#######################################################################
#
#                 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_RT_double_cell


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'U O2 Cl4, N2 C10 H10'
_chemical_formula_sum            'C10 H10 Cl4 N2 O2 U'
_chemical_formula_weight         570.03

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -4.3638 13.4090 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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                   8.9680(3)
_cell_length_b                   9.9186(3)
_cell_length_c                   10.4833(3)
_cell_angle_alpha                66.002(1)
_cell_angle_beta                 87.096(1)
_cell_angle_gamma                64.555(1)
_cell_volume                     760.50(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9953
_cell_measurement_theta_min      5.4
_cell_measurement_theta_max      59.1

_exptl_crystal_description       'triangular plate'
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.01
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.489
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             520
_exptl_absorpt_coefficient_mu    36.507
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.1377
_exptl_absorpt_correction_T_max  0.7116
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'ImuS sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker D8 with ApexII detector'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            16701
_diffrn_reflns_av_R_equivalents  0.0427
_diffrn_reflns_av_sigmaI/netI    0.0232
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         4.67
_diffrn_reflns_theta_max         59.11
_reflns_number_total             2119
_reflns_number_gt                1933
_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)+(0.0387P)²+0.3272P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2119
_refine_ls_number_parameters     215
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0212
_refine_ls_R_factor_gt           0.0199
_refine_ls_wR_factor_ref         0.0587
_refine_ls_wR_factor_gt          0.0538
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_restrained_S_all      1.061
_refine_ls_shift/su_max          0.024
_refine_ls_shift/su_mean         0.002

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 0.0000 0.5000 0.5000 0.03231(11) Uani 1 2 d S . .
U2 U 0.0000 0.0000 0.0000 0.03202(11) Uani 1 2 d S . .
O1 O 0.0914(4) 0.6271(4) 0.4000(4) 0.0553(9) Uani 1 1 d . . .
O2 O -0.0380(4) -0.1740(4) 0.0788(4) 0.0500(8) Uani 1 1 d . . .
N2 N -0.7381(6) 0.8082(7) -0.5368(6) 0.0496(12) Uani 1 1 d . . .
N1 N -0.2395(7) 0.6476(7) 0.0432(6) 0.0552(13) Uani 1 1 d . . .
Cl1 Cl 0.30195(16) 0.27889(16) 0.64918(15) 0.0518(3) Uani 1 1 d . . .
Cl2 Cl 0.04538(16) 0.36925(15) 0.31462(13) 0.0614(3) Uani 1 1 d . . .
Cl3 Cl -0.06601(16) 0.07243(16) 0.22177(12) 0.0581(3) Uani 1 1 d . . .
Cl4 Cl -0.31820(15) 0.18317(16) -0.12347(15) 0.0502(3) Uani 1 1 d . . .
C1 C -0.2313(9) 0.5201(8) 0.0215(7) 0.0647(17) Uani 1 1 d . . .
C2 C -0.3259(8) 0.5501(7) -0.0926(7) 0.0581(15) Uani 1 1 d . . .
C3 C -0.4307(6) 0.7118(6) -0.1879(6) 0.0378(11) Uani 1 1 d . . .
C4 C -0.4345(7) 0.8368(7) -0.1589(7) 0.0483(13) Uani 1 1 d . . .
C5 C -0.3384(8) 0.8035(8) -0.0430(7) 0.0522(15) Uani 1 1 d . . .
C6 C -0.5352(6) 0.7468(6) -0.3138(6) 0.0373(11) Uani 1 1 d . . .
C7 C -0.5420(8) 0.6184(8) -0.3343(7) 0.0525(14) Uani 1 1 d . . .
C8 C -0.6454(8) 0.6537(8) -0.4453(7) 0.0551(15) Uani 1 1 d . . .
C9 C -0.7326(8) 0.9333(8) -0.5239(7) 0.0545(15) Uani 1 1 d . . .
C10 C -0.6328(7) 0.9075(7) -0.4148(6) 0.0478(13) Uani 1 1 d . . .
H2N H -0.816(8) 0.836(7) -0.603(7) 0.074(19) Uiso 1 1 d . . .
H1N H -0.171(7) 0.619(6) 0.106(6) 0.048(15) Uiso 1 1 d . . .
H1 H -0.154(6) 0.412(6) 0.073(6) 0.092(17) Uiso 1 1 d . . .
H2 H -0.303(6) 0.465(7) -0.112(5) 0.088(18) Uiso 1 1 d . . .
H4 H -0.511(8) 0.945(8) -0.224(6) 0.08(2) Uiso 1 1 d . . .
H5 H -0.328(7) 0.882(7) -0.007(6) 0.065(17) Uiso 1 1 d . . .
H7 H -0.474(7) 0.500(7) -0.254(6) 0.09(2) Uiso 1 1 d . . .
H8 H -0.655(7) 0.576(7) -0.469(6) 0.08(2) Uiso 1 1 d . . .
H9 H -0.790(7) 1.016(8) -0.599(6) 0.094(19) Uiso 1 1 d . . .
H10 H -0.625(7) 0.990(8) -0.385(6) 0.11(2) Uiso 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 O1 1.756(3) . ?
U1 O1 1.756(3) 2_566 ?
U1 Cl1 2.6692(12) . ?
U1 Cl1 2.6692(12) 2_566 ?
U1 Cl2 2.6722(11) 2_566 ?
U1 Cl2 2.6722(11) . ?
U2 O2 1.759(3) 2 ?
U2 O2 1.759(3) . ?
U2 Cl4 2.6694(12) . ?
U2 Cl4 2.6694(12) 2 ?
U2 Cl3 2.6693(11) 2 ?
U2 Cl3 2.6693(11) . ?
N2 C8 1.323(9) . ?
N2 C9 1.323(9) . ?
N2 H2N 0.88(7) . ?
N1 C5 1.327(9) . ?
N1 C1 1.345(9) . ?
N1 H1N 0.79(6) . ?
C1 C2 1.354(9) . ?
C1 H1 0.92(5) . ?
C2 C3 1.397(9) . ?
C2 H2 0.89(6) . ?
C3 C4 1.379(8) . ?
C3 C6 1.488(10) . ?
C4 C5 1.365(9) . ?
C4 H4 0.95(6) . ?
C5 H5 1.03(6) . ?
C6 C10 1.397(8) . ?
C6 C7 1.400(8) . ?
C7 C8 1.355(9) . ?
C7 H7 1.04(6) . ?
C8 H8 0.94(6) . ?
C9 C10 1.358(9) . ?
C9 H9 0.84(6) . ?
C10 H10 1.02(7) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 U1 O1 180.00(15) . 2_566 ?
O1 U1 Cl1 87.96(11) . . ?
O1 U1 Cl1 92.04(11) 2_566 . ?
O1 U1 Cl1 92.04(11) . 2_566 ?
O1 U1 Cl1 87.96(11) 2_566 2_566 ?
Cl1 U1 Cl1 180.0 . 2_566 ?
O1 U1 Cl2 89.45(11) . 2_566 ?
O1 U1 Cl2 90.54(11) 2_566 2_566 ?
Cl1 U1 Cl2 87.50(4) . 2_566 ?
Cl1 U1 Cl2 92.50(4) 2_566 2_566 ?
O1 U1 Cl2 90.55(11) . . ?
O1 U1 Cl2 89.46(11) 2_566 . ?
Cl1 U1 Cl2 92.50(4) . . ?
Cl1 U1 Cl2 87.50(4) 2_566 . ?
Cl2 U1 Cl2 180.0 2_566 . ?
O2 U2 O2 180.0 2 . ?
O2 U2 Cl4 90.49(11) 2 . ?
O2 U2 Cl4 89.51(11) . . ?
O2 U2 Cl4 89.51(11) 2 2 ?
O2 U2 Cl4 90.49(11) . 2 ?
Cl4 U2 Cl4 180.0 . 2 ?
O2 U2 Cl3 92.91(11) 2 2 ?
O2 U2 Cl3 87.09(11) . 2 ?
Cl4 U2 Cl3 87.46(4) . 2 ?
Cl4 U2 Cl3 92.54(4) 2 2 ?
O2 U2 Cl3 87.09(11) 2 . ?
O2 U2 Cl3 92.91(11) . . ?
Cl4 U2 Cl3 92.54(4) . . ?
Cl4 U2 Cl3 87.46(4) 2 . ?
Cl3 U2 Cl3 180.0 2 . ?
C8 N2 C9 121.4(6) . . ?
C8 N2 H2N 123(4) . . ?
C9 N2 H2N 115(4) . . ?
C5 N1 C1 122.4(6) . . ?
C5 N1 H1N 125(4) . . ?
C1 N1 H1N 112(4) . . ?
N1 C1 C2 119.5(6) . . ?
N1 C1 H1 123(3) . . ?
C2 C1 H1 117(3) . . ?
C1 C2 C3 120.7(6) . . ?
C1 C2 H2 117(3) . . ?
C3 C2 H2 122(3) . . ?
C4 C3 C2 117.0(5) . . ?
C4 C3 C6 121.7(6) . . ?
C2 C3 C6 121.3(5) . . ?
C5 C4 C3 121.3(6) . . ?
C5 C4 H4 124(4) . . ?
C3 C4 H4 115(4) . . ?
N1 C5 C4 119.2(6) . . ?
N1 C5 H5 110(3) . . ?
C4 C5 H5 130(3) . . ?
C10 C6 C7 117.1(5) . . ?
C10 C6 C3 122.0(5) . . ?
C7 C6 C3 120.9(6) . . ?
C8 C7 C6 119.8(6) . . ?
C8 C7 H7 124(3) . . ?
C6 C7 H7 116(3) . . ?
N2 C8 C7 120.9(6) . . ?
N2 C8 H8 114(4) . . ?
C7 C8 H8 125(4) . . ?
N2 C9 C10 121.0(6) . . ?
N2 C9 H9 104(4) . . ?
C10 C9 H9 134(4) . . ?
C9 C10 C6 119.7(5) . . ?
C9 C10 H10 130(3) . . ?
C6 C10 H10 110(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
C5 N1 C1 C2 0.4(11) . . . . ?
N1 C1 C2 C3 0.4(11) . . . . ?
C1 C2 C3 C4 -1.0(9) . . . . ?
C1 C2 C3 C6 179.9(7) . . . . ?
C2 C3 C4 C5 0.8(9) . . . . ?
C6 C3 C4 C5 179.8(6) . . . . ?
C1 N1 C5 C4 -0.6(10) . . . . ?
C3 C4 C5 N1 0.0(10) . . . . ?
C4 C3 C6 C10 5.0(9) . . . . ?
C2 C3 C6 C10 -176.0(4) . . . . ?
C4 C3 C6 C7 -173.8(3) . . . . ?
C2 C3 C6 C7 5.3(9) . . . . ?
C10 C6 C7 C8 -2.6(9) . . . . ?
C3 C6 C7 C8 176.2(6) . . . . ?
C9 N2 C8 C7 0.5(10) . . . . ?
C6 C7 C8 N2 1.4(10) . . . . ?
C8 N2 C9 C10 -0.9(10) . . . . ?
N2 C9 C10 C6 -0.5(9) . . . . ?
C7 C6 C10 C9 2.2(8) . . . . ?
C3 C6 C10 C9 -176.6(6) . . . . ?

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
N2 H2N Cl3 0.88(7) 2.51(7) 3.265(5) 144(5) 1_464
N2 H2N Cl4 0.88(7) 3.10(6) 3.543(6) 113(4) 2_464
N2 H2N O1 0.88(7) 2.53(6) 3.072(6) 120(5) 1_454
N1 H1N Cl2 0.79(6) 2.57(5) 3.245(6) 145(5) .
N1 H1N Cl1 0.79(6) 3.13(5) 3.553(6) 116(4) 2_566
N1 H1N O2 0.79(6) 2.71(6) 3.145(6) 117(4) 1_565

_diffrn_measured_fraction_theta_max 0.968
_diffrn_reflns_theta_full        55.00
_diffrn_measured_fraction_theta_full 0.983
_refine_diff_density_max         1.259
_refine_diff_density_min         -0.770
_refine_diff_density_rms         0.122
_database_code_depnum_ccdc_archive 'CCDC 987400'
#######################################################################
#
#                 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_100K_double_cell
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'U O2 Cl4, N2 C10 H10'
_chemical_formula_sum            'C10 H10 Cl4 N2 O2 U'
_chemical_formula_weight         570.03

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'
Cl Cl 0.1484 0.1585 '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                   8.9215(6)
_cell_length_b                   9.8582(7)
_cell_length_c                   10.3689(7)
_cell_angle_alpha                65.720(2)
_cell_angle_beta                 86.220(2)
_cell_angle_gamma                64.640(2)
_cell_volume                     744.42(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9940
_cell_measurement_theta_min      3.95
_cell_measurement_theta_max      33.6

_exptl_crystal_description       'triangular plate'
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.01
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.543
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             520
_exptl_absorpt_coefficient_mu    11.616
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4212
_exptl_absorpt_correction_T_max  0.8927
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker D8 with ApexII detector'
_diffrn_measurement_method       'omega and ohi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            55165
_diffrn_reflns_av_R_equivalents  0.0794
_diffrn_reflns_av_sigmaI/netI    0.0703
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.53
_diffrn_reflns_theta_max         40.60
_reflns_number_total             8941
_reflns_number_gt                5500
_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)+(0.0203P)²+0.5440P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8941
_refine_ls_number_parameters     213
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0824
_refine_ls_R_factor_gt           0.0337
_refine_ls_wR_factor_ref         0.0652
_refine_ls_wR_factor_gt          0.0555
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_restrained_S_all      0.998
_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 0.0000 0.5000 0.5000 0.01327(4) Uani 1 2 d S . .
U2 U 0.0000 0.0000 0.0000 0.01409(4) Uani 1 2 d S . .
O1 O 0.0994(3) 0.6227(3) 0.3946(3) 0.0218(5) Uani 1 1 d . . .
O2 O -0.0334(3) -0.1805(3) 0.0776(3) 0.0197(5) Uani 1 1 d . . .
N2 N -0.7352(4) 0.8013(4) -0.5386(3) 0.0205(6) Uani 1 1 d . . .
H2N H -0.795(5) 0.816(5) -0.607(5) 0.012(7) Uiso 1 1 d . . .
N1 N -0.2338(4) 0.6389(4) 0.0456(3) 0.0232(6) Uani 1 1 d . . .
H1N H -0.175(5) 0.623(5) 0.110(5) 0.012(7) Uiso 1 1 d . . .
Cl1 Cl 0.30004(11) 0.27412(9) 0.65217(9) 0.02013(15) Uani 1 1 d . . .
Cl2 Cl 0.04077(12) 0.36239(10) 0.31759(10) 0.02615(18) Uani 1 1 d . . .
Cl3 Cl -0.06736(11) 0.06230(10) 0.22972(9) 0.02271(16) Uani 1 1 d . . .
Cl4 Cl -0.32006(10) 0.17692(10) -0.11915(9) 0.02029(15) Uani 1 1 d . . .
C1 C -0.2269(6) 0.5123(5) 0.0220(4) 0.0295(8) Uani 1 1 d . . .
H1 H -0.153(6) 0.401(6) 0.091(5) 0.026(12) Uiso 1 1 d . . .
C2 C -0.3198(5) 0.5420(4) -0.0946(4) 0.0259(8) Uani 1 1 d . . .
H2 H -0.313(6) 0.453(6) -0.116(5) 0.028(12) Uiso 1 1 d . . .
C3 C -0.4267(4) 0.7061(4) -0.1887(4) 0.0166(6) Uani 1 1 d . . .
C4 C -0.4313(5) 0.8330(4) -0.1586(4) 0.0202(6) Uani 1 1 d . . .
H4 H -0.507(5) 0.952(5) -0.214(4) 0.011(6) Uiso 1 1 d . . .
C5 C -0.3334(5) 0.7967(4) -0.0411(4) 0.0218(7) Uani 1 1 d . . .
H5 H -0.329(5) 0.875(5) -0.012(4) 0.011(9) Uiso 1 1 d . . .
C6 C -0.5306(4) 0.7400(4) -0.3152(3) 0.0168(6) Uani 1 1 d . . .
C7 C -0.5402(5) 0.6114(4) -0.3327(4) 0.0219(7) Uani 1 1 d . . .
H7 H -0.465(6) 0.490(6) -0.269(5) 0.024(11) Uiso 1 1 d . . .
C8 C -0.6444(5) 0.6443(4) -0.4443(4) 0.0246(7) Uani 1 1 d . . .
H8 H -0.643(6) 0.550(6) -0.448(5) 0.022(11) Uiso 1 1 d . . .
C9 C -0.7281(5) 0.9295(4) -0.5278(4) 0.0210(6) Uani 1 1 d . . .
H9 H -0.801(7) 1.038(6) -0.599(6) 0.032(13) Uiso 1 1 d . . .
C10 C -0.6264(5) 0.9025(4) -0.4166(4) 0.0203(6) Uani 1 1 d . . .
H10 H -0.615(5) 0.994(5) -0.404(4) 0.011(6) Uiso 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 O1 1.774(2) 2_566 ?
U1 O1 1.774(2) . ?
U1 Cl2 2.6733(8) 2_566 ?
U1 Cl2 2.6733(8) . ?
U1 Cl1 2.6786(8) 2_566 ?
U1 Cl1 2.6786(8) . ?
U2 O2 1.774(2) . ?
U2 O2 1.774(2) 2 ?
U2 Cl3 2.6665(8) 2 ?
U2 Cl3 2.6665(8) . ?
U2 Cl4 2.6737(8) 2 ?
U2 Cl4 2.6737(8) . ?
N2 C8 1.339(5) . ?
N2 C9 1.342(5) . ?
N2 H2N 0.84(4) . ?
N1 C5 1.338(5) . ?
N1 C1 1.344(5) . ?
N1 H1N 0.80(5) . ?
C1 C2 1.366(5) . ?
C1 H1 0.97(5) . ?
C2 C3 1.408(5) . ?
C2 H2 0.97(5) . ?
C3 C4 1.393(4) . ?
C3 C6 1.492(5) . ?
C4 C5 1.374(5) . ?
C4 H4 0.99(4) . ?
C5 H5 0.96(4) . ?
C6 C7 1.391(5) . ?
C6 C10 1.401(5) . ?
C7 C8 1.372(5) . ?
C7 H7 1.02(5) . ?
C8 H8 0.94(4) . ?
C9 C10 1.379(5) . ?
C9 H9 0.97(5) . ?
C10 H10 1.00(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 U1 O1 179.999(1) 2_566 . ?
O1 U1 Cl2 90.53(9) 2_566 2_566 ?
O1 U1 Cl2 89.47(9) . 2_566 ?
O1 U1 Cl2 89.47(9) 2_566 . ?
O1 U1 Cl2 90.53(9) . . ?
Cl2 U1 Cl2 180.0 2_566 . ?
O1 U1 Cl1 87.81(9) 2_566 2_566 ?
O1 U1 Cl1 92.19(9) . 2_566 ?
Cl2 U1 Cl1 92.69(3) 2_566 2_566 ?
Cl2 U1 Cl1 87.31(3) . 2_566 ?
O1 U1 Cl1 92.19(9) 2_566 . ?
O1 U1 Cl1 87.81(9) . . ?
Cl2 U1 Cl1 87.31(3) 2_566 . ?
Cl2 U1 Cl1 92.69(3) . . ?
Cl1 U1 Cl1 180.0 2_566 . ?
O2 U2 O2 180.0 . 2 ?
O2 U2 Cl3 87.15(8) . 2 ?
O2 U2 Cl3 92.85(8) 2 2 ?
O2 U2 Cl3 92.85(8) . . ?
O2 U2 Cl3 87.15(8) 2 . ?
Cl3 U2 Cl3 180.0 2 . ?
O2 U2 Cl4 90.74(8) . 2 ?
O2 U2 Cl4 89.26(8) 2 2 ?
Cl3 U2 Cl4 92.89(3) 2 2 ?
Cl3 U2 Cl4 87.11(3) . 2 ?
O2 U2 Cl4 89.26(8) . . ?
O2 U2 Cl4 90.74(8) 2 . ?
Cl3 U2 Cl4 87.11(3) 2 . ?
Cl3 U2 Cl4 92.89(3) . . ?
Cl4 U2 Cl4 180.0 2 . ?
C8 N2 C9 122.0(3) . . ?
C8 N2 H2N 117(3) . . ?
C9 N2 H2N 121(3) . . ?
C5 N1 C1 121.7(3) . . ?
C5 N1 H1N 117(3) . . ?
C1 N1 H1N 121(3) . . ?
N1 C1 C2 120.4(3) . . ?
N1 C1 H1 117(3) . . ?
C2 C1 H1 123(3) . . ?
C1 C2 C3 119.9(3) . . ?
C1 C2 H2 122(3) . . ?
C3 C2 H2 118(3) . . ?
C4 C3 C2 117.5(3) . . ?
C4 C3 C6 122.1(3) . . ?
C2 C3 C6 120.4(3) . . ?
C5 C4 C3 120.4(3) . . ?
C5 C4 H4 115(2) . . ?
C3 C4 H4 124(2) . . ?
N1 C5 C4 120.1(3) . . ?
N1 C5 H5 114(3) . . ?
C4 C5 H5 126(3) . . ?
C7 C6 C10 118.1(3) . . ?
C7 C6 C3 120.8(3) . . ?
C10 C6 C3 121.1(3) . . ?
C8 C7 C6 120.5(3) . . ?
C8 C7 H7 117(3) . . ?
C6 C7 H7 122(3) . . ?
N2 C8 C7 119.7(3) . . ?
N2 C8 H8 125(3) . . ?
C7 C8 H8 115(3) . . ?
N2 C9 C10 120.3(3) . . ?
N2 C9 H9 116(3) . . ?
C10 C9 H9 124(3) . . ?
C9 C10 C6 119.4(3) . . ?
C9 C10 H10 123(2) . . ?
C6 C10 H10 117(2) . . ?

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
C5 N1 C1 C2 1.5(7) . . . . ?
N1 C1 C2 C3 -1.6(7) . . . . ?
C1 C2 C3 C4 0.7(6) . . . . ?
C1 C2 C3 C6 -179.1(4) . . . . ?
C2 C3 C4 C5 0.3(5) . . . . ?
C6 C3 C4 C5 -179.9(3) . . . . ?
C1 N1 C5 C4 -0.5(6) . . . . ?
C3 C4 C5 N1 -0.4(6) . . . . ?
C4 C3 C6 C7 -171.6(3) . . . . ?
C2 C3 C6 C7 8.2(5) . . . . ?
C4 C3 C6 C10 5.8(5) . . . . ?
C2 C3 C6 C10 -174.4(3) . . . . ?
C10 C6 C7 C8 -1.7(6) . . . . ?
C3 C6 C7 C8 175.8(4) . . . . ?
C9 N2 C8 C7 -0.1(6) . . . . ?
C6 C7 C8 N2 1.2(6) . . . . ?
C8 N2 C9 C10 -0.6(6) . . . . ?
N2 C9 C10 C6 0.1(5) . . . . ?
C7 C6 C10 C9 1.0(5) . . . . ?
C3 C6 C10 C9 -176.4(3) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N2 H2N Cl3 0.84(4) 2.61(4) 3.240(3) 133(3) 1_464
N2 H2N Cl4 0.84(4) 2.94(4) 3.481(3) 124(3) 2_464
N2 H2N O1 0.84(4) 2.46(4) 3.021(4) 125(3) 1_454
N1 H1N Cl2 0.80(5) 2.59(4) 3.202(3) 135(4) .
N1 H1N Cl1 0.80(5) 3.02(4) 3.526(3) 124(4) 2_566
N1 H1N O2 0.80(5) 2.64(4) 3.125(4) 121(4) 1_565

_diffrn_measured_fraction_theta_max 0.934
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         2.117
_refine_diff_density_min         -2.410
_refine_diff_density_rms         0.259

_database_code_depnum_ccdc_archive 'CCDC 987401'
