430(2) 0.073(7) Uiso 1 1 d . . .
C3 C 0.1110(17) -0.1376(18) 0.824(3) 0.103(10) Uiso 1 1 d . . .
C4 C 0.0721(18) -0.1448(19) 0.383(3) 0.106(10) Uiso 1 1 d . . .
C5 C 0.5039(19) -0.149(2) 0.810(3) 0.116(12) Uiso 1 1 d . . .
C6 C -0.0281(18) 0.0879(19) 0.676(3) 0.107(10) Uiso 1 1 d . . .
C7 C 0.463(3) 0.111(3) 0.676(4) 0.178(19) Uiso 1 1 d . . .
C8 C 0.493(3) 0.042(3) 0.626(4) 0.170(18) 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 O13 1.760(10) . ?
U1 O10 1.772(10) . ?
U1 O8 2.275(10) . ?
U1 O14 2.296(10) 2_554 ?
U1 O2 2.412(9) . ?
U1 O1 2.423(9) . ?
U1 O5 2.429(10) 2_554 ?
U1 Se2 3.4687(14) . ?
U2 O9 1.737(14) . ?
U2 O6 1.745(14) . ?
U2 O2 2.467(9) 7_565 ?
U2 O2 2.467(9) . ?
U2 O1 2.483(9) 7_565 ?
U2 O1 2.483(9) . ?
U2 O3 2.491(9) . ?
U2 O3 2.491(9) 7_565 ?
U2 Se1 3.3323(19) . ?
U2 Se3 3.3463(13) . ?
U2 Se3 3.3464(13) 7_565 ?
U3 O7 1.759(13) . ?
U3 O11 1.788(14) . ?
U3 O12 2.325(10) 8_666 ?
U3 O12 2.325(10) 2 ?
U3 O4 2.448(13) 1_556 ?
U3 O3 2.472(9) . ?
U3 O3 2.472(9) 7_565 ?
Se1 O4 1.635(13) . ?
Se1 O2 1.740(9) 7_565 ?
Se1 O2 1.740(9) . ?
Se2 O12 1.676(10) . ?
Se2 O14 1.683(10) . ?
Se2 O8 1.703(10) . ?
Se3 O5 1.670(10) . ?
Se3 O3 1.714(9) . ?
Se3 O1 1.728(9) . ?
O4 U3 2.448(13) 1_554 ?
O5 U1 2.429(10) 2 ?
O12 U3 2.325(10) 2_554 ?
O14 U1 2.296(10) 2 ?
N1 C1 1.39(3) . ?
N1 C5 1.41(4) 6_557 ?
N1 C3 1.52(3) . ?
N2 C1 1.30(3) . ?
N2 C4 1.40(4) . ?
N2 C2 1.41(3) 5_556 ?
C2 C5 1.35(4) 2_554 ?
C2 N2 1.41(3) 5_556 ?
C4 C6 1.48(4) 5_556 ?
C5 C2 1.35(4) 2 ?
C5 N1 1.41(4) 6_657 ?
C6 C4 1.48(4) 5_556 ?
C6 C7 1.71(5) 6_557 ?
C7 C8 1.47(6) . ?
C7 C6 1.71(5) 6_657 ?

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
O13 U1 O10 176.9(5) . . ?
O13 U1 O8 89.4(4) . . ?
O10 U1 O8 88.7(4) . . ?
O13 U1 O14 92.2(4) . 2_554 ?
O10 U1 O14 88.2(4) . 2_554 ?
O8 U1 O14 150.3(4) . 2_554 ?
O13 U1 O2 91.7(4) . . ?
O10 U1 O2 91.4(4) . . ?
O8 U1 O2 142.7(3) . . ?
O14 U1 O2 66.9(3) 2_554 . ?
O13 U1 O1 91.1(4) . . ?
O10 U1 O1 91.0(4) . . ?
O8 U1 O1 79.4(3) . . ?
O14 U1 O1 130.2(3) 2_554 . ?
O2 U1 O1 63.4(3) . . ?
O13 U1 O5 86.2(4) . 2_554 ?
O10 U1 O5 90.9(4) . 2_554 ?
O8 U1 O5 74.8(3) . 2_554 ?
O14 U1 O5 75.7(3) 2_554 2_554 ?
O2 U1 O5 142.4(3) . 2_554 ?
O1 U1 O5 154.1(3) . 2_554 ?
O13 U1 Se2 114.4(3) . . ?
O10 U1 Se2 63.8(3) . . ?
O8 U1 Se2 25.0(2) . . ?
O14 U1 Se2 141.1(3) 2_554 . ?
O2 U1 Se2 135.1(2) . . ?
O1 U1 Se2 79.5(2) . . ?
O5 U1 Se2 78.2(2) 2_554 . ?
O9 U2 O6 178.9(7) . . ?
O9 U2 O2 90.5(5) . 7_565 ?
O6 U2 O2 88.5(5) . 7_565 ?
O9 U2 O2 90.5(5) . . ?
O6 U2 O2 88.5(5) . . ?
O2 U2 O2 58.1(4) 7_565 . ?
O9 U2 O1 90.2(2) . 7_565 ?
O6 U2 O1 89.8(2) . 7_565 ?
O2 U2 O1 61.7(3) 7_565 7_565 ?
O2 U2 O1 119.8(3) . 7_565 ?
O9 U2 O1 90.2(2) . . ?
O6 U2 O1 89.8(2) . . ?
O2 U2 O1 119.8(3) 7_565 . ?
O2 U2 O1 61.7(3) . . ?
O1 U2 O1 178.4(4) 7_565 . ?
O9 U2 O3 89.0(5) . . ?
O6 U2 O3 91.9(5) . . ?
O2 U2 O3 179.2(3) 7_565 . ?
O2 U2 O3 121.3(3) . . ?
O1 U2 O3 118.9(3) 7_565 . ?
O1 U2 O3 59.6(3) . . ?
O9 U2 O3 89.0(5) . 7_565 ?
O6 U2 O3 91.9(5) . 7_565 ?
O2 U2 O3 121.3(3) 7_565 7_565 ?
O2 U2 O3 179.2(3) . 7_565 ?
O1 U2 O3 59.6(3) 7_565 7_565 ?
O1 U2 O3 118.9(3) . 7_565 ?
O3 U2 O3 59.3(4) . 7_565 ?
O9 U2 Se1 100.4(5) . . ?
O6 U2 Se1 78.5(5) . . ?
O2 U2 Se1 30.5(2) 7_565 . ?
O2 U2 Se1 30.5(2) . . ?
O1 U2 Se1 90.7(2) 7_565 . ?
O1 U2 Se1 90.7(2) . . ?
O3 U2 Se1 149.1(2) . . ?
O3 U2 Se1 149.1(2) 7_565 . ?
O9 U2 Se3 86.2(2) . . ?
O6 U2 Se3 94.3(2) . . ?
O2 U2 Se3 149.5(2) 7_565 . ?
O2 U2 Se3 91.6(2) . . ?
O1 U2 Se3 148.4(2) 7_565 . ?
O1 U2 Se3 30.1(2) . . ?
O3 U2 Se3 29.8(2) . . ?
O3 U2 Se3 89.0(2) 7_565 . ?
Se1 U2 Se3 120.80(2) . . ?
O9 U2 Se3 86.2(2) . 7_565 ?
O6 U2 Se3 94.3(2) . 7_565 ?
O2 U2 Se3 91.6(2) 7_565 7_565 ?
O2 U2 Se3 149.5(2) . 7_565 ?
O1 U2 Se3 30.1(2) 7_565 7_565 ?
O1 U2 Se3 148.4(2) . 7_565 ?
O3 U2 Se3 89.0(2) . 7_565 ?
O3 U2 Se3 29.8(2) 7_565 7_565 ?
Se1 U2 Se3 120.80(2) . 7_565 ?
Se3 U2 Se3 118.31(5) . 7_565 ?
O7 U3 O11 177.9(6) . . ?
O7 U3 O12 85.3(3) . 8_666 ?
O11 U3 O12 94.4(3) . 8_666 ?
O7 U3 O12 85.3(3) . 2 ?
O11 U3 O12 94.4(3) . 2 ?
O12 U3 O12 158.2(5) 8_666 2 ?
O7 U3 O4 91.8(5) . 1_556 ?
O11 U3 O4 86.1(5) . 1_556 ?
O12 U3 O4 80.3(2) 8_666 1_556 ?
O12 U3 O4 80.3(2) 2 1_556 ?
O7 U3 O3 91.6(4) . . ?
O11 U3 O3 90.2(4) . . ?
O12 U3 O3 129.8(3) 8_666 . ?
O12 U3 O3 70.2(3) 2 . ?
O4 U3 O3 149.9(2) 1_556 . ?
O7 U3 O3 91.6(4) . 7_565 ?
O11 U3 O3 90.2(4) . 7_565 ?
O12 U3 O3 70.2(3) 8_666 7_565 ?
O12 U3 O3 129.8(3) 2 7_565 ?
O4 U3 O3 149.9(2) 1_556 7_565 ?
O3 U3 O3 59.8(4) . 7_565 ?
O4 Se1 O2 107.2(4) . 7_565 ?
O4 Se1 O2 107.2(4) . . ?
O2 Se1 O2 87.0(6) 7_565 . ?
O4 Se1 U2 131.0(5) . . ?
O2 Se1 U2 46.1(3) 7_565 . ?
O2 Se1 U2 46.1(3) . . ?
O12 Se2 O14 101.8(5) . . ?
O12 Se2 O8 102.7(5) . . ?
O14 Se2 O8 98.7(5) . . ?
O12 Se2 U1 106.3(3) . . ?
O14 Se2 U1 129.2(4) . . ?
O8 Se2 U1 34.3(3) . . ?
O5 Se3 O3 104.9(5) . . ?
O5 Se3 O1 103.5(4) . . ?
O3 Se3 O1 91.8(4) . . ?
O5 Se3 U2 116.6(3) . . ?
O3 Se3 U2 46.3(3) . . ?
O1 Se3 U2 46.1(3) . . ?
Se3 O1 U1 140.5(5) . . ?
Se3 O1 U2 103.8(4) . . ?
U1 O1 U2 114.8(4) . . ?
Se1 O2 U1 127.2(4) . . ?
Se1 O2 U2 103.4(4) . . ?
U1 O2 U2 115.8(3) . . ?
Se3 O3 U3 131.9(5) . . ?
Se3 O3 U2 103.9(4) . . ?
U3 O3 U2 117.9(4) . . ?
Se1 O4 U3 125.6(7) . 1_554 ?
Se3 O5 U1 129.2(5) . 2 ?
Se2 O8 U1 120.7(5) . . ?
Se2 O12 U3 138.5(5) . 2_554 ?
Se2 O14 U1 123.4(5) . 2 ?
C1 N1 C5 109(2) . 6_557 ?
C1 N1 C3 131(2) . . ?
C5 N1 C3 118(2) 6_557 . ?
C1 N2 C4 123(3) . . ?
C1 N2 C2 106(2) . 5_556 ?
C4 N2 C2 130(3) . 5_556 ?
N2 C1 N1 109(2) . . ?
C5 C2 N2 112(3) 2_554 5_556 ?
N2 C4 C6 109(3) . 5_556 ?
C2 C5 N1 102(3) 2 6_657 ?
C4 C6 C7 102(3) 5_556 6_557 ?
C8 C7 C6 97(4) . 6_657 ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        27.54
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         5.895
_refine_diff_density_min         -2.083
_refine_diff_density_rms         0.378

_database_code_depnum_ccdc_archive 'CCDC 984853'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_p21n

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_structural     (C6H11N2)2[(UO2)3(C2H5PO4)4]
_chemical_formula_moiety         'C8 O22 P4 U3, 2(C6 N2)'
_chemical_formula_sum            'C20 N4 O22 P4 U3'
_chemical_formula_weight         1486.21

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'
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'
P P 0.1023 0.0942 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'

loop_
_symmetry_equiv_pos_as_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                   9.954(7)
_cell_length_b                   10.264(7)
_cell_length_c                   19.566(14)
_cell_angle_alpha                90.00
_cell_angle_beta                 101.758(10)
_cell_angle_gamma                90.00
_cell_volume                     1957(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    174(2)
_cell_measurement_reflns_used    823
_cell_measurement_theta_min      2.14
_cell_measurement_theta_max      27.43

_exptl_crystal_description       prismatic
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    2.522
_exptl_crystal_density_method    none
_exptl_crystal_F_000             1320
_exptl_absorpt_coefficient_mu    12.628
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.473
_exptl_absorpt_correction_T_max  0.603
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      174(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'BRUKER AXS Apex-2 CCD-4k'
_diffrn_measurement_method       'phi-omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            22325
_diffrn_reflns_av_R_equivalents  0.1369
_diffrn_reflns_av_sigmaI/netI    0.1171
_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       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.13
_diffrn_reflns_theta_max         27.34
_reflns_number_total             4427
_reflns_number_gt                1909
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0395P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    none
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4427
_refine_ls_number_parameters     181
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1448
_refine_ls_R_factor_gt           0.0497
_refine_ls_wR_factor_ref         0.1326
_refine_ls_wR_factor_gt          0.1014
_refine_ls_goodness_of_fit_ref   0.979
_refine_ls_restrained_S_all      0.982
_refine_ls_shift/su_max          0.028
_refine_ls_shift/su_mean         0.001

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.5000 0.5000 0.0000 0.01873(18) Uani 1 2 d S . .
U2 U 0.82830(5) 0.50495(6) 0.25424(3) 0.02216(16) Uani 1 1 d . . .
P1 P 0.6467(4) 0.7389(4) 0.1272(2) 0.0236(11) Uani 1 1 d . . .
P2 P 0.6980(5) 0.2702(4) 0.1210(2) 0.0334(13) Uani 1 1 d . . .
O1 O 0.5752(12) 0.3398(9) 0.0794(6) 0.039(3) Uani 1 1 d . . .
O2 O 0.5315(11) 0.6514(9) 0.0890(5) 0.027(3) Uani 1 1 d . . .
O3 O 0.7605(11) 0.6639(10) 0.1729(6) 0.032(3) Uani 1 1 d . . .
O4 O 0.6703(10) 0.5217(10) -0.0113(5) 0.031(3) Uani 1 1 d . . .
O5 O 0.6571(10) 0.4729(9) 0.2629(6) 0.035(3) Uani 1 1 d . . .
O6 O 0.5867(11) 0.8436(9) 0.1682(5) 0.027(3) Uani 1 1 d . . .
O7 O 0.6545(12) 0.1593(11) 0.1614(6) 0.042(3) Uani 1 1 d . . .
O8 O 0.9992(10) 0.5342(9) 0.2450(5) 0.032(3) Uani 1 1 d . . .
O9 O 0.2803(12) 1.1915(10) -0.0723(6) 0.036(3) Uani 1 1 d . . .
O10 O 0.7993(12) 0.3596(10) 0.1644(6) 0.040(3) Uani 1 1 d . . .
O11 O 0.7680(15) 0.2130(12) 0.0622(7) 0.057(4) Uani 1 1 d . . .
N1 N 1.4112(16) 0.2032(14) 0.3856(8) 0.050(4) Uiso 1 1 d . . .
N2 N 1.3366(15) 0.3432(13) 0.3029(8) 0.043(4) Uiso 1 1 d . . .
C1 C 0.3753(18) 1.1038(18) -0.0203(9) 0.045(5) Uiso 1 1 d . . .
C2 C 1.225(2) 0.3167(18) 0.3319(10) 0.050(5) Uiso 1 1 d . . .
C3 C 1.4525(17) 0.2810(16) 0.3350(9) 0.038(4) Uiso 1 1 d . . .
C4 C 1.272(2) 0.2268(19) 0.3808(11) 0.056(5) Uiso 1 1 d . . .
C5 C 1.330(2) 0.4414(19) 0.2408(11) 0.060(6) Uiso 1 1 d . . .
C6 C 1.508(2) 0.1163(19) 0.4294(10) 0.057(6) Uiso 1 1 d . . .
C7 C 0.312(2) 1.097(2) 0.0452(11) 0.065(6) Uiso 1 1 d . . .
C8 C 1.292(3) 0.358(2) 0.1805(14) 0.096(9) Uiso 1 1 d . . .
C10 C 0.884(4) 0.152(4) 0.0749(19) 0.153(14) Uiso 1 1 d D . .
C9 C 1.001(4) 0.116(4) 0.120(2) 0.22(2) 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
U1 O4 1.768(10) . ?
U1 O4 1.768(10) 3_665 ?
U1 O1 2.281(11) . ?
U1 O1 2.281(11) 3_665 ?
U1 O2 2.308(9) . ?
U1 O2 2.308(9) 3_665 ?
U2 O8 1.772(10) . ?
U2 O5 1.777(10) . ?
U2 O7 2.269(11) 2_655 ?
U2 O10 2.278(11) . ?
U2 O3 2.283(10) . ?
U2 O6 2.289(10) 2_645 ?
P1 O3 1.504(11) . ?
P1 O2 1.526(11) . ?
P1 O6 1.533(11) . ?
P1 O9 1.584(12) 3_675 ?
P2 O10 1.494(12) . ?
P2 O7 1.499(12) . ?
P2 O1 1.504(12) . ?
P2 O11 1.575(14) . ?
O6 U2 2.289(10) 2_655 ?
O7 U2 2.269(11) 2_645 ?
O9 C1 1.53(2) . ?
O9 P1 1.584(12) 3_675 ?
O11 C10 1.29(4) . ?
N1 C4 1.39(2) . ?
N1 C3 1.40(2) . ?
N1 C6 1.46(2) . ?
N2 C3 1.36(2) . ?
N2 C2 1.37(2) . ?
N2 C5 1.57(2) . ?
C1 C7 1.54(2) . ?
C2 C4 1.34(2) . ?
C5 C8 1.44(3) . ?
C10 C9 1.36(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
O4 U1 O4 179.999(1) . 3_665 ?
O4 U1 O1 89.2(4) . . ?
O4 U1 O1 90.8(4) 3_665 . ?
O4 U1 O1 90.8(4) . 3_665 ?
O4 U1 O1 89.2(4) 3_665 3_665 ?
O1 U1 O1 179.999(1) . 3_665 ?
O4 U1 O2 91.4(4) . . ?
O4 U1 O2 88.6(4) 3_665 . ?
O1 U1 O2 89.8(4) . . ?
O1 U1 O2 90.2(4) 3_665 . ?
O4 U1 O2 88.6(4) . 3_665 ?
O4 U1 O2 91.4(4) 3_665 3_665 ?
O1 U1 O2 90.2(4) . 3_665 ?
O1 U1 O2 89.8(4) 3_665 3_665 ?
O2 U1 O2 179.999(1) . 3_665 ?
O8 U2 O5 179.0(5) . . ?
O8 U2 O7 91.4(4) . 2_655 ?
O5 U2 O7 89.5(4) . 2_655 ?
O8 U2 O10 90.3(5) . . ?
O5 U2 O10 88.8(4) . . ?
O7 U2 O10 175.7(4) 2_655 . ?
O8 U2 O3 87.8(4) . . ?
O5 U2 O3 92.6(4) . . ?
O7 U2 O3 88.6(4) 2_655 . ?
O10 U2 O3 87.6(4) . . ?
O8 U2 O6 87.5(4) . 2_645 ?
O5 U2 O6 92.0(4) . 2_645 ?
O7 U2 O6 93.4(4) 2_655 2_645 ?
O10 U2 O6 90.5(4) . 2_645 ?
O3 U2 O6 175.0(4) . 2_645 ?
O3 P1 O2 112.9(6) . . ?
O3 P1 O6 112.0(7) . . ?
O2 P1 O6 109.5(6) . . ?
O3 P1 O9 103.9(7) . 3_675 ?
O2 P1 O9 109.6(7) . 3_675 ?
O6 P1 O9 108.7(6) . 3_675 ?
O10 P2 O7 113.6(7) . . ?
O10 P2 O1 113.3(7) . . ?
O7 P2 O1 110.9(7) . . ?
O10 P2 O11 107.3(8) . . ?
O7 P2 O11 108.7(7) . . ?
O1 P2 O11 102.3(8) . . ?
P2 O1 U1 146.0(7) . . ?
P1 O2 U1 137.6(7) . . ?
P1 O3 U2 149.3(7) . . ?
P1 O6 U2 136.3(6) . 2_655 ?
P2 O7 U2 157.9(8) . 2_645 ?
C1 O9 P1 114.1(10) . 3_675 ?
P2 O10 U2 143.7(8) . . ?
C10 O11 P2 123(2) . . ?
C4 N1 C3 106.6(16) . . ?
C4 N1 C6 132.7(17) . . ?
C3 N1 C6 120.7(17) . . ?
C3 N2 C2 113.5(16) . . ?
C3 N2 C5 124.1(15) . . ?
C2 N2 C5 122.3(15) . . ?
O9 C1 C7 106.0(14) . . ?
C4 C2 N2 103.7(17) . . ?
N2 C3 N1 104.6(16) . . ?
C2 C4 N1 111.4(18) . . ?
C8 C5 N2 102.6(17) . . ?
O11 C10 C9 150(4) . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        27.34
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         3.486
_refine_diff_density_min         -1.624
_refine_diff_density_rms         0.304

_database_code_depnum_ccdc_archive 'CCDC 984854'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_pccn

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
  
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_structural     (C5H5N)2((UO2)2(SeO4)3)
_chemical_formula_moiety         'O16 Se3 U2, 2(C5 N)'
_chemical_formula_sum            'C10 N2 O16 Se3 U2'
_chemical_formula_weight         1117.06

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'
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'
Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   Pccn

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

_cell_length_a                   9.987(7)
_cell_length_b                   10.251(7)
_cell_length_c                   20.957(14)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2146(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    174(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      27.58

_exptl_crystal_description       Cube
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    3.458
_exptl_crystal_density_method    none
_exptl_crystal_F_000             1952
_exptl_absorpt_coefficient_mu    20.248
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6113
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      174(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'BRUKER AXS Apex-2 CCD-4k'
_diffrn_measurement_method       'phi-omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            23233
_diffrn_reflns_av_R_equivalents  0.1201
_diffrn_reflns_av_sigmaI/netI    0.0578
_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       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         1.94
_diffrn_reflns_theta_max         27.58
_reflns_number_total             2479
_reflns_number_gt                1791
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0838P)²+122.2569P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    none
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2479
_refine_ls_number_parameters     120
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0941
_refine_ls_R_factor_gt           0.0647
_refine_ls_wR_factor_ref         0.1784
_refine_ls_wR_factor_gt          0.1623
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.033
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.05581(6) 0.44469(6) 0.30273(3) 0.0188(2) Uani 1 1 d . . .
Se1 Se 0.2500 0.7500 0.25478(13) 0.0235(5) Uani 1 2 d S . .
Se2 Se -0.0880(3) 0.5954(2) 0.15812(13) 0.0475(6) Uani 1 1 d . . .
O1 O -0.001(2) 0.5158(19) 0.1181(8) 0.053(5) Uani 1 1 d . . .
O2 O 0.1590(15) 0.6623(14) 0.2988(6) 0.040(4) Uani 1 1 d . . .
O3 O -0.1590(15) 0.3377(14) 0.2902(7) 0.040(4) Uani 1 1 d . . .
O4 O -0.0672(13) 0.5730(13) 0.2299(8) 0.038(4) Uani 1 1 d . . .
O5 O -0.0191(13) 0.5103(14) 0.3716(6) 0.028(3) Uani 1 1 d . . .
O6 O -0.2364(14) 0.5640(18) 0.1446(7) 0.049(5) Uani 1 1 d . . .
O7 O 0.1317(13) 0.3753(13) 0.2346(5) 0.029(3) Uani 1 1 d . . .
O8 O -0.0622(19) 0.7413(14) 0.1441(7) 0.050(5) Uani 1 1 d . . .
N1 N 0.2500 0.2500 0.1219(15) 0.053(8) Uiso 1 2 d S . .
C1 C -0.2500 0.7500 0.006(2) 0.068(11) Uiso 1 2 d S . .
C2 C 0.140(3) 0.276(3) 0.0919(13) 0.060(7) Uiso 1 1 d . . .
N2 N -0.2500 0.2500 0.4259(18) 0.074(10) Uiso 1 2 d S . .
C3 C 0.132(3) 0.278(3) 0.0238(14) 0.066(8) Uiso 1 1 d . . .
C4 C -0.240(4) 0.357(4) 0.4501(18) 0.095(12) Uiso 1 1 d . . .
C5 C -0.263(4) 0.360(5) 0.021(2) 0.114(14) Uiso 1 1 d . . .
C6 C -0.2500 0.2500 0.048(2) 0.083(14) Uiso 1 2 d S . .


_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 O5 1.759(13) . ?
U1 O7 1.765(12) . ?
U1 O6 2.353(14) 4_565 ?
U1 O4 2.361(13) . ?
U1 O8 2.365(14) 3_545 ?
U1 O3 2.423(14) . ?
U1 O2 2.458(14) . ?
Se1 O2 1.577(13) . ?
Se1 O2 1.577(13) 2_565 ?
Se1 O3 1.589(13) 4_565 ?
Se1 O3 1.589(13) 3 ?
Se2 O1 1.457(17) . ?
Se2 O4 1.535(16) . ?
Se2 O6 1.542(14) . ?
Se2 O8 1.545(14) . ?
O3 Se1 1.589(13) 3_545 ?
O6 U1 2.353(14) 4_465 ?
O8 U1 2.365(14) 3 ?
N1 C2 1.29(3) 2 ?
N1 C2 1.29(3) . ?
C1 C3 1.36(4) 6_565 ?
C1 C3 1.36(4) 5_565 ?
C2 C3 1.43(4) . ?
N2 C4 1.21(4) 2_455 ?
N2 C4 1.21(4) . ?
C3 C1 1.36(4) 5_565 ?
C4 C5 1.48(5) 8_556 ?
C5 C6 1.27(5) . ?
C5 C4 1.48(5) 8 ?
C6 C5 1.27(5) 2_455 ?

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
O5 U1 O7 178.6(6) . . ?
O5 U1 O6 90.3(6) . 4_565 ?
O7 U1 O6 89.2(5) . 4_565 ?
O5 U1 O4 95.5(6) . . ?
O7 U1 O4 85.7(6) . . ?
O6 U1 O4 141.6(6) 4_565 . ?
O5 U1 O8 87.8(6) . 3_545 ?
O7 U1 O8 90.8(6) . 3_545 ?
O6 U1 O8 73.8(6) 4_565 3_545 ?
O4 U1 O8 144.1(6) . 3_545 ?
O5 U1 O3 83.4(5) . . ?
O7 U1 O3 96.3(6) . . ?
O6 U1 O3 144.5(6) 4_565 . ?
O4 U1 O3 73.8(5) . . ?
O8 U1 O3 71.1(6) 3_545 . ?
O5 U1 O2 81.9(6) . . ?
O7 U1 O2 99.1(6) . . ?
O6 U1 O2 71.4(6) 4_565 . ?
O4 U1 O2 72.0(5) . . ?
O8 U1 O2 143.5(6) 3_545 . ?
O3 U1 O2 141.1(5) . . ?
O2 Se1 O2 108.4(10) . 2_565 ?
O2 Se1 O3 110.8(8) . 4_565 ?
O2 Se1 O3 109.9(8) 2_565 4_565 ?
O2 Se1 O3 109.9(8) . 3 ?
O2 Se1 O3 110.8(8) 2_565 3 ?
O3 Se1 O3 107.2(11) 4_565 3 ?
O1 Se2 O4 113.6(9) . . ?
O1 Se2 O6 110.5(10) . . ?
O4 Se2 O6 106.2(8) . . ?
O1 Se2 O8 109.4(10) . . ?
O4 Se2 O8 108.0(8) . . ?
O6 Se2 O8 109.1(10) . . ?
Se1 O2 U1 141.1(8) . . ?
Se1 O3 U1 145.8(8) 3_545 . ?
Se2 O4 U1 141.9(9) . . ?
Se2 O6 U1 140.3(8) . 4_465 ?
Se2 O8 U1 140.2(8) . 3 ?
C2 N1 C2 122(3) 2 . ?
C3 C1 C3 126(4) 6_565 5_565 ?
N1 C2 C3 123(3) . . ?
C4 N2 C4 130(5) 2_455 . ?
C1 C3 C2 114(3) 5_565 . ?
N2 C4 C5 116(4) . 8_556 ?
C6 C5 C4 115(5) . 8 ?
C5 C6 C5 127(6) . 2_455 ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        27.58
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         2.718
_refine_diff_density_min         -4.545
_refine_diff_density_rms         0.436

_database_code_depnum_ccdc_archive 'CCDC 984855'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_p21n

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_structural     (C4H7N2)((UO2)5(PO4)3(HPO4)(H2O)2)3H2O
_chemical_formula_moiety         'O28 P4 U5, 0.5(C8 N4), 3(O)'
_chemical_formula_sum            'C4 N2 O31 P4 U5'
_chemical_formula_weight         1886.09

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'
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'
P P 0.1023 0.0942 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'

loop_
_symmetry_equiv_pos_as_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                   9.5152(9)
_cell_length_b                   33.144(3)
_cell_length_c                   9.6569(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.2110(10)
_cell_angle_gamma                90.00
_cell_volume                     3040.7(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      27.09

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    4.120
_exptl_crystal_density_method    none
_exptl_crystal_F_000             3480
_exptl_absorpt_coefficient_mu    27.146
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3903
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'BRUKER AXS Apex-2 CCD-4k'
_diffrn_measurement_method       'phi-omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            30943
_diffrn_reflns_av_R_equivalents  0.0958
_diffrn_reflns_av_sigmaI/netI    0.0807
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         1.23
_diffrn_reflns_theta_max         27.53
_reflns_number_total             6967
_reflns_number_gt                5093
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0436P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    none
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6967
_refine_ls_number_parameters     230
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0684
_refine_ls_R_factor_gt           0.0450
_refine_ls_wR_factor_ref         0.1163
_refine_ls_wR_factor_gt          0.1036
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_restrained_S_all      1.015
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.08050(5) 0.240207(14) 0.66336(4) 0.01173(12) Uani 1 1 d . . .
U2 U 0.18149(5) 0.240604(14) 0.26670(4) 0.01134(12) Uani 1 1 d . . .
U3 U 0.54940(5) 0.007359(15) 0.79980(4) 0.01262(12) Uani 1 1 d . . .
U4 U 0.94924(5) 0.007633(14) 0.69537(4) 0.01184(12) Uani 1 1 d . . .
U5 U 0.64402(5) 0.130482(15) 0.44288(5) 0.01550(12) Uani 1 1 d . . .
P1 P 0.7116(3) 0.02024(10) 0.4587(3) 0.0101(6) Uani 1 1 d . . .
P2 P 0.4282(3) 0.22173(10) 0.4949(3) 0.0113(6) Uani 1 1 d . . .
P3 P 0.7850(3) 0.02118(11) 1.0387(3) 0.0153(7) Uani 1 1 d . . .
P4 P -0.1681(3) 0.23074(10) 0.4329(3) 0.0120(6) Uani 1 1 d . . .
O1 O -0.2410(9) 0.2592(2) 0.3313(8) 0.0144(18) Uiso 1 1 d . . .
O2 O 0.6161(9) -0.0102(3) 0.3844(8) 0.018(2) Uiso 1 1 d . . .
O3 O 0.6991(9) 0.0178(3) 0.6179(8) 0.0150(18) Uiso 1 1 d . . .
O4 O 0.8830(10) -0.0052(3) 1.1266(9) 0.021(2) Uiso 1 1 d . . .
O5 O 0.4358(9) 0.2369(3) 0.3449(8) 0.0171(19) Uiso 1 1 d . . .
O6 O 0.8020(9) 0.0169(3) 0.8828(8) 0.0177(19) Uiso 1 1 d . . .
O7 O -0.1719(9) 0.2470(3) 0.5839(9) 0.0158(19) Uiso 1 1 d . . .
O8 O -0.0056(9) 0.2303(3) 0.4150(8) 0.0153(18) Uiso 1 1 d . . .
O9 O 0.5031(10) 0.2510(3) 0.5939(9) 0.018(2) Uiso 1 1 d . . .
O10 O 0.2654(9) 0.2238(3) 0.5126(8) 0.0138(18) Uiso 1 1 d . . .
O11 O 0.8681(10) 0.0075(3) 0.4484(9) 0.022(2) Uiso 1 1 d . . .
O12 O 0.4803(9) 0.1796(3) 0.5121(8) 0.021(2) Uiso 1 1 d . . .
O13 O 0.6317(10) 0.0088(3) 1.0520(9) 0.022(2) Uiso 1 1 d . . .
O14 O 0.5215(10) 0.0590(3) 0.8165(9) 0.025(2) Uiso 1 1 d . . .
O15 O 0.9787(9) 0.0595(3) 0.6815(9) 0.023(2) Uiso 1 1 d . . .
O16 O 0.1831(9) 0.2923(3) 0.3087(9) 0.022(2) Uiso 1 1 d . . .
O17 O 0.9189(9) -0.0447(3) 0.7066(9) 0.022(2) Uiso 1 1 d . . .
O18 O 0.0485(9) 0.1893(3) 0.6985(8) 0.021(2) Uiso 1 1 d . . .
O19 O 0.6854(9) 0.0614(3) 0.4050(8) 0.021(2) Uiso 1 1 d . . .
O20 O 0.5823(10) -0.0448(3) 0.7846(9) 0.028(2) Uiso 1 1 d . . .
O21 O 0.1779(9) 0.1880(3) 0.2305(8) 0.020(2) Uiso 1 1 d . . .
O22 O 0.1121(9) 0.2913(3) 0.6199(8) 0.020(2) Uiso 1 1 d . . .
O23 O 0.5721(10) 0.1342(3) 0.2747(9) 0.026(2) Uiso 1 1 d . . .
O24 O 0.8080(10) 0.0659(3) 1.0804(9) 0.030(2) Uiso 1 1 d . . .
O25 O 0.7121(10) 0.1243(3) 0.6150(10) 0.030(2) Uiso 1 1 d . . .
O26 O -0.2292(9) 0.1894(3) 0.4212(9) 0.022(2) Uiso 1 1 d . . .
O27 O 0.8769(10) 0.1179(3) 0.3320(10) 0.029(2) Uiso 1 1 d . . .
O28 O 0.4269(11) 0.0945(3) 0.5040(10) 0.032(2) Uiso 1 1 d . . .
O29 O 0.8755(11) 0.1716(3) 0.1022(11) 0.043(3) Uiso 1 1 d . . .
O30 O 0.1675(14) 0.1247(4) 0.4730(13) 0.065(4) Uiso 1 1 d . . .
O31 O 0.7919(17) 0.1184(5) 0.8992(16) 0.093(5) Uiso 1 1 d . . .
N1 N 0.2529(15) 0.1190(4) 0.9547(14) 0.043(4) Uiso 1 1 d . . .
C1 C 0.233(2) 0.1224(6) 0.817(2) 0.060(5) Uiso 1 1 d . . .
N2 N 0.355(2) 0.1440(6) 0.7815(19) 0.081(6) Uiso 1 1 d . . .
C2 C 0.377(2) 0.1379(6) 0.007(2) 0.061(6) Uiso 1 1 d . . .
C3 C -0.060(2) 0.3493(6) 0.392(2) 0.059(5) Uiso 1 1 d . . .
C4 C 0.851(2) -0.0994(7) 0.958(2) 0.079(7) 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 O18 1.750(9) . ?
U1 O22 1.773(9) . ?
U1 O1 2.282(8) 4_666 ?
U1 O10 2.408(8) . ?
U1 O5 2.412(8) 4_566 ?
U1 O7 2.490(9) . ?
U1 O8 2.512(8) . ?
U1 P4 3.171(3) . ?
U1 U2 4.0012(7) . ?
U1 U2 4.0298(7) 4_566 ?
U2 O16 1.759(9) . ?
U2 O21 1.779(9) . ?
U2 O9 2.330(9) 4_565 ?
U2 O7 2.346(9) 4_665 ?
U2 O8 2.372(8) . ?
U2 O5 2.498(9) . ?
U2 O10 2.524(8) . ?
U2 P2 3.190(3) . ?
U2 U1 4.0298(7) 4_665 ?
U3 O14 1.741(10) . ?
U3 O20 1.763(10) . ?
U3 O2 2.310(8) 3_656 ?
U3 O3 2.348(8) . ?
U3 O13 2.362(9) 3_657 ?
U3 O6 2.511(8) . ?
U3 O13 2.516(9) . ?
U3 P3 3.159(3) . ?
U3 U4 3.9902(7) . ?
U3 U3 4.0595(9) 3_657 ?
U4 O15 1.748(9) . ?
U4 O17 1.761(9) . ?
U4 O4 2.281(9) 3_757 ?
U4 O11 2.339(9) 3_756 ?
U4 O6 2.370(8) . ?
U4 O11 2.465(9) . ?
U4 O3 2.478(8) . ?
U4 P1 3.152(3) . ?
U4 U4 3.9794(9) 3_756 ?
U5 O23 1.731(9) . ?
U5 O25 1.762(9) . ?
U5 O26 2.310(9) 1_655 ?
U5 O19 2.357(9) . ?
U5 O12 2.376(9) . ?
U5 O28 2.485(10) . ?
U5 O27 2.549(10) . ?
P1 O19 1.474(9) . ?
P1 O2 1.512(9) . ?
P1 O3 1.551(8) . ?
P1 O11 1.557(10) . ?
P2 O12 1.487(9) . ?
P2 O9 1.512(9) . ?
P2 O5 1.539(9) . ?
P2 O10 1.569(9) . ?
P3 O4 1.506(9) . ?
P3 O13 1.528(10) . ?
P3 O6 1.529(8) . ?
P3 O24 1.548(11) . ?
P4 O26 1.491(10) . ?
P4 O1 1.502(9) . ?
P4 O7 1.557(9) . ?
P4 O8 1.566(9) . ?
O1 U1 2.282(8) 4_565 ?
O2 U3 2.310(8) 3_656 ?
O4 U4 2.281(9) 3_757 ?
O5 U1 2.412(8) 4_665 ?
O7 U2 2.346(9) 4_566 ?
O9 U2 2.330(9) 4_666 ?
O11 U4 2.339(9) 3_756 ?
O13 U3 2.362(9) 3_657 ?
O26 U5 2.310(9) 1_455 ?
N1 C1 1.33(2) . ?
N1 C2 1.41(2) 1_556 ?
N1 C4 1.48(3) 3_657 ?
C1 N2 1.42(2) . ?
N2 C3 1.32(2) 4_666 ?
C2 C3 1.36(3) 4_665 ?
C2 N1 1.41(2) 1_554 ?
C3 N2 1.32(2) 4_565 ?
C3 C2 1.36(3) 4_566 ?
C4 N1 1.48(3) 3_657 ?

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
O18 U1 O22 177.5(4) . . ?
O18 U1 O1 90.1(3) . 4_666 ?
O22 U1 O1 91.8(3) . 4_666 ?
O18 U1 O10 92.4(3) . . ?
O22 U1 O10 86.1(3) . . ?
O1 U1 O10 83.8(3) 4_666 . ?
O18 U1 O5 92.8(3) . 4_566 ?
O22 U1 O5 89.0(3) . 4_566 ?
O1 U1 O5 85.0(3) 4_666 4_566 ?
O10 U1 O5 167.6(3) . 4_566 ?
O18 U1 O7 88.4(3) . . ?
O22 U1 O7 90.8(3) . . ?
O1 U1 O7 152.2(3) 4_666 . ?
O10 U1 O7 124.0(3) . . ?
O5 U1 O7 67.4(3) 4_566 . ?
O18 U1 O8 90.5(3) . . ?
O22 U1 O8 87.1(3) . . ?
O1 U1 O8 150.4(3) 4_666 . ?
O10 U1 O8 66.6(3) . . ?
O5 U1 O8 124.5(3) 4_566 . ?
O7 U1 O8 57.3(3) . . ?
O18 U1 P4 84.8(3) . . ?
O22 U1 P4 93.3(3) . . ?
O1 U1 P4 174.8(2) 4_666 . ?
O10 U1 P4 95.45(19) . . ?
O5 U1 P4 96.2(2) 4_566 . ?
O7 U1 P4 28.8(2) . . ?
O8 U1 P4 29.1(2) . . ?
O18 U1 U2 104.0(3) . . ?
O22 U1 U2 73.6(3) . . ?
O1 U1 U2 118.1(2) 4_666 . ?
O10 U1 U2 36.77(18) . . ?
O5 U1 U2 150.8(2) 4_566 . ?
O7 U1 U2 89.09(19) . . ?
O8 U1 U2 33.85(19) . . ?
P4 U1 U2 62.50(6) . . ?
O18 U1 U2 85.8(3) . 4_566 ?
O22 U1 U2 94.7(3) . 4_566 ?
O1 U1 U2 119.8(2) 4_666 4_566 ?
O10 U1 U2 156.32(18) . 4_566 ?
O5 U1 U2 35.5(2) 4_566 4_566 ?
O7 U1 U2 32.46(19) . 4_566 ?
O8 U1 U2 89.75(19) . 4_566 ?
P4 U1 U2 60.87(6) . 4_566 ?
U2 U1 U2 121.109(15) . 4_566 ?
O16 U2 O21 177.9(4) . . ?
O16 U2 O9 92.6(4) . 4_565 ?
O21 U2 O9 88.3(3) . 4_565 ?
O16 U2 O7 90.3(4) . 4_665 ?
O21 U2 O7 91.7(3) . 4_665 ?
O9 U2 O7 83.1(3) 4_565 4_665 ?
O16 U2 O8 89.9(4) . . ?
O21 U2 O8 88.3(3) . . ?
O9 U2 O8 84.7(3) 4_565 . ?
O7 U2 O8 167.9(3) 4_665 . ?
O16 U2 O5 89.0(3) . . ?
O21 U2 O5 91.1(3) . . ?
O9 U2 O5 151.3(3) 4_565 . ?
O7 U2 O5 68.2(3) 4_665 . ?
O8 U2 O5 123.9(3) . . ?
O16 U2 O10 90.0(3) . . ?
O21 U2 O10 88.3(3) . . ?
O9 U2 O10 151.6(3) 4_565 . ?
O7 U2 O10 125.2(3) 4_665 . ?
O8 U2 O10 67.0(3) . . ?
O5 U2 O10 56.9(3) . . ?
O16 U2 P2 92.0(3) . . ?
O21 U2 P2 87.1(3) . . ?
O9 U2 P2 175.3(2) 4_565 . ?
O7 U2 P2 96.2(2) 4_665 . ?
O8 U2 P2 95.9(2) . . ?
O5 U2 P2 28.2(2) . . ?
O10 U2 P2 28.98(19) . . ?
O16 U2 U1 77.4(3) . . ?
O21 U2 U1 100.5(3) . . ?
O9 U2 U1 118.8(2) 4_565 . ?
O7 U2 U1 154.9(2) 4_665 . ?
O8 U2 U1 36.2(2) . . ?
O5 U2 U1 89.47(19) . . ?
O10 U2 U1 34.83(19) . . ?
P2 U2 U1 62.93(6) . . ?
O16 U2 U1 84.7(3) . 4_665 ?
O21 U2 U1 96.5(3) . 4_665 ?
O9 U2 U1 117.6(2) 4_565 4_665 ?
O7 U2 U1 34.7(2) 4_665 4_665 ?
O8 U2 U1 157.2(2) . 4_665 ?
O5 U2 U1 34.14(19) . 4_665 ?
O10 U2 U1 90.85(19) . 4_665 ?
P2 U2 U1 62.30(6) . 4_665 ?
U1 U2 U1 121.179(15) . 4_665 ?
O14 U3 O20 178.5(4) . . ?
O14 U3 O2 86.0(4) . 3_656 ?
O20 U3 O2 95.3(4) . 3_656 ?
O14 U3 O3 91.5(4) . . ?
O20 U3 O3 87.9(4) . . ?
O2 U3 O3 80.4(3) 3_656 . ?
O14 U3 O13 92.6(4) . 3_657 ?
O20 U3 O13 88.1(4) . 3_657 ?
O2 U3 O13 89.3(3) 3_656 3_657 ?
O3 U3 O13 168.6(3) . 3_657 ?
O14 U3 O6 89.7(4) . . ?
O20 U3 O6 88.8(4) . . ?
O2 U3 O6 147.1(3) 3_656 . ?
O3 U3 O6 67.1(3) . . ?
O13 U3 O6 123.6(3) 3_657 . ?
O14 U3 O13 86.2(3) . . ?
O20 U3 O13 92.9(4) . . ?
O2 U3 O13 155.0(3) 3_656 . ?
O3 U3 O13 123.5(3) . . ?
O13 U3 O13 67.4(4) 3_657 . ?
O6 U3 O13 56.5(3) . . ?
O14 U3 P3 84.0(3) . . ?
O20 U3 P3 94.6(3) . . ?
O2 U3 P3 169.0(2) 3_656 . ?
O3 U3 P3 95.1(2) . . ?
O13 U3 P3 95.9(2) 3_657 . ?
O6 U3 P3 28.48(19) . . ?
O13 U3 P3 28.5(2) . . ?
O14 U3 U4 100.0(3) . . ?
O20 U3 U4 78.8(3) . . ?
O2 U3 U4 115.1(2) 3_656 . ?
O3 U3 U4 35.28(19) . . ?
O13 U3 U4 153.1(2) 3_657 . ?
O6 U3 U4 34.02(18) . . ?
O13 U3 U4 89.7(2) . . ?
P3 U3 U4 62.39(6) . . ?
O14 U3 U3 89.2(3) . 3_657 ?
O20 U3 U3 90.7(3) . 3_657 ?
O2 U3 U3 123.6(2) 3_656 3_657 ?
O3 U3 U3 155.89(19) . 3_657 ?
O13 U3 U3 34.9(2) 3_657 3_657 ?
O6 U3 U3 88.84(18) . 3_657 ?
O13 U3 U3 32.5(2) . 3_657 ?
P3 U3 U3 60.96(6) . 3_657 ?
U4 U3 U3 121.063(17) . 3_657 ?
O15 U4 O17 179.1(4) . . ?
O15 U4 O4 89.1(4) . 3_757 ?
O17 U4 O4 91.7(4) . 3_757 ?
O15 U4 O11 92.1(4) . 3_756 ?
O17 U4 O11 87.5(4) . 3_756 ?
O4 U4 O11 85.9(3) 3_757 3_756 ?
O15 U4 O6 92.0(4) . . ?
O17 U4 O6 88.6(4) . . ?
O4 U4 O6 81.2(3) 3_757 . ?
O11 U4 O6 166.4(3) 3_756 . ?
O15 U4 O11 88.3(3) . . ?
O17 U4 O11 90.8(3) . . ?
O4 U4 O11 153.8(3) 3_757 . ?
O11 U4 O11 68.1(4) 3_756 . ?
O6 U4 O11 124.9(3) . . ?
O15 U4 O3 90.0(3) . . ?
O17 U4 O3 89.7(4) . . ?
O4 U4 O3 148.5(3) 3_757 . ?
O11 U4 O3 125.7(3) 3_756 . ?
O6 U4 O3 67.3(3) . . ?
O11 U4 O3 57.6(3) . . ?
O15 U4 P1 85.7(3) . . ?
O17 U4 P1 93.5(3) . . ?
O4 U4 P1 174.1(2) 3_757 . ?
O11 U4 P1 97.1(2) 3_756 . ?
O6 U4 P1 96.1(2) . . ?
O11 U4 P1 29.0(2) . . ?
O3 U4 P1 28.96(19) . . ?
O15 U4 U4 90.2(3) . 3_756 ?
O17 U4 U4 89.0(3) . 3_756 ?
O4 U4 U4 120.9(2) 3_757 3_756 ?
O11 U4 U4 35.1(2) 3_756 3_756 ?
O6 U4 U4 157.8(2) . 3_756 ?
O11 U4 U4 33.1(2) . 3_756 ?
O3 U4 U4 90.63(18) . 3_756 ?
P1 U4 U4 62.06(6) . 3_756 ?
O15 U4 U3 100.4(3) . . ?
O17 U4 U3 79.7(3) . . ?
O4 U4 U3 116.5(2) 3_757 . ?
O11 U4 U3 154.2(2) 3_756 . ?
O6 U4 U3 36.3(2) . . ?
O11 U4 U3 89.6(2) . . ?
O3 U4 U3 33.18(18) . . ?
P1 U4 U3 61.85(6) . . ?
U4 U4 U3 121.661(17) 3_756 . ?
O23 U5 O25 177.0(5) . . ?
O23 U5 O26 92.1(4) . 1_655 ?
O25 U5 O26 91.0(4) . 1_655 ?
O23 U5 O19 89.1(4) . . ?
O25 U5 O19 88.8(4) . . ?
O26 U5 O19 135.6(3) 1_655 . ?
O23 U5 O12 89.1(4) . . ?
O25 U5 O12 91.5(4) . . ?
O26 U5 O12 78.4(3) 1_655 . ?
O19 U5 O12 145.9(3) . . ?
O23 U5 O28 88.1(4) . . ?
O25 U5 O28 89.3(4) . . ?
O26 U5 O28 150.7(3) 1_655 . ?
O19 U5 O28 73.7(3) . . ?
O12 U5 O28 72.3(3) . . ?
O23 U5 O27 85.7(4) . . ?
O25 U5 O27 95.4(4) . . ?
O26 U5 O27 68.3(3) 1_655 . ?
O19 U5 O27 67.6(3) . . ?
O12 U5 O27 146.0(3) . . ?
O28 U5 O27 140.8(3) . . ?
O19 P1 O2 111.4(5) . . ?
O19 P1 O3 112.1(5) . . ?
O2 P1 O3 110.9(5) . . ?
O19 P1 O11 111.9(5) . . ?
O2 P1 O11 109.9(5) . . ?
O3 P1 O11 100.1(5) . . ?
O19 P1 U4 118.6(4) . . ?
O2 P1 U4 130.1(4) . . ?
O3 P1 U4 50.6(3) . . ?
O11 P1 U4 50.2(3) . . ?
O12 P2 O9 112.9(5) . . ?
O12 P2 O5 112.3(5) . . ?
O9 P2 O5 109.9(5) . . ?
O12 P2 O10 110.8(5) . . ?
O9 P2 O10 109.6(5) . . ?
O5 P2 O10 100.8(5) . . ?
O12 P2 U2 119.3(4) . . ?
O9 P2 U2 127.8(4) . . ?
O5 P2 U2 50.0(3) . . ?
O10 P2 U2 51.2(3) . . ?
O4 P3 O13 111.1(5) . . ?
O4 P3 O6 113.9(5) . . ?
O13 P3 O6 102.2(5) . . ?
O4 P3 O24 109.6(5) . . ?
O13 P3 O24 110.9(5) . . ?
O6 P3 O24 108.9(5) . . ?
O4 P3 U3 136.0(4) . . ?
O13 P3 U3 51.7(3) . . ?
O6 P3 U3 51.5(3) . . ?
O24 P3 U3 114.4(4) . . ?
O26 P4 O1 111.3(5) . . ?
O26 P4 O7 111.1(5) . . ?
O1 P4 O7 111.1(5) . . ?
O26 P4 O8 111.5(5) . . ?
O1 P4 O8 110.9(5) . . ?
O7 P4 O8 100.5(5) . . ?
O26 P4 U1 114.6(4) . . ?
O1 P4 U1 134.0(4) . . ?
O7 P4 U1 50.5(3) . . ?
O8 P4 U1 51.4(3) . . ?
P4 O1 U1 140.1(5) . 4_565 ?
P1 O2 U3 134.7(5) . 3_656 ?
P1 O3 U3 146.4(5) . . ?
P1 O3 U4 100.4(4) . . ?
U3 O3 U4 111.5(3) . . ?
P3 O4 U4 146.1(6) . 3_757 ?
P2 O5 U1 147.8(5) . 4_665 ?
P2 O5 U2 101.8(4) . . ?
U1 O5 U2 110.3(3) 4_665 . ?
P3 O6 U4 149.7(5) . . ?
P3 O6 U3 100.0(4) . . ?
U4 O6 U3 109.6(3) . . ?
P4 O7 U2 144.2(5) . 4_566 ?
P4 O7 U1 100.6(4) . . ?
U2 O7 U1 112.8(3) 4_566 . ?
P4 O8 U2 147.6(5) . . ?
P4 O8 U1 99.5(4) . . ?
U2 O8 U1 110.0(3) . . ?
P2 O9 U2 145.9(5) . 4_666 ?
P2 O10 U1 146.6(5) . . ?
P2 O10 U2 99.8(4) . . ?
U1 O10 U2 108.4(3) . . ?
P1 O11 U4 147.3(5) . 3_756 ?
P1 O11 U4 100.8(4) . . ?
U4 O11 U4 111.9(4) 3_756 . ?
P2 O12 U5 146.3(5) . . ?
P3 O13 U3 147.6(5) . 3_657 ?
P3 O13 U3 99.8(4) . . ?
U3 O13 U3 112.6(4) 3_657 . ?
P1 O19 U5 150.5(5) . . ?
P4 O26 U5 166.8(6) . 1_455 ?
C1 N1 C2 113.0(16) . 1_556 ?
C1 N1 C4 122.6(17) . 3_657 ?
C2 N1 C4 124.3(16) 1_556 3_657 ?
N1 C1 N2 102.2(17) . . ?
C3 N2 C1 111.2(18) 4_666 . ?
C3 C2 N1 104.1(17) 4_665 1_554 ?
N2 C3 C2 109(2) 4_565 4_566 ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        27.53
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         2.930
_refine_diff_density_min         -2.577
_refine_diff_density_rms         0.474

_database_code_depnum_ccdc_archive 'CCDC 984856'
