# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# 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_ajr4
_database_code_depnum_ccdc_archive 'CCDC 1872635'
_audit_update_record             
;
2018-10-10 deposited with the CCDC.
2019-01-02 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            'C36 H90 K N5 O6 Si6 U'
_chemical_formula_weight         1134.79

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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 '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      trigonal
_space_group_IT_number           155
_space_group_name_H-M_alt        'R 3 2 :H'
_space_group_name_Hall           'R 3 2"'

_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'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+1/3'
'x-y+2/3, -y+1/3, -z+1/3'
'-x+2/3, -x+y+1/3, -z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+2/3'
'x-y+1/3, -y+2/3, -z+2/3'
'-x+1/3, -x+y+2/3, -z+2/3'

_cell_length_a                   18.4169(17)
_cell_length_b                   18.4169(17)
_cell_length_c                   18.1996(17)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     5346.0(11)
_cell_formula_units_Z            3
_cell_measurement_temperature    88(2)
_cell_measurement_reflns_used    7989
_cell_measurement_theta_min      2.21
_cell_measurement_theta_max      25.78

_exptl_crystal_description       irregular
_exptl_crystal_colour            Black
_exptl_crystal_density_meas      not_measured
_exptl_crystal_density_method    not_measured
_exptl_crystal_density_diffrn    1.057
_exptl_crystal_F_000             1752
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.389
_exptl_crystal_size_mid          0.318
_exptl_crystal_size_min          0.214
_exptl_absorpt_coefficient_mu    2.468
_shelx_estimated_absorpt_T_min   0.447
_shelx_estimated_absorpt_T_max   0.620
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3334
_exptl_absorpt_correction_T_max  0.4296
_exptl_absorpt_process_details   'Bruker SADABS 2014/5'
_exptl_absorpt_special_details   
; 
Reflections not merged 
19712 Corrected reflections written to file ajr4s.hkl 
Estimated minimum and maximum transmission:  0.3334  0.4296 
The ratio (0.7761) 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      88(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            19702
_diffrn_reflns_av_unetI/netI     0.0213
_diffrn_reflns_av_R_equivalents  0.0373
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.698
_diffrn_reflns_theta_max         26.384
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             2443
_reflns_number_gt                2317
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.823
_reflns_Friedel_fraction_max     0.999
_reflns_Friedel_fraction_full    1.000

_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 black crystal of approximate dimensions 0.214 x 0.318 x 0.389 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 (60 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 systematic 
absences were consistent with the hexagonal space group R32.  The trigonal 
space group R32 was assigned and 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.  Several atoms were 
disordered and included with partial site-occupancy-factors.

Least-squares analysis yielded wR2 = 0.0590 and Goof = 1.049 for 110 
variables refined against 2443 data (0.80 Å), R1 = 0.0238 for those 2317 
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 THF solvent was present.  The SQUEEZE routine in 
the PLATON program package was used to account for the electrons in the 
solvent accessible voids.  The structure was refined as a two-component 
inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0389P)²+0.5323P] 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_abs_structure_details 
; 
 Refined as an inversion twin. 
;
_refine_ls_abs_structure_Flack   0.008(7)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         2443
_refine_ls_number_parameters     110
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0266
_refine_ls_R_factor_gt           0.0238
_refine_ls_wR_factor_ref         0.0590
_refine_ls_wR_factor_gt          0.0583
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_restrained_S_all      1.049
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 1.0000 1.0000 0.47740(2) 0.02179(12) Uani 0.5 3 d S T P A 1
Si1 Si 0.94565(8) 0.80204(7) 0.56765(5) 0.0374(3) Uani 1 1 d . . . . .
N1 N 1.0000 0.8731(2) 0.5000 0.0316(9) Uani 1 2 d S T P A .
C1 C 1.0150(3) 0.7967(3) 0.64024(16) 0.0428(9) Uani 1 1 d . . . . .
H1A H 1.0472 0.7725 0.6193 0.064 Uiso 1 1 calc R U . . .
H1B H 0.9805 0.7615 0.6809 0.064 Uiso 1 1 calc R U . . .
H1C H 1.0536 0.8533 0.6585 0.064 Uiso 1 1 calc R U . . .
C2 C 0.8885(8) 0.8492(7) 0.6173(6) 0.041(2) Uani 0.5 1 d . . P B 1
H2A H 0.9292 0.9055 0.6348 0.061 Uiso 0.5 1 calc R U P B 1
H2B H 0.8578 0.8137 0.6592 0.061 Uiso 0.5 1 calc R U P B 1
H2C H 0.8490 0.8528 0.5835 0.061 Uiso 0.5 1 calc R U P B 1
C2A C 0.8563(8) 0.8107(8) 0.6130(7) 0.047(3) Uani 0.5 1 d . . P B 2
H2D H 0.8796 0.8630 0.6412 0.070 Uiso 0.5 1 calc R U P B 2
H2E H 0.8250 0.7629 0.6461 0.070 Uiso 0.5 1 calc R U P B 2
H2F H 0.8185 0.8106 0.5750 0.070 Uiso 0.5 1 calc R U P B 2
C3 C 0.869(2) 0.689(2) 0.530(2) 0.049(5) Uani 0.5 1 d . . P B 2
H3A H 0.8330 0.6921 0.4919 0.073 Uiso 0.5 1 calc R U P B 2
H3B H 0.8336 0.6534 0.5704 0.073 Uiso 0.5 1 calc R U P B 2
H3C H 0.9012 0.6649 0.5095 0.073 Uiso 0.5 1 calc R U P B 2
C3A C 0.890(3) 0.697(2) 0.535(2) 0.069(9) Uani 0.5 1 d . . P B 1
H3D H 0.8494 0.6918 0.4975 0.104 Uiso 0.5 1 calc R U P B 1
H3E H 0.8593 0.6591 0.5763 0.104 Uiso 0.5 1 calc R U P B 1
H3F H 0.9290 0.6813 0.5144 0.104 Uiso 0.5 1 calc R U P B 1
K1 K 0.6667 0.3333 0.3333 0.0236(3) Uani 1 6 d S T P . .
O1 O 0.80982(16) 0.45714(16) 0.40855(10) 0.0348(6) Uani 1 1 d . . . . .
N2 N 0.6667 0.3333 0.49523(18) 0.0280(8) Uani 1 3 d S T P . .
C4 C 0.75396(19) 0.3838(3) 0.52131(14) 0.0343(8) Uani 1 1 d . . . . .
H4A H 0.7834 0.3520 0.5124 0.041 Uiso 1 1 calc R U . . .
H4B H 0.7533 0.3919 0.5750 0.041 Uiso 1 1 calc R U . . .
C5 C 0.8027(2) 0.4681(2) 0.48546(14) 0.0367(9) Uani 1 1 d . . . . .
H5A H 0.7737 0.5005 0.4932 0.044 Uiso 1 1 calc R U . . .
H5B H 0.8592 0.4996 0.5077 0.044 Uiso 1 1 calc R U . . .
C6 C 0.8563(3) 0.5362(2) 0.37254(18) 0.0434(9) Uani 1 1 d . . . . .
H6A H 0.9112 0.5700 0.3971 0.052 Uiso 1 1 calc R U . . .
H6B H 0.8253 0.5672 0.3756 0.052 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 U1 0.8226(6) 4_556 ?
U1 N1 2.372(4) . ?
U1 N1 2.372(4) 2_765 ?
U1 N1 2.372(4) 3_675 ?
U1 C2 3.033(12) 4_556 ?
U1 C2 3.033(11) 6_766 ?
U1 C2 3.033(11) 5_676 ?
U1 Si1 3.3640(11) 6_766 ?
U1 Si1 3.3641(11) 5_676 ?
U1 Si1 3.3642(11) 4_556 ?
Si1 N1 1.709(2) . ?
Si1 C3A 1.78(4) . ?
Si1 C1 1.874(4) . ?
Si1 C2 1.895(12) . ?
Si1 C2A 1.918(13) . ?
Si1 C3 1.96(3) . ?
Si1 U1 3.3641(11) 4_556 ?
N1 Si1 1.709(2) 6_766 ?
N1 U1 2.372(4) 4_556 ?
C2 U1 3.033(11) 4_556 ?
K1 O1 2.830(2) 18_655 ?
K1 O1 2.830(2) 3_665 ?
K1 O1 2.831(2) 16_545 ?
K1 O1 2.831(2) . ?
K1 O1 2.831(2) 2_655 ?
K1 O1 2.831(2) 17 ?
K1 N2 2.946(3) . ?
K1 N2 2.947(3) 16_545 ?
O1 C6 1.427(4) . ?
O1 C5 1.430(3) . ?
N2 C4 1.476(3) 3_665 ?
N2 C4 1.476(3) 2_655 ?
N2 C4 1.476(3) . ?
C4 C5 1.499(6) . ?
C6 C6 1.488(7) 16_545 ?

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
U1 U1 N1 80.016(19) 4_556 . ?
U1 U1 N1 80.02(2) 4_556 2_765 ?
N1 U1 N1 117.060(11) . 2_765 ?
U1 U1 N1 80.02(2) 4_556 3_675 ?
N1 U1 N1 117.060(12) . 3_675 ?
N1 U1 N1 117.060(11) 2_765 3_675 ?
U1 U1 C2 124.6(2) 4_556 4_556 ?
N1 U1 C2 83.3(2) . 4_556 ?
N1 U1 C2 152.0(2) 2_765 4_556 ?
N1 U1 C2 62.0(2) 3_675 4_556 ?
U1 U1 C2 124.6(2) 4_556 6_766 ?
N1 U1 C2 62.0(2) . 6_766 ?
N1 U1 C2 83.3(2) 2_765 6_766 ?
N1 U1 C2 152.0(2) 3_675 6_766 ?
C2 U1 C2 90.9(3) 4_556 6_766 ?
U1 U1 C2 124.6(2) 4_556 5_676 ?
N1 U1 C2 152.0(2) . 5_676 ?
N1 U1 C2 62.0(2) 2_765 5_676 ?
N1 U1 C2 83.3(2) 3_675 5_676 ?
C2 U1 C2 90.9(3) 4_556 5_676 ?
C2 U1 C2 90.9(3) 6_766 5_676 ?
U1 U1 Si1 104.107(16) 4_556 6_766 ?
N1 U1 Si1 28.53(2) . 6_766 ?
N1 U1 Si1 106.43(2) 2_765 6_766 ?
N1 U1 Si1 136.26(2) 3_675 6_766 ?
C2 U1 Si1 82.0(2) 4_556 6_766 ?
C2 U1 Si1 34.0(2) 6_766 6_766 ?
C2 U1 Si1 123.6(2) 5_676 6_766 ?
U1 U1 Si1 104.107(16) 4_556 5_676 ?
N1 U1 Si1 136.26(2) . 5_676 ?
N1 U1 Si1 28.53(2) 2_765 5_676 ?
N1 U1 Si1 106.43(2) 3_675 5_676 ?
C2 U1 Si1 123.6(2) 4_556 5_676 ?
C2 U1 Si1 82.0(2) 6_766 5_676 ?
C2 U1 Si1 34.0(2) 5_676 5_676 ?
Si1 U1 Si1 114.262(12) 6_766 5_676 ?
U1 U1 Si1 104.107(16) 4_556 4_556 ?
N1 U1 Si1 106.43(2) . 4_556 ?
N1 U1 Si1 136.26(2) 2_765 4_556 ?
N1 U1 Si1 28.53(2) 3_675 4_556 ?
C2 U1 Si1 34.0(2) 4_556 4_556 ?
C2 U1 Si1 123.6(2) 6_766 4_556 ?
C2 U1 Si1 82.0(2) 5_676 4_556 ?
Si1 U1 Si1 114.262(12) 6_766 4_556 ?
Si1 U1 Si1 114.259(12) 5_676 4_556 ?
N1 Si1 C3A 113.3(13) . . ?
N1 Si1 C1 113.24(15) . . ?
C3A Si1 C1 102.4(13) . . ?
N1 Si1 C2 103.8(4) . . ?
C3A Si1 C2 120.2(15) . . ?
C1 Si1 C2 103.7(4) . . ?
N1 Si1 C2A 116.4(4) . . ?
C1 Si1 C2A 109.7(4) . . ?
N1 Si1 C3 113.4(12) . . ?
C1 Si1 C3 109.8(11) . . ?
C2A Si1 C3 92.5(13) . . ?
N1 Si1 U1 41.52(12) . 4_556 ?
C3A Si1 U1 142.8(13) . 4_556 ?
C1 Si1 U1 112.80(14) . 4_556 ?
C2 Si1 U1 63.4(3) . 4_556 ?
Si1 N1 Si1 123.5(3) 6_766 . ?
Si1 N1 U1 109.95(11) 6_766 . ?
Si1 N1 U1 126.23(14) . . ?
Si1 N1 U1 126.23(14) 6_766 4_556 ?
Si1 N1 U1 109.95(11) . 4_556 ?
U1 N1 U1 19.97(4) . 4_556 ?
Si1 C2 U1 82.6(4) . 4_556 ?
O1 K1 O1 116.17(11) 18_655 3_665 ?
O1 K1 O1 98.58(5) 18_655 16_545 ?
O1 K1 O1 140.27(11) 3_665 16_545 ?
O1 K1 O1 140.27(11) 18_655 . ?
O1 K1 O1 98.58(5) 3_665 . ?
O1 K1 O1 59.44(8) 16_545 . ?
O1 K1 O1 59.44(8) 18_655 2_655 ?
O1 K1 O1 98.58(5) 3_665 2_655 ?
O1 K1 O1 116.17(11) 16_545 2_655 ?
O1 K1 O1 98.58(5) . 2_655 ?
O1 K1 O1 98.58(5) 18_655 17 ?
O1 K1 O1 59.44(8) 3_665 17 ?
O1 K1 O1 98.58(5) 16_545 17 ?
O1 K1 O1 116.17(11) . 17 ?
O1 K1 O1 140.27(11) 2_655 17 ?
O1 K1 N2 118.92(4) 18_655 . ?
O1 K1 N2 61.08(4) 3_665 . ?
O1 K1 N2 118.92(4) 16_545 . ?
O1 K1 N2 61.08(4) . . ?
O1 K1 N2 61.08(4) 2_655 . ?
O1 K1 N2 118.92(4) 17 . ?
O1 K1 N2 61.08(4) 18_655 16_545 ?
O1 K1 N2 118.92(4) 3_665 16_545 ?
O1 K1 N2 61.08(4) 16_545 16_545 ?
O1 K1 N2 118.92(4) . 16_545 ?
O1 K1 N2 118.92(4) 2_655 16_545 ?
O1 K1 N2 61.08(4) 17 16_545 ?
N2 K1 N2 180.0 . 16_545 ?
C6 O1 C5 110.9(3) . . ?
C6 O1 K1 116.22(18) . . ?
C5 O1 K1 118.2(2) . . ?
C4 N2 C4 110.18(16) 3_665 2_655 ?
C4 N2 C4 110.18(16) 3_665 . ?
C4 N2 C4 110.18(16) 2_655 . ?
C4 N2 K1 108.75(16) 3_665 . ?
C4 N2 K1 108.75(16) 2_655 . ?
C4 N2 K1 108.76(16) . . ?
N2 C4 C5 114.3(3) . . ?
O1 C5 C4 109.3(3) . . ?
O1 C6 C6 109.7(3) . 16_545 ?

_refine_diff_density_max         1.078
_refine_diff_density_min         -0.449
_refine_diff_density_rms         0.050



_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Heat-sensitive,Oxygen-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_maa7
_database_code_depnum_ccdc_archive 'CCDC 1872636'
_audit_update_record             
;
2018-10-10 deposited with the CCDC.
2019-01-02 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            'C49 H83 K N2 O7 U'
_chemical_formula_weight         1089.30

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'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

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

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

_cell_length_a                   30.199(5)
_cell_length_b                   13.568(2)
_cell_length_c                   30.609(7)
_cell_angle_alpha                90
_cell_angle_beta                 114.7838(17)
_cell_angle_gamma                90
_cell_volume                     11387(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    133(2)
_cell_measurement_reflns_used    9977
_cell_measurement_theta_min      2.42
_cell_measurement_theta_max      26.99

_exptl_crystal_description       irregular
_exptl_crystal_colour            black
_exptl_crystal_density_meas      not_measured
_exptl_crystal_density_method    not_measured
_exptl_crystal_density_diffrn    1.271
_exptl_crystal_F_000             4464
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.345
_exptl_crystal_size_mid          0.195
_exptl_crystal_size_min          0.141
_exptl_absorpt_coefficient_mu    2.967
_shelx_estimated_absorpt_T_min   0.428
_shelx_estimated_absorpt_T_max   0.680
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5981
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_process_details   'Bruker SADABS 2014/5'
_exptl_absorpt_special_details   
; 
Reflections not merged 
65603 Corrected reflections written to file maa7s.hkl 
Estimated minimum and maximum transmission:  0.5981  0.7455 
The ratio (0.8023) 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            64077
_diffrn_reflns_av_unetI/netI     0.0490
_diffrn_reflns_av_R_equivalents  0.0621
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_theta_min         1.466
_diffrn_reflns_theta_max         27.174
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             12621
_reflns_number_gt                9615
_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 black crystal of approximate dimensions 0.141 x 0.195 x 0.345 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 (30 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.  There was one molecule of tetrahydrofuran solvent present.

Least-squares analysis yielded wR2 = 0.0864 and Goof = 1.009 for 528 variables 
refined against 12621 data (0.78 Å), R1 = 0.0362 for those 9615 data 
with I > 2.0sigma(I).

There were 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 
additional tetrahydrofuran solvent was present.  The SQUEEZE routine in the PLATON 
program package was used to account for the electrons in the solvent accessible voids.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0428P)²+20.4674P] 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         12621
_refine_ls_number_parameters     528
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0582
_refine_ls_R_factor_gt           0.0362
_refine_ls_wR_factor_ref         0.0864
_refine_ls_wR_factor_gt          0.0795
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_restrained_S_all      1.009
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000

# start Validation Reply Form
_vrf_PLAT360_maa7                
;
PROBLEM: Short  C(sp3)-C(sp3) Bond   C48    -   C49    ..       1.25 Ang.  
RESPONSE: ...Short distance is due to poorly resolved solvent molecule
;
# 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 0.67149(2) 0.69821(2) 0.83103(2) 0.01862(5) Uani 1 1 d . . . . .
C1 C 0.63105(15) 0.6349(4) 0.89447(15) 0.0305(11) Uani 1 1 d . . . . .
C2 C 0.58868(14) 0.6657(3) 0.85446(14) 0.0261(10) Uani 1 1 d . . . . .
C3 C 0.59121(14) 0.7697(3) 0.85003(14) 0.0257(10) Uani 1 1 d . . . . .
C4 C 0.63506(14) 0.8031(4) 0.88716(14) 0.0287(10) Uani 1 1 d . . . . .
C5 C 0.65888(15) 0.7201(4) 0.91450(14) 0.0299(11) Uani 1 1 d . . . . .
H5A H 0.6862 0.7234 0.9474 0.036 Uiso 1 1 calc R U . . .
C6 C 0.64162(17) 0.5316(4) 0.91437(18) 0.0457(14) Uani 1 1 d . . . . .
H6A H 0.6671 0.5335 0.9473 0.069 Uiso 1 1 calc R U . . .
H6B H 0.6527 0.4914 0.8943 0.069 Uiso 1 1 calc R U . . .
H6C H 0.6119 0.5027 0.9144 0.069 Uiso 1 1 calc R U . . .
C7 C 0.54586(14) 0.6014(4) 0.82594(15) 0.0332(11) Uani 1 1 d . . . . .
H7A H 0.5318 0.6222 0.7922 0.050 Uiso 1 1 calc R U . . .
H7B H 0.5212 0.6075 0.8388 0.050 Uiso 1 1 calc R U . . .
H7C H 0.5566 0.5327 0.8283 0.050 Uiso 1 1 calc R U . . .
C8 C 0.55159(15) 0.8359(4) 0.81631(15) 0.0303(10) Uani 1 1 d . . . . .
H8A H 0.5254 0.7956 0.7930 0.045 Uiso 1 1 calc R U . . .
H8B H 0.5651 0.8791 0.7993 0.045 Uiso 1 1 calc R U . . .
H8C H 0.5385 0.8760 0.8348 0.045 Uiso 1 1 calc R U . . .
C9 C 0.64854(17) 0.9091(4) 0.89870(17) 0.0441(13) Uani 1 1 d . . . . .
H9A H 0.6523 0.9404 0.8716 0.066 Uiso 1 1 calc R U . . .
H9B H 0.6793 0.9136 0.9276 0.066 Uiso 1 1 calc R U . . .
H9C H 0.6228 0.9428 0.9045 0.066 Uiso 1 1 calc R U . . .
C10 C 0.61312(14) 0.6065(3) 0.74340(13) 0.0217(9) Uani 1 1 d . . . . .
C11 C 0.65653(14) 0.6244(3) 0.73748(12) 0.0218(9) Uani 1 1 d . . . . .
C12 C 0.66129(15) 0.7279(3) 0.73371(13) 0.0235(9) Uani 1 1 d . . . . .
C13 C 0.62100(14) 0.7738(3) 0.73773(13) 0.0209(9) Uani 1 1 d . . . . .
C14 C 0.59157(14) 0.6985(3) 0.74304(13) 0.0212(8) Uani 1 1 d . . . . .
H14A H 0.5571 0.7077 0.7387 0.025 Uiso 1 1 calc R U . . .
C15 C 0.59187(16) 0.5065(3) 0.74446(15) 0.0300(10) Uani 1 1 d . . . . .
H15A H 0.6129 0.4719 0.7740 0.045 Uiso 1 1 calc R U . . .
H15B H 0.5896 0.4682 0.7165 0.045 Uiso 1 1 calc R U . . .
H15C H 0.5593 0.5144 0.7436 0.045 Uiso 1 1 calc R U . . .
C16 C 0.68848(16) 0.5462(3) 0.73121(15) 0.0312(10) Uani 1 1 d . . . . .
H16A H 0.7207 0.5740 0.7381 0.047 Uiso 1 1 calc R U . . .
H16B H 0.6737 0.5219 0.6980 0.047 Uiso 1 1 calc R U . . .
H16C H 0.6919 0.4916 0.7534 0.047 Uiso 1 1 calc R U . . .
C17 C 0.69786(16) 0.7793(3) 0.72035(15) 0.0321(11) Uani 1 1 d . . . . .
H17A H 0.7255 0.7352 0.7262 0.048 Uiso 1 1 calc R U . . .
H17B H 0.7095 0.8389 0.7399 0.048 Uiso 1 1 calc R U . . .
H17C H 0.6825 0.7973 0.6862 0.048 Uiso 1 1 calc R U . . .
C18 C 0.60855(17) 0.8816(3) 0.72860(16) 0.0357(11) Uani 1 1 d . . . . .
H18A H 0.6367 0.9214 0.7492 0.054 Uiso 1 1 calc R U . . .
H18B H 0.5806 0.8968 0.7359 0.054 Uiso 1 1 calc R U . . .
H18C H 0.6002 0.8968 0.6948 0.054 Uiso 1 1 calc R U . . .
C19 C 0.76370(14) 0.6082(3) 0.86508(14) 0.0248(9) Uani 1 1 d . . . . .
C20 C 0.76524(13) 0.6505(3) 0.90768(14) 0.0234(9) Uani 1 1 d . . . . .
C21 C 0.76629(14) 0.7540(3) 0.90387(14) 0.0232(9) Uani 1 1 d . . . . .
C22 C 0.76500(14) 0.7773(3) 0.85821(14) 0.0230(9) Uani 1 1 d . . . . .
C23 C 0.76418(13) 0.6867(3) 0.83493(14) 0.0236(9) Uani 1 1 d . . . . .
H23A H 0.7716 0.6794 0.8062 0.028 Uiso 1 1 calc R U . . .
C24 C 0.77089(16) 0.5010(3) 0.85802(16) 0.0359(11) Uani 1 1 d . . . . .
H24A H 0.7615 0.4880 0.8238 0.054 Uiso 1 1 calc R U . . .
H24B H 0.7506 0.4613 0.8692 0.054 Uiso 1 1 calc R U . . .
H24C H 0.8053 0.4835 0.8764 0.054 Uiso 1 1 calc R U . . .
C25 C 0.77105(14) 0.5927(4) 0.95174(14) 0.0313(10) Uani 1 1 d . . . . .
H25A H 0.7662 0.6365 0.9748 0.047 Uiso 1 1 calc R U . . .
H25B H 0.8039 0.5644 0.9666 0.047 Uiso 1 1 calc R U . . .
H25C H 0.7469 0.5395 0.9426 0.047 Uiso 1 1 calc R U . . .
C26 C 0.77408(16) 0.8281(4) 0.94340(16) 0.0341(11) Uani 1 1 d . . . . .
H26A H 0.7596 0.8030 0.9645 0.051 Uiso 1 1 calc R U . . .
H26B H 0.7585 0.8907 0.9291 0.051 Uiso 1 1 calc R U . . .
H26C H 0.8091 0.8386 0.9622 0.051 Uiso 1 1 calc R U . . .
C27 C 0.77043(16) 0.8786(3) 0.84198(16) 0.0338(11) Uani 1 1 d . . . . .
H27A H 0.7695 0.8753 0.8096 0.051 Uiso 1 1 calc R U . . .
H27B H 0.8016 0.9067 0.8643 0.051 Uiso 1 1 calc R U . . .
H27C H 0.7437 0.9203 0.8414 0.051 Uiso 1 1 calc R U . . .
K1 K 0.51667(3) 0.74092(7) 0.48697(3) 0.02093(18) Uani 1 1 d . . . . .
O1 O 0.45984(9) 0.6065(2) 0.41357(9) 0.0257(6) Uani 1 1 d . . . . .
O2 O 0.55968(10) 0.5674(2) 0.47372(10) 0.0256(6) Uani 1 1 d . . . . .
O3 O 0.50904(11) 0.8960(2) 0.42384(11) 0.0396(8) Uani 1 1 d . . . . .
O4 O 0.59859(10) 0.8634(2) 0.50580(11) 0.0341(8) Uani 1 1 d . . . . .
O5 O 0.44599(10) 0.8034(2) 0.51710(11) 0.0309(7) Uani 1 1 d . . . . .
O6 O 0.53043(10) 0.7108(2) 0.58351(10) 0.0258(6) Uani 1 1 d . . . . .
N1 N 0.41836(12) 0.8028(3) 0.41289(13) 0.0329(9) Uani 1 1 d . . . . .
N2 N 0.61531(12) 0.6783(2) 0.56104(11) 0.0235(8) Uani 1 1 d . . . . .
C28 C 0.39108(15) 0.7151(3) 0.38758(17) 0.0357(11) Uani 1 1 d . . . . .
H28A H 0.3622 0.7365 0.3587 0.043 Uiso 1 1 calc R U . . .
H28B H 0.3792 0.6798 0.4089 0.043 Uiso 1 1 calc R U . . .
C29 C 0.42024(16) 0.6454(4) 0.37237(15) 0.0331(11) Uani 1 1 d . . . . .
H29A H 0.3991 0.5908 0.3535 0.040 Uiso 1 1 calc R U . . .
H29B H 0.4330 0.6802 0.3516 0.040 Uiso 1 1 calc R U . . .
C30 C 0.48954(15) 0.5436(3) 0.40003(15) 0.0287(10) Uani 1 1 d . . . . .
H30A H 0.5059 0.5823 0.3837 0.034 Uiso 1 1 calc R U . . .
H30B H 0.4691 0.4926 0.3774 0.034 Uiso 1 1 calc R U . . .
C31 C 0.52658(15) 0.4959(3) 0.44369(16) 0.0331(11) Uani 1 1 d . . . . .
H31A H 0.5102 0.4624 0.4616 0.040 Uiso 1 1 calc R U . . .
H31B H 0.5446 0.4457 0.4342 0.040 Uiso 1 1 calc R U . . .
C32 C 0.59717(15) 0.5219(3) 0.51406(15) 0.0288(10) Uani 1 1 d . . . . .
H32A H 0.6126 0.4687 0.5032 0.035 Uiso 1 1 calc R U . . .
H32B H 0.5832 0.4925 0.5351 0.035 Uiso 1 1 calc R U . . .
C33 C 0.63465(14) 0.5984(3) 0.54151(15) 0.0284(10) Uani 1 1 d . . . . .
H33A H 0.6618 0.5658 0.5684 0.034 Uiso 1 1 calc R U . . .
H33B H 0.6481 0.6274 0.5199 0.034 Uiso 1 1 calc R U . . .
C34 C 0.42407(17) 0.8697(4) 0.37819(17) 0.0398(12) Uani 1 1 d . . . . .
H34A H 0.3927 0.9040 0.3602 0.048 Uiso 1 1 calc R U . . .
H34B H 0.4314 0.8303 0.3548 0.048 Uiso 1 1 calc R U . . .
C35 C 0.46347(17) 0.9454(4) 0.40043(18) 0.0439(13) Uani 1 1 d . . . . .
H35A H 0.4644 0.9899 0.3752 0.053 Uiso 1 1 calc R U . . .
H35B H 0.4568 0.9855 0.4240 0.053 Uiso 1 1 calc R U . . .
C36 C 0.54809(19) 0.9662(4) 0.4413(2) 0.0602(17) Uani 1 1 d . . . . .
H36A H 0.5439 1.0103 0.4651 0.072 Uiso 1 1 calc R U . . .
H36B H 0.5475 1.0071 0.4143 0.072 Uiso 1 1 calc R U . . .
C37 C 0.59552(17) 0.9137(4) 0.46415(19) 0.0528(16) Uani 1 1 d . . . . .
H37A H 0.5985 0.8660 0.4411 0.063 Uiso 1 1 calc R U . . .
H37B H 0.6226 0.9616 0.4730 0.063 Uiso 1 1 calc R U . . .
C38 C 0.64599(15) 0.8204(3) 0.53021(16) 0.0324(11) Uani 1 1 d . . . . .
H38A H 0.6711 0.8728 0.5407 0.039 Uiso 1 1 calc R U . . .
H38B H 0.6527 0.7756 0.5082 0.039 Uiso 1 1 calc R U . . .
C39 C 0.64789(16) 0.7640(3) 0.57317(15) 0.0306(10) Uani 1 1 d . . . . .
H39A H 0.6818 0.7414 0.5921 0.037 Uiso 1 1 calc R U . . .
H39B H 0.6392 0.8090 0.5938 0.037 Uiso 1 1 calc R U . . .
C40 C 0.39186(16) 0.8529(4) 0.43767(18) 0.0443(13) Uani 1 1 d . . . . .
H40A H 0.3569 0.8575 0.4153 0.053 Uiso 1 1 calc R U . . .
H40B H 0.4045 0.9209 0.4459 0.053 Uiso 1 1 calc R U . . .
C41 C 0.39631(16) 0.8015(4) 0.48291(18) 0.0461(13) Uani 1 1 d . . . . .
H41A H 0.3757 0.8351 0.4963 0.055 Uiso 1 1 calc R U . . .
H41B H 0.3850 0.7325 0.4756 0.055 Uiso 1 1 calc R U . . .
C42 C 0.45000(17) 0.7708(3) 0.56300(17) 0.0340(11) Uani 1 1 d . . . . .
H42A H 0.4372 0.7027 0.5603 0.041 Uiso 1 1 calc R U . . .
H42B H 0.4303 0.8139 0.5740 0.041 Uiso 1 1 calc R U . . .
C43 C 0.50147(17) 0.7732(3) 0.59837(16) 0.0299(11) Uani 1 1 d . . . . .
H43A H 0.5139 0.8416 0.6018 0.036 Uiso 1 1 calc R U . . .
H43B H 0.5039 0.7513 0.6301 0.036 Uiso 1 1 calc R U . . .
C44 C 0.57927(15) 0.7076(3) 0.62003(14) 0.0291(10) Uani 1 1 d . . . . .
H44A H 0.5794 0.6811 0.6502 0.035 Uiso 1 1 calc R U . . .
H44B H 0.5932 0.7749 0.6265 0.035 Uiso 1 1 calc R U . . .
C45 C 0.60941(15) 0.6433(3) 0.60349(14) 0.0276(10) Uani 1 1 d . . . . .
H45A H 0.6422 0.6361 0.6303 0.033 Uiso 1 1 calc R U . . .
H45B H 0.5944 0.5770 0.5964 0.033 Uiso 1 1 calc R U . . .
O7 O 0.8403(3) 0.7521(7) 0.7403(3) 0.185(3) Uiso 1 1 d . . . . .
C46 C 0.8327(4) 0.6415(8) 0.7326(4) 0.142(4) Uiso 1 1 d . . . . .
H46A H 0.8644 0.6073 0.7432 0.170 Uiso 1 1 calc R U . . .
H46B H 0.8153 0.6152 0.7513 0.170 Uiso 1 1 calc R U . . .
C47 C 0.8055(5) 0.6275(10) 0.6845(5) 0.189(5) Uiso 1 1 d . . . . .
H47A H 0.7722 0.6072 0.6794 0.227 Uiso 1 1 calc R U . . .
H47B H 0.8200 0.5727 0.6735 0.227 Uiso 1 1 calc R U . . .
C48 C 0.8020(5) 0.7095(10) 0.6561(5) 0.168(5) Uiso 1 1 d . . . . .
H48A H 0.8225 0.7012 0.6382 0.201 Uiso 1 1 calc R U . . .
H48B H 0.7678 0.7203 0.6327 0.201 Uiso 1 1 calc R U . . .
C49 C 0.8169(5) 0.7805(10) 0.6849(5) 0.171(5) Uiso 1 1 d . . . . .
H49A H 0.7892 0.8257 0.6787 0.205 Uiso 1 1 calc R U . . .
H49B H 0.8415 0.8173 0.6779 0.205 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 Cnt1 2.566 . ?
U1 Cnt2 2.563 . ?
U1 Cnt3 2.564 . ?
U1 C5 2.753(4) . ?
U1 C23 2.755(4) . ?
U1 C14 2.762(4) . ?
U1 C4 2.788(4) . ?
U1 C22 2.801(4) . ?
U1 C13 2.807(4) . ?
U1 C10 2.808(4) . ?
U1 C19 2.811(4) . ?
U1 C1 2.826(4) . ?
U1 C11 2.885(4) . ?
U1 C3 2.888(4) . ?
U1 C12 2.892(4) . ?
U1 C20 2.893(4) . ?
U1 C21 2.897(4) . ?
U1 C2 2.910(4) . ?
C1 C5 1.410(6) . ?
C1 C2 1.413(6) . ?
C1 C6 1.508(7) . ?
C2 C3 1.423(7) . ?
C2 C7 1.499(6) . ?
C3 C4 1.410(6) . ?
C3 C8 1.506(6) . ?
C4 C5 1.407(6) . ?
C4 C9 1.496(7) . ?
C10 C14 1.405(6) . ?
C10 C11 1.418(5) . ?
C10 C15 1.507(6) . ?
C11 C12 1.422(6) . ?
C11 C16 1.499(6) . ?
C12 C13 1.417(6) . ?
C12 C17 1.500(6) . ?
C13 C14 1.408(6) . ?
C13 C18 1.507(6) . ?
C19 C20 1.408(6) . ?
C19 C23 1.413(6) . ?
C19 C24 1.500(6) . ?
C20 C21 1.411(6) . ?
C20 C25 1.505(6) . ?
C21 C22 1.417(5) . ?
C21 C26 1.513(6) . ?
C22 C23 1.416(6) . ?
C22 C27 1.493(6) . ?
K1 O5 2.788(3) . ?
K1 O2 2.800(3) . ?
K1 O3 2.801(3) . ?
K1 O4 2.832(3) . ?
K1 O6 2.836(3) . ?
K1 O1 2.844(3) . ?
K1 N1 3.003(4) . ?
K1 N2 3.012(3) . ?
O1 C30 1.420(5) . ?
O1 C29 1.426(5) . ?
O2 C31 1.419(5) . ?
O2 C32 1.419(5) . ?
O3 C35 1.424(5) . ?
O3 C36 1.433(6) . ?
O4 C37 1.414(5) . ?
O4 C38 1.432(5) . ?
O5 C41 1.425(5) . ?
O5 C42 1.429(5) . ?
O6 C43 1.422(5) . ?
O6 C44 1.430(5) . ?
N1 C34 1.461(6) . ?
N1 C28 1.469(5) . ?
N1 C40 1.479(6) . ?
N2 C45 1.463(5) . ?
N2 C39 1.467(5) . ?
N2 C33 1.471(5) . ?
C28 C29 1.493(6) . ?
C30 C31 1.484(6) . ?
C32 C33 1.506(6) . ?
C34 C35 1.502(6) . ?
C36 C37 1.486(7) . ?
C38 C39 1.502(6) . ?
C40 C41 1.505(7) . ?
C42 C43 1.476(7) . ?
C44 C45 1.494(6) . ?
O7 C46 1.522(13) . ?
O7 C49 1.588(14) . ?
C46 C47 1.366(14) . ?
C47 C48 1.389(15) . ?
C48 C49 1.255(14) . ?

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
Cnt1 U1 Cnt2 120.0 . . ?
Cnt1 U1 Cnt3 119.8 . . ?
Cnt2 U1 Cnt3 120.1 . . ?
C5 U1 C23 119.94(12) . . ?
C5 U1 C14 120.04(12) . . ?
C23 U1 C14 119.93(11) . . ?
C5 U1 C4 29.42(13) . . ?
C23 U1 C4 131.17(12) . . ?
C14 U1 C4 101.01(12) . . ?
C5 U1 C22 101.38(12) . . ?
C23 U1 C22 29.50(12) . . ?
C14 U1 C22 130.48(12) . . ?
C4 U1 C22 103.32(12) . . ?
C5 U1 C13 132.63(12) . . ?
C23 U1 C13 99.99(12) . . ?
C14 U1 C13 29.27(11) . . ?
C4 U1 C13 104.72(12) . . ?
C22 U1 C13 102.25(12) . . ?
C5 U1 C10 131.21(12) . . ?
C23 U1 C10 103.64(11) . . ?
C14 U1 C10 29.21(11) . . ?
C4 U1 C10 124.26(12) . . ?
C22 U1 C10 127.19(11) . . ?
C13 U1 C10 48.28(12) . . ?
C5 U1 C19 101.76(12) . . ?
C23 U1 C19 29.40(12) . . ?
C14 U1 C19 133.40(12) . . ?
C4 U1 C19 125.38(12) . . ?
C22 U1 C19 48.52(12) . . ?
C13 U1 C19 124.55(12) . . ?
C10 U1 C19 106.81(12) . . ?
C5 U1 C1 29.23(13) . . ?
C23 U1 C1 132.58(12) . . ?
C14 U1 C1 102.58(12) . . ?
C4 U1 C1 48.38(15) . . ?
C22 U1 C1 125.76(12) . . ?
C13 U1 C1 127.09(12) . . ?
C10 U1 C1 104.04(13) . . ?
C19 U1 C1 105.04(12) . . ?
C5 U1 C11 159.03(13) . . ?
C23 U1 C11 75.94(11) . . ?
C14 U1 C11 47.42(11) . . ?
C4 U1 C11 148.31(11) . . ?
C22 U1 C11 98.44(11) . . ?
C13 U1 C11 47.54(12) . . ?
C10 U1 C11 28.80(11) . . ?
C19 U1 C11 86.31(11) . . ?
C1 U1 C11 130.05(13) . . ?
C5 U1 C3 47.33(12) . . ?
C23 U1 C3 159.00(12) . . ?
C14 U1 C3 74.44(11) . . ?
C4 U1 C3 28.70(11) . . ?
C22 U1 C3 129.66(12) . . ?
C13 U1 C3 86.47(11) . . ?
C10 U1 C3 95.59(11) . . ?
C19 U1 C3 148.90(11) . . ?
C1 U1 C3 47.36(12) . . ?
C11 U1 C3 121.42(11) . . ?
C5 U1 C12 160.85(13) . . ?
C23 U1 C12 73.75(12) . . ?
C14 U1 C12 47.40(11) . . ?
C4 U1 C12 131.65(12) . . ?
C22 U1 C12 84.92(11) . . ?
C13 U1 C12 28.75(11) . . ?
C10 U1 C12 47.52(12) . . ?
C19 U1 C12 95.95(12) . . ?
C1 U1 C12 149.32(12) . . ?
C11 U1 C12 28.50(12) . . ?
C3 U1 C12 115.14(11) . . ?
C5 U1 C20 74.96(12) . . ?
C23 U1 C20 47.25(11) . . ?
C14 U1 C20 161.64(12) . . ?
C4 U1 C20 96.85(12) . . ?
C22 U1 C20 47.39(12) . . ?
C13 U1 C20 146.75(12) . . ?
C10 U1 C20 133.19(12) . . ?
C19 U1 C20 28.53(11) . . ?
C1 U1 C20 86.13(12) . . ?
C11 U1 C20 114.84(11) . . ?
C3 U1 C20 122.04(11) . . ?
C12 U1 C20 120.80(11) . . ?
C5 U1 C21 74.57(12) . . ?
C23 U1 C21 47.40(11) . . ?
C14 U1 C21 158.13(12) . . ?
C4 U1 C21 84.85(11) . . ?
C22 U1 C21 28.74(11) . . ?
C13 U1 C21 128.87(12) . . ?
C10 U1 C21 150.84(11) . . ?
C19 U1 C21 47.33(12) . . ?
C1 U1 C21 97.06(12) . . ?
C11 U1 C21 123.22(11) . . ?
C3 U1 C21 113.54(11) . . ?
C12 U1 C21 113.62(11) . . ?
C20 U1 C21 28.21(12) . . ?
C5 U1 C2 47.16(12) . . ?
C23 U1 C2 160.58(12) . . ?
C14 U1 C2 75.55(11) . . ?
C4 U1 C2 47.43(13) . . ?
C22 U1 C2 148.03(12) . . ?
C13 U1 C2 98.61(12) . . ?
C10 U1 C2 84.72(11) . . ?
C19 U1 C2 131.53(12) . . ?
C1 U1 C2 28.48(11) . . ?
C11 U1 C2 113.50(11) . . ?
C3 U1 C2 28.41(13) . . ?
C12 U1 C2 122.93(11) . . ?
C20 U1 C2 114.59(11) . . ?
C21 U1 C2 121.61(11) . . ?
C5 C1 C2 107.0(4) . . ?
C5 C1 C6 126.9(4) . . ?
C2 C1 C6 125.9(4) . . ?
C5 C1 U1 72.5(2) . . ?
C2 C1 U1 79.0(2) . . ?
C6 C1 U1 118.7(3) . . ?
C1 C2 C3 108.1(4) . . ?
C1 C2 C7 125.4(4) . . ?
C3 C2 C7 126.1(4) . . ?
C1 C2 U1 72.5(2) . . ?
C3 C2 U1 74.9(2) . . ?
C7 C2 U1 124.4(3) . . ?
C4 C3 C2 108.2(4) . . ?
C4 C3 C8 124.7(4) . . ?
C2 C3 C8 126.7(4) . . ?
C4 C3 U1 71.7(2) . . ?
C2 C3 U1 76.6(2) . . ?
C8 C3 U1 123.7(3) . . ?
C5 C4 C3 107.2(4) . . ?
C5 C4 C9 127.4(4) . . ?
C3 C4 C9 124.7(4) . . ?
C5 C4 U1 73.9(2) . . ?
C3 C4 U1 79.6(2) . . ?
C9 C4 U1 119.8(3) . . ?
C4 C5 C1 109.5(4) . . ?
C4 C5 U1 76.7(2) . . ?
C1 C5 U1 78.3(2) . . ?
C14 C10 C11 107.3(4) . . ?
C14 C10 C15 126.8(4) . . ?
C11 C10 C15 125.6(4) . . ?
C14 C10 U1 73.6(2) . . ?
C11 C10 U1 78.6(2) . . ?
C15 C10 U1 118.7(2) . . ?
C10 C11 C12 108.0(4) . . ?
C10 C11 C16 125.1(4) . . ?
C12 C11 C16 126.6(4) . . ?
C10 C11 U1 72.6(2) . . ?
C12 C11 U1 76.0(2) . . ?
C16 C11 U1 122.1(2) . . ?
C13 C12 C11 107.9(4) . . ?
C13 C12 C17 125.2(4) . . ?
C11 C12 C17 126.3(4) . . ?
C13 C12 U1 72.3(2) . . ?
C11 C12 U1 75.5(2) . . ?
C17 C12 U1 124.9(3) . . ?
C14 C13 C12 107.3(3) . . ?
C14 C13 C18 127.3(4) . . ?
C12 C13 C18 124.5(4) . . ?
C14 C13 U1 73.6(2) . . ?
C12 C13 U1 78.9(2) . . ?
C18 C13 U1 122.0(3) . . ?
C10 C14 C13 109.4(4) . . ?
C10 C14 U1 77.2(2) . . ?
C13 C14 U1 77.2(2) . . ?
C20 C19 C23 107.0(4) . . ?
C20 C19 C24 125.3(4) . . ?
C23 C19 C24 126.6(4) . . ?
C20 C19 U1 79.0(2) . . ?
C23 C19 U1 73.1(2) . . ?
C24 C19 U1 123.3(3) . . ?
C19 C20 C21 108.8(4) . . ?
C19 C20 C25 124.3(4) . . ?
C21 C20 C25 126.5(4) . . ?
C19 C20 U1 72.5(2) . . ?
C21 C20 U1 76.0(2) . . ?
C25 C20 U1 123.4(2) . . ?
C20 C21 C22 108.1(4) . . ?
C20 C21 C26 126.6(4) . . ?
C22 C21 C26 124.8(4) . . ?
C20 C21 U1 75.8(2) . . ?
C22 C21 U1 71.9(2) . . ?
C26 C21 U1 124.1(3) . . ?
C23 C22 C21 106.9(4) . . ?
C23 C22 C27 127.8(4) . . ?
C21 C22 C27 124.9(4) . . ?
C23 C22 U1 73.4(2) . . ?
C21 C22 U1 79.4(2) . . ?
C27 C22 U1 119.4(3) . . ?
C19 C23 C22 109.2(3) . . ?
C19 C23 U1 77.5(2) . . ?
C22 C23 U1 77.0(2) . . ?
O5 K1 O2 140.31(9) . . ?
O5 K1 O3 98.44(10) . . ?
O2 K1 O3 116.17(10) . . ?
O5 K1 O4 118.61(10) . . ?
O2 K1 O4 95.98(9) . . ?
O3 K1 O4 60.76(8) . . ?
O5 K1 O6 59.82(9) . . ?
O2 K1 O6 98.96(8) . . ?
O3 K1 O6 139.54(10) . . ?
O4 K1 O6 97.96(9) . . ?
O5 K1 O1 99.45(9) . . ?
O2 K1 O1 60.60(8) . . ?
O3 K1 O1 95.10(9) . . ?
O4 K1 O1 136.35(9) . . ?
O6 K1 O1 120.48(9) . . ?
O5 K1 N1 60.87(10) . . ?
O2 K1 N1 119.84(10) . . ?
O3 K1 N1 59.97(10) . . ?
O4 K1 N1 119.51(10) . . ?
O6 K1 N1 119.59(10) . . ?
O1 K1 N1 60.29(9) . . ?
O5 K1 N2 119.31(9) . . ?
O2 K1 N2 59.94(9) . . ?
O3 K1 N2 120.05(9) . . ?
O4 K1 N2 60.56(9) . . ?
O6 K1 N2 60.55(9) . . ?
O1 K1 N2 119.50(9) . . ?
N1 K1 N2 179.78(11) . . ?
C30 O1 C29 111.2(3) . . ?
C30 O1 K1 111.7(2) . . ?
C29 O1 K1 117.8(2) . . ?
C31 O2 C32 110.8(3) . . ?
C31 O2 K1 115.1(2) . . ?
C32 O2 K1 119.2(2) . . ?
C35 O3 C36 110.2(4) . . ?
C35 O3 K1 118.9(3) . . ?
C36 O3 K1 115.2(3) . . ?
C37 O4 C38 109.9(3) . . ?
C37 O4 K1 112.2(2) . . ?
C38 O4 K1 117.7(2) . . ?
C41 O5 C42 110.2(3) . . ?
C41 O5 K1 117.9(3) . . ?
C42 O5 K1 118.0(2) . . ?
C43 O6 C44 109.8(3) . . ?
C43 O6 K1 114.0(2) . . ?
C44 O6 K1 118.1(2) . . ?
C34 N1 C28 109.3(4) . . ?
C34 N1 C40 110.0(4) . . ?
C28 N1 C40 109.8(4) . . ?
C34 N1 K1 110.0(2) . . ?
C28 N1 K1 109.3(2) . . ?
C40 N1 K1 108.5(3) . . ?
C45 N2 C39 110.5(3) . . ?
C45 N2 C33 109.8(3) . . ?
C39 N2 C33 110.4(3) . . ?
C45 N2 K1 108.0(2) . . ?
C39 N2 K1 108.3(2) . . ?
C33 N2 K1 109.7(2) . . ?
N1 C28 C29 113.8(4) . . ?
O1 C29 C28 110.1(3) . . ?
O1 C30 C31 109.2(3) . . ?
O2 C31 C30 110.3(4) . . ?
O2 C32 C33 109.0(3) . . ?
N2 C33 C32 113.6(3) . . ?
N1 C34 C35 114.1(4) . . ?
O3 C35 C34 108.8(4) . . ?
O3 C36 C37 109.7(4) . . ?
O4 C37 C36 110.0(4) . . ?
O4 C38 C39 109.1(4) . . ?
N2 C39 C38 114.0(3) . . ?
N1 C40 C41 113.6(4) . . ?
O5 C41 C40 109.2(4) . . ?
O5 C42 C43 110.1(3) . . ?
O6 C43 C42 110.6(4) . . ?
O6 C44 C45 109.2(3) . . ?
N2 C45 C44 115.5(4) . . ?
C46 O7 C49 96.0(8) . . ?
C47 C46 O7 106.7(10) . . ?
C46 C47 C48 114.7(13) . . ?
C49 C48 C47 105.3(14) . . ?
C48 C49 O7 115.6(12) . . ?

_refine_diff_density_max         1.941
_refine_diff_density_min         -0.935
_refine_diff_density_rms         0.109



_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
