# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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_16034_sq
_database_code_depnum_ccdc_archive 'CCDC 1533054'
_audit_update_record             
;
2017-02-16 deposited with the CCDC.
2017-03-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
#_shelx_SHELXL_version_number      '2014/7' 
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C34 H38 Cl2 N4 O4 U'
_chemical_formula_sum            'C34 H38 Cl2 N4 O4 U'
_chemical_formula_weight         875.61

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 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'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   19.233(6)
_cell_length_b                   19.034(6)
_cell_length_c                   12.202(4)
_cell_angle_alpha                90
_cell_angle_beta                 122.796(3)
_cell_angle_gamma                90
_cell_volume                     3755(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    4649
_cell_measurement_theta_min      2.53
_cell_measurement_theta_max      23.40

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.549
_exptl_crystal_F_000             1712
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.090
_exptl_absorpt_coefficient_mu    4.504
_shelx_estimated_absorpt_T_min   0.411
_shelx_estimated_absorpt_T_max   0.687
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.411
_exptl_absorpt_correction_T_max  0.687
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2015c)'
#_exptl_absorpt_special_details    ? 
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            24171
_diffrn_reflns_av_unetI/netI     0.0519
_diffrn_reflns_av_R_equivalents  0.0666
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.653
_diffrn_reflns_theta_max         27.517
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             4301
_reflns_number_gt                3346
_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. 
;

_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015a)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015b)'
_computing_molecular_graphics    'Mercury (CCDC, 2016)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2015b)'
_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)+(0.0900P)²+19.0000P] 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         4301
_refine_ls_number_parameters     204
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0713
_refine_ls_R_factor_gt           0.0424
_refine_ls_wR_factor_ref         0.1424
_refine_ls_wR_factor_gt          0.1118
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_restrained_S_all      1.020
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.5000 0.34804(2) 0.7500 0.03037(14) Uani 1 2 d S T P . .
Cl1 Cl 0.63312(10) 0.38687(8) 0.98445(15) 0.0320(3) Uani 1 1 d . . . . .
O1 O 0.4156(3) 0.3207(2) 0.8096(4) 0.0289(9) Uani 1 1 d . . . . .
O2 O 0.3212(3) 0.2245(2) 0.8244(5) 0.0333(10) Uani 1 1 d . . . . .
N1 N 0.4535(3) 0.4635(3) 0.8088(5) 0.0277(11) Uani 1 1 d . . . . .
C1 C 0.5043(5) 0.6622(4) 0.8162(8) 0.0380(16) Uani 1 1 d . . . . .
H1A H 0.5635 0.6620 0.8873 0.046 Uiso 1 1 calc R U . . .
H1B H 0.4786 0.7052 0.8250 0.046 Uiso 1 1 calc R U . . .
C2 C 0.4622(5) 0.5979(3) 0.8268(7) 0.0350(15) Uani 1 1 d . . . . .
H2A H 0.4025 0.5999 0.7582 0.042 Uiso 1 1 calc R U . . .
H2B H 0.4679 0.5983 0.9124 0.042 Uiso 1 1 calc R U . . .
C3 C 0.4987(4) 0.5289(3) 0.8126(7) 0.0330(14) Uani 1 1 d . . . . .
H3 H 0.5569 0.5251 0.8893 0.040 Uiso 1 1 calc R U . . .
C4 C 0.3993(4) 0.4704(3) 0.8385(6) 0.0288(13) Uani 1 1 d . . . . .
H4 H 0.3908 0.5167 0.8580 0.035 Uiso 1 1 calc R U . . .
C5 C 0.3488(4) 0.4147(3) 0.8455(6) 0.0278(13) Uani 1 1 d . . . . .
C6 C 0.3578(4) 0.3441(3) 0.8299(6) 0.0246(12) Uani 1 1 d . . . . .
C7 C 0.3064(4) 0.2934(3) 0.8375(6) 0.0314(14) Uani 1 1 d . . . . .
C8 C 0.2449(4) 0.3153(4) 0.8586(7) 0.0329(14) Uani 1 1 d . . . . .
H8 H 0.2090 0.2820 0.8612 0.039 Uiso 1 1 calc R U . . .
C9 C 0.2374(4) 0.3874(4) 0.8757(7) 0.0361(15) Uani 1 1 d . . . . .
H9 H 0.1962 0.4026 0.8909 0.043 Uiso 1 1 calc R U . . .
C10 C 0.2885(4) 0.4365(4) 0.8708(7) 0.0328(14) Uani 1 1 d . . . . .
H10 H 0.2832 0.4848 0.8845 0.039 Uiso 1 1 calc R U . . .
C11 C 0.2692(5) 0.1722(4) 0.8267(7) 0.0373(16) Uani 1 1 d . . . . .
H11A H 0.2126 0.1761 0.7481 0.045 Uiso 1 1 calc R U . . .
H11B H 0.2663 0.1781 0.9048 0.045 Uiso 1 1 calc R U . . .
C12 C 0.3065(5) 0.1003(4) 0.8298(8) 0.0441(18) Uani 1 1 d . . . . .
H12A H 0.3067 0.0942 0.7502 0.066 Uiso 1 1 d R U . . .
H12B H 0.2732 0.0631 0.8352 0.066 Uiso 1 1 d R U . . .
H12C H 0.3633 0.0978 0.9060 0.066 Uiso 1 1 d R U . . .
N2 N 0.4359(3) 0.2310(3) 0.6104(5) 0.0316(12) Uani 1 1 d . . . . .
C13 C 0.3611(4) 0.2091(4) 0.5788(7) 0.0348(15) Uani 1 1 d . . . . .
H13 H 0.3318 0.2362 0.6063 0.042 Uiso 1 1 calc R U . . .
C14 C 0.3247(5) 0.1482(4) 0.5073(7) 0.0386(16) Uani 1 1 d . . . . .
H14 H 0.2711 0.1347 0.4853 0.046 Uiso 1 1 calc R U . . .
C15 C 0.3666(6) 0.1081(5) 0.4692(9) 0.053(2) Uani 1 1 d . . . . .
H15 H 0.3426 0.0663 0.4203 0.063 Uiso 1 1 calc R U . . .
C16 C 0.4448(6) 0.1292(5) 0.5029(10) 0.057(2) Uani 1 1 d . . . . .
H16 H 0.4757 0.1017 0.4788 0.069 Uiso 1 1 calc R U . . .
C17 C 0.4774(5) 0.1914(4) 0.5727(8) 0.0426(18) Uani 1 1 d . . . . .
H17 H 0.5305 0.2064 0.5945 0.051 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 O1 2.170(4) . ?
U1 O1 2.170(4) 2_656 ?
U1 N1 2.614(5) 2_656 ?
U1 N1 2.614(5) . ?
U1 N2 2.666(6) . ?
U1 N2 2.666(6) 2_656 ?
U1 Cl1 2.7112(17) 2_656 ?
U1 Cl1 2.7112(17) . ?
O1 C6 1.341(7) . ?
O2 C7 1.369(8) . ?
O2 C11 1.421(8) . ?
N1 C4 1.283(8) . ?
N1 C3 1.505(8) . ?
C1 C2 1.511(9) . ?
C1 C1 1.533(15) 2_656 ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.542(9) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C3 1.555(13) 2_656 ?
C3 H3 1.0000 . ?
C4 C5 1.472(9) . ?
C4 H4 0.9500 . ?
C5 C6 1.381(8) . ?
C5 C10 1.414(9) . ?
C6 C7 1.420(9) . ?
C7 C8 1.403(10) . ?
C8 C9 1.409(10) . ?
C8 H8 0.9500 . ?
C9 C10 1.380(9) . ?
C9 H9 0.9500 . ?
C10 H10 0.9500 . ?
C11 C12 1.535(11) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
N2 C13 1.338(9) . ?
N2 C17 1.346(9) . ?
C13 C14 1.391(10) . ?
C13 H13 0.9500 . ?
C14 C15 1.362(12) . ?
C14 H14 0.9500 . ?
C15 C16 1.388(12) . ?
C15 H15 0.9500 . ?
C16 C17 1.394(11) . ?
C16 H16 0.9500 . ?
C17 H17 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 U1 O1 152.2(2) . 2_656 ?
O1 U1 N1 136.26(16) . 2_656 ?
O1 U1 N1 71.41(16) 2_656 2_656 ?
O1 U1 N1 71.41(16) . . ?
O1 U1 N1 136.26(17) 2_656 . ?
N1 U1 N1 65.7(2) 2_656 . ?
O1 U1 N2 80.95(17) . . ?
O1 U1 N2 75.87(17) 2_656 . ?
N1 U1 N2 129.42(17) 2_656 . ?
N1 U1 N2 140.27(17) . . ?
O1 U1 N2 75.87(17) . 2_656 ?
O1 U1 N2 80.95(17) 2_656 2_656 ?
N1 U1 N2 140.27(17) 2_656 2_656 ?
N1 U1 N2 129.42(17) . 2_656 ?
N2 U1 N2 66.7(2) . 2_656 ?
O1 U1 Cl1 88.22(13) . 2_656 ?
O1 U1 Cl1 99.33(13) 2_656 2_656 ?
N1 U1 Cl1 75.47(13) 2_656 2_656 ?
N1 U1 Cl1 78.04(13) . 2_656 ?
N2 U1 Cl1 73.02(12) . 2_656 ?
N2 U1 Cl1 138.37(12) 2_656 2_656 ?
O1 U1 Cl1 99.33(13) . . ?
O1 U1 Cl1 88.22(13) 2_656 . ?
N1 U1 Cl1 78.04(13) 2_656 . ?
N1 U1 Cl1 75.47(13) . . ?
N2 U1 Cl1 138.37(12) . . ?
N2 U1 Cl1 73.02(12) 2_656 . ?
Cl1 U1 Cl1 148.36(7) 2_656 . ?
C6 O1 U1 145.9(4) . . ?
C7 O2 C11 118.5(5) . . ?
C4 N1 C3 116.7(5) . . ?
C4 N1 U1 128.0(4) . . ?
C3 N1 U1 115.3(4) . . ?
C2 C1 C1 109.5(6) . 2_656 ?
C2 C1 H1A 109.8 . . ?
C1 C1 H1A 109.8 2_656 . ?
C2 C1 H1B 109.8 . . ?
C1 C1 H1B 109.8 2_656 . ?
H1A C1 H1B 108.2 . . ?
C1 C2 C3 112.5(6) . . ?
C1 C2 H2A 109.1 . . ?
C3 C2 H2A 109.1 . . ?
C1 C2 H2B 109.1 . . ?
C3 C2 H2B 109.1 . . ?
H2A C2 H2B 107.8 . . ?
N1 C3 C2 114.7(5) . . ?
N1 C3 C3 107.2(4) . 2_656 ?
C2 C3 C3 111.7(4) . 2_656 ?
N1 C3 H3 107.7 . . ?
C2 C3 H3 107.7 . . ?
C3 C3 H3 107.7 2_656 . ?
N1 C4 C5 127.3(6) . . ?
N1 C4 H4 116.4 . . ?
C5 C4 H4 116.4 . . ?
C6 C5 C10 119.7(6) . . ?
C6 C5 C4 123.8(6) . . ?
C10 C5 C4 116.6(6) . . ?
O1 C6 C5 121.9(6) . . ?
O1 C6 C7 117.5(6) . . ?
C5 C6 C7 120.5(6) . . ?
O2 C7 C8 123.7(6) . . ?
O2 C7 C6 116.6(6) . . ?
C8 C7 C6 119.7(6) . . ?
C7 C8 C9 118.8(6) . . ?
C7 C8 H8 120.6 . . ?
C9 C8 H8 120.6 . . ?
C10 C9 C8 121.3(6) . . ?
C10 C9 H9 119.3 . . ?
C8 C9 H9 119.3 . . ?
C9 C10 C5 119.9(6) . . ?
C9 C10 H10 120.0 . . ?
C5 C10 H10 120.0 . . ?
O2 C11 C12 107.5(6) . . ?
O2 C11 H11A 110.2 . . ?
C12 C11 H11A 110.2 . . ?
O2 C11 H11B 110.2 . . ?
C12 C11 H11B 110.2 . . ?
H11A C11 H11B 108.5 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C13 N2 C17 118.0(6) . . ?
C13 N2 U1 119.8(4) . . ?
C17 N2 U1 122.1(5) . . ?
N2 C13 C14 122.6(7) . . ?
N2 C13 H13 118.7 . . ?
C14 C13 H13 118.7 . . ?
C15 C14 C13 119.4(7) . . ?
C15 C14 H14 120.3 . . ?
C13 C14 H14 120.3 . . ?
C14 C15 C16 118.9(8) . . ?
C14 C15 H15 120.6 . . ?
C16 C15 H15 120.6 . . ?
C15 C16 C17 118.9(8) . . ?
C15 C16 H16 120.5 . . ?
C17 C16 H16 120.5 . . ?
N2 C17 C16 122.1(7) . . ?
N2 C17 H17 118.9 . . ?
C16 C17 H17 118.9 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C1 C2 C3 58.8(10) 2_656 . . . ?
C4 N1 C3 C2 -10.8(8) . . . . ?
U1 N1 C3 C2 171.2(4) . . . . ?
C4 N1 C3 C3 -135.5(6) . . . 2_656 ?
U1 N1 C3 C3 46.6(7) . . . 2_656 ?
C1 C2 C3 N1 -174.2(6) . . . . ?
C1 C2 C3 C3 -51.9(9) . . . 2_656 ?
C3 N1 C4 C5 -178.3(6) . . . . ?
U1 N1 C4 C5 -0.6(10) . . . . ?
N1 C4 C5 C6 5.1(11) . . . . ?
N1 C4 C5 C10 -175.3(7) . . . . ?
U1 O1 C6 C5 -18.4(11) . . . . ?
U1 O1 C6 C7 162.9(5) . . . . ?
C10 C5 C6 O1 -178.0(6) . . . . ?
C4 C5 C6 O1 1.6(10) . . . . ?
C10 C5 C6 C7 0.7(10) . . . . ?
C4 C5 C6 C7 -179.7(6) . . . . ?
C11 O2 C7 C8 2.8(9) . . . . ?
C11 O2 C7 C6 -177.7(6) . . . . ?
O1 C6 C7 O2 0.5(9) . . . . ?
C5 C6 C7 O2 -178.2(6) . . . . ?
O1 C6 C7 C8 -180.0(6) . . . . ?
C5 C6 C7 C8 1.3(10) . . . . ?
O2 C7 C8 C9 177.5(6) . . . . ?
C6 C7 C8 C9 -1.9(10) . . . . ?
C7 C8 C9 C10 0.6(10) . . . . ?
C8 C9 C10 C5 1.4(11) . . . . ?
C6 C5 C10 C9 -2.0(10) . . . . ?
C4 C5 C10 C9 178.4(6) . . . . ?
C7 O2 C11 C12 -172.1(5) . . . . ?
C17 N2 C13 C14 -1.1(10) . . . . ?
U1 N2 C13 C14 -179.3(5) . . . . ?
N2 C13 C14 C15 1.1(11) . . . . ?
C13 C14 C15 C16 0.0(13) . . . . ?
C14 C15 C16 C17 -1.1(15) . . . . ?
C13 N2 C17 C16 0.0(12) . . . . ?
U1 N2 C17 C16 178.2(7) . . . . ?
C15 C16 C17 N2 1.1(15) . . . . ?

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
C2 H2B Cl1 0.99 2.84 3.650(7) 139.1 5_667
C3 H3 Cl1 1.00 2.93 3.539(7) 120.2 .
C4 H4 Cl1 0.95 2.87 3.728(7) 150.9 5_667
C11 H11A Cl1 0.99 2.97 3.703(8) 132.0 8_455
C13 H13 O1 0.95 2.65 3.215(8) 118.9 .
C14 H14 Cl1 0.95 2.68 3.603(8) 164.6 8_455
C17 H17 O1 0.95 2.42 3.024(9) 121.2 2_656
C17 H17 O2 0.95 2.49 3.423(9) 169.2 2_656

_refine_diff_density_max         2.368
_refine_diff_density_min         -2.619
_refine_diff_density_rms         0.168



####################################################################### 
# 
# 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_16101
_database_code_depnum_ccdc_archive 'CCDC 1533055'
_audit_update_record             
;
2017-02-16 deposited with the CCDC.
2017-03-23 downloaded from the CCDC.
;

_vrf_THETM01_Alert_3_A           
; 
 Problem:   The value of sine(theta_max)/wavelength > 0.550  (0.5376)
 Response:  The intensity data were truncated to 0.93 \A because data in 
            higher resolution shells all had <I/sigma> < 2. 
;
_vrf_RINTA01_Alert_3_B           
; 
 Problem:   The value of Rint is greater than 0.18  (0.230)
 Response:  The sample was an ugly twin (> 5-components).  
;
_vrf_PLAT020_Alert_3_B           
; 
 Problem:   The value of Rint is greater than 0.12   (0.230)
 Response:  See response for the alert above.
;
_vrf_PLAT342_Alert_3_B           
; 
 Problem:   Low bond precision on C-C bonds  (0.04206 \A)
 Response:  With twinning and poor diffraction, we were lucky to get this
            precision.  
;

_audit_creation_method           SHELXL-2014/7
#_shelx_SHELXL_version_number      '2014/7' 
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C34 H38 Cl2 N4 O4 Th, C5 H5 N'
_chemical_formula_sum            'C39 H43 Cl2 N5 O4 Th'
_chemical_formula_weight         948.72

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'
Th Th -7.2400 8.8979 '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                   16.806(13)
_cell_length_b                   14.283(11)
_cell_length_c                   15.268(12)
_cell_angle_alpha                90
_cell_angle_beta                 92.515(14)
_cell_angle_gamma                90
_cell_volume                     3661(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    2106
_cell_measurement_theta_min      2.27
_cell_measurement_theta_max      26.09

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.721
_exptl_crystal_F_000             1872
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    4.267
_shelx_estimated_absorpt_T_min   0.675
_shelx_estimated_absorpt_T_max   0.726
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.675
_exptl_absorpt_correction_T_max  0.726
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2015c)'
#_exptl_absorpt_special_details    ? 
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            85853
_diffrn_reflns_av_unetI/netI     0.1787
_diffrn_reflns_av_R_equivalents  0.2301
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.268
_diffrn_reflns_theta_max         22.464
_diffrn_reflns_theta_full        22.464
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measured_fraction_theta_full 0.963
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_Laue_measured_fraction_full 0.963
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_point_group_measured_fraction_full 0.963
_reflns_number_total             4595
_reflns_number_gt                2708
_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       'APEX2 (Bruker, 2007)'
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015a)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Mercury (CCDC, 2016)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2015b)'
_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)+(0.0200P)²+240.0000P] 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         4595
_refine_ls_number_parameters     462
_refine_ls_number_restraints     493
_refine_ls_R_factor_all          0.1747
_refine_ls_R_factor_gt           0.1052
_refine_ls_wR_factor_ref         0.2203
_refine_ls_wR_factor_gt          0.1978
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_restrained_S_all      1.016
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Th1 Th 0.27157(6) 0.52696(7) 0.62358(7) 0.0251(3) Uani 1 1 d . U . . .
Cl1 Cl 0.3384(4) 0.3634(5) 0.5640(5) 0.0315(17) Uani 1 1 d . U . . .
Cl2 Cl 0.2310(4) 0.7113(5) 0.5977(5) 0.0366(18) Uani 1 1 d . U . . .
O1 O 0.3706(10) 0.5708(12) 0.7143(11) 0.029(4) Uani 1 1 d . U . . .
O2 O 0.1545(10) 0.4621(12) 0.5907(11) 0.031(3) Uani 1 1 d . U . . .
O3 O 0.4250(11) 0.6100(14) 0.8753(11) 0.037(5) Uani 1 1 d . U . . .
O4 O 0.0265(11) 0.3772(12) 0.6464(12) 0.036(4) Uani 1 1 d . U . . .
N1 N 0.3892(13) 0.5826(15) 0.5295(14) 0.028(4) Uani 1 1 d . U . . .
N2 N 0.2404(12) 0.5373(16) 0.4557(13) 0.030(4) Uani 1 1 d . U . . .
N3 N 0.2648(13) 0.3996(14) 0.7526(14) 0.027(4) Uani 1 1 d . U . . .
N4 N 0.1891(13) 0.5767(15) 0.7580(14) 0.029(4) Uani 1 1 d . U . . .
C1 C 0.3991(17) 0.594(2) 1.0229(18) 0.047(8) Uani 1 1 d . U . . .
H1A H 0.3590 0.6440 1.0247 0.070 Uiso 1 1 calc R U . . .
H1B H 0.4239 0.5853 1.0816 0.070 Uiso 1 1 calc R U . . .
H1C H 0.3735 0.5359 1.0031 0.070 Uiso 1 1 calc R U . . .
C2 C 0.4598(16) 0.621(2) 0.9622(16) 0.036(7) Uani 1 1 d . U . . .
H2A H 0.4766 0.6863 0.9724 0.043 Uiso 1 1 calc R U . . .
H2B H 0.5071 0.5797 0.9704 0.043 Uiso 1 1 calc R U . . .
C3 C 0.4750(16) 0.6329(19) 0.8056(17) 0.028(5) Uani 1 1 d . U . . .
C4 C 0.4408(15) 0.6107(17) 0.7214(16) 0.022(5) Uani 1 1 d . U . . .
C5 C 0.5501(15) 0.6731(19) 0.8192(18) 0.031(6) Uani 1 1 d . U . . .
H5 H 0.5718 0.6844 0.8768 0.037 Uiso 1 1 calc R U . . .
C6 C 0.5939(17) 0.697(2) 0.7429(18) 0.036(6) Uani 1 1 d . U . . .
H6 H 0.6439 0.7282 0.7479 0.043 Uiso 1 1 calc R U . . .
C7 C 0.5597(16) 0.6724(17) 0.6626(18) 0.027(5) Uani 1 1 d . U . . .
H7 H 0.5890 0.6851 0.6121 0.032 Uiso 1 1 calc R U . . .
C8 C 0.4865(16) 0.6309(19) 0.6499(17) 0.030(6) Uani 1 1 d . U . . .
C9 C 0.4572(15) 0.6103(16) 0.5607(16) 0.020(5) Uani 1 1 d . U . . .
H9 H 0.4957 0.6191 0.5177 0.024 Uiso 1 1 calc R U . . .
C10 C 0.3813(15) 0.5651(19) 0.4379(16) 0.028(4) Uani 1 1 d . U . . .
H10 H 0.3845 0.4958 0.4294 0.034 Uiso 1 1 calc R U . . .
C11 C 0.4441(17) 0.610(2) 0.3800(18) 0.040(6) Uani 1 1 d . U . . .
H11A H 0.4500 0.6769 0.3970 0.048 Uiso 1 1 calc R U . . .
H11B H 0.4960 0.5793 0.3931 0.048 Uiso 1 1 calc R U . . .
C12 C 0.4265(17) 0.606(2) 0.2843(18) 0.040(6) Uani 1 1 d . U . . .
H12A H 0.4686 0.6393 0.2537 0.048 Uiso 1 1 calc R U . . .
H12B H 0.4273 0.5394 0.2653 0.048 Uiso 1 1 calc R U . . .
C13 C 0.3513(17) 0.645(2) 0.260(2) 0.048(7) Uani 1 1 d . U . . .
H13A H 0.3433 0.6448 0.1950 0.058 Uiso 1 1 calc R U . . .
H13B H 0.3493 0.7113 0.2797 0.058 Uiso 1 1 calc R U . . .
C14 C 0.2866(17) 0.590(2) 0.3004(18) 0.045(6) Uani 1 1 d . U . . .
H14A H 0.2884 0.5239 0.2804 0.054 Uiso 1 1 calc R U . . .
H14B H 0.2338 0.6161 0.2828 0.054 Uiso 1 1 calc R U . . .
C15 C 0.3009(16) 0.5948(19) 0.4077(17) 0.030(4) Uani 1 1 d . U . . .
H15 H 0.2943 0.6616 0.4256 0.036 Uiso 1 1 calc R U . . .
C16 C 0.1813(15) 0.4992(15) 0.4129(18) 0.027(5) Uani 1 1 d . U . . .
H16 H 0.1807 0.5081 0.3512 0.032 Uiso 1 1 calc R U . . .
C17 C 0.1174(16) 0.4465(17) 0.4429(18) 0.030(5) Uani 1 1 d . U . . .
C18 C 0.1008(16) 0.4328(17) 0.5312(18) 0.028(5) Uani 1 1 d . U . . .
C19 C 0.0579(15) 0.4141(18) 0.3776(18) 0.028(5) Uani 1 1 d . U . . .
H19 H 0.0628 0.4269 0.3170 0.033 Uiso 1 1 calc R U . . .
C20 C -0.0046(16) 0.3652(19) 0.4065(19) 0.032(5) Uani 1 1 d . U . . .
H20 H -0.0417 0.3398 0.3641 0.039 Uiso 1 1 calc R U . . .
C21 C -0.0176(15) 0.3502(19) 0.4933(18) 0.030(6) Uani 1 1 d . U . . .
H21 H -0.0626 0.3148 0.5091 0.036 Uiso 1 1 calc R U . . .
C22 C 0.0329(16) 0.3851(17) 0.5573(18) 0.027(5) Uani 1 1 d . U . . .
C23 C -0.0389(17) 0.3257(19) 0.674(2) 0.040(6) Uani 1 1 d . U . . .
H23A H -0.0321 0.2584 0.6606 0.048 Uiso 1 1 calc R U . . .
H23B H -0.0887 0.3480 0.6437 0.048 Uiso 1 1 calc R U . . .
C24 C -0.0424(18) 0.340(2) 0.769(2) 0.050(8) Uani 1 1 d . U . . .
H24A H 0.0089 0.3229 0.7973 0.076 Uiso 1 1 calc R U . . .
H24B H -0.0844 0.3001 0.7916 0.076 Uiso 1 1 calc R U . . .
H24C H -0.0542 0.4056 0.7807 0.076 Uiso 1 1 calc R U . . .
C25 C 0.3085(18) 0.409(2) 0.8308(19) 0.042(7) Uani 1 1 d . U . . .
H25 H 0.3430 0.4613 0.8399 0.050 Uiso 1 1 calc R U . . .
C26 C 0.3018(18) 0.342(2) 0.896(2) 0.044(8) Uani 1 1 d . U . . .
H26 H 0.3363 0.3459 0.9471 0.053 Uiso 1 1 calc R U . . .
C27 C 0.2474(19) 0.272(2) 0.889(2) 0.055(10) Uani 1 1 d . U . . .
H27 H 0.2410 0.2293 0.9359 0.066 Uiso 1 1 calc R U . . .
C28 C 0.2012(19) 0.265(2) 0.811(2) 0.052(9) Uani 1 1 d . U . . .
H28 H 0.1626 0.2172 0.8035 0.062 Uiso 1 1 calc R U . . .
C29 C 0.2130(16) 0.3314(19) 0.7451(19) 0.035(7) Uani 1 1 d . U . . .
H29 H 0.1817 0.3262 0.6920 0.043 Uiso 1 1 calc R U . . .
C30 C 0.2222(18) 0.6335(18) 0.8214(18) 0.033(5) Uani 1 1 d . U . . .
H30 H 0.2713 0.6629 0.8096 0.040 Uiso 1 1 calc R U . . .
C31 C 0.1909(17) 0.6512(18) 0.8994(19) 0.034(6) Uani 1 1 d . U . . .
H31 H 0.2173 0.6934 0.9391 0.041 Uiso 1 1 calc R U . . .
C32 C 0.1206(19) 0.609(2) 0.922(2) 0.046(7) Uani 1 1 d . U . . .
H32 H 0.0975 0.6191 0.9772 0.055 Uiso 1 1 calc R U . . .
C33 C 0.0874(17) 0.5509(19) 0.8610(19) 0.039(6) Uani 1 1 d . U . . .
H33 H 0.0406 0.5167 0.8729 0.047 Uiso 1 1 calc R U . . .
C34 C 0.1211(16) 0.542(2) 0.7816(18) 0.037(6) Uani 1 1 d . U . . .
H34 H 0.0920 0.5059 0.7387 0.044 Uiso 1 1 calc R U . . .
N1S N 0.099(2) 0.481(3) 0.0842(18) 0.122(12) Uani 1 1 d D U . . .
C1S C 0.175(2) 0.496(3) 0.1154(17) 0.114(11) Uani 1 1 d D U . . .
H1S H 0.1831 0.5582 0.1357 0.137 Uiso 1 1 calc R U . . .
C2S C 0.240(2) 0.443(3) 0.124(2) 0.138(19) Uani 1 1 d D U . . .
H2S H 0.2899 0.4646 0.1478 0.166 Uiso 1 1 calc R U . . .
C3S C 0.226(2) 0.349(3) 0.0929(18) 0.092(10) Uani 1 1 d D U . . .
H3S H 0.2682 0.3046 0.0958 0.111 Uiso 1 1 calc R U . . .
C4S C 0.149(3) 0.320(3) 0.057(2) 0.117(11) Uani 1 1 d D U . . .
H4S H 0.1370 0.2586 0.0364 0.141 Uiso 1 1 calc R U . . .
C5S C 0.095(2) 0.389(3) 0.058(2) 0.132(18) Uani 1 1 d D U . . .
H5S H 0.0440 0.3714 0.0346 0.158 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Th1 O1 2.208(16) . ?
Th1 O2 2.212(16) . ?
Th1 N2 2.60(2) . ?
Th1 N1 2.62(2) . ?
Th1 N4 2.62(2) . ?
Th1 N3 2.69(2) . ?
Th1 Cl2 2.744(7) . ?
Th1 Cl1 2.764(7) . ?
O1 C4 1.31(3) . ?
O2 C18 1.32(3) . ?
O3 C3 1.42(3) . ?
O3 C2 1.43(3) . ?
O4 C22 1.37(3) . ?
O4 C23 1.40(3) . ?
N1 C9 1.28(3) . ?
N1 C10 1.42(3) . ?
N2 C16 1.29(3) . ?
N2 C15 1.52(3) . ?
N3 C29 1.31(3) . ?
N3 C25 1.38(3) . ?
N4 C34 1.31(3) . ?
N4 C30 1.36(3) . ?
C1 C2 1.46(4) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C5 1.39(4) . ?
C3 C4 1.42(3) . ?
C4 C8 1.39(4) . ?
C5 C6 1.45(4) . ?
C5 H5 0.9500 . ?
C6 C7 1.38(3) . ?
C6 H6 0.9500 . ?
C7 C8 1.37(3) . ?
C7 H7 0.9500 . ?
C8 C9 1.46(3) . ?
C9 H9 0.9500 . ?
C10 C15 1.47(3) . ?
C10 C11 1.55(4) . ?
C10 H10 1.0000 . ?
C11 C12 1.48(4) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C13 1.42(4) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C14 1.50(4) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C15 1.65(4) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 H15 1.0000 . ?
C16 C17 1.40(4) . ?
C16 H16 0.9500 . ?
C17 C18 1.40(4) . ?
C17 C19 1.46(3) . ?
C18 C22 1.40(4) . ?
C19 C20 1.35(4) . ?
C19 H19 0.9500 . ?
C20 C21 1.37(4) . ?
C20 H20 0.9500 . ?
C21 C22 1.36(4) . ?
C21 H21 0.9500 . ?
C23 C24 1.46(4) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 C26 1.39(4) . ?
C25 H25 0.9500 . ?
C26 C27 1.36(4) . ?
C26 H26 0.9500 . ?
C27 C28 1.39(4) . ?
C27 H27 0.9500 . ?
C28 C29 1.40(4) . ?
C28 H28 0.9500 . ?
C29 H29 0.9500 . ?
C30 C31 1.35(4) . ?
C30 H30 0.9500 . ?
C31 C32 1.39(4) . ?
C31 H31 0.9500 . ?
C32 C33 1.35(4) . ?
C32 H32 0.9500 . ?
C33 C34 1.37(4) . ?
C33 H33 0.9500 . ?
C34 H34 0.9500 . ?
N1S C1S 1.36(4) . ?
N1S C5S 1.36(4) . ?
C1S C2S 1.34(4) . ?
C1S H1S 0.9500 . ?
C2S C3S 1.44(4) . ?
C2S H2S 0.9500 . ?
C3S C4S 1.44(4) . ?
C3S H3S 0.9500 . ?
C4S C5S 1.34(4) . ?
C4S H4S 0.9500 . ?
C5S H5S 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Th1 O2 154.1(6) . . ?
O1 Th1 N2 135.8(7) . . ?
O2 Th1 N2 70.2(6) . . ?
O1 Th1 N1 72.0(6) . . ?
O2 Th1 N1 133.5(6) . . ?
N2 Th1 N1 64.3(6) . . ?
O1 Th1 N4 80.9(7) . . ?
O2 Th1 N4 78.3(6) . . ?
N2 Th1 N4 131.8(6) . . ?
N1 Th1 N4 141.7(7) . . ?
O1 Th1 N3 77.7(6) . . ?
O2 Th1 N3 79.5(6) . . ?
N2 Th1 N3 138.5(7) . . ?
N1 Th1 N3 131.7(6) . . ?
N4 Th1 N3 64.5(6) . . ?
O1 Th1 Cl2 89.6(5) . . ?
O2 Th1 Cl2 99.0(5) . . ?
N2 Th1 Cl2 76.4(5) . . ?
N1 Th1 Cl2 79.6(5) . . ?
N4 Th1 Cl2 73.5(5) . . ?
N3 Th1 Cl2 137.5(5) . . ?
O1 Th1 Cl1 98.1(5) . . ?
O2 Th1 Cl1 86.7(5) . . ?
N2 Th1 Cl1 77.9(5) . . ?
N1 Th1 Cl1 75.4(5) . . ?
N4 Th1 Cl1 136.3(5) . . ?
N3 Th1 Cl1 72.5(5) . . ?
Cl2 Th1 Cl1 150.0(2) . . ?
C4 O1 Th1 145.7(16) . . ?
C18 O2 Th1 149.8(18) . . ?
C3 O3 C2 116(2) . . ?
C22 O4 C23 116(2) . . ?
C9 N1 C10 118(2) . . ?
C9 N1 Th1 124.9(17) . . ?
C10 N1 Th1 116.5(16) . . ?
C16 N2 C15 120(2) . . ?
C16 N2 Th1 126.5(18) . . ?
C15 N2 Th1 113.3(14) . . ?
C29 N3 C25 118(2) . . ?
C29 N3 Th1 119.3(17) . . ?
C25 N3 Th1 121.9(17) . . ?
C34 N4 C30 111(3) . . ?
C34 N4 Th1 127.4(18) . . ?
C30 N4 Th1 120.2(19) . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O3 C2 C1 107(2) . . ?
O3 C2 H2A 110.3 . . ?
C1 C2 H2A 110.3 . . ?
O3 C2 H2B 110.3 . . ?
C1 C2 H2B 110.3 . . ?
H2A C2 H2B 108.6 . . ?
C5 C3 C4 124(3) . . ?
C5 C3 O3 123(2) . . ?
C4 C3 O3 113(2) . . ?
O1 C4 C8 123(2) . . ?
O1 C4 C3 120(2) . . ?
C8 C4 C3 117(3) . . ?
C3 C5 C6 118(2) . . ?
C3 C5 H5 121.1 . . ?
C6 C5 H5 121.1 . . ?
C7 C6 C5 117(3) . . ?
C7 C6 H6 121.7 . . ?
C5 C6 H6 121.7 . . ?
C8 C7 C6 125(3) . . ?
C8 C7 H7 117.5 . . ?
C6 C7 H7 117.5 . . ?
C7 C8 C4 120(2) . . ?
C7 C8 C9 119(3) . . ?
C4 C8 C9 121(2) . . ?
N1 C9 C8 132(3) . . ?
N1 C9 H9 114.0 . . ?
C8 C9 H9 114.0 . . ?
N1 C10 C15 108(2) . . ?
N1 C10 C11 117(2) . . ?
C15 C10 C11 110(2) . . ?
N1 C10 H10 107.3 . . ?
C15 C10 H10 107.3 . . ?
C11 C10 H10 107.3 . . ?
C12 C11 C10 116(2) . . ?
C12 C11 H11A 108.4 . . ?
C10 C11 H11A 108.4 . . ?
C12 C11 H11B 108.4 . . ?
C10 C11 H11B 108.4 . . ?
H11A C11 H11B 107.4 . . ?
C13 C12 C11 112(3) . . ?
C13 C12 H12A 109.1 . . ?
C11 C12 H12A 109.1 . . ?
C13 C12 H12B 109.1 . . ?
C11 C12 H12B 109.1 . . ?
H12A C12 H12B 107.9 . . ?
C12 C13 C14 109(3) . . ?
C12 C13 H13A 109.8 . . ?
C14 C13 H13A 109.8 . . ?
C12 C13 H13B 109.8 . . ?
C14 C13 H13B 109.8 . . ?
H13A C13 H13B 108.3 . . ?
C13 C14 C15 108(2) . . ?
C13 C14 H14A 110.1 . . ?
C15 C14 H14A 110.1 . . ?
C13 C14 H14B 110.1 . . ?
C15 C14 H14B 110.1 . . ?
H14A C14 H14B 108.4 . . ?
C10 C15 N2 109(2) . . ?
C10 C15 C14 113(2) . . ?
N2 C15 C14 113(2) . . ?
C10 C15 H15 107.5 . . ?
N2 C15 H15 107.5 . . ?
C14 C15 H15 107.5 . . ?
N2 C16 C17 130(3) . . ?
N2 C16 H16 114.9 . . ?
C17 C16 H16 114.9 . . ?
C18 C17 C16 125(2) . . ?
C18 C17 C19 117(3) . . ?
C16 C17 C19 117(3) . . ?
O2 C18 C17 117(2) . . ?
O2 C18 C22 120(3) . . ?
C17 C18 C22 123(2) . . ?
C20 C19 C17 117(3) . . ?
C20 C19 H19 121.3 . . ?
C17 C19 H19 121.3 . . ?
C19 C20 C21 124(3) . . ?
C19 C20 H20 118.1 . . ?
C21 C20 H20 118.1 . . ?
C22 C21 C20 121(3) . . ?
C22 C21 H21 119.5 . . ?
C20 C21 H21 119.5 . . ?
C21 C22 O4 127(3) . . ?
C21 C22 C18 118(3) . . ?
O4 C22 C18 115(2) . . ?
O4 C23 C24 107(2) . . ?
O4 C23 H23A 110.3 . . ?
C24 C23 H23A 110.3 . . ?
O4 C23 H23B 110.3 . . ?
C24 C23 H23B 110.3 . . ?
H23A C23 H23B 108.6 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
N3 C25 C26 120(3) . . ?
N3 C25 H25 120.2 . . ?
C26 C25 H25 120.2 . . ?
C27 C26 C25 122(3) . . ?
C27 C26 H26 119.1 . . ?
C25 C26 H26 119.1 . . ?
C26 C27 C28 118(3) . . ?
C26 C27 H27 121.1 . . ?
C28 C27 H27 121.1 . . ?
C27 C28 C29 118(3) . . ?
C27 C28 H28 120.8 . . ?
C29 C28 H28 120.8 . . ?
N3 C29 C28 123(3) . . ?
N3 C29 H29 118.3 . . ?
C28 C29 H29 118.3 . . ?
C31 C30 N4 125(3) . . ?
C31 C30 H30 117.4 . . ?
N4 C30 H30 117.4 . . ?
C30 C31 C32 121(3) . . ?
C30 C31 H31 119.7 . . ?
C32 C31 H31 119.7 . . ?
C33 C32 C31 115(3) . . ?
C33 C32 H32 122.5 . . ?
C31 C32 H32 122.5 . . ?
C32 C33 C34 120(3) . . ?
C32 C33 H33 120.0 . . ?
C34 C33 H33 120.0 . . ?
N4 C34 C33 127(3) . . ?
N4 C34 H34 116.3 . . ?
C33 C34 H34 116.3 . . ?
C1S N1S C5S 107(4) . . ?
C2S C1S N1S 134(4) . . ?
C2S C1S H1S 112.9 . . ?
N1S C1S H1S 112.9 . . ?
C1S C2S C3S 112(4) . . ?
C1S C2S H2S 124.1 . . ?
C3S C2S H2S 124.1 . . ?
C2S C3S C4S 121(5) . . ?
C2S C3S H3S 119.3 . . ?
C4S C3S H3S 119.3 . . ?
C5S C4S C3S 112(4) . . ?
C5S C4S H4S 123.8 . . ?
C3S C4S H4S 123.8 . . ?
C4S C5S N1S 134(4) . . ?
C4S C5S H5S 113.2 . . ?
N1S C5S H5S 113.2 . . ?

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
C3 O3 C2 C1 180(2) . . . . ?
C2 O3 C3 C5 -7(4) . . . . ?
C2 O3 C3 C4 173(2) . . . . ?
Th1 O1 C4 C8 -11(4) . . . . ?
Th1 O1 C4 C3 171.0(19) . . . . ?
C5 C3 C4 O1 178(2) . . . . ?
O3 C3 C4 O1 -2(3) . . . . ?
C5 C3 C4 C8 0(4) . . . . ?
O3 C3 C4 C8 -180(2) . . . . ?
C4 C3 C5 C6 3(4) . . . . ?
O3 C3 C5 C6 -177(2) . . . . ?
C3 C5 C6 C7 -4(4) . . . . ?
C5 C6 C7 C8 3(4) . . . . ?
C6 C7 C8 C4 0(4) . . . . ?
C6 C7 C8 C9 179(2) . . . . ?
O1 C4 C8 C7 -180(2) . . . . ?
C3 C4 C8 C7 -2(4) . . . . ?
O1 C4 C8 C9 2(4) . . . . ?
C3 C4 C8 C9 180(2) . . . . ?
C10 N1 C9 C8 -177(3) . . . . ?
Th1 N1 C9 C8 -9(4) . . . . ?
C7 C8 C9 N1 -171(3) . . . . ?
C4 C8 C9 N1 8(4) . . . . ?
C9 N1 C10 C15 -144(2) . . . . ?
Th1 N1 C10 C15 47(2) . . . . ?
C9 N1 C10 C11 -19(3) . . . . ?
Th1 N1 C10 C11 171.2(18) . . . . ?
N1 C10 C11 C12 -169(2) . . . . ?
C15 C10 C11 C12 -46(3) . . . . ?
C10 C11 C12 C13 56(4) . . . . ?
C11 C12 C13 C14 -63(4) . . . . ?
C12 C13 C14 C15 61(3) . . . . ?
N1 C10 C15 N2 -61(3) . . . . ?
C11 C10 C15 N2 171(2) . . . . ?
N1 C10 C15 C14 173(2) . . . . ?
C11 C10 C15 C14 45(3) . . . . ?
C16 N2 C15 C10 -133(2) . . . . ?
Th1 N2 C15 C10 47(2) . . . . ?
C16 N2 C15 C14 -7(3) . . . . ?
Th1 N2 C15 C14 172.9(17) . . . . ?
C13 C14 C15 C10 -54(3) . . . . ?
C13 C14 C15 N2 -178(2) . . . . ?
C15 N2 C16 C17 -178(2) . . . . ?
Th1 N2 C16 C17 3(4) . . . . ?
N2 C16 C17 C18 7(4) . . . . ?
N2 C16 C17 C19 179(3) . . . . ?
Th1 O2 C18 C17 -2(5) . . . . ?
Th1 O2 C18 C22 174(2) . . . . ?
C16 C17 C18 O2 -9(4) . . . . ?
C19 C17 C18 O2 -180(2) . . . . ?
C16 C17 C18 C22 175(2) . . . . ?
C19 C17 C18 C22 4(4) . . . . ?
C18 C17 C19 C20 -6(4) . . . . ?
C16 C17 C19 C20 -179(2) . . . . ?
C17 C19 C20 C21 5(4) . . . . ?
C19 C20 C21 C22 0(4) . . . . ?
C20 C21 C22 O4 179(2) . . . . ?
C20 C21 C22 C18 -3(4) . . . . ?
C23 O4 C22 C21 1(4) . . . . ?
C23 O4 C22 C18 -177(2) . . . . ?
O2 C18 C22 C21 -175(2) . . . . ?
C17 C18 C22 C21 1(4) . . . . ?
O2 C18 C22 O4 3(4) . . . . ?
C17 C18 C22 O4 179(2) . . . . ?
C22 O4 C23 C24 -170(2) . . . . ?
C29 N3 C25 C26 6(4) . . . . ?
Th1 N3 C25 C26 179(2) . . . . ?
N3 C25 C26 C27 -7(5) . . . . ?
C25 C26 C27 C28 4(5) . . . . ?
C26 C27 C28 C29 0(5) . . . . ?
C25 N3 C29 C28 -2(4) . . . . ?
Th1 N3 C29 C28 -175(2) . . . . ?
C27 C28 C29 N3 0(5) . . . . ?
C34 N4 C30 C31 1(4) . . . . ?
Th1 N4 C30 C31 -169(2) . . . . ?
N4 C30 C31 C32 2(4) . . . . ?
C30 C31 C32 C33 -1(4) . . . . ?
C31 C32 C33 C34 -3(4) . . . . ?
C30 N4 C34 C33 -6(4) . . . . ?
Th1 N4 C34 C33 163(2) . . . . ?
C32 C33 C34 N4 7(5) . . . . ?
C5S N1S C1S C2S 0.0(4) . . . . ?
N1S C1S C2S C3S 0.0(3) . . . . ?
C1S C2S C3S C4S 0.0(8) . . . . ?
C2S C3S C4S C5S 0.0(10) . . . . ?
C3S C4S C5S N1S 0.1(13) . . . . ?
C1S N1S C5S C4S 0.0(10) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C10 H10 Cl1 1.00 2.92 3.56(3) 122.2 .
C11 H11B Cl1 0.99 2.95 3.73(3) 137.3 3_666
C15 H15 Cl2 1.00 2.96 3.59(3) 121.3 .
C25 H25 O1 0.95 2.53 3.12(3) 120.3 .
C25 H25 O3 0.95 2.58 3.52(3) 173.7 .
C29 H29 O2 0.95 2.51 3.13(3) 123.0 .
C30 H30 O1 0.95 2.62 3.17(4) 117.6 .
C31 H31 Cl2 0.95 2.78 3.65(3) 152.3 4_576
C33 H33 N1S 0.95 2.46 3.30(5) 148.1 3_566
C34 H34 O2 0.95 2.61 3.20(3) 120.8 .
C34 H34 O4 0.95 2.54 3.47(3) 166.1 .

_refine_diff_density_max         2.233
_refine_diff_density_min         -1.716
_refine_diff_density_rms         0.267

####################################################################### 
# 
# 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_17011_sq
_database_code_depnum_ccdc_archive 'CCDC 1533056'
_audit_update_record             
;
2017-02-16 deposited with the CCDC.
2017-03-23 downloaded from the CCDC.
;

_vrf_PLAT973_Alert_2_B           
; 
Problem:   Check calcd positive residual density on U1  1.79 3A-3
Response:  The data were collected on a 3 component twin.  The 
           intensity data were effectively detwinned by both the 
           data reduction and scaling programs.  This small residual 
           compared to the # of electrons at U could easily be an 
           artifact of the overall scale factor and truncation errors.  
;

_audit_creation_method           SHELXL-2014/7
#_shelx_SHELXL_version_number      '2014/7' 
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C34 H38 N10 O4 U'
_chemical_formula_sum            'C34 H38 N10 O4 U'
_chemical_formula_weight         888.77

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      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                   16.872(4)
_cell_length_b                   15.338(3)
_cell_length_c                   15.062(3)
_cell_angle_alpha                90
_cell_angle_beta                 93.301(2)
_cell_angle_gamma                90
_cell_volume                     3891.3(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9930
_cell_measurement_theta_min      2.21
_cell_measurement_theta_max      26.13

_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.517
_exptl_crystal_F_000             1744
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.710
_exptl_crystal_size_mid          0.640
_exptl_crystal_size_min          0.480
_exptl_absorpt_coefficient_mu    4.219
_shelx_estimated_absorpt_T_min   0.154
_shelx_estimated_absorpt_T_max   0.237
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.154
_exptl_absorpt_correction_T_max  0.237
_exptl_absorpt_process_details   'TWINABS (Sheldrick, 2015c)'
#_exptl_absorpt_special_details    ? 
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            81766
_diffrn_reflns_av_unetI/netI     0.3016
_diffrn_reflns_av_R_equivalents  0.1176
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.897
_diffrn_reflns_theta_max         26.257
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.907
_diffrn_measured_fraction_theta_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.907
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.907
_diffrn_reflns_point_group_measured_fraction_full 0.978
_reflns_number_total             7117
_reflns_number_gt                4959
_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. 
;

_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015a)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015b)'
_computing_molecular_graphics    'Mercury (CCDC, 2016)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2015b)'
_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)+(0.0700P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7117
_refine_ls_number_parameters     442
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0780
_refine_ls_R_factor_gt           0.0468
_refine_ls_wR_factor_ref         0.1202
_refine_ls_wR_factor_gt          0.1132
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_restrained_S_all      1.001
_refine_ls_shift/su_max          0.003
_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 0.72140(2) 0.46407(2) 0.41088(2) 0.02356(11) Uani 1 1 d . . . . .
O1 O 0.6266(2) 0.4427(3) 0.3110(3) 0.0338(14) Uani 1 1 d . . . . .
O2 O 0.8417(2) 0.5051(3) 0.4487(3) 0.0254(11) Uani 1 1 d . . . . .
O3 O 0.5840(3) 0.4224(4) 0.1411(3) 0.0444(14) Uani 1 1 d . . . . .
O4 O 0.9659(2) 0.5973(4) 0.4044(3) 0.0349(13) Uani 1 1 d . . . . .
N1 N 0.5950(3) 0.4143(4) 0.4890(3) 0.0278(14) Uani 1 1 d . . . . .
N2 N 0.7421(3) 0.4500(4) 0.5804(4) 0.0353(17) Uani 1 1 d . . . . .
N3 N 0.7446(3) 0.3085(5) 0.4341(4) 0.0334(15) Uani 1 1 d . . . . .
N4 N 0.7925(4) 0.2605(4) 0.4141(3) 0.0291(14) Uani 1 1 d . . . . .
N5 N 0.8404(4) 0.2099(5) 0.3961(4) 0.052(2) Uani 1 1 d . . . . .
N6 N 0.6725(4) 0.5971(6) 0.4754(4) 0.0418(18) Uani 1 1 d . . . . .
N7 N 0.6668(3) 0.6706(6) 0.4667(3) 0.0293(16) Uani 1 1 d . . . . .
N8 N 0.6607(4) 0.7469(5) 0.4620(4) 0.051(2) Uani 1 1 d . . . . .
N9 N 0.8003(3) 0.4123(4) 0.2746(3) 0.0284(14) Uani 1 1 d . . . . .
N10 N 0.7399(3) 0.5928(4) 0.2964(3) 0.0277(15) Uani 1 1 d . . . . .
C1 C 0.6322(7) 0.4539(8) -0.0038(6) 0.089(4) Uani 1 1 d . . . . .
H1A H 0.6390 0.5135 0.0187 0.134 Uiso 1 1 d R U . . .
H1B H 0.6158 0.4557 -0.0673 0.134 Uiso 1 1 d R U . . .
H1C H 0.6826 0.4223 0.0046 0.134 Uiso 1 1 d R U . . .
C2 C 0.5687(5) 0.4066(8) 0.0466(4) 0.068(3) Uani 1 1 d . . . . .
H2A H 0.5153 0.4285 0.0271 0.081 Uiso 1 1 calc R U . . .
H2B H 0.5705 0.3433 0.0343 0.081 Uiso 1 1 calc R U . . .
C3 C 0.5326(4) 0.3892(5) 0.1991(4) 0.0311(18) Uani 1 1 d . . . . .
C4 C 0.5583(4) 0.4030(5) 0.2905(4) 0.0276(17) Uani 1 1 d . . . . .
C5 C 0.4612(4) 0.3495(6) 0.1771(5) 0.038(2) Uani 1 1 d . . . . .
H5 H 0.4442 0.3420 0.1163 0.046 Uiso 1 1 calc R U . . .
C6 C 0.4136(4) 0.3204(6) 0.2436(5) 0.046(2) Uani 1 1 d . . . . .
H6 H 0.3647 0.2921 0.2281 0.055 Uiso 1 1 calc R U . . .
C7 C 0.4373(4) 0.3324(6) 0.3309(5) 0.038(2) Uani 1 1 d . . . . .
H7 H 0.4036 0.3133 0.3754 0.046 Uiso 1 1 calc R U . . .
C8 C 0.5096(3) 0.3721(5) 0.3570(4) 0.0290(18) Uani 1 1 d . . . . .
C9 C 0.5301(4) 0.3846(5) 0.4508(4) 0.0302(18) Uani 1 1 d . . . . .
H9 H 0.4902 0.3686 0.4897 0.036 Uiso 1 1 calc R U . . .
C10 C 0.6007(4) 0.4241(6) 0.5886(4) 0.038(2) Uani 1 1 d . . . . .
H10 H 0.5978 0.4879 0.6015 0.045 Uiso 1 1 calc R U . . .
C11 C 0.5321(4) 0.3802(6) 0.6355(4) 0.044(2) Uani 1 1 d . . . . .
H11A H 0.4822 0.4122 0.6201 0.053 Uiso 1 1 calc R U . . .
H11B H 0.5255 0.3198 0.6133 0.053 Uiso 1 1 calc R U . . .
C12 C 0.5465(4) 0.3783(7) 0.7366(5) 0.052(3) Uani 1 1 d . . . . .
H12A H 0.5449 0.4386 0.7599 0.062 Uiso 1 1 calc R U . . .
H12B H 0.5034 0.3448 0.7627 0.062 Uiso 1 1 calc R U . . .
C13 C 0.6215(4) 0.3395(7) 0.7632(5) 0.055(3) Uani 1 1 d . . . . .
H13A H 0.6226 0.2787 0.7414 0.067 Uiso 1 1 calc R U . . .
H13B H 0.6280 0.3383 0.8289 0.067 Uiso 1 1 calc R U . . .
C14 C 0.6895(4) 0.3900(7) 0.7265(4) 0.046(2) Uani 1 1 d . . . . .
H14A H 0.7404 0.3617 0.7453 0.056 Uiso 1 1 calc R U . . .
H14B H 0.6902 0.4500 0.7508 0.056 Uiso 1 1 calc R U . . .
C15 C 0.6809(4) 0.3939(7) 0.6227(4) 0.043(2) Uani 1 1 d . . . . .
H15 H 0.6877 0.3331 0.6005 0.052 Uiso 1 1 calc R U . . .
C16 C 0.7964(4) 0.4870(6) 0.6303(4) 0.038(2) Uani 1 1 d . . . . .
H16 H 0.7939 0.4783 0.6925 0.045 Uiso 1 1 calc R U . . .
C17 C 0.8612(4) 0.5408(5) 0.6022(4) 0.0295(18) Uani 1 1 d . . . . .
C18 C 0.8829(4) 0.5469(5) 0.5143(4) 0.0261(17) Uani 1 1 d . . . . .
C19 C 0.9066(4) 0.5876(5) 0.6689(4) 0.0322(19) Uani 1 1 d . . . . .
H19 H 0.8935 0.5834 0.7293 0.039 Uiso 1 1 calc R U . . .
C20 C 0.9689(4) 0.6384(6) 0.6468(5) 0.041(2) Uani 1 1 d . . . . .
H20 H 0.9976 0.6710 0.6916 0.050 Uiso 1 1 calc R U . . .
C21 C 0.9909(4) 0.6431(6) 0.5587(5) 0.042(2) Uani 1 1 d . . . . .
H21 H 1.0351 0.6777 0.5443 0.051 Uiso 1 1 calc R U . . .
C22 C 0.9487(4) 0.5979(6) 0.4930(5) 0.0352(19) Uani 1 1 d . . . . .
C23 C 1.0280(4) 0.6543(6) 0.3775(5) 0.039(2) Uani 1 1 d . . . . .
H23A H 1.0792 0.6387 0.4088 0.047 Uiso 1 1 calc R U . . .
H23B H 1.0154 0.7156 0.3917 0.047 Uiso 1 1 calc R U . . .
C24 C 1.0326(4) 0.6428(6) 0.2786(5) 0.045(2) Uani 1 1 d . . . . .
H24A H 1.0437 0.5816 0.2652 0.067 Uiso 1 1 d R U . . .
H24B H 1.0753 0.6796 0.2578 0.067 Uiso 1 1 d R U . . .
H24C H 0.9820 0.6600 0.2485 0.067 Uiso 1 1 d R U . . .
C25 C 0.7693(4) 0.3514(6) 0.2179(4) 0.040(2) Uani 1 1 d . . . . .
H25 H 0.7229 0.3212 0.2330 0.048 Uiso 1 1 calc R U . . .
C26 C 0.8026(5) 0.3313(6) 0.1387(4) 0.049(2) Uani 1 1 d . . . . .
H26 H 0.7782 0.2892 0.0998 0.058 Uiso 1 1 calc R U . . .
C27 C 0.8722(4) 0.3731(6) 0.1162(4) 0.041(2) Uani 1 1 d . . . . .
H27 H 0.8960 0.3601 0.0621 0.049 Uiso 1 1 calc R U . . .
C28 C 0.9049(4) 0.4330(6) 0.1742(5) 0.043(2) Uani 1 1 d . . . . .
H28 H 0.9523 0.4627 0.1613 0.051 Uiso 1 1 calc R U . . .
C29 C 0.8675(4) 0.4504(5) 0.2535(5) 0.036(2) Uani 1 1 d . . . . .
H29 H 0.8915 0.4914 0.2939 0.043 Uiso 1 1 calc R U . . .
C30 C 0.7025(4) 0.5936(6) 0.2151(4) 0.040(2) Uani 1 1 d . . . . .
H30 H 0.6659 0.5483 0.1994 0.047 Uiso 1 1 calc R U . . .
C31 C 0.7160(5) 0.6593(6) 0.1528(5) 0.044(2) Uani 1 1 d . . . . .
H31 H 0.6880 0.6590 0.0962 0.053 Uiso 1 1 calc R U . . .
C32 C 0.7687(4) 0.7226(6) 0.1741(5) 0.045(2) Uani 1 1 d . . . . .
H32 H 0.7800 0.7660 0.1316 0.054 Uiso 1 1 calc R U . . .
C33 C 0.8070(4) 0.7243(6) 0.2590(5) 0.041(2) Uani 1 1 d . . . . .
H33 H 0.8433 0.7695 0.2761 0.049 Uiso 1 1 calc R U . . .
C34 C 0.7905(4) 0.6587(6) 0.3167(5) 0.0335(19) Uani 1 1 d . . . . .
H34 H 0.8162 0.6597 0.3744 0.040 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 O1 2.157(4) . ?
U1 O2 2.170(4) . ?
U1 N6 2.425(8) . ?
U1 N3 2.440(7) . ?
U1 N2 2.567(6) . ?
U1 N1 2.609(5) . ?
U1 N9 2.632(6) . ?
U1 N10 2.652(6) . ?
O1 C4 1.323(8) . ?
O2 C18 1.337(7) . ?
O3 C3 1.365(8) . ?
O3 C2 1.452(8) . ?
O4 C22 1.383(8) . ?
O4 C23 1.440(8) . ?
N1 C9 1.290(7) . ?
N1 C10 1.504(8) . ?
N2 C16 1.283(9) . ?
N2 C15 1.513(9) . ?
N3 N4 1.147(8) . ?
N4 N5 1.165(9) . ?
N6 N7 1.138(9) . ?
N7 N8 1.176(9) . ?
N9 C29 1.331(9) . ?
N9 C25 1.351(9) . ?
N10 C30 1.344(8) . ?
N10 C34 1.347(9) . ?
C1 C2 1.532(12) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C5 1.372(9) . ?
C3 C4 1.435(8) . ?
C4 C8 1.414(9) . ?
C5 C6 1.393(10) . ?
C5 H5 0.9500 . ?
C6 C7 1.365(9) . ?
C6 H6 0.9500 . ?
C7 C8 1.399(9) . ?
C7 H7 0.9500 . ?
C8 C9 1.448(9) . ?
C9 H9 0.9500 . ?
C10 C15 1.492(9) . ?
C10 C11 1.544(10) . ?
C10 H10 1.0000 . ?
C11 C12 1.528(9) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C13 1.435(10) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C14 1.515(11) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C15 1.562(9) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 H15 1.0000 . ?
C16 C17 1.451(10) . ?
C16 H16 0.9500 . ?
C17 C18 1.398(10) . ?
C17 C19 1.422(9) . ?
C18 C22 1.409(10) . ?
C19 C20 1.366(11) . ?
C19 H19 0.9500 . ?
C20 C21 1.400(11) . ?
C20 H20 0.9500 . ?
C21 C22 1.373(10) . ?
C21 H21 0.9500 . ?
C23 C24 1.507(10) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 C26 1.381(10) . ?
C25 H25 0.9500 . ?
C26 C27 1.397(11) . ?
C26 H26 0.9500 . ?
C27 C28 1.362(11) . ?
C27 H27 0.9500 . ?
C28 C29 1.408(10) . ?
C28 H28 0.9500 . ?
C29 H29 0.9500 . ?
C30 C31 1.405(11) . ?
C30 H30 0.9500 . ?
C31 C32 1.344(11) . ?
C31 H31 0.9500 . ?
C32 C33 1.400(9) . ?
C32 H32 0.9500 . ?
C33 C34 1.368(10) . ?
C33 H33 0.9500 . ?
C34 H34 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 U1 O2 150.73(16) . . ?
O1 U1 N6 98.7(2) . . ?
O2 U1 N6 89.1(2) . . ?
O1 U1 N3 93.30(19) . . ?
O2 U1 N3 96.11(19) . . ?
N6 U1 N3 145.2(2) . . ?
O1 U1 N2 137.25(17) . . ?
O2 U1 N2 72.01(16) . . ?
N6 U1 N2 72.7(2) . . ?
N3 U1 N2 76.3(2) . . ?
O1 U1 N1 71.19(15) . . ?
O2 U1 N1 137.99(15) . . ?
N6 U1 N1 76.1(2) . . ?
N3 U1 N1 77.16(19) . . ?
N2 U1 N1 66.08(16) . . ?
O1 U1 N9 78.37(16) . . ?
O2 U1 N9 77.59(16) . . ?
N6 U1 N9 139.9(2) . . ?
N3 U1 N9 74.48(19) . . ?
N2 U1 N9 134.77(17) . . ?
N1 U1 N9 136.62(18) . . ?
O1 U1 N10 76.71(17) . . ?
O2 U1 N10 79.13(16) . . ?
N6 U1 N10 71.9(2) . . ?
N3 U1 N10 142.90(18) . . ?
N2 U1 N10 134.04(19) . . ?
N1 U1 N10 129.87(16) . . ?
N9 U1 N10 68.54(18) . . ?
C4 O1 U1 146.4(4) . . ?
C18 O2 U1 140.5(4) . . ?
C3 O3 C2 118.8(6) . . ?
C22 O4 C23 117.7(5) . . ?
C9 N1 C10 119.0(5) . . ?
C9 N1 U1 126.6(4) . . ?
C10 N1 U1 114.4(4) . . ?
C16 N2 C15 119.1(6) . . ?
C16 N2 U1 126.7(5) . . ?
C15 N2 U1 114.2(4) . . ?
N4 N3 U1 134.5(5) . . ?
N3 N4 N5 177.7(8) . . ?
N7 N6 U1 144.7(5) . . ?
N6 N7 N8 177.0(7) . . ?
C29 N9 C25 117.1(6) . . ?
C29 N9 U1 122.0(5) . . ?
C25 N9 U1 120.5(5) . . ?
C30 N10 C34 117.2(6) . . ?
C30 N10 U1 122.2(5) . . ?
C34 N10 U1 120.6(4) . . ?
C2 C1 H1A 109.9 . . ?
C2 C1 H1B 109.3 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.1 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O3 C2 C1 108.5(7) . . ?
O3 C2 H2A 110.0 . . ?
C1 C2 H2A 110.0 . . ?
O3 C2 H2B 110.0 . . ?
C1 C2 H2B 110.0 . . ?
H2A C2 H2B 108.4 . . ?
O3 C3 C5 126.3(6) . . ?
O3 C3 C4 113.0(6) . . ?
C5 C3 C4 120.7(6) . . ?
O1 C4 C8 121.5(5) . . ?
O1 C4 C3 120.2(6) . . ?
C8 C4 C3 118.3(6) . . ?
C3 C5 C6 120.1(6) . . ?
C3 C5 H5 119.9 . . ?
C6 C5 H5 119.9 . . ?
C7 C6 C5 120.1(7) . . ?
C7 C6 H6 120.0 . . ?
C5 C6 H6 120.0 . . ?
C6 C7 C8 122.1(7) . . ?
C6 C7 H7 118.9 . . ?
C8 C7 H7 118.9 . . ?
C7 C8 C4 118.7(6) . . ?
C7 C8 C9 119.2(6) . . ?
C4 C8 C9 122.0(6) . . ?
N1 C9 C8 129.2(6) . . ?
N1 C9 H9 115.4 . . ?
C8 C9 H9 115.4 . . ?
C15 C10 N1 108.5(6) . . ?
C15 C10 C11 113.3(6) . . ?
N1 C10 C11 114.0(5) . . ?
C15 C10 H10 106.9 . . ?
N1 C10 H10 106.9 . . ?
C11 C10 H10 106.9 . . ?
C12 C11 C10 112.6(6) . . ?
C12 C11 H11A 109.1 . . ?
C10 C11 H11A 109.1 . . ?
C12 C11 H11B 109.1 . . ?
C10 C11 H11B 109.1 . . ?
H11A C11 H11B 107.8 . . ?
C13 C12 C11 111.9(7) . . ?
C13 C12 H12A 109.2 . . ?
C11 C12 H12A 109.2 . . ?
C13 C12 H12B 109.2 . . ?
C11 C12 H12B 109.2 . . ?
H12A C12 H12B 107.9 . . ?
C12 C13 C14 111.1(7) . . ?
C12 C13 H13A 109.4 . . ?
C14 C13 H13A 109.4 . . ?
C12 C13 H13B 109.4 . . ?
C14 C13 H13B 109.4 . . ?
H13A C13 H13B 108.0 . . ?
C13 C14 C15 110.8(6) . . ?
C13 C14 H14A 109.5 . . ?
C15 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
C15 C14 H14B 109.5 . . ?
H14A C14 H14B 108.1 . . ?
C10 C15 N2 107.8(6) . . ?
C10 C15 C14 112.8(6) . . ?
N2 C15 C14 114.6(6) . . ?
C10 C15 H15 107.1 . . ?
N2 C15 H15 107.1 . . ?
C14 C15 H15 107.1 . . ?
N2 C16 C17 127.2(6) . . ?
N2 C16 H16 116.4 . . ?
C17 C16 H16 116.4 . . ?
C18 C17 C19 118.4(7) . . ?
C18 C17 C16 123.9(6) . . ?
C19 C17 C16 117.7(6) . . ?
O2 C18 C17 120.9(6) . . ?
O2 C18 C22 118.8(6) . . ?
C17 C18 C22 120.4(6) . . ?
C20 C19 C17 120.4(7) . . ?
C20 C19 H19 119.8 . . ?
C17 C19 H19 119.8 . . ?
C19 C20 C21 120.7(7) . . ?
C19 C20 H20 119.6 . . ?
C21 C20 H20 119.6 . . ?
C22 C21 C20 120.1(8) . . ?
C22 C21 H21 119.9 . . ?
C20 C21 H21 119.9 . . ?
C21 C22 O4 124.7(7) . . ?
C21 C22 C18 120.0(7) . . ?
O4 C22 C18 115.3(6) . . ?
O4 C23 C24 106.7(6) . . ?
O4 C23 H23A 110.4 . . ?
C24 C23 H23A 110.4 . . ?
O4 C23 H23B 110.4 . . ?
C24 C23 H23B 110.4 . . ?
H23A C23 H23B 108.6 . . ?
C23 C24 H24A 109.7 . . ?
C23 C24 H24B 109.3 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.4 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
N9 C25 C26 122.6(7) . . ?
N9 C25 H25 118.7 . . ?
C26 C25 H25 118.7 . . ?
C25 C26 C27 119.8(7) . . ?
C25 C26 H26 120.1 . . ?
C27 C26 H26 120.1 . . ?
C28 C27 C26 118.0(7) . . ?
C28 C27 H27 121.0 . . ?
C26 C27 H27 121.0 . . ?
C27 C28 C29 119.2(8) . . ?
C27 C28 H28 120.4 . . ?
C29 C28 H28 120.4 . . ?
N9 C29 C28 123.3(7) . . ?
N9 C29 H29 118.3 . . ?
C28 C29 H29 118.3 . . ?
N10 C30 C31 122.0(7) . . ?
N10 C30 H30 119.0 . . ?
C31 C30 H30 119.0 . . ?
C32 C31 C30 119.3(7) . . ?
C32 C31 H31 120.4 . . ?
C30 C31 H31 120.4 . . ?
C31 C32 C33 119.8(7) . . ?
C31 C32 H32 120.1 . . ?
C33 C32 H32 120.1 . . ?
C34 C33 C32 117.7(8) . . ?
C34 C33 H33 121.1 . . ?
C32 C33 H33 121.1 . . ?
N10 C34 C33 123.9(7) . . ?
N10 C34 H34 118.0 . . ?
C33 C34 H34 118.0 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C3 O3 C2 C1 177.4(8) . . . . ?
C2 O3 C3 C5 -8.0(12) . . . . ?
C2 O3 C3 C4 174.9(7) . . . . ?
U1 O1 C4 C8 20.9(13) . . . . ?
U1 O1 C4 C3 -158.2(6) . . . . ?
O3 C3 C4 O1 -1.5(10) . . . . ?
C5 C3 C4 O1 -178.8(7) . . . . ?
O3 C3 C4 C8 179.4(7) . . . . ?
C5 C3 C4 C8 2.1(11) . . . . ?
O3 C3 C5 C6 -178.4(8) . . . . ?
C4 C3 C5 C6 -1.5(12) . . . . ?
C3 C5 C6 C7 1.1(13) . . . . ?
C5 C6 C7 C8 -1.3(14) . . . . ?
C6 C7 C8 C4 2.0(12) . . . . ?
C6 C7 C8 C9 178.6(8) . . . . ?
O1 C4 C8 C7 178.6(7) . . . . ?
C3 C4 C8 C7 -2.3(11) . . . . ?
O1 C4 C8 C9 2.1(11) . . . . ?
C3 C4 C8 C9 -178.8(7) . . . . ?
C10 N1 C9 C8 177.8(7) . . . . ?
U1 N1 C9 C8 -1.0(12) . . . . ?
C7 C8 C9 N1 175.3(8) . . . . ?
C4 C8 C9 N1 -8.3(12) . . . . ?
C9 N1 C10 C15 138.2(7) . . . . ?
U1 N1 C10 C15 -42.8(8) . . . . ?
C9 N1 C10 C11 11.0(11) . . . . ?
U1 N1 C10 C11 -170.0(6) . . . . ?
C15 C10 C11 C12 45.9(11) . . . . ?
N1 C10 C11 C12 170.7(7) . . . . ?
C10 C11 C12 C13 -53.7(11) . . . . ?
C11 C12 C13 C14 60.3(11) . . . . ?
C12 C13 C14 C15 -58.6(10) . . . . ?
N1 C10 C15 N2 59.8(8) . . . . ?
C11 C10 C15 N2 -172.6(7) . . . . ?
N1 C10 C15 C14 -172.7(7) . . . . ?
C11 C10 C15 C14 -45.1(10) . . . . ?
C16 N2 C15 C10 128.5(8) . . . . ?
U1 N2 C15 C10 -49.6(8) . . . . ?
C16 N2 C15 C14 2.0(11) . . . . ?
U1 N2 C15 C14 -176.1(5) . . . . ?
C13 C14 C15 C10 50.9(11) . . . . ?
C13 C14 C15 N2 174.7(7) . . . . ?
C15 N2 C16 C17 178.1(8) . . . . ?
U1 N2 C16 C17 -4.1(12) . . . . ?
N2 C16 C17 C18 -12.8(13) . . . . ?
N2 C16 C17 C19 169.4(8) . . . . ?
U1 O2 C18 C17 32.7(11) . . . . ?
U1 O2 C18 C22 -146.9(6) . . . . ?
C19 C17 C18 O2 -179.2(6) . . . . ?
C16 C17 C18 O2 3.0(11) . . . . ?
C19 C17 C18 C22 0.4(10) . . . . ?
C16 C17 C18 C22 -177.4(7) . . . . ?
C18 C17 C19 C20 1.3(11) . . . . ?
C16 C17 C19 C20 179.2(7) . . . . ?
C17 C19 C20 C21 -2.2(11) . . . . ?
C19 C20 C21 C22 1.5(12) . . . . ?
C20 C21 C22 O4 -179.2(7) . . . . ?
C20 C21 C22 C18 0.2(12) . . . . ?
C23 O4 C22 C21 -6.0(11) . . . . ?
C23 O4 C22 C18 174.6(6) . . . . ?
O2 C18 C22 C21 178.5(7) . . . . ?
C17 C18 C22 C21 -1.1(11) . . . . ?
O2 C18 C22 O4 -2.0(10) . . . . ?
C17 C18 C22 O4 178.4(6) . . . . ?
C22 O4 C23 C24 -178.3(6) . . . . ?
C29 N9 C25 C26 -3.1(11) . . . . ?
U1 N9 C25 C26 170.3(6) . . . . ?
N9 C25 C26 C27 1.8(13) . . . . ?
C25 C26 C27 C28 -0.1(12) . . . . ?
C26 C27 C28 C29 -0.1(12) . . . . ?
C25 N9 C29 C28 2.9(11) . . . . ?
U1 N9 C29 C28 -170.4(6) . . . . ?
C27 C28 C29 N9 -1.3(12) . . . . ?
C34 N10 C30 C31 0.9(10) . . . . ?
U1 N10 C30 C31 -176.3(6) . . . . ?
N10 C30 C31 C32 1.2(12) . . . . ?
C30 C31 C32 C33 -2.7(12) . . . . ?
C31 C32 C33 C34 2.0(12) . . . . ?
C30 N10 C34 C33 -1.6(11) . . . . ?
U1 N10 C34 C33 175.6(6) . . . . ?
C32 C33 C34 N10 0.2(11) . . . . ?

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
C5 H5 N8 0.95 2.53 3.255(9) 133.1 2_645
C29 H29 O2 0.95 2.53 3.113(8) 119.6 .
C29 H29 O4 0.95 2.60 3.545(9) 176.1 .
C30 H30 O1 0.95 2.45 3.049(10) 120.6 .
C30 H30 O3 0.95 2.50 3.447(10) 171.4 .
C31 H31 N8 0.95 2.51 3.300(9) 141.3 4_575
C34 H34 O2 0.95 2.65 3.171(9) 115.3 .

_refine_diff_density_max         1.574
_refine_diff_density_min         -1.971
_refine_diff_density_rms         0.195



####################################################################### 
# 
# 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_17016
_database_code_depnum_ccdc_archive 'CCDC 1533057'
_audit_update_record             
;
2017-02-16 deposited with the CCDC.
2017-03-23 downloaded from the CCDC.
;

_vrf_PLAT410_Alert_2_A           
; 
Problem:   Short intra H..H contact H9 .. H11C .. 1.75 Ang
Response:  Atom H11C is disordered.  These "contacts" really do happen.
;
_vrf_PLAT410_Alert_2_B           
; 
Problem:   Short intra H..H contact H14B .. H16 .. 1.89 Ang
Response:  Atom H14B is disordered.  These "contacts" really do happen.
;
_vrf_PLAT971_Alert_2_B           
; 
Problem:   Check calcd residual density 0.76 A from U1   2.54 eA-3
Response:  This peak is << Z of uranium.  Believe it or not U has 
           both d and f orbitals so the spherical model of core 
           electrons the most likely sorce of this problem.  
;

# The selected crystal was split by 8.2 degrees and by 5.3 degrees.  
# The splitting was corrected by the data reduction and scaling programs. 

_audit_creation_method           SHELXL-2014/7
#_shelx_SHELXL_version_number      '2014/7' 
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C34 H38 N10 O4 U, C7 H8'
_chemical_formula_sum            'C41 H46 N10 O4 U'
_chemical_formula_weight         980.91

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

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

_cell_length_a                   9.572(5)
_cell_length_b                   13.791(7)
_cell_length_c                   16.103(2)
_cell_angle_alpha                76.878(2)
_cell_angle_beta                 86.987(2)
_cell_angle_gamma                71.973(2)
_cell_volume                     1968.2(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9951
_cell_measurement_theta_min      2.23
_cell_measurement_theta_max      29.88

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.655
_exptl_crystal_F_000             972
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.410
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    4.179
_shelx_estimated_absorpt_T_min   0.279
_shelx_estimated_absorpt_T_max   0.680
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.279
_exptl_absorpt_correction_T_max  0.680
_exptl_absorpt_process_details   'TWINABS (Sheldrick, 2015c)'
#_exptl_absorpt_special_details    ? 
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            90881
_diffrn_reflns_av_unetI/netI     0.0596
_diffrn_reflns_av_R_equivalents  0.0574
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.299
_diffrn_reflns_theta_max         31.673
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.893
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.893
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.893
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             11866
_reflns_number_gt                9414
_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       'APEX2 (Bruker, 2007)'
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015a)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015b)'
_computing_molecular_graphics    'Mercury (CCDC, 2016)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2015b)'
_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)+(0.0560P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         11866
_refine_ls_number_parameters     648
_refine_ls_number_restraints     1149
_refine_ls_R_factor_all          0.0616
_refine_ls_R_factor_gt           0.0420
_refine_ls_wR_factor_ref         0.0945
_refine_ls_wR_factor_gt          0.0891
_refine_ls_goodness_of_fit_ref   0.990
_refine_ls_restrained_S_all      0.955
_refine_ls_shift/su_max          0.003
_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 0.36811(2) 0.70011(2) 0.70548(2) 0.02514(5) Uani 1 1 d . U . . .
O1 O 0.0854(4) 0.7244(3) 0.4726(2) 0.0521(9) Uani 1 1 d D U . . .
O2 O 0.2369(3) 0.7567(2) 0.58923(16) 0.0313(6) Uani 1 1 d . U . . .
O3 O 0.4796(3) 0.5787(2) 0.81209(16) 0.0287(6) Uani 1 1 d . U . . .
O4 O 0.5282(3) 0.3880(2) 0.90633(18) 0.0375(7) Uani 1 1 d D U . . .
N1 N 0.3469(4) 0.8932(3) 0.6477(2) 0.0407(8) Uani 1 1 d D U . . .
N2 N 0.5403(4) 0.7686(2) 0.7816(2) 0.0340(7) Uani 1 1 d D U . . .
N3 N 0.5812(4) 0.6918(3) 0.6181(2) 0.0355(8) Uani 1 1 d . U . . .
N4 N 0.6316(4) 0.7470(3) 0.5737(2) 0.0351(8) Uani 1 1 d . U . . .
N5 N 0.6894(7) 0.8006(4) 0.5278(4) 0.092(2) Uani 1 1 d . U . . .
N6 N 0.1887(4) 0.7894(3) 0.7952(2) 0.0327(7) Uani 1 1 d . U . . .
N7 N 0.0819(4) 0.7791(2) 0.8304(2) 0.0271(7) Uani 1 1 d . U . . .
N8 N -0.0233(4) 0.7715(3) 0.8660(2) 0.0383(8) Uani 1 1 d . U . . .
N9 N 0.4372(3) 0.5274(3) 0.64544(19) 0.0261(6) Uani 1 1 d . U . . .
N10 N 0.1698(3) 0.6028(3) 0.7393(2) 0.0290(7) Uani 1 1 d . U . . .
C1 C -0.0072(8) 0.6029(5) 0.4369(4) 0.0512(17) Uani 0.727(8) 1 d D U P A 1
H1A H 0.0919 0.5550 0.4337 0.077 Uiso 0.727(8) 1 calc R U P A 1
H1B H -0.0742 0.5904 0.3994 0.077 Uiso 0.727(8) 1 calc R U P A 1
H1C H -0.0410 0.5907 0.4957 0.077 Uiso 0.727(8) 1 calc R U P A 1
C2 C -0.0045(7) 0.7134(5) 0.4089(3) 0.0436(15) Uani 0.727(8) 1 d D U P A 1
H2A H 0.0389 0.7256 0.3518 0.052 Uiso 0.727(8) 1 calc R U P A 1
H2B H -0.1048 0.7632 0.4072 0.052 Uiso 0.727(8) 1 calc R U P A 1
C1' C -0.0027(18) 0.6516(15) 0.3759(9) 0.048(3) Uani 0.273(8) 1 d D U P A 2
H1'1 H 0.0284 0.6994 0.3293 0.072 Uiso 0.273(8) 1 calc R U P A 2
H1'2 H -0.0882 0.6367 0.3572 0.072 Uiso 0.273(8) 1 calc R U P A 2
H1'3 H 0.0779 0.5862 0.3922 0.072 Uiso 0.273(8) 1 calc R U P A 2
C2' C -0.0428(11) 0.7011(16) 0.4509(10) 0.048(3) Uani 0.273(8) 1 d D U P A 2
H2'1 H -0.1268 0.7659 0.4361 0.057 Uiso 0.273(8) 1 calc R U P A 2
H2'2 H -0.0705 0.6525 0.4995 0.057 Uiso 0.273(8) 1 calc R U P A 2
C3 C 0.1092(5) 0.8186(4) 0.4569(3) 0.0432(11) Uani 1 1 d . U . . .
C4 C 0.1925(4) 0.8324(4) 0.5203(2) 0.0346(9) Uani 1 1 d . U . . .
C5 C 0.0573(5) 0.8990(5) 0.3864(3) 0.0536(13) Uani 1 1 d . U . . .
H5 H -0.0003 0.8896 0.3444 0.064 Uiso 1 1 calc R U . . .
C6 C 0.0871(6) 0.9912(5) 0.3761(3) 0.0542(13) Uani 1 1 d . U . . .
H6 H 0.0499 1.0457 0.3274 0.065 Uiso 1 1 calc R U . . .
C7 C 0.1716(5) 1.0054(4) 0.4365(3) 0.0481(12) Uani 1 1 d . U . . .
H7 H 0.1939 1.0693 0.4288 0.058 Uiso 1 1 calc R U . . .
C8 C 0.2248(5) 0.9254(4) 0.5095(3) 0.0367(9) Uani 1 1 d . U . . .
C9 C 0.2984(5) 0.9508(4) 0.5745(3) 0.0424(11) Uani 1 1 d . U . . .
H9 H 0.3122 1.0179 0.5611 0.051 Uiso 1 1 calc R U . . .
C10 C 0.3889(6) 0.9433(4) 0.7134(3) 0.0301(10) Uani 0.750(5) 1 d D U P B 1
H10 H 0.3237 0.9352 0.7634 0.036 Uiso 0.750(5) 1 calc R U P B 1
C11 C 0.3734(7) 1.0593(5) 0.6835(4) 0.0365(11) Uani 0.750(5) 1 d D U P B 1
H11A H 0.4333 1.0698 0.6322 0.044 Uiso 0.750(5) 1 calc R U P B 1
H11B H 0.2694 1.0986 0.6674 0.044 Uiso 0.750(5) 1 calc R U P B 1
C12 C 0.4219(6) 1.1021(4) 0.7519(4) 0.0396(11) Uani 0.750(5) 1 d D U P B 1
H12A H 0.3612 1.0935 0.8031 0.048 Uiso 0.750(5) 1 calc R U P B 1
H12B H 0.4094 1.1776 0.7307 0.048 Uiso 0.750(5) 1 calc R U P B 1
C13 C 0.5822(6) 1.0430(4) 0.7744(4) 0.0413(11) Uani 0.750(5) 1 d D U P B 1
H13A H 0.6156 1.0699 0.8192 0.050 Uiso 0.750(5) 1 calc R U P B 1
H13B H 0.6429 1.0539 0.7235 0.050 Uiso 0.750(5) 1 calc R U P B 1
C14 C 0.6018(7) 0.9271(4) 0.8061(4) 0.0378(12) Uani 0.750(5) 1 d D U P B 1
H14A H 0.5490 0.9166 0.8603 0.045 Uiso 0.750(5) 1 calc R U P B 1
H14B H 0.7075 0.8895 0.8183 0.045 Uiso 0.750(5) 1 calc R U P B 1
C15 C 0.5460(6) 0.8789(3) 0.7430(4) 0.0315(10) Uani 0.750(5) 1 d D U P B 1
H15 H 0.6111 0.8774 0.6924 0.038 Uiso 0.750(5) 1 calc R U P B 1
C10' C 0.4695(14) 0.9275(12) 0.6765(8) 0.0340(16) Uani 0.250(5) 1 d D U P B 2
H10' H 0.5659 0.8961 0.6511 0.041 Uiso 0.250(5) 1 calc R U P B 2
C11' C 0.423(2) 1.0483(15) 0.6547(12) 0.0369(17) Uani 0.250(5) 1 d D U P B 2
H11C H 0.4367 1.0734 0.5931 0.044 Uiso 0.250(5) 1 calc R U P B 2
H11D H 0.3173 1.0762 0.6667 0.044 Uiso 0.250(5) 1 calc R U P B 2
C12' C 0.512(2) 1.0892(13) 0.7059(8) 0.0399(17) Uani 0.250(5) 1 d D U P B 2
H12C H 0.4734 1.1665 0.6937 0.048 Uiso 0.250(5) 1 calc R U P B 2
H12D H 0.6153 1.0694 0.6881 0.048 Uiso 0.250(5) 1 calc R U P B 2
C13' C 0.505(2) 1.0462(11) 0.8009(9) 0.0385(17) Uani 0.250(5) 1 d D U P B 2
H13C H 0.4021 1.0719 0.8196 0.046 Uiso 0.250(5) 1 calc R U P B 2
H13D H 0.5664 1.0729 0.8317 0.046 Uiso 0.250(5) 1 calc R U P B 2
C14' C 0.5561(19) 0.9276(11) 0.8248(12) 0.0353(17) Uani 0.250(5) 1 d D U P B 2
H14C H 0.5415 0.9031 0.8864 0.042 Uiso 0.250(5) 1 calc R U P B 2
H14D H 0.6622 0.9012 0.8133 0.042 Uiso 0.250(5) 1 calc R U P B 2
C15' C 0.4692(16) 0.8855(4) 0.7728(8) 0.0325(16) Uani 0.250(5) 1 d D U P B 2
H15' H 0.3657 0.8996 0.7930 0.039 Uiso 0.250(5) 1 calc R U P B 2
C16 C 0.6422(5) 0.7141(3) 0.8360(3) 0.0340(9) Uani 1 1 d . U . . .
H16 H 0.7082 0.7486 0.8479 0.041 Uiso 1 1 calc R U . . .
C17 C 0.6706(4) 0.6073(3) 0.8821(2) 0.0278(8) Uani 1 1 d . U . . .
C18 C 0.5859(4) 0.5447(3) 0.8709(2) 0.0264(7) Uani 1 1 d . U . . .
C19 C 0.7839(5) 0.5679(3) 0.9441(3) 0.0349(9) Uani 1 1 d . U . . .
H19 H 0.8419 0.6103 0.9515 0.042 Uiso 1 1 calc R U . . .
C20 C 0.8117(5) 0.4689(4) 0.9941(3) 0.0392(10) Uani 1 1 d . U . . .
H20 H 0.8889 0.4430 1.0357 0.047 Uiso 1 1 calc R U . . .
C21 C 0.7277(5) 0.4065(3) 0.9841(3) 0.0374(9) Uani 1 1 d . U . . .
H21 H 0.7470 0.3383 1.0194 0.045 Uiso 1 1 calc R U . . .
C22 C 0.6158(5) 0.4425(3) 0.9231(2) 0.0306(8) Uani 1 1 d . U . . .
C23 C 0.5531(5) 0.2840(3) 0.9571(3) 0.0400(10) Uani 1 1 d D U . . .
H23A H 0.5439 0.2850 1.0184 0.048 Uiso 1 1 calc R U . . .
H23B H 0.6527 0.2390 0.9475 0.048 Uiso 1 1 calc R U . . .
C24 C 0.4385(6) 0.2442(4) 0.9295(3) 0.0489(12) Uani 1 1 d D U . . .
H24A H 0.3417 0.2831 0.9470 0.073 Uiso 1 1 calc R U . . .
H24B H 0.4595 0.1697 0.9562 0.073 Uiso 1 1 calc R U . . .
H24C H 0.4394 0.2536 0.8673 0.073 Uiso 1 1 calc R U . . .
C25 C 0.3528(4) 0.5158(3) 0.5866(2) 0.0262(7) Uani 1 1 d . U . . .
H25 H 0.2661 0.5712 0.5662 0.031 Uiso 1 1 calc R U . . .
C26 C 0.3870(4) 0.4267(3) 0.5547(2) 0.0310(8) Uani 1 1 d . U . . .
H26 H 0.3245 0.4214 0.5131 0.037 Uiso 1 1 calc R U . . .
C27 C 0.5114(5) 0.3460(3) 0.5833(3) 0.0334(9) Uani 1 1 d . U . . .
H27 H 0.5365 0.2839 0.5622 0.040 Uiso 1 1 calc R U . . .
C28 C 0.6000(5) 0.3570(3) 0.6437(3) 0.0354(9) Uani 1 1 d . U . . .
H28 H 0.6876 0.3027 0.6645 0.043 Uiso 1 1 calc R U . . .
C29 C 0.5588(4) 0.4480(3) 0.6729(2) 0.0307(8) Uani 1 1 d . U . . .
H29 H 0.6197 0.4549 0.7146 0.037 Uiso 1 1 calc R U . . .
C30 C 0.0352(4) 0.6425(3) 0.7016(3) 0.0323(8) Uani 1 1 d . U . . .
H30 H 0.0109 0.7096 0.6641 0.039 Uiso 1 1 calc R U . . .
C31 C -0.0685(5) 0.5907(4) 0.7148(3) 0.0402(10) Uani 1 1 d . U . . .
H31 H -0.1619 0.6216 0.6868 0.048 Uiso 1 1 calc R U . . .
C32 C -0.0361(5) 0.4952(4) 0.7678(3) 0.0432(10) Uani 1 1 d . U . . .
H32 H -0.1061 0.4580 0.7776 0.052 Uiso 1 1 calc R U . . .
C33 C 0.1001(5) 0.4527(4) 0.8074(3) 0.0441(11) Uani 1 1 d . U . . .
H33 H 0.1251 0.3856 0.8448 0.053 Uiso 1 1 calc R U . . .
C34 C 0.2005(5) 0.5084(4) 0.7924(3) 0.0348(9) Uani 1 1 d . U . . .
H34 H 0.2938 0.4788 0.8206 0.042 Uiso 1 1 calc R U . . .
C1A C -0.1280(6) 0.9269(4) 0.0593(3) 0.0358(12) Uani 0.660(5) 1 d D U P C 1
C2A C -0.0427(7) 0.8242(5) 0.0775(3) 0.0397(12) Uani 0.660(5) 1 d D U P C 1
H2AA H -0.0628 0.7766 0.0491 0.048 Uiso 0.660(5) 1 calc R U P C 1
C3A C 0.0725(7) 0.7884(6) 0.1366(4) 0.0412(14) Uani 0.660(5) 1 d D U P C 1
H3A H 0.1303 0.7169 0.1485 0.049 Uiso 0.660(5) 1 calc R U P C 1
C4A C 0.1027(9) 0.8575(5) 0.1781(5) 0.0414(13) Uani 0.660(5) 1 d D U P C 1
H4A H 0.1815 0.8341 0.2186 0.050 Uiso 0.660(5) 1 calc R U P C 1
C5A C 0.0162(7) 0.9614(5) 0.1597(4) 0.0423(13) Uani 0.660(5) 1 d D U P C 1
H5A H 0.0359 1.0096 0.1877 0.051 Uiso 0.660(5) 1 calc R U P C 1
C6A C -0.0990(7) 0.9954(5) 0.1008(3) 0.0390(13) Uani 0.660(5) 1 d D U P C 1
H6A H -0.1583 1.0665 0.0890 0.047 Uiso 0.660(5) 1 calc R U P C 1
C7A C -0.2509(8) 0.9639(5) -0.0045(4) 0.0495(17) Uani 0.660(5) 1 d D U P C 1
H7A1 H -0.3448 0.9750 0.0250 0.074 Uiso 0.660(5) 1 calc R U P C 1
H7A2 H -0.2406 0.9113 -0.0382 0.074 Uiso 0.660(5) 1 calc R U P C 1
H7A3 H -0.2481 1.0298 -0.0424 0.074 Uiso 0.660(5) 1 calc R U P C 1
C1B C -0.1166(10) 0.9540(7) 0.0854(5) 0.0377(16) Uani 0.340(5) 1 d D U P C 2
C2B C -0.0992(11) 0.8662(8) 0.0547(5) 0.0373(17) Uani 0.340(5) 1 d D U P C 2
H2BA H -0.1637 0.8686 0.0110 0.045 Uiso 0.340(5) 1 calc R U P C 2
C3B C 0.0112(12) 0.7740(7) 0.0863(7) 0.0409(18) Uani 0.340(5) 1 d D U P C 2
H3B H 0.0207 0.7142 0.0640 0.049 Uiso 0.340(5) 1 calc R U P C 2
C4B C 0.1078(15) 0.7678(11) 0.1500(8) 0.0400(17) Uani 0.340(5) 1 d D U P C 2
H4B H 0.1838 0.7049 0.1717 0.048 Uiso 0.340(5) 1 calc R U P C 2
C5B C 0.0887(14) 0.8571(9) 0.1806(9) 0.0410(17) Uani 0.340(5) 1 d D U P C 2
H5B H 0.1529 0.8555 0.2242 0.049 Uiso 0.340(5) 1 calc R U P C 2
C6B C -0.0225(13) 0.9488(9) 0.1487(7) 0.0386(16) Uani 0.340(5) 1 d D U P C 2
H6B H -0.0336 1.0088 0.1711 0.046 Uiso 0.340(5) 1 calc R U P C 2
C7B C -0.2350(13) 1.0529(8) 0.0511(7) 0.048(3) Uani 0.340(5) 1 d D U P C 2
H7B1 H -0.2698 1.0906 0.0966 0.071 Uiso 0.340(5) 1 calc R U P C 2
H7B2 H -0.3168 1.0366 0.0293 0.071 Uiso 0.340(5) 1 calc R U P C 2
H7B3 H -0.1964 1.0965 0.0047 0.071 Uiso 0.340(5) 1 calc R U P C 2


_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 2.160(3) . ?
U1 O3 2.161(3) . ?
U1 N3 2.404(4) . ?
U1 N6 2.407(4) . ?
U1 N1 2.561(4) . ?
U1 N10 2.615(3) . ?
U1 N2 2.610(3) . ?
U1 N9 2.655(3) . ?
O1 C3 1.352(6) . ?
O1 C2 1.435(4) . ?
O1 C2' 1.440(5) . ?
O2 C4 1.323(5) . ?
O3 C18 1.325(4) . ?
O4 C22 1.359(5) . ?
O4 C23 1.434(4) . ?
N1 C9 1.281(5) . ?
N1 C10 1.519(5) . ?
N1 C10' 1.522(5) . ?
N2 C16 1.273(5) . ?
N2 C15' 1.520(5) . ?
N2 C15 1.524(5) . ?
N3 N4 1.126(5) . ?
N4 N5 1.167(6) . ?
N6 N7 1.175(5) . ?
N7 N8 1.153(4) . ?
N9 C29 1.339(5) . ?
N9 C25 1.344(4) . ?
N10 C34 1.341(5) . ?
N10 C30 1.350(5) . ?
C1 C2 1.497(6) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C1' C2' 1.495(6) . ?
C1' H1'1 0.9800 . ?
C1' H1'2 0.9800 . ?
C1' H1'3 0.9800 . ?
C2' H2'1 0.9900 . ?
C2' H2'2 0.9900 . ?
C3 C5 1.382(7) . ?
C3 C4 1.408(6) . ?
C4 C8 1.382(7) . ?
C5 C6 1.361(8) . ?
C5 H5 0.9500 . ?
C6 C7 1.380(7) . ?
C6 H6 0.9500 . ?
C7 C8 1.409(6) . ?
C7 H7 0.9500 . ?
C8 C9 1.453(6) . ?
C9 H9 0.9500 . ?
C10 C15 1.527(7) . ?
C10 C11 1.525(7) . ?
C10 H10 1.0000 . ?
C11 C12 1.516(4) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C13 1.517(4) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C14 1.518(4) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C15 1.531(8) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 H15 1.0000 . ?
C10' C15' 1.527(7) . ?
C10' C11' 1.54(2) . ?
C10' H10' 1.0000 . ?
C11' C12' 1.517(5) . ?
C11' H11C 0.9900 . ?
C11' H11D 0.9900 . ?
C12' C13' 1.517(5) . ?
C12' H12C 0.9900 . ?
C12' H12D 0.9900 . ?
C13' C14' 1.517(5) . ?
C13' H13C 0.9900 . ?
C13' H13D 0.9900 . ?
C14' C15' 1.524(8) . ?
C14' H14C 0.9900 . ?
C14' H14D 0.9900 . ?
C15' H15' 1.0000 . ?
C16 C17 1.440(6) . ?
C16 H16 0.9500 . ?
C17 C18 1.398(5) . ?
C17 C19 1.404(5) . ?
C18 C22 1.419(5) . ?
C19 C20 1.372(6) . ?
C19 H19 0.9500 . ?
C20 C21 1.385(6) . ?
C20 H20 0.9500 . ?
C21 C22 1.385(5) . ?
C21 H21 0.9500 . ?
C23 C24 1.495(5) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 C26 1.379(6) . ?
C25 H25 0.9500 . ?
C26 C27 1.369(6) . ?
C26 H26 0.9500 . ?
C27 C28 1.386(6) . ?
C27 H27 0.9500 . ?
C28 C29 1.377(6) . ?
C28 H28 0.9500 . ?
C29 H29 0.9500 . ?
C30 C31 1.374(6) . ?
C30 H30 0.9500 . ?
C31 C32 1.350(7) . ?
C31 H31 0.9500 . ?
C32 C33 1.377(6) . ?
C32 H32 0.9500 . ?
C33 C34 1.385(6) . ?
C33 H33 0.9500 . ?
C34 H34 0.9500 . ?
C1A C2A 1.371(6) . ?
C1A C6A 1.372(6) . ?
C1A C7A 1.489(8) . ?
C2A C3A 1.387(4) . ?
C2A H2AA 0.9500 . ?
C3A C4A 1.385(4) . ?
C3A H3A 0.9500 . ?
C4A C5A 1.388(4) . ?
C4A H4A 0.9500 . ?
C5A C6A 1.387(4) . ?
C5A H5A 0.9500 . ?
C6A H6A 0.9500 . ?
C7A H7A1 0.9800 . ?
C7A H7A2 0.9800 . ?
C7A H7A3 0.9800 . ?
C1B C2B 1.370(6) . ?
C1B C6B 1.371(6) . ?
C1B C7B 1.488(9) . ?
C2B C3B 1.387(5) . ?
C2B H2BA 0.9500 . ?
C3B C4B 1.386(5) . ?
C3B H3B 0.9500 . ?
C4B C5B 1.386(5) . ?
C4B H4B 0.9500 . ?
C5B C6B 1.387(4) . ?
C5B H5B 0.9500 . ?
C6B H6B 0.9500 . ?
C7B H7B1 0.9800 . ?
C7B H7B2 0.9800 . ?
C7B H7B3 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 U1 O3 152.86(11) . . ?
O2 U1 N3 87.66(12) . . ?
O3 U1 N3 96.04(12) . . ?
O2 U1 N6 97.46(12) . . ?
O3 U1 N6 92.85(11) . . ?
N3 U1 N6 149.56(12) . . ?
O2 U1 N1 71.26(11) . . ?
O3 U1 N1 135.79(10) . . ?
N3 U1 N1 77.19(13) . . ?
N6 U1 N1 76.17(12) . . ?
O2 U1 N10 77.75(11) . . ?
O3 U1 N10 81.61(11) . . ?
N3 U1 N10 137.70(11) . . ?
N6 U1 N10 72.40(11) . . ?
N1 U1 N10 131.92(12) . . ?
O2 U1 N2 135.50(11) . . ?
O3 U1 N2 70.76(10) . . ?
N3 U1 N2 73.88(12) . . ?
N6 U1 N2 81.79(12) . . ?
N1 U1 N2 65.36(11) . . ?
N10 U1 N2 140.97(10) . . ?
O2 U1 N9 79.52(10) . . ?
O3 U1 N9 76.40(10) . . ?
N3 U1 N9 70.89(11) . . ?
N6 U1 N9 139.55(11) . . ?
N1 U1 N9 137.18(11) . . ?
N10 U1 N9 67.52(10) . . ?
N2 U1 N9 128.12(10) . . ?
C3 O1 C2 113.8(4) . . ?
C3 O1 C2' 128.0(9) . . ?
C4 O2 U1 146.9(3) . . ?
C18 O3 U1 147.6(2) . . ?
C22 O4 C23 116.9(3) . . ?
C9 N1 C10 118.6(4) . . ?
C9 N1 C10' 108.6(6) . . ?
C9 N1 U1 128.2(3) . . ?
C10 N1 U1 113.1(3) . . ?
C10' N1 U1 115.0(6) . . ?
C16 N2 C15' 122.8(6) . . ?
C16 N2 C15 114.7(4) . . ?
C16 N2 U1 126.8(3) . . ?
C15' N2 U1 107.8(6) . . ?
C15 N2 U1 116.8(3) . . ?
N4 N3 U1 138.5(3) . . ?
N3 N4 N5 177.0(5) . . ?
N7 N6 U1 137.0(3) . . ?
N8 N7 N6 178.0(4) . . ?
C29 N9 C25 117.4(3) . . ?
C29 N9 U1 120.8(2) . . ?
C25 N9 U1 121.8(2) . . ?
C34 N10 C30 117.1(3) . . ?
C34 N10 U1 120.9(3) . . ?
C30 N10 U1 122.0(3) . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O1 C2 C1 104.0(4) . . ?
O1 C2 H2A 111.0 . . ?
C1 C2 H2A 111.0 . . ?
O1 C2 H2B 111.0 . . ?
C1 C2 H2B 111.0 . . ?
H2A C2 H2B 109.0 . . ?
C2' C1' H1'1 109.5 . . ?
C2' C1' H1'2 109.5 . . ?
H1'1 C1' H1'2 109.5 . . ?
C2' C1' H1'3 109.5 . . ?
H1'1 C1' H1'3 109.5 . . ?
H1'2 C1' H1'3 109.5 . . ?
O1 C2' C1' 106.4(6) . . ?
O1 C2' H2'1 110.5 . . ?
C1' C2' H2'1 110.5 . . ?
O1 C2' H2'2 110.5 . . ?
C1' C2' H2'2 110.5 . . ?
H2'1 C2' H2'2 108.6 . . ?
O1 C3 C5 125.6(4) . . ?
O1 C3 C4 114.7(4) . . ?
C5 C3 C4 119.7(5) . . ?
O2 C4 C8 121.4(4) . . ?
O2 C4 C3 119.5(4) . . ?
C8 C4 C3 119.1(4) . . ?
C6 C5 C3 121.3(5) . . ?
C6 C5 H5 119.3 . . ?
C3 C5 H5 119.3 . . ?
C5 C6 C7 119.8(5) . . ?
C5 C6 H6 120.1 . . ?
C7 C6 H6 120.1 . . ?
C6 C7 C8 120.2(5) . . ?
C6 C7 H7 119.9 . . ?
C8 C7 H7 119.9 . . ?
C4 C8 C7 119.7(4) . . ?
C4 C8 C9 123.2(4) . . ?
C7 C8 C9 116.7(5) . . ?
N1 C9 C8 127.5(4) . . ?
N1 C9 H9 116.2 . . ?
C8 C9 H9 116.2 . . ?
N1 C10 C15 106.6(4) . . ?
N1 C10 C11 115.4(4) . . ?
C15 C10 C11 111.7(4) . . ?
N1 C10 H10 107.6 . . ?
C15 C10 H10 107.6 . . ?
C11 C10 H10 107.6 . . ?
C12 C11 C10 112.0(5) . . ?
C12 C11 H11A 109.2 . . ?
C10 C11 H11A 109.2 . . ?
C12 C11 H11B 109.2 . . ?
C10 C11 H11B 109.2 . . ?
H11A C11 H11B 107.9 . . ?
C11 C12 C13 108.7(5) . . ?
C11 C12 H12A 110.0 . . ?
C13 C12 H12A 110.0 . . ?
C11 C12 H12B 110.0 . . ?
C13 C12 H12B 110.0 . . ?
H12A C12 H12B 108.3 . . ?
C12 C13 C14 110.0(5) . . ?
C12 C13 H13A 109.7 . . ?
C14 C13 H13A 109.7 . . ?
C12 C13 H13B 109.7 . . ?
C14 C13 H13B 109.7 . . ?
H13A C13 H13B 108.2 . . ?
C13 C14 C15 113.7(5) . . ?
C13 C14 H14A 108.8 . . ?
C15 C14 H14A 108.8 . . ?
C13 C14 H14B 108.8 . . ?
C15 C14 H14B 108.8 . . ?
H14A C14 H14B 107.7 . . ?
N2 C15 C10 105.7(4) . . ?
N2 C15 C14 113.0(4) . . ?
C10 C15 C14 110.6(4) . . ?
N2 C15 H15 109.1 . . ?
C10 C15 H15 109.1 . . ?
C14 C15 H15 109.1 . . ?
N1 C10' C15' 100.7(8) . . ?
N1 C10' C11' 108.5(10) . . ?
C15' C10' C11' 110.7(12) . . ?
N1 C10' H10' 112.1 . . ?
C15' C10' H10' 112.1 . . ?
C11' C10' H10' 112.1 . . ?
C12' C11' C10' 111.6(13) . . ?
C12' C11' H11C 109.3 . . ?
C10' C11' H11C 109.3 . . ?
C12' C11' H11D 109.3 . . ?
C10' C11' H11D 109.3 . . ?
H11C C11' H11D 108.0 . . ?
C11' C12' C13' 111.7(14) . . ?
C11' C12' H12C 109.3 . . ?
C13' C12' H12C 109.3 . . ?
C11' C12' H12D 109.3 . . ?
C13' C12' H12D 109.3 . . ?
H12C C12' H12D 107.9 . . ?
C12' C13' C14' 112.7(14) . . ?
C12' C13' H13C 109.1 . . ?
C14' C13' H13C 109.1 . . ?
C12' C13' H13D 109.1 . . ?
C14' C13' H13D 109.1 . . ?
H13C C13' H13D 107.8 . . ?
C13' C14' C15' 109.5(12) . . ?
C13' C14' H14C 109.8 . . ?
C15' C14' H14C 109.8 . . ?
C13' C14' H14D 109.8 . . ?
C15' C14' H14D 109.8 . . ?
H14C C14' H14D 108.2 . . ?
N2 C15' C10' 102.5(9) . . ?
N2 C15' C14' 110.0(9) . . ?
C10' C15' C14' 114.7(12) . . ?
N2 C15' H15' 109.8 . . ?
C10' C15' H15' 109.8 . . ?
C14' C15' H15' 109.8 . . ?
N2 C16 C17 128.7(4) . . ?
N2 C16 H16 115.7 . . ?
C17 C16 H16 115.7 . . ?
C18 C17 C19 119.6(4) . . ?
C18 C17 C16 123.0(3) . . ?
C19 C17 C16 117.3(4) . . ?
O3 C18 C17 121.3(3) . . ?
O3 C18 C22 119.7(3) . . ?
C17 C18 C22 119.1(3) . . ?
C20 C19 C17 120.6(4) . . ?
C20 C19 H19 119.7 . . ?
C17 C19 H19 119.7 . . ?
C19 C20 C21 120.3(4) . . ?
C19 C20 H20 119.9 . . ?
C21 C20 H20 119.9 . . ?
C20 C21 C22 120.6(4) . . ?
C20 C21 H21 119.7 . . ?
C22 C21 H21 119.7 . . ?
O4 C22 C21 126.0(4) . . ?
O4 C22 C18 114.3(3) . . ?
C21 C22 C18 119.8(4) . . ?
O4 C23 C24 106.3(3) . . ?
O4 C23 H23A 110.5 . . ?
C24 C23 H23A 110.5 . . ?
O4 C23 H23B 110.5 . . ?
C24 C23 H23B 110.5 . . ?
H23A C23 H23B 108.7 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
N9 C25 C26 122.6(4) . . ?
N9 C25 H25 118.7 . . ?
C26 C25 H25 118.7 . . ?
C27 C26 C25 119.6(4) . . ?
C27 C26 H26 120.2 . . ?
C25 C26 H26 120.2 . . ?
C26 C27 C28 118.5(4) . . ?
C26 C27 H27 120.8 . . ?
C28 C27 H27 120.8 . . ?
C29 C28 C27 118.8(4) . . ?
C29 C28 H28 120.6 . . ?
C27 C28 H28 120.6 . . ?
N9 C29 C28 123.2(4) . . ?
N9 C29 H29 118.4 . . ?
C28 C29 H29 118.4 . . ?
N10 C30 C31 123.3(4) . . ?
N10 C30 H30 118.4 . . ?
C31 C30 H30 118.4 . . ?
C32 C31 C30 119.3(4) . . ?
C32 C31 H31 120.4 . . ?
C30 C31 H31 120.4 . . ?
C31 C32 C33 118.8(4) . . ?
C31 C32 H32 120.6 . . ?
C33 C32 H32 120.6 . . ?
C32 C33 C34 119.7(4) . . ?
C32 C33 H33 120.2 . . ?
C34 C33 H33 120.2 . . ?
N10 C34 C33 121.9(4) . . ?
N10 C34 H34 119.1 . . ?
C33 C34 H34 119.1 . . ?
C2A C1A C6A 119.2(6) . . ?
C2A C1A C7A 120.6(5) . . ?
C6A C1A C7A 120.3(4) . . ?
C1A C2A C3A 121.4(5) . . ?
C1A C2A H2AA 119.3 . . ?
C3A C2A H2AA 119.3 . . ?
C4A C3A C2A 119.6(7) . . ?
C4A C3A H3A 120.2 . . ?
C2A C3A H3A 120.2 . . ?
C3A C4A C5A 119.0(8) . . ?
C3A C4A H4A 120.5 . . ?
C5A C4A H4A 120.5 . . ?
C6A C5A C4A 120.4(6) . . ?
C6A C5A H5A 119.8 . . ?
C4A C5A H5A 119.8 . . ?
C1A C6A C5A 120.4(5) . . ?
C1A C6A H6A 119.8 . . ?
C5A C6A H6A 119.8 . . ?
C1A C7A H7A1 109.5 . . ?
C1A C7A H7A2 109.5 . . ?
H7A1 C7A H7A2 109.5 . . ?
C1A C7A H7A3 109.5 . . ?
H7A1 C7A H7A3 109.5 . . ?
H7A2 C7A H7A3 109.5 . . ?
C2B C1B C6B 118.4(8) . . ?
C2B C1B C7B 120.9(6) . . ?
C6B C1B C7B 120.6(5) . . ?
C1B C2B C3B 121.1(7) . . ?
C1B C2B H2BA 119.4 . . ?
C3B C2B H2BA 119.4 . . ?
C4B C3B C2B 121.1(10) . . ?
C4B C3B H3B 119.5 . . ?
C2B C3B H3B 119.5 . . ?
C5B C4B C3B 117.2(14) . . ?
C5B C4B H4B 121.4 . . ?
C3B C4B H4B 121.4 . . ?
C4B C5B C6B 121.2(11) . . ?
C4B C5B H5B 119.4 . . ?
C6B C5B H5B 119.4 . . ?
C1B C6B C5B 121.0(8) . . ?
C1B C6B H6B 119.5 . . ?
C5B C6B H6B 119.5 . . ?
C1B C7B H7B1 109.5 . . ?
C1B C7B H7B2 109.5 . . ?
H7B1 C7B H7B2 109.5 . . ?
C1B C7B H7B3 109.5 . . ?
H7B1 C7B H7B3 109.5 . . ?
H7B2 C7B H7B3 109.5 . . ?

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
C3 O1 C2 C1 176.5(5) . . . . ?
C3 O1 C2' C1' 104.1(14) . . . . ?
C2 O1 C3 C5 -1.2(7) . . . . ?
C2' O1 C3 C5 -33.3(9) . . . . ?
C2 O1 C3 C4 177.7(4) . . . . ?
C2' O1 C3 C4 145.6(7) . . . . ?
U1 O2 C4 C8 -7.5(7) . . . . ?
U1 O2 C4 C3 173.1(3) . . . . ?
O1 C3 C4 O2 -1.6(6) . . . . ?
C5 C3 C4 O2 177.3(4) . . . . ?
O1 C3 C4 C8 179.0(4) . . . . ?
C5 C3 C4 C8 -2.1(6) . . . . ?
O1 C3 C5 C6 180.0(5) . . . . ?
C4 C3 C5 C6 1.2(7) . . . . ?
C3 C5 C6 C7 0.4(8) . . . . ?
C5 C6 C7 C8 -1.1(7) . . . . ?
O2 C4 C8 C7 -178.0(4) . . . . ?
C3 C4 C8 C7 1.4(6) . . . . ?
O2 C4 C8 C9 -5.0(7) . . . . ?
C3 C4 C8 C9 174.3(4) . . . . ?
C6 C7 C8 C4 0.2(7) . . . . ?
C6 C7 C8 C9 -173.2(4) . . . . ?
C10 N1 C9 C8 -166.4(5) . . . . ?
C10' N1 C9 C8 155.3(8) . . . . ?
U1 N1 C9 C8 9.0(8) . . . . ?
C4 C8 C9 N1 2.1(8) . . . . ?
C7 C8 C9 N1 175.2(5) . . . . ?
C9 N1 C10 C15 -126.6(5) . . . . ?
U1 N1 C10 C15 57.4(4) . . . . ?
C9 N1 C10 C11 -2.0(7) . . . . ?
U1 N1 C10 C11 -178.0(4) . . . . ?
N1 C10 C11 C12 -178.2(5) . . . . ?
C15 C10 C11 C12 -56.3(6) . . . . ?
C10 C11 C12 C13 60.2(7) . . . . ?
C11 C12 C13 C14 -59.1(7) . . . . ?
C12 C13 C14 C15 56.3(7) . . . . ?
C16 N2 C15 C10 -155.6(4) . . . . ?
U1 N2 C15 C10 38.2(5) . . . . ?
C16 N2 C15 C14 -34.5(6) . . . . ?
U1 N2 C15 C14 159.3(4) . . . . ?
N1 C10 C15 N2 -60.5(5) . . . . ?
C11 C10 C15 N2 172.7(4) . . . . ?
N1 C10 C15 C14 176.9(4) . . . . ?
C11 C10 C15 C14 50.0(6) . . . . ?
C13 C14 C15 N2 -169.5(5) . . . . ?
C13 C14 C15 C10 -51.2(7) . . . . ?
C9 N1 C10' C15' 158.2(7) . . . . ?
U1 N1 C10' C15' -50.6(10) . . . . ?
C9 N1 C10' C11' 42.0(13) . . . . ?
U1 N1 C10' C11' -166.8(10) . . . . ?
N1 C10' C11' C12' 161.0(13) . . . . ?
C15' C10' C11' C12' 51.4(17) . . . . ?
C10' C11' C12' C13' -54(2) . . . . ?
C11' C12' C13' C14' 57(2) . . . . ?
C12' C13' C14' C15' -55(2) . . . . ?
C16 N2 C15' C10' 133.1(7) . . . . ?
U1 N2 C15' C10' -64.1(9) . . . . ?
C16 N2 C15' C14' 10.7(15) . . . . ?
U1 N2 C15' C14' 173.5(10) . . . . ?
N1 C10' C15' N2 74.2(11) . . . . ?
C11' C10' C15' N2 -171.2(10) . . . . ?
N1 C10' C15' C14' -166.6(10) . . . . ?
C11' C10' C15' C14' -52.0(14) . . . . ?
C13' C14' C15' N2 168.0(12) . . . . ?
C13' C14' C15' C10' 53.1(18) . . . . ?
C15' N2 C16 C17 145.9(8) . . . . ?
C15 N2 C16 C17 -178.1(4) . . . . ?
U1 N2 C16 C17 -13.5(7) . . . . ?
N2 C16 C17 C18 1.3(7) . . . . ?
N2 C16 C17 C19 -174.9(4) . . . . ?
U1 O3 C18 C17 6.3(7) . . . . ?
U1 O3 C18 C22 -173.0(3) . . . . ?
C19 C17 C18 O3 -178.9(4) . . . . ?
C16 C17 C18 O3 4.9(6) . . . . ?
C19 C17 C18 C22 0.4(6) . . . . ?
C16 C17 C18 C22 -175.8(4) . . . . ?
C18 C17 C19 C20 -0.3(6) . . . . ?
C16 C17 C19 C20 176.1(4) . . . . ?
C17 C19 C20 C21 -0.2(7) . . . . ?
C19 C20 C21 C22 0.7(7) . . . . ?
C23 O4 C22 C21 0.6(6) . . . . ?
C23 O4 C22 C18 -180.0(4) . . . . ?
C20 C21 C22 O4 178.7(4) . . . . ?
C20 C21 C22 C18 -0.7(7) . . . . ?
O3 C18 C22 O4 0.0(5) . . . . ?
C17 C18 C22 O4 -179.3(4) . . . . ?
O3 C18 C22 C21 179.4(4) . . . . ?
C17 C18 C22 C21 0.1(6) . . . . ?
C22 O4 C23 C24 176.9(4) . . . . ?
C29 N9 C25 C26 0.1(5) . . . . ?
U1 N9 C25 C26 180.0(3) . . . . ?
N9 C25 C26 C27 0.0(6) . . . . ?
C25 C26 C27 C28 -0.3(6) . . . . ?
C26 C27 C28 C29 0.5(6) . . . . ?
C25 N9 C29 C28 0.1(6) . . . . ?
U1 N9 C29 C28 -179.7(3) . . . . ?
C27 C28 C29 N9 -0.4(6) . . . . ?
C34 N10 C30 C31 -0.6(6) . . . . ?
U1 N10 C30 C31 176.5(3) . . . . ?
N10 C30 C31 C32 0.0(7) . . . . ?
C30 C31 C32 C33 0.2(7) . . . . ?
C31 C32 C33 C34 0.2(7) . . . . ?
C30 N10 C34 C33 0.9(6) . . . . ?
U1 N10 C34 C33 -176.2(3) . . . . ?
C32 C33 C34 N10 -0.8(7) . . . . ?
C6A C1A C2A C3A -0.3(3) . . . . ?
C7A C1A C2A C3A 179.8(3) . . . . ?
C1A C2A C3A C4A -0.2(3) . . . . ?
C2A C3A C4A C5A 0.2(5) . . . . ?
C3A C4A C5A C6A 0.1(7) . . . . ?
C2A C1A C6A C5A 0.7(5) . . . . ?
C7A C1A C6A C5A -179.4(4) . . . . ?
C4A C5A C6A C1A -0.6(7) . . . . ?
C6B C1B C2B C3B -0.2(3) . . . . ?
C7B C1B C2B C3B 179.8(3) . . . . ?
C1B C2B C3B C4B -0.2(3) . . . . ?
C2B C3B C4B C5B 0.3(6) . . . . ?
C3B C4B C5B C6B 0.0(8) . . . . ?
C2B C1B C6B C5B 0.5(6) . . . . ?
C7B C1B C6B C5B -179.5(5) . . . . ?
C4B C5B C6B C1B -0.4(9) . . . . ?

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
C2' H2'1 N5 0.99 2.24 2.872(13) 120.3 1_455
C9 H9 N5 0.95 2.58 3.484(7) 158.9 2_676
C10 H10 N6 1.00 2.66 3.301(6) 122.4 .
C14 H14B N8 0.99 2.63 3.615(8) 172.3 1_655
C10' H10' N4 1.00 2.54 3.249(17) 127.6 .
C10' H10' N5 1.00 2.66 3.510(17) 143.6 .
C11' H11C N5 0.99 2.38 3.21(2) 140.5 2_676
C15' H15' N6 1.00 2.60 3.314(16) 128.5 .
C25 H25 O1 0.95 2.51 3.426(5) 162.3 .
C25 H25 O2 0.95 2.60 3.170(5) 119.2 .
C29 H29 O3 0.95 2.60 3.107(5) 113.8 .
C30 H30 O2 0.95 2.61 3.116(5) 113.9 .
C31 H31 N3 0.95 2.56 3.504(6) 175.3 1_455
C31 H31 N4 0.95 2.66 3.561(6) 159.6 1_455
C34 H34 O3 0.95 2.55 3.164(5) 122.8 .
C34 H34 O4 0.95 2.51 3.458(5) 173.8 .

_refine_diff_density_max         2.478
_refine_diff_density_min         -1.960
_refine_diff_density_rms         0.141

####################################################################### 
# 
# 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_16038
_database_code_depnum_ccdc_archive 'CCDC 1533058'
_audit_update_record             
;
2017-02-16 deposited with the CCDC.
2017-03-23 downloaded from the CCDC.
;
#BCS-004-083

_vrf_PLAT973_Alert_2_B           
; 
Problem:   Check calcd positive residual density on U1  1.62eA-3
Response:  The atom assignment is correct.  No evidence of twinning 
           was observed.
;

_audit_creation_method           SHELXL-2014/7
#_shelx_SHELXL_version_number      '2014/7' 
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C29 H33 N3 O6 U, C D Cl3'
_chemical_formula_sum            'C30 H33 Cl3 D N3 O6 U'
_chemical_formula_weight         877.99

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'
D D 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 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'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   27.313(4)
_cell_length_b                   9.2102(13)
_cell_length_c                   26.618(4)
_cell_angle_alpha                90
_cell_angle_beta                 97.694(2)
_cell_angle_gamma                90
_cell_volume                     6635.7(17)
_cell_formula_units_Z            8
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    9924
_cell_measurement_theta_min      2.30
_cell_measurement_theta_max      24.82

_exptl_crystal_description       plate
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.758
_exptl_crystal_F_000             3408
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.310
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    5.179
_shelx_estimated_absorpt_T_min   0.297
_shelx_estimated_absorpt_T_max   0.860
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.297
_exptl_absorpt_correction_T_max  0.860
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2015c)'
#_exptl_absorpt_special_details    ? 
_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            76032
_diffrn_reflns_av_unetI/netI     0.0301
_diffrn_reflns_av_R_equivalents  0.0561
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_theta_min         1.505
_diffrn_reflns_theta_max         28.359
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             8293
_reflns_number_gt                6454
_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       'APEX2 (Bruker, 2007)'
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015a)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015b)'
_computing_molecular_graphics    'Mercury (CCDC, 2016)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2015b)'
_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)+(0.0611P)²+9.5000P] 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         8293
_refine_ls_number_parameters     433
_refine_ls_number_restraints     38
_refine_ls_R_factor_all          0.0505
_refine_ls_R_factor_gt           0.0355
_refine_ls_wR_factor_ref         0.1016
_refine_ls_wR_factor_gt          0.0931
_refine_ls_goodness_of_fit_ref   0.977
_refine_ls_restrained_S_all      0.997
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.26346(2) 0.44179(2) 0.63797(2) 0.04415(7) Uani 1 1 d . . . . .
O1 O 0.28858(14) 0.6185(4) 0.65195(12) 0.0590(8) Uani 1 1 d . . . . .
O2 O 0.23901(12) 0.2649(3) 0.62554(11) 0.0541(8) Uani 1 1 d . . . . .
O3 O 0.32722(12) 0.3785(4) 0.59653(11) 0.0563(8) Uani 1 1 d . . . . .
O4 O 0.18671(12) 0.5226(4) 0.64607(13) 0.0574(8) Uani 1 1 d . . . . .
O5 O 0.35178(14) 0.2968(4) 0.50811(12) 0.0667(9) Uani 1 1 d . . . . .
O6 O 0.09663(15) 0.5683(5) 0.59874(17) 0.0796(12) Uani 1 1 d . . . . .
N1 N 0.33326(16) 0.3309(5) 0.69916(13) 0.0635(11) Uani 1 1 d D . . . .
N2 N 0.24656(16) 0.4063(5) 0.72937(14) 0.0563(10) Uani 1 1 d D . . . .
C1 C 0.35416(16) 0.2602(5) 0.59561(17) 0.0484(10) Uani 1 1 d . . . . .
C2 C 0.36985(18) 0.2153(6) 0.54911(18) 0.0550(11) Uani 1 1 d . . . . .
C3 C 0.4001(2) 0.0973(6) 0.5478(2) 0.0655(13) Uani 1 1 d . . . . .
H3 H 0.4106 0.0705 0.5173 0.079 Uiso 1 1 calc R U . . .
C4 C 0.4155(2) 0.0168(7) 0.5912(2) 0.0735(15) Uani 1 1 d . . . . .
H4 H 0.4352 -0.0649 0.5895 0.088 Uiso 1 1 calc R U . . .
C5 C 0.4014(2) 0.0587(6) 0.6367(2) 0.0687(15) Uani 1 1 d . . . . .
H5 H 0.4121 0.0058 0.6658 0.082 Uiso 1 1 calc R U . . .
C6 C 0.37070(18) 0.1820(6) 0.63957(18) 0.0578(11) Uani 1 1 d . . . . .
C7 C 0.3618(2) 0.2293(7) 0.68904(19) 0.0751(16) Uani 1 1 d . . . . .
H7 H 0.3787 0.1802 0.7166 0.090 Uiso 1 1 calc R U . . .
C8 C 0.3350(3) 0.4064(11) 0.7499(3) 0.058(3) Uani 0.608(13) 1 d D . P A 1
H8 H 0.3340 0.5116 0.7443 0.070 Uiso 0.608(13) 1 calc R U P A 1
C9 C 0.3816(5) 0.370(4) 0.7879(5) 0.0707(15) Uani 0.608(13) 1 d D . P A 1
H9A H 0.3830 0.2660 0.7946 0.085 Uiso 0.608(13) 1 calc R U P A 1
H9B H 0.4112 0.3975 0.7739 0.085 Uiso 0.608(13) 1 calc R U P A 1
C10 C 0.3784(5) 0.4531(19) 0.8373(4) 0.079(4) Uani 0.608(13) 1 d D . P A 1
H10A H 0.4063 0.4279 0.8623 0.095 Uiso 0.608(13) 1 calc R U P A 1
H10B H 0.3796 0.5567 0.8310 0.095 Uiso 0.608(13) 1 calc R U P A 1
C11 C 0.3307(5) 0.4152(17) 0.8572(6) 0.083(5) Uani 0.608(13) 1 d D . P A 1
H11A H 0.3287 0.4696 0.8880 0.099 Uiso 0.608(13) 1 calc R U P A 1
H11B H 0.3310 0.3127 0.8657 0.099 Uiso 0.608(13) 1 calc R U P A 1
C12 C 0.2848(7) 0.448(4) 0.8190(5) 0.067(2) Uani 0.608(13) 1 d D . P A 1
H12A H 0.2829 0.5510 0.8116 0.080 Uiso 0.608(13) 1 calc R U P A 1
H12B H 0.2552 0.4198 0.8330 0.080 Uiso 0.608(13) 1 calc R U P A 1
C13 C 0.2885(3) 0.3609(12) 0.7695(3) 0.062(3) Uani 0.608(13) 1 d D . P A 1
H13 H 0.2880 0.2560 0.7756 0.074 Uiso 0.608(13) 1 calc R U P A 1
C8' C 0.3285(5) 0.3232(15) 0.7553(2) 0.049(3) Uani 0.392(13) 1 d D . P A 2
H8' H 0.3183 0.2260 0.7647 0.059 Uiso 0.392(13) 1 calc R U P A 2
C9' C 0.3788(7) 0.366(7) 0.7861(8) 0.0707(15) Uani 0.392(13) 1 d D . P A 2
H9C H 0.4037 0.2953 0.7803 0.085 Uiso 0.392(13) 1 calc R U P A 2
H9D H 0.3891 0.4599 0.7747 0.085 Uiso 0.392(13) 1 calc R U P A 2
C10' C 0.3743(8) 0.373(2) 0.8430(7) 0.070(5) Uani 0.392(13) 1 d D . P A 2
H10C H 0.3652 0.2785 0.8546 0.084 Uiso 0.392(13) 1 calc R U P A 2
H10D H 0.4060 0.3996 0.8617 0.084 Uiso 0.392(13) 1 calc R U P A 2
C11' C 0.3358(9) 0.483(2) 0.8531(10) 0.078(7) Uani 0.392(13) 1 d D . P A 2
H11C H 0.3452 0.5789 0.8422 0.094 Uiso 0.392(13) 1 calc R U P A 2
H11D H 0.3337 0.4877 0.8891 0.094 Uiso 0.392(13) 1 calc R U P A 2
C12' C 0.2854(10) 0.441(6) 0.8242(7) 0.067(2) Uani 0.392(13) 1 d D . P A 2
H12C H 0.2605 0.5113 0.8299 0.080 Uiso 0.392(13) 1 calc R U P A 2
H12D H 0.2753 0.3462 0.8354 0.080 Uiso 0.392(13) 1 calc R U P A 2
C13' C 0.2921(3) 0.4357(15) 0.7671(4) 0.047(3) Uani 0.392(13) 1 d D . P A 2
H13' H 0.3051 0.5304 0.7586 0.056 Uiso 0.392(13) 1 calc R U P A 2
C14 C 0.2043(2) 0.3752(6) 0.74257(19) 0.0655(13) Uani 1 1 d . . . . .
H14 H 0.2044 0.3399 0.7753 0.079 Uiso 1 1 calc R U . . .
C15 C 0.1563(2) 0.3886(6) 0.7122(2) 0.0630(13) Uani 1 1 d . . . . .
C16 C 0.1157(2) 0.3341(8) 0.7337(3) 0.0853(18) Uani 1 1 d . . . . .
H16 H 0.1206 0.2852 0.7645 0.102 Uiso 1 1 calc R U . . .
C17 C 0.0692(3) 0.3533(10) 0.7092(3) 0.104(2) Uani 1 1 d . . . . .
H17 H 0.0423 0.3139 0.7224 0.125 Uiso 1 1 calc R U . . .
C18 C 0.0622(3) 0.4317(9) 0.6645(3) 0.104(3) Uani 1 1 d . . . . .
H18 H 0.0301 0.4462 0.6488 0.124 Uiso 1 1 calc R U . . .
C19 C 0.1001(2) 0.4887(8) 0.6425(2) 0.0698(14) Uani 1 1 d . . . . .
C20 C 0.1496(2) 0.4653(5) 0.6661(2) 0.0578(12) Uani 1 1 d . . . . .
C21 C 0.3654(2) 0.2587(7) 0.45907(19) 0.0703(14) Uani 1 1 d . . . . .
H21A H 0.3407 0.2966 0.4327 0.084 Uiso 1 1 calc R U . . .
H21B H 0.3656 0.1538 0.4558 0.084 Uiso 1 1 calc R U . . .
C22 C 0.4148(2) 0.3168(8) 0.4516(2) 0.0854(18) Uani 1 1 d . . . . .
H22A H 0.4169 0.4173 0.4613 0.128 Uiso 1 1 calc R U . . .
H22B H 0.4193 0.3075 0.4166 0.128 Uiso 1 1 calc R U . . .
H22C H 0.4401 0.2629 0.4722 0.128 Uiso 1 1 calc R U . . .
C23 C 0.0485(3) 0.6163(11) 0.5763(3) 0.105(2) Uani 1 1 d . . . . .
H23A H 0.0318 0.6641 0.6017 0.126 Uiso 1 1 calc R U . . .
H23B H 0.0288 0.5334 0.5634 0.126 Uiso 1 1 calc R U . . .
C24 C 0.0538(3) 0.7168(10) 0.5351(3) 0.109(3) Uani 1 1 d . . . . .
H24A H 0.0741 0.7972 0.5479 0.164 Uiso 1 1 calc R U . . .
H24B H 0.0218 0.7517 0.5208 0.164 Uiso 1 1 calc R U . . .
H24C H 0.0690 0.6676 0.5093 0.164 Uiso 1 1 calc R U . . .
N1A N 0.23075(15) 0.5270(4) 0.54612(14) 0.0502(9) Uani 1 1 d . . . . .
C1A C 0.2462(2) 0.4652(5) 0.50522(19) 0.0548(11) Uani 1 1 d . . . . .
H1A H 0.2678 0.3870 0.5103 0.066 Uiso 1 1 calc R U . . .
C2A C 0.2317(2) 0.5116(7) 0.45634(19) 0.0644(13) Uani 1 1 d . . . . .
H2A H 0.2423 0.4635 0.4290 0.077 Uiso 1 1 calc R U . . .
C3A C 0.2013(2) 0.6301(7) 0.4488(2) 0.0724(16) Uani 1 1 d . . . . .
H3A H 0.1920 0.6659 0.4163 0.087 Uiso 1 1 calc R U . . .
C4A C 0.1849(2) 0.6955(6) 0.4898(2) 0.0667(14) Uani 1 1 d . . . . .
H4A H 0.1637 0.7749 0.4854 0.080 Uiso 1 1 calc R U . . .
C5A C 0.20037(19) 0.6410(6) 0.53761(19) 0.0619(12) Uani 1 1 d . . . . .
H5A H 0.1892 0.6857 0.5653 0.074 Uiso 1 1 calc R U . . .
Cl1B Cl 0.4330(2) 0.6704(4) 0.6623(2) 0.261(3) Uani 1 1 d . U . . .
Cl2B Cl 0.48083(14) 0.4052(6) 0.6742(2) 0.243(2) Uani 1 1 d . U . . .
Cl3B Cl 0.4657(2) 0.5348(7) 0.58029(17) 0.247(2) Uani 1 1 d . U . . .
C1B C 0.4426(3) 0.5107(10) 0.6352(3) 0.093(2) Uani 1 1 d . U . . .
D1B D 0.4107 0.4607 0.6279 0.112 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 O2 1.775(3) . ?
U1 O1 1.786(3) . ?
U1 O3 2.259(3) . ?
U1 O4 2.262(3) . ?
U1 N1 2.549(4) . ?
U1 N2 2.557(4) . ?
U1 N1A 2.609(4) . ?
O3 C1 1.317(6) . ?
O4 C20 1.317(6) . ?
O5 C2 1.362(6) . ?
O5 C21 1.447(6) . ?
O6 C19 1.369(8) . ?
O6 C23 1.439(7) . ?
N1 C7 1.269(7) . ?
N1 C8 1.515(5) . ?
N1 C8' 1.519(6) . ?
N2 C14 1.284(7) . ?
N2 C13' 1.516(6) . ?
N2 C13 1.517(6) . ?
C1 C6 1.397(6) . ?
C1 C2 1.424(6) . ?
C2 C3 1.369(7) . ?
C3 C4 1.390(8) . ?
C3 H3 0.9300 . ?
C4 C5 1.372(8) . ?
C4 H4 0.9300 . ?
C5 C6 1.420(7) . ?
C5 H5 0.9300 . ?
C6 C7 1.439(7) . ?
C7 H7 0.9300 . ?
C8 C13 1.498(9) . ?
C8 C9 1.553(12) . ?
C8 H8 0.9800 . ?
C9 C10 1.536(12) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C11 1.511(12) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C12 1.536(12) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 C13 1.554(12) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 H13 0.9800 . ?
C8' C13' 1.497(9) . ?
C8' C9' 1.554(12) . ?
C8' H8' 0.9800 . ?
C9' C10' 1.536(12) . ?
C9' H9C 0.9700 . ?
C9' H9D 0.9700 . ?
C10' C11' 1.511(12) . ?
C10' H10C 0.9700 . ?
C10' H10D 0.9700 . ?
C11' C12' 1.536(13) . ?
C11' H11C 0.9700 . ?
C11' H11D 0.9700 . ?
C12' C13' 1.554(12) . ?
C12' H12C 0.9700 . ?
C12' H12D 0.9700 . ?
C13' H13' 0.9800 . ?
C14 C15 1.450(8) . ?
C14 H14 0.9300 . ?
C15 C20 1.407(8) . ?
C15 C16 1.408(8) . ?
C16 C17 1.358(9) . ?
C16 H16 0.9300 . ?
C17 C18 1.383(11) . ?
C17 H17 0.9300 . ?
C18 C19 1.362(10) . ?
C18 H18 0.9300 . ?
C19 C20 1.428(8) . ?
C21 C22 1.491(8) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 C24 1.458(12) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
N1A C5A 1.339(6) . ?
N1A C1A 1.345(6) . ?
C1A C2A 1.377(7) . ?
C1A H1A 0.9300 . ?
C2A C3A 1.369(9) . ?
C2A H2A 0.9300 . ?
C3A C4A 1.373(8) . ?
C3A H3A 0.9300 . ?
C4A C5A 1.382(7) . ?
C4A H4A 0.9300 . ?
C5A H5A 0.9300 . ?
Cl1B C1B 1.674(9) . ?
Cl2B C1B 1.679(9) . ?
Cl3B C1B 1.684(9) . ?
C1B D1B 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 U1 O1 178.67(14) . . ?
O2 U1 O3 88.14(14) . . ?
O1 U1 O3 92.12(15) . . ?
O2 U1 O4 89.39(14) . . ?
O1 U1 O4 90.89(15) . . ?
O3 U1 O4 156.39(12) . . ?
O2 U1 N1 88.96(15) . . ?
O1 U1 N1 89.92(16) . . ?
O3 U1 N1 69.46(12) . . ?
O4 U1 N1 133.97(12) . . ?
O2 U1 N2 87.06(14) . . ?
O1 U1 N2 91.81(14) . . ?
O3 U1 N2 132.90(12) . . ?
O4 U1 N2 70.35(12) . . ?
N1 U1 N2 63.63(13) . . ?
O2 U1 N1A 91.62(13) . . ?
O1 U1 N1A 89.70(14) . . ?
O3 U1 N1A 79.03(12) . . ?
O4 U1 N1A 77.58(12) . . ?
N1 U1 N1A 148.45(13) . . ?
N2 U1 N1A 147.91(13) . . ?
C1 O3 U1 133.8(3) . . ?
C20 O4 U1 132.9(3) . . ?
C2 O5 C21 118.7(4) . . ?
C19 O6 C23 118.2(5) . . ?
C7 N1 C8 125.5(6) . . ?
C7 N1 C8' 108.1(5) . . ?
C7 N1 U1 126.0(3) . . ?
C8 N1 U1 108.5(5) . . ?
C8' N1 U1 119.5(5) . . ?
C14 N2 C13' 123.2(7) . . ?
C14 N2 C13 111.6(5) . . ?
C14 N2 U1 124.9(3) . . ?
C13' N2 U1 111.8(6) . . ?
C13 N2 U1 119.4(4) . . ?
O3 C1 C6 122.0(4) . . ?
O3 C1 C2 119.4(4) . . ?
C6 C1 C2 118.5(4) . . ?
O5 C2 C3 125.0(4) . . ?
O5 C2 C1 114.7(4) . . ?
C3 C2 C1 120.3(5) . . ?
C2 C3 C4 121.3(5) . . ?
C2 C3 H3 119.4 . . ?
C4 C3 H3 119.4 . . ?
C5 C4 C3 119.6(6) . . ?
C5 C4 H4 120.2 . . ?
C3 C4 H4 120.2 . . ?
C4 C5 C6 120.7(5) . . ?
C4 C5 H5 119.7 . . ?
C6 C5 H5 119.7 . . ?
C1 C6 C5 119.6(5) . . ?
C1 C6 C7 122.3(5) . . ?
C5 C6 C7 117.8(5) . . ?
N1 C7 C6 127.0(5) . . ?
N1 C7 H7 116.5 . . ?
C6 C7 H7 116.5 . . ?
C13 C8 N1 104.8(6) . . ?
C13 C8 C9 111.8(11) . . ?
N1 C8 C9 114.0(9) . . ?
C13 C8 H8 108.7 . . ?
N1 C8 H8 108.7 . . ?
C9 C8 H8 108.7 . . ?
C10 C9 C8 108.2(14) . . ?
C10 C9 H9A 110.1 . . ?
C8 C9 H9A 110.1 . . ?
C10 C9 H9B 110.1 . . ?
C8 C9 H9B 110.1 . . ?
H9A C9 H9B 108.4 . . ?
C11 C10 C9 109.5(14) . . ?
C11 C10 H10A 109.8 . . ?
C9 C10 H10A 109.8 . . ?
C11 C10 H10B 109.8 . . ?
C9 C10 H10B 109.8 . . ?
H10A C10 H10B 108.2 . . ?
C10 C11 C12 112.9(15) . . ?
C10 C11 H11A 109.0 . . ?
C12 C11 H11A 109.0 . . ?
C10 C11 H11B 109.0 . . ?
C12 C11 H11B 109.0 . . ?
H11A C11 H11B 107.8 . . ?
C11 C12 C13 108.7(15) . . ?
C11 C12 H12A 110.0 . . ?
C13 C12 H12A 110.0 . . ?
C11 C12 H12B 110.0 . . ?
C13 C12 H12B 110.0 . . ?
H12A C12 H12B 108.3 . . ?
C8 C13 N2 105.8(6) . . ?
C8 C13 C12 107.8(12) . . ?
N2 C13 C12 109.1(10) . . ?
C8 C13 H13 111.3 . . ?
N2 C13 H13 111.3 . . ?
C12 C13 H13 111.3 . . ?
C13' C8' N1 108.7(8) . . ?
C13' C8' C9' 106.1(19) . . ?
N1 C8' C9' 108.7(12) . . ?
C13' C8' H8' 111.0 . . ?
N1 C8' H8' 111.0 . . ?
C9' C8' H8' 111.0 . . ?
C10' C9' C8' 110.5(17) . . ?
C10' C9' H9C 109.6 . . ?
C8' C9' H9C 109.6 . . ?
C10' C9' H9D 109.6 . . ?
C8' C9' H9D 109.6 . . ?
H9C C9' H9D 108.1 . . ?
C11' C10' C9' 111(3) . . ?
C11' C10' H10C 109.5 . . ?
C9' C10' H10C 109.5 . . ?
C11' C10' H10D 109.5 . . ?
C9' C10' H10D 109.5 . . ?
H10C C10' H10D 108.1 . . ?
C10' C11' C12' 110(2) . . ?
C10' C11' H11C 109.7 . . ?
C12' C11' H11C 109.7 . . ?
C10' C11' H11D 109.7 . . ?
C12' C11' H11D 109.7 . . ?
H11C C11' H11D 108.2 . . ?
C11' C12' C13' 106.3(19) . . ?
C11' C12' H12C 110.5 . . ?
C13' C12' H12C 110.5 . . ?
C11' C12' H12D 110.5 . . ?
C13' C12' H12D 110.5 . . ?
H12C C12' H12D 108.7 . . ?
C8' C13' N2 104.2(7) . . ?
C8' C13' C12' 113(2) . . ?
N2 C13' C12' 117.3(12) . . ?
C8' C13' H13' 107.2 . . ?
N2 C13' H13' 107.2 . . ?
C12' C13' H13' 107.2 . . ?
N2 C14 C15 127.4(5) . . ?
N2 C14 H14 116.3 . . ?
C15 C14 H14 116.3 . . ?
C20 C15 C16 121.1(6) . . ?
C20 C15 C14 122.1(5) . . ?
C16 C15 C14 116.4(5) . . ?
C17 C16 C15 119.7(6) . . ?
C17 C16 H16 120.2 . . ?
C15 C16 H16 120.2 . . ?
C16 C17 C18 119.6(6) . . ?
C16 C17 H17 120.2 . . ?
C18 C17 H17 120.2 . . ?
C19 C18 C17 123.0(7) . . ?
C19 C18 H18 118.5 . . ?
C17 C18 H18 118.5 . . ?
C18 C19 O6 127.1(6) . . ?
C18 C19 C20 118.8(6) . . ?
O6 C19 C20 114.1(5) . . ?
O4 C20 C15 122.4(5) . . ?
O4 C20 C19 119.8(5) . . ?
C15 C20 C19 117.7(5) . . ?
O5 C21 C22 112.3(5) . . ?
O5 C21 H21A 109.2 . . ?
C22 C21 H21A 109.2 . . ?
O5 C21 H21B 109.2 . . ?
C22 C21 H21B 109.2 . . ?
H21A C21 H21B 107.9 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
O6 C23 C24 109.3(6) . . ?
O6 C23 H23A 109.8 . . ?
C24 C23 H23A 109.8 . . ?
O6 C23 H23B 109.8 . . ?
C24 C23 H23B 109.8 . . ?
H23A C23 H23B 108.3 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C5A N1A C1A 116.7(4) . . ?
C5A N1A U1 121.4(3) . . ?
C1A N1A U1 121.7(3) . . ?
N1A C1A C2A 123.5(5) . . ?
N1A C1A H1A 118.2 . . ?
C2A C1A H1A 118.2 . . ?
C3A C2A C1A 118.5(5) . . ?
C3A C2A H2A 120.7 . . ?
C1A C2A H2A 120.7 . . ?
C2A C3A C4A 119.3(5) . . ?
C2A C3A H3A 120.3 . . ?
C4A C3A H3A 120.3 . . ?
C3A C4A C5A 118.7(5) . . ?
C3A C4A H4A 120.7 . . ?
C5A C4A H4A 120.7 . . ?
N1A C5A C4A 123.2(5) . . ?
N1A C5A H5A 118.4 . . ?
C4A C5A H5A 118.4 . . ?
Cl1B C1B Cl2B 111.3(6) . . ?
Cl1B C1B Cl3B 110.9(6) . . ?
Cl2B C1B Cl3B 109.7(5) . . ?
Cl1B C1B D1B 108.3 . . ?
Cl2B C1B D1B 108.3 . . ?
Cl3B C1B D1B 108.3 . . ?

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 O3 C1 C6 -41.5(6) . . . . ?
U1 O3 C1 C2 142.8(4) . . . . ?
C21 O5 C2 C3 -0.5(7) . . . . ?
C21 O5 C2 C1 -179.5(4) . . . . ?
O3 C1 C2 O5 -4.6(6) . . . . ?
C6 C1 C2 O5 179.6(4) . . . . ?
O3 C1 C2 C3 176.4(5) . . . . ?
C6 C1 C2 C3 0.5(7) . . . . ?
O5 C2 C3 C4 -177.6(5) . . . . ?
C1 C2 C3 C4 1.3(8) . . . . ?
C2 C3 C4 C5 -2.1(9) . . . . ?
C3 C4 C5 C6 1.0(9) . . . . ?
O3 C1 C6 C5 -177.3(5) . . . . ?
C2 C1 C6 C5 -1.6(7) . . . . ?
O3 C1 C6 C7 -3.4(8) . . . . ?
C2 C1 C6 C7 172.3(5) . . . . ?
C4 C5 C6 C1 0.8(8) . . . . ?
C4 C5 C6 C7 -173.3(6) . . . . ?
C8 N1 C7 C6 -161.6(6) . . . . ?
C8' N1 C7 C6 169.7(8) . . . . ?
U1 N1 C7 C6 18.5(9) . . . . ?
C1 C6 C7 N1 10.6(10) . . . . ?
C5 C6 C7 N1 -175.5(6) . . . . ?
C7 N1 C8 C13 -111.9(8) . . . . ?
U1 N1 C8 C13 68.0(8) . . . . ?
C7 N1 C8 C9 10.6(18) . . . . ?
U1 N1 C8 C9 -169.5(15) . . . . ?
C13 C8 C9 C10 -61(2) . . . . ?
N1 C8 C9 C10 -180.0(14) . . . . ?
C8 C9 C10 C11 56(3) . . . . ?
C9 C10 C11 C12 -58(3) . . . . ?
C10 C11 C12 C13 58(3) . . . . ?
N1 C8 C13 N2 -57.3(10) . . . . ?
C9 C8 C13 N2 178.8(13) . . . . ?
N1 C8 C13 C12 -173.8(12) . . . . ?
C9 C8 C13 C12 62(2) . . . . ?
C14 N2 C13 C8 -178.7(7) . . . . ?
U1 N2 C13 C8 23.1(10) . . . . ?
C14 N2 C13 C12 -63.0(15) . . . . ?
U1 N2 C13 C12 138.8(13) . . . . ?
C11 C12 C13 C8 -59(2) . . . . ?
C11 C12 C13 N2 -173.2(15) . . . . ?
C7 N1 C8' C13' -176.0(10) . . . . ?
U1 N1 C8' C13' -22.6(13) . . . . ?
C7 N1 C8' C9' 69(2) . . . . ?
U1 N1 C8' C9' -138(2) . . . . ?
C13' C8' C9' C10' 58(4) . . . . ?
N1 C8' C9' C10' 175(3) . . . . ?
C8' C9' C10' C11' -59(5) . . . . ?
C9' C10' C11' C12' 60(4) . . . . ?
C10' C11' C12' C13' -59(4) . . . . ?
N1 C8' C13' N2 53.0(15) . . . . ?
C9' C8' C13' N2 169.8(19) . . . . ?
N1 C8' C13' C12' -178.4(18) . . . . ?
C9' C8' C13' C12' -62(3) . . . . ?
C14 N2 C13' C8' 120.7(10) . . . . ?
U1 N2 C13' C8' -62.7(11) . . . . ?
C14 N2 C13' C12' -5(3) . . . . ?
U1 N2 C13' C12' 171(3) . . . . ?
C11' C12' C13' C8' 63(4) . . . . ?
C11' C12' C13' N2 -176(2) . . . . ?
C13' N2 C14 C15 159.4(7) . . . . ?
C13 N2 C14 C15 -173.4(7) . . . . ?
U1 N2 C14 C15 -16.6(8) . . . . ?
N2 C14 C15 C20 -12.4(9) . . . . ?
N2 C14 C15 C16 174.1(6) . . . . ?
C20 C15 C16 C17 1.2(10) . . . . ?
C14 C15 C16 C17 174.8(7) . . . . ?
C15 C16 C17 C18 -2.9(12) . . . . ?
C16 C17 C18 C19 1.9(13) . . . . ?
C17 C18 C19 O6 -179.5(7) . . . . ?
C17 C18 C19 C20 0.8(12) . . . . ?
C23 O6 C19 C18 9.5(10) . . . . ?
C23 O6 C19 C20 -170.8(6) . . . . ?
U1 O4 C20 C15 41.8(7) . . . . ?
U1 O4 C20 C19 -142.5(4) . . . . ?
C16 C15 C20 O4 177.2(5) . . . . ?
C14 C15 C20 O4 4.0(8) . . . . ?
C16 C15 C20 C19 1.4(8) . . . . ?
C14 C15 C20 C19 -171.8(5) . . . . ?
C18 C19 C20 O4 -178.3(6) . . . . ?
O6 C19 C20 O4 2.0(8) . . . . ?
C18 C19 C20 C15 -2.4(9) . . . . ?
O6 C19 C20 C15 177.9(5) . . . . ?
C2 O5 C21 C22 -81.8(6) . . . . ?
C19 O6 C23 C24 171.3(6) . . . . ?
C5A N1A C1A C2A -1.2(7) . . . . ?
U1 N1A C1A C2A -176.7(4) . . . . ?
N1A C1A C2A C3A 2.4(8) . . . . ?
C1A C2A C3A C4A -2.3(8) . . . . ?
C2A C3A C4A C5A 1.3(8) . . . . ?
C1A N1A C5A C4A 0.0(7) . . . . ?
U1 N1A C5A C4A 175.6(4) . . . . ?
C3A C4A C5A N1A -0.1(8) . . . . ?

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
C12 H12A O2 0.97 2.70 3.37(3) 126.8 4_556
C21 H21A O2 0.97 2.56 3.395(6) 144.0 7_556
C1A H1A O3 0.93 2.63 3.163(6) 117.0 .
C1A H1A O5 0.93 2.45 3.266(7) 147.0 .
C2A H2A O2 0.93 2.64 3.513(7) 155.7 7_556
C5A H5A O4 0.93 2.63 3.155(6) 116.2 .
C1B D1B O3 0.98 2.44 3.406(8) 167.7 .

_refine_diff_density_max         1.579
_refine_diff_density_min         -1.017
_refine_diff_density_rms         0.102

