# 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_kannan27_1
_audit_block_doi                 10.5517/ccdc.csd.cc1kkr40
_database_code_depnum_ccdc_archive 'CCDC 1447022'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/C7DT02760E 2017
_audit_update_record             
;
2016-01-13 deposited with the CCDC.
2017-11-24 downloaded from the CCDC.
;
_audit_creation_date             2016-01-07
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C22 H46 N4 O10 U'
_chemical_formula_sum            'C22 H46 N4 O10 U'
_chemical_formula_weight         764.66
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C22 H46 N4 O10 U'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -4.3638 13.4090 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
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                   8.54447(15)
_cell_length_b                   17.3590(3)
_cell_length_c                   10.5566(2)
_cell_angle_alpha                90
_cell_angle_beta                 103.0576(19)
_cell_angle_gamma                90
_cell_volume                     1525.31(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    3178
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      73.2600
_cell_measurement_theta_min      4.9880
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    15.438
_exptl_absorpt_correction_T_max  0.705
_exptl_absorpt_correction_T_min  0.192
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_density_diffrn    1.665
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             756
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 11 1 0.0280
5 1 -3 0.2099
0 -11 0 0.0171
0 4 -6 0.1285
0 0 7 0.1101
-5 -4 0 0.1650
-5 1 4 0.2275
0 0 -7 0.1261
5 0 0 0.1627

_exptl_crystal_size_max          0.403
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.061
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0.1241 11.2007 0.6600 0.9393 -0.0202 0.3426
4.9998 0.9990 -3.0023 -0.2394 0.0609 0.9043
0.0016 -11.0052 0.0014 -0.9060 0.1231 -0.3442
0.0013 3.9940 -6.0006 0.1232 -0.8851 0.3670
-0.0021 0.0092 7.0001 0.2406 0.9804 -0.2821
-4.9984 -4.0044 0.0026 -0.1108 -0.4475 -0.8772
-5.2431 0.5038 3.6174 0.3949 -0.0155 -0.9186
-0.0023 0.0055 -6.9988 -0.2391 -0.9809 0.2818
5.0014 -0.0056 -0.0026 -0.2195 0.4925 0.7522

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0785
_diffrn_reflns_av_unetI/netI     0.0722
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5868
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.519
_diffrn_reflns_theta_min         4.999
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.3200
_diffrn_detector_type            Titan
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -62.00  23.00   1.00    1.00    --  -44.48  38.00-120.00   85
  2  ω     26.00 114.00   1.00    1.00    --   44.48  77.00  60.00   88
  3  ω     90.00 158.00   1.00    1.00    --  101.96  45.00 -60.00   68
  4  ω     36.00  69.00   1.00    1.00    --  101.96 -30.00 -90.00   33
  5  ω     21.00  46.00   1.00    1.00    --  101.96 -95.00-180.00   25
  6  ω     51.00  96.00   1.00    1.00    --  101.96 -95.00-180.00   45
  7  ω     34.00  63.00   1.00    1.00    --  101.96 -30.00 150.00   29
  8  ω     31.00  61.00   1.00    1.00    --  101.96 -30.00  30.00   30
  9  ω     45.00  76.00   1.00    1.00    --  101.96 -45.00-180.00   31
 10  ω     48.00  74.00   1.00    1.00    --  101.96 -45.00 -60.00   26
 11  ω     29.00  57.00   1.00    1.00    --  101.96 -30.00-150.00   28
 12  ω     45.00 101.00   1.00    1.00    --  101.96 -95.00  90.00   56
 13  ω     29.00  65.00   1.00    1.00    --  101.96 -30.00 120.00   36
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Titan'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0437713000
_diffrn_orient_matrix_UB_12      0.0823249000
_diffrn_orient_matrix_UB_13      0.0342487000
_diffrn_orient_matrix_UB_21      0.0985422000
_diffrn_orient_matrix_UB_22      -0.0111529000
_diffrn_orient_matrix_UB_23      0.1401056000
_diffrn_orient_matrix_UB_31      0.1504107000
_diffrn_orient_matrix_UB_32      0.0312932000
_diffrn_orient_matrix_UB_33      -0.0402953000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1993
_reflns_number_total             2957
_reflns_odcompleteness_completeness 99.75
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         5.135
_refine_diff_density_min         -3.638
_refine_diff_density_rms         0.310
_refine_ls_extinction_coef       0.0010(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     177
_refine_ls_number_reflns         2957
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0975
_refine_ls_R_factor_gt           0.0808
_refine_ls_restrained_S_all      1.068
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1571P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2157
_refine_ls_wR_factor_ref         0.2402
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C6(H6), C9(H9)
2.b Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C7(H7A,H7B,H7C), C8(H8A,
 H8B,H8C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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 0.0000 0.5000 0.0405(3) Uani 1 2 d S T P . .
O1 O 0.3594(9) 0.0757(4) 0.4822(8) 0.057(2) Uani 1 1 d . . . . .
O2 O 0.6100(10) 0.0424(5) 0.7301(8) 0.070(2) Uani 1 1 d . . . . .
O3 O 0.7294(10) 0.0903(5) 0.5930(9) 0.068(2) Uani 1 1 d . . . . .
O4 O 0.8135(11) 0.1180(6) 0.7959(10) 0.086(3) Uani 1 1 d . . . . .
O5 O 0.6106(8) 0.0656(4) 0.3399(7) 0.0505(17) Uani 1 1 d . . . . .
N1 N 0.7212(12) 0.0853(5) 0.7084(11) 0.062(2) Uani 1 1 d . . . . .
N2 N 0.6339(10) 0.1553(5) 0.1957(9) 0.052(2) Uani 1 1 d . . . . .
C1 C 0.6769(12) 0.0876(5) 0.2546(11) 0.048(2) Uani 1 1 d . . . . .
C2 C 0.8067(16) 0.0363(8) 0.2151(16) 0.064(4) Uani 1 1 d . . . . .
C3 C 0.744(5) 0.0048(8) 0.076(3) 0.096(9) Uani 1 1 d . . . . .
H3A H 0.6505 -0.0261 0.0729 0.144 Uiso 1 1 calc GR . . . .
H3B H 0.8263 -0.0261 0.0518 0.144 Uiso 1 1 calc GR . . . .
H3C H 0.7176 0.0471 0.0162 0.144 Uiso 1 1 calc GR . . . .
C4 C 0.9725(13) 0.0775(10) 0.2391(18) 0.101(5) Uani 1 1 d . . . . .
H4A H 0.9667 0.1196 0.1791 0.151 Uiso 1 1 calc GR . . . .
H4B H 1.0530 0.0416 0.2264 0.151 Uiso 1 1 calc GR . . . .
H4C H 1.0001 0.0968 0.3265 0.151 Uiso 1 1 calc GR . . . .
C5 C 0.830(2) -0.0353(11) 0.3058(19) 0.088(6) Uani 1 1 d . . . . .
H5A H 0.8572 -0.0187 0.3949 0.132 Uiso 1 1 calc GR . . . .
H5B H 0.9148 -0.0668 0.2882 0.132 Uiso 1 1 calc GR . . . .
H5C H 0.7320 -0.0645 0.2904 0.132 Uiso 1 1 calc GR . . . .
C6 C 0.5161(14) 0.2061(6) 0.2390(12) 0.060(3) Uani 1 1 d . . . . .
H6 H 0.5100 0.2527 0.1857 0.072 Uiso 1 1 calc R . . . .
C7 C 0.577(2) 0.2325(7) 0.3765(15) 0.076(4) Uani 1 1 d . . . . .
H7A H 0.5787 0.1898 0.4345 0.114 Uiso 1 1 calc GR . . . .
H7B H 0.5079 0.2720 0.3963 0.114 Uiso 1 1 calc GR . . . .
H7C H 0.6840 0.2525 0.3867 0.114 Uiso 1 1 calc GR . . . .
C8 C 0.3493(13) 0.1721(7) 0.2060(14) 0.073(4) Uani 1 1 d . . . . .
H8A H 0.3178 0.1628 0.1142 0.110 Uiso 1 1 calc GR . . . .
H8B H 0.2753 0.2075 0.2310 0.110 Uiso 1 1 calc GR . . . .
H8C H 0.3486 0.1245 0.2521 0.110 Uiso 1 1 calc GR . . . .
C9 C 0.7007(15) 0.1882(7) 0.0882(12) 0.071(3) Uani 1 1 d . . . . .
H9 H 0.7738 0.1496 0.0661 0.085 Uiso 1 1 calc R . . . .
C10 C 0.572(2) 0.2011(10) -0.0306(14) 0.101(5) Uani 1 1 d . . . . .
H10A H 0.5280 0.1525 -0.0642 0.151 Uiso 1 1 calc GR . . . .
H10B H 0.6165 0.2269 -0.0950 0.151 Uiso 1 1 calc GR . . . .
H10C H 0.4890 0.2324 -0.0095 0.151 Uiso 1 1 calc GR . . . .
C11 C 0.799(2) 0.2600(8) 0.1293(19) 0.108(6) Uani 1 1 d . . . . .
H11A H 0.7307 0.2996 0.1509 0.162 Uiso 1 1 calc GR . . . .
H11B H 0.8446 0.2773 0.0593 0.162 Uiso 1 1 calc GR . . . .
H11C H 0.8831 0.2487 0.2039 0.162 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 O1 1.762(7) 3_656 ?
U1 O1 1.762(7) . ?
U1 O2 2.509(8) . ?
U1 O2 2.509(8) 3_656 ?
U1 O3 2.529(9) 3_656 ?
U1 O3 2.529(9) . ?
U1 O5 2.402(6) . ?
U1 O5 2.402(6) 3_656 ?
U1 N1 2.954(11) . ?
U1 N1 2.954(11) 3_656 ?
O2 N1 1.269(12) . ?
O3 N1 1.239(12) . ?
O4 N1 1.211(12) . ?
O5 C1 1.228(12) . ?
N2 C1 1.341(12) . ?
N2 C6 1.486(13) . ?
N2 C9 1.494(13) . ?
C1 C2 1.551(18) . ?
C2 C3 1.55(3) . ?
C2 C4 1.557(18) . ?
C2 C5 1.55(2) . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 H6 0.9800 . ?
C6 C7 1.499(18) . ?
C6 C8 1.508(16) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 H9 0.9800 . ?
C9 C10 1.486(18) . ?
C9 C11 1.509(19) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 U1 O1 180.0(5) 3_656 . ?
O1 U1 O2 89.0(4) . . ?
O1 U1 O2 91.0(4) 3_656 . ?
O1 U1 O2 91.0(4) . 3_656 ?
O1 U1 O2 89.0(4) 3_656 3_656 ?
O1 U1 O3 91.7(3) 3_656 3_656 ?
O1 U1 O3 88.3(3) . 3_656 ?
O1 U1 O3 91.7(3) . . ?
O1 U1 O3 88.3(3) 3_656 . ?
O1 U1 O5 93.5(3) 3_656 . ?
O1 U1 O5 93.5(3) . 3_656 ?
O1 U1 O5 86.5(3) 3_656 3_656 ?
O1 U1 O5 86.5(3) . . ?
O1 U1 N1 89.3(4) 3_656 . ?
O1 U1 N1 90.7(4) . . ?
O1 U1 N1 89.3(4) . 3_656 ?
O1 U1 N1 90.7(4) 3_656 3_656 ?
O2 U1 O2 180.0 3_656 . ?
O2 U1 O3 49.8(3) 3_656 3_656 ?
O2 U1 O3 49.8(3) . . ?
O2 U1 O3 130.2(3) 3_656 . ?
O2 U1 O3 130.2(3) . 3_656 ?
O2 U1 N1 154.8(3) . 3_656 ?
O2 U1 N1 154.8(3) 3_656 . ?
O2 U1 N1 25.2(3) 3_656 3_656 ?
O2 U1 N1 25.2(3) . . ?
O3 U1 O3 180.0(3) 3_656 . ?
O3 U1 N1 155.4(3) 3_656 . ?
O3 U1 N1 155.4(3) . 3_656 ?
O3 U1 N1 24.6(3) 3_656 3_656 ?
O3 U1 N1 24.6(3) . . ?
O5 U1 O2 65.1(3) 3_656 . ?
O5 U1 O2 114.9(3) . . ?
O5 U1 O2 65.1(3) . 3_656 ?
O5 U1 O2 114.9(3) 3_656 3_656 ?
O5 U1 O3 114.5(3) 3_656 . ?
O5 U1 O3 114.5(3) . 3_656 ?
O5 U1 O3 65.5(3) 3_656 3_656 ?
O5 U1 O3 65.5(3) . . ?
O5 U1 O5 180.0(3) . 3_656 ?
O5 U1 N1 90.1(3) 3_656 . ?
O5 U1 N1 89.9(3) 3_656 3_656 ?
O5 U1 N1 89.9(3) . . ?
O5 U1 N1 90.1(3) . 3_656 ?
N1 U1 N1 180.0 . 3_656 ?
N1 O2 U1 97.4(7) . . ?
N1 O3 U1 97.3(7) . . ?
C1 O5 U1 169.6(7) . . ?
O2 N1 U1 57.4(6) . . ?
O3 N1 U1 58.1(6) . . ?
O3 N1 O2 115.5(10) . . ?
O4 N1 U1 177.9(8) . . ?
O4 N1 O2 121.5(11) . . ?
O4 N1 O3 123.0(12) . . ?
C1 N2 C6 120.7(9) . . ?
C1 N2 C9 125.2(9) . . ?
C6 N2 C9 114.0(8) . . ?
O5 C1 N2 119.3(10) . . ?
O5 C1 C2 119.6(9) . . ?
N2 C1 C2 121.1(11) . . ?
C1 C2 C4 111.8(12) . . ?
C1 C2 C5 107.1(12) . . ?
C3 C2 C1 110.2(16) . . ?
C3 C2 C4 115.0(17) . . ?
C3 C2 C5 105.8(16) . . ?
C5 C2 C4 106.4(13) . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C2 C4 H4A 109.5 . . ?
C2 C4 H4B 109.5 . . ?
C2 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C2 C5 H5A 109.5 . . ?
C2 C5 H5B 109.5 . . ?
C2 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N2 C6 H6 105.4 . . ?
N2 C6 C7 111.6(10) . . ?
N2 C6 C8 111.6(10) . . ?
C7 C6 H6 105.4 . . ?
C7 C6 C8 116.5(11) . . ?
C8 C6 H6 105.4 . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C6 C8 H8A 109.5 . . ?
C6 C8 H8B 109.5 . . ?
C6 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N2 C9 H9 106.9 . . ?
N2 C9 C11 112.3(12) . . ?
C10 C9 N2 111.3(11) . . ?
C10 C9 H9 106.9 . . ?
C10 C9 C11 112.0(12) . . ?
C11 C9 H9 106.9 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 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
U1 O2 N1 O3 1.3(10) . . . . ?
U1 O2 N1 O4 -177.9(9) . . . . ?
U1 O3 N1 O2 -1.2(10) . . . . ?
U1 O3 N1 O4 177.9(10) . . . . ?
U1 O5 C1 N2 163(3) . . . . ?
U1 O5 C1 C2 -16(4) . . . . ?
O5 C1 C2 C3 111.6(15) . . . . ?
O5 C1 C2 C4 -119.3(12) . . . . ?
O5 C1 C2 C5 -3.1(19) . . . . ?
N2 C1 C2 C3 -67.3(16) . . . . ?
N2 C1 C2 C4 61.8(16) . . . . ?
N2 C1 C2 C5 178.0(13) . . . . ?
C1 N2 C6 C7 62.6(13) . . . . ?
C1 N2 C6 C8 -69.7(13) . . . . ?
C1 N2 C9 C10 120.6(13) . . . . ?
C1 N2 C9 C11 -112.9(14) . . . . ?
C6 N2 C1 O5 4.4(15) . . . . ?
C6 N2 C1 C2 -176.6(11) . . . . ?
C6 N2 C9 C10 -61.9(14) . . . . ?
C6 N2 C9 C11 64.6(14) . . . . ?
C9 N2 C1 O5 -178.2(10) . . . . ?
C9 N2 C1 C2 0.7(17) . . . . ?
C9 N2 C6 C7 -115.0(12) . . . . ?
C9 N2 C6 C8 112.7(11) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_date_sample_data_collection 2015-10-21
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 7.095
_oxdiff_exptl_absorpt_empirical_full_min 0.310
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: CHCl3/dodecane'
####################################################################### 
# 
# 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_kannan29_1
_audit_block_doi                 10.5517/ccdc.csd.cc1kkr51
_database_code_depnum_ccdc_archive 'CCDC 1447023'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/C7DT02760E 2017
_audit_update_record             
;
2016-01-13 deposited with the CCDC.
2017-11-24 downloaded from the CCDC.
;
_audit_creation_date             2016-01-12
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C30 H64 N6 O10 U'
_chemical_formula_sum            'C30 H58 N6 O10 U'
_chemical_formula_weight         900.85
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C30 H64 N6 O10 U'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -4.3638 13.4090 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
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                   9.5274(2)
_cell_length_b                   13.9381(3)
_cell_length_c                   15.4478(3)
_cell_angle_alpha                90
_cell_angle_beta                 89.689(2)
_cell_angle_gamma                90
_cell_volume                     2051.34(8)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    3865
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      72.9230
_cell_measurement_theta_min      4.2790
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    11.584
_exptl_absorpt_correction_T_max  0.404
_exptl_absorpt_correction_T_min  0.111
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.458
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             904
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
6 2 1 0.1523
0 6 -8 0.0680
0 7 6 0.0199
-5 -4 -1 0.2080
1 6 -7 0.0518
0 -3 -9 0.0672
1 -8 -4 0.0482
1 -5 8 0.0475
-3 -5 7 0.1003
-5 -5 4 0.1576
-4 1 7 0.1335
-2 8 -2 0.1033
0 -8 4 0.0390
2 -8 4 0.0509

_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.091
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
6.0030 2.1352 0.5692 -0.1257 0.0366 -0.9914
0.0820 5.8940 -7.6085 0.9408 -0.2219 -0.2562
-0.3247 7.0909 6.1944 -0.2288 -0.9579 -0.1735
-5.0000 -4.0001 -1.0001 0.0527 0.2032 0.9021
1.0000 6.0000 -7.0000 0.8651 -0.2182 -0.3976
0.0000 -3.0000 -9.0000 0.6713 0.6787 0.0653
1.0000 -8.0000 -4.0000 -0.0271 0.9776 0.1124
1.0000 -5.0000 8.0000 -0.9666 0.1676 0.0607
-3.0000 -5.0001 6.9999 -0.7640 0.0355 0.6681
-5.0000 -5.0001 3.9999 -0.4391 0.0790 0.9604
-4.0000 0.9999 7.0000 -0.4683 -0.5773 0.6083
-2.0000 8.0000 -2.0000 0.5920 -0.7588 0.0132
-0.0000 -8.0000 4.0000 -0.7143 0.5832 0.3019
2.0000 -8.0000 4.0000 -0.7709 0.6712 -0.0041

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0636
_diffrn_reflns_av_unetI/netI     0.0709
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            8272
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.474
_diffrn_reflns_theta_min         4.272
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 4.1600
_diffrn_detector_type            Titan
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -24.00  69.00   1.00    1.00    --   43.29 -19.00 -30.00   93
  2  ω     79.00 150.00   1.00    1.70    --  102.90  45.00-120.00   71
  3  ω    130.00 156.00   1.00    1.70    --  102.90  15.00 -90.00   26
  4  ω     81.00 157.00   1.00    1.70    --  102.90  30.00   0.00   76
  5  ω     80.00 116.00   1.00    1.70    --  102.90 -61.00 120.00   36
  6  ω     31.00 114.00   1.00    1.70    --  102.90-126.00  60.00   83
  7  ω     61.00  93.00   1.00    1.70    --  102.90 -95.00 -90.00   32
  8  ω     78.00 103.00   1.00    1.70    --  102.90  15.00 -90.00   25
  9  ω     20.00 110.00   1.00    1.70    --  102.90 -95.00 120.00   90
 10  ω    -22.00  62.00   1.00    1.00    --   43.29 -38.00-120.00   84
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Titan'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0283009000
_diffrn_orient_matrix_UB_12      0.0445630000
_diffrn_orient_matrix_UB_13      -0.0894376000
_diffrn_orient_matrix_UB_21      0.0439659000
_diffrn_orient_matrix_UB_22      -0.0948059000
_diffrn_orient_matrix_UB_23      -0.0438055000
_diffrn_orient_matrix_UB_31      -0.1529735000
_diffrn_orient_matrix_UB_32      -0.0354530000
_diffrn_orient_matrix_UB_33      0.0045572000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2412
_reflns_number_total             3967
_reflns_odcompleteness_completeness 99.48
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         1.966
_refine_diff_density_min         -0.896
_refine_diff_density_rms         0.132
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.338
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     222
_refine_ls_number_reflns         3967
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0949
_refine_ls_R_factor_gt           0.0540
_refine_ls_restrained_S_all      1.338
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0331P)²+6.3457P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1391
_refine_ls_wR_factor_ref         0.1526
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C2(H2), C5(H5), C9(H9), C13(H13)
2.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C12(H12A,H12B)
2.c Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C10(H10A,
 H10B,H10C), C11(H11A,H11B,H11C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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 1.0000 0.5000 0.04993(18) Uani 1 2 d S T P A .
O1 O 0.3916(11) 1.0864(7) 0.5489(6) 0.078(3) Uani 1 1 d . . . . .
O4 O 0.2435(13) 1.0150(12) 0.2815(7) 0.121(5) Uani 1 1 d . . . . .
O5 O 0.3529(9) 0.8791(6) 0.5606(6) 0.059(2) Uani 1 1 d . . . . .
N1 N 0.3219(14) 1.0092(12) 0.3447(7) 0.083(4) Uani 1 1 d . . . . .
N2 N 0.1782(11) 0.8095(7) 0.6386(6) 0.054(2) Uani 1 1 d . . . . .
N3 N 0.3027(10) 0.7232(8) 0.5337(6) 0.053(2) Uani 1 1 d . . . . .
C1 C 0.2805(12) 0.8067(8) 0.5762(7) 0.047(3) Uani 1 1 d . . . . .
C2 C 0.1215(17) 0.9024(11) 0.6677(10) 0.081(5) Uani 1 1 d . . . . .
H2 H 0.0438 0.8870 0.7072 0.097 Uiso 1 1 calc R . . . .
C3 C 0.059(2) 0.9551(16) 0.5959(13) 0.131(9) Uani 1 1 d . . . . .
H3A H 0.1319 0.9790 0.5586 0.196 Uiso 1 1 calc GR . . . .
H3B H 0.0049 1.0078 0.6181 0.196 Uiso 1 1 calc GR . . . .
H3C H -0.0011 0.9130 0.5637 0.196 Uiso 1 1 calc GR . . . .
C4 C 0.225(2) 0.9628(12) 0.7207(12) 0.106(7) Uani 1 1 d . . . . .
H4A H 0.2828 0.9212 0.7547 0.159 Uiso 1 1 calc GR . . . .
H4B H 0.1734 1.0051 0.7583 0.159 Uiso 1 1 calc GR . . . .
H4C H 0.2827 0.9999 0.6823 0.159 Uiso 1 1 calc GR . . . .
C5 C 0.1455(17) 0.7261(10) 0.6945(9) 0.075(4) Uani 1 1 d . . . . .
H5 H 0.1902 0.6696 0.6684 0.091 Uiso 1 1 calc R . . . .
C6 C -0.007(2) 0.7058(15) 0.7022(15) 0.137(9) Uani 1 1 d . . . . .
H6A H -0.0525 0.7580 0.7314 0.206 Uiso 1 1 calc GR . . . .
H6B H -0.0206 0.6478 0.7346 0.206 Uiso 1 1 calc GR . . . .
H6C H -0.0462 0.6984 0.6455 0.206 Uiso 1 1 calc GR . . . .
C7 C 0.209(2) 0.7400(13) 0.7843(11) 0.120(8) Uani 1 1 d . . . . .
H7A H 0.3086 0.7474 0.7791 0.180 Uiso 1 1 calc GR . . . .
H7B H 0.1880 0.6851 0.8196 0.180 Uiso 1 1 calc GR . . . .
H7C H 0.1692 0.7964 0.8106 0.180 Uiso 1 1 calc GR . . . .
C8 C 0.1913(14) 0.6576(10) 0.5082(8) 0.064(3) Uani 1 1 d . . . . .
H8A H 0.1052 0.6776 0.5367 0.077 Uiso 1 1 calc R . . . .
H8B H 0.2143 0.5942 0.5298 0.077 Uiso 1 1 calc R . . . .
C9 C 0.1633(18) 0.6498(13) 0.4121(10) 0.087(5) Uani 1 1 d . . . . .
H9 H 0.2500 0.6286 0.3835 0.104 Uiso 1 1 calc R . . . .
C10 C 0.0525(16) 0.5766(14) 0.3954(12) 0.098(6) Uani 1 1 d . . . . .
H10A H 0.0791 0.5168 0.4213 0.147 Uiso 1 1 calc GR . . . .
H10B H 0.0420 0.5681 0.3341 0.147 Uiso 1 1 calc GR . . . .
H10C H -0.0348 0.5979 0.4200 0.147 Uiso 1 1 calc GR . . . .
C11 C 0.124(3) 0.7449(16) 0.3756(15) 0.160(12) Uani 1 1 d . . . . .
H11A H 0.0570 0.7754 0.4132 0.239 Uiso 1 1 calc GR . . . .
H11B H 0.0833 0.7362 0.3194 0.239 Uiso 1 1 calc GR . . . .
H11C H 0.2061 0.7844 0.3706 0.239 Uiso 1 1 calc GR . . . .
C12 C 0.4426(13) 0.7059(10) 0.4979(8) 0.058(3) Uani 1 1 d . . . . .
H12A H 0.4759 0.7645 0.4707 0.070 Uiso 1 1 calc R . . . .
H12B H 0.4359 0.6573 0.4532 0.070 Uiso 1 1 calc R . . . .
C13 C 0.5469(18) 0.675(2) 0.5623(12) 0.132(10) Uani 1 1 d . . . . .
H13 H 0.5682 0.7351 0.5918 0.158 Uiso 1 1 calc R . . . .
C14 C 0.688(2) 0.655(2) 0.5128(14) 0.174(14) Uani 1 1 d . . . . .
H14A H 0.6738 0.6054 0.4703 0.261 Uiso 1 1 calc GR . . . .
H14B H 0.7582 0.6338 0.5533 0.261 Uiso 1 1 calc GR . . . .
H14C H 0.7196 0.7122 0.4847 0.261 Uiso 1 1 calc GR . . . .
C15 C 0.530(3) 0.617(2) 0.6268(16) 0.186(15) Uani 1 1 d . . . . .
H15A H 0.4389 0.6265 0.6518 0.279 Uiso 1 1 calc GR . . . .
H15B H 0.6006 0.6299 0.6696 0.279 Uiso 1 1 calc GR . . . .
H15C H 0.5391 0.5520 0.6072 0.279 Uiso 1 1 calc GR . . . .
O2 O 0.3003(12) 0.9503(9) 0.4031(7) 0.094(4) Uani 1 1 d . . . A 1
O3 O 0.4250(12) 1.0654(9) 0.3550(7) 0.086(3) Uani 1 1 d . . . A 1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 O1 1.754(11) 3_676 ?
U1 O1 1.754(11) . ?
U1 O5 2.380(8) . ?
U1 O5 2.380(8) 3_676 ?
U1 N1 2.949(12) 3_676 ?
U1 N1 2.949(12) . ?
U1 O2 2.524(10) 3_676 ?
U1 O2 2.524(10) . ?
U1 O3 2.525(10) . ?
U1 O3 2.525(10) 3_676 ?
O4 N1 1.235(15) . ?
O5 C1 1.246(13) . ?
N1 O2 1.237(16) . ?
N1 O3 1.266(16) . ?
N2 C1 1.368(14) . ?
N2 C2 1.473(17) . ?
N2 C5 1.480(16) . ?
N3 C1 1.353(15) . ?
N3 C8 1.456(15) . ?
N3 C12 1.460(15) . ?
C2 C3 1.46(2) . ?
C2 C4 1.53(2) . ?
C5 C6 1.48(2) . ?
C5 C7 1.53(2) . ?
C8 C9 1.514(19) . ?
C9 C10 1.49(2) . ?
C9 C11 1.49(3) . ?
C12 C13 1.48(2) . ?
C13 C14 1.57(2) . ?
C13 C15 1.29(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 U1 O1 180.0 3_676 . ?
O1 U1 O5 91.6(4) . 3_676 ?
O1 U1 O5 88.4(4) 3_676 3_676 ?
O1 U1 O5 88.4(4) . . ?
O1 U1 O5 91.6(4) 3_676 . ?
O1 U1 N1 91.1(4) 3_676 . ?
O1 U1 N1 88.9(4) 3_676 3_676 ?
O1 U1 N1 91.1(4) . 3_676 ?
O1 U1 N1 88.9(4) . . ?
O1 U1 O2 90.0(5) . 3_676 ?
O1 U1 O2 90.0(5) 3_676 . ?
O1 U1 O2 90.0(5) 3_676 3_676 ?
O1 U1 O2 90.0(5) . . ?
O1 U1 O3 92.0(4) . 3_676 ?
O1 U1 O3 88.0(4) . . ?
O1 U1 O3 88.0(4) 3_676 3_676 ?
O1 U1 O3 92.0(4) 3_676 . ?
O5 U1 O5 180.0 . 3_676 ?
O5 U1 N1 89.4(4) 3_676 . ?
O5 U1 N1 90.6(4) . . ?
O5 U1 N1 89.4(4) . 3_676 ?
O5 U1 N1 90.6(4) 3_676 3_676 ?
O5 U1 O2 113.9(3) . 3_676 ?
O5 U1 O2 66.1(3) 3_676 3_676 ?
O5 U1 O2 113.9(3) 3_676 . ?
O5 U1 O2 66.1(3) . . ?
O5 U1 O3 64.2(3) 3_676 . ?
O5 U1 O3 115.8(3) 3_676 3_676 ?
O5 U1 O3 64.2(3) . 3_676 ?
O5 U1 O3 115.8(3) . . ?
N1 U1 N1 180.0(5) . 3_676 ?
O2 U1 N1 24.6(4) 3_676 3_676 ?
O2 U1 N1 155.4(4) . 3_676 ?
O2 U1 N1 155.4(4) 3_676 . ?
O2 U1 N1 24.6(4) . . ?
O2 U1 O2 180.0(3) 3_676 . ?
O2 U1 O3 49.8(3) . . ?
O2 U1 O3 130.2(3) . 3_676 ?
O2 U1 O3 49.8(3) 3_676 3_676 ?
O2 U1 O3 130.2(3) 3_676 . ?
O3 U1 N1 154.7(3) 3_676 . ?
O3 U1 N1 154.7(3) . 3_676 ?
O3 U1 N1 25.3(3) . . ?
O3 U1 N1 25.3(3) 3_676 3_676 ?
O3 U1 O3 180.0 3_676 . ?
C1 O5 U1 167.0(8) . . ?
O4 N1 U1 177.5(12) . . ?
O4 N1 O2 121.4(15) . . ?
O4 N1 O3 122.1(15) . . ?
O2 N1 U1 58.1(7) . . ?
O2 N1 O3 116.4(12) . . ?
O3 N1 U1 58.3(7) . . ?
C1 N2 C2 120.0(10) . . ?
C1 N2 C5 122.4(11) . . ?
C2 N2 C5 115.9(10) . . ?
C1 N3 C8 124.0(10) . . ?
C1 N3 C12 117.7(10) . . ?
C8 N3 C12 117.4(10) . . ?
O5 C1 N2 120.4(11) . . ?
O5 C1 N3 121.2(10) . . ?
N3 C1 N2 118.4(10) . . ?
N2 C2 C4 114.2(13) . . ?
C3 C2 N2 111.1(14) . . ?
C3 C2 C4 113.3(16) . . ?
N2 C5 C6 113.6(15) . . ?
N2 C5 C7 110.3(12) . . ?
C6 C5 C7 110.0(15) . . ?
N3 C8 C9 116.3(11) . . ?
C10 C9 C8 110.4(14) . . ?
C11 C9 C8 110.7(16) . . ?
C11 C9 C10 111.3(16) . . ?
N3 C12 C13 114.2(11) . . ?
C12 C13 C14 107.7(14) . . ?
C15 C13 C12 129(2) . . ?
C15 C13 C14 112(2) . . ?
N1 O2 U1 97.3(9) . . ?
N1 O3 U1 96.4(8) . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_date_sample_data_collection 2015-11-09
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.876
_oxdiff_exptl_absorpt_empirical_full_min 0.394
####################################################################### 
# 
# 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_kannan30_10
_audit_block_doi                 10.5517/ccdc.csd.cc1kkr62
_database_code_depnum_ccdc_archive 'CCDC 1447024'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/C7DT02760E 2017
_audit_update_record             
;
2016-01-13 deposited with the CCDC.
2017-11-24 downloaded from the CCDC.
;
_audit_creation_date             2016-01-13
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(C14 N2 O5 U0.5)'
_chemical_formula_sum            'C28 N4 O10 U'
_chemical_formula_weight         790.35
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C26 H54 N4 O10 U'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -4.3638 13.4090 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.2463(5)
_cell_length_b                   10.0893(4)
_cell_length_c                   21.5471(13)
_cell_angle_alpha                89.942(4)
_cell_angle_beta                 88.883(5)
_cell_angle_gamma                73.411(4)
_cell_volume                     1926.04(18)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    4105
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      71.9130
_cell_measurement_theta_min      4.0370
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    12.279
_exptl_absorpt_correction_T_max  0.474
_exptl_absorpt_correction_T_min  0.092
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.363
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             736
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-6 0 -2 0.0493
6 0 2 0.0505
0 -6 -1 0.1373
1 0 -14 0.0181
0 6 1 0.4375
-1 0 14 0.0545
4 0 -9 0.0313
4 0 11 0.0537

_exptl_crystal_size_max          0.632
_exptl_crystal_size_mid          0.105
_exptl_crystal_size_min          0.086
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-5.6529 0.1128 -2.4305 -0.7309 -0.6247 -0.2749
5.7246 0.1465 2.3599 0.7384 0.6316 0.2363
-0.1064 -6.3031 -0.5261 0.1428 -0.1567 0.9773
0.6662 -0.2563 -13.8239 0.6474 -0.7556 -0.0996
0.1017 6.2998 0.6222 -0.1472 0.1619 -0.9758
-0.6714 0.0670 13.8492 -0.6451 0.7531 0.1294
4.0030 0.0093 -9.0249 0.9390 -0.1840 0.0511
4.0069 0.0008 10.9742 0.1518 0.9850 0.2937

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1355
_diffrn_reflns_av_unetI/netI     0.1188
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            13236
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.199
_diffrn_reflns_theta_min         4.104
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 4.1600
_diffrn_detector_type            Titan
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -69.00  26.00   1.00    1.00    --  -43.29  57.00 -90.00   95
  2  ω     39.00 123.00   1.00    1.00    --   43.29 177.00 126.00   84
  3  ω     83.00 127.00   1.00    2.00    --  102.90  45.00   0.00   44
  4  ω     62.00 122.00   1.00    2.00    --  102.90 -45.00   0.00   60
  5  ω     82.00 109.00   1.00    2.00    --  102.90 -95.00 120.00   27
  6  ω     33.00 130.00   1.00    2.00    --  102.90 -61.00 120.00   97
  7  ω     64.00 154.00   1.00    2.00    --  102.90  15.00 150.00   90
  8  ω     56.00 100.00   1.00    2.00    --  102.90 -45.00 -60.00   44
  9  ω     63.00 158.00   1.00    2.00    --  102.90  15.00-120.00   95
 10  ω     75.00 109.00   1.00    2.00    --  102.90-126.00 -60.00   34
 11  ω     35.00  62.00   1.00    2.00    --  102.90-126.00 -60.00   27
 12  ω     21.00  64.00   1.00    2.00    --  102.90 -95.00 -60.00   43
 13  ω     21.00 107.00   1.00    2.00    --  102.90 -95.00 -30.00   86
 14  ω     25.00 110.00   1.00    2.00    --  102.90 -95.00  60.00   85
 15  ω   -117.00 -92.00   1.00    1.00    --  -43.29-126.00-120.00   25
 16  ω   -113.00 -18.00   1.00    1.00    --  -43.29 -57.00 120.00   95
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Titan'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1457970000
_diffrn_orient_matrix_UB_12      -0.0218295000
_diffrn_orient_matrix_UB_13      -0.0394031000
_diffrn_orient_matrix_UB_21      0.0857572000
_diffrn_orient_matrix_UB_22      0.0185388000
_diffrn_orient_matrix_UB_23      0.0584466000
_diffrn_orient_matrix_UB_31      0.0403117000
_diffrn_orient_matrix_UB_32      -0.1567309000
_diffrn_orient_matrix_UB_33      0.0120557000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3715
_reflns_number_total             7413
_reflns_odcompleteness_completeness 99.68
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.529
_refine_diff_density_min         -2.109
_refine_diff_density_rms         0.181
_refine_ls_extinction_coef       0.00071(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     356
_refine_ls_number_reflns         7413
_refine_ls_number_restraints     48
_refine_ls_R_factor_all          0.1402
_refine_ls_R_factor_gt           0.0853
_refine_ls_restrained_S_all      1.007
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1163P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2096
_refine_ls_wR_factor_ref         0.2640
_refine_special_details          ?
_olex2_refinement_description    
;
1. Uiso/Uaniso restraints and constraints
C7 \\sim C8 \\sim C9 \\sim C10: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C23 \\sim C22 \\sim C24: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
C1 \\sim C2 \\sim N2 \\sim C11: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
Uanis(C13) = Uanis(C12) = Uanis(C14) = Uanis(C11)
Uanis(C25) = Uanis(C26) = Uanis(C27) = Uanis(C28)
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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 1.0000 1.0000 0.0896(4) Uani 1 2 d S T P . .
O1 O 0.3206(18) 1.1017(14) 1.0154(8) 0.128(5) Uani 1 1 d . . . . .
O2 O 0.5008(17) 0.8940(11) 1.1035(6) 0.113(4) Uani 1 1 d . . . . .
O3 O 0.4217(17) 0.7948(11) 1.0302(7) 0.107(4) Uani 1 1 d . . . . .
O4 O 0.432(2) 0.7052(13) 1.1239(8) 0.140(6) Uani 1 1 d . . . . .
O5 O 0.4054(16) 0.8913(11) 0.9198(6) 0.104(4) Uani 1 1 d . . . . .
N1 N 0.447(2) 0.7897(18) 1.0878(10) 0.114(5) Uani 1 1 d . . . . .
N2 N 0.271(3) 0.7605(19) 0.8926(9) 0.150(7) Uani 1 1 d . U . . .
C1 C 0.395(3) 0.779(2) 0.8998(9) 0.125(7) Uani 1 1 d . U . . .
C2 C 0.534(2) 0.6525(16) 0.8897(9) 0.094(5) Uani 1 1 d . U . . .
C3 C 0.616(4) 0.665(3) 0.8279(14) 0.148(9) Uani 1 1 d . . . . .
C4 C 0.763(4) 0.534(3) 0.8237(16) 0.208(17) Uani 1 1 d . . . . .
C5 C 0.520(5) 0.651(3) 0.7741(15) 0.210(16) Uani 1 1 d . . . . .
C6 C 0.687(6) 0.787(3) 0.823(2) 0.30(3) Uani 1 1 d . . . . .
C7 C 0.238(3) 0.6300(19) 0.8727(10) 0.134(8) Uani 1 1 d . U . . .
C8 C 0.208(4) 0.546(3) 0.9247(15) 0.176(10) Uani 1 1 d . U . . .
C9 C 0.167(3) 0.415(2) 0.9033(16) 0.175(12) Uani 1 1 d . U . . .
C10 C 0.188(5) 0.572(4) 0.983(2) 0.213(16) Uani 1 1 d . U . . .
C11 C 0.124(5) 0.891(4) 0.9104(18) 0.232(9) Uani 1 1 d . U . . .
C12 C 0.081(6) 1.009(4) 0.852(2) 0.232(9) Uani 1 1 d . . . . .
C13 C 0.079(5) 0.951(3) 0.795(2) 0.232(9) Uani 1 1 d . . . . .
C14 C -0.070(6) 1.091(4) 0.8759(19) 0.232(9) Uani 1 1 d . . . . .
U2 U 0.5000 1.5000 0.5000 0.0799(3) Uani 1 2 d S T P . .
O6 O 0.3274(13) 1.5891(15) 0.4860(7) 0.112(5) Uani 1 1 d . . . . .
O7 O 0.4310(15) 1.2882(11) 0.4704(7) 0.101(4) Uani 1 1 d . . . . .
O8 O 0.5206(16) 1.3869(10) 0.3942(6) 0.106(4) Uani 1 1 d . . . . .
O9 O 0.462(3) 1.1995(13) 0.3763(8) 0.159(8) Uani 1 1 d . . . . .
O10 O 0.3962(15) 1.3925(10) 0.5812(6) 0.099(4) Uani 1 1 d . . . . .
N3 N 0.4656(19) 1.2872(13) 0.4124(8) 0.095(4) Uani 1 1 d . . . . .
N4 N 0.249(2) 1.2640(17) 0.6061(7) 0.114(5) Uani 1 1 d . . . . .
C15 C 0.379(3) 1.280(2) 0.5999(9) 0.101(6) Uani 1 1 d . . . . .
C16 C 0.513(2) 1.1573(17) 0.6118(9) 0.089(5) Uani 1 1 d . . . . .
C17 C 0.587(3) 1.167(2) 0.6758(13) 0.138(9) Uani 1 1 d . . . . .
C18 C 0.475(4) 1.160(3) 0.7291(12) 0.196(15) Uani 1 1 d . . . . .
C19 C 0.735(3) 1.049(3) 0.6774(16) 0.193(15) Uani 1 1 d . . . . .
C20 C 0.648(5) 1.299(3) 0.6779(18) 0.224(18) Uani 1 1 d . . . . .
C21 C 0.210(3) 1.1387(19) 0.6278(11) 0.119(7) Uani 1 1 d . . . . .
C22 C 0.173(5) 1.052(3) 0.5755(18) 0.199(13) Uani 1 1 d . U . . .
C23 C 0.227(6) 1.059(4) 0.515(2) 0.231(18) Uani 1 1 d . U . . .
C24 C 0.140(3) 0.928(2) 0.5987(15) 0.147(9) Uani 1 1 d . U . . .
C25 C 0.106(4) 1.398(3) 0.584(2) 0.231(10) Uani 1 1 d . . . . .
C26 C 0.039(4) 1.479(4) 0.645(2) 0.231(10) Uani 1 1 d . . . . .
C27 C 0.098(4) 1.506(3) 0.690(2) 0.231(10) Uani 1 1 d . . . . .
C28 C -0.089(4) 1.611(4) 0.621(2) 0.231(10) 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 1.709(16) . ?
U1 O1 1.709(16) 2_677 ?
U1 O2 2.471(14) 2_677 ?
U1 O2 2.471(14) . ?
U1 O3 2.463(12) 2_677 ?
U1 O3 2.463(12) . ?
U1 O5 2.359(11) 2_677 ?
U1 O5 2.359(11) . ?
U1 N1 2.98(2) . ?
U1 N1 2.98(2) 2_677 ?
O2 N1 1.33(2) . ?
O3 N1 1.27(2) . ?
O4 N1 1.19(2) . ?
O5 C1 1.24(2) . ?
N2 C1 1.23(3) . ?
N2 C7 1.50(2) . ?
N2 C11 1.64(4) . ?
C1 C2 1.54(3) . ?
C2 C3 1.54(3) . ?
C3 C4 1.60(3) . ?
C3 C5 1.50(4) . ?
C3 C6 1.55(4) . ?
C7 C8 1.47(3) . ?
C8 C9 1.55(3) . ?
C8 C10 1.29(5) . ?
C11 C12 1.71(5) . ?
C12 C13 1.35(5) . ?
C12 C14 1.49(5) . ?
U2 O6 1.626(15) . ?
U2 O6 1.626(15) 2_686 ?
U2 O7 2.486(10) 2_686 ?
U2 O7 2.486(10) . ?
U2 O8 2.529(12) . ?
U2 O8 2.529(12) 2_686 ?
U2 O10 2.384(11) 2_686 ?
U2 O10 2.384(11) . ?
U2 N3 2.949(13) . ?
U2 N3 2.949(13) 2_686 ?
O7 N3 1.28(2) . ?
O8 N3 1.307(18) . ?
O9 N3 1.187(18) . ?
O10 C15 1.25(2) . ?
N4 C15 1.26(3) . ?
N4 C21 1.48(2) . ?
N4 C25 1.67(4) . ?
C15 C16 1.50(3) . ?
C16 C17 1.57(3) . ?
C17 C18 1.55(4) . ?
C17 C19 1.54(3) . ?
C17 C20 1.59(3) . ?
C21 C22 1.53(3) . ?
C22 C23 1.40(5) . ?
C22 C24 1.45(3) . ?
C25 C26 1.56(5) . ?
C26 C27 1.20(5) . ?
C26 C28 1.60(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 U1 O1 180.0 . 2_677 ?
O1 U1 O2 90.9(7) 2_677 . ?
O1 U1 O2 89.1(7) 2_677 2_677 ?
O1 U1 O2 89.1(7) . . ?
O1 U1 O2 90.9(7) . 2_677 ?
O1 U1 O3 89.5(6) 2_677 2_677 ?
O1 U1 O3 89.5(6) . . ?
O1 U1 O3 90.5(6) 2_677 . ?
O1 U1 O3 90.5(6) . 2_677 ?
O1 U1 O5 90.9(6) 2_677 . ?
O1 U1 O5 89.1(6) 2_677 2_677 ?
O1 U1 O5 90.9(6) . 2_677 ?
O1 U1 O5 89.1(6) . . ?
O1 U1 N1 90.7(6) . 2_677 ?
O1 U1 N1 90.7(6) 2_677 . ?
O1 U1 N1 89.3(6) 2_677 2_677 ?
O1 U1 N1 89.4(6) . . ?
O2 U1 O2 180.0 . 2_677 ?
O2 U1 N1 153.8(4) . 2_677 ?
O2 U1 N1 26.2(4) . . ?
O2 U1 N1 26.2(4) 2_677 2_677 ?
O2 U1 N1 153.8(4) 2_677 . ?
O3 U1 O2 50.9(4) . . ?
O3 U1 O2 129.1(4) 2_677 . ?
O3 U1 O2 129.1(4) . 2_677 ?
O3 U1 O2 50.9(4) 2_677 2_677 ?
O3 U1 O3 180.0 2_677 . ?
O3 U1 N1 155.3(4) 2_677 . ?
O3 U1 N1 24.7(4) . . ?
O3 U1 N1 24.7(4) 2_677 2_677 ?
O3 U1 N1 155.3(4) . 2_677 ?
O5 U1 O2 65.1(4) 2_677 . ?
O5 U1 O2 65.1(4) . 2_677 ?
O5 U1 O2 114.9(4) . . ?
O5 U1 O2 114.9(4) 2_677 2_677 ?
O5 U1 O3 116.0(5) . 2_677 ?
O5 U1 O3 64.0(5) . . ?
O5 U1 O3 64.0(5) 2_677 2_677 ?
O5 U1 O3 116.0(5) 2_677 . ?
O5 U1 O5 180.0(6) 2_677 . ?
O5 U1 N1 91.3(5) 2_677 . ?
O5 U1 N1 88.7(5) 2_677 2_677 ?
O5 U1 N1 91.3(5) . 2_677 ?
O5 U1 N1 88.7(5) . . ?
N1 U1 N1 180.0 2_677 . ?
N1 O2 U1 98.6(12) . . ?
N1 O3 U1 101.0(11) . . ?
C1 O5 U1 144.9(13) . . ?
O2 N1 U1 55.2(10) . . ?
O3 N1 U1 54.3(9) . . ?
O3 N1 O2 109.4(17) . . ?
O4 N1 U1 177.3(17) . . ?
O4 N1 O2 123(2) . . ?
O4 N1 O3 127.6(18) . . ?
C1 N2 C7 128(3) . . ?
C1 N2 C11 116(2) . . ?
C7 N2 C11 116(3) . . ?
O5 C1 C2 123(2) . . ?
N2 C1 O5 120(3) . . ?
N2 C1 C2 116.6(17) . . ?
C3 C2 C1 110.6(17) . . ?
C2 C3 C4 107(2) . . ?
C2 C3 C6 116(2) . . ?
C5 C3 C2 110(3) . . ?
C5 C3 C4 106(3) . . ?
C5 C3 C6 115(3) . . ?
C6 C3 C4 101(3) . . ?
C8 C7 N2 113.8(19) . . ?
C7 C8 C9 113(3) . . ?
C10 C8 C7 131(3) . . ?
C10 C8 C9 114(3) . . ?
N2 C11 C12 112(3) . . ?
C13 C12 C11 113(4) . . ?
C13 C12 C14 115(5) . . ?
C14 C12 C11 98(4) . . ?
O6 U2 O6 180.0 . 2_686 ?
O6 U2 O7 88.3(5) 2_686 2_686 ?
O6 U2 O7 91.7(5) . 2_686 ?
O6 U2 O7 91.7(5) 2_686 . ?
O6 U2 O7 88.3(5) . . ?
O6 U2 O8 89.9(5) 2_686 . ?
O6 U2 O8 90.1(5) 2_686 2_686 ?
O6 U2 O8 90.1(5) . . ?
O6 U2 O8 89.9(5) . 2_686 ?
O6 U2 O10 86.6(6) . . ?
O6 U2 O10 93.4(6) 2_686 . ?
O6 U2 O10 86.6(6) 2_686 2_686 ?
O6 U2 O10 93.4(6) . 2_686 ?
O6 U2 N3 88.8(5) . . ?
O6 U2 N3 91.2(5) . 2_686 ?
O6 U2 N3 91.2(5) 2_686 . ?
O6 U2 N3 88.8(5) 2_686 2_686 ?
O7 U2 O7 180.0 . 2_686 ?
O7 U2 O8 51.7(4) 2_686 2_686 ?
O7 U2 O8 51.7(4) . . ?
O7 U2 O8 128.3(4) 2_686 . ?
O7 U2 O8 128.3(4) . 2_686 ?
O7 U2 N3 25.5(4) 2_686 2_686 ?
O7 U2 N3 154.5(4) 2_686 . ?
O7 U2 N3 154.5(4) . 2_686 ?
O7 U2 N3 25.5(4) . . ?
O8 U2 O8 180.0 2_686 . ?
O8 U2 N3 153.8(4) . 2_686 ?
O8 U2 N3 153.8(4) 2_686 . ?
O8 U2 N3 26.2(4) . . ?
O8 U2 N3 26.2(4) 2_686 2_686 ?
O10 U2 O7 115.8(4) . 2_686 ?
O10 U2 O7 64.2(4) 2_686 2_686 ?
O10 U2 O7 64.2(4) . . ?
O10 U2 O7 115.8(4) 2_686 . ?
O10 U2 O8 64.1(4) . 2_686 ?
O10 U2 O8 115.9(4) 2_686 2_686 ?
O10 U2 O8 115.9(4) . . ?
O10 U2 O8 64.1(4) 2_686 . ?
O10 U2 O10 180.0(4) . 2_686 ?
O10 U2 N3 90.3(4) . 2_686 ?
O10 U2 N3 89.7(4) . . ?
O10 U2 N3 90.3(4) 2_686 . ?
O10 U2 N3 89.7(4) 2_686 2_686 ?
N3 U2 N3 180.0(5) . 2_686 ?
N3 O7 U2 97.9(8) . . ?
N3 O8 U2 95.2(10) . . ?
C15 O10 U2 144.4(12) . . ?
O7 N3 U2 56.6(7) . . ?
O7 N3 O8 115.2(12) . . ?
O8 N3 U2 58.6(7) . . ?
O9 N3 U2 175.7(16) . . ?
O9 N3 O7 125.5(16) . . ?
O9 N3 O8 119.0(18) . . ?
C15 N4 C21 127(2) . . ?
C15 N4 C25 116(2) . . ?
C21 N4 C25 117(2) . . ?
O10 C15 N4 121(2) . . ?
O10 C15 C16 121.5(19) . . ?
N4 C15 C16 117.6(19) . . ?
C15 C16 C17 112.5(14) . . ?
C16 C17 C20 111(2) . . ?
C18 C17 C16 109(2) . . ?
C18 C17 C20 115(3) . . ?
C19 C17 C16 107.1(19) . . ?
C19 C17 C18 113(3) . . ?
C19 C17 C20 102(3) . . ?
N4 C21 C22 114(2) . . ?
C23 C22 C21 121(3) . . ?
C23 C22 C24 122(3) . . ?
C24 C22 C21 112(3) . . ?
C26 C25 N4 107(3) . . ?
C25 C26 C28 105(3) . . ?
C27 C26 C25 132(4) . . ?
C27 C26 C28 111(3) . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_date_sample_data_collection 2015-12-07
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.412
_oxdiff_exptl_absorpt_empirical_full_min 0.101
####################################################################### 
# 
# 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_kannan31_3
_audit_block_doi                 10.5517/ccdc.csd.cc1kkr73
_database_code_depnum_ccdc_archive 'CCDC 1447025'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/C7DT02760E 2017
_audit_update_record             
;
2016-01-13 deposited with the CCDC.
2017-11-24 downloaded from the CCDC.
;
_audit_creation_date             2016-01-12
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C26 H54 N4 O10 U'
_chemical_formula_sum            'C26 H54 N4 O10 U'
_chemical_formula_weight         820.76
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C26 H54 N4 O10 U'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -4.3638 13.4090 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
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                   10.4689(2)
_cell_length_b                   10.8223(2)
_cell_length_c                   15.8019(3)
_cell_angle_alpha                90
_cell_angle_beta                 95.238(2)
_cell_angle_gamma                90
_cell_volume                     1782.83(6)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    4043
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      73.0650
_cell_measurement_theta_min      4.8530
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    13.249
_exptl_absorpt_correction_T_max  0.256
_exptl_absorpt_correction_T_min  0.062
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.529
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             820
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
3 -3 8 0.1987
-4 -4 6 0.1269
-4 5 -1 0.1731
-1 4 -8 0.2071
-1 -3 9 0.1448
-1 -5 7 0.1614
1 6 5 0.1526
0 6 5 0.1488
4 -2 7 0.2037
-1 5 7 0.1342
1 -7 -4 0.1016
0 -6 -5 0.1097
-6 0 6 0.0790
6 1 -4 0.1112
4 3 -7 0.1054
-5 2 7 0.0816
-5 2 -6 0.2526
0 6 -5 0.1417
6 -1 -6 0.1060

_exptl_crystal_size_max          0.448
_exptl_crystal_size_mid          0.297
_exptl_crystal_size_min          0.19
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
2.6358 -3.2528 7.7801 0.3242 0.2702 -0.9066
-4.0001 -4.0000 6.0000 0.9618 0.1205 -0.1286
-4.0003 4.9998 -1.0000 -0.0833 0.4053 0.8397
-1.0001 3.9998 -7.9999 -0.5552 -0.2321 0.7864
-1.0000 -2.9998 8.9999 0.7005 0.4123 -0.5446
-0.9999 -4.9999 6.9999 0.7965 0.0826 -0.5820
0.9998 6.0002 4.9999 -0.4229 0.9065 0.0506
-0.0003 6.0002 4.9999 -0.3263 0.9142 0.1622
4.0002 -1.9997 6.9999 0.0543 0.3140 -0.9337
-1.0003 5.0002 6.9999 -0.0667 0.9817 0.1050
1.0003 -7.0001 -3.9999 0.3543 -0.9368 -0.3924
0.0003 -6.0002 -4.9999 0.3263 -0.9142 -0.1622
-5.9912 0.0005 5.9982 0.8088 0.4954 0.3685
5.9918 1.0007 -3.9970 -0.8186 -0.2554 -0.3998
3.9912 2.9987 -6.9968 -0.9127 -0.2852 0.1106
-4.9925 2.0017 7.0005 0.5780 0.7428 0.3444
-5.0002 1.9997 -6.0000 0.0807 -0.2314 0.9952
-0.0054 5.9985 -4.9958 -0.7087 0.1651 0.6625
5.7840 -1.1740 -5.8635 -0.6823 -0.5892 -0.4327

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0856
_diffrn_reflns_av_unetI/netI     0.0748
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.954
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            6910
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.302
_diffrn_reflns_theta_min         4.870
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 4.1600
_diffrn_detector_type            Titan
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -15.00  63.00   1.00    1.00    --   43.29 -57.00 -90.00   78
  2  ω     20.00 110.00   1.00    1.00    --  102.90 -95.00 -60.00   90
  3  ω     26.00  97.00   1.00    1.00    --   43.29  57.00-150.00   71
  4  ω    117.00 158.00   1.00    1.00    --  102.90  61.00 -90.00   41
  5  ω     74.00 155.00   1.00    1.00    --  102.90  77.00-120.00   81
  6  ω     72.00 158.00   1.00    1.00    --  102.90  77.00   0.00   86
  7  ω     97.00 144.00   1.00    1.00    --  102.90 126.00  90.00   47
  8  ω     87.00 113.00   1.00    1.00    --   43.29 126.00 120.00   26
  9  ω     81.00 149.00   1.00    1.00    --  102.90  61.00 150.00   68
 10  ω   -104.00 -73.00   1.00    1.00    --  -43.29-126.00  30.00   31
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Titan'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0966441000
_diffrn_orient_matrix_UB_12      -0.0863156000
_diffrn_orient_matrix_UB_13      0.0383210000
_diffrn_orient_matrix_UB_21      -0.0076638000
_diffrn_orient_matrix_UB_22      0.0899184000
_diffrn_orient_matrix_UB_23      0.0749267000
_diffrn_orient_matrix_UB_31      -0.1115609000
_diffrn_orient_matrix_UB_32      0.0686922000
_diffrn_orient_matrix_UB_33      -0.0500093000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2632
_reflns_number_total             3412
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         5.693
_refine_diff_density_min         -2.113
_refine_diff_density_rms         0.355
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     194
_refine_ls_number_reflns         3412
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1047
_refine_ls_R_factor_gt           0.0952
_refine_ls_restrained_S_all      1.053
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1707P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2337
_refine_ls_wR_factor_ref         0.2500
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C7(H7), C11(H11)
2.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C10(H10A,H10B)
2.c Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C8(H8A,H8B,H8C), C9(H9A,
 H9B,H9C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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 0.0000 0.5000 0.0000 0.0445(3) Uani 1 2 d S T P . .
O1 O 0.1620(7) 0.4448(8) 0.0158(5) 0.0572(18) Uani 1 1 d . . . . .
O2 O 0.0424(7) 0.6544(8) 0.1054(5) 0.072(2) Uani 1 1 d . . . . .
O3 O -0.0282(10) 0.4292(12) 0.1500(6) 0.090(3) Uani 1 1 d . . . . .
O4 O -0.0722(10) 0.2955(9) 0.0519(7) 0.083(3) Uani 1 1 d . . . . .
O5 O -0.0772(13) 0.2426(15) 0.1881(10) 0.119(5) Uani 1 1 d . . . . .
N1 N -0.0617(11) 0.3156(13) 0.1309(10) 0.087(4) Uani 1 1 d . . . . .
N2 N -0.0331(9) 0.7906(9) 0.1942(5) 0.043(2) Uani 1 1 d . . . . .
C1 C 0.0615(10) 0.7296(8) 0.1642(6) 0.044(2) Uani 1 1 d . . . . .
C2 C 0.2036(13) 0.7496(10) 0.1966(7) 0.057(3) Uani 1 1 d . . . . .
C3 C 0.2293(13) 0.7211(13) 0.2913(9) 0.067(4) Uani 1 1 d . . . . .
H3A H 0.2102 0.7927 0.3237 0.101 Uiso 1 1 calc GR . . . .
H3B H 0.3179 0.6991 0.3038 0.101 Uiso 1 1 calc GR . . . .
H3C H 0.1760 0.6535 0.3058 0.101 Uiso 1 1 calc GR . . . .
C4 C 0.2424(13) 0.8833(12) 0.1749(9) 0.074(3) Uani 1 1 d . . . . .
H4A H 0.2297 0.8956 0.1146 0.111 Uiso 1 1 calc GR . . . .
H4B H 0.3311 0.8963 0.1940 0.111 Uiso 1 1 calc GR . . . .
H4C H 0.1904 0.9408 0.2028 0.111 Uiso 1 1 calc GR . . . .
C5 C 0.2867(13) 0.6613(12) 0.1488(8) 0.081(4) Uani 1 1 d . . . . .
H5A H 0.2602 0.5777 0.1573 0.122 Uiso 1 1 calc GR . . . .
H5B H 0.3750 0.6708 0.1699 0.122 Uiso 1 1 calc GR . . . .
H5C H 0.2767 0.6804 0.0892 0.122 Uiso 1 1 calc GR . . . .
C6 C -0.1685(12) 0.7737(11) 0.1526(8) 0.062(3) Uani 1 1 d . . . . .
H6A H -0.1670 0.7085 0.1106 0.074 Uiso 1 1 calc R . . . .
H6B H -0.2222 0.7456 0.1956 0.074 Uiso 1 1 calc R . . . .
C7 C -0.2302(13) 0.8850(13) 0.1101(8) 0.076(4) Uani 1 1 d . . . . .
H7 H -0.2333 0.9498 0.1532 0.091 Uiso 1 1 calc R . . . .
C8 C -0.3629(17) 0.858(2) 0.0768(15) 0.146(9) Uani 1 1 d . . . . .
H8A H -0.3624 0.8025 0.0291 0.220 Uiso 1 1 calc GR . . . .
H8B H -0.4057 0.9329 0.0590 0.220 Uiso 1 1 calc GR . . . .
H8C H -0.4074 0.8193 0.1204 0.220 Uiso 1 1 calc GR . . . .
C9 C -0.149(2) 0.933(2) 0.0418(13) 0.139(8) Uani 1 1 d . . . . .
H9A H -0.0788 0.9802 0.0679 0.209 Uiso 1 1 calc GR . . . .
H9B H -0.2012 0.9843 0.0029 0.209 Uiso 1 1 calc GR . . . .
H9C H -0.1171 0.8644 0.0116 0.209 Uiso 1 1 calc GR . . . .
C10 C -0.0239(10) 0.8826(10) 0.2608(7) 0.054(2) Uani 1 1 d . . . . .
H10A H -0.0442 0.9627 0.2356 0.065 Uiso 1 1 calc R . . . .
H10B H 0.0641 0.8856 0.2860 0.065 Uiso 1 1 calc R . . . .
C11 C -0.1123(11) 0.8598(13) 0.3317(7) 0.068(3) Uani 1 1 d . . . . .
H11 H -0.2017 0.8691 0.3083 0.082 Uiso 1 1 calc R . . . .
C12 C -0.0935(16) 0.730(2) 0.3693(9) 0.114(7) Uani 1 1 d . . . . .
H12A H -0.0963 0.6704 0.3241 0.171 Uiso 1 1 calc GR . . . .
H12B H -0.1605 0.7126 0.4052 0.171 Uiso 1 1 calc GR . . . .
H12C H -0.0118 0.7253 0.4021 0.171 Uiso 1 1 calc GR . . . .
C13 C -0.081(3) 0.960(2) 0.3973(15) 0.123(8) Uani 1 1 d . . . . .
H13A H -0.0085 0.9350 0.4352 0.184 Uiso 1 1 calc GR . . . .
H13B H -0.1534 0.9735 0.4292 0.184 Uiso 1 1 calc GR . . . .
H13C H -0.0606 1.0353 0.3692 0.184 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 O1 1.794(7) 3_565 ?
U1 O1 1.794(7) . ?
U1 O2 2.372(7) 3_565 ?
U1 O2 2.372(7) . ?
U1 O3 2.534(10) . ?
U1 O3 2.534(10) 3_565 ?
U1 O4 2.500(9) . ?
U1 O4 2.500(9) 3_565 ?
U1 N1 2.987(13) . ?
U1 N1 2.987(13) 3_565 ?
O2 C1 1.238(11) . ?
O3 N1 1.306(17) . ?
O4 N1 1.263(15) . ?
O5 N1 1.223(16) . ?
N2 C1 1.314(13) . ?
N2 C6 1.518(15) . ?
N2 C10 1.446(12) . ?
C1 C2 1.544(16) . ?
C2 C3 1.53(2) . ?
C2 C4 1.550(17) . ?
C2 C5 1.536(16) . ?
C6 C7 1.496(18) . ?
C7 C8 1.47(2) . ?
C7 C9 1.52(2) . ?
C10 C11 1.536(14) . ?
C11 C12 1.53(2) . ?
C11 C13 1.52(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 U1 O1 180.0 3_565 . ?
O1 U1 O2 88.7(3) . 3_565 ?
O1 U1 O2 91.3(3) 3_565 3_565 ?
O1 U1 O2 91.3(3) . . ?
O1 U1 O2 88.7(3) 3_565 . ?
O1 U1 O3 87.6(3) . . ?
O1 U1 O3 87.6(3) 3_565 3_565 ?
O1 U1 O3 92.4(3) 3_565 . ?
O1 U1 O3 92.4(3) . 3_565 ?
O1 U1 O4 91.7(4) 3_565 . ?
O1 U1 O4 88.3(4) 3_565 3_565 ?
O1 U1 O4 88.3(4) . . ?
O1 U1 O4 91.7(4) . 3_565 ?
O1 U1 N1 86.7(3) 3_565 3_565 ?
O1 U1 N1 93.3(3) 3_565 . ?
O1 U1 N1 86.7(3) . . ?
O1 U1 N1 93.3(3) . 3_565 ?
O2 U1 O2 180.0 . 3_565 ?
O2 U1 O3 114.4(4) 3_565 . ?
O2 U1 O3 65.6(4) . . ?
O2 U1 O3 65.6(4) 3_565 3_565 ?
O2 U1 O3 114.4(4) . 3_565 ?
O2 U1 O4 64.1(4) 3_565 . ?
O2 U1 O4 64.1(4) . 3_565 ?
O2 U1 O4 115.9(4) . . ?
O2 U1 O4 115.9(4) 3_565 3_565 ?
O2 U1 N1 91.3(4) . . ?
O2 U1 N1 88.7(4) . 3_565 ?
O2 U1 N1 91.3(4) 3_565 3_565 ?
O2 U1 N1 88.7(4) 3_565 . ?
O3 U1 O3 180.0 3_565 . ?
O3 U1 N1 154.3(4) . 3_565 ?
O3 U1 N1 25.7(4) 3_565 3_565 ?
O3 U1 N1 25.7(4) . . ?
O3 U1 N1 154.3(4) 3_565 . ?
O4 U1 O3 50.3(4) 3_565 3_565 ?
O4 U1 O3 129.7(4) 3_565 . ?
O4 U1 O3 129.7(4) . 3_565 ?
O4 U1 O3 50.3(4) . . ?
O4 U1 O4 180.0 3_565 . ?
O4 U1 N1 155.4(3) 3_565 . ?
O4 U1 N1 24.6(3) 3_565 3_565 ?
O4 U1 N1 24.6(3) . . ?
O4 U1 N1 155.4(3) . 3_565 ?
N1 U1 N1 180.0 . 3_565 ?
C1 O2 U1 175.8(9) . . ?
N1 O3 U1 96.9(8) . . ?
N1 O4 U1 99.8(8) . . ?
O3 N1 U1 57.4(6) . . ?
O4 N1 U1 55.6(7) . . ?
O4 N1 O3 112.8(11) . . ?
O5 N1 U1 174.6(12) . . ?
O5 N1 O3 119.3(17) . . ?
O5 N1 O4 127.9(17) . . ?
C1 N2 C6 119.2(8) . . ?
C1 N2 C10 127.4(9) . . ?
C10 N2 C6 113.3(8) . . ?
O2 C1 N2 121.7(9) . . ?
O2 C1 C2 115.2(9) . . ?
N2 C1 C2 123.0(8) . . ?
C1 C2 C4 108.7(10) . . ?
C3 C2 C1 112.0(9) . . ?
C3 C2 C4 112.3(10) . . ?
C3 C2 C5 107.4(11) . . ?
C5 C2 C1 108.8(10) . . ?
C5 C2 C4 107.5(11) . . ?
C7 C6 N2 116.5(10) . . ?
C6 C7 C9 110.3(13) . . ?
C8 C7 C6 110.7(14) . . ?
C8 C7 C9 112.5(17) . . ?
N2 C10 C11 114.6(9) . . ?
C12 C11 C10 111.4(11) . . ?
C13 C11 C10 106.0(12) . . ?
C13 C11 C12 112.3(15) . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_date_sample_data_collection 2015-12-03
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.553
_oxdiff_exptl_absorpt_empirical_full_min 0.150
