# Electronic Supplementary Material (ESI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 2020

####################################################################### 
# 
# 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_TMBiPDA_U_O_com1
_database_code_depnum_ccdc_archive 'CCDC 1996133'
loop_
_audit_author_name
_audit_author_address
'Yanqiu Yang'
;Institute of Nuclear Physics and Chemistry, China Academy of Engineering Physics
China
;
_audit_update_record             
;
2020-04-10 deposited with the CCDC.	2020-07-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C32 H40 Cl2 N8 O19 U2'
_chemical_formula_weight         1387.68

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'
U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'C 2/m'
_space_group_name_Hall           '-C 2y'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   13.2894(7)
_cell_length_b                   13.4844(11)
_cell_length_c                   12.0007(5)
_cell_angle_alpha                90
_cell_angle_beta                 100.455(5)
_cell_angle_gamma                90
_cell_volume                     2114.8(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1669
_cell_measurement_theta_min      3.4680
_cell_measurement_theta_max      28.6840

_exptl_crystal_description       block
_exptl_crystal_colour            ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.179
_exptl_crystal_F_000             1316
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.250
_exptl_absorpt_coefficient_mu    7.861
_shelx_estimated_absorpt_T_min   0.170
_shelx_estimated_absorpt_T_max   0.244
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.46025
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            4625
_diffrn_reflns_av_unetI/netI     0.0453
_diffrn_reflns_av_R_equivalents  0.0269
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.944
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             2255
_reflns_number_gt                2014
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0464P)²+3.4292P] 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         2255
_refine_ls_number_parameters     146
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0424
_refine_ls_R_factor_gt           0.0351
_refine_ls_wR_factor_ref         0.0896
_refine_ls_wR_factor_gt          0.0851
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_restrained_S_all      1.095
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.55407(2) 0.000000 0.84707(2) 0.02750(13) Uani 1 2 d S T P . .
O1 O 0.5521(4) 0.1786(4) 0.8588(4) 0.0482(13) Uani 1 1 d . . . . .
O2 O 0.6840(5) 0.000000 0.9180(6) 0.051(2) Uani 1 2 d S T P . .
O3 O 0.4282(4) 0.000000 0.7611(5) 0.0381(16) Uani 1 2 d S T P . .
O4 O 0.500000 0.000000 1.000000 0.050(3) Uani 1 4 d S T P . .
N1 N 0.6151(4) 0.0970(5) 0.6833(4) 0.0402(15) Uani 1 1 d . . . . .
N2 N 0.6589(5) 0.3051(5) 0.8583(6) 0.0572(19) Uani 1 1 d . . . . .
C1 C 0.6241(5) 0.0541(6) 0.5852(5) 0.0410(18) Uani 1 1 d . . . . .
C2 C 0.6327(6) 0.1119(9) 0.4909(6) 0.057(3) Uani 1 1 d . . . . .
H2 H 0.640224 0.081966 0.423102 0.069 Uiso 1 1 calc R U . . .
C3 C 0.6301(6) 0.2123(9) 0.4992(7) 0.068(3) Uani 1 1 d . . . . .
H3 H 0.630612 0.251180 0.435257 0.082 Uiso 1 1 calc R U . . .
C4 C 0.6266(6) 0.2569(8) 0.6013(7) 0.062(2) Uani 1 1 d . . . . .
H4 H 0.627163 0.325529 0.608541 0.074 Uiso 1 1 calc R U . . .
C5 C 0.6221(5) 0.1949(7) 0.6946(6) 0.048(2) Uani 1 1 d . . . . .
C6 C 0.6108(5) 0.2302(6) 0.8098(6) 0.0433(17) Uani 1 1 d . . . . .
C7 C 0.7407(8) 0.3579(10) 0.8132(9) 0.097(4) Uani 1 1 d . . . . .
H7A H 0.774599 0.312436 0.770738 0.145 Uiso 1 1 calc R U . . .
H7B H 0.789336 0.384472 0.874969 0.145 Uiso 1 1 calc R U . . .
H7C H 0.711200 0.410949 0.764720 0.145 Uiso 1 1 calc R U . . .
C8 C 0.6324(7) 0.3403(8) 0.9638(8) 0.073(3) Uani 1 1 d . . . . .
H8A H 0.590191 0.398354 0.949222 0.109 Uiso 1 1 calc R U . . .
H8B H 0.693777 0.356510 1.016178 0.109 Uiso 1 1 calc R U . . .
H8C H 0.595787 0.289456 0.995681 0.109 Uiso 1 1 calc R U . . .
Cl1 Cl 0.9217(4) 1.000000 0.7167(6) 0.197 Uani 1 2 d DS T P . .
O6 O 0.9535(18) 1.000000 0.842(3) 0.314(11) Uani 1 2 d S T P A .
O7 O 1.0202(19) 1.000000 0.717(2) 0.314(11) Uani 1 2 d S T P A .
O8 O 0.8611(15) 0.9000(16) 0.726(2) 0.314(11) Uani 0.745(15) 1 d D . P A 1
O8A O 0.868(3) 1.000000 0.592(2) 0.314(11) Uani 0.51(3) 2 d DS T P A 2
O5 O 0.8483(14) 1.000000 0.4265(14) 0.178(7) Uani 1 2 d S T P . .
H5B H 0.876011 1.051470 0.404505 0.266 Uiso 0.5 1 d R U P . .
H5C H 0.876011 0.948530 0.404505 0.266 Uiso 0.5 1 d R U P . .


_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 O2 1.782(6) . ?
U1 O3 1.799(6) . ?
U1 O4 2.0888(3) . ?
U1 O1 2.413(6) 6 ?
U1 O1 2.413(6) . ?
U1 N1 2.610(5) 6 ?
U1 N1 2.610(5) . ?
O1 C6 1.266(8) . ?
N1 C5 1.328(10) . ?
N1 C1 1.337(8) . ?
N2 C6 1.278(9) . ?
N2 C8 1.454(12) . ?
N2 C7 1.482(11) . ?
C1 C2 1.395(10) . ?
C1 C1 1.460(16) 6 ?
C2 C3 1.359(14) . ?
C3 C4 1.373(13) . ?
C4 C5 1.407(11) . ?
C5 C6 1.495(11) . ?
Cl1 O7 1.31(3) . ?
Cl1 O6 1.49(3) . ?
Cl1 O8A 1.53(2) . ?
Cl1 O8 1.585(18) 6_575 ?
Cl1 O8 1.585(18) . ?

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
O2 U1 O3 173.7(3) . . ?
O2 U1 O4 92.2(2) . . ?
O3 U1 O4 94.1(2) . . ?
O2 U1 O1 89.54(11) . 6 ?
O3 U1 O1 90.84(11) . 6 ?
O4 U1 O1 86.56(11) . 6 ?
O2 U1 O1 89.54(12) . . ?
O3 U1 O1 90.84(11) . . ?
O4 U1 O1 86.56(11) . . ?
O1 U1 O1 173.0(2) 6 . ?
O2 U1 N1 87.3(2) . 6 ?
O3 U1 N1 87.2(2) . 6 ?
O4 U1 N1 149.90(15) . 6 ?
O1 U1 N1 63.35(19) 6 6 ?
O1 U1 N1 123.52(19) . 6 ?
O2 U1 N1 87.3(2) . . ?
O3 U1 N1 87.2(2) . . ?
O4 U1 N1 149.90(15) . . ?
O1 U1 N1 123.52(19) 6 . ?
O1 U1 N1 63.35(19) . . ?
N1 U1 N1 60.2(3) 6 . ?
C6 O1 U1 120.5(5) . . ?
U1 O4 U1 180.0 5_657 . ?
C5 N1 C1 120.3(6) . . ?
C5 N1 U1 116.5(5) . . ?
C1 N1 U1 122.5(5) . . ?
C6 N2 C8 118.4(7) . . ?
C6 N2 C7 123.6(8) . . ?
C8 N2 C7 118.1(8) . . ?
N1 C1 C2 120.4(8) . . ?
N1 C1 C1 115.6(4) . 6 ?
C2 C1 C1 123.9(5) . 6 ?
C3 C2 C1 119.4(8) . . ?
C2 C3 C4 120.4(8) . . ?
C3 C4 C5 117.6(9) . . ?
N1 C5 C4 121.4(8) . . ?
N1 C5 C6 113.2(6) . . ?
C4 C5 C6 124.9(8) . . ?
O1 C6 N2 121.4(7) . . ?
O1 C6 C5 115.3(6) . . ?
N2 C6 C5 123.2(7) . . ?
O7 Cl1 O6 84.3(15) . . ?
O7 Cl1 O8A 107(2) . . ?
O6 Cl1 O8A 169(2) . . ?
O7 Cl1 O8 121.4(9) . 6_575 ?
O6 Cl1 O8 89.2(11) . 6_575 ?
O8A Cl1 O8 85.1(12) . 6_575 ?
O7 Cl1 O8 121.4(9) . . ?
O6 Cl1 O8 89.2(11) . . ?
O8 Cl1 O8 116.7(18) 6_575 . ?

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 -5.2(10) . . . . ?
U1 N1 C1 C2 164.5(5) . . . . ?
C5 N1 C1 C1 174.8(5) . . . 6 ?
U1 N1 C1 C1 -15.4(5) . . . 6 ?
N1 C1 C2 C3 -1.1(11) . . . . ?
C1 C1 C2 C3 178.8(5) 6 . . . ?
C1 C2 C3 C4 4.8(12) . . . . ?
C2 C3 C4 C5 -2.3(12) . . . . ?
C1 N1 C5 C4 7.8(11) . . . . ?
U1 N1 C5 C4 -162.5(6) . . . . ?
C1 N1 C5 C6 -179.7(6) . . . . ?
U1 N1 C5 C6 10.0(8) . . . . ?
C3 C4 C5 N1 -4.1(12) . . . . ?
C3 C4 C5 C6 -175.6(7) . . . . ?
U1 O1 C6 N2 -137.4(6) . . . . ?
U1 O1 C6 C5 40.5(8) . . . . ?
C8 N2 C6 O1 -10.0(12) . . . . ?
C7 N2 C6 O1 169.7(8) . . . . ?
C8 N2 C6 C5 172.3(7) . . . . ?
C7 N2 C6 C5 -7.9(13) . . . . ?
N1 C5 C6 O1 -32.0(9) . . . . ?
C4 C5 C6 O1 140.2(7) . . . . ?
N1 C5 C6 N2 145.8(7) . . . . ?
C4 C5 C6 N2 -42.0(12) . . . . ?

_refine_diff_density_max         1.372
_refine_diff_density_min         -0.848
_refine_diff_density_rms         0.169



####################################################################### 
# 
# 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_TMBiPDA_U_O2
_database_code_depnum_ccdc_archive 'CCDC 1996134'
loop_
_audit_author_name
_audit_author_address
'Yanqiu Yang'
;Institute of Nuclear Physics and Chemistry, China Academy of Engineering Physics
China
;
_audit_update_record             
;
2020-04-10 deposited with the CCDC.	2020-07-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C32 H36 Cl2 N8 O18 U2'
_chemical_formula_weight         1367.65

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'
U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'C 2/m'
_space_group_name_Hall           '-C 2y'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   13.2397(16)
_cell_length_b                   13.5158(15)
_cell_length_c                   12.1619(13)
_cell_angle_alpha                90
_cell_angle_beta                 101.628(4)
_cell_angle_gamma                90
_cell_volume                     2131.6(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    8049
_cell_measurement_theta_min      2.56
_cell_measurement_theta_max      28.28

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.131
_exptl_crystal_F_000             1292
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.090
_exptl_absorpt_coefficient_mu    7.796
_shelx_estimated_absorpt_T_min   0.455
_shelx_estimated_absorpt_T_max   0.540
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.1120
_exptl_absorpt_correction_T_max  0.2627
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            7695
_diffrn_reflns_av_unetI/netI     0.0232
_diffrn_reflns_av_R_equivalents  0.0262
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.565
_diffrn_reflns_theta_max         25.004
_diffrn_reflns_theta_full        25.004
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measured_fraction_theta_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_point_group_measured_fraction_full 0.988
_reflns_number_total             1944
_reflns_number_gt                1890
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0468P)²+12.2846P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1944
_refine_ls_number_parameters     165
_refine_ls_number_restraints     240
_refine_ls_R_factor_all          0.0279
_refine_ls_R_factor_gt           0.0272
_refine_ls_wR_factor_ref         0.0774
_refine_ls_wR_factor_gt          0.0769
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_restrained_S_all      1.174
_refine_ls_shift/su_max          0.006
_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 0.2567(8) 0.1416(8) 0.1853(8) 0.087(3) Uani 1 1 d . . . . .
H1A H 0.284614 0.085275 0.229244 0.131 Uiso 1 1 calc R U . . .
H1B H 0.206110 0.119885 0.121858 0.131 Uiso 1 1 calc R U . . .
H1C H 0.224992 0.185348 0.230487 0.131 Uiso 1 1 calc R U . . .
C2 C 0.3646(7) 0.1593(6) 0.0400(7) 0.073(2) Uani 1 1 d . . . . .
H2A H 0.377365 0.215423 -0.003672 0.110 Uiso 1 1 calc R U . . .
H2B H 0.307877 0.121854 -0.001238 0.110 Uiso 1 1 calc R U . . .
H2C H 0.425087 0.118404 0.055798 0.110 Uiso 1 1 calc R U . . .
C3 C 0.3891(5) 0.2704(4) 0.1962(5) 0.0426(13) Uani 1 1 d . . . . .
C4 C 0.3775(5) 0.3048(5) 0.3096(5) 0.0436(13) Uani 1 1 d . . . . .
C5 C 0.3714(5) 0.2442(6) 0.4004(6) 0.0563(17) Uani 1 1 d . . . . .
H5 H 0.369797 0.175732 0.392797 0.068 Uiso 1 1 calc R U . . .
C6 C 0.3680(5) 0.2878(6) 0.5016(6) 0.0586(19) Uani 1 1 d . . . . .
H6 H 0.366369 0.248964 0.564374 0.070 Uiso 1 1 calc R U . . .
C7 C 0.3669(5) 0.3885(6) 0.5095(5) 0.0529(17) Uani 1 1 d . . . . .
H7 H 0.361419 0.419061 0.576589 0.064 Uiso 1 1 calc R U . . .
C8 C 0.3741(4) 0.4450(5) 0.4150(5) 0.0424(13) Uani 1 1 d . . . . .
N1 N 0.3395(5) 0.1936(4) 0.1462(5) 0.0568(14) Uani 1 1 d . . . . .
N2 N 0.3836(3) 0.4028(4) 0.3184(4) 0.0379(11) Uani 1 1 d . . . . .
O1 O 0.4491(3) 0.3209(4) 0.1506(3) 0.0486(11) Uani 1 1 d . U . . .
O2 O 0.5720(4) 0.500000 0.2410(5) 0.0385(12) Uani 1 2 d S TU P . .
O3 O 0.3157(5) 0.500000 0.0848(6) 0.0588(18) Uani 1 2 d S TU P . .
O4 O 0.500000 0.4454(5) 0.000000 0.0596(17) Uani 1 2 d S TU P . .
O5 O 0.436(2) 0.000000 0.838(2) 0.171(5) Uani 0.660(18) 2 d S TU P A 1
O6 O 0.3803(11) 0.0824(11) 0.7103(12) 0.188(3) Uani 0.660(18) 1 d . U P A 1
O7 O 0.5230(15) 0.000000 0.7241(17) 0.170(4) Uani 0.660(18) 2 d S TU P A 1
Cl1 Cl 0.4248(6) 0.000000 0.7167(12) 0.115(2) Uani 0.660(18) 2 d S TU P A 1
Cl1' Cl 0.415(2) 0.000000 0.652(3) 0.149(4) Uani 0.340(18) 2 d S TU P A 2
O6' O 0.3803(11) 0.0824(11) 0.7103(12) 0.188(3) Uani 0.340(18) 1 d . U P A 2
O7' O 0.5230(15) 0.000000 0.7241(17) 0.170(4) Uani 0.340(18) 2 d S TU P A 2
O5' O 0.358(4) 0.000000 0.564(5) 0.166(5) Uani 0.340(18) 2 d S TU P A 2
U1 U 0.44533(2) 0.500000 0.15688(2) 0.02880(13) Uani 1 2 d S T P . .


_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 N1 1.460(10) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 N1 1.471(10) . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C3 O1 1.258(7) . ?
C3 N1 1.311(8) . ?
C3 C4 1.493(9) . ?
C4 N2 1.330(8) . ?
C4 C5 1.390(9) . ?
C5 C6 1.374(11) . ?
C5 H5 0.9300 . ?
C6 C7 1.364(12) . ?
C6 H6 0.9300 . ?
C7 C8 1.400(9) . ?
C7 H7 0.9300 . ?
C8 N2 1.334(8) . ?
C8 C8 1.486(14) 6_565 ?
N2 U1 2.627(5) . ?
O1 U1 2.422(5) . ?
O2 U1 1.780(5) . ?
O3 U1 1.763(7) . ?
O4 O4 1.477(13) 5_665 ?
O4 U1 2.295(2) 5_665 ?
O4 U1 2.295(2) . ?
O5 Cl1 1.46(3) . ?
O6 Cl1 1.255(15) . ?
O7 Cl1 1.28(2) . ?
Cl1' O5' 1.19(6) . ?
Cl1' O6' 1.44(2) . ?
Cl1' O7' 1.51(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
N1 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
N1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C2 H2A 109.5 . . ?
N1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
N1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
O1 C3 N1 121.8(6) . . ?
O1 C3 C4 115.5(5) . . ?
N1 C3 C4 122.7(6) . . ?
N2 C4 C5 122.3(6) . . ?
N2 C4 C3 111.6(5) . . ?
C5 C4 C3 125.7(6) . . ?
C6 C5 C4 118.5(7) . . ?
C6 C5 H5 120.8 . . ?
C4 C5 H5 120.8 . . ?
C7 C6 C5 119.6(6) . . ?
C7 C6 H6 120.2 . . ?
C5 C6 H6 120.2 . . ?
C6 C7 C8 118.9(7) . . ?
C6 C7 H7 120.6 . . ?
C8 C7 H7 120.6 . . ?
N2 C8 C7 121.6(7) . . ?
N2 C8 C8 115.3(4) . 6_565 ?
C7 C8 C8 123.1(4) . 6_565 ?
C3 N1 C1 124.7(7) . . ?
C3 N1 C2 118.4(6) . . ?
C1 N1 C2 116.8(6) . . ?
C4 N2 C8 118.8(5) . . ?
C4 N2 U1 117.4(4) . . ?
C8 N2 U1 122.9(4) . . ?
C3 O1 U1 120.6(4) . . ?
O4 O4 U1 71.23(15) 5_665 5_665 ?
O4 O4 U1 71.23(15) 5_665 . ?
U1 O4 U1 142.5(3) 5_665 . ?
O6 Cl1 O6 125.1(15) . 6 ?
O6 Cl1 O7 117.4(7) . . ?
O6 Cl1 O7 117.4(7) 6 . ?
O6 Cl1 O5 90.7(10) . . ?
O6 Cl1 O5 90.7(10) 6 . ?
O7 Cl1 O5 92.1(15) . . ?
O5' Cl1' O6' 103(2) . . ?
O5' Cl1' O7' 152(4) . . ?
O6' Cl1' O7' 94(2) . . ?
O3 U1 O2 174.9(3) . . ?
O3 U1 O4 91.4(2) . 5_665 ?
O2 U1 O4 93.39(18) . 5_665 ?
O3 U1 O4 91.4(2) . . ?
O2 U1 O4 93.39(18) . . ?
O4 U1 O4 37.5(3) 5_665 . ?
O3 U1 O1 90.49(10) . . ?
O2 U1 O1 89.72(10) . . ?
O4 U1 O1 106.44(18) 5_665 . ?
O4 U1 O1 68.90(18) . . ?
O3 U1 O1 90.49(10) . 6_565 ?
O2 U1 O1 89.72(10) . 6_565 ?
O4 U1 O1 68.91(18) 5_665 6_565 ?
O4 U1 O1 106.44(18) . 6_565 ?
O1 U1 O1 175.27(19) . 6_565 ?
O3 U1 N2 87.3(2) . 6_565 ?
O2 U1 N2 88.25(19) . 6_565 ?
O4 U1 N2 131.21(19) 5_665 6_565 ?
O4 U1 N2 168.68(19) . 6_565 ?
O1 U1 N2 122.34(15) . 6_565 ?
O1 U1 N2 62.34(14) 6_565 6_565 ?
O3 U1 N2 87.3(2) . . ?
O2 U1 N2 88.25(19) . . ?
O4 U1 N2 168.68(19) 5_665 . ?
O4 U1 N2 131.21(19) . . ?
O1 U1 N2 62.34(14) . . ?
O1 U1 N2 122.34(15) 6_565 . ?
N2 U1 N2 60.0(2) 6_565 . ?

_refine_diff_density_max         2.535
_refine_diff_density_min         -1.238
_refine_diff_density_rms         0.134



####################################################################### 
# 
# 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_TMPhenDA_U_O2_com3
_database_code_depnum_ccdc_archive 'CCDC 1996135'
loop_
_audit_author_name
_audit_author_address
'Yanqiu Yang'
;Institute of Nuclear Physics and Chemistry, China Academy of Engineering Physics
China
;
_audit_update_record             
;
2020-04-10 deposited with the CCDC.	2020-07-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H36 Cl2 N8 O18 U2'
_chemical_formula_weight         1415.69

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'
U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   12.9407(8)
_cell_length_b                   13.6890(7)
_cell_length_c                   26.7426(16)
_cell_angle_alpha                90
_cell_angle_beta                 100.647(5)
_cell_angle_gamma                90
_cell_volume                     4655.8(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4737
_cell_measurement_theta_min      3.3720
_cell_measurement_theta_max      28.2010

_exptl_crystal_description       block
_exptl_crystal_colour            ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.020
_exptl_crystal_F_000             2680
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.250
_exptl_absorpt_coefficient_mu    7.142
_shelx_estimated_absorpt_T_min   0.189
_shelx_estimated_absorpt_T_max   0.268
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.51086
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            19749
_diffrn_reflns_av_unetI/netI     0.0945
_diffrn_reflns_av_R_equivalents  0.0539
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         2.968
_diffrn_reflns_theta_max         27.099
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measured_fraction_theta_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_point_group_measured_fraction_full 0.989
_reflns_number_total             9943
_reflns_number_gt                6567
_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.
 
 Structure factors included contributions from the .fab file.
 
 _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.
;

_vrf_PLAT342_191126_s2_yyq_p_u_34_sq 
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.03071 Ang.  
RESPONSE: The crystal is too small, and the diffraction is weak, which cause 
the problem.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0678P)²+95.8844P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9943
_refine_ls_number_parameters     585
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1186
_refine_ls_R_factor_gt           0.0748
_refine_ls_wR_factor_ref         0.2081
_refine_ls_wR_factor_gt          0.1820
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_restrained_S_all      1.069
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.31363(4) 0.17466(4) 0.17886(2) 0.03174(17) Uani 1 1 d . . . . .
U2 U 0.19937(4) 0.20378(4) 0.32024(2) 0.03236(17) Uani 1 1 d . . . . .
O1 O 0.2999(8) -0.0012(7) 0.1904(4) 0.042(3) Uani 1 1 d . . . . .
O2 O 0.3200(9) 0.3550(8) 0.1746(4) 0.044(3) Uani 1 1 d . . . . .
O3 O 0.1827(8) 0.1788(8) 0.1450(4) 0.041(3) Uani 1 1 d . . . . .
O4 O 0.4497(9) 0.1710(9) 0.2067(5) 0.056(3) Uani 1 1 d . . . . .
O5 O 0.2694(15) 0.1384(9) 0.2557(5) 0.091(6) Uani 1 1 d . . . . .
O6 O 0.2012(10) 0.3853(8) 0.3120(4) 0.049(3) Uani 1 1 d . . . . .
O7 O 0.1921(9) 0.0268(10) 0.3196(5) 0.056(3) Uani 1 1 d . . . . .
O8 O 0.0714(10) 0.2050(9) 0.2847(5) 0.056(3) Uani 1 1 d . . . . .
O9 O 0.3229(7) 0.2054(7) 0.3618(4) 0.038(2) Uani 1 1 d . . . . .
O10 O 0.2722(14) 0.2461(8) 0.2512(5) 0.078(5) Uani 1 1 d . . . . .
N1 N 0.3585(9) 0.0590(10) 0.1081(5) 0.035(3) Uani 1 1 d . . . . .
N2 N 0.3726(9) 0.2511(9) 0.0989(5) 0.033(3) Uani 1 1 d . . . . .
N3 N 0.3888(11) -0.1429(10) 0.1906(5) 0.044(3) Uani 1 1 d . . . . .
N4 N 0.4346(12) 0.4703(10) 0.1641(6) 0.053(4) Uani 1 1 d . . . . .
N5 N 0.1345(9) 0.3101(9) 0.3900(5) 0.035(3) Uani 1 1 d . . . . .
N6 N 0.1323(10) 0.1182(12) 0.3956(6) 0.051(4) Uani 1 1 d . . . . .
N7 N 0.1026(13) 0.5149(11) 0.3080(6) 0.057(4) Uani 1 1 d . . . . .
N8 N 0.0782(12) -0.0994(12) 0.3253(7) 0.063(5) Uani 1 1 d . . . . .
C1 C 0.3592(14) -0.0375(13) 0.1153(7) 0.049(4) Uani 1 1 d . . . . .
C2 C 0.3577(14) -0.1027(15) 0.0742(8) 0.058(5) Uani 1 1 d . . . . .
H2 H 0.353622 -0.169769 0.079078 0.070 Uiso 1 1 calc R U . . .
C3 C 0.3622(15) -0.0664(16) 0.0279(8) 0.064(6) Uani 1 1 d . . . . .
H3 H 0.360821 -0.109629 0.001017 0.077 Uiso 1 1 calc R U . . .
C4 C 0.3687(12) 0.0315(15) 0.0188(6) 0.048(3) Uani 1 1 d . . . . .
C5 C 0.3819(14) 0.0767(17) -0.0266(7) 0.058(5) Uani 1 1 d . . . . .
H5 H 0.386501 0.037122 -0.054397 0.070 Uiso 1 1 calc R U . . .
C6 C 0.3882(14) 0.1743(17) -0.0325(7) 0.061(6) Uani 1 1 d . . . . .
H6 H 0.396189 0.199102 -0.063934 0.073 Uiso 1 1 calc R U . . .
C7 C 0.3828(13) 0.2421(15) 0.0089(6) 0.048(3) Uani 1 1 d . . . . .
C8 C 0.3938(14) 0.3399(16) 0.0087(7) 0.058(5) Uani 1 1 d . . . . .
H8 H 0.402331 0.370698 -0.021230 0.069 Uiso 1 1 calc R U . . .
C9 C 0.3929(16) 0.3970(16) 0.0525(8) 0.066(6) Uani 1 1 d . . . . .
H9 H 0.397249 0.464712 0.051472 0.080 Uiso 1 1 calc R U . . .
C10 C 0.3853(13) 0.3480(13) 0.0975(8) 0.054(5) Uani 1 1 d . . . . .
C11 C 0.3728(10) 0.1949(11) 0.0584(6) 0.033(3) Uani 1 1 d . . . . .
C12 C 0.3669(11) 0.0937(13) 0.0615(6) 0.042(4) Uani 1 1 d . . . . .
C13 C 0.3483(12) -0.0634(11) 0.1707(7) 0.041(2) Uani 1 1 d . . . . .
C14 C 0.4633(17) -0.2078(16) 0.1716(9) 0.075(7) Uani 1 1 d . . . . .
H14A H 0.426092 -0.262630 0.154584 0.113 Uiso 1 1 calc R U . . .
H14B H 0.514928 -0.230631 0.199718 0.113 Uiso 1 1 calc R U . . .
H14C H 0.497624 -0.172731 0.148269 0.113 Uiso 1 1 calc R U . . .
C15 C 0.3680(16) -0.1668(15) 0.2417(8) 0.064(5) Uani 1 1 d . . . . .
H15A H 0.335616 -0.111767 0.254900 0.096 Uiso 1 1 calc R U . . .
H15B H 0.433062 -0.181897 0.263994 0.096 Uiso 1 1 calc R U . . .
H15C H 0.321825 -0.222108 0.239411 0.096 Uiso 1 1 calc R U . . .
C16 C 0.3804(12) 0.3935(11) 0.1484(7) 0.041(2) Uani 1 1 d . . . . .
C17 C 0.5172(16) 0.5184(17) 0.1415(10) 0.088(8) Uani 1 1 d . . . . .
H17A H 0.553619 0.470255 0.125186 0.132 Uiso 1 1 calc R U . . .
H17B H 0.566003 0.550520 0.167689 0.132 Uiso 1 1 calc R U . . .
H17C H 0.485536 0.565613 0.116765 0.132 Uiso 1 1 calc R U . . .
C18 C 0.421(2) 0.5120(15) 0.2132(9) 0.083(7) Uani 1 1 d . . . . .
H18A H 0.349634 0.534488 0.210618 0.125 Uiso 1 1 calc R U . . .
H18B H 0.468196 0.565797 0.221817 0.125 Uiso 1 1 calc R U . . .
H18C H 0.435167 0.462827 0.239151 0.125 Uiso 1 1 calc R U . . .
C19 C 0.1275(12) 0.4087(13) 0.3835(6) 0.043(4) Uani 1 1 d . . . . .
C20 C 0.1180(14) 0.4701(17) 0.4241(8) 0.063(6) Uani 1 1 d . . . . .
H20 H 0.114114 0.537183 0.418609 0.075 Uiso 1 1 calc R U . . .
C21 C 0.1143(14) 0.4367(19) 0.4700(8) 0.071(7) Uani 1 1 d . . . . .
H21 H 0.112291 0.478915 0.497017 0.085 Uiso 1 1 calc R U . . .
C22 C 0.1136(13) 0.3304(19) 0.4766(7) 0.065(6) Uani 1 1 d . . . . .
C23 C 0.1096(18) 0.279(3) 0.5242(9) 0.083(9) Uani 1 1 d . . . . .
H23 H 0.105016 0.314534 0.553248 0.100 Uiso 1 1 calc R U . . .
C24 C 0.1124(17) 0.187(3) 0.5266(9) 0.098(11) Uani 1 1 d . . . . .
H24 H 0.109018 0.159028 0.557924 0.118 Uiso 1 1 calc R U . . .
C25 C 0.1206(13) 0.1191(18) 0.4834(8) 0.061(6) Uani 1 1 d . . . . .
C26 C 0.1205(15) 0.020(2) 0.4842(8) 0.078(8) Uani 1 1 d . . . . .
H26 H 0.119909 -0.014068 0.514338 0.094 Uiso 1 1 calc R U . . .
C27 C 0.1212(16) -0.0290(18) 0.4406(9) 0.074(7) Uani 1 1 d . . . . .
H27 H 0.119572 -0.096935 0.440653 0.088 Uiso 1 1 calc R U . . .
C28 C 0.1244(12) 0.0194(13) 0.3958(7) 0.046(4) Uani 1 1 d . . . . .
C29 C 0.1284(13) 0.1683(15) 0.4388(6) 0.048(5) Uani 1 1 d . . . . .
C30 C 0.1264(11) 0.2709(15) 0.4349(6) 0.045(4) Uani 1 1 d . . . . .
C31 C 0.1464(13) 0.4358(11) 0.3313(7) 0.041(2) Uani 1 1 d . . . . .
C32 C 0.0203(17) 0.5730(17) 0.3239(8) 0.076(7) Uani 1 1 d . . . . .
H32A H -0.007595 0.538366 0.349629 0.114 Uiso 1 1 calc R U . . .
H32B H -0.034805 0.584633 0.295157 0.114 Uiso 1 1 calc R U . . .
H32C H 0.049051 0.634244 0.337312 0.114 Uiso 1 1 calc R U . . .
C33 C 0.1314(17) 0.5454(14) 0.2600(9) 0.072(6) Uani 1 1 d . . . . .
H33A H 0.182674 0.596737 0.266395 0.108 Uiso 1 1 calc R U . . .
H33B H 0.069972 0.568736 0.237391 0.108 Uiso 1 1 calc R U . . .
H33C H 0.160326 0.490849 0.244760 0.108 Uiso 1 1 calc R U . . .
C34 C 0.1336(13) -0.0220(13) 0.3453(7) 0.048(4) Uani 1 1 d . . . . .
C35 C -0.0012(15) -0.1471(16) 0.3481(10) 0.080(7) Uani 1 1 d . . . . .
H35A H 0.031051 -0.196763 0.371201 0.121 Uiso 1 1 calc R U . . .
H35B H -0.052648 -0.176427 0.321961 0.121 Uiso 1 1 calc R U . . .
H35C H -0.034697 -0.099914 0.366339 0.121 Uiso 1 1 calc R U . . .
C36 C 0.0955(18) -0.1355(17) 0.2764(9) 0.079(7) Uani 1 1 d . . . . .
H36A H 0.133684 -0.087648 0.260891 0.118 Uiso 1 1 calc R U . . .
H36B H 0.028932 -0.147691 0.254699 0.118 Uiso 1 1 calc R U . . .
H36C H 0.135223 -0.195086 0.281310 0.118 Uiso 1 1 calc R U . . .
Cl1 Cl 0.3086(5) -0.2707(5) 0.3904(3) 0.0796(17) Uani 1 1 d . . . . .
O11 O 0.3851(19) -0.325(3) 0.4156(12) 0.216(18) Uani 1 1 d . . . . .
O12 O 0.216(2) -0.276(3) 0.4098(17) 0.245(19) Uani 1 1 d . . . . .
O13 O 0.335(3) -0.186(3) 0.403(3) 0.37(4) Uani 1 1 d . . . . .
O14 O 0.287(5) -0.279(4) 0.3432(10) 0.35(3) Uani 1 1 d . . . . .
Cl2 Cl 0.1760(5) 0.6441(6) 0.1117(3) 0.093(2) Uani 1 1 d . . . . .
O15 O 0.129(3) 0.555(2) 0.1152(11) 0.229(17) Uani 1 1 d . . . . .
O16 O 0.275(2) 0.630(3) 0.1017(13) 0.26(2) Uani 1 1 d . . . . .
O17 O 0.125(2) 0.692(2) 0.0683(12) 0.202(15) Uani 1 1 d . . . . .
O18 O 0.190(3) 0.707(3) 0.1491(16) 0.30(3) Uani 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 O3 1.767(11) . ?
U1 O4 1.781(12) . ?
U1 O5 2.286(11) . ?
U1 O10 2.318(11) . ?
U1 O1 2.438(10) . ?
U1 O2 2.473(10) . ?
U1 N1 2.613(12) . ?
U1 N2 2.618(12) . ?
U2 O8 1.751(11) . ?
U2 O9 1.770(10) . ?
U2 O5 2.277(11) . ?
U2 O10 2.296(11) . ?
U2 O7 2.425(14) . ?
U2 O6 2.495(11) . ?
U2 N6 2.614(14) . ?
U2 N5 2.624(12) . ?
O1 C13 1.229(18) . ?
O2 C16 1.259(19) . ?
O6 C31 1.176(19) . ?
O7 C34 1.298(19) . ?
N1 C1 1.33(2) . ?
N1 C12 1.357(19) . ?
N2 C11 1.328(19) . ?
N2 C10 1.34(2) . ?
N3 C13 1.28(2) . ?
N3 C14 1.47(2) . ?
N3 C15 1.48(2) . ?
N4 C16 1.29(2) . ?
N4 C17 1.48(2) . ?
N4 C18 1.47(3) . ?
N5 C30 1.34(2) . ?
N5 C19 1.36(2) . ?
N6 C29 1.35(2) . ?
N6 C28 1.36(2) . ?
N7 C31 1.32(2) . ?
N7 C33 1.46(2) . ?
N7 C32 1.45(2) . ?
N8 C34 1.33(2) . ?
N8 C36 1.45(3) . ?
N8 C35 1.44(2) . ?
C1 C2 1.41(2) . ?
C1 C13 1.56(2) . ?
C2 C3 1.34(3) . ?
C3 C4 1.37(3) . ?
C4 C5 1.40(2) . ?
C4 C12 1.43(2) . ?
C5 C6 1.35(3) . ?
C6 C7 1.46(3) . ?
C7 C8 1.35(3) . ?
C7 C11 1.50(2) . ?
C8 C9 1.41(3) . ?
C9 C10 1.40(2) . ?
C10 C16 1.51(3) . ?
C11 C12 1.39(2) . ?
C19 C20 1.40(2) . ?
C19 C31 1.51(2) . ?
C20 C21 1.32(3) . ?
C21 C22 1.47(3) . ?
C22 C30 1.41(3) . ?
C22 C23 1.47(3) . ?
C23 C24 1.25(4) . ?
C24 C25 1.50(4) . ?
C25 C26 1.36(3) . ?
C25 C29 1.39(2) . ?
C26 C27 1.34(3) . ?
C27 C28 1.38(3) . ?
C28 C34 1.49(3) . ?
C29 C30 1.41(3) . ?
Cl1 O13 1.23(4) . ?
Cl1 O14 1.25(3) . ?
Cl1 O11 1.32(2) . ?
Cl1 O12 1.39(3) . ?
Cl2 O15 1.37(3) . ?
Cl2 O18 1.31(2) . ?
Cl2 O16 1.37(2) . ?
Cl2 O17 1.39(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 U1 O4 174.1(5) . . ?
O3 U1 O5 95.2(6) . . ?
O4 U1 O5 90.6(6) . . ?
O3 U1 O10 93.8(6) . . ?
O4 U1 O10 91.5(6) . . ?
O5 U1 O10 37.5(4) . . ?
O3 U1 O1 90.6(4) . . ?
O4 U1 O1 90.5(5) . . ?
O5 U1 O1 68.7(4) . . ?
O10 U1 O1 106.2(4) . . ?
O3 U1 O2 88.9(4) . . ?
O4 U1 O2 90.5(5) . . ?
O5 U1 O2 105.9(4) . . ?
O10 U1 O2 68.4(4) . . ?
O1 U1 O2 174.5(3) . . ?
O3 U1 N1 88.2(4) . . ?
O4 U1 N1 87.2(5) . . ?
O5 U1 N1 130.1(4) . . ?
O10 U1 N1 167.6(4) . . ?
O1 U1 N1 61.6(4) . . ?
O2 U1 N1 123.9(4) . . ?
O3 U1 N2 88.0(4) . . ?
O4 U1 N2 86.4(5) . . ?
O5 U1 N2 168.5(4) . . ?
O10 U1 N2 131.4(4) . . ?
O1 U1 N2 122.5(4) . . ?
O2 U1 N2 63.0(4) . . ?
N1 U1 N2 60.9(4) . . ?
O8 U2 O9 174.1(5) . . ?
O8 U2 O5 93.5(7) . . ?
O9 U2 O5 92.3(6) . . ?
O8 U2 O10 92.8(6) . . ?
O9 U2 O10 92.5(6) . . ?
O5 U2 O10 37.8(4) . . ?
O8 U2 O7 88.5(5) . . ?
O9 U2 O7 92.7(4) . . ?
O5 U2 O7 67.8(4) . . ?
O10 U2 O7 105.5(4) . . ?
O8 U2 O6 88.0(5) . . ?
O9 U2 O6 91.2(4) . . ?
O5 U2 O6 108.2(4) . . ?
O10 U2 O6 70.5(4) . . ?
O7 U2 O6 174.6(4) . . ?
O8 U2 N6 90.5(5) . . ?
O9 U2 N6 85.0(5) . . ?
O5 U2 N6 130.1(5) . . ?
O10 U2 N6 167.6(5) . . ?
O7 U2 N6 62.6(4) . . ?
O6 U2 N6 121.6(4) . . ?
O8 U2 N5 89.2(5) . . ?
O9 U2 N5 85.3(4) . . ?
O5 U2 N5 169.1(4) . . ?
O10 U2 N5 131.6(4) . . ?
O7 U2 N5 122.8(4) . . ?
O6 U2 N5 61.3(4) . . ?
N6 U2 N5 60.3(5) . . ?
C13 O1 U1 125.1(10) . . ?
C16 O2 U1 118.2(10) . . ?
U2 O5 U1 142.8(6) . . ?
C31 O6 U2 122.0(11) . . ?
C34 O7 U2 122.4(11) . . ?
U2 O10 U1 139.2(5) . . ?
C1 N1 C12 118.6(14) . . ?
C1 N1 U1 119.5(10) . . ?
C12 N1 U1 121.2(11) . . ?
C11 N2 C10 122.1(15) . . ?
C11 N2 U1 118.7(9) . . ?
C10 N2 U1 118.4(11) . . ?
C13 N3 C14 128.1(16) . . ?
C13 N3 C15 116.1(15) . . ?
C14 N3 C15 115.4(15) . . ?
C16 N4 C17 128.3(18) . . ?
C16 N4 C18 117.3(16) . . ?
C17 N4 C18 114.2(17) . . ?
C30 N5 C19 119.8(14) . . ?
C30 N5 U2 120.3(11) . . ?
C19 N5 U2 118.8(10) . . ?
C29 N6 C28 119.2(16) . . ?
C29 N6 U2 120.1(12) . . ?
C28 N6 U2 119.1(12) . . ?
C31 N7 C33 119.4(16) . . ?
C31 N7 C32 125.6(18) . . ?
C33 N7 C32 114.8(16) . . ?
C34 N8 C36 118.1(17) . . ?
C34 N8 C35 124.1(19) . . ?
C36 N8 C35 117.7(18) . . ?
N1 C1 C2 121.0(17) . . ?
N1 C1 C13 111.2(14) . . ?
C2 C1 C13 127.3(17) . . ?
C3 C2 C1 119.0(19) . . ?
C4 C3 C2 122.8(19) . . ?
C3 C4 C5 127.5(19) . . ?
C3 C4 C12 115.5(16) . . ?
C5 C4 C12 116.9(18) . . ?
C6 C5 C4 123.9(19) . . ?
C5 C6 C7 122.0(16) . . ?
C8 C7 C6 127.6(17) . . ?
C8 C7 C11 117.2(17) . . ?
C6 C7 C11 114.9(17) . . ?
C7 C8 C9 122.1(18) . . ?
C10 C9 C8 117(2) . . ?
N2 C10 C9 122(2) . . ?
N2 C10 C16 111.0(15) . . ?
C9 C10 C16 126.8(18) . . ?
N2 C11 C12 121.3(14) . . ?
N2 C11 C7 119.0(15) . . ?
C12 C11 C7 119.7(15) . . ?
N1 C12 C11 114.7(14) . . ?
N1 C12 C4 122.8(16) . . ?
C11 C12 C4 122.5(15) . . ?
O1 C13 N3 127.8(17) . . ?
O1 C13 C1 113.1(14) . . ?
N3 C13 C1 119.1(15) . . ?
O2 C16 N4 121.0(16) . . ?
O2 C16 C10 117.6(13) . . ?
N4 C16 C10 121.4(16) . . ?
N5 C19 C20 120.7(17) . . ?
N5 C19 C31 110.1(14) . . ?
C20 C19 C31 128.6(18) . . ?
C21 C20 C19 123(2) . . ?
C20 C21 C22 117.3(18) . . ?
C30 C22 C23 116(2) . . ?
C30 C22 C21 118.1(18) . . ?
C23 C22 C21 126(2) . . ?
C24 C23 C22 121(3) . . ?
C23 C24 C25 126(3) . . ?
C26 C25 C29 120(2) . . ?
C26 C25 C24 127(2) . . ?
C29 C25 C24 113(2) . . ?
C25 C26 C27 119(2) . . ?
C28 C27 C26 121(2) . . ?
C27 C28 N6 120(2) . . ?
C27 C28 C34 128.7(19) . . ?
N6 C28 C34 110.9(15) . . ?
N6 C29 C30 116.5(15) . . ?
N6 C29 C25 120(2) . . ?
C30 C29 C25 122.9(18) . . ?
N5 C30 C29 117.5(15) . . ?
N5 C30 C22 121.1(18) . . ?
C29 C30 C22 121.3(17) . . ?
O6 C31 N7 121.0(18) . . ?
O6 C31 C19 118.4(15) . . ?
N7 C31 C19 120.6(16) . . ?
O7 C34 N8 121.2(18) . . ?
O7 C34 C28 115.9(16) . . ?
N8 C34 C28 122.6(15) . . ?
O13 Cl1 O14 111(4) . . ?
O13 Cl1 O11 104(3) . . ?
O14 Cl1 O11 118(3) . . ?
O13 Cl1 O12 100(3) . . ?
O14 Cl1 O12 109(3) . . ?
O11 Cl1 O12 114(2) . . ?
O15 Cl2 O18 122(3) . . ?
O15 Cl2 O16 109(3) . . ?
O18 Cl2 O16 104(3) . . ?
O15 Cl2 O17 109(2) . . ?
O18 Cl2 O17 108(3) . . ?
O16 Cl2 O17 103(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
C12 N1 C1 C2 -6(2) . . . . ?
U1 N1 C1 C2 164.6(13) . . . . ?
C12 N1 C1 C13 -179.7(13) . . . . ?
U1 N1 C1 C13 -8.7(18) . . . . ?
N1 C1 C2 C3 4(3) . . . . ?
C13 C1 C2 C3 176.2(17) . . . . ?
C1 C2 C3 C4 0(3) . . . . ?
C2 C3 C4 C5 174.7(19) . . . . ?
C2 C3 C4 C12 -2(3) . . . . ?
C3 C4 C5 C6 -179.6(19) . . . . ?
C12 C4 C5 C6 -3(3) . . . . ?
C4 C5 C6 C7 1(3) . . . . ?
C5 C6 C7 C8 176.0(19) . . . . ?
C5 C6 C7 C11 2(2) . . . . ?
C6 C7 C8 C9 -176.2(18) . . . . ?
C11 C7 C8 C9 -2(3) . . . . ?
C7 C8 C9 C10 3(3) . . . . ?
C11 N2 C10 C9 4(2) . . . . ?
U1 N2 C10 C9 -165.2(14) . . . . ?
C11 N2 C10 C16 179.4(13) . . . . ?
U1 N2 C10 C16 10.0(17) . . . . ?
C8 C9 C10 N2 -4(3) . . . . ?
C8 C9 C10 C16 -178.5(16) . . . . ?
C10 N2 C11 C12 175.4(14) . . . . ?
U1 N2 C11 C12 -15.2(17) . . . . ?
C10 N2 C11 C7 -3(2) . . . . ?
U1 N2 C11 C7 166.5(10) . . . . ?
C8 C7 C11 N2 2(2) . . . . ?
C6 C7 C11 N2 176.8(13) . . . . ?
C8 C7 C11 C12 -176.5(15) . . . . ?
C6 C7 C11 C12 -2(2) . . . . ?
C1 N1 C12 C11 -175.8(14) . . . . ?
U1 N1 C12 C11 13.4(17) . . . . ?
C1 N1 C12 C4 5(2) . . . . ?
U1 N1 C12 C4 -166.2(11) . . . . ?
N2 C11 C12 N1 1(2) . . . . ?
C7 C11 C12 N1 179.8(12) . . . . ?
N2 C11 C12 C4 -179.0(13) . . . . ?
C7 C11 C12 C4 -1(2) . . . . ?
C3 C4 C12 N1 0(2) . . . . ?
C5 C4 C12 N1 -177.6(15) . . . . ?
C3 C4 C12 C11 -180.0(15) . . . . ?
C5 C4 C12 C11 3(2) . . . . ?
U1 O1 C13 N3 141.5(15) . . . . ?
U1 O1 C13 C1 -38.1(19) . . . . ?
C14 N3 C13 O1 -167.1(19) . . . . ?
C15 N3 C13 O1 5(3) . . . . ?
C14 N3 C13 C1 13(3) . . . . ?
C15 N3 C13 C1 -175.1(15) . . . . ?
N1 C1 C13 O1 28(2) . . . . ?
C2 C1 C13 O1 -144.6(18) . . . . ?
N1 C1 C13 N3 -151.5(15) . . . . ?
C2 C1 C13 N3 36(3) . . . . ?
U1 O2 C16 N4 -139.6(13) . . . . ?
U1 O2 C16 C10 41.7(18) . . . . ?
C17 N4 C16 O2 172.6(18) . . . . ?
C18 N4 C16 O2 -1(3) . . . . ?
C17 N4 C16 C10 -9(3) . . . . ?
C18 N4 C16 C10 177.2(17) . . . . ?
N2 C10 C16 O2 -34(2) . . . . ?
C9 C10 C16 O2 141.3(19) . . . . ?
N2 C10 C16 N4 147.8(15) . . . . ?
C9 C10 C16 N4 -37(3) . . . . ?
C30 N5 C19 C20 4(2) . . . . ?
U2 N5 C19 C20 -164.7(12) . . . . ?
C30 N5 C19 C31 176.1(13) . . . . ?
U2 N5 C19 C31 7.7(16) . . . . ?
N5 C19 C20 C21 -1(3) . . . . ?
C31 C19 C20 C21 -171.5(17) . . . . ?
C19 C20 C21 C22 -4(3) . . . . ?
C20 C21 C22 C30 6(3) . . . . ?
C20 C21 C22 C23 -180.0(19) . . . . ?
C30 C22 C23 C24 -3(3) . . . . ?
C21 C22 C23 C24 -178(2) . . . . ?
C22 C23 C24 C25 0(4) . . . . ?
C23 C24 C25 C26 -178(3) . . . . ?
C23 C24 C25 C29 2(3) . . . . ?
C29 C25 C26 C27 -4(3) . . . . ?
C24 C25 C26 C27 175.4(19) . . . . ?
C25 C26 C27 C28 1(3) . . . . ?
C26 C27 C28 N6 3(3) . . . . ?
C26 C27 C28 C34 175.0(18) . . . . ?
C29 N6 C28 C27 -5(2) . . . . ?
U2 N6 C28 C27 160.0(13) . . . . ?
C29 N6 C28 C34 -178.3(14) . . . . ?
U2 N6 C28 C34 -13.0(18) . . . . ?
C28 N6 C29 C30 -173.8(14) . . . . ?
U2 N6 C29 C30 21.0(19) . . . . ?
C28 N6 C29 C25 2(2) . . . . ?
U2 N6 C29 C25 -162.7(12) . . . . ?
C26 C25 C29 N6 2(3) . . . . ?
C24 C25 C29 N6 -177.4(16) . . . . ?
C26 C25 C29 C30 178.4(17) . . . . ?
C24 C25 C29 C30 -1(2) . . . . ?
C19 N5 C30 C29 176.6(14) . . . . ?
U2 N5 C30 C29 -15.2(18) . . . . ?
C19 N5 C30 C22 -2(2) . . . . ?
U2 N5 C30 C22 166.4(11) . . . . ?
N6 C29 C30 N5 -4(2) . . . . ?
C25 C29 C30 N5 -179.9(15) . . . . ?
N6 C29 C30 C22 174.7(15) . . . . ?
C25 C29 C30 C22 -2(3) . . . . ?
C23 C22 C30 N5 -177.8(16) . . . . ?
C21 C22 C30 N5 -3(2) . . . . ?
C23 C22 C30 C29 4(2) . . . . ?
C21 C22 C30 C29 178.8(16) . . . . ?
U2 O6 C31 N7 -142.1(13) . . . . ?
U2 O6 C31 C19 38(2) . . . . ?
C33 N7 C31 O6 -6(3) . . . . ?
C32 N7 C31 O6 168.8(18) . . . . ?
C33 N7 C31 C19 173.2(16) . . . . ?
C32 N7 C31 C19 -12(3) . . . . ?
N5 C19 C31 O6 -29(2) . . . . ?
C20 C19 C31 O6 142.5(18) . . . . ?
N5 C19 C31 N7 151.3(15) . . . . ?
C20 C19 C31 N7 -37(3) . . . . ?
U2 O7 C34 N8 137.9(14) . . . . ?
U2 O7 C34 C28 -36(2) . . . . ?
C36 N8 C34 O7 8(3) . . . . ?
C35 N8 C34 O7 -169.4(18) . . . . ?
C36 N8 C34 C28 -178.3(17) . . . . ?
C35 N8 C34 C28 4(3) . . . . ?
C27 C28 C34 O7 -141.6(18) . . . . ?
N6 C28 C34 O7 31(2) . . . . ?
C27 C28 C34 N8 44(3) . . . . ?
N6 C28 C34 N8 -143.5(16) . . . . ?

_refine_diff_density_max         4.387
_refine_diff_density_min         -2.298
_refine_diff_density_rms         0.247




_vrf_PLAT342_TMPhenDA_U_O2_com3  
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.03071 Ang.  
RESPONSE: Low Bond Precision on  C-C Bonds is caused by the weak diffraction of
small crystal.
;
####################################################################### 
# 
# 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_TMPhenDA_U_O2_com4
_database_code_depnum_ccdc_archive 'CCDC 1996136'
loop_
_audit_author_name
_audit_author_address
'Yanqiu Yang'
;Institute of Nuclear Physics and Chemistry, China Academy of Engineering Physics
China
;
_audit_update_record             
;
2020-04-10 deposited with the CCDC.	2020-07-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H39 Cl2 N9 O18 U2'
_chemical_formula_weight         1456.74

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'
U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_H-M_alt        'P c'
_space_group_name_Hall           'P -2yc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   9.5965(3)
_cell_length_b                   13.8670(4)
_cell_length_c                   19.3265(7)
_cell_angle_alpha                90
_cell_angle_beta                 91.578(3)
_cell_angle_gamma                90
_cell_volume                     2570.89(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3767
_cell_measurement_theta_min      3.3660
_cell_measurement_theta_max      27.1520

_exptl_crystal_description       block
_exptl_crystal_colour            ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.882
_exptl_crystal_F_000             1384
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.250
_exptl_absorpt_coefficient_mu    6.471
_shelx_estimated_absorpt_T_min   0.210
_shelx_estimated_absorpt_T_max   0.295
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.87491
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            11620
_diffrn_reflns_av_unetI/netI     0.0669
_diffrn_reflns_av_R_equivalents  0.0406
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.938
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.668
_diffrn_reflns_point_group_measured_fraction_full 0.684
_reflns_number_total             7008
_reflns_number_gt                6297
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.336
_reflns_Friedel_fraction_max     0.336
_reflns_Friedel_fraction_full    0.368

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0261P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.446(9)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         7008
_refine_ls_number_parameters     608
_refine_ls_number_restraints     8
_refine_ls_R_factor_all          0.0442
_refine_ls_R_factor_gt           0.0370
_refine_ls_wR_factor_ref         0.0766
_refine_ls_wR_factor_gt          0.0728
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_restrained_S_all      1.016
_refine_ls_shift/su_max          0.082
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.57118(4) 0.49074(3) 0.51416(3) 0.03275(14) Uani 1 1 d . . . . .
U2 U 0.41956(4) 0.20780(3) 0.45971(3) 0.03297(13) Uani 1 1 d . . . . .
O1 O 0.3956(13) 0.4984(7) 0.6034(7) 0.055(3) Uani 1 1 d . . . . .
O2 O 0.7642(9) 0.4646(7) 0.4340(5) 0.036(2) Uani 1 1 d . . . . .
O3 O 0.4676(8) 0.5573(8) 0.4535(6) 0.050(3) Uani 1 1 d . . . . .
O4 O 0.6751(9) 0.4338(8) 0.5773(5) 0.059(3) Uani 1 1 d . . . . .
O5 O 0.5372(11) 0.3515(8) 0.4494(7) 0.079(4) Uani 1 1 d . . . . .
O6 O 0.4209(12) 0.3607(9) 0.4987(7) 0.096(5) Uani 1 1 d . . . . .
O7 O 0.2355(10) 0.2395(8) 0.5402(6) 0.0495(19) Uani 1 1 d . . . . .
O8 O 0.6007(11) 0.1916(8) 0.3775(7) 0.0495(19) Uani 1 1 d . . . . .
O9 O 0.3015(10) 0.2378(8) 0.3903(6) 0.052(3) Uani 1 1 d . . . . .
O10 O 0.5325(9) 0.1647(9) 0.5264(5) 0.056(3) Uani 1 1 d . . . . .
N1 N 0.5507(10) 0.6480(8) 0.5873(6) 0.036(3) Uani 1 1 d . . . . .
N2 N 0.7467(10) 0.6329(9) 0.4958(6) 0.034(3) Uani 1 1 d . . . . .
N3 N 0.3476(11) 0.5353(10) 0.7142(6) 0.051(3) Uani 1 1 d . . . . .
N4 N 0.9973(11) 0.4781(9) 0.4201(6) 0.039(3) Uani 1 1 d . . . . .
N5 N 0.2520(10) 0.0674(8) 0.4898(5) 0.029(3) Uani 1 1 d . . . . .
N6 N 0.4618(11) 0.0396(8) 0.4017(6) 0.033(3) Uani 1 1 d . . . . .
N7 N 0.0069(11) 0.2271(10) 0.5574(8) 0.053(4) Uani 1 1 d . . . . .
N8 N 0.7022(11) 0.1376(9) 0.2836(6) 0.045(3) Uani 1 1 d . . . . .
C1 C 0.4541(13) 0.6527(11) 0.6355(8) 0.040(4) Uani 1 1 d . . . . .
C2 C 0.4049(15) 0.7414(13) 0.6605(8) 0.056(5) Uani 1 1 d . . . . .
H2 H 0.336804 0.743577 0.693764 0.067 Uiso 1 1 calc R U . . .
C3 C 0.4618(16) 0.8269(12) 0.6336(8) 0.055(4) Uani 1 1 d . . . . .
H3 H 0.427136 0.886204 0.647489 0.066 Uiso 1 1 calc R U . . .
C4 C 0.5662(14) 0.8240(10) 0.5878(8) 0.041(4) Uani 1 1 d . . . . .
C5 C 0.6368(14) 0.9063(13) 0.5580(8) 0.053(4) Uani 1 1 d . U . . .
H5 H 0.611907 0.967596 0.572796 0.064 Uiso 1 1 calc R U . . .
C6 C 0.7355(15) 0.8993(11) 0.5105(7) 0.045(4) Uani 1 1 d . . . . .
H6 H 0.773312 0.954637 0.491310 0.054 Uiso 1 1 calc R U . . .
C7 C 0.7823(14) 0.8056(11) 0.4896(7) 0.041(4) Uani 1 1 d . . . . .
C8 C 0.8856(14) 0.7877(13) 0.4414(8) 0.049(4) Uani 1 1 d . . . . .
H8 H 0.929030 0.839801 0.420696 0.059 Uiso 1 1 calc R U . . .
C9 C 0.9247(15) 0.6971(11) 0.4241(8) 0.044(4) Uani 1 1 d . . . . .
H9 H 0.996761 0.687328 0.393666 0.053 Uiso 1 1 calc R U . . .
C10 C 0.8541(12) 0.6176(12) 0.4528(6) 0.036(4) Uani 1 1 d . . . . .
C11 C 0.7120(14) 0.7217(10) 0.5153(7) 0.033(3) Uani 1 1 d . . . . .
C12 C 0.6063(13) 0.7300(11) 0.5651(7) 0.033(3) Uani 1 1 d . . . . .
C13 C 0.3963(13) 0.5568(11) 0.6529(8) 0.045(4) Uani 1 1 d . . . . .
C14 C 0.3709(17) 0.5913(14) 0.7747(8) 0.067(5) Uani 1 1 d . . . . .
H14A H 0.465150 0.614539 0.776060 0.101 Uiso 1 1 calc R U . . .
H14B H 0.355590 0.552196 0.814830 0.101 Uiso 1 1 calc R U . . .
H14C H 0.307766 0.644974 0.774368 0.101 Uiso 1 1 calc R U . . .
C15 C 0.2658(15) 0.4475(12) 0.7227(9) 0.064(5) Uani 1 1 d . . . . .
H15A H 0.168300 0.462638 0.718697 0.096 Uiso 1 1 calc R U . . .
H15B H 0.286199 0.420152 0.767487 0.096 Uiso 1 1 calc R U . . .
H15C H 0.289126 0.401829 0.687498 0.096 Uiso 1 1 calc R U . . .
C16 C 0.8744(14) 0.5143(10) 0.4354(7) 0.034(3) Uani 1 1 d . . . . .
C17 C 1.1304(13) 0.5267(14) 0.4281(9) 0.061(5) Uani 1 1 d . . . . .
H17A H 1.119664 0.583476 0.455930 0.091 Uiso 1 1 calc R U . . .
H17B H 1.163070 0.544754 0.383424 0.091 Uiso 1 1 calc R U . . .
H17C H 1.196756 0.484228 0.450323 0.091 Uiso 1 1 calc R U . . .
C18 C 1.0038(14) 0.3782(12) 0.3928(7) 0.053(4) Uani 1 1 d . . . . .
H18A H 0.946889 0.336748 0.420069 0.080 Uiso 1 1 calc R U . . .
H18B H 1.098523 0.355844 0.395176 0.080 Uiso 1 1 calc R U . . .
H18C H 0.970271 0.377302 0.345567 0.080 Uiso 1 1 calc R U . . .
C19 C 0.1473(12) 0.0806(11) 0.5309(7) 0.034(3) Uani 1 1 d . . . . .
C20 C 0.0821(16) 0.0060(13) 0.5630(9) 0.052(4) Uani 1 1 d . . . . .
H20 H 0.012981 0.018243 0.594626 0.062 Uiso 1 1 calc R U . . .
C21 C 0.1186(16) -0.0855(13) 0.5483(9) 0.056(5) Uani 1 1 d . . . . .
H21 H 0.075154 -0.136076 0.570802 0.068 Uiso 1 1 calc R U . . .
C22 C 0.2192(16) -0.1055(12) 0.5007(8) 0.045(4) Uani 1 1 d . . . . .
C23 C 0.2581(17) -0.1993(13) 0.4824(9) 0.061(5) Uani 1 1 d . . . . .
H23 H 0.211912 -0.251569 0.501314 0.073 Uiso 1 1 calc R U . . .
C24 C 0.361(2) -0.2149(11) 0.4382(10) 0.064(5) Uani 1 1 d . . . . .
H24 H 0.386739 -0.277676 0.427728 0.077 Uiso 1 1 calc R U . . .
C25 C 0.4304(16) -0.1348(11) 0.4067(8) 0.050(4) Uani 1 1 d . . . . .
C26 C 0.5479(17) -0.1437(12) 0.3618(8) 0.056(5) Uani 1 1 d . . . . .
H26 H 0.579205 -0.204240 0.348583 0.067 Uiso 1 1 calc R U . . .
C27 C 0.6115(17) -0.0638(12) 0.3393(8) 0.053(4) Uani 1 1 d . . . . .
H27 H 0.688026 -0.069403 0.311085 0.064 Uiso 1 1 calc R U . . .
C28 C 0.5645(13) 0.0271(11) 0.3577(7) 0.041(4) Uani 1 1 d . . . . .
C29 C 0.3902(14) -0.0405(11) 0.4257(7) 0.037(3) Uani 1 1 d . . . . .
C30 C 0.2824(13) -0.0234(11) 0.4725(8) 0.036(4) Uani 1 1 d . . . . .
C31 C 0.1269(14) 0.1868(13) 0.5442(8) 0.047(4) Uani 1 1 d . . . . .
C32 C -0.1291(15) 0.1760(15) 0.5521(10) 0.084(7) Uani 1 1 d . . . . .
H32A H -0.113843 0.109819 0.539928 0.127 Uiso 1 1 calc R U . . .
H32B H -0.187226 0.206178 0.517181 0.127 Uiso 1 1 calc R U . . .
H32C H -0.174043 0.179061 0.595836 0.127 Uiso 1 1 calc R U . . .
C33 C 0.0045(16) 0.3292(13) 0.5788(9) 0.069(5) Uani 1 1 d . . . . .
H33A H -0.028169 0.333861 0.625205 0.104 Uiso 1 1 calc R U . . .
H33B H -0.056846 0.364748 0.548093 0.104 Uiso 1 1 calc R U . . .
H33C H 0.096805 0.355586 0.577026 0.104 Uiso 1 1 calc R U . . .
C34 C 0.6287(13) 0.1225(12) 0.3389(8) 0.043(4) Uani 1 1 d . . . . .
C35 C 0.7463(16) 0.0644(12) 0.2339(8) 0.060(4) Uani 1 1 d . . . . .
H35A H 0.824028 0.029024 0.253182 0.090 Uiso 1 1 calc R U . . .
H35B H 0.773275 0.095451 0.191880 0.090 Uiso 1 1 calc R U . . .
H35C H 0.670448 0.021006 0.223963 0.090 Uiso 1 1 calc R U . . .
C36 C 0.7595(16) 0.2343(15) 0.2745(9) 0.071(6) Uani 1 1 d . . . . .
H36A H 0.686268 0.277495 0.259780 0.107 Uiso 1 1 calc R U . . .
H36B H 0.829719 0.232555 0.240060 0.107 Uiso 1 1 calc R U . . .
H36C H 0.800080 0.256471 0.317557 0.107 Uiso 1 1 calc R U . . .
Cl1 Cl 0.0303(6) 0.8152(4) 0.2585(3) 0.0880(16) Uani 1 1 d . . . . .
O11 O 0.096(2) 0.8483(15) 0.3189(8) 0.175(9) Uani 1 1 d . . . . .
O12 O 0.077(2) 0.8622(18) 0.2018(8) 0.184(10) Uani 1 1 d . . . . .
O13 O 0.053(2) 0.7199(16) 0.2581(13) 0.193(7) Uani 1 1 d . . . . .
O14 O -0.107(2) 0.8302(16) 0.2627(13) 0.193(7) Uani 1 1 d . . . . .
Cl2 Cl 0.0139(4) 0.6622(4) 0.6483(2) 0.0652(12) Uani 1 1 d . . . . .
O15 O 0.1096(14) 0.6460(12) 0.5983(6) 0.115(5) Uani 1 1 d . . . . .
O16 O -0.0635(19) 0.7474(18) 0.6308(9) 0.166(5) Uani 1 1 d . . . . .
O17 O 0.0658(18) 0.6518(17) 0.7143(9) 0.166(5) Uani 1 1 d . . . . .
O18 O -0.0925(19) 0.6053(18) 0.6426(9) 0.166(5) Uani 1 1 d . . . . .
C37 C 0.421(3) 0.123(2) 0.6828(13) 0.112(10) Uani 1 1 d . . . . .
C38 C 0.448(3) 0.2304(16) 0.6846(13) 0.150(12) Uani 1 1 d . . . . .
H38A H 0.427220 0.255138 0.729564 0.225 Uiso 1 1 calc R U . . .
H38B H 0.389314 0.261693 0.650283 0.225 Uiso 1 1 calc R U . . .
H38C H 0.543792 0.242573 0.675029 0.225 Uiso 1 1 calc R U . . .
N01I N 0.412(2) 0.0469(16) 0.6822(14) 0.135(9) Uani 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 O4 1.743(10) . ?
U1 O3 1.774(10) . ?
U1 O5 2.318(10) . ?
U1 O6 2.324(10) . ?
U1 O1 2.446(11) . ?
U1 O2 2.474(9) . ?
U1 N1 2.609(11) . ?
U1 N2 2.623(11) . ?
U2 O10 1.765(10) . ?
U2 O9 1.782(11) . ?
U2 O6 2.250(11) . ?
U2 O5 2.302(10) . ?
U2 O8 2.398(12) . ?
U2 O7 2.425(10) . ?
U2 N5 2.601(10) . ?
U2 N6 2.625(11) . ?
O1 C13 1.254(17) . ?
O2 C16 1.262(17) . ?
O5 O6 1.493(11) . ?
O7 C31 1.277(17) . ?
O8 C34 1.248(17) . ?
N1 C12 1.332(17) . ?
N1 C1 1.334(17) . ?
N2 C11 1.333(16) . ?
N2 C10 1.359(16) . ?
N3 C13 1.319(18) . ?
N3 C14 1.417(18) . ?
N3 C15 1.461(18) . ?
N4 C16 1.323(16) . ?
N4 C17 1.450(17) . ?
N4 C18 1.484(18) . ?
N5 C19 1.311(15) . ?
N5 C30 1.338(17) . ?
N6 C28 1.330(16) . ?
N6 C29 1.391(17) . ?
N7 C31 1.312(17) . ?
N7 C33 1.476(19) . ?
N7 C32 1.486(19) . ?
N8 C34 1.313(16) . ?
N8 C36 1.46(2) . ?
N8 C35 1.468(18) . ?
C1 C2 1.41(2) . ?
C1 C13 1.484(19) . ?
C2 C3 1.41(2) . ?
C3 C4 1.36(2) . ?
C4 C12 1.431(19) . ?
C4 C5 1.45(2) . ?
C5 C6 1.340(19) . ?
C6 C7 1.44(2) . ?
C7 C8 1.40(2) . ?
C7 C11 1.439(18) . ?
C8 C9 1.356(19) . ?
C9 C10 1.416(19) . ?
C10 C16 1.485(19) . ?
C11 C12 1.42(2) . ?
C19 C20 1.37(2) . ?
C19 C31 1.51(2) . ?
C20 C21 1.35(2) . ?
C21 C22 1.38(2) . ?
C22 C23 1.40(2) . ?
C22 C30 1.408(19) . ?
C23 C24 1.34(2) . ?
C24 C25 1.44(2) . ?
C25 C29 1.415(19) . ?
C25 C26 1.45(2) . ?
C26 C27 1.34(2) . ?
C27 C28 1.39(2) . ?
C28 C34 1.51(2) . ?
C29 C30 1.41(2) . ?
Cl1 O13 1.34(2) . ?
Cl1 O14 1.343(19) . ?
Cl1 O12 1.360(16) . ?
Cl1 O11 1.391(16) . ?
Cl2 O18 1.29(2) . ?
Cl2 O17 1.364(16) . ?
Cl2 O15 1.371(12) . ?
Cl2 O16 1.43(2) . ?
C37 N01I 1.05(3) . ?
C37 C38 1.52(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 O3 175.5(6) . . ?
O4 U1 O5 94.0(6) . . ?
O3 U1 O5 90.5(5) . . ?
O4 U1 O6 94.6(6) . . ?
O3 U1 O6 89.1(5) . . ?
O5 U1 O6 37.5(3) . . ?
O4 U1 O1 85.3(4) . . ?
O3 U1 O1 93.4(4) . . ?
O5 U1 O1 109.1(3) . . ?
O6 U1 O1 71.8(3) . . ?
O4 U1 O2 87.0(4) . . ?
O3 U1 O2 94.5(4) . . ?
O5 U1 O2 68.7(3) . . ?
O6 U1 O2 106.2(3) . . ?
O1 U1 O2 171.9(4) . . ?
O4 U1 N1 92.8(5) . . ?
O3 U1 N1 82.7(4) . . ?
O5 U1 N1 167.6(3) . . ?
O6 U1 N1 131.5(3) . . ?
O1 U1 N1 61.2(3) . . ?
O2 U1 N1 122.0(3) . . ?
O4 U1 N2 94.4(4) . . ?
O3 U1 N2 82.5(4) . . ?
O5 U1 N2 129.4(3) . . ?
O6 U1 N2 164.7(4) . . ?
O1 U1 N2 121.3(4) . . ?
O2 U1 N2 62.0(3) . . ?
N1 U1 N2 60.2(4) . . ?
O10 U2 O9 173.7(6) . . ?
O10 U2 O6 94.4(6) . . ?
O9 U2 O6 91.7(6) . . ?
O10 U2 O5 93.6(5) . . ?
O9 U2 O5 92.1(5) . . ?
O6 U2 O5 38.3(3) . . ?
O10 U2 O8 90.6(4) . . ?
O9 U2 O8 88.9(4) . . ?
O6 U2 O8 108.2(3) . . ?
O5 U2 O8 70.0(3) . . ?
O10 U2 O7 92.1(4) . . ?
O9 U2 O7 88.9(4) . . ?
O6 U2 O7 67.2(3) . . ?
O5 U2 O7 105.4(3) . . ?
O8 U2 O7 174.8(4) . . ?
O10 U2 N5 87.4(4) . . ?
O9 U2 N5 87.7(4) . . ?
O6 U2 N5 128.9(3) . . ?
O5 U2 N5 167.2(3) . . ?
O8 U2 N5 122.8(4) . . ?
O7 U2 N5 61.7(4) . . ?
O10 U2 N6 84.9(4) . . ?
O9 U2 N6 89.3(4) . . ?
O6 U2 N6 168.9(3) . . ?
O5 U2 N6 130.6(3) . . ?
O8 U2 N6 60.7(4) . . ?
O7 U2 N6 124.0(4) . . ?
N5 U2 N6 62.2(4) . . ?
C13 O1 U1 125.3(9) . . ?
C16 O2 U1 123.3(8) . . ?
O6 O5 U2 69.0(5) . . ?
O6 O5 U1 71.4(5) . . ?
U2 O5 U1 137.4(5) . . ?
O5 O6 U2 72.8(5) . . ?
O5 O6 U1 71.0(5) . . ?
U2 O6 U1 140.5(5) . . ?
C31 O7 U2 123.0(10) . . ?
C34 O8 U2 129.8(9) . . ?
C12 N1 C1 118.3(12) . . ?
C12 N1 U1 120.2(9) . . ?
C1 N1 U1 118.9(9) . . ?
C11 N2 C10 121.1(13) . . ?
C11 N2 U1 119.4(9) . . ?
C10 N2 U1 117.8(9) . . ?
C13 N3 C14 124.5(14) . . ?
C13 N3 C15 119.6(13) . . ?
C14 N3 C15 115.9(13) . . ?
C16 N4 C17 126.0(13) . . ?
C16 N4 C18 118.7(11) . . ?
C17 N4 C18 115.3(11) . . ?
C19 N5 C30 117.4(12) . . ?
C19 N5 U2 121.3(10) . . ?
C30 N5 U2 120.5(8) . . ?
C28 N6 C29 119.4(12) . . ?
C28 N6 U2 120.9(9) . . ?
C29 N6 U2 118.9(9) . . ?
C31 N7 C33 119.0(12) . . ?
C31 N7 C32 123.9(14) . . ?
C33 N7 C32 117.1(12) . . ?
C34 N8 C36 117.1(13) . . ?
C34 N8 C35 126.5(14) . . ?
C36 N8 C35 116.0(12) . . ?
N1 C1 C2 121.9(14) . . ?
N1 C1 C13 112.7(12) . . ?
C2 C1 C13 125.1(13) . . ?
C1 C2 C3 118.1(14) . . ?
C4 C3 C2 121.1(15) . . ?
C3 C4 C12 115.9(14) . . ?
C3 C4 C5 126.6(15) . . ?
C12 C4 C5 117.5(13) . . ?
C6 C5 C4 124.1(17) . . ?
C5 C6 C7 119.4(15) . . ?
C8 C7 C6 125.4(14) . . ?
C8 C7 C11 115.7(15) . . ?
C6 C7 C11 118.7(14) . . ?
C9 C8 C7 122.3(15) . . ?
C8 C9 C10 119.1(14) . . ?
N2 C10 C9 119.8(14) . . ?
N2 C10 C16 113.3(12) . . ?
C9 C10 C16 126.5(13) . . ?
N2 C11 C12 117.0(13) . . ?
N2 C11 C7 121.7(14) . . ?
C12 C11 C7 121.2(14) . . ?
N1 C12 C11 116.6(13) . . ?
N1 C12 C4 124.5(13) . . ?
C11 C12 C4 118.9(13) . . ?
O1 C13 N3 123.1(14) . . ?
O1 C13 C1 113.5(13) . . ?
N3 C13 C1 123.4(14) . . ?
O2 C16 N4 122.6(13) . . ?
O2 C16 C10 114.6(11) . . ?
N4 C16 C10 122.7(13) . . ?
N5 C19 C20 122.5(15) . . ?
N5 C19 C31 110.1(12) . . ?
C20 C19 C31 126.8(14) . . ?
C21 C20 C19 119.5(16) . . ?
C20 C21 C22 121.3(15) . . ?
C21 C22 C23 123.5(16) . . ?
C21 C22 C30 114.3(16) . . ?
C23 C22 C30 122.2(16) . . ?
C24 C23 C22 121.1(16) . . ?
C23 C24 C25 120.3(17) . . ?
C29 C25 C24 118.0(16) . . ?
C29 C25 C26 117.1(14) . . ?
C24 C25 C26 124.6(16) . . ?
C27 C26 C25 119.5(15) . . ?
C26 C27 C28 120.8(15) . . ?
N6 C28 C27 122.2(15) . . ?
N6 C28 C34 110.9(12) . . ?
C27 C28 C34 126.6(14) . . ?
N6 C29 C30 117.1(13) . . ?
N6 C29 C25 120.7(14) . . ?
C30 C29 C25 122.0(15) . . ?
N5 C30 C22 124.4(15) . . ?
N5 C30 C29 119.2(13) . . ?
C22 C30 C29 116.3(15) . . ?
O7 C31 N7 119.3(16) . . ?
O7 C31 C19 116.0(13) . . ?
N7 C31 C19 124.6(13) . . ?
O8 C34 N8 119.6(15) . . ?
O8 C34 C28 115.6(12) . . ?
N8 C34 C28 124.6(14) . . ?
O13 Cl1 O14 108.5(14) . . ?
O13 Cl1 O12 114.2(16) . . ?
O14 Cl1 O12 108.6(15) . . ?
O13 Cl1 O11 105.0(14) . . ?
O14 Cl1 O11 108.9(14) . . ?
O12 Cl1 O11 111.5(11) . . ?
O18 Cl2 O17 106.4(12) . . ?
O18 Cl2 O15 112.5(12) . . ?
O17 Cl2 O15 114.1(10) . . ?
O18 Cl2 O16 94.6(12) . . ?
O17 Cl2 O16 118.9(13) . . ?
O15 Cl2 O16 108.7(10) . . ?
N01I C37 C38 174(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
U1 O5 O6 U2 -164.0(6) . . . . ?
U2 O5 O6 U1 164.0(6) . . . . ?
C12 N1 C1 C2 3.3(19) . . . . ?
U1 N1 C1 C2 -158.5(10) . . . . ?
C12 N1 C1 C13 177.2(11) . . . . ?
U1 N1 C1 C13 15.4(15) . . . . ?
N1 C1 C2 C3 -1(2) . . . . ?
C13 C1 C2 C3 -173.7(14) . . . . ?
C1 C2 C3 C4 -4(2) . . . . ?
C2 C3 C4 C12 5(2) . . . . ?
C2 C3 C4 C5 -177.9(13) . . . . ?
C3 C4 C5 C6 -177.0(14) . . . . ?
C12 C4 C5 C6 1(2) . . . . ?
C4 C5 C6 C7 -4(2) . . . . ?
C5 C6 C7 C8 -179.0(13) . . . . ?
C5 C6 C7 C11 6.0(19) . . . . ?
C6 C7 C8 C9 -180.0(13) . . . . ?
C11 C7 C8 C9 -4.8(19) . . . . ?
C7 C8 C9 C10 3(2) . . . . ?
C11 N2 C10 C9 -4.6(18) . . . . ?
U1 N2 C10 C9 160.2(10) . . . . ?
C11 N2 C10 C16 -178.4(11) . . . . ?
U1 N2 C10 C16 -13.6(13) . . . . ?
C8 C9 C10 N2 2(2) . . . . ?
C8 C9 C10 C16 174.6(13) . . . . ?
C10 N2 C11 C12 -174.6(11) . . . . ?
U1 N2 C11 C12 20.8(15) . . . . ?
C10 N2 C11 C7 2.7(19) . . . . ?
U1 N2 C11 C7 -161.8(9) . . . . ?
C8 C7 C11 N2 1.9(18) . . . . ?
C6 C7 C11 N2 177.4(11) . . . . ?
C8 C7 C11 C12 179.1(12) . . . . ?
C6 C7 C11 C12 -5.4(19) . . . . ?
C1 N1 C12 C11 178.1(12) . . . . ?
U1 N1 C12 C11 -20.2(15) . . . . ?
C1 N1 C12 C4 -2.2(19) . . . . ?
U1 N1 C12 C4 159.4(10) . . . . ?
N2 C11 C12 N1 -0.6(18) . . . . ?
C7 C11 C12 N1 -177.9(11) . . . . ?
N2 C11 C12 C4 179.7(11) . . . . ?
C7 C11 C12 C4 2.4(19) . . . . ?
C3 C4 C12 N1 -1.7(19) . . . . ?
C5 C4 C12 N1 -179.6(12) . . . . ?
C3 C4 C12 C11 177.9(13) . . . . ?
C5 C4 C12 C11 0.1(18) . . . . ?
U1 O1 C13 N3 -147.3(11) . . . . ?
U1 O1 C13 C1 34.0(18) . . . . ?
C14 N3 C13 O1 167.0(15) . . . . ?
C15 N3 C13 O1 -12(2) . . . . ?
C14 N3 C13 C1 -14(2) . . . . ?
C15 N3 C13 C1 166.8(13) . . . . ?
N1 C1 C13 O1 -30.3(17) . . . . ?
C2 C1 C13 O1 143.3(15) . . . . ?
N1 C1 C13 N3 151.0(13) . . . . ?
C2 C1 C13 N3 -35(2) . . . . ?
U1 O2 C16 N4 146.6(11) . . . . ?
U1 O2 C16 C10 -35.8(16) . . . . ?
C17 N4 C16 O2 -172.4(14) . . . . ?
C18 N4 C16 O2 7(2) . . . . ?
C17 N4 C16 C10 10(2) . . . . ?
C18 N4 C16 C10 -170.6(12) . . . . ?
N2 C10 C16 O2 30.9(16) . . . . ?
C9 C10 C16 O2 -142.4(14) . . . . ?
N2 C10 C16 N4 -151.4(13) . . . . ?
C9 C10 C16 N4 35(2) . . . . ?
C30 N5 C19 C20 8.7(18) . . . . ?
U2 N5 C19 C20 -161.3(11) . . . . ?
C30 N5 C19 C31 -179.3(11) . . . . ?
U2 N5 C19 C31 10.7(13) . . . . ?
N5 C19 C20 C21 -5(2) . . . . ?
C31 C19 C20 C21 -175.7(13) . . . . ?
C19 C20 C21 C22 -1(2) . . . . ?
C20 C21 C22 C23 -178.2(14) . . . . ?
C20 C21 C22 C30 3(2) . . . . ?
C21 C22 C23 C24 -177.0(16) . . . . ?
C30 C22 C23 C24 2(2) . . . . ?
C22 C23 C24 C25 -2(2) . . . . ?
C23 C24 C25 C29 2(2) . . . . ?
C23 C24 C25 C26 175.9(14) . . . . ?
C29 C25 C26 C27 -1.2(19) . . . . ?
C24 C25 C26 C27 -175.1(15) . . . . ?
C25 C26 C27 C28 -1(2) . . . . ?
C29 N6 C28 C27 -5.8(18) . . . . ?
U2 N6 C28 C27 164.0(10) . . . . ?
C29 N6 C28 C34 -179.5(11) . . . . ?
U2 N6 C28 C34 -9.8(13) . . . . ?
C26 C27 C28 N6 5(2) . . . . ?
C26 C27 C28 C34 177.4(14) . . . . ?
C28 N6 C29 C30 179.8(11) . . . . ?
U2 N6 C29 C30 9.8(14) . . . . ?
C28 N6 C29 C25 3.4(17) . . . . ?
U2 N6 C29 C25 -166.6(9) . . . . ?
C24 C25 C29 N6 174.4(12) . . . . ?
C26 C25 C29 N6 0.0(18) . . . . ?
C24 C25 C29 C30 -2(2) . . . . ?
C26 C25 C29 C30 -176.2(12) . . . . ?
C19 N5 C30 C22 -6.7(18) . . . . ?
U2 N5 C30 C22 163.4(9) . . . . ?
C19 N5 C30 C29 177.0(12) . . . . ?
U2 N5 C30 C29 -12.9(15) . . . . ?
C21 C22 C30 N5 1.0(19) . . . . ?
C23 C22 C30 N5 -177.9(12) . . . . ?
C21 C22 C30 C29 177.4(12) . . . . ?
C23 C22 C30 C29 -1.5(19) . . . . ?
N6 C29 C30 N5 1.8(18) . . . . ?
C25 C29 C30 N5 178.1(12) . . . . ?
N6 C29 C30 C22 -174.8(11) . . . . ?
C25 C29 C30 C22 1.6(18) . . . . ?
U2 O7 C31 N7 -144.4(12) . . . . ?
U2 O7 C31 C19 34.0(18) . . . . ?
C33 N7 C31 O7 -10(2) . . . . ?
C32 N7 C31 O7 169.8(16) . . . . ?
C33 N7 C31 C19 171.7(13) . . . . ?
C32 N7 C31 C19 -8(3) . . . . ?
N5 C19 C31 O7 -27.5(17) . . . . ?
C20 C19 C31 O7 144.1(15) . . . . ?
N5 C19 C31 N7 150.8(15) . . . . ?
C20 C19 C31 N7 -38(2) . . . . ?
U2 O8 C34 N8 159.1(10) . . . . ?
U2 O8 C34 C28 -17(2) . . . . ?
C36 N8 C34 O8 6(2) . . . . ?
C35 N8 C34 O8 178.7(14) . . . . ?
C36 N8 C34 C28 -178.5(12) . . . . ?
C35 N8 C34 C28 -6(2) . . . . ?
N6 C28 C34 O8 15.9(17) . . . . ?
C27 C28 C34 O8 -157.5(14) . . . . ?
N6 C28 C34 N8 -159.7(13) . . . . ?
C27 C28 C34 N8 27(2) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C38 H38B O7 0.96 2.57 3.41(2) 145.8 . yes
C27 H27 O14 0.93 2.60 3.44(2) 150.6 1_645 yes
C18 H18B O9 0.96 2.55 3.458(18) 158.3 1_655 yes

_refine_diff_density_max         1.441
_refine_diff_density_min         -0.806
_refine_diff_density_rms         0.134




_vrf_PLAT342_TMPhenDA_U_O2_com4  
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.03071 Ang.  
RESPONSE: Low Bond Precision on  C-C Bonds is caused by the weak diffraction of
small crystal.
;
