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

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

data_dnh40
_database_code_depnum_ccdc_archive 'CCDC 1852095'
_audit_update_record             
;
2018-06-27 deposited with the CCDC.
2018-08-15 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         ?
_chemical_formula_sum            'C22 H46 Cl3 La N2 O7'
_chemical_formula_weight         695.87

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'
La La -0.2871 2.4523 '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                   13.8322(11)
_cell_length_b                   16.2467(13)
_cell_length_c                   13.1611(10)
_cell_angle_alpha                90
_cell_angle_beta                 106.0577(9)
_cell_angle_gamma                90
_cell_volume                     2842.3(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    133(2)
_cell_measurement_reflns_used    9957
_cell_measurement_theta_min      2.27
_cell_measurement_theta_max      28.75

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      not_measured
_exptl_crystal_density_method    not_measured
_exptl_crystal_density_diffrn    1.626
_exptl_crystal_F_000             1424
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.283
_exptl_crystal_size_mid          0.117
_exptl_crystal_size_min          0.089
_exptl_absorpt_coefficient_mu    1.827
_shelx_estimated_absorpt_T_min   0.626
_shelx_estimated_absorpt_T_max   0.854
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6485
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_process_details   'Bruker SADABS 2014/5'
_exptl_absorpt_special_details   
; 
Reflections not merged 
17190 Corrected reflections written to file dnh40s.hkl 
Estimated minimum and maximum transmission:  0.6485  0.7458 
The ratio (0.8695) of these values is more reliable than their absolute values 
Additional spherical absorption correction applied with mu*r =  0.2000 
Lambda/2 correction factor = 0.00150 
;
_diffrn_ambient_temperature      133(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            16831
_diffrn_reflns_av_unetI/netI     0.0220
_diffrn_reflns_av_R_equivalents  0.0321
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.980
_diffrn_reflns_theta_max         28.770
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.944
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.944
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.944
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             3496
_reflns_number_gt                3298
_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       'Bruker APEX2 2014.11-0, 2014'
_computing_cell_refinement       'Bruker SAINT 8.34a, 2013'
_computing_data_reduction        'Bruker SAINT 8.34a, 2013'
_computing_structure_solution    'Bruker SHELXTL 2014/4'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
A colorless crystal of approximate dimensions 0.089 x 0.117 x 0.283 mm 
was mounted in a cryoloop and transferred to a Bruker SMART APEX II 
diffractometer.  The APEX2 program package was used to determine the 
unit-cell parameters and for data collection (25 sec/frame scan time for 
a sphere of diffraction data).  The raw frame data was processed using 
SAINT and SADABS to yield the reflection data file.  Subsequent 
calculations were carried out using the SHELXTL program.  The 
diffraction symmetry was 2/m and the systematic absences were consistent 
with the monoclinic space groups Cc and C2/c.  It was later determined 
that space group C2/c was correct.

The structure was solved by dual space methods and refined on F2 by 
full-matrix least-squares techniques.  The analytical scattering 
factors for neutral atoms were used throughout the analysis. Hydrogen 
atoms were included using a riding model.  The molecule and chloride 
ion were located on two-fold rotation axes. There was one molecule of 
diethylether solvent present.  The solvent was located on an inversion 
center.  Both the solvent and chloride ion were disordered and included 
using multiple components with partial site-occupancy-factors.

Least-squares analysis yielded wR2 = 0.0554 and Goof = 1.069 for 183 
variables refined against 3496 data (0.74 Å), R1 = 0.0210 for those 
3298 data with I > 2.0sigma(I).  
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0298P)²+3.6575P] 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         3496
_refine_ls_number_parameters     183
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0232
_refine_ls_R_factor_gt           0.0210
_refine_ls_wR_factor_ref         0.0554
_refine_ls_wR_factor_gt          0.0541
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_restrained_S_all      1.069
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

# start Validation Reply Form
_vrf_PLAT043_dnh40               
;
PROBLEM: Calculated and Reported Mol. Weight Differ by ..      10.08 Check 
RESPONSE: ...Hydrogen atoms associated with the disordred diethylether
solvent molecule were not included in the refinement
;
# end Validation Reply Form 

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
La1 La 0.5000 0.65476(2) 0.2500 0.01324(5) Uani 1 2 d S T P . .
Cl1 Cl 0.66115(3) 0.59504(3) 0.41457(4) 0.02184(10) Uani 1 1 d . . . . .
O1 O 0.52673(10) 0.76375(9) 0.40968(11) 0.0222(3) Uani 1 1 d . . . . .
O2 O 0.64870(11) 0.76514(9) 0.28249(12) 0.0260(3) Uani 1 1 d . . . . .
O3 O 0.43867(10) 0.50990(8) 0.31438(10) 0.0196(3) Uani 1 1 d . . . . .
N1 N 0.35959(13) 0.65801(10) 0.37705(14) 0.0210(3) Uani 1 1 d . . . . .
C1 C 0.38672(16) 0.71899(14) 0.46410(17) 0.0263(4) Uani 1 1 d . . . . .
H1A H 0.3633 0.6992 0.5244 0.032 Uiso 1 1 calc R U . . .
H1B H 0.3527 0.7719 0.4397 0.032 Uiso 1 1 calc R U . . .
C2 C 0.49829(16) 0.73222(14) 0.49971(16) 0.0258(4) Uani 1 1 d . . . . .
H2A H 0.5160 0.7721 0.5588 0.031 Uiso 1 1 calc R U . . .
H2B H 0.5335 0.6797 0.5239 0.031 Uiso 1 1 calc R U . . .
C3 C 0.61911(16) 0.80903(14) 0.44234(18) 0.0281(5) Uani 1 1 d . . . . .
H3A H 0.6735 0.7737 0.4853 0.034 Uiso 1 1 calc R U . . .
H3B H 0.6112 0.8572 0.4855 0.034 Uiso 1 1 calc R U . . .
C4 C 0.64408(18) 0.83651(13) 0.3451(2) 0.0327(5) Uani 1 1 d . . . . .
H4A H 0.5919 0.8749 0.3047 0.039 Uiso 1 1 calc R U . . .
H4B H 0.7096 0.8654 0.3638 0.039 Uiso 1 1 calc R U . . .
C5 C 0.73887(16) 0.75930(15) 0.25068(18) 0.0297(5) Uani 1 1 d . . . . .
H5A H 0.7981 0.7634 0.3132 0.036 Uiso 1 1 calc R U . . .
H5B H 0.7421 0.8049 0.2018 0.036 Uiso 1 1 calc R U . . .
C6 C 0.73971(15) 0.67793(15) 0.19637(18) 0.0281(5) Uani 1 1 d . . . . .
H6A H 0.7908 0.6795 0.1565 0.034 Uiso 1 1 calc R U . . .
H6B H 0.7591 0.6340 0.2503 0.034 Uiso 1 1 calc R U . . .
C7 C 0.35458(17) 0.57621(14) 0.42476(17) 0.0266(4) Uani 1 1 d . . . . .
H7A H 0.2945 0.5741 0.4517 0.032 Uiso 1 1 calc R U . . .
H7B H 0.4147 0.5688 0.4857 0.032 Uiso 1 1 calc R U . . .
C8 C 0.34943(16) 0.50701(14) 0.34838(18) 0.0269(4) Uani 1 1 d . . . . .
H8A H 0.3448 0.4536 0.3831 0.032 Uiso 1 1 calc R U . . .
H8B H 0.2894 0.5131 0.2871 0.032 Uiso 1 1 calc R U . . .
C9 C 0.44863(16) 0.43668(12) 0.25746(17) 0.0237(4) Uani 1 1 d . . . . .
H9A H 0.3973 0.4359 0.1880 0.028 Uiso 1 1 calc R U . . .
H9B H 0.4391 0.3874 0.2978 0.028 Uiso 1 1 calc R U . . .
Cl2 Cl 0.5000 0.78064(10) 0.7500 0.0280(2) Uani 0.7 2 d S T P . .
Cl3 Cl 0.5000 0.8278(3) 0.7500 0.0308(6) Uani 0.3 2 d S T P . .
O4 O 0.5000 1.0000 0.0000 0.0646(9) Uani 1 2 d S . P . .
C10 C 0.5857(4) 0.9426(3) 0.0104(6) 0.0498(15) Uani 0.5 1 d . . P A 1
C10B C 0.4313(5) 1.0075(4) -0.0976(6) 0.0559(17) Uani 0.5 1 d . . P A 2
C11 C 0.6518(4) 0.9261(3) 0.0960(5) 0.0506(16) Uani 0.5 1 d . . P . .
C12 C 0.5271(11) 0.9665(8) -0.0884(11) 0.045(3) Uiso 0.25 1 d . . P A 1
C12B C 0.4874(11) 0.9742(8) -0.1147(10) 0.041(3) Uiso 0.25 1 d . . P A 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
La1 O2 2.6725(14) 2_655 ?
La1 O2 2.6726(14) . ?
La1 O1 2.6942(14) . ?
La1 O1 2.6942(14) 2_655 ?
La1 O3 2.7155(13) 2_655 ?
La1 O3 2.7156(13) . ?
La1 Cl1 2.8161(5) 2_655 ?
La1 Cl1 2.8161(5) . ?
La1 N1 2.8927(17) . ?
La1 N1 2.8927(17) 2_655 ?
O1 C3 1.434(2) . ?
O1 C2 1.442(3) . ?
O2 C5 1.424(2) . ?
O2 C4 1.434(3) . ?
O3 C8 1.425(2) . ?
O3 C9 1.433(2) . ?
N1 C7 1.480(3) . ?
N1 C6 1.480(3) 2_655 ?
N1 C1 1.482(3) . ?
C1 C2 1.499(3) . ?
C3 C4 1.484(4) . ?
C5 C6 1.504(3) . ?
C6 N1 1.480(3) 2_655 ?
C7 C8 1.497(3) . ?
C9 C9 1.487(4) 2_655 ?
Cl2 Cl3 0.766(4) . ?
O4 C10B 1.375(6) 5_675 ?
O4 C10B 1.376(6) . ?
O4 C12 1.425(13) . ?
O4 C12 1.425(13) 5_675 ?
O4 C10 1.484(6) . ?
O4 C10 1.484(6) 5_675 ?
O4 C12B 1.530(12) 5_675 ?
O4 C12B 1.530(12) . ?
C10 C11 1.267(8) . ?
C10 C12 1.383(16) . ?
C10B C12B 1.021(14) . ?
C10B C11 1.581(10) 5_675 ?
C11 C10B 1.581(10) 5_675 ?

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 La1 O2 95.71(7) 2_655 . ?
O2 La1 O1 67.50(4) 2_655 . ?
O2 La1 O1 60.05(4) . . ?
O2 La1 O1 60.05(4) 2_655 2_655 ?
O2 La1 O1 67.50(4) . 2_655 ?
O1 La1 O1 97.83(6) . 2_655 ?
O2 La1 O3 145.55(4) 2_655 2_655 ?
O2 La1 O3 109.78(4) . 2_655 ?
O1 La1 O3 145.66(4) . 2_655 ?
O1 La1 O3 108.27(4) 2_655 2_655 ?
O2 La1 O3 109.78(4) 2_655 . ?
O2 La1 O3 145.55(4) . . ?
O1 La1 O3 108.27(4) . . ?
O1 La1 O3 145.66(4) 2_655 . ?
O3 La1 O3 59.85(6) 2_655 . ?
O2 La1 Cl1 72.41(4) 2_655 2_655 ?
O2 La1 Cl1 139.88(4) . 2_655 ?
O1 La1 Cl1 137.31(3) . 2_655 ?
O1 La1 Cl1 73.61(3) 2_655 2_655 ?
O3 La1 Cl1 73.17(3) 2_655 2_655 ?
O3 La1 Cl1 72.07(3) . 2_655 ?
O2 La1 Cl1 139.88(4) 2_655 . ?
O2 La1 Cl1 72.41(4) . . ?
O1 La1 Cl1 73.61(3) . . ?
O1 La1 Cl1 137.31(3) 2_655 . ?
O3 La1 Cl1 72.07(3) 2_655 . ?
O3 La1 Cl1 73.17(3) . . ?
Cl1 La1 Cl1 139.69(2) 2_655 . ?
O2 La1 N1 58.00(5) 2_655 . ?
O2 La1 N1 120.35(5) . . ?
O1 La1 N1 60.42(4) . . ?
O1 La1 N1 118.01(5) 2_655 . ?
O3 La1 N1 120.92(4) 2_655 . ?
O3 La1 N1 61.17(4) . . ?
Cl1 La1 N1 86.31(4) 2_655 . ?
Cl1 La1 N1 94.41(4) . . ?
O2 La1 N1 120.35(5) 2_655 2_655 ?
O2 La1 N1 58.01(5) . 2_655 ?
O1 La1 N1 118.01(5) . 2_655 ?
O1 La1 N1 60.42(4) 2_655 2_655 ?
O3 La1 N1 61.17(4) 2_655 2_655 ?
O3 La1 N1 120.92(4) . 2_655 ?
Cl1 La1 N1 94.41(4) 2_655 2_655 ?
Cl1 La1 N1 86.31(4) . 2_655 ?
N1 La1 N1 177.91(7) . 2_655 ?
C3 O1 C2 111.05(15) . . ?
C3 O1 La1 119.33(12) . . ?
C2 O1 La1 113.44(11) . . ?
C5 O2 C4 113.86(16) . . ?
C5 O2 La1 127.30(13) . . ?
C4 O2 La1 118.68(12) . . ?
C8 O3 C9 110.71(15) . . ?
C8 O3 La1 119.93(12) . . ?
C9 O3 La1 118.23(11) . . ?
C7 N1 C6 109.24(17) . 2_655 ?
C7 N1 C1 107.69(17) . . ?
C6 N1 C1 110.45(16) 2_655 . ?
C7 N1 La1 110.28(11) . . ?
C6 N1 La1 106.07(12) 2_655 . ?
C1 N1 La1 113.08(12) . . ?
N1 C1 C2 110.86(16) . . ?
O1 C2 C1 106.58(16) . . ?
O1 C3 C4 107.25(17) . . ?
O2 C4 C3 108.08(18) . . ?
O2 C5 C6 108.70(17) . . ?
N1 C6 C5 112.00(18) 2_655 . ?
N1 C7 C8 112.88(17) . . ?
O3 C8 C7 107.56(16) . . ?
O3 C9 C9 107.62(14) . 2_655 ?
C10B O4 C10B 180.0 5_675 . ?
C12 O4 C12 180.0 . 5_675 ?
C12 O4 C10 56.7(6) . . ?
C12 O4 C10 123.3(6) 5_675 . ?
C12 O4 C10 123.3(6) . 5_675 ?
C12 O4 C10 56.7(6) 5_675 5_675 ?
C10 O4 C10 180.0(3) . 5_675 ?
C10B O4 C12B 40.7(6) 5_675 5_675 ?
C10B O4 C12B 139.3(6) . 5_675 ?
C10B O4 C12B 139.3(6) 5_675 . ?
C10B O4 C12B 40.7(6) . . ?
C12B O4 C12B 180.0 5_675 . ?
C11 C10 C12 170.1(8) . . ?
C11 C10 O4 125.2(6) . . ?
C12 C10 O4 59.5(6) . . ?
C12B C10B O4 77.8(8) . . ?
C12B C10B C11 164.7(10) . 5_675 ?
O4 C10B C11 111.4(6) . 5_675 ?
C10 C12 O4 63.8(6) . . ?
C10B C12B O4 61.5(7) . . ?

_refine_diff_density_max         0.696
_refine_diff_density_min         -0.505
_refine_diff_density_rms         0.083


_chemical_properties_physical    Moisture-sensitive
####################################################################### 
# 
# 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_dnh34
_database_code_depnum_ccdc_archive 'CCDC 1852096'
_audit_update_record             
;
2018-06-27 deposited with the CCDC.
2018-08-15 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         ?
_chemical_formula_sum            'C21 H42 Cl6 I3 N2 O6 U'
_chemical_formula_weight         1249.99

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'
I I -0.4742 1.8119 '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                   11.485(2)
_cell_length_b                   26.766(5)
_cell_length_c                   12.275(2)
_cell_angle_alpha                90
_cell_angle_beta                 101.244(2)
_cell_angle_gamma                90
_cell_volume                     3700.8(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    133(2)
_cell_measurement_reflns_used    9941
_cell_measurement_theta_min      2.28
_cell_measurement_theta_max      28.52

_exptl_crystal_description       irregular
_exptl_crystal_colour            green
_exptl_crystal_density_meas      not_measured
_exptl_crystal_density_method    not_measured
_exptl_crystal_density_diffrn    2.243
_exptl_crystal_F_000             2332
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.331
_exptl_crystal_size_mid          0.205
_exptl_crystal_size_min          0.084
_exptl_absorpt_coefficient_mu    7.356
_shelx_estimated_absorpt_T_min   0.194
_shelx_estimated_absorpt_T_max   0.577
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.2781
_exptl_absorpt_correction_T_max  0.4316
_exptl_absorpt_process_details   'Bruker SADABS 2014/5'
_exptl_absorpt_special_details   
; 
Reflections not merged 
44900 Corrected reflections written to file dnh34s.hkl 
Estimated minimum and maximum transmission:  0.2781  0.4316 
The ratio (0.6443) of these values is more reliable than their absolute values 
Additional spherical absorption correction applied with mu*r =  0.6000 
Lambda/2 correction factor = 0.00150 
;
_diffrn_ambient_temperature      133(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            43788
_diffrn_reflns_av_unetI/netI     0.0324
_diffrn_reflns_av_R_equivalents  0.0457
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.522
_diffrn_reflns_theta_max         27.874
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             8749
_reflns_number_gt                7986
_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       'Bruker APEX2 2014.11-0, 2014'
_computing_cell_refinement       'Bruker SAINT 8.34a, 2013'
_computing_data_reduction        'Bruker SAINT 8.34a, 2013'
_computing_structure_solution    'Bruker SHELXTL 2014/4'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
A green crystal of approximate dimensions 0.084 x 0.205 x 0.331 mm was 
mounted in a cryoloop and transferred to a Bruker SMART APEX II diffractometer.  
The APEX2 program package was used to determine the unit-cell parameters and 
for data collection (20 sec/frame scan time for a sphere of diffraction data).  
The raw frame data was processed using SAINT and SADABS to yield the reflection 
data file.  Subsequent calculations were carried out using the SHELXTL program.  
The diffraction symmetry was 2/m and the systematic absences were consistent with 
the monoclinic space group P21/c that was later determined to be correct.

The structure was solved by dual space methods and refined on F2 by full-matrix 
least-squares techniques.  The analytical scattering factors for neutral atoms 
were used throughout the analysis.  Hydrogen atoms were included using a riding 
model.  There were three molecules of dichloromethane solvent present.

Least-squares analysis yielded wR2 = 0.0497 and Goof = 1.059 for 352 variables 
refined against 8749 data (0.76 Å), R1 = 0.0225 for those 7986 data 
with I > 2.0sigma(I).  
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0168P)²+2.6999P] 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         8749
_refine_ls_number_parameters     352
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0265
_refine_ls_R_factor_gt           0.0225
_refine_ls_wR_factor_ref         0.0497
_refine_ls_wR_factor_gt          0.0483
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_restrained_S_all      1.059
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.27612(2) 0.61635(2) 0.16107(2) 0.01160(3) Uani 1 1 d . . . . .
I1 I 0.21669(2) 0.73818(2) 0.14687(2) 0.02120(5) Uani 1 1 d . . . . .
I2 I 0.22943(2) 0.51480(2) 0.00464(2) 0.01866(5) Uani 1 1 d . . . . .
O1 O 0.2556(2) 0.54267(8) 0.29004(18) 0.0190(5) Uani 1 1 d . . . . .
O2 O 0.45878(19) 0.55568(8) 0.22406(18) 0.0173(5) Uani 1 1 d . . . . .
O3 O 0.26542(19) 0.64796(8) 0.36514(17) 0.0166(5) Uani 1 1 d . . . . .
O4 O 0.45718(19) 0.66307(8) 0.28173(18) 0.0192(5) Uani 1 1 d . . . . .
O5 O 0.0662(2) 0.63074(8) 0.02560(17) 0.0172(5) Uani 1 1 d . . . . .
O6 O 0.2641(2) 0.64302(8) -0.05272(17) 0.0184(5) Uani 1 1 d . . . . .
N1 N 0.0675(2) 0.59874(10) 0.2415(2) 0.0137(5) Uani 1 1 d . . . . .
N2 N 0.4906(2) 0.63388(10) 0.0827(2) 0.0178(6) Uani 1 1 d . . . . .
C1 C 0.0467(3) 0.54420(12) 0.2288(3) 0.0200(7) Uani 1 1 d . . . . .
H1A H 0.0361 0.5351 0.1493 0.024 Uiso 1 1 calc R U . . .
H1B H -0.0271 0.5354 0.2547 0.024 Uiso 1 1 calc R U . . .
C2 C 0.1491(3) 0.51499(12) 0.2943(3) 0.0221(7) Uani 1 1 d . . . . .
H2A H 0.1393 0.5111 0.3722 0.027 Uiso 1 1 calc R U . . .
H2B H 0.1529 0.4814 0.2616 0.027 Uiso 1 1 calc R U . . .
C3 C 0.3617(3) 0.52214(13) 0.3584(3) 0.0225(7) Uani 1 1 d . . . . .
H3A H 0.3422 0.4912 0.3954 0.027 Uiso 1 1 calc R U . . .
H3B H 0.3965 0.5465 0.4164 0.027 Uiso 1 1 calc R U . . .
C4 C 0.4472(3) 0.51096(12) 0.2857(3) 0.0218(7) Uani 1 1 d . . . . .
H4A H 0.5250 0.5013 0.3309 0.026 Uiso 1 1 calc R U . . .
H4B H 0.4177 0.4832 0.2346 0.026 Uiso 1 1 calc R U . . .
C5 C 0.5413(3) 0.54834(13) 0.1507(3) 0.0224(7) Uani 1 1 d . . . . .
H5A H 0.5007 0.5331 0.0800 0.027 Uiso 1 1 calc R U . . .
H5B H 0.6069 0.5261 0.1857 0.027 Uiso 1 1 calc R U . . .
C6 C 0.5884(3) 0.59912(14) 0.1301(3) 0.0249(8) Uani 1 1 d . . . . .
H6A H 0.6331 0.6129 0.2008 0.030 Uiso 1 1 calc R U . . .
H6B H 0.6439 0.5960 0.0780 0.030 Uiso 1 1 calc R U . . .
C7 C 0.0767(3) 0.61267(12) 0.3596(3) 0.0181(7) Uani 1 1 d . . . . .
H7A H 0.1133 0.5848 0.4073 0.022 Uiso 1 1 calc R U . . .
H7B H -0.0038 0.6183 0.3747 0.022 Uiso 1 1 calc R U . . .
C8 C 0.1496(3) 0.65889(13) 0.3882(3) 0.0189(7) Uani 1 1 d . . . . .
H8A H 0.1132 0.6874 0.3426 0.023 Uiso 1 1 calc R U . . .
H8B H 0.1557 0.6674 0.4676 0.023 Uiso 1 1 calc R U . . .
C9 C 0.3516(3) 0.68206(12) 0.4227(3) 0.0198(7) Uani 1 1 d . . . . .
H9A H 0.3522 0.6811 0.5035 0.024 Uiso 1 1 calc R U . . .
H9B H 0.3333 0.7166 0.3956 0.024 Uiso 1 1 calc R U . . .
C10 C 0.4682(3) 0.66591(14) 0.4001(3) 0.0224(7) Uani 1 1 d . . . . .
H10A H 0.5306 0.6902 0.4317 0.027 Uiso 1 1 calc R U . . .
H10B H 0.4901 0.6329 0.4342 0.027 Uiso 1 1 calc R U . . .
C11 C 0.5464(3) 0.69110(15) 0.2420(3) 0.0295(8) Uani 1 1 d . . . . .
H11A H 0.6262 0.6784 0.2757 0.035 Uiso 1 1 calc R U . . .
H11B H 0.5419 0.7267 0.2623 0.035 Uiso 1 1 calc R U . . .
C12 C 0.5248(4) 0.68552(14) 0.1170(3) 0.0296(8) Uani 1 1 d . . . . .
H12A H 0.4609 0.7087 0.0826 0.036 Uiso 1 1 calc R U . . .
H12B H 0.5978 0.6947 0.0901 0.036 Uiso 1 1 calc R U . . .
C13 C -0.0347(3) 0.62636(13) 0.1761(3) 0.0191(7) Uani 1 1 d . . . . .
H13A H -0.0248 0.6625 0.1929 0.023 Uiso 1 1 calc R U . . .
H13B H -0.1086 0.6151 0.1988 0.023 Uiso 1 1 calc R U . . .
C14 C -0.0462(3) 0.61868(13) 0.0539(3) 0.0206(7) Uani 1 1 d . . . . .
H14A H -0.0674 0.5835 0.0343 0.025 Uiso 1 1 calc R U . . .
H14B H -0.1092 0.6406 0.0127 0.025 Uiso 1 1 calc R U . . .
C15 C 0.0560(3) 0.63173(14) -0.0929(3) 0.0223(7) Uani 1 1 d . . . . .
H15A H -0.0210 0.6465 -0.1285 0.027 Uiso 1 1 calc R U . . .
H15B H 0.0604 0.5974 -0.1217 0.027 Uiso 1 1 calc R U . . .
C16 C 0.1556(3) 0.66238(13) -0.1177(3) 0.0223(7) Uani 1 1 d . . . . .
H16A H 0.1578 0.6604 -0.1978 0.027 Uiso 1 1 calc R U . . .
H16B H 0.1451 0.6978 -0.0983 0.027 Uiso 1 1 calc R U . . .
C17 C 0.3645(3) 0.65951(14) -0.0954(3) 0.0262(8) Uani 1 1 d . . . . .
H17A H 0.3783 0.6956 -0.0803 0.031 Uiso 1 1 calc R U . . .
H17B H 0.3507 0.6542 -0.1767 0.031 Uiso 1 1 calc R U . . .
C18 C 0.4698(3) 0.62991(15) -0.0391(3) 0.0277(8) Uani 1 1 d . . . . .
H18A H 0.4576 0.5944 -0.0605 0.033 Uiso 1 1 calc R U . . .
H18B H 0.5412 0.6418 -0.0653 0.033 Uiso 1 1 calc R U . . .
I3 I 0.24592(2) 0.41633(2) 0.55875(2) 0.02136(5) Uani 1 1 d . . . . .
C19 C 0.7009(3) 0.65128(14) 0.7065(3) 0.0298(8) Uani 1 1 d . . . . .
H19A H 0.7144 0.6376 0.6351 0.036 Uiso 1 1 calc R U . . .
H19B H 0.7579 0.6789 0.7286 0.036 Uiso 1 1 calc R U . . .
Cl1 Cl 0.72586(8) 0.60415(3) 0.80866(8) 0.02937(19) Uani 1 1 d . . . . .
Cl2 Cl 0.55417(9) 0.67461(4) 0.68899(8) 0.0353(2) Uani 1 1 d . . . . .
C20 C -0.1991(3) 0.45120(14) 0.3152(3) 0.0283(8) Uani 1 1 d . . . . .
H20A H -0.2131 0.4501 0.2330 0.034 Uiso 1 1 calc R U . . .
H20B H -0.2065 0.4864 0.3378 0.034 Uiso 1 1 calc R U . . .
Cl3 Cl -0.05495(8) 0.42984(4) 0.36928(7) 0.0316(2) Uani 1 1 d . . . . .
Cl4 Cl -0.30806(9) 0.41445(4) 0.36233(9) 0.0348(2) Uani 1 1 d . . . . .
C21 C 0.8928(3) 0.71961(14) 0.4780(3) 0.0284(8) Uani 1 1 d . . . . .
H21A H 0.9737 0.7268 0.5200 0.034 Uiso 1 1 calc R U . . .
H21B H 0.8796 0.6831 0.4810 0.034 Uiso 1 1 calc R U . . .
Cl5 Cl 0.88224(9) 0.73810(4) 0.33886(8) 0.0366(2) Uani 1 1 d . . . . .
Cl6 Cl 0.78808(11) 0.75098(4) 0.54071(10) 0.0472(3) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 O1 2.568(2) . ?
U1 O4 2.623(2) . ?
U1 O2 2.646(2) . ?
U1 O3 2.669(2) . ?
U1 O5 2.676(2) . ?
U1 O6 2.697(2) . ?
U1 N1 2.803(3) . ?
U1 N2 2.853(3) . ?
U1 I2 3.3106(5) . ?
U1 I1 3.3292(6) . ?
O1 C2 1.440(4) . ?
O1 C3 1.446(4) . ?
O2 C4 1.436(4) . ?
O2 C5 1.442(4) . ?
O3 C9 1.428(4) . ?
O3 C8 1.442(4) . ?
O4 C11 1.430(4) . ?
O4 C10 1.436(4) . ?
O5 C15 1.436(4) . ?
O5 C14 1.438(4) . ?
O6 C17 1.426(4) . ?
O6 C16 1.438(4) . ?
N1 C7 1.481(4) . ?
N1 C1 1.483(4) . ?
N1 C13 1.483(4) . ?
N2 C18 1.472(4) . ?
N2 C12 1.475(4) . ?
N2 C6 1.487(4) . ?
C1 C2 1.507(5) . ?
C3 C4 1.481(5) . ?
C5 C6 1.503(5) . ?
C7 C8 1.497(5) . ?
C9 C10 1.484(5) . ?
C11 C12 1.514(5) . ?
C13 C14 1.494(5) . ?
C15 C16 1.486(5) . ?
C17 C18 1.497(5) . ?
C19 Cl1 1.762(4) . ?
C19 Cl2 1.770(4) . ?
C20 Cl3 1.755(4) . ?
C20 Cl4 1.776(4) . ?
C21 Cl5 1.760(4) . ?
C21 Cl6 1.762(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 U1 O4 100.13(7) . . ?
O1 U1 O2 60.75(7) . . ?
O4 U1 O2 68.38(7) . . ?
O1 U1 O3 68.81(7) . . ?
O4 U1 O3 59.70(7) . . ?
O2 U1 O3 95.70(7) . . ?
O1 U1 O5 108.29(7) . . ?
O4 U1 O5 143.23(7) . . ?
O2 U1 O5 146.79(7) . . ?
O3 U1 O5 109.68(7) . . ?
O1 U1 O6 144.05(7) . . ?
O4 U1 O6 107.93(7) . . ?
O2 U1 O6 109.52(7) . . ?
O3 U1 O6 145.70(7) . . ?
O5 U1 O6 59.22(7) . . ?
O1 U1 N1 57.76(7) . . ?
O4 U1 N1 121.28(7) . . ?
O2 U1 N1 118.50(7) . . ?
O3 U1 N1 61.58(7) . . ?
O5 U1 N1 60.98(7) . . ?
O6 U1 N1 120.12(7) . . ?
O1 U1 N2 121.54(7) . . ?
O4 U1 N2 58.01(7) . . ?
O2 U1 N2 60.79(7) . . ?
O3 U1 N2 117.70(7) . . ?
O5 U1 N2 119.96(7) . . ?
O6 U1 N2 60.81(7) . . ?
N1 U1 N2 179.06(7) . . ?
O1 U1 I2 72.73(5) . . ?
O4 U1 I2 137.71(5) . . ?
O2 U1 I2 72.25(5) . . ?
O3 U1 I2 140.59(5) . . ?
O5 U1 I2 74.54(5) . . ?
O6 U1 I2 71.41(5) . . ?
N1 U1 I2 90.76(5) . . ?
N2 U1 I2 89.57(6) . . ?
O1 U1 I1 137.89(5) . . ?
O4 U1 I1 72.21(5) . . ?
O2 U1 I1 139.38(5) . . ?
O3 U1 I1 72.07(5) . . ?
O5 U1 I1 71.08(5) . . ?
O6 U1 I1 73.66(5) . . ?
N1 U1 I1 90.15(5) . . ?
N2 U1 I1 90.17(6) . . ?
I2 U1 I1 139.946(10) . . ?
C2 O1 C3 114.1(2) . . ?
C2 O1 U1 126.73(18) . . ?
C3 O1 U1 118.79(18) . . ?
C4 O2 C5 110.8(2) . . ?
C4 O2 U1 121.07(18) . . ?
C5 O2 U1 118.77(18) . . ?
C9 O3 C8 110.5(2) . . ?
C9 O3 U1 120.85(18) . . ?
C8 O3 U1 117.47(17) . . ?
C11 O4 C10 112.9(3) . . ?
C11 O4 U1 126.83(19) . . ?
C10 O4 U1 120.02(18) . . ?
C15 O5 C14 110.4(2) . . ?
C15 O5 U1 121.17(19) . . ?
C14 O5 U1 124.06(18) . . ?
C17 O6 C16 111.1(2) . . ?
C17 O6 U1 123.19(19) . . ?
C16 O6 U1 120.62(18) . . ?
C7 N1 C1 109.3(2) . . ?
C7 N1 C13 107.6(2) . . ?
C1 N1 C13 109.8(2) . . ?
C7 N1 U1 113.57(18) . . ?
C1 N1 U1 105.07(18) . . ?
C13 N1 U1 111.49(18) . . ?
C18 N2 C12 109.8(3) . . ?
C18 N2 C6 108.2(3) . . ?
C12 N2 C6 109.7(3) . . ?
C18 N2 U1 110.5(2) . . ?
C12 N2 U1 104.89(19) . . ?
C6 N2 U1 113.67(19) . . ?
N1 C1 C2 111.2(3) . . ?
O1 C2 C1 107.1(3) . . ?
O1 C3 C4 108.0(3) . . ?
O2 C4 C3 106.8(3) . . ?
O2 C5 C6 106.5(3) . . ?
N2 C6 C5 111.3(3) . . ?
N1 C7 C8 111.6(3) . . ?
O3 C8 C7 106.4(3) . . ?
O3 C9 C10 106.5(3) . . ?
O4 C10 C9 107.5(3) . . ?
O4 C11 C12 107.9(3) . . ?
N2 C12 C11 111.3(3) . . ?
N1 C13 C14 112.3(3) . . ?
O5 C14 C13 107.7(3) . . ?
O5 C15 C16 107.7(3) . . ?
O6 C16 C15 107.8(3) . . ?
O6 C17 C18 107.8(3) . . ?
N2 C18 C17 112.8(3) . . ?
Cl1 C19 Cl2 111.0(2) . . ?
Cl3 C20 Cl4 111.65(19) . . ?
Cl5 C21 Cl6 111.5(2) . . ?

_refine_diff_density_max         0.880
_refine_diff_density_min         -0.608
_refine_diff_density_rms         0.122


_chemical_properties_physical    Moisture-sensitive
####################################################################### 
# 
# 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_cjw56
_database_code_depnum_ccdc_archive 'CCDC 1852098'
_audit_update_record             
;
2018-08-10 deposited with the CCDC.
2018-08-15 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         ?
_chemical_formula_sum            'C18 H38 I3 N2 O7 U'
_chemical_formula_weight         1013.23

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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/n'
_space_group_name_Hall           '-P 2yn'

_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+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   10.8943(11)
_cell_length_b                   19.313(2)
_cell_length_c                   13.3229(14)
_cell_angle_alpha                90
_cell_angle_beta                 96.0099(13)
_cell_angle_gamma                90
_cell_volume                     2787.8(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    133(2)
_cell_measurement_reflns_used    9851
_cell_measurement_theta_min      2.16
_cell_measurement_theta_max      28.65

_exptl_crystal_description       irregular
_exptl_crystal_colour            green
_exptl_crystal_density_meas      not_measured
_exptl_crystal_density_method    not_measured
_exptl_crystal_density_diffrn    2.414
_exptl_crystal_F_000             1868
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.404
_exptl_crystal_size_mid          0.241
_exptl_crystal_size_min          0.154
_exptl_absorpt_coefficient_mu    9.181
_shelx_estimated_absorpt_T_min   0.119
_shelx_estimated_absorpt_T_max   0.332
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3056
_exptl_absorpt_correction_T_max  0.4316
_exptl_absorpt_process_details   'Bruker SADABS 2014/5'
_exptl_absorpt_special_details   
;
Reflections not merged
33397 Corrected reflections written to file cjw56s.hkl
Estimated minimum and maximum transmission:  0.3056  0.4316
The ratio (0.7081) of these values is more reliable than their 
absolute values. Additional spherical absorption correction 
applied with mu*r =  0.6000. Lambda/2 correction factor = 0.00150
;

_diffrn_ambient_temperature      133(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            31414
_diffrn_reflns_av_unetI/netI     0.0362
_diffrn_reflns_av_R_equivalents  0.0494
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.864
_diffrn_reflns_theta_max         27.103
_diffrn_reflns_theta_full        25.500
_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             6137
_reflns_number_gt                5617
_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       'Bruker APEX2 2014.11-0, 2014'
_computing_cell_refinement       'Bruker SAINT 8.34a, 2013'
_computing_data_reduction        'Bruker SAINT 8.34a, 2013'
_computing_structure_solution    'Bruker SHELXTL 2014/4'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
A green crystal of approximate dimensions 0.154 x 0.241 x 0.404 mm 
was mounted in a cryoloop and transferred to a Bruker SMART APEX II 
diffractometer.  The APEX2 program package was used to determine 
the unit-cell parameters and for data collection (20 sec/frame scan 
time for a sphere of diffraction data).  The raw frame data was 
processed using SAINT and SADABS to yield the reflection data file.  
Subsequent calculations were carried out using the SHELXTL program.  
The diffraction symmetry was 2/m and the systematic absences were 
consistent with the monoclinic space group P21/n that was later 
determined to be correct.

The structure was solved by dual space methods and refined on F2 by 
full-matrix least-squares techniques.  The analytical scattering 
factors for neutral atoms were used throughout the analysis.  
Hydrogen atoms H(71) and H(72) were located from a difference-map 
and refined (x,y,z and Uiso).  The remaining hydrogen atoms were 
included using a riding model.

At convergence, wR2 = 0.1096 and Goof = 1.257 for 288 variables 
refined against 6137 data (0.78Å), R1 = 0.0474 for those 5617 
data with I > 2.0sigma(I).
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0244P)²+46.0217P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6137
_refine_ls_number_parameters     288
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0523
_refine_ls_R_factor_gt           0.0474
_refine_ls_wR_factor_ref         0.1096
_refine_ls_wR_factor_gt          0.1077
_refine_ls_goodness_of_fit_ref   1.257
_refine_ls_restrained_S_all      1.257
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

# start Validation Reply Form
_vrf_PLAT213_cjw56               
;
PROBLEM: Atom C8              has ADP max/min Ratio .....        5.0 prolat
RESPONSE: ...No residual density was seen near atom C8. Significant 
disorder was not observed.  
;
_vrf_PLAT410_cjw56               
;
PROBLEM: Short Intra H...H Contact  H8A      ..H14B             1.84 Ang.  
RESPONSE: ...Short H-H distances were due to hydrogen atoms
being included in calculated positions.
;
_vrf_PLAT971_cjw56               
;
PROBLEM: Check Calcd Resid. Dens.  0.92A   From U1              2.83 eA-3  
RESPONSE: ...Residual density (around uranium) is often observed with 
elements of high atomic number.
;
# end Validation Reply Form

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 0.24776(3) 0.61190(2) 0.20497(2) 0.01542(9) Uani 1 1 d . . . . .
I1 I 0.22220(6) 0.46412(3) 0.08696(5) 0.02931(16) Uani 1 1 d . . . . .
I2 I 0.68859(5) 0.65991(3) 0.42483(5) 0.02433(14) Uani 1 1 d . . . . .
I3 I 0.27697(6) 0.66421(4) 0.60792(5) 0.03365(17) Uani 1 1 d . . . . .
O1 O 0.2675(7) 0.5167(4) 0.3474(6) 0.040(2) Uani 1 1 d . . . . .
O2 O 0.4635(6) 0.5493(3) 0.2550(5) 0.0244(14) Uani 1 1 d . . . . .
O3 O 0.1270(7) 0.7028(5) 0.3001(7) 0.049(2) Uani 1 1 d . . . . .
O4 O 0.2983(7) 0.7439(4) 0.1827(6) 0.0367(18) Uani 1 1 d . . . . .
O5 O 0.0307(6) 0.6377(4) 0.1097(6) 0.0307(16) Uani 1 1 d . . . . .
O6 O 0.2191(6) 0.6364(3) 0.0057(5) 0.0224(13) Uani 1 1 d . . . . .
O7 O 0.3710(6) 0.6612(4) 0.3620(5) 0.0280(16) Uani 1 1 d . . . . .
H71 H 0.456(16) 0.658(8) 0.374(12) 0.08(5) Uiso 1 1 d . . . . .
H72 H 0.349(14) 0.671(8) 0.424(12) 0.06(5) Uiso 1 1 d . . . . .
N1 N 0.0396(8) 0.5673(6) 0.2930(7) 0.039(2) Uani 1 1 d . . . . .
N2 N 0.4477(7) 0.6426(5) 0.0948(6) 0.0274(18) Uani 1 1 d . . . . .
C1 C 0.0542(13) 0.4939(9) 0.3274(10) 0.060(4) Uani 1 1 d . . . . .
H1A H -0.0166 0.4806 0.3641 0.072 Uiso 1 1 calc R U . . .
H1B H 0.0551 0.4631 0.2681 0.072 Uiso 1 1 calc R U . . .
C2 C 0.1701(14) 0.4855(8) 0.3941(10) 0.060(4) Uani 1 1 d . . . . .
H2A H 0.1625 0.5078 0.4601 0.072 Uiso 1 1 calc R U . . .
H2B H 0.1876 0.4357 0.4059 0.072 Uiso 1 1 calc R U . . .
C3 C 0.3889(12) 0.4998(7) 0.3967(10) 0.048(3) Uani 1 1 d . . . . .
H3A H 0.3849 0.4570 0.4371 0.057 Uiso 1 1 calc R U . . .
H3B H 0.4193 0.5379 0.4426 0.057 Uiso 1 1 calc R U . . .
C4 C 0.4726(11) 0.4899(6) 0.3185(9) 0.040(3) Uani 1 1 d . . . . .
H4A H 0.5585 0.4843 0.3500 0.048 Uiso 1 1 calc R U . . .
H4B H 0.4492 0.4478 0.2786 0.048 Uiso 1 1 calc R U . . .
C5 C 0.5627(9) 0.5515(6) 0.1926(8) 0.037(3) Uani 1 1 d . . . . .
H5A H 0.5490 0.5168 0.1378 0.044 Uiso 1 1 calc R U . . .
H5B H 0.6418 0.5407 0.2331 0.044 Uiso 1 1 calc R U . . .
C6 C 0.5673(9) 0.6217(7) 0.1495(8) 0.036(3) Uani 1 1 d . . . . .
H6A H 0.6319 0.6233 0.1025 0.043 Uiso 1 1 calc R U . . .
H6B H 0.5902 0.6552 0.2045 0.043 Uiso 1 1 calc R U . . .
C7 C 0.0313(11) 0.6112(9) 0.3824(9) 0.055(4) Uani 1 1 d . . . . .
H7A H 0.1027 0.6011 0.4325 0.066 Uiso 1 1 calc R U . . .
H7B H -0.0445 0.5989 0.4133 0.066 Uiso 1 1 calc R U . . .
C8 C 0.0291(11) 0.6873(10) 0.3605(11) 0.071(6) Uani 1 1 d . . . . .
H8A H -0.0513 0.7004 0.3239 0.086 Uiso 1 1 calc R U . . .
H8B H 0.0403 0.7138 0.4244 0.086 Uiso 1 1 calc R U . . .
C9 C 0.1252(13) 0.7738(7) 0.2691(13) 0.068(5) Uani 1 1 d . . . . .
H9A H 0.0964 0.8035 0.3224 0.081 Uiso 1 1 calc R U . . .
H9B H 0.0684 0.7798 0.2067 0.081 Uiso 1 1 calc R U . . .
C10 C 0.2547(12) 0.7933(6) 0.2504(11) 0.052(4) Uani 1 1 d . . . . .
H10A H 0.2553 0.8403 0.2206 0.062 Uiso 1 1 calc R U . . .
H10B H 0.3089 0.7935 0.3148 0.062 Uiso 1 1 calc R U . . .
C11 C 0.4240(11) 0.7596(6) 0.1629(10) 0.042(3) Uani 1 1 d . . . . .
H11A H 0.4823 0.7479 0.2225 0.051 Uiso 1 1 calc R U . . .
H11B H 0.4321 0.8096 0.1484 0.051 Uiso 1 1 calc R U . . .
C12 C 0.4516(11) 0.7184(7) 0.0756(9) 0.043(3) Uani 1 1 d . . . . .
H12A H 0.5347 0.7310 0.0578 0.051 Uiso 1 1 calc R U . . .
H12B H 0.3912 0.7299 0.0173 0.051 Uiso 1 1 calc R U . . .
C13 C -0.0745(10) 0.5720(9) 0.2217(9) 0.055(4) Uani 1 1 d . . . . .
H13A H -0.1464 0.5725 0.2614 0.066 Uiso 1 1 calc R U . . .
H13B H -0.0808 0.5297 0.1796 0.066 Uiso 1 1 calc R U . . .
C14 C -0.0835(9) 0.6332(8) 0.1535(8) 0.043(3) Uani 1 1 d . . . . .
H14A H -0.1531 0.6275 0.1001 0.052 Uiso 1 1 calc R U . . .
H14B H -0.0974 0.6758 0.1921 0.052 Uiso 1 1 calc R U . . .
C15 C 0.0220(9) 0.6794(5) 0.0209(9) 0.035(3) Uani 1 1 d . . . . .
H15A H 0.0513 0.7270 0.0373 0.042 Uiso 1 1 calc R U . . .
H15B H -0.0645 0.6817 -0.0102 0.042 Uiso 1 1 calc R U . . .
C16 C 0.1014(9) 0.6458(5) -0.0486(8) 0.028(2) Uani 1 1 d . . . . .
H16A H 0.0660 0.6006 -0.0716 0.033 Uiso 1 1 calc R U . . .
H16B H 0.1080 0.6754 -0.1085 0.033 Uiso 1 1 calc R U . . .
C17 C 0.3100(9) 0.6229(7) -0.0628(8) 0.035(3) Uani 1 1 d . . . . .
H17A H 0.3224 0.6646 -0.1038 0.042 Uiso 1 1 calc R U . . .
H17B H 0.2822 0.5845 -0.1090 0.042 Uiso 1 1 calc R U . . .
C18 C 0.4281(9) 0.6036(7) -0.0008(7) 0.036(3) Uani 1 1 d . . . . .
H18A H 0.4270 0.5535 0.0144 0.044 Uiso 1 1 calc R U . . .
H18B H 0.4982 0.6125 -0.0408 0.044 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 O7 2.549(7) . ?
U1 O3 2.602(7) . ?
U1 O5 2.612(7) . ?
U1 O4 2.632(7) . ?
U1 O1 2.635(7) . ?
U1 O2 2.665(6) . ?
U1 O6 2.683(6) . ?
U1 N1 2.796(8) . ?
U1 N2 2.814(8) . ?
U1 I1 3.2564(7) . ?
I2 H71 2.55(18) . ?
I3 H72 2.66(16) . ?
O1 C2 1.420(14) . ?
O1 C3 1.451(14) . ?
O2 C4 1.422(12) . ?
O2 C5 1.431(12) . ?
O3 C9 1.430(18) . ?
O3 C8 1.434(17) . ?
O4 C10 1.428(15) . ?
O4 C11 1.453(14) . ?
O5 C15 1.426(13) . ?
O5 C14 1.432(12) . ?
O6 C16 1.417(11) . ?
O6 C17 1.439(12) . ?
O7 H71 0.92(18) . ?
O7 H72 0.90(16) . ?
N1 C7 1.473(16) . ?
N1 C13 1.486(14) . ?
N1 C1 1.492(19) . ?
N2 C18 1.476(14) . ?
N2 C6 1.480(13) . ?
N2 C12 1.488(15) . ?
C1 C2 1.48(2) . ?
C3 C4 1.467(19) . ?
C5 C6 1.476(17) . ?
C7 C8 1.50(2) . ?
C9 C10 1.51(2) . ?
C11 C12 1.466(18) . ?
C13 C14 1.49(2) . ?
C15 C16 1.482(16) . ?
C17 C18 1.502(15) . ?

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
O7 U1 O3 66.3(2) . . ?
O7 U1 O5 134.4(2) . . ?
O3 U1 O5 68.3(2) . . ?
O7 U1 O4 68.4(2) . . ?
O3 U1 O4 61.5(3) . . ?
O5 U1 O4 87.1(2) . . ?
O7 U1 O1 70.9(2) . . ?
O3 U1 O1 97.4(3) . . ?
O5 U1 O1 119.0(2) . . ?
O4 U1 O1 139.0(2) . . ?
O7 U1 O2 65.7(2) . . ?
O3 U1 O2 131.5(2) . . ?
O5 U1 O2 159.7(2) . . ?
O4 U1 O2 106.2(2) . . ?
O1 U1 O2 60.0(2) . . ?
O7 U1 O6 138.0(2) . . ?
O3 U1 O6 110.5(3) . . ?
O5 U1 O6 58.7(2) . . ?
O4 U1 O6 73.8(2) . . ?
O1 U1 O6 145.9(2) . . ?
O2 U1 O6 109.6(2) . . ?
O7 U1 N1 98.7(2) . . ?
O3 U1 N1 62.0(3) . . ?
O5 U1 N1 62.0(3) . . ?
O4 U1 N1 122.3(3) . . ?
O1 U1 N1 59.5(3) . . ?
O2 U1 N1 119.2(3) . . ?
O6 U1 N1 117.0(2) . . ?
O7 U1 N2 88.8(2) . . ?
O3 U1 N2 124.8(3) . . ?
O5 U1 N2 114.7(2) . . ?
O4 U1 N2 63.6(3) . . ?
O1 U1 N2 120.9(3) . . ?
O2 U1 N2 61.0(2) . . ?
O6 U1 N2 57.5(2) . . ?
N1 U1 N2 171.8(3) . . ?
O7 U1 I1 137.27(17) . . ?
O3 U1 I1 143.59(18) . . ?
O5 U1 I1 84.56(16) . . ?
O4 U1 I1 143.42(18) . . ?
O1 U1 I1 74.46(19) . . ?
O2 U1 I1 75.61(14) . . ?
O6 U1 I1 71.42(14) . . ?
N1 U1 I1 84.3(2) . . ?
N2 U1 I1 87.96(19) . . ?
C2 O1 C3 113.2(9) . . ?
C2 O1 U1 127.1(8) . . ?
C3 O1 U1 119.0(6) . . ?
C4 O2 C5 111.1(8) . . ?
C4 O2 U1 121.3(6) . . ?
C5 O2 U1 122.7(6) . . ?
C9 O3 C8 111.9(11) . . ?
C9 O3 U1 119.9(8) . . ?
C8 O3 U1 125.2(9) . . ?
C10 O4 C11 110.9(9) . . ?
C10 O4 U1 119.3(8) . . ?
C11 O4 U1 115.8(6) . . ?
C15 O5 C14 112.8(8) . . ?
C15 O5 U1 119.3(6) . . ?
C14 O5 U1 124.9(6) . . ?
C16 O6 C17 110.2(7) . . ?
C16 O6 U1 122.2(6) . . ?
C17 O6 U1 125.4(6) . . ?
U1 O7 H71 123(10) . . ?
U1 O7 H72 131(10) . . ?
H71 O7 H72 102(10) . . ?
C7 N1 C13 111.3(10) . . ?
C7 N1 C1 108.2(11) . . ?
C13 N1 C1 108.1(10) . . ?
C7 N1 U1 106.4(7) . . ?
C13 N1 U1 111.9(6) . . ?
C1 N1 U1 110.9(7) . . ?
C18 N2 C6 109.1(8) . . ?
C18 N2 C12 111.0(9) . . ?
C6 N2 C12 108.2(8) . . ?
C18 N2 U1 107.1(5) . . ?
C6 N2 U1 112.1(6) . . ?
C12 N2 U1 109.5(7) . . ?
C2 C1 N1 110.3(10) . . ?
O1 C2 C1 108.7(10) . . ?
O1 C3 C4 108.2(10) . . ?
O2 C4 C3 107.9(9) . . ?
O2 C5 C6 108.2(8) . . ?
C5 C6 N2 112.2(9) . . ?
N1 C7 C8 114.2(11) . . ?
O3 C8 C7 108.5(10) . . ?
O3 C9 C10 107.6(9) . . ?
O4 C10 C9 108.4(9) . . ?
O4 C11 C12 107.8(8) . . ?
C11 C12 N2 112.7(9) . . ?
N1 C13 C14 115.9(10) . . ?
O5 C14 C13 107.1(9) . . ?
O5 C15 C16 106.1(8) . . ?
O6 C16 C15 107.0(8) . . ?
O6 C17 C18 107.6(8) . . ?
N2 C18 C17 112.8(10) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O7 H71 I2 0.92(18) 2.55(18) 3.473(7) 173(14) .
O7 H72 I3 0.90(16) 2.66(16) 3.535(8) 166(13) .

_refine_diff_density_max         2.792
_refine_diff_density_min         -1.209
_refine_diff_density_rms         0.243

####################################################################### 
# 
# 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_dnh54
_database_code_depnum_ccdc_archive 'CCDC 1852097'
_audit_update_record             
;
2018-06-27 deposited with the CCDC.
2018-08-15 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         ?
_chemical_formula_sum            'C44 H61 B I2 N3 O7 U'
_chemical_formula_weight         1246.59

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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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/n'
_space_group_name_Hall           '-P 2yn'

_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+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   20.142(3)
_cell_length_b                   9.6317(16)
_cell_length_c                   26.979(5)
_cell_angle_alpha                90
_cell_angle_beta                 107.307(2)
_cell_angle_gamma                90
_cell_volume                     4996.9(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    133(2)
_cell_measurement_reflns_used    9993
_cell_measurement_theta_min      2.23
_cell_measurement_theta_max      27.77

_exptl_crystal_description       rectangle
_exptl_crystal_colour            green
_exptl_crystal_density_meas      not_measured
_exptl_crystal_density_method    not_measured
_exptl_crystal_density_diffrn    1.657
_exptl_crystal_F_000             2420
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.207
_exptl_crystal_size_mid          0.136
_exptl_crystal_size_min          0.121
_exptl_absorpt_coefficient_mu    4.531
_shelx_estimated_absorpt_T_min   0.454
_shelx_estimated_absorpt_T_max   0.610
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3498
_exptl_absorpt_correction_T_max  0.4311
_exptl_absorpt_process_details   'Bruker SADABS 2014/5'
_exptl_absorpt_special_details   
; 
Reflections not merged 
60734 Corrected reflections written to file dnh54s.hkl 
Estimated minimum and maximum transmission:  0.3498  0.4311 
The ratio (0.8114) of these values is more reliable than their absolute values 
Additional spherical absorption correction applied with mu*r =  0.6000 
Lambda/2 correction factor = 0.00150 
;
_diffrn_ambient_temperature      133(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            58739
_diffrn_reflns_av_unetI/netI     0.0503
_diffrn_reflns_av_R_equivalents  0.0588
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       25
_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         1.498
_diffrn_reflns_theta_max         28.343
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             12099
_reflns_number_gt                9551
_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       'Bruker APEX2 2014.11-0, 2014'
_computing_cell_refinement       'Bruker SAINT 8.34a, 2013'
_computing_data_reduction        'Bruker SAINT 8.34a, 2013'
_computing_structure_solution    'Bruker SHELXTL 2014/4'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;A green crystal of approximate dimensions 0.121 x 0.136 x 207 mm was 
mounted in a cryoloop and transferred to a Bruker SMART APEX II 
diffractometer.  The APEX2 program package was used to determine the 
unit-cell parameters and for data collection (20 sec/frame scan time for 
a sphere of diffraction data).  The raw frame data was processed using 
SAINT and SADABS to yield the reflection data file.  Subsequent 
calculations were carried out using the SHELXTL program.  The diffraction 
symmetry was 2/m and the systematic absences were consistent with the 
monoclinic space group P21/n that was later determined to be correct.

The structure was solved by dual space methods and refined on F2 by 
full-matrix least-squares techniques.  The analytical scattering factors 
for neutral atoms were used throughout the analysis.  Hydrogen atoms were 
included using a riding model.  There was one molecule of acetonitrile 
solvent present.

Least-squares analysis yielded wR2 = 0.0766 and Goof = 1.019 for 525 
variables refined against 12099 data (0.75 Å), R1 = 0.0346 for those 9551 
data with I > 2.0sigma(I).  

There were several high residuals present in the final difference-Fourier 
map.  It was not possible to determine the nature of the residuals although 
it was probable that either acetonitrile or diethylether solvent was present.  
The SQUEEZE routine in the PLATON program package was used to account 
for the electrons in the solvent accessible voids.,SQUEEZE
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0353P)²+1.5018P] 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         12099
_refine_ls_number_parameters     525
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0528
_refine_ls_R_factor_gt           0.0346
_refine_ls_wR_factor_ref         0.0766
_refine_ls_wR_factor_gt          0.0709
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_restrained_S_all      1.019
_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 0.70596(2) 0.66013(2) 0.46916(2) 0.01760(5) Uani 1 1 d . . . . .
I1 I 0.78019(2) 0.95753(3) 0.45828(2) 0.02805(7) Uani 1 1 d . . . . .
I2 I 0.42798(2) 0.71025(3) 0.43984(2) 0.03415(8) Uani 1 1 d . . . . .
O1 O 0.59611(15) 0.5771(3) 0.48471(11) 0.0251(7) Uani 1 1 d . . . . .
H1A H 0.5535 0.6131 0.4724 0.038 Uiso 1 1 d R U . . .
H1B H 0.5908 0.5049 0.5039 0.038 Uiso 1 1 d R U . . .
O2 O 0.68209(15) 0.8237(3) 0.53972(11) 0.0245(6) Uani 1 1 d . . . . .
O3 O 0.60112(14) 0.8383(3) 0.44255(10) 0.0200(6) Uani 1 1 d . . . . .
O4 O 0.71771(15) 0.4337(3) 0.52398(11) 0.0268(7) Uani 1 1 d . . . . .
O5 O 0.66767(14) 0.4264(3) 0.41964(11) 0.0234(6) Uani 1 1 d . . . . .
O6 O 0.82875(18) 0.5463(4) 0.48863(14) 0.0494(10) Uani 1 1 d . . . . .
O7 O 0.76600(15) 0.6384(3) 0.39405(12) 0.0297(7) Uani 1 1 d . . . . .
N1 N 0.79706(19) 0.6624(4) 0.57140(14) 0.0291(8) Uani 1 1 d . . . . .
N2 N 0.63169(18) 0.6824(3) 0.36459(13) 0.0230(8) Uani 1 1 d . . . . .
C1 C 0.8002(2) 0.8056(5) 0.59208(18) 0.0340(11) Uani 1 1 d . . . . .
H1C H 0.8223 0.8671 0.5721 0.041 Uiso 1 1 calc R U . . .
H1D H 0.8296 0.8063 0.6287 0.041 Uiso 1 1 calc R U . . .
C2 C 0.7293(2) 0.8617(5) 0.58903(17) 0.0336(11) Uani 1 1 d . . . . .
H2A H 0.7133 0.8225 0.6174 0.040 Uiso 1 1 calc R U . . .
H2B H 0.7312 0.9640 0.5927 0.040 Uiso 1 1 calc R U . . .
C3 C 0.6148(2) 0.8855(4) 0.53058(16) 0.0237(9) Uani 1 1 d . . . . .
H3A H 0.6166 0.9595 0.5564 0.028 Uiso 1 1 calc R U . . .
H3B H 0.5807 0.8146 0.5337 0.028 Uiso 1 1 calc R U . . .
C4 C 0.5939(2) 0.9448(4) 0.47733(16) 0.0228(9) Uani 1 1 d . . . . .
H4A H 0.5451 0.9772 0.4679 0.027 Uiso 1 1 calc R U . . .
H4B H 0.6240 1.0248 0.4756 0.027 Uiso 1 1 calc R U . . .
C5 C 0.5663(2) 0.8740(4) 0.39005(16) 0.0289(10) Uani 1 1 d . . . . .
H5A H 0.5920 0.9483 0.3783 0.035 Uiso 1 1 calc R U . . .
H5B H 0.5188 0.9082 0.3869 0.035 Uiso 1 1 calc R U . . .
C6 C 0.5626(2) 0.7462(4) 0.35746(16) 0.0277(10) Uani 1 1 d . . . . .
H6A H 0.5317 0.6774 0.3666 0.033 Uiso 1 1 calc R U . . .
H6B H 0.5420 0.7708 0.3204 0.033 Uiso 1 1 calc R U . . .
C7 C 0.7650(3) 0.5670(4) 0.60054(17) 0.0330(11) Uani 1 1 d . . . . .
H7A H 0.7191 0.6040 0.6004 0.040 Uiso 1 1 calc R U . . .
H7B H 0.7947 0.5623 0.6371 0.040 Uiso 1 1 calc R U . . .
C8 C 0.7559(3) 0.4237(5) 0.57781(17) 0.0348(11) Uani 1 1 d . . . . .
H8A H 0.8019 0.3809 0.5818 0.042 Uiso 1 1 calc R U . . .
H8B H 0.7304 0.3649 0.5961 0.042 Uiso 1 1 calc R U . . .
C9 C 0.7202(2) 0.3043(4) 0.49814(18) 0.0302(10) Uani 1 1 d . . . . .
H9A H 0.7150 0.2258 0.5204 0.036 Uiso 1 1 calc R U . . .
H9B H 0.7654 0.2947 0.4909 0.036 Uiso 1 1 calc R U . . .
C10 C 0.6624(2) 0.3038(4) 0.44878(17) 0.0264(10) Uani 1 1 d . . . . .
H10A H 0.6653 0.2197 0.4284 0.032 Uiso 1 1 calc R U . . .
H10B H 0.6172 0.3028 0.4562 0.032 Uiso 1 1 calc R U . . .
C11 C 0.6077(2) 0.4353(4) 0.37376(16) 0.0281(10) Uani 1 1 d . . . . .
H11A H 0.5657 0.4594 0.3838 0.034 Uiso 1 1 calc R U . . .
H11B H 0.5996 0.3447 0.3556 0.034 Uiso 1 1 calc R U . . .
C12 C 0.6214(2) 0.5440(4) 0.33897(16) 0.0263(10) Uani 1 1 d . . . . .
H12A H 0.5816 0.5486 0.3069 0.032 Uiso 1 1 calc R U . . .
H12B H 0.6634 0.5188 0.3291 0.032 Uiso 1 1 calc R U . . .
C13 C 0.8694(2) 0.6171(5) 0.5753(2) 0.0387(12) Uani 1 1 d . . . . .
H13A H 0.9030 0.6774 0.6004 0.046 Uiso 1 1 calc R U . . .
H13B H 0.8764 0.5206 0.5885 0.046 Uiso 1 1 calc R U . . .
C14 C 0.8826(3) 0.6244(6) 0.5240(2) 0.0532(16) Uani 1 1 d . . . . .
H14A H 0.8815 0.7221 0.5123 0.064 Uiso 1 1 calc R U . . .
H14B H 0.9287 0.5845 0.5263 0.064 Uiso 1 1 calc R U . . .
C15 C 0.8450(3) 0.4867(7) 0.4442(3) 0.0639(18) Uani 1 1 d . . . . .
H15A H 0.8940 0.4547 0.4547 0.077 Uiso 1 1 calc R U . . .
H15B H 0.8148 0.4053 0.4313 0.077 Uiso 1 1 calc R U . . .
C16 C 0.8348(3) 0.5871(6) 0.4037(2) 0.0490(14) Uani 1 1 d . . . . .
H16A H 0.8689 0.6636 0.4146 0.059 Uiso 1 1 calc R U . . .
H16B H 0.8407 0.5438 0.3720 0.059 Uiso 1 1 calc R U . . .
C17 C 0.7441(3) 0.7148(5) 0.34635(18) 0.0389(12) Uani 1 1 d . . . . .
H17A H 0.7429 0.6530 0.3168 0.047 Uiso 1 1 calc R U . . .
H17B H 0.7772 0.7912 0.3469 0.047 Uiso 1 1 calc R U . . .
C18 C 0.6728(2) 0.7730(5) 0.34016(17) 0.0318(11) Uani 1 1 d . . . . .
H18A H 0.6773 0.8663 0.3562 0.038 Uiso 1 1 calc R U . . .
H18B H 0.6478 0.7833 0.3027 0.038 Uiso 1 1 calc R U . . .
B1 B 0.5130(2) 0.1578(5) 0.22618(18) 0.0239(10) Uani 1 1 d . . . . .
C19 C 0.5945(2) 0.2130(4) 0.24677(15) 0.0204(8) Uani 1 1 d . . . . .
C20 C 0.6199(2) 0.3245(4) 0.22514(17) 0.0276(10) Uani 1 1 d . . . . .
H20A H 0.5899 0.3694 0.1956 0.033 Uiso 1 1 calc R U . . .
C21 C 0.6878(3) 0.3724(5) 0.24533(19) 0.0344(11) Uani 1 1 d . . . . .
H21A H 0.7030 0.4499 0.2298 0.041 Uiso 1 1 calc R U . . .
C22 C 0.7331(2) 0.3090(5) 0.2874(2) 0.0382(12) Uani 1 1 d . . . . .
H22A H 0.7798 0.3401 0.3003 0.046 Uiso 1 1 calc R U . . .
C23 C 0.7099(2) 0.1996(5) 0.31071(19) 0.0366(12) Uani 1 1 d . . . . .
H23A H 0.7402 0.1562 0.3405 0.044 Uiso 1 1 calc R U . . .
C24 C 0.6416(2) 0.1531(5) 0.29022(17) 0.0292(10) Uani 1 1 d . . . . .
H24A H 0.6265 0.0772 0.3066 0.035 Uiso 1 1 calc R U . . .
C25 C 0.5106(2) -0.0112(5) 0.22174(15) 0.0281(10) Uani 1 1 d . . . . .
C26 C 0.5641(3) -0.0896(5) 0.21217(17) 0.0340(11) Uani 1 1 d . . . . .
H26A H 0.6055 -0.0426 0.2121 0.041 Uiso 1 1 calc R U . . .
C27 C 0.5604(3) -0.2338(5) 0.20267(19) 0.0455(14) Uani 1 1 d . . . . .
H27A H 0.5980 -0.2814 0.1958 0.055 Uiso 1 1 calc R U . . .
C28 C 0.5020(4) -0.3036(6) 0.20352(19) 0.0510(16) Uani 1 1 d . . . . .
H28A H 0.4987 -0.4008 0.1972 0.061 Uiso 1 1 calc R U . . .
C29 C 0.4480(3) -0.2342(6) 0.21344(18) 0.0529(17) Uani 1 1 d . . . . .
H29A H 0.4080 -0.2843 0.2149 0.064 Uiso 1 1 calc R U . . .
C30 C 0.4511(3) -0.0880(5) 0.22161(17) 0.0389(12) Uani 1 1 d . . . . .
H30A H 0.4123 -0.0415 0.2271 0.047 Uiso 1 1 calc R U . . .
C31 C 0.4773(2) 0.2188(5) 0.26919(17) 0.0280(10) Uani 1 1 d . . . . .
C32 C 0.4668(3) 0.1376(5) 0.30915(18) 0.0381(12) Uani 1 1 d . . . . .
H32A H 0.4774 0.0413 0.3100 0.046 Uiso 1 1 calc R U . . .
C33 C 0.4417(3) 0.1915(6) 0.3475(2) 0.0543(16) Uani 1 1 d . . . . .
H33A H 0.4357 0.1319 0.3739 0.065 Uiso 1 1 calc R U . . .
C34 C 0.4252(3) 0.3299(6) 0.3482(2) 0.0494(15) Uani 1 1 d . . . . .
H34A H 0.4078 0.3662 0.3746 0.059 Uiso 1 1 calc R U . . .
C35 C 0.4346(2) 0.4159(6) 0.30916(19) 0.0392(12) Uani 1 1 d . . . . .
H35A H 0.4228 0.5115 0.3082 0.047 Uiso 1 1 calc R U . . .
C36 C 0.4615(2) 0.3600(5) 0.27174(18) 0.0321(11) Uani 1 1 d . . . . .
H36A H 0.4697 0.4208 0.2464 0.038 Uiso 1 1 calc R U . . .
C37 C 0.4749(2) 0.2124(4) 0.16624(16) 0.0237(9) Uani 1 1 d . . . . .
C38 C 0.5013(2) 0.1681(5) 0.12663(16) 0.0267(10) Uani 1 1 d . . . . .
H38A H 0.5412 0.1098 0.1356 0.032 Uiso 1 1 calc R U . . .
C39 C 0.4728(2) 0.2041(5) 0.07481(17) 0.0306(10) Uani 1 1 d . . . . .
H39A H 0.4930 0.1705 0.0495 0.037 Uiso 1 1 calc R U . . .
C40 C 0.4150(2) 0.2885(5) 0.06013(18) 0.0327(11) Uani 1 1 d . . . . .
H40A H 0.3953 0.3149 0.0249 0.039 Uiso 1 1 calc R U . . .
C41 C 0.3867(2) 0.3337(4) 0.09798(18) 0.0322(11) Uani 1 1 d . . . . .
H41A H 0.3468 0.3919 0.0885 0.039 Uiso 1 1 calc R U . . .
C42 C 0.4153(2) 0.2958(4) 0.14995(17) 0.0275(10) Uani 1 1 d . . . . .
H42A H 0.3939 0.3273 0.1749 0.033 Uiso 1 1 calc R U . . .
N3 N 0.9627(4) 1.2622(7) 0.4410(3) 0.091(2) Uani 1 1 d . . . . .
C43 C 0.9518(3) 1.1551(7) 0.4256(2) 0.0495(14) Uani 1 1 d . . . . .
C44 C 0.9399(4) 1.0196(6) 0.4058(3) 0.076(2) Uani 1 1 d . . . . .
H44A H 0.9792 0.9900 0.3939 0.114 Uiso 1 1 calc R U . . .
H44B H 0.8971 1.0176 0.3767 0.114 Uiso 1 1 calc R U . . .
H44C H 0.9353 0.9566 0.4332 0.114 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 2.503(3) . ?
U1 O4 2.606(3) . ?
U1 O6 2.612(3) . ?
U1 O5 2.615(3) . ?
U1 O2 2.623(3) . ?
U1 O3 2.649(3) . ?
U1 O7 2.659(3) . ?
U1 N2 2.780(3) . ?
U1 N1 2.822(4) . ?
U1 I1 3.2844(5) . ?
O2 C3 1.432(5) . ?
O2 C2 1.433(5) . ?
O3 C5 1.423(5) . ?
O3 C4 1.427(4) . ?
O4 C8 1.430(5) . ?
O4 C9 1.436(5) . ?
O5 C10 1.440(5) . ?
O5 C11 1.453(5) . ?
O6 C14 1.427(7) . ?
O6 C15 1.453(7) . ?
O7 C16 1.421(6) . ?
O7 C17 1.433(6) . ?
N1 C7 1.476(6) . ?
N1 C1 1.483(5) . ?
N1 C13 1.494(6) . ?
N2 C6 1.480(5) . ?
N2 C18 1.486(5) . ?
N2 C12 1.487(5) . ?
C1 C2 1.507(7) . ?
C3 C4 1.486(6) . ?
C5 C6 1.502(6) . ?
C7 C8 1.499(6) . ?
C9 C10 1.486(6) . ?
C11 C12 1.485(6) . ?
C13 C14 1.487(7) . ?
C15 C16 1.427(8) . ?
C17 C18 1.503(7) . ?
B1 C25 1.632(7) . ?
B1 C31 1.645(6) . ?
B1 C19 1.655(6) . ?
B1 C37 1.656(6) . ?
C19 C20 1.391(6) . ?
C19 C24 1.395(6) . ?
C20 C21 1.392(6) . ?
C21 C22 1.369(7) . ?
C22 C23 1.378(7) . ?
C23 C24 1.395(6) . ?
C25 C26 1.402(7) . ?
C25 C30 1.407(6) . ?
C26 C27 1.410(7) . ?
C27 C28 1.360(8) . ?
C28 C29 1.368(8) . ?
C29 C30 1.424(7) . ?
C31 C32 1.398(6) . ?
C31 C36 1.403(6) . ?
C32 C33 1.381(7) . ?
C33 C34 1.375(8) . ?
C34 C35 1.396(7) . ?
C35 C36 1.388(6) . ?
C37 C38 1.394(6) . ?
C37 C42 1.402(6) . ?
C38 C39 1.388(6) . ?
C39 C40 1.377(6) . ?
C40 C41 1.381(7) . ?
C41 C42 1.397(6) . ?
N3 C43 1.109(7) . ?
C43 C44 1.403(8) . ?

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 O4 64.71(9) . . ?
O1 U1 O6 131.57(11) . . ?
O4 U1 O6 67.29(11) . . ?
O1 U1 O5 70.68(9) . . ?
O4 U1 O5 62.13(9) . . ?
O6 U1 O5 81.90(11) . . ?
O1 U1 O2 73.04(9) . . ?
O4 U1 O2 95.51(9) . . ?
O6 U1 O2 118.24(10) . . ?
O5 U1 O2 142.94(9) . . ?
O1 U1 O3 65.12(8) . . ?
O4 U1 O3 128.78(9) . . ?
O6 U1 O3 163.19(11) . . ?
O5 U1 O3 109.21(8) . . ?
O2 U1 O3 60.28(8) . . ?
O1 U1 O7 136.70(9) . . ?
O4 U1 O7 112.43(9) . . ?
O6 U1 O7 60.14(10) . . ?
O5 U1 O7 71.02(9) . . ?
O2 U1 O7 145.43(9) . . ?
O3 U1 O7 110.56(9) . . ?
O1 U1 N2 87.65(10) . . ?
O4 U1 N2 124.81(9) . . ?
O6 U1 N2 115.34(11) . . ?
O5 U1 N2 63.90(9) . . ?
O2 U1 N2 122.04(9) . . ?
O3 U1 N2 61.98(9) . . ?
O7 U1 N2 57.48(10) . . ?
O1 U1 N1 100.88(10) . . ?
O4 U1 N1 61.89(10) . . ?
O6 U1 N1 60.34(11) . . ?
O5 U1 N1 120.88(9) . . ?
O2 U1 N1 59.49(10) . . ?
O3 U1 N1 119.60(9) . . ?
O7 U1 N1 115.76(10) . . ?
N2 U1 N1 171.19(10) . . ?
O1 U1 I1 137.93(6) . . ?
O4 U1 I1 144.46(6) . . ?
O6 U1 I1 87.43(9) . . ?
O5 U1 I1 141.11(6) . . ?
O2 U1 I1 74.20(6) . . ?
O3 U1 I1 76.01(6) . . ?
O7 U1 I1 71.24(7) . . ?
N2 U1 I1 87.94(7) . . ?
N1 U1 I1 84.24(7) . . ?
C3 O2 C2 112.7(3) . . ?
C3 O2 U1 119.5(2) . . ?
C2 O2 U1 127.8(3) . . ?
C5 O3 C4 111.4(3) . . ?
C5 O3 U1 122.9(2) . . ?
C4 O3 U1 121.1(2) . . ?
C8 O4 C9 110.4(3) . . ?
C8 O4 U1 124.3(2) . . ?
C9 O4 U1 117.5(2) . . ?
C10 O5 C11 109.6(3) . . ?
C10 O5 U1 119.1(2) . . ?
C11 O5 U1 115.4(2) . . ?
C14 O6 C15 116.6(4) . . ?
C14 O6 U1 113.5(3) . . ?
C15 O6 U1 115.6(3) . . ?
C16 O7 C17 111.5(4) . . ?
C16 O7 U1 121.9(3) . . ?
C17 O7 U1 123.7(3) . . ?
C7 N1 C1 110.8(4) . . ?
C7 N1 C13 110.6(4) . . ?
C1 N1 C13 108.3(3) . . ?
C7 N1 U1 104.8(2) . . ?
C1 N1 U1 108.5(2) . . ?
C13 N1 U1 113.8(3) . . ?
C6 N2 C18 109.0(3) . . ?
C6 N2 C12 108.4(3) . . ?
C18 N2 C12 109.8(3) . . ?
C6 N2 U1 111.4(2) . . ?
C18 N2 U1 107.0(2) . . ?
C12 N2 U1 111.2(2) . . ?
N1 C1 C2 112.3(4) . . ?
O2 C2 C1 108.4(4) . . ?
O2 C3 C4 107.9(3) . . ?
O3 C4 C3 107.7(3) . . ?
O3 C5 C6 108.0(3) . . ?
N2 C6 C5 112.5(4) . . ?
N1 C7 C8 112.0(4) . . ?
O4 C8 C7 108.5(3) . . ?
O4 C9 C10 107.9(3) . . ?
O5 C10 C9 108.7(3) . . ?
O5 C11 C12 108.5(3) . . ?
C11 C12 N2 111.4(3) . . ?
C14 C13 N1 111.1(4) . . ?
O6 C14 C13 106.7(4) . . ?
C16 C15 O6 110.3(5) . . ?
O7 C16 C15 106.6(4) . . ?
O7 C17 C18 108.7(3) . . ?
N2 C18 C17 111.8(4) . . ?
C25 B1 C31 113.4(4) . . ?
C25 B1 C19 110.5(3) . . ?
C31 B1 C19 104.3(3) . . ?
C25 B1 C37 104.5(3) . . ?
C31 B1 C37 113.7(4) . . ?
C19 B1 C37 110.6(3) . . ?
C20 C19 C24 115.4(4) . . ?
C20 C19 B1 124.0(4) . . ?
C24 C19 B1 120.5(4) . . ?
C19 C20 C21 122.3(4) . . ?
C22 C21 C20 120.7(4) . . ?
C21 C22 C23 119.2(4) . . ?
C22 C23 C24 119.5(5) . . ?
C19 C24 C23 123.0(4) . . ?
C26 C25 C30 114.6(4) . . ?
C26 C25 B1 122.9(4) . . ?
C30 C25 B1 122.2(4) . . ?
C25 C26 C27 124.2(5) . . ?
C28 C27 C26 118.9(5) . . ?
C27 C28 C29 120.2(5) . . ?
C28 C29 C30 120.8(5) . . ?
C25 C30 C29 121.3(5) . . ?
C32 C31 C36 114.6(4) . . ?
C32 C31 B1 122.8(4) . . ?
C36 C31 B1 122.3(4) . . ?
C33 C32 C31 122.7(5) . . ?
C34 C33 C32 121.2(5) . . ?
C33 C34 C35 118.5(5) . . ?
C36 C35 C34 119.2(5) . . ?
C35 C36 C31 123.7(5) . . ?
C38 C37 C42 114.9(4) . . ?
C38 C37 B1 118.7(4) . . ?
C42 C37 B1 126.4(4) . . ?
C39 C38 C37 123.9(4) . . ?
C40 C39 C38 119.9(4) . . ?
C39 C40 C41 118.3(4) . . ?
C40 C41 C42 121.4(4) . . ?
C41 C42 C37 121.6(4) . . ?
N3 C43 C44 178.2(7) . . ?

_refine_diff_density_max         1.717
_refine_diff_density_min         -1.217
_refine_diff_density_rms         0.135



