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

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

data_K(TDA)
_database_code_depnum_ccdc_archive 'CCDC 1559383'
_audit_update_record             
;
2018-01-05 deposited with the CCDC.
2018-01-10 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            'C29 H50 K N O7'
_chemical_formula_weight         563.80

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0040 0.0020 '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 0.0076 0.0040 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0132 0.0074 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2261 0.2966 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

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

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

_cell_length_a                   9.692(5)
_cell_length_b                   21.888(13)
_cell_length_c                   14.814(9)
_cell_angle_alpha                90
_cell_angle_beta                 101.007(4)
_cell_angle_gamma                90
_cell_volume                     3085(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    6509
_cell_measurement_theta_min      2.53
_cell_measurement_theta_max      30.41

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.214
_exptl_crystal_F_000             1224
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.12
_exptl_absorpt_coefficient_mu    0.268
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.623
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_process_details   'SADABS-2014/5 - Bruker AXS, Madison WI'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.7749
_diffrn_radiation_type           synchrotron
_diffrn_source                   'Advanced light source, station 11.3.1'
_diffrn_measurement_device_type  
'Synchrotron (ALS station 11.3.1) equipped with Bruker D8 goniometer and Photon 100 detector'
_diffrn_measurement_method       'omega phi scans, shutterless'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            32500
_diffrn_reflns_av_unetI/netI     0.0195
_diffrn_reflns_av_R_equivalents  0.0254
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.534
_diffrn_reflns_theta_max         30.411
_diffrn_reflns_theta_full        27.706
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             7183
_reflns_number_gt                6509
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX3 Bruker, Madison WI'
_computing_cell_refinement       'SAINT V8.37A Bruker, Madison WI'
_computing_data_reduction        'SAINT V8.37A Bruker, Madison WI'
_computing_structure_solution    'SHELXT 2014/4 Bruker, Madison WI'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  WinGX
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0388P)²+1.0597P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.0073(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         7183
_refine_ls_number_parameters     344
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0336
_refine_ls_R_factor_gt           0.0300
_refine_ls_wR_factor_ref         0.0814
_refine_ls_wR_factor_gt          0.0785
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_restrained_S_all      1.049
_refine_ls_shift/su_max          0.002
_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
K1 K 0.46063(2) 0.58655(2) 0.16559(2) 0.01865(7) Uani 1 1 d . . . . .
O1 O 0.39028(7) 0.61439(3) 0.31789(5) 0.01603(14) Uani 1 1 d . . . . .
O103 O 0.69548(8) 0.54111(4) 0.08614(5) 0.02027(16) Uani 1 1 d . . . . .
O105 O 0.27901(8) 0.47956(3) 0.20544(5) 0.01975(15) Uani 1 1 d . . . . .
O104 O 0.54953(8) 0.46828(3) 0.18415(5) 0.01951(15) Uani 1 1 d . . . . .
O106 O 0.11528(8) 0.57314(3) 0.09525(5) 0.02180(16) Uani 1 1 d . . . . .
O100 O 0.29545(8) 0.67088(3) 0.06618(5) 0.02086(16) Uani 1 1 d . . . . .
O102 O 0.54377(8) 0.64510(3) 0.00908(5) 0.02128(16) Uani 1 1 d . . . . .
N1 N 0.51856(8) 0.68654(4) 0.41191(5) 0.01339(16) Uani 1 1 d . . . . .
C1 C 0.42032(9) 0.64574(4) 0.39146(6) 0.01238(17) Uani 1 1 d . . . . .
C6 C 0.60590(10) 0.69964(4) 0.34950(6) 0.01324(18) Uani 1 1 d . . . . .
C7 C 0.71988(10) 0.66146(4) 0.34180(6) 0.01458(18) Uani 1 1 d . . . . .
C11 C 0.58750(10) 0.75570(4) 0.30199(6) 0.01531(18) Uani 1 1 d . . . . .
C2 C 0.32910(11) 0.63563(5) 0.46370(7) 0.01724(19) Uani 1 1 d . . . . .
C12 C 0.73724(10) 0.60099(4) 0.39251(7) 0.01629(19) Uani 1 1 d . . . . .
H12 H 0.6433 0.5832 0.3875 0.020 Uiso 1 1 calc R U . . .
C15 C 0.46063(10) 0.79415(4) 0.30975(7) 0.01707(19) Uani 1 1 d . . . . .
H15 H 0.4437 0.7889 0.3724 0.020 Uiso 1 1 calc R U . . .
C8 C 0.81630(10) 0.68155(5) 0.28977(7) 0.0185(2) Uani 1 1 d . . . . .
H8 H 0.8927 0.6569 0.2849 0.022 Uiso 1 1 calc R U . . .
C108 C 0.16558(11) 0.51056(5) 0.23384(7) 0.0204(2) Uani 1 1 d . . . . .
H10A H 0.1997 0.5467 0.2691 0.024 Uiso 1 1 calc R U . . .
H10B H 0.1209 0.4840 0.2722 0.024 Uiso 1 1 calc R U . . .
C9 C 0.80099(11) 0.73731(5) 0.24520(7) 0.0216(2) Uani 1 1 d . . . . .
H9 H 0.8675 0.7503 0.2117 0.026 Uiso 1 1 calc R U . . .
C10 C 0.68625(11) 0.77367(5) 0.25073(7) 0.0195(2) Uani 1 1 d . . . . .
H10 H 0.6751 0.8108 0.2196 0.023 Uiso 1 1 calc R U . . .
C103 C 0.72552(11) 0.57354(6) 0.00905(7) 0.0252(2) Uani 1 1 d . . . . .
H10C H 0.6698 0.5572 -0.0472 0.030 Uiso 1 1 calc R U . . .
H10D H 0.8241 0.5690 0.0060 0.030 Uiso 1 1 calc R U . . .
C105 C 0.67072(11) 0.44491(5) 0.15548(7) 0.0218(2) Uani 1 1 d . . . . .
H10E H 0.6603 0.4014 0.1440 0.026 Uiso 1 1 calc R U . . .
H10F H 0.7530 0.4514 0.2032 0.026 Uiso 1 1 calc R U . . .
C107 C 0.38280(12) 0.46028(5) 0.28069(7) 0.0224(2) Uani 1 1 d . . . . .
H10G H 0.3417 0.4332 0.3201 0.027 Uiso 1 1 calc R U . . .
H10H H 0.4223 0.4953 0.3167 0.027 Uiso 1 1 calc R U . . .
C109 C 0.06268(11) 0.52827(5) 0.14916(8) 0.0228(2) Uani 1 1 d . . . . .
H10I H 0.0370 0.4921 0.1118 0.027 Uiso 1 1 calc R U . . .
H10J H -0.0218 0.5438 0.1671 0.027 Uiso 1 1 calc R U . . .
C104 C 0.68772(11) 0.47728(5) 0.06962(7) 0.0223(2) Uani 1 1 d . . . . .
H10K H 0.7727 0.4634 0.0505 0.027 Uiso 1 1 calc R U . . .
H10L H 0.6085 0.4682 0.0207 0.027 Uiso 1 1 calc R U . . .
C100 C 0.34513(13) 0.70892(5) 0.00179(7) 0.0256(2) Uani 1 1 d . . . . .
H10M H 0.3142 0.7506 0.0078 0.031 Uiso 1 1 calc R U . . .
H10N H 0.3077 0.6951 -0.0603 0.031 Uiso 1 1 calc R U . . .
C13 C 0.82636(12) 0.55508(5) 0.35147(8) 0.0234(2) Uani 1 1 d . . . . .
H13A H 0.8336 0.5179 0.3863 0.035 Uiso 1 1 calc R U . . .
H13B H 0.7831 0.5468 0.2888 0.035 Uiso 1 1 calc R U . . .
H13C H 0.9186 0.5717 0.3534 0.035 Uiso 1 1 calc R U . . .
C14 C 0.79662(12) 0.61013(5) 0.49494(7) 0.0218(2) Uani 1 1 d . . . . .
H14A H 0.8065 0.5712 0.5253 0.033 Uiso 1 1 calc R U . . .
H14B H 0.8869 0.6296 0.5023 0.033 Uiso 1 1 calc R U . . .
H14C H 0.7338 0.6354 0.5215 0.033 Uiso 1 1 calc R U . . .
C102 C 0.69162(12) 0.63931(6) 0.01866(8) 0.0264(2) Uani 1 1 d . . . . .
H10O H 0.7378 0.6543 0.0784 0.032 Uiso 1 1 calc R U . . .
H10P H 0.7243 0.6631 -0.0283 0.032 Uiso 1 1 calc R U . . .
C106 C 0.49508(12) 0.42765(5) 0.24293(7) 0.0239(2) Uani 1 1 d . . . . .
H10Q H 0.5694 0.4146 0.2927 0.029 Uiso 1 1 calc R U . . .
H10R H 0.4562 0.3917 0.2089 0.029 Uiso 1 1 calc R U . . .
C16 C 0.32976(11) 0.77129(5) 0.24445(8) 0.0250(2) Uani 1 1 d . . . . .
H16A H 0.2508 0.7964 0.2506 0.038 Uiso 1 1 calc R U . . .
H16B H 0.3447 0.7734 0.1823 0.038 Uiso 1 1 calc R U . . .
H16C H 0.3114 0.7298 0.2593 0.038 Uiso 1 1 calc R U . . .
C5 C 0.37310(12) 0.67571(5) 0.54811(7) 0.0223(2) Uani 1 1 d . . . . .
H5A H 0.3672 0.7179 0.5300 0.033 Uiso 1 1 calc R U . . .
H5B H 0.3119 0.6684 0.5908 0.033 Uiso 1 1 calc R U . . .
H5C H 0.4681 0.6662 0.5768 0.033 Uiso 1 1 calc R U . . .
C101 C 0.50148(13) 0.70634(5) 0.01973(8) 0.0274(2) Uani 1 1 d . . . . .
H10S H 0.5374 0.7327 -0.0231 0.033 Uiso 1 1 calc R U . . .
H10T H 0.5389 0.7204 0.0817 0.033 Uiso 1 1 calc R U . . .
C17 C 0.47940(13) 0.86217(5) 0.29535(9) 0.0274(2) Uani 1 1 d . . . . .
H17A H 0.3949 0.8834 0.3013 0.041 Uiso 1 1 calc R U . . .
H17B H 0.5563 0.8771 0.3406 0.041 Uiso 1 1 calc R U . . .
H17C H 0.4989 0.8690 0.2350 0.041 Uiso 1 1 calc R U . . .
C110 C 0.10377(11) 0.63372(5) 0.12789(8) 0.0239(2) Uani 1 1 d . . . . .
H11A H 0.1631 0.6385 0.1881 0.029 Uiso 1 1 calc R U . . .
H11B H 0.0074 0.6421 0.1333 0.029 Uiso 1 1 calc R U . . .
C111 C 0.14877(12) 0.67699(5) 0.06125(8) 0.0259(2) Uani 1 1 d . . . . .
H11C H 0.0992 0.6679 -0.0006 0.031 Uiso 1 1 calc R U . . .
H11D H 0.1266 0.7186 0.0761 0.031 Uiso 1 1 calc R U . . .
C4 C 0.33846(16) 0.56886(5) 0.49222(8) 0.0336(3) Uani 1 1 d . . . . .
H4A H 0.3107 0.5436 0.4389 0.050 Uiso 1 1 calc R U . . .
H4B H 0.4334 0.5593 0.5209 0.050 Uiso 1 1 calc R U . . .
H4C H 0.2772 0.5615 0.5349 0.050 Uiso 1 1 calc R U . . .
C3 C 0.17819(12) 0.65178(7) 0.41864(9) 0.0341(3) Uani 1 1 d . . . . .
H3A H 0.1735 0.6940 0.4009 0.051 Uiso 1 1 calc R U . . .
H3B H 0.1492 0.6267 0.3652 0.051 Uiso 1 1 calc R U . . .
H3C H 0.1171 0.6447 0.4615 0.051 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
K1 O1 2.5523(14) . ?
K1 O100 2.6905(12) . ?
K1 O104 2.7257(16) . ?
K1 O102 2.8949(14) . ?
K1 O103 2.9290(14) . ?
K1 O105 3.0543(14) . ?
K1 O106 3.3232(19) . ?
K1 C107 3.4068(18) . ?
K1 C101 3.4679(18) . ?
O1 C1 1.2737(13) . ?
O103 C104 1.4179(15) . ?
O103 C103 1.4213(14) . ?
O105 C107 1.4157(14) . ?
O105 C108 1.4221(13) . ?
O104 C106 1.4153(14) . ?
O104 C105 1.4185(13) . ?
O106 C109 1.4205(14) . ?
O106 C110 1.4231(14) . ?
O100 C111 1.4158(15) . ?
O100 C100 1.4179(14) . ?
O102 C102 1.4184(15) . ?
O102 C101 1.4193(15) . ?
N1 C1 1.2984(13) . ?
N1 C6 1.3973(13) . ?
C1 C2 1.5288(14) . ?
C6 C7 1.4072(15) . ?
C6 C11 1.4087(15) . ?
C7 C8 1.3913(14) . ?
C7 C12 1.5153(15) . ?
C11 C10 1.3874(15) . ?
C11 C15 1.5125(15) . ?
C2 C4 1.5191(17) . ?
C2 C5 1.5204(15) . ?
C2 C3 1.5287(17) . ?
C12 C13 1.5251(15) . ?
C12 C14 1.5298(16) . ?
C12 H12 0.9800 . ?
C15 C17 1.5198(16) . ?
C15 C16 1.5253(15) . ?
C15 H15 0.9800 . ?
C8 C9 1.3822(16) . ?
C8 H8 0.9300 . ?
C108 C109 1.4969(17) . ?
C108 H10A 0.9700 . ?
C108 H10B 0.9700 . ?
C9 C10 1.3826(16) . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?
C103 C102 1.4895(19) . ?
C103 H10C 0.9700 . ?
C103 H10D 0.9700 . ?
C105 C104 1.4923(17) . ?
C105 H10E 0.9700 . ?
C105 H10F 0.9700 . ?
C107 C106 1.4967(16) . ?
C107 H10G 0.9700 . ?
C107 H10H 0.9700 . ?
C109 H10I 0.9700 . ?
C109 H10J 0.9700 . ?
C104 H10K 0.9700 . ?
C104 H10L 0.9700 . ?
C100 C101 1.4887(19) . ?
C100 H10M 0.9700 . ?
C100 H10N 0.9700 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C102 H10O 0.9700 . ?
C102 H10P 0.9700 . ?
C106 H10Q 0.9700 . ?
C106 H10R 0.9700 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C101 H10S 0.9700 . ?
C101 H10T 0.9700 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C110 C111 1.4921(18) . ?
C110 H11A 0.9700 . ?
C110 H11B 0.9700 . ?
C111 H11C 0.9700 . ?
C111 H11D 0.9700 . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 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 K1 O100 95.08(4) . . ?
O1 K1 O104 105.68(3) . . ?
O100 K1 O104 148.26(3) . . ?
O1 K1 O102 139.87(4) . . ?
O100 K1 O102 59.03(4) . . ?
O104 K1 O102 111.73(3) . . ?
O1 K1 O103 142.71(2) . . ?
O100 K1 O103 116.10(4) . . ?
O104 K1 O103 57.52(2) . . ?
O102 K1 O103 58.13(3) . . ?
O1 K1 O105 75.59(3) . . ?
O100 K1 O105 109.10(5) . . ?
O104 K1 O105 55.60(4) . . ?
O102 K1 O105 138.85(2) . . ?
O103 K1 O105 109.76(4) . . ?
O1 K1 O106 82.83(3) . . ?
O100 K1 O106 55.29(3) . . ?
O104 K1 O106 103.16(3) . . ?
O102 K1 O106 101.87(3) . . ?
O103 K1 O106 131.11(4) . . ?
O105 K1 O106 53.82(3) . . ?
O1 K1 C107 68.23(4) . . ?
O100 K1 C107 131.69(4) . . ?
O104 K1 C107 43.53(3) . . ?
O102 K1 C107 151.89(2) . . ?
O103 K1 C107 100.89(4) . . ?
O105 K1 C107 24.54(3) . . ?
O106 K1 C107 77.25(3) . . ?
O1 K1 C101 116.86(4) . . ?
O100 K1 C101 42.87(4) . . ?
O104 K1 C101 135.19(3) . . ?
O102 K1 C101 23.65(3) . . ?
O103 K1 C101 79.42(4) . . ?
O105 K1 C101 147.00(3) . . ?
O106 K1 C101 95.70(3) . . ?
C107 K1 C101 171.01(3) . . ?
C1 O1 K1 146.00(6) . . ?
C104 O103 C103 111.45(8) . . ?
C104 O103 K1 112.60(6) . . ?
C103 O103 K1 116.58(7) . . ?
C107 O105 C108 112.49(9) . . ?
C107 O105 K1 91.81(6) . . ?
C108 O105 K1 101.41(7) . . ?
C106 O104 C105 112.64(8) . . ?
C106 O104 K1 120.73(6) . . ?
C105 O104 K1 125.18(6) . . ?
C109 O106 C110 113.16(9) . . ?
C109 O106 K1 109.44(6) . . ?
C110 O106 K1 87.17(5) . . ?
C111 O100 C100 112.11(8) . . ?
C111 O100 K1 125.43(7) . . ?
C100 O100 K1 121.88(7) . . ?
C102 O102 C101 112.38(9) . . ?
C102 O102 K1 108.10(6) . . ?
C101 O102 K1 101.45(6) . . ?
C1 N1 C6 119.78(8) . . ?
O1 C1 N1 127.43(9) . . ?
O1 C1 C2 116.92(9) . . ?
N1 C1 C2 115.63(8) . . ?
N1 C6 C7 121.06(9) . . ?
N1 C6 C11 118.32(9) . . ?
C7 C6 C11 120.22(9) . . ?
C8 C7 C6 118.55(9) . . ?
C8 C7 C12 121.87(9) . . ?
C6 C7 C12 119.55(9) . . ?
C10 C11 C6 119.05(9) . . ?
C10 C11 C15 122.66(9) . . ?
C6 C11 C15 118.29(9) . . ?
C4 C2 C5 109.51(10) . . ?
C4 C2 C3 110.20(10) . . ?
C5 C2 C3 108.69(9) . . ?
C4 C2 C1 108.80(8) . . ?
C5 C2 C1 112.54(9) . . ?
C3 C2 C1 107.09(9) . . ?
C7 C12 C13 113.30(9) . . ?
C7 C12 C14 111.27(8) . . ?
C13 C12 C14 110.31(9) . . ?
C7 C12 H12 107.2 . . ?
C13 C12 H12 107.2 . . ?
C14 C12 H12 107.2 . . ?
C11 C15 C17 114.43(9) . . ?
C11 C15 C16 111.03(9) . . ?
C17 C15 C16 109.86(9) . . ?
C11 C15 H15 107.0 . . ?
C17 C15 H15 107.0 . . ?
C16 C15 H15 107.0 . . ?
C9 C8 C7 121.44(10) . . ?
C9 C8 H8 119.3 . . ?
C7 C8 H8 119.3 . . ?
O105 C108 C109 107.74(9) . . ?
O105 C108 H10A 110.2 . . ?
C109 C108 H10A 110.2 . . ?
O105 C108 H10B 110.2 . . ?
C109 C108 H10B 110.2 . . ?
H10A C108 H10B 108.5 . . ?
C8 C9 C10 119.61(10) . . ?
C8 C9 H9 120.2 . . ?
C10 C9 H9 120.2 . . ?
C9 C10 C11 121.07(10) . . ?
C9 C10 H10 119.5 . . ?
C11 C10 H10 119.5 . . ?
O103 C103 C102 108.85(9) . . ?
O103 C103 H10C 109.9 . . ?
C102 C103 H10C 109.9 . . ?
O103 C103 H10D 109.9 . . ?
C102 C103 H10D 109.9 . . ?
H10C C103 H10D 108.3 . . ?
O104 C105 C104 108.46(9) . . ?
O104 C105 H10E 110.0 . . ?
C104 C105 H10E 110.0 . . ?
O104 C105 H10F 110.0 . . ?
C104 C105 H10F 110.0 . . ?
H10E C105 H10F 108.4 . . ?
O105 C107 C106 107.81(9) . . ?
O105 C107 K1 63.65(6) . . ?
C106 C107 K1 87.35(7) . . ?
O105 C107 H10G 110.1 . . ?
C106 C107 H10G 110.1 . . ?
K1 C107 H10G 162.4 . . ?
O105 C107 H10H 110.1 . . ?
C106 C107 H10H 110.1 . . ?
K1 C107 H10H 62.2 . . ?
H10G C107 H10H 108.5 . . ?
O106 C109 C108 113.39(9) . . ?
O106 C109 H10I 108.9 . . ?
C108 C109 H10I 108.9 . . ?
O106 C109 H10J 108.9 . . ?
C108 C109 H10J 108.9 . . ?
H10I C109 H10J 107.7 . . ?
O103 C104 C105 109.36(9) . . ?
O103 C104 H10K 109.8 . . ?
C105 C104 H10K 109.8 . . ?
O103 C104 H10L 109.8 . . ?
C105 C104 H10L 109.8 . . ?
H10K C104 H10L 108.3 . . ?
O100 C100 C101 108.80(9) . . ?
O100 C100 H10M 109.9 . . ?
C101 C100 H10M 109.9 . . ?
O100 C100 H10N 109.9 . . ?
C101 C100 H10N 109.9 . . ?
H10M C100 H10N 108.3 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
O102 C102 C103 108.29(9) . . ?
O102 C102 H10O 110.0 . . ?
C103 C102 H10O 110.0 . . ?
O102 C102 H10P 110.0 . . ?
C103 C102 H10P 110.0 . . ?
H10O C102 H10P 108.4 . . ?
O104 C106 C107 108.25(9) . . ?
O104 C106 H10Q 110.0 . . ?
C107 C106 H10Q 110.0 . . ?
O104 C106 H10R 110.0 . . ?
C107 C106 H10R 110.0 . . ?
H10Q C106 H10R 108.4 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C2 C5 H5A 109.5 . . ?
C2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
O102 C101 C100 108.77(9) . . ?
O102 C101 K1 54.90(6) . . ?
C100 C101 K1 84.64(6) . . ?
O102 C101 H10S 109.9 . . ?
C100 C101 H10S 109.9 . . ?
K1 C101 H10S 162.7 . . ?
O102 C101 H10T 109.9 . . ?
C100 C101 H10T 109.9 . . ?
K1 C101 H10T 73.6 . . ?
H10S C101 H10T 108.3 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
O106 C110 C111 108.35(10) . . ?
O106 C110 H11A 110.0 . . ?
C111 C110 H11A 110.0 . . ?
O106 C110 H11B 110.0 . . ?
C111 C110 H11B 110.0 . . ?
H11A C110 H11B 108.4 . . ?
O100 C111 C110 108.86(9) . . ?
O100 C111 H11C 109.9 . . ?
C110 C111 H11C 109.9 . . ?
O100 C111 H11D 109.9 . . ?
C110 C111 H11D 109.9 . . ?
H11C C111 H11D 108.3 . . ?
C2 C4 H4A 109.5 . . ?
C2 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C2 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?

_refine_diff_density_max         0.342
_refine_diff_density_min         -0.288
_refine_diff_density_rms         0.044

####################################################################### 
# 
# 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_K(18C6)U(TDA)4
_database_code_depnum_ccdc_archive 'CCDC 1559386'
_audit_update_record             
;
2018-01-05 deposited with the CCDC.
2018-01-10 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT973_K(18C6)U(TDA)4      
;
PROBLEM: Check Calcd Positive Resid. Density on        U1       3.42 eA-3
RESPONSE: This alert is caused by unresovled electron density very close to the uranium center, probably caused by moderate crystal quality.
;
_vrf_PLAT094_K(18C6)U(TDA)4      
;
PROBLEM: Ratio of Maximum / Minimum Residual Density ....       5.22 Report
RESPONSE: This alert is caused by unresovled electron density very close to the uranium center, probably caused by moderate crystal quality.
;
# Added during the CSD deposition process: Friday 05 January 2018 06:46 PM
# end Validation Reply Form


_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            'C92 H158 K N4 O13 U'
_chemical_formula_weight         1805.34

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   13.479(4)
_cell_length_b                   18.049(6)
_cell_length_c                   20.964(7)
_cell_angle_alpha                87.530(7)
_cell_angle_beta                 79.614(10)
_cell_angle_gamma                74.365(6)
_cell_volume                     4831(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    16754
_cell_measurement_theta_min      0.99
_cell_measurement_theta_max      26.37

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.241
_exptl_crystal_F_000             1906
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_exptl_absorpt_coefficient_mu    1.781
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.653
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker Quazar'
_diffrn_measurement_method       'omega phi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            100876
_diffrn_reflns_av_unetI/netI     0.0593
_diffrn_reflns_av_R_equivalents  0.0586
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         0.987
_diffrn_reflns_theta_max         26.373
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             19634
_reflns_number_gt                16754
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker ApexIII suite, 2016'
_computing_cell_refinement       'Bruker ApexIII suite, 2016'
_computing_data_reduction        'Bruker ApexIII suite, 2016'
_computing_structure_solution    ShelXT
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Mercury 3.0'
_computing_publication_material  WinGX
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0403P)²+0.5704P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         19634
_refine_ls_number_parameters     1000
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0511
_refine_ls_R_factor_gt           0.0394
_refine_ls_wR_factor_ref         0.0840
_refine_ls_wR_factor_gt          0.0805
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_restrained_S_all      1.079
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.50313(2) 0.73231(2) 0.74952(2) 0.01444(5) Uani 1 1 d . . . . .
K1 K 0.87671(5) 0.22532(4) 0.69490(3) 0.01929(16) Uani 1 1 d . . . . .
O1 O 0.61019(15) 0.61417(12) 0.73109(10) 0.0180(5) Uani 1 1 d . . . . .
O2 O 0.58900(15) 0.82432(11) 0.74302(10) 0.0165(5) Uani 1 1 d . . . . .
O3 O 0.37577(15) 0.76730(12) 0.69034(10) 0.0172(5) Uani 1 1 d . . . . .
O603 O 0.68313(16) 0.18814(12) 0.72361(11) 0.0214(5) Uani 1 1 d . . . . .
O604 O 0.79100(16) 0.18852(12) 0.59570(11) 0.0220(5) Uani 1 1 d . . . . .
O601 O 0.94942(17) 0.27931(13) 0.79470(11) 0.0242(5) Uani 1 1 d . . . . .
O605 O 0.96766(16) 0.24931(12) 0.56854(10) 0.0220(5) Uani 1 1 d . . . . .
N3 N 0.28942(18) 0.78243(14) 0.60278(12) 0.0148(6) Uani 1 1 d . . . . .
O900 O 1.30646(17) 0.37228(13) 0.74588(12) 0.0293(6) Uani 1 1 d . . . . .
O602 O 0.78662(16) 0.20888(12) 0.82485(10) 0.0225(5) Uani 1 1 d . . . . .
O600 O 1.07466(16) 0.25852(12) 0.67063(11) 0.0237(5) Uani 1 1 d . . . . .
O700 O 1.00556(16) 0.07464(12) 0.66378(11) 0.0255(5) Uani 1 1 d . . . . .
C3 C 0.2921(2) 0.77211(16) 0.66315(15) 0.0145(7) Uani 1 1 d . . . . .
O800 O 1.13654(18) 0.27737(14) 0.93581(12) 0.0316(6) Uani 1 1 d . . . . .
N1 N 0.75056(19) 0.50690(14) 0.70174(13) 0.0200(6) Uani 1 1 d . . . . .
C10 C 0.8421(2) 0.55640(18) 0.60565(17) 0.0213(8) Uani 1 1 d . . . . .
N2 N 0.64913(18) 0.93362(14) 0.72853(12) 0.0152(6) Uani 1 1 d . . . . .
O4 O 0.42799(15) 0.73364(12) 0.85375(10) 0.0188(5) Uani 1 1 d . . . . .
C11 C 0.9237(2) 0.58730(19) 0.57742(18) 0.0249(8) Uani 1 1 d . . . . .
H11 H 0.9377 0.5928 0.5317 0.030 Uiso 1 1 calc R U . . .
C15 C 0.7774(2) 0.52765(19) 0.56471(16) 0.0238(8) Uani 1 1 d . . . . .
H15 H 0.7041 0.5394 0.5894 0.029 Uiso 1 1 calc R U . . .
C21 C 0.7028(2) 0.83944(17) 0.64164(15) 0.0167(7) Uani 1 1 d . . . . .
C1 C 0.6565(2) 0.53879(18) 0.72737(15) 0.0170(7) Uani 1 1 d . . . . .
C2 C 0.6410(2) 0.86959(17) 0.70881(15) 0.0137(7) Uani 1 1 d . . . . .
C9 C 0.8226(2) 0.54881(17) 0.67369(17) 0.0199(7) Uani 1 1 d . . . . .
C37 C 0.1943(2) 0.76397(17) 0.70992(15) 0.0166(7) Uani 1 1 d . . . . .
N4 N 0.34414(18) 0.72908(14) 0.96001(12) 0.0166(6) Uani 1 1 d . . . . .
C35 C 0.3385(3) 0.9584(2) 0.78235(19) 0.0305(9) Uani 1 1 d . . . . .
H35A H 0.2929 0.9608 0.7504 0.046 Uiso 1 1 calc R U . . .
H35B H 0.3747 0.9046 0.7893 0.046 Uiso 1 1 calc R U . . .
H35C H 0.2963 0.9811 0.8234 0.046 Uiso 1 1 calc R U . . .
C16 C 0.8168(3) 0.43970(19) 0.55643(18) 0.0299(9) Uani 1 1 d . . . . .
H16A H 0.7745 0.4220 0.5300 0.045 Uiso 1 1 calc R U . . .
H16B H 0.8902 0.4258 0.5349 0.045 Uiso 1 1 calc R U . . .
H16C H 0.8108 0.4153 0.5991 0.045 Uiso 1 1 calc R U . . .
C14 C 0.8826(2) 0.57386(18) 0.71274(17) 0.0217(8) Uani 1 1 d . . . . .
C40 C 0.1610(2) 0.82994(18) 0.75939(16) 0.0204(7) Uani 1 1 d . . . . .
H40A H 0.2183 0.8279 0.7829 0.031 Uiso 1 1 calc R U . . .
H40B H 0.1441 0.8792 0.7368 0.031 Uiso 1 1 calc R U . . .
H40C H 0.0992 0.8249 0.7902 0.031 Uiso 1 1 calc R U . . .
C67 C 0.1117(3) 0.93857(19) 0.91668(17) 0.0267(8) Uani 1 1 d . . . . .
H67A H 0.1090 0.9274 0.8718 0.040 Uiso 1 1 calc R U . . .
H67B H 0.0423 0.9448 0.9434 0.040 Uiso 1 1 calc R U . . .
H67C H 0.1333 0.9861 0.9181 0.040 Uiso 1 1 calc R U . . .
C30 C 0.6643(2) 0.96281(17) 0.83800(15) 0.0162(7) Uani 1 1 d . . . . .
C41 C 0.3789(2) 0.79027(18) 0.55871(15) 0.0161(7) Uani 1 1 d . . . . .
C20 C 0.9023(3) 0.6162(2) 0.82392(19) 0.0352(9) Uani 1 1 d . . . . .
H20A H 0.8848 0.6070 0.8705 0.053 Uiso 1 1 calc R U . . .
H20B H 0.9785 0.6044 0.8110 0.053 Uiso 1 1 calc R U . . .
H20C H 0.8709 0.6703 0.8146 0.053 Uiso 1 1 calc R U . . .
C52 C 0.4499(3) 0.5985(2) 0.46941(17) 0.0283(8) Uani 1 1 d . . . . .
H52A H 0.4301 0.5502 0.4786 0.042 Uiso 1 1 calc R U . . .
H52B H 0.4158 0.6255 0.4343 0.042 Uiso 1 1 calc R U . . .
H52C H 0.5260 0.5873 0.4563 0.042 Uiso 1 1 calc R U . . .
C34 C 0.4197(2) 1.00340(18) 0.75711(16) 0.0204(7) Uani 1 1 d . . . . .
H34 H 0.4633 0.9782 0.7161 0.025 Uiso 1 1 calc R U . . .
C26 C 0.4917(2) 1.00061(17) 0.80576(15) 0.0167(7) Uani 1 1 d . . . . .
C602 C 0.9090(3) 0.2644(2) 0.86048(16) 0.0285(8) Uani 1 1 d . . . . .
H60A H 0.9175 0.3031 0.8896 0.034 Uiso 1 1 calc R U . . .
H60B H 0.9477 0.2128 0.8734 0.034 Uiso 1 1 calc R U . . .
C28 C 0.5128(3) 1.03423(19) 0.91276(17) 0.0239(8) Uani 1 1 d . . . . .
H28 H 0.4830 1.0575 0.9540 0.029 Uiso 1 1 calc R U . . .
C702 C 1.0825(2) 0.0694(2) 0.70397(17) 0.0264(8) Uani 1 1 d . . . . .
H70A H 1.1110 0.1148 0.6959 0.032 Uiso 1 1 calc R U . . .
H70B H 1.1409 0.0230 0.6912 0.032 Uiso 1 1 calc R U . . .
C46 C 0.4424(2) 0.72617(18) 0.52106(15) 0.0183(7) Uani 1 1 d . . . . .
C18 C 0.8598(2) 0.56441(18) 0.78593(17) 0.0240(8) Uani 1 1 d . . . . .
H18 H 0.7820 0.5791 0.7995 0.029 Uiso 1 1 calc R U . . .
C604 C 0.6837(2) 0.1982(2) 0.83622(17) 0.0253(8) Uani 1 1 d . . . . .
H60C H 0.6312 0.2486 0.8363 0.030 Uiso 1 1 calc R U . . .
H60D H 0.6701 0.1739 0.8790 0.030 Uiso 1 1 calc R U . . .
C5 C 0.5891(2) 0.48624(19) 0.76056(16) 0.0209(7) Uani 1 1 d . . . . .
C50 C 0.4149(2) 0.64961(18) 0.53072(16) 0.0216(8) Uani 1 1 d . . . . .
H50 H 0.3369 0.6615 0.5414 0.026 Uiso 1 1 calc R U . . .
C38 C 0.2205(3) 0.68721(19) 0.74620(17) 0.0293(9) Uani 1 1 d . . . . .
H38A H 0.2775 0.6857 0.7698 0.044 Uiso 1 1 calc R U . . .
H38B H 0.1585 0.6825 0.7769 0.044 Uiso 1 1 calc R U . . .
H38C H 0.2422 0.6445 0.7150 0.044 Uiso 1 1 calc R U . . .
C605 C 0.6753(3) 0.14747(19) 0.78325(17) 0.0255(8) Uani 1 1 d . . . . .
H60E H 0.7322 0.0991 0.7803 0.031 Uiso 1 1 calc R U . . .
H60F H 0.6074 0.1343 0.7929 0.031 Uiso 1 1 calc R U . . .
C700 C 0.9330(3) 0.0009(2) 0.60102(19) 0.0336(9) Uani 1 1 d . . . . .
H70C H 0.9099 -0.0462 0.6007 0.050 Uiso 1 1 calc R U . . .
H70D H 0.8741 0.0458 0.5976 0.050 Uiso 1 1 calc R U . . .
H70E H 0.9896 -0.0001 0.5642 0.050 Uiso 1 1 calc R U . . .
C61 C 0.0730(2) 0.78704(19) 0.92658(16) 0.0234(8) Uani 1 1 d . . . . .
H61 H 0.0187 0.8324 0.9232 0.028 Uiso 1 1 calc R U . . .
C39 C 0.1054(2) 0.7666(2) 0.67303(17) 0.0260(8) Uani 1 1 d . . . . .
H39A H 0.1273 0.7242 0.6415 0.039 Uiso 1 1 calc R U . . .
H39B H 0.0436 0.7614 0.7037 0.039 Uiso 1 1 calc R U . . .
H39C H 0.0885 0.8157 0.6503 0.039 Uiso 1 1 calc R U . . .
C42 C 0.3949(2) 0.86433(18) 0.54623(15) 0.0185(7) Uani 1 1 d . . . . .
C23 C 0.8183(2) 0.8070(2) 0.64877(17) 0.0264(8) Uani 1 1 d . . . . .
H23A H 0.8435 0.8475 0.6648 0.040 Uiso 1 1 calc R U . . .
H23B H 0.8245 0.7642 0.6795 0.040 Uiso 1 1 calc R U . . .
H23C H 0.8604 0.7886 0.6065 0.040 Uiso 1 1 calc R U . . .
C45 C 0.5260(2) 0.7368(2) 0.47474(16) 0.0244(8) Uani 1 1 d . . . . .
H45 H 0.5710 0.6938 0.4502 0.029 Uiso 1 1 calc R U . . .
C606 C 0.6620(3) 0.1490(2) 0.67215(16) 0.0257(8) Uani 1 1 d . . . . .
H60G H 0.5883 0.1466 0.6812 0.031 Uiso 1 1 calc R U . . .
H60H H 0.7079 0.0958 0.6681 0.031 Uiso 1 1 calc R U . . .
C8 C 0.6351(3) 0.4034(2) 0.73449(19) 0.0350(9) Uani 1 1 d . . . . .
H8A H 0.7078 0.3847 0.7411 0.053 Uiso 1 1 calc R U . . .
H8B H 0.5939 0.3702 0.7577 0.053 Uiso 1 1 calc R U . . .
H8C H 0.6327 0.4026 0.6881 0.053 Uiso 1 1 calc R U . . .
C24 C 0.6926(3) 0.90587(19) 0.59295(16) 0.0233(8) Uani 1 1 d . . . . .
H24A H 0.7167 0.9471 0.6088 0.035 Uiso 1 1 calc R U . . .
H24B H 0.7353 0.8872 0.5509 0.035 Uiso 1 1 calc R U . . .
H24C H 0.6191 0.9257 0.5881 0.035 Uiso 1 1 calc R U . . .
C53 C 0.5214(2) 0.74144(18) 0.94125(16) 0.0192(7) Uani 1 1 d . . . . .
C25 C 0.6000(2) 0.96340(17) 0.79138(15) 0.0143(7) Uani 1 1 d . . . . .
C611 C 1.1036(3) 0.2857(2) 0.60652(17) 0.0284(8) Uani 1 1 d . . . . .
H61A H 1.1793 0.2824 0.5978 0.034 Uiso 1 1 calc R U . . .
H61B H 1.0645 0.3402 0.6027 0.034 Uiso 1 1 calc R U . . .
C32 C 0.8014(2) 0.83527(18) 0.82882(17) 0.0242(8) Uani 1 1 d . . . . .
H32A H 0.7580 0.8166 0.8039 0.036 Uiso 1 1 calc R U . . .
H32B H 0.8754 0.8103 0.8129 0.036 Uiso 1 1 calc R U . . .
H32C H 0.7835 0.8231 0.8748 0.036 Uiso 1 1 calc R U . . .
C47 C 0.3158(2) 0.93467(18) 0.58068(16) 0.0189(7) Uani 1 1 d . . . . .
H47 H 0.2942 0.9204 0.6267 0.023 Uiso 1 1 calc R U . . .
C33 C 0.8486(2) 0.95247(19) 0.85966(17) 0.0263(8) Uani 1 1 d . . . . .
H33A H 0.9222 0.9246 0.8462 0.039 Uiso 1 1 calc R U . . .
H33B H 0.8399 1.0076 0.8516 0.039 Uiso 1 1 calc R U . . .
H33C H 0.8268 0.9442 0.9060 0.039 Uiso 1 1 calc R U . . .
C49 C 0.2182(2) 0.95608(19) 0.54837(17) 0.0247(8) Uani 1 1 d . . . . .
H49A H 0.1905 0.9112 0.5480 0.037 Uiso 1 1 calc R U . . .
H49B H 0.1647 0.9980 0.5728 0.037 Uiso 1 1 calc R U . . .
H49C H 0.2370 0.9727 0.5038 0.037 Uiso 1 1 calc R U . . .
C57 C 0.2491(2) 0.72465(18) 0.94217(15) 0.0162(7) Uani 1 1 d . . . . .
C36 C 0.3647(3) 1.08649(19) 0.74145(18) 0.0278(8) Uani 1 1 d . . . . .
H36A H 0.3190 1.0863 0.7100 0.042 Uiso 1 1 calc R U . . .
H36B H 0.3228 1.1127 0.7813 0.042 Uiso 1 1 calc R U . . .
H36C H 0.4172 1.1136 0.7230 0.042 Uiso 1 1 calc R U . . .
C803 C 1.1667(3) 0.1411(2) 0.94220(19) 0.0384(10) Uani 1 1 d . . . . .
H80K H 1.2066 0.0945 0.9612 0.058 Uiso 1 1 calc R U . . .
H80J H 1.0917 0.1469 0.9566 0.058 Uiso 1 1 calc R U . . .
H80I H 1.1833 0.1370 0.8948 0.058 Uiso 1 1 calc R U . . .
C29 C 0.6194(2) 0.99844(18) 0.89775(16) 0.0203(7) Uani 1 1 d . . . . .
H29 H 0.6625 0.9983 0.9290 0.024 Uiso 1 1 calc R U . . .
C65 C 0.3025(3) 0.50693(19) 0.91339(19) 0.0343(9) Uani 1 1 d . . . . .
H65A H 0.3603 0.4624 0.9195 0.051 Uiso 1 1 calc R U . . .
H65B H 0.2361 0.4976 0.9350 0.051 Uiso 1 1 calc R U . . .
H65C H 0.3015 0.5148 0.8669 0.051 Uiso 1 1 calc R U . . .
C31 C 0.7813(2) 0.92301(18) 0.82090(16) 0.0192(7) Uani 1 1 d . . . . .
H31 H 0.8045 0.9332 0.7741 0.023 Uiso 1 1 calc R U . . .
C801 C 1.1461(3) 0.3471(2) 0.96120(19) 0.0347(9) Uani 1 1 d . . . . .
H80A H 1.2195 0.3499 0.9503 0.042 Uiso 1 1 calc R U . . .
H80B H 1.1254 0.3485 1.0090 0.042 Uiso 1 1 calc R U . . .
C600 C 1.0899(3) 0.3062(2) 0.71903(17) 0.0312(9) Uani 1 1 d . . . . .
H60I H 1.0467 0.3596 0.7154 0.037 Uiso 1 1 calc R U . . .
H60J H 1.1642 0.3069 0.7124 0.037 Uiso 1 1 calc R U . . .
C603 C 0.7954(3) 0.26819(19) 0.86579(16) 0.0248(8) Uani 1 1 d . . . . .
H60K H 0.7648 0.2602 0.9113 0.030 Uiso 1 1 calc R U . . .
H60L H 0.7569 0.3193 0.8518 0.030 Uiso 1 1 calc R U . . .
C62 C 0.1695(2) 0.79354(18) 0.93758(15) 0.0182(7) Uani 1 1 d . . . . .
C27 C 0.4512(2) 1.03529(18) 0.86668(16) 0.0217(8) Uani 1 1 d . . . . .
H27 H 0.3787 1.0605 0.8767 0.026 Uiso 1 1 calc R U . . .
C608 C 0.8184(3) 0.2261(2) 0.53627(16) 0.0260(8) Uani 1 1 d . . . . .
H60M H 0.7854 0.2821 0.5406 0.031 Uiso 1 1 calc R U . . .
H60N H 0.7931 0.2061 0.5008 0.031 Uiso 1 1 calc R U . . .
C903 C 1.3745(3) 0.2748(2) 0.8175(2) 0.0461(11) Uani 1 1 d . . . . .
H90A H 1.4266 0.2256 0.8203 0.069 Uiso 1 1 calc R U . . .
H90B H 1.3870 0.3133 0.8443 0.069 Uiso 1 1 calc R U . . .
H90C H 1.3042 0.2684 0.8329 0.069 Uiso 1 1 calc R U . . .
C601 C 1.0591(3) 0.2751(2) 0.78484(17) 0.0317(9) Uani 1 1 d . . . . .
H60O H 1.1002 0.2210 0.7879 0.038 Uiso 1 1 calc R U . . .
H60P H 1.0733 0.3056 0.8186 0.038 Uiso 1 1 calc R U . . .
C609 C 0.9353(3) 0.2110(2) 0.52091(16) 0.0256(8) Uani 1 1 d . . . . .
H60Q H 0.9687 0.1550 0.5216 0.031 Uiso 1 1 calc R U . . .
H60R H 0.9565 0.2306 0.4772 0.031 Uiso 1 1 calc R U . . .
C902 C 1.3830(3) 0.3009(2) 0.74841(19) 0.0358(10) Uani 1 1 d . . . . .
H90D H 1.4539 0.3073 0.7323 0.043 Uiso 1 1 calc R U . . .
H90E H 1.3707 0.2622 0.7209 0.043 Uiso 1 1 calc R U . . .
C13 C 0.9635(2) 0.60421(18) 0.68184(18) 0.0264(8) Uani 1 1 d . . . . .
H13 H 1.0049 0.6211 0.7073 0.032 Uiso 1 1 calc R U . . .
C701 C 0.9718(3) 0.0056(2) 0.66340(19) 0.0354(9) Uani 1 1 d . . . . .
H70F H 0.9150 0.0061 0.7008 0.042 Uiso 1 1 calc R U . . .
H70G H 1.0308 -0.0399 0.6673 0.042 Uiso 1 1 calc R U . . .
C4 C 0.4241(2) 0.73297(16) 0.91748(15) 0.0149(7) Uani 1 1 d . . . . .
C703 C 1.0416(3) 0.0653(2) 0.77551(17) 0.0329(9) Uani 1 1 d . . . . .
H70H H 1.0983 0.0619 0.7998 0.049 Uiso 1 1 calc R U . . .
H70I H 0.9850 0.1117 0.7890 0.049 Uiso 1 1 calc R U . . .
H70J H 1.0149 0.0198 0.7842 0.049 Uiso 1 1 calc R U . . .
C19 C 0.9003(3) 0.48025(19) 0.80574(18) 0.0290(8) Uani 1 1 d . . . . .
H19A H 0.8844 0.4761 0.8530 0.043 Uiso 1 1 calc R U . . .
H19B H 0.8661 0.4480 0.7857 0.043 Uiso 1 1 calc R U . . .
H19C H 0.9761 0.4629 0.7911 0.043 Uiso 1 1 calc R U . . .
C51 C 0.4573(3) 0.60541(19) 0.58812(17) 0.0278(8) Uani 1 1 d . . . . .
H51A H 0.4380 0.5566 0.5928 0.042 Uiso 1 1 calc R U . . .
H51B H 0.5336 0.5952 0.5806 0.042 Uiso 1 1 calc R U . . .
H51C H 0.4273 0.6361 0.6278 0.042 Uiso 1 1 calc R U . . .
C607 C 0.6820(2) 0.1918(2) 0.61056(17) 0.0264(8) Uani 1 1 d . . . . .
H60S H 0.6616 0.1684 0.5748 0.032 Uiso 1 1 calc R U . . .
H60T H 0.6398 0.2461 0.6157 0.032 Uiso 1 1 calc R U . . .
C68 C 0.1940(3) 0.8902(2) 1.01277(17) 0.0344(9) Uani 1 1 d . . . . .
H68A H 0.2081 0.9405 1.0144 0.052 Uiso 1 1 calc R U . . .
H68B H 0.1264 0.8914 1.0400 0.052 Uiso 1 1 calc R U . . .
H68C H 0.2494 0.8507 1.0288 0.052 Uiso 1 1 calc R U . . .
C44 C 0.5448(2) 0.8085(2) 0.46375(17) 0.0271(8) Uani 1 1 d . . . . .
H44 H 0.6027 0.8143 0.4325 0.032 Uiso 1 1 calc R U . . .
C901 C 1.3122(3) 0.4051(2) 0.68334(19) 0.0353(9) Uani 1 1 d . . . . .
H90F H 1.3025 0.3694 0.6519 0.042 Uiso 1 1 calc R U . . .
H90G H 1.3817 0.4148 0.6691 0.042 Uiso 1 1 calc R U . . .
C7 C 0.4753(3) 0.5160(2) 0.75045(19) 0.0345(9) Uani 1 1 d . . . . .
H7A H 0.4727 0.5158 0.7040 0.052 Uiso 1 1 calc R U . . .
H7B H 0.4340 0.4828 0.7734 0.052 Uiso 1 1 calc R U . . .
H7C H 0.4463 0.5687 0.7675 0.052 Uiso 1 1 calc R U . . .
C55 C 0.6222(2) 0.6944(2) 0.89870(18) 0.0321(9) Uani 1 1 d . . . . .
H55A H 0.6230 0.7109 0.8535 0.048 Uiso 1 1 calc R U . . .
H55B H 0.6832 0.7028 0.9137 0.048 Uiso 1 1 calc R U . . .
H55C H 0.6247 0.6396 0.9018 0.048 Uiso 1 1 calc R U . . .
C12 C 0.9851(3) 0.61028(19) 0.61521(18) 0.0293(9) Uani 1 1 d . . . . .
H12 H 1.0416 0.6301 0.5952 0.035 Uiso 1 1 calc R U . . .
C17 C 0.7727(3) 0.5666(2) 0.49891(17) 0.0336(9) Uani 1 1 d . . . . .
H17A H 0.7299 0.5452 0.4755 0.050 Uiso 1 1 calc R U . . .
H17B H 0.7415 0.6220 0.5052 0.050 Uiso 1 1 calc R U . . .
H17C H 0.8436 0.5575 0.4737 0.050 Uiso 1 1 calc R U . . .
C66 C 0.1912(2) 0.87151(18) 0.94306(16) 0.0223(8) Uani 1 1 d . . . . .
H66 H 0.2619 0.8688 0.9168 0.027 Uiso 1 1 calc R U . . .
C48 C 0.3577(3) 1.00502(19) 0.58092(17) 0.0273(8) Uani 1 1 d . . . . .
H48A H 0.3029 1.0475 0.6037 0.041 Uiso 1 1 calc R U . . .
H48B H 0.4182 0.9926 0.6031 0.041 Uiso 1 1 calc R U . . .
H48C H 0.3788 1.0202 0.5362 0.041 Uiso 1 1 calc R U . . .
C900 C 1.2277(3) 0.4795(2) 0.6860(2) 0.0475(11) Uani 1 1 d . . . . .
H90H H 1.2307 0.5029 0.6429 0.071 Uiso 1 1 calc R U . . .
H90I H 1.1592 0.4693 0.6999 0.071 Uiso 1 1 calc R U . . .
H90J H 1.2381 0.5146 0.7170 0.071 Uiso 1 1 calc R U . . .
C800 C 1.0753(3) 0.4141(2) 0.9314(2) 0.0487(12) Uani 1 1 d . . . . .
H80C H 1.0806 0.4625 0.9482 0.073 Uiso 1 1 calc R U . . .
H80D H 1.0967 0.4123 0.8842 0.073 Uiso 1 1 calc R U . . .
H80E H 1.0028 0.4108 0.9427 0.073 Uiso 1 1 calc R U . . .
C60 C 0.0547(2) 0.7162(2) 0.92058(16) 0.0251(8) Uani 1 1 d . . . . .
H60 H -0.0118 0.7134 0.9135 0.030 Uiso 1 1 calc R U . . .
C610 C 1.0787(2) 0.2372(2) 0.55826(17) 0.0281(8) Uani 1 1 d . . . . .
H61C H 1.1043 0.2520 0.5135 0.034 Uiso 1 1 calc R U . . .
H61D H 1.1134 0.1822 0.5642 0.034 Uiso 1 1 calc R U . . .
C59 C 0.1333(2) 0.64924(19) 0.92492(16) 0.0234(8) Uani 1 1 d . . . . .
H59 H 0.1201 0.6008 0.9203 0.028 Uiso 1 1 calc R U . . .
C63 C 0.3173(2) 0.57871(18) 0.94274(17) 0.0225(8) Uani 1 1 d . . . . .
H63 H 0.3843 0.5872 0.9186 0.027 Uiso 1 1 calc R U . . .
C56 C 0.5198(3) 0.8277(2) 0.9360(2) 0.0384(10) Uani 1 1 d . . . . .
H56A H 0.5197 0.8443 0.8908 0.058 Uiso 1 1 calc R U . . .
H56B H 0.4567 0.8584 0.9636 0.058 Uiso 1 1 calc R U . . .
H56C H 0.5819 0.8350 0.9501 0.058 Uiso 1 1 calc R U . . .
C64 C 0.3301(3) 0.5644(2) 1.01380(17) 0.0341(9) Uani 1 1 d . . . . .
H64A H 0.3858 0.5172 1.0168 0.051 Uiso 1 1 calc R U . . .
H64B H 0.3485 0.6080 1.0304 0.051 Uiso 1 1 calc R U . . .
H64C H 0.2642 0.5589 1.0396 0.051 Uiso 1 1 calc R U . . .
C54 C 0.5216(3) 0.7152(3) 1.01089(18) 0.0404(11) Uani 1 1 d . . . . .
H54A H 0.5845 0.7212 1.0249 0.061 Uiso 1 1 calc R U . . .
H54B H 0.4593 0.7464 1.0388 0.061 Uiso 1 1 calc R U . . .
H54C H 0.5210 0.6610 1.0140 0.061 Uiso 1 1 calc R U . . .
C43 C 0.4788(2) 0.8714(2) 0.49865(16) 0.0227(8) Uani 1 1 d . . . . .
H43 H 0.4908 0.9207 0.4901 0.027 Uiso 1 1 calc R U . . .
C58 C 0.2310(2) 0.65197(18) 0.93591(15) 0.0186(7) Uani 1 1 d . . . . .
C6 C 0.5927(2) 0.4868(2) 0.83335(16) 0.0254(8) Uani 1 1 d . . . . .
H6A H 0.6653 0.4678 0.8400 0.038 Uiso 1 1 calc R U . . .
H6B H 0.5636 0.5394 0.8503 0.038 Uiso 1 1 calc R U . . .
H6C H 0.5513 0.4535 0.8562 0.038 Uiso 1 1 calc R U . . .
C22 C 0.6649(3) 0.77524(19) 0.61648(16) 0.0253(8) Uani 1 1 d . . . . .
H22A H 0.6713 0.7326 0.6474 0.038 Uiso 1 1 calc R U . . .
H22B H 0.5915 0.7953 0.6116 0.038 Uiso 1 1 calc R U . . .
H22C H 0.7077 0.7568 0.5744 0.038 Uiso 1 1 calc R U . . .
C802 C 1.1953(3) 0.2107(2) 0.96391(18) 0.0321(9) Uani 1 1 d . . . . .
H80F H 1.1792 0.2150 1.0118 0.038 Uiso 1 1 calc R U . . .
H80G H 1.2711 0.2051 0.9498 0.038 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 O1 2.234(2) . ?
U1 O4 2.235(2) . ?
U1 O3 2.236(2) . ?
U1 O2 2.253(2) . ?
K1 O604 2.738(2) . ?
K1 O601 2.778(2) . ?
K1 O605 2.779(2) . ?
K1 O602 2.814(2) . ?
K1 O603 2.822(2) . ?
K1 O700 2.835(2) . ?
K1 O600 2.843(2) . ?
O1 C1 1.334(4) . ?
O2 C2 1.323(3) . ?
O3 C3 1.334(3) . ?
O603 C606 1.424(4) . ?
O603 C605 1.424(4) . ?
O604 C608 1.430(4) . ?
O604 C607 1.432(4) . ?
O601 C602 1.431(4) . ?
O601 C601 1.436(4) . ?
O605 C609 1.430(4) . ?
O605 C610 1.431(4) . ?
N3 C3 1.277(4) . ?
N3 C41 1.417(4) . ?
O900 C901 1.413(4) . ?
O900 C902 1.423(4) . ?
O602 C604 1.428(4) . ?
O602 C603 1.442(4) . ?
O600 C600 1.434(4) . ?
O600 C611 1.434(4) . ?
O700 C702 1.432(4) . ?
O700 C701 1.437(4) . ?
C3 C37 1.532(4) . ?
O800 C802 1.420(4) . ?
O800 C801 1.432(4) . ?
N1 C1 1.271(4) . ?
N1 C9 1.418(4) . ?
C10 C11 1.392(4) . ?
C10 C9 1.411(5) . ?
C10 C15 1.523(5) . ?
N2 C2 1.282(4) . ?
N2 C25 1.421(4) . ?
O4 C4 1.327(4) . ?
C11 C12 1.391(5) . ?
C11 H11 0.9500 . ?
C15 C17 1.524(5) . ?
C15 C16 1.539(5) . ?
C15 H15 1.0000 . ?
C21 C22 1.533(4) . ?
C21 C24 1.534(4) . ?
C21 C2 1.540(4) . ?
C21 C23 1.540(4) . ?
C1 C5 1.545(4) . ?
C9 C14 1.413(5) . ?
C37 C39 1.528(4) . ?
C37 C40 1.531(4) . ?
C37 C38 1.538(4) . ?
N4 C4 1.284(4) . ?
N4 C57 1.420(4) . ?
C35 C34 1.541(5) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C14 C13 1.395(5) . ?
C14 C18 1.521(5) . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C67 C66 1.542(4) . ?
C67 H67A 0.9800 . ?
C67 H67B 0.9800 . ?
C67 H67C 0.9800 . ?
C30 C29 1.391(4) . ?
C30 C25 1.416(4) . ?
C30 C31 1.530(4) . ?
C41 C46 1.413(4) . ?
C41 C42 1.417(4) . ?
C20 C18 1.535(5) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C52 C50 1.541(4) . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C34 C26 1.520(4) . ?
C34 C36 1.534(5) . ?
C34 H34 1.0000 . ?
C26 C27 1.398(4) . ?
C26 C25 1.416(4) . ?
C602 C603 1.498(5) . ?
C602 H60A 0.9900 . ?
C602 H60B 0.9900 . ?
C28 C27 1.379(4) . ?
C28 C29 1.390(4) . ?
C28 H28 0.9500 . ?
C702 C703 1.508(5) . ?
C702 H70A 0.9900 . ?
C702 H70B 0.9900 . ?
C46 C45 1.398(4) . ?
C46 C50 1.521(5) . ?
C18 C19 1.536(5) . ?
C18 H18 1.0000 . ?
C604 C605 1.508(5) . ?
C604 H60C 0.9900 . ?
C604 H60D 0.9900 . ?
C5 C7 1.534(4) . ?
C5 C6 1.536(5) . ?
C5 C8 1.538(5) . ?
C50 C51 1.526(4) . ?
C50 H50 1.0000 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C605 H60E 0.9900 . ?
C605 H60F 0.9900 . ?
C700 C701 1.507(5) . ?
C700 H70C 0.9800 . ?
C700 H70D 0.9800 . ?
C700 H70E 0.9800 . ?
C61 C60 1.380(5) . ?
C61 C62 1.397(4) . ?
C61 H61 0.9500 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C42 C43 1.396(4) . ?
C42 C47 1.531(4) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C45 C44 1.387(5) . ?
C45 H45 0.9500 . ?
C606 C607 1.496(5) . ?
C606 H60G 0.9900 . ?
C606 H60H 0.9900 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C53 C54 1.516(5) . ?
C53 C4 1.530(4) . ?
C53 C55 1.540(4) . ?
C53 C56 1.552(5) . ?
C611 C610 1.504(5) . ?
C611 H61A 0.9900 . ?
C611 H61B 0.9900 . ?
C32 C31 1.540(4) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C47 C48 1.523(4) . ?
C47 C49 1.538(4) . ?
C47 H47 1.0000 . ?
C33 C31 1.526(4) . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?
C57 C58 1.413(4) . ?
C57 C62 1.419(4) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C803 C802 1.518(5) . ?
C803 H80K 0.9800 . ?
C803 H80J 0.9800 . ?
C803 H80I 0.9800 . ?
C29 H29 0.9500 . ?
C65 C63 1.533(5) . ?
C65 H65A 0.9800 . ?
C65 H65B 0.9800 . ?
C65 H65C 0.9800 . ?
C31 H31 1.0000 . ?
C801 C800 1.513(5) . ?
C801 H80A 0.9900 . ?
C801 H80B 0.9900 . ?
C600 C601 1.498(5) . ?
C600 H60I 0.9900 . ?
C600 H60J 0.9900 . ?
C603 H60K 0.9900 . ?
C603 H60L 0.9900 . ?
C62 C66 1.525(4) . ?
C27 H27 0.9500 . ?
C608 C609 1.500(5) . ?
C608 H60M 0.9900 . ?
C608 H60N 0.9900 . ?
C903 C902 1.497(5) . ?
C903 H90A 0.9800 . ?
C903 H90B 0.9800 . ?
C903 H90C 0.9800 . ?
C601 H60O 0.9900 . ?
C601 H60P 0.9900 . ?
C609 H60Q 0.9900 . ?
C609 H60R 0.9900 . ?
C902 H90D 0.9900 . ?
C902 H90E 0.9900 . ?
C13 C12 1.380(5) . ?
C13 H13 0.9500 . ?
C701 H70F 0.9900 . ?
C701 H70G 0.9900 . ?
C703 H70H 0.9800 . ?
C703 H70I 0.9800 . ?
C703 H70J 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C51 H51A 0.9800 . ?
C51 H51B 0.9800 . ?
C51 H51C 0.9800 . ?
C607 H60S 0.9900 . ?
C607 H60T 0.9900 . ?
C68 C66 1.523(5) . ?
C68 H68A 0.9800 . ?
C68 H68B 0.9800 . ?
C68 H68C 0.9800 . ?
C44 C43 1.382(5) . ?
C44 H44 0.9500 . ?
C901 C900 1.504(5) . ?
C901 H90F 0.9900 . ?
C901 H90G 0.9900 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C55 H55A 0.9800 . ?
C55 H55B 0.9800 . ?
C55 H55C 0.9800 . ?
C12 H12 0.9500 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C66 H66 1.0000 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C900 H90H 0.9800 . ?
C900 H90I 0.9800 . ?
C900 H90J 0.9800 . ?
C800 H80C 0.9800 . ?
C800 H80D 0.9800 . ?
C800 H80E 0.9800 . ?
C60 C59 1.388(5) . ?
C60 H60 0.9500 . ?
C610 H61C 0.9900 . ?
C610 H61D 0.9900 . ?
C59 C58 1.392(4) . ?
C59 H59 0.9500 . ?
C63 C58 1.528(4) . ?
C63 C64 1.534(5) . ?
C63 H63 1.0000 . ?
C56 H56A 0.9800 . ?
C56 H56B 0.9800 . ?
C56 H56C 0.9800 . ?
C64 H64A 0.9800 . ?
C64 H64B 0.9800 . ?
C64 H64C 0.9800 . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
C43 H43 0.9500 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C802 H80F 0.9900 . ?
C802 H80G 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 U1 O4 105.43(8) . . ?
O1 U1 O3 116.28(8) . . ?
O4 U1 O3 107.85(8) . . ?
O1 U1 O2 113.03(7) . . ?
O4 U1 O2 104.24(7) . . ?
O3 U1 O2 109.11(8) . . ?
O604 K1 O601 173.57(7) . . ?
O604 K1 O605 61.95(7) . . ?
O601 K1 O605 117.46(7) . . ?
O604 K1 O602 120.58(7) . . ?
O601 K1 O602 59.78(7) . . ?
O605 K1 O602 176.74(7) . . ?
O604 K1 O603 60.71(7) . . ?
O601 K1 O603 118.39(7) . . ?
O605 K1 O603 121.89(7) . . ?
O602 K1 O603 60.28(6) . . ?
O604 K1 O700 79.31(7) . . ?
O601 K1 O700 107.04(7) . . ?
O605 K1 O700 80.44(7) . . ?
O602 K1 O700 101.89(7) . . ?
O603 K1 O700 97.60(7) . . ?
O604 K1 O600 121.09(7) . . ?
O601 K1 O600 60.05(7) . . ?
O605 K1 O600 60.23(7) . . ?
O602 K1 O600 117.67(7) . . ?
O603 K1 O600 177.44(7) . . ?
O700 K1 O600 81.22(7) . . ?
C1 O1 U1 167.50(19) . . ?
C2 O2 U1 151.18(19) . . ?
C3 O3 U1 164.51(19) . . ?
C606 O603 C605 112.4(2) . . ?
C606 O603 K1 113.52(17) . . ?
C605 O603 K1 110.40(17) . . ?
C608 O604 C607 112.9(2) . . ?
C608 O604 K1 113.03(18) . . ?
C607 O604 K1 116.13(18) . . ?
C602 O601 C601 112.3(2) . . ?
C602 O601 K1 119.30(18) . . ?
C601 O601 K1 117.05(18) . . ?
C609 O605 C610 112.3(2) . . ?
C609 O605 K1 113.41(18) . . ?
C610 O605 K1 114.87(18) . . ?
C3 N3 C41 120.8(3) . . ?
C901 O900 C902 113.0(3) . . ?
C604 O602 C603 112.2(2) . . ?
C604 O602 K1 116.71(18) . . ?
C603 O602 K1 111.74(18) . . ?
C600 O600 C611 111.4(2) . . ?
C600 O600 K1 114.24(18) . . ?
C611 O600 K1 114.75(18) . . ?
C702 O700 C701 113.3(3) . . ?
C702 O700 K1 100.65(17) . . ?
C701 O700 K1 126.77(19) . . ?
N3 C3 O3 124.9(3) . . ?
N3 C3 C37 119.9(3) . . ?
O3 C3 C37 115.3(3) . . ?
C802 O800 C801 112.5(3) . . ?
C1 N1 C9 123.2(3) . . ?
C11 C10 C9 118.6(3) . . ?
C11 C10 C15 121.6(3) . . ?
C9 C10 C15 119.7(3) . . ?
C2 N2 C25 121.6(3) . . ?
C4 O4 U1 156.07(19) . . ?
C12 C11 C10 121.0(3) . . ?
C12 C11 H11 119.5 . . ?
C10 C11 H11 119.5 . . ?
C10 C15 C17 114.2(3) . . ?
C10 C15 C16 110.4(3) . . ?
C17 C15 C16 110.5(3) . . ?
C10 C15 H15 107.2 . . ?
C17 C15 H15 107.2 . . ?
C16 C15 H15 107.2 . . ?
C22 C21 C24 109.1(3) . . ?
C22 C21 C2 112.3(3) . . ?
C24 C21 C2 109.6(2) . . ?
C22 C21 C23 108.7(3) . . ?
C24 C21 C23 109.8(3) . . ?
C2 C21 C23 107.3(3) . . ?
N1 C1 O1 126.5(3) . . ?
N1 C1 C5 117.6(3) . . ?
O1 C1 C5 115.8(3) . . ?
N2 C2 O2 125.4(3) . . ?
N2 C2 C21 117.8(3) . . ?
O2 C2 C21 116.6(3) . . ?
C10 C9 C14 120.9(3) . . ?
C10 C9 N1 118.7(3) . . ?
C14 C9 N1 120.0(3) . . ?
C39 C37 C40 109.9(3) . . ?
C39 C37 C3 110.6(3) . . ?
C40 C37 C3 108.6(2) . . ?
C39 C37 C38 109.6(3) . . ?
C40 C37 C38 108.7(3) . . ?
C3 C37 C38 109.4(2) . . ?
C4 N4 C57 121.9(3) . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C13 C14 C9 118.0(3) . . ?
C13 C14 C18 122.5(3) . . ?
C9 C14 C18 119.5(3) . . ?
C37 C40 H40A 109.5 . . ?
C37 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C37 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C66 C67 H67A 109.5 . . ?
C66 C67 H67B 109.5 . . ?
H67A C67 H67B 109.5 . . ?
C66 C67 H67C 109.5 . . ?
H67A C67 H67C 109.5 . . ?
H67B C67 H67C 109.5 . . ?
C29 C30 C25 119.2(3) . . ?
C29 C30 C31 122.0(3) . . ?
C25 C30 C31 118.8(3) . . ?
C46 C41 N3 119.4(3) . . ?
C46 C41 C42 120.6(3) . . ?
N3 C41 C42 119.4(3) . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C50 C52 H52A 109.5 . . ?
C50 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C50 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C26 C34 C36 111.5(3) . . ?
C26 C34 C35 110.6(3) . . ?
C36 C34 C35 110.3(3) . . ?
C26 C34 H34 108.1 . . ?
C36 C34 H34 108.1 . . ?
C35 C34 H34 108.1 . . ?
C27 C26 C25 118.2(3) . . ?
C27 C26 C34 120.0(3) . . ?
C25 C26 C34 121.8(3) . . ?
O601 C602 C603 108.5(3) . . ?
O601 C602 H60A 110.0 . . ?
C603 C602 H60A 110.0 . . ?
O601 C602 H60B 110.0 . . ?
C603 C602 H60B 110.0 . . ?
H60A C602 H60B 108.4 . . ?
C27 C28 C29 118.8(3) . . ?
C27 C28 H28 120.6 . . ?
C29 C28 H28 120.6 . . ?
O700 C702 C703 114.1(3) . . ?
O700 C702 H70A 108.7 . . ?
C703 C702 H70A 108.7 . . ?
O700 C702 H70B 108.7 . . ?
C703 C702 H70B 108.7 . . ?
H70A C702 H70B 107.6 . . ?
C45 C46 C41 118.2(3) . . ?
C45 C46 C50 122.8(3) . . ?
C41 C46 C50 118.9(3) . . ?
C14 C18 C20 114.1(3) . . ?
C14 C18 C19 111.4(3) . . ?
C20 C18 C19 109.5(3) . . ?
C14 C18 H18 107.2 . . ?
C20 C18 H18 107.2 . . ?
C19 C18 H18 107.2 . . ?
O602 C604 C605 108.7(3) . . ?
O602 C604 H60C 110.0 . . ?
C605 C604 H60C 110.0 . . ?
O602 C604 H60D 110.0 . . ?
C605 C604 H60D 110.0 . . ?
H60C C604 H60D 108.3 . . ?
C7 C5 C6 109.3(3) . . ?
C7 C5 C8 109.9(3) . . ?
C6 C5 C8 109.0(3) . . ?
C7 C5 C1 111.4(3) . . ?
C6 C5 C1 106.9(3) . . ?
C8 C5 C1 110.4(3) . . ?
C46 C50 C51 111.8(3) . . ?
C46 C50 C52 113.3(3) . . ?
C51 C50 C52 110.4(3) . . ?
C46 C50 H50 107.0 . . ?
C51 C50 H50 107.0 . . ?
C52 C50 H50 107.0 . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
O603 C605 C604 108.3(3) . . ?
O603 C605 H60E 110.0 . . ?
C604 C605 H60E 110.0 . . ?
O603 C605 H60F 110.0 . . ?
C604 C605 H60F 110.0 . . ?
H60E C605 H60F 108.4 . . ?
C701 C700 H70C 109.5 . . ?
C701 C700 H70D 109.5 . . ?
H70C C700 H70D 109.5 . . ?
C701 C700 H70E 109.5 . . ?
H70C C700 H70E 109.5 . . ?
H70D C700 H70E 109.5 . . ?
C60 C61 C62 121.6(3) . . ?
C60 C61 H61 119.2 . . ?
C62 C61 H61 119.2 . . ?
C37 C39 H39A 109.5 . . ?
C37 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C37 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C43 C42 C41 118.4(3) . . ?
C43 C42 C47 121.8(3) . . ?
C41 C42 C47 119.6(3) . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C44 C45 C46 121.6(3) . . ?
C44 C45 H45 119.2 . . ?
C46 C45 H45 119.2 . . ?
O603 C606 C607 108.5(3) . . ?
O603 C606 H60G 110.0 . . ?
C607 C606 H60G 110.0 . . ?
O603 C606 H60H 110.0 . . ?
C607 C606 H60H 110.0 . . ?
H60G C606 H60H 108.4 . . ?
C5 C8 H8A 109.5 . . ?
C5 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C5 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C21 C24 H24A 109.5 . . ?
C21 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C21 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C54 C53 C4 111.1(3) . . ?
C54 C53 C55 108.7(3) . . ?
C4 C53 C55 111.2(3) . . ?
C54 C53 C56 109.9(3) . . ?
C4 C53 C56 107.4(3) . . ?
C55 C53 C56 108.5(3) . . ?
C30 C25 C26 119.9(3) . . ?
C30 C25 N2 118.1(3) . . ?
C26 C25 N2 121.7(3) . . ?
O600 C611 C610 109.0(3) . . ?
O600 C611 H61A 109.9 . . ?
C610 C611 H61A 109.9 . . ?
O600 C611 H61B 109.9 . . ?
C610 C611 H61B 109.9 . . ?
H61A C611 H61B 108.3 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C48 C47 C42 114.2(3) . . ?
C48 C47 C49 108.8(3) . . ?
C42 C47 C49 109.3(3) . . ?
C48 C47 H47 108.1 . . ?
C42 C47 H47 108.1 . . ?
C49 C47 H47 108.1 . . ?
C31 C33 H33A 109.5 . . ?
C31 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C31 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C47 C49 H49A 109.5 . . ?
C47 C49 H49B 109.5 . . ?
H49A C49 H49B 109.5 . . ?
C47 C49 H49C 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
C58 C57 C62 120.9(3) . . ?
C58 C57 N4 119.7(3) . . ?
C62 C57 N4 119.1(3) . . ?
C34 C36 H36A 109.5 . . ?
C34 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C34 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C802 C803 H80K 109.5 . . ?
C802 C803 H80J 109.5 . . ?
H80K C803 H80J 109.5 . . ?
C802 C803 H80I 109.5 . . ?
H80K C803 H80I 109.5 . . ?
H80J C803 H80I 109.5 . . ?
C28 C29 C30 121.5(3) . . ?
C28 C29 H29 119.3 . . ?
C30 C29 H29 119.3 . . ?
C63 C65 H65A 109.5 . . ?
C63 C65 H65B 109.5 . . ?
H65A C65 H65B 109.5 . . ?
C63 C65 H65C 109.5 . . ?
H65A C65 H65C 109.5 . . ?
H65B C65 H65C 109.5 . . ?
C33 C31 C30 113.9(3) . . ?
C33 C31 C32 109.8(3) . . ?
C30 C31 C32 110.6(3) . . ?
C33 C31 H31 107.4 . . ?
C30 C31 H31 107.4 . . ?
C32 C31 H31 107.4 . . ?
O800 C801 C800 108.1(3) . . ?
O800 C801 H80A 110.1 . . ?
C800 C801 H80A 110.1 . . ?
O800 C801 H80B 110.1 . . ?
C800 C801 H80B 110.1 . . ?
H80A C801 H80B 108.4 . . ?
O600 C600 C601 109.2(3) . . ?
O600 C600 H60I 109.8 . . ?
C601 C600 H60I 109.8 . . ?
O600 C600 H60J 109.8 . . ?
C601 C600 H60J 109.8 . . ?
H60I C600 H60J 108.3 . . ?
O602 C603 C602 108.3(3) . . ?
O602 C603 H60K 110.0 . . ?
C602 C603 H60K 110.0 . . ?
O602 C603 H60L 110.0 . . ?
C602 C603 H60L 110.0 . . ?
H60K C603 H60L 108.4 . . ?
C61 C62 C57 117.8(3) . . ?
C61 C62 C66 122.0(3) . . ?
C57 C62 C66 120.2(3) . . ?
C28 C27 C26 122.4(3) . . ?
C28 C27 H27 118.8 . . ?
C26 C27 H27 118.8 . . ?
O604 C608 C609 108.8(3) . . ?
O604 C608 H60M 109.9 . . ?
C609 C608 H60M 109.9 . . ?
O604 C608 H60N 109.9 . . ?
C609 C608 H60N 109.9 . . ?
H60M C608 H60N 108.3 . . ?
C902 C903 H90A 109.5 . . ?
C902 C903 H90B 109.5 . . ?
H90A C903 H90B 109.5 . . ?
C902 C903 H90C 109.5 . . ?
H90A C903 H90C 109.5 . . ?
H90B C903 H90C 109.5 . . ?
O601 C601 C600 108.6(3) . . ?
O601 C601 H60O 110.0 . . ?
C600 C601 H60O 110.0 . . ?
O601 C601 H60P 110.0 . . ?
C600 C601 H60P 110.0 . . ?
H60O C601 H60P 108.3 . . ?
O605 C609 C608 108.4(3) . . ?
O605 C609 H60Q 110.0 . . ?
C608 C609 H60Q 110.0 . . ?
O605 C609 H60R 110.0 . . ?
C608 C609 H60R 110.0 . . ?
H60Q C609 H60R 108.4 . . ?
O900 C902 C903 108.1(3) . . ?
O900 C902 H90D 110.1 . . ?
C903 C902 H90D 110.1 . . ?
O900 C902 H90E 110.1 . . ?
C903 C902 H90E 110.1 . . ?
H90D C902 H90E 108.4 . . ?
C12 C13 C14 121.7(3) . . ?
C12 C13 H13 119.1 . . ?
C14 C13 H13 119.1 . . ?
O700 C701 C700 109.4(3) . . ?
O700 C701 H70F 109.8 . . ?
C700 C701 H70F 109.8 . . ?
O700 C701 H70G 109.8 . . ?
C700 C701 H70G 109.8 . . ?
H70F C701 H70G 108.2 . . ?
N4 C4 O4 125.1(3) . . ?
N4 C4 C53 118.3(3) . . ?
O4 C4 C53 116.5(3) . . ?
C702 C703 H70H 109.5 . . ?
C702 C703 H70I 109.5 . . ?
H70H C703 H70I 109.5 . . ?
C702 C703 H70J 109.5 . . ?
H70H C703 H70J 109.5 . . ?
H70I C703 H70J 109.5 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C50 C51 H51A 109.5 . . ?
C50 C51 H51B 109.5 . . ?
H51A C51 H51B 109.5 . . ?
C50 C51 H51C 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
O604 C607 C606 108.7(3) . . ?
O604 C607 H60S 109.9 . . ?
C606 C607 H60S 109.9 . . ?
O604 C607 H60T 109.9 . . ?
C606 C607 H60T 109.9 . . ?
H60S C607 H60T 108.3 . . ?
C66 C68 H68A 109.5 . . ?
C66 C68 H68B 109.5 . . ?
H68A C68 H68B 109.5 . . ?
C66 C68 H68C 109.5 . . ?
H68A C68 H68C 109.5 . . ?
H68B C68 H68C 109.5 . . ?
C43 C44 C45 119.5(3) . . ?
C43 C44 H44 120.3 . . ?
C45 C44 H44 120.3 . . ?
O900 C901 C900 108.5(3) . . ?
O900 C901 H90F 110.0 . . ?
C900 C901 H90F 110.0 . . ?
O900 C901 H90G 110.0 . . ?
C900 C901 H90G 110.0 . . ?
H90F C901 H90G 108.4 . . ?
C5 C7 H7A 109.5 . . ?
C5 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C5 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C53 C55 H55A 109.5 . . ?
C53 C55 H55B 109.5 . . ?
H55A C55 H55B 109.5 . . ?
C53 C55 H55C 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
C13 C12 C11 119.7(3) . . ?
C13 C12 H12 120.1 . . ?
C11 C12 H12 120.1 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C68 C66 C62 111.8(3) . . ?
C68 C66 C67 108.4(3) . . ?
C62 C66 C67 113.5(3) . . ?
C68 C66 H66 107.6 . . ?
C62 C66 H66 107.6 . . ?
C67 C66 H66 107.6 . . ?
C47 C48 H48A 109.5 . . ?
C47 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C47 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C901 C900 H90H 109.5 . . ?
C901 C900 H90I 109.5 . . ?
H90H C900 H90I 109.5 . . ?
C901 C900 H90J 109.5 . . ?
H90H C900 H90J 109.5 . . ?
H90I C900 H90J 109.5 . . ?
C801 C800 H80C 109.5 . . ?
C801 C800 H80D 109.5 . . ?
H80C C800 H80D 109.5 . . ?
C801 C800 H80E 109.5 . . ?
H80C C800 H80E 109.5 . . ?
H80D C800 H80E 109.5 . . ?
C61 C60 C59 120.1(3) . . ?
C61 C60 H60 119.9 . . ?
C59 C60 H60 119.9 . . ?
O605 C610 C611 108.1(3) . . ?
O605 C610 H61C 110.1 . . ?
C611 C610 H61C 110.1 . . ?
O605 C610 H61D 110.1 . . ?
C611 C610 H61D 110.1 . . ?
H61C C610 H61D 108.4 . . ?
C60 C59 C58 121.0(3) . . ?
C60 C59 H59 119.5 . . ?
C58 C59 H59 119.5 . . ?
C58 C63 C65 114.0(3) . . ?
C58 C63 C64 111.1(3) . . ?
C65 C63 C64 110.2(3) . . ?
C58 C63 H63 107.1 . . ?
C65 C63 H63 107.1 . . ?
C64 C63 H63 107.1 . . ?
C53 C56 H56A 109.5 . . ?
C53 C56 H56B 109.5 . . ?
H56A C56 H56B 109.5 . . ?
C53 C56 H56C 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
C63 C64 H64A 109.5 . . ?
C63 C64 H64B 109.5 . . ?
H64A C64 H64B 109.5 . . ?
C63 C64 H64C 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
C53 C54 H54A 109.5 . . ?
C53 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C53 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C44 C43 C42 121.6(3) . . ?
C44 C43 H43 119.2 . . ?
C42 C43 H43 119.2 . . ?
C59 C58 C57 118.6(3) . . ?
C59 C58 C63 121.6(3) . . ?
C57 C58 C63 119.8(3) . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
O800 C802 C803 108.4(3) . . ?
O800 C802 H80F 110.0 . . ?
C803 C802 H80F 110.0 . . ?
O800 C802 H80G 110.0 . . ?
C803 C802 H80G 110.0 . . ?
H80F C802 H80G 108.4 . . ?

_refine_diff_density_max         2.723
_refine_diff_density_min         -0.522
_refine_diff_density_rms         0.105

####################################################################### 
# 
# 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_U(TDA)4
_database_code_depnum_ccdc_archive 'CCDC 1559385'
_audit_update_record             
;
2018-01-05 deposited with the CCDC.
2018-01-10 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT220_U(TDA)4             
;
PROBLEM: Non-Solvent  Resd 1  C   Ueq(max)/Ueq(min) Range        9.2 Ratio
RESPONSE: The error result from a unresolvable disorder in two of the isopropyl groups of the diisopropylphenyl moieties on the ligand. 
;
_vrf_PLAT230_U(TDA)4             
;
PROBLEM: Hirshfeld Test Diff for   C15      --C17       .        8.7 s.u.
RESPONSE: The error result from a unresolvable disorder in two of the isopropyl groups of the diisopropylphenyl moieties on the ligand. 
;
# Added during the CSD deposition process: Friday 05 January 2018 06:46 PM
# end Validation Reply Form


_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            'C68 H104 N4 O4 U'
_chemical_formula_weight         1279.58

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

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

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

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

_cell_length_a                   13.4219(5)
_cell_length_b                   13.6222(6)
_cell_length_c                   21.0557(9)
_cell_angle_alpha                88.668(2)
_cell_angle_beta                 77.566(2)
_cell_angle_gamma                87.760(2)
_cell_volume                     3756.1(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    12424
_cell_measurement_theta_min      1.50
_cell_measurement_theta_max      25.42

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.131
_exptl_crystal_F_000             1328
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_exptl_absorpt_coefficient_mu    2.202
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.639
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker Quazar'
_diffrn_measurement_method       'omega phi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            98499
_diffrn_reflns_av_unetI/netI     0.0304
_diffrn_reflns_av_R_equivalents  0.0403
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.496
_diffrn_reflns_theta_max         25.417
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             13844
_reflns_number_gt                12424
_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 ApexIII suite, 2016'
_computing_cell_refinement       'Bruker ApexIII suite, 2016'
_computing_data_reduction        'Bruker ApexIII suite, 2016'
_computing_structure_solution    ShelXT
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Diamond 3D'
_computing_publication_material  WinGX
_refine_special_details          SQUEEZE
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0343P)²+4.9941P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         13844
_refine_ls_number_parameters     722
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0355
_refine_ls_R_factor_gt           0.0302
_refine_ls_wR_factor_ref         0.0736
_refine_ls_wR_factor_gt          0.0711
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_restrained_S_all      1.088
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.69186(2) 0.22219(2) 0.70756(2) 0.01868(5) Uani 1 1 d . . . . .
O2 O 0.70770(15) 0.06453(15) 0.66626(10) 0.0219(5) Uani 1 1 d . . . . .
O3 O 0.80884(15) 0.25541(16) 0.61210(11) 0.0251(5) Uani 1 1 d . . . . .
O4 O 0.73073(17) 0.20047(18) 0.80705(11) 0.0293(5) Uani 1 1 d . . . . .
O1 O 0.56398(16) 0.33229(16) 0.69874(11) 0.0280(5) Uani 1 1 d . . . . .
N2 N 0.60318(18) 0.15838(19) 0.62277(12) 0.0191(5) Uani 1 1 d . . . . .
N4 N 0.5755(2) 0.1465(2) 0.81796(13) 0.0286(6) Uani 1 1 d . . . . .
N3 N 0.88377(19) 0.1934(2) 0.68775(13) 0.0236(6) Uani 1 1 d . . . . .
N1 N 0.6826(2) 0.4199(2) 0.72503(15) 0.0329(7) Uani 1 1 d . . . . .
C2 C 0.6527(2) 0.0738(2) 0.62172(14) 0.0196(6) Uani 1 1 d . . . . .
C30 C 0.5634(2) 0.2498(2) 0.52778(15) 0.0249(7) Uani 1 1 d . . . . .
C31 C 0.3896(2) 0.1222(2) 0.67352(15) 0.0240(7) Uani 1 1 d . . . . .
H31 H 0.4492 0.0842 0.6843 0.029 Uiso 1 1 calc R U . . .
C3 C 0.8934(2) 0.2186(2) 0.62643(16) 0.0239(7) Uani 1 1 d . . . . .
C25 C 0.5318(2) 0.1929(2) 0.58522(15) 0.0210(7) Uani 1 1 d . . . . .
C41 C 0.9595(2) 0.1543(3) 0.72110(16) 0.0273(7) Uani 1 1 d . . . . .
C46 C 1.0088(2) 0.2207(3) 0.75385(17) 0.0287(8) Uani 1 1 d . . . . .
C34 C 0.6748(2) 0.2688(3) 0.49791(16) 0.0289(8) Uani 1 1 d . . . . .
H34 H 0.7181 0.2227 0.5190 0.035 Uiso 1 1 calc R U . . .
C57 C 0.4805(2) 0.1033(3) 0.84849(15) 0.0288(8) Uani 1 1 d . . . . .
C32 C 0.3077(2) 0.0492(3) 0.66867(17) 0.0305(8) Uani 1 1 d . . . . .
H32A H 0.2458 0.0852 0.6625 0.046 Uiso 1 1 calc R U . . .
H32B H 0.2920 0.0096 0.7088 0.046 Uiso 1 1 calc R U . . .
H32C H 0.3330 0.0060 0.6316 0.046 Uiso 1 1 calc R U . . .
C37 C 0.9859(2) 0.2077(3) 0.56987(17) 0.0314(8) Uani 1 1 d . . . . .
C29 C 0.4881(3) 0.2937(3) 0.49878(16) 0.0295(8) Uani 1 1 d . . . . .
H29 H 0.5080 0.3322 0.4602 0.035 Uiso 1 1 calc R U . . .
C27 C 0.3563(2) 0.2266(3) 0.58018(16) 0.0286(8) Uani 1 1 d . . . . .
H27 H 0.2856 0.2191 0.5978 0.034 Uiso 1 1 calc R U . . .
C26 C 0.4277(2) 0.1803(2) 0.61127(15) 0.0233(7) Uani 1 1 d . . . . .
C1 C 0.5947(3) 0.4198(2) 0.70920(17) 0.0287(8) Uani 1 1 d . . . . .
C5 C 0.5185(3) 0.5029(3) 0.69752(19) 0.0346(8) Uani 1 1 d . . . . .
C42 C 0.9754(2) 0.0518(3) 0.72799(16) 0.0273(7) Uani 1 1 d . . . . .
C21 C 0.6578(2) -0.0120(2) 0.57502(15) 0.0244(7) Uani 1 1 d . . . . .
C24 C 0.7221(3) -0.0981(2) 0.59554(17) 0.0297(8) Uani 1 1 d . . . . .
H24A H 0.7910 -0.0764 0.5951 0.045 Uiso 1 1 calc R U . . .
H24B H 0.7261 -0.1522 0.5651 0.045 Uiso 1 1 calc R U . . .
H24C H 0.6902 -0.1205 0.6395 0.045 Uiso 1 1 calc R U . . .
C4 C 0.6535(3) 0.1560(3) 0.84427(16) 0.0287(8) Uani 1 1 d . . . . .
C47 C 0.9216(3) -0.0234(3) 0.69571(18) 0.0318(8) Uani 1 1 d . . . . .
H47 H 0.8922 0.0115 0.6613 0.038 Uiso 1 1 calc R U . . .
C33 C 0.3483(3) 0.1933(3) 0.72936(17) 0.0314(8) Uani 1 1 d . . . . .
H33A H 0.4026 0.2364 0.7348 0.047 Uiso 1 1 calc R U . . .
H33B H 0.3247 0.1557 0.7697 0.047 Uiso 1 1 calc R U . . .
H33C H 0.2911 0.2331 0.7192 0.047 Uiso 1 1 calc R U . . .
C28 C 0.3857(3) 0.2826(3) 0.52482(17) 0.0324(8) Uani 1 1 d . . . . .
H28 H 0.3358 0.3136 0.5045 0.039 Uiso 1 1 calc R U . . .
C45 C 1.0712(3) 0.1819(3) 0.79366(17) 0.0342(8) Uani 1 1 d . . . . .
H45 H 1.1043 0.2256 0.8162 0.041 Uiso 1 1 calc R U . . .
C36 C 0.7002(3) 0.3733(3) 0.51078(19) 0.0364(9) Uani 1 1 d . . . . .
H36A H 0.6565 0.4197 0.4920 0.055 Uiso 1 1 calc R U . . .
H36B H 0.7720 0.3843 0.4908 0.055 Uiso 1 1 calc R U . . .
H36C H 0.6886 0.3831 0.5578 0.055 Uiso 1 1 calc R U . . .
C43 C 1.0394(3) 0.0182(3) 0.76863(17) 0.0334(8) Uani 1 1 d . . . . .
H43 H 1.0506 -0.0506 0.7739 0.040 Uiso 1 1 calc R U . . .
C9 C 0.7313(3) 0.5056(3) 0.7413(2) 0.0367(9) Uani 1 1 d . . . . .
C53 C 0.6747(3) 0.1221(3) 0.91051(17) 0.0356(9) Uani 1 1 d . . . . .
C23 C 0.5508(3) -0.0467(3) 0.57397(17) 0.0311(8) Uani 1 1 d . . . . .
H23A H 0.5176 -0.0695 0.6176 0.047 Uiso 1 1 calc R U . . .
H23B H 0.5564 -0.1007 0.5433 0.047 Uiso 1 1 calc R U . . .
H23C H 0.5102 0.0079 0.5603 0.047 Uiso 1 1 calc R U . . .
C50 C 0.9926(3) 0.3308(3) 0.74799(19) 0.0353(9) Uani 1 1 d . . . . .
H50 H 0.9582 0.3442 0.7108 0.042 Uiso 1 1 calc R U . . .
C48 C 0.8340(3) -0.0662(3) 0.7457(2) 0.0404(9) Uani 1 1 d . . . . .
H48A H 0.8608 -0.0981 0.7810 0.061 Uiso 1 1 calc R U . . .
H48B H 0.8000 -0.1146 0.7248 0.061 Uiso 1 1 calc R U . . .
H48C H 0.7849 -0.0133 0.7633 0.061 Uiso 1 1 calc R U . . .
C60 C 0.2923(3) 0.0234(3) 0.90262(17) 0.0380(9) Uani 1 1 d . . . . .
H60 H 0.2285 -0.0040 0.9217 0.046 Uiso 1 1 calc R U . . .
C44 C 1.0867(3) 0.0826(3) 0.80147(17) 0.0351(9) Uani 1 1 d . . . . .
H44 H 1.1296 0.0583 0.8292 0.042 Uiso 1 1 calc R U . . .
C14 C 0.8088(3) 0.5490(3) 0.6947(2) 0.0428(10) Uani 1 1 d . . . . .
C22 C 0.7090(3) 0.0211(3) 0.50604(16) 0.0338(8) Uani 1 1 d . . . . .
H22A H 0.6640 0.0690 0.4896 0.051 Uiso 1 1 calc R U . . .
H22B H 0.7220 -0.0359 0.4775 0.051 Uiso 1 1 calc R U . . .
H22C H 0.7738 0.0513 0.5069 0.051 Uiso 1 1 calc R U . . .
C59 C 0.3082(3) 0.1198(3) 0.91063(18) 0.0448(10) Uani 1 1 d . . . . .
H59 H 0.2543 0.1594 0.9351 0.054 Uiso 1 1 calc R U . . .
C39 C 1.0810(3) 0.2511(4) 0.5852(2) 0.0470(11) Uani 1 1 d . . . . .
H39A H 1.0666 0.3202 0.5971 0.070 Uiso 1 1 calc R U . . .
H39B H 1.1372 0.2467 0.5469 0.070 Uiso 1 1 calc R U . . .
H39C H 1.1003 0.2144 0.6216 0.070 Uiso 1 1 calc R U . . .
C62 C 0.4646(3) 0.0045(3) 0.83880(18) 0.0364(9) Uani 1 1 d . . . . .
C61 C 0.3696(3) -0.0337(3) 0.86654(19) 0.0396(9) Uani 1 1 d . . . . .
H61 H 0.3583 -0.1008 0.8603 0.048 Uiso 1 1 calc R U . . .
C58 C 0.4007(3) 0.1624(3) 0.88418(19) 0.0435(10) Uani 1 1 d . . . . .
C35 C 0.7019(3) 0.2508(3) 0.42416(17) 0.0413(9) Uani 1 1 d . . . . .
H35A H 0.6679 0.3016 0.4018 0.062 Uiso 1 1 calc R U . . .
H35B H 0.6790 0.1860 0.4154 0.062 Uiso 1 1 calc R U . . .
H35C H 0.7760 0.2534 0.4084 0.062 Uiso 1 1 calc R U . . .
C38 C 0.9622(3) 0.2595(3) 0.50921(18) 0.0453(10) Uani 1 1 d . . . . .
H38A H 0.9468 0.3294 0.5181 0.068 Uiso 1 1 calc R U . . .
H38B H 0.9032 0.2298 0.4977 0.068 Uiso 1 1 calc R U . . .
H38C H 1.0215 0.2524 0.4730 0.068 Uiso 1 1 calc R U . . .
C7 C 0.4178(3) 0.4844(3) 0.7455(2) 0.0423(10) Uani 1 1 d . . . . .
H7A H 0.4284 0.4862 0.7901 0.063 Uiso 1 1 calc R U . . .
H7B H 0.3936 0.4198 0.7376 0.063 Uiso 1 1 calc R U . . .
H7C H 0.3668 0.5353 0.7397 0.063 Uiso 1 1 calc R U . . .
C51 C 0.9216(3) 0.3704(3) 0.8099(2) 0.0457(10) Uani 1 1 d . . . . .
H51A H 0.8528 0.3467 0.8130 0.069 Uiso 1 1 calc R U . . .
H51B H 0.9195 0.4424 0.8082 0.069 Uiso 1 1 calc R U . . .
H51C H 0.9474 0.3475 0.8480 0.069 Uiso 1 1 calc R U . . .
C13 C 0.8567(4) 0.6293(3) 0.7133(3) 0.0549(12) Uani 1 1 d . . . . .
H13 H 0.9083 0.6602 0.6821 0.066 Uiso 1 1 calc R U . . .
C54 C 0.7684(4) 0.0520(3) 0.8981(2) 0.0528(11) Uani 1 1 d . . . . .
H54A H 0.7528 -0.0074 0.8773 0.079 Uiso 1 1 calc R U . . .
H54B H 0.7869 0.0341 0.9395 0.079 Uiso 1 1 calc R U . . .
H54C H 0.8256 0.0843 0.8695 0.079 Uiso 1 1 calc R U . . .
C8 C 0.5497(3) 0.6081(3) 0.7041(3) 0.0586(13) Uani 1 1 d . . . . .
H8A H 0.4988 0.6541 0.6920 0.088 Uiso 1 1 calc R U . . .
H8B H 0.6164 0.6184 0.6753 0.088 Uiso 1 1 calc R U . . .
H8C H 0.5540 0.6192 0.7492 0.088 Uiso 1 1 calc R U . . .
C49 C 0.9938(3) -0.1067(3) 0.6635(2) 0.0509(11) Uani 1 1 d . . . . .
H49A H 1.0159 -0.1477 0.6971 0.076 Uiso 1 1 calc R U . . .
H49B H 1.0535 -0.0787 0.6346 0.076 Uiso 1 1 calc R U . . .
H49C H 0.9580 -0.1468 0.6381 0.076 Uiso 1 1 calc R U . . .
C10 C 0.7065(3) 0.5405(3) 0.8048(2) 0.0518(11) Uani 1 1 d . . . . .
C12 C 0.8315(3) 0.6648(3) 0.7751(3) 0.0577(13) Uani 1 1 d . . . . .
H12 H 0.8649 0.7201 0.7863 0.069 Uiso 1 1 calc R U . . .
C66 C 0.5453(3) -0.0643(3) 0.8001(3) 0.0642(16) Uani 1 1 d . . . . .
H66 H 0.6033 -0.0245 0.7766 0.077 Uiso 1 1 calc R U . . .
C6 C 0.4987(3) 0.4912(3) 0.6287(2) 0.0482(10) Uani 1 1 d . . . . .
H6A H 0.4809 0.4233 0.6231 0.072 Uiso 1 1 calc R U . . .
H6B H 0.5604 0.5070 0.5963 0.072 Uiso 1 1 calc R U . . .
H6C H 0.4422 0.5359 0.6229 0.072 Uiso 1 1 calc R U . . .
C40 C 1.0085(3) 0.0990(3) 0.5547(2) 0.0566(12) Uani 1 1 d . . . . .
H40A H 1.0605 0.0926 0.5143 0.085 Uiso 1 1 calc R U . . .
H40B H 0.9459 0.0684 0.5495 0.085 Uiso 1 1 calc R U . . .
H40C H 1.0335 0.0663 0.5904 0.085 Uiso 1 1 calc R U . . .
C55 C 0.5879(4) 0.0721(4) 0.9570(2) 0.0623(14) Uani 1 1 d . . . . .
H55A H 0.5292 0.1183 0.9681 0.094 Uiso 1 1 calc R U . . .
H55B H 0.6104 0.0513 0.9966 0.094 Uiso 1 1 calc R U . . .
H55C H 0.5683 0.0146 0.9360 0.094 Uiso 1 1 calc R U . . .
C11 C 0.7586(4) 0.6208(3) 0.8206(3) 0.0569(13) Uani 1 1 d . . . . .
H11 H 0.7427 0.6447 0.8638 0.068 Uiso 1 1 calc R U . . .
C20 C 0.9585(4) 0.5094(4) 0.6023(2) 0.0650(14) Uani 1 1 d . . . . .
H20A H 0.9836 0.5764 0.5987 0.098 Uiso 1 1 calc R U . . .
H20B H 0.9774 0.4781 0.5598 0.098 Uiso 1 1 calc R U . . .
H20C H 0.9891 0.4715 0.6338 0.098 Uiso 1 1 calc R U . . .
C18 C 0.8430(4) 0.5131(3) 0.6250(2) 0.0535(12) Uani 1 1 d . . . . .
H18 H 0.8187 0.4449 0.6237 0.064 Uiso 1 1 calc R U . . .
C52 C 1.0938(3) 0.3848(3) 0.7337(2) 0.0497(11) Uani 1 1 d . . . . .
H52A H 1.1272 0.3756 0.7706 0.075 Uiso 1 1 calc R U . . .
H52B H 1.0801 0.4550 0.7270 0.075 Uiso 1 1 calc R U . . .
H52C H 1.1386 0.3581 0.6944 0.075 Uiso 1 1 calc R U . . .
C56 C 0.7045(5) 0.2124(3) 0.9436(2) 0.0652(14) Uani 1 1 d . . . . .
H56A H 0.7623 0.2433 0.9148 0.098 Uiso 1 1 calc R U . . .
H56B H 0.7238 0.1920 0.9844 0.098 Uiso 1 1 calc R U . . .
H56C H 0.6463 0.2595 0.9529 0.098 Uiso 1 1 calc R U . . .
C19 C 0.7964(4) 0.5773(4) 0.5775(2) 0.0657(14) Uani 1 1 d . . . . .
H19A H 0.8073 0.6466 0.5843 0.099 Uiso 1 1 calc R U . . .
H19B H 0.7230 0.5665 0.5849 0.099 Uiso 1 1 calc R U . . .
H19C H 0.8290 0.5597 0.5328 0.099 Uiso 1 1 calc R U . . .
C68 C 0.5866(4) -0.1398(4) 0.8446(3) 0.083(2) Uani 1 1 d . . . . .
H68A H 0.5317 -0.1826 0.8655 0.125 Uiso 1 1 calc R U . . .
H68B H 0.6119 -0.1052 0.8779 0.125 Uiso 1 1 calc R U . . .
H68C H 0.6425 -0.1794 0.8185 0.125 Uiso 1 1 calc R U . . .
C67 C 0.5045(5) -0.1207(4) 0.7506(2) 0.091(2) Uani 1 1 d . . . . .
H67A H 0.4552 -0.1679 0.7731 0.137 Uiso 1 1 calc R U . . .
H67B H 0.5610 -0.1559 0.7218 0.137 Uiso 1 1 calc R U . . .
H67C H 0.4708 -0.0747 0.7248 0.137 Uiso 1 1 calc R U . . .
C15 C 0.6254(4) 0.4980(4) 0.8573(3) 0.0717(14) Uani 1 1 d . U . . .
H15 H 0.5966 0.4408 0.8394 0.086 Uiso 1 1 calc R U . . .
C17 C 0.6736(5) 0.4618(5) 0.9124(3) 0.0873(17) Uani 1 1 d . U . . .
H17A H 0.7230 0.4080 0.8972 0.131 Uiso 1 1 calc R U . . .
H17B H 0.6205 0.4381 0.9484 0.131 Uiso 1 1 calc R U . . .
H17C H 0.7085 0.5157 0.9274 0.131 Uiso 1 1 calc R U . . .
C64 C 0.3175(6) 0.3322(4) 0.8788(2) 0.088(2) Uani 1 1 d . . . . .
H64A H 0.3080 0.3169 0.8352 0.132 Uiso 1 1 calc R U . . .
H64B H 0.3290 0.4025 0.8810 0.132 Uiso 1 1 calc R U . . .
H64C H 0.2562 0.3152 0.9112 0.132 Uiso 1 1 calc R U . . .
C16 C 0.5373(4) 0.5720(6) 0.8846(3) 0.098(2) Uani 1 1 d . . . . .
H16A H 0.5640 0.6264 0.9048 0.147 Uiso 1 1 calc R U . . .
H16B H 0.4855 0.5390 0.9171 0.147 Uiso 1 1 calc R U . . .
H16C H 0.5066 0.5976 0.8490 0.147 Uiso 1 1 calc R U . . .
C63 C 0.4089(4) 0.2734(5) 0.8926(3) 0.101(3) Uani 1 1 d . . . . .
H63 H 0.4725 0.2966 0.8630 0.121 Uiso 1 1 calc R U . . .
C65 C 0.4132(7) 0.2935(7) 0.9641(5) 0.181(5) Uani 1 1 d . . . . .
H65A H 0.4251 0.3632 0.9687 0.272 Uiso 1 1 calc R U . . .
H65B H 0.4688 0.2535 0.9761 0.272 Uiso 1 1 calc R U . . .
H65C H 0.3482 0.2765 0.9928 0.272 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 O1 2.270(2) . ?
U1 O4 2.276(2) . ?
U1 O3 2.316(2) . ?
U1 O2 2.321(2) . ?
U1 N2 2.535(2) . ?
U1 N3 2.535(2) . ?
U1 N4 2.713(3) . ?
U1 N1 2.721(3) . ?
U1 C3 2.870(3) . ?
U1 C2 2.879(3) . ?
U1 C4 2.940(3) . ?
U1 C1 2.943(3) . ?
O2 C2 1.314(4) . ?
O3 C3 1.313(4) . ?
O4 C4 1.317(4) . ?
O1 C1 1.315(4) . ?
N2 C2 1.305(4) . ?
N2 C25 1.428(4) . ?
N4 C4 1.297(4) . ?
N4 C57 1.440(4) . ?
N3 C3 1.309(4) . ?
N3 C41 1.434(4) . ?
N1 C1 1.293(4) . ?
N1 C9 1.443(4) . ?
C2 C21 1.536(4) . ?
C30 C29 1.398(5) . ?
C30 C25 1.415(5) . ?
C30 C34 1.522(4) . ?
C31 C26 1.516(5) . ?
C31 C32 1.532(4) . ?
C31 C33 1.535(4) . ?
C31 H31 1.0000 . ?
C3 C37 1.529(4) . ?
C25 C26 1.403(4) . ?
C41 C42 1.414(5) . ?
C41 C46 1.415(5) . ?
C46 C45 1.390(5) . ?
C46 C50 1.513(5) . ?
C34 C36 1.520(5) . ?
C34 C35 1.540(5) . ?
C34 H34 1.0000 . ?
C57 C62 1.398(5) . ?
C57 C58 1.404(5) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C37 C39 1.527(5) . ?
C37 C40 1.527(6) . ?
C37 C38 1.532(5) . ?
C29 C28 1.378(5) . ?
C29 H29 0.9500 . ?
C27 C28 1.372(5) . ?
C27 C26 1.395(4) . ?
C27 H27 0.9500 . ?
C1 C5 1.547(5) . ?
C5 C8 1.526(5) . ?
C5 C7 1.529(5) . ?
C5 C6 1.541(6) . ?
C42 C43 1.395(5) . ?
C42 C47 1.527(5) . ?
C21 C22 1.533(5) . ?
C21 C23 1.534(4) . ?
C21 C24 1.538(5) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C4 C53 1.540(5) . ?
C47 C48 1.524(5) . ?
C47 C49 1.534(5) . ?
C47 H47 1.0000 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C28 H28 0.9500 . ?
C45 C44 1.372(5) . ?
C45 H45 0.9500 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C43 C44 1.383(5) . ?
C43 H43 0.9500 . ?
C9 C10 1.398(6) . ?
C9 C14 1.406(6) . ?
C53 C55 1.523(6) . ?
C53 C54 1.529(6) . ?
C53 C56 1.535(6) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C50 C51 1.535(5) . ?
C50 C52 1.539(5) . ?
C50 H50 1.0000 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C60 C59 1.358(6) . ?
C60 C61 1.373(5) . ?
C60 H60 0.9500 . ?
C44 H44 0.9500 . ?
C14 C13 1.394(5) . ?
C14 C18 1.526(6) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C59 C58 1.390(6) . ?
C59 H59 0.9500 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C62 C61 1.397(5) . ?
C62 C66 1.514(5) . ?
C61 H61 0.9500 . ?
C58 C63 1.538(7) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C51 H51A 0.9800 . ?
C51 H51B 0.9800 . ?
C51 H51C 0.9800 . ?
C13 C12 1.368(7) . ?
C13 H13 0.9500 . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?
C10 C11 1.404(6) . ?
C10 C15 1.499(7) . ?
C12 C11 1.361(7) . ?
C12 H12 0.9500 . ?
C66 C67 1.514(8) . ?
C66 C68 1.540(7) . ?
C66 H66 1.0000 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C55 H55A 0.9800 . ?
C55 H55B 0.9800 . ?
C55 H55C 0.9800 . ?
C11 H11 0.9500 . ?
C20 C18 1.520(7) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C18 C19 1.532(6) . ?
C18 H18 1.0000 . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C56 H56A 0.9800 . ?
C56 H56B 0.9800 . ?
C56 H56C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C68 H68A 0.9800 . ?
C68 H68B 0.9800 . ?
C68 H68C 0.9800 . ?
C67 H67A 0.9800 . ?
C67 H67B 0.9800 . ?
C67 H67C 0.9800 . ?
C15 C17 1.509(8) . ?
C15 C16 1.544(8) . ?
C15 H15 1.0000 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C64 C63 1.516(9) . ?
C64 H64A 0.9800 . ?
C64 H64B 0.9800 . ?
C64 H64C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C63 C65 1.551(10) . ?
C63 H63 1.0000 . ?
C65 H65A 0.9800 . ?
C65 H65B 0.9800 . ?
C65 H65C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 U1 O4 117.67(8) . . ?
O1 U1 O3 100.67(8) . . ?
O4 U1 O3 124.91(8) . . ?
O1 U1 O2 124.40(7) . . ?
O4 U1 O2 103.38(8) . . ?
O3 U1 O2 82.66(8) . . ?
O1 U1 N2 72.73(8) . . ?
O4 U1 N2 147.68(8) . . ?
O3 U1 N2 78.36(8) . . ?
O2 U1 N2 53.42(8) . . ?
O1 U1 N3 145.03(8) . . ?
O4 U1 N3 73.41(8) . . ?
O3 U1 N3 53.60(8) . . ?
O2 U1 N3 79.61(8) . . ?
N2 U1 N3 116.90(8) . . ?
O1 U1 N4 90.28(8) . . ?
O4 U1 N4 51.45(8) . . ?
O3 U1 N4 168.13(8) . . ?
O2 U1 N4 87.39(8) . . ?
N2 U1 N4 100.83(8) . . ?
N3 U1 N4 118.21(9) . . ?
O1 U1 N1 51.26(8) . . ?
O4 U1 N1 89.27(9) . . ?
O3 U1 N1 85.41(9) . . ?
O2 U1 N1 166.12(8) . . ?
N2 U1 N1 117.04(9) . . ?
N3 U1 N1 98.93(8) . . ?
N4 U1 N1 105.21(9) . . ?
O1 U1 C3 125.37(9) . . ?
O4 U1 C3 100.13(9) . . ?
O3 U1 C3 26.70(8) . . ?
O2 U1 C3 77.52(8) . . ?
N2 U1 C3 96.17(8) . . ?
N3 U1 C3 27.13(9) . . ?
N4 U1 C3 143.83(9) . . ?
N1 U1 C3 94.82(9) . . ?
O1 U1 C2 99.27(8) . . ?
O4 U1 C2 127.90(9) . . ?
O3 U1 C2 77.43(8) . . ?
O2 U1 C2 26.60(8) . . ?
N2 U1 C2 26.95(8) . . ?
N3 U1 C2 97.25(8) . . ?
N4 U1 C2 96.42(8) . . ?
N1 U1 C2 142.45(9) . . ?
C3 U1 C2 84.62(8) . . ?
O1 U1 C4 106.65(9) . . ?
O4 U1 C4 25.40(9) . . ?
O3 U1 C4 148.40(8) . . ?
O2 U1 C4 94.51(8) . . ?
N2 U1 C4 124.70(9) . . ?
N3 U1 C4 94.86(9) . . ?
N4 U1 C4 26.14(9) . . ?
N1 U1 C4 99.37(9) . . ?
C3 U1 C4 121.94(9) . . ?
C2 U1 C4 112.74(9) . . ?
O1 U1 C1 25.26(8) . . ?
O4 U1 C1 105.49(9) . . ?
O3 U1 C1 92.57(9) . . ?
O2 U1 C1 147.63(8) . . ?
N2 U1 C1 94.23(9) . . ?
N3 U1 C1 122.68(9) . . ?
N4 U1 C1 99.30(9) . . ?
N1 U1 C1 26.02(9) . . ?
C3 U1 C1 111.07(9) . . ?
C2 U1 C1 121.13(9) . . ?
C4 U1 C1 105.41(10) . . ?
C2 O2 U1 101.13(18) . . ?
C3 O3 U1 100.90(19) . . ?
C4 O4 U1 106.78(19) . . ?
C1 O1 U1 107.30(19) . . ?
C2 N2 C25 129.8(3) . . ?
C2 N2 U1 91.37(18) . . ?
C25 N2 U1 138.73(19) . . ?
C4 N4 C57 126.0(3) . . ?
C4 N4 U1 86.7(2) . . ?
C57 N4 U1 147.1(2) . . ?
C3 N3 C41 129.3(3) . . ?
C3 N3 U1 90.84(18) . . ?
C41 N3 U1 139.4(2) . . ?
C1 N1 C9 125.5(3) . . ?
C1 N1 U1 86.6(2) . . ?
C9 N1 U1 147.9(2) . . ?
N2 C2 O2 113.6(3) . . ?
N2 C2 C21 129.2(3) . . ?
O2 C2 C21 117.2(3) . . ?
N2 C2 U1 61.68(15) . . ?
O2 C2 U1 52.27(14) . . ?
C21 C2 U1 166.8(2) . . ?
C29 C30 C25 118.1(3) . . ?
C29 C30 C34 118.6(3) . . ?
C25 C30 C34 123.2(3) . . ?
C26 C31 C32 113.9(3) . . ?
C26 C31 C33 109.5(3) . . ?
C32 C31 C33 109.6(3) . . ?
C26 C31 H31 107.9 . . ?
C32 C31 H31 107.9 . . ?
C33 C31 H31 107.9 . . ?
N3 C3 O3 113.8(3) . . ?
N3 C3 C37 129.7(3) . . ?
O3 C3 C37 116.5(3) . . ?
N3 C3 U1 62.03(16) . . ?
O3 C3 U1 52.40(14) . . ?
C37 C3 U1 164.9(2) . . ?
C26 C25 C30 120.4(3) . . ?
C26 C25 N2 118.0(3) . . ?
C30 C25 N2 121.1(3) . . ?
C42 C41 C46 120.5(3) . . ?
C42 C41 N3 120.9(3) . . ?
C46 C41 N3 118.1(3) . . ?
C45 C46 C41 118.0(3) . . ?
C45 C46 C50 120.1(3) . . ?
C41 C46 C50 121.8(3) . . ?
C36 C34 C30 110.7(3) . . ?
C36 C34 C35 109.3(3) . . ?
C30 C34 C35 112.4(3) . . ?
C36 C34 H34 108.1 . . ?
C30 C34 H34 108.1 . . ?
C35 C34 H34 108.1 . . ?
C62 C57 C58 119.7(3) . . ?
C62 C57 N4 120.3(3) . . ?
C58 C57 N4 119.8(3) . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C39 C37 C40 108.5(3) . . ?
C39 C37 C3 112.0(3) . . ?
C40 C37 C3 109.6(3) . . ?
C39 C37 C38 109.0(3) . . ?
C40 C37 C38 108.1(3) . . ?
C3 C37 C38 109.5(3) . . ?
C28 C29 C30 121.5(3) . . ?
C28 C29 H29 119.2 . . ?
C30 C29 H29 119.2 . . ?
C28 C27 C26 121.6(3) . . ?
C28 C27 H27 119.2 . . ?
C26 C27 H27 119.2 . . ?
C27 C26 C25 118.6(3) . . ?
C27 C26 C31 118.8(3) . . ?
C25 C26 C31 122.6(3) . . ?
N1 C1 O1 114.7(3) . . ?
N1 C1 C5 133.0(3) . . ?
O1 C1 C5 112.3(3) . . ?
N1 C1 U1 67.37(18) . . ?
O1 C1 U1 47.44(15) . . ?
C5 C1 U1 159.1(2) . . ?
C8 C5 C7 109.6(3) . . ?
C8 C5 C6 108.5(4) . . ?
C7 C5 C6 106.9(3) . . ?
C8 C5 C1 116.7(3) . . ?
C7 C5 C1 106.6(3) . . ?
C6 C5 C1 108.1(3) . . ?
C43 C42 C41 118.2(3) . . ?
C43 C42 C47 118.8(3) . . ?
C41 C42 C47 122.9(3) . . ?
C22 C21 C23 108.5(3) . . ?
C22 C21 C2 109.3(3) . . ?
C23 C21 C2 111.3(3) . . ?
C22 C21 C24 108.3(3) . . ?
C23 C21 C24 109.5(3) . . ?
C2 C21 C24 109.8(3) . . ?
C21 C24 H24A 109.5 . . ?
C21 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C21 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
N4 C4 O4 114.6(3) . . ?
N4 C4 C53 132.2(3) . . ?
O4 C4 C53 113.1(3) . . ?
N4 C4 U1 67.11(18) . . ?
O4 C4 U1 47.83(15) . . ?
C53 C4 U1 159.7(2) . . ?
C48 C47 C42 109.8(3) . . ?
C48 C47 C49 109.7(3) . . ?
C42 C47 C49 113.0(3) . . ?
C48 C47 H47 108.1 . . ?
C42 C47 H47 108.1 . . ?
C49 C47 H47 108.1 . . ?
C31 C33 H33A 109.5 . . ?
C31 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C31 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C27 C28 C29 119.6(3) . . ?
C27 C28 H28 120.2 . . ?
C29 C28 H28 120.2 . . ?
C44 C45 C46 122.2(3) . . ?
C44 C45 H45 118.9 . . ?
C46 C45 H45 118.9 . . ?
C34 C36 H36A 109.5 . . ?
C34 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C34 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C44 C43 C42 121.5(3) . . ?
C44 C43 H43 119.2 . . ?
C42 C43 H43 119.2 . . ?
C10 C9 C14 120.1(3) . . ?
C10 C9 N1 119.7(4) . . ?
C14 C9 N1 120.0(3) . . ?
C55 C53 C54 108.7(4) . . ?
C55 C53 C56 109.0(4) . . ?
C54 C53 C56 106.5(4) . . ?
C55 C53 C4 116.2(3) . . ?
C54 C53 C4 108.2(3) . . ?
C56 C53 C4 107.8(3) . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C46 C50 C51 110.3(3) . . ?
C46 C50 C52 112.3(3) . . ?
C51 C50 C52 110.4(3) . . ?
C46 C50 H50 107.9 . . ?
C51 C50 H50 107.9 . . ?
C52 C50 H50 107.9 . . ?
C47 C48 H48A 109.5 . . ?
C47 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C47 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C59 C60 C61 119.0(4) . . ?
C59 C60 H60 120.5 . . ?
C61 C60 H60 120.5 . . ?
C45 C44 C43 119.4(3) . . ?
C45 C44 H44 120.3 . . ?
C43 C44 H44 120.3 . . ?
C13 C14 C9 118.2(4) . . ?
C13 C14 C18 118.4(4) . . ?
C9 C14 C18 123.4(3) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C60 C59 C58 122.2(4) . . ?
C60 C59 H59 118.9 . . ?
C58 C59 H59 118.9 . . ?
C37 C39 H39A 109.5 . . ?
C37 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C37 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C61 C62 C57 118.7(3) . . ?
C61 C62 C66 117.9(4) . . ?
C57 C62 C66 123.5(3) . . ?
C60 C61 C62 121.7(4) . . ?
C60 C61 H61 119.2 . . ?
C62 C61 H61 119.2 . . ?
C59 C58 C57 118.7(4) . . ?
C59 C58 C63 118.2(4) . . ?
C57 C58 C63 123.1(4) . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C5 C7 H7A 109.5 . . ?
C5 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C5 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C50 C51 H51A 109.5 . . ?
C50 C51 H51B 109.5 . . ?
H51A C51 H51B 109.5 . . ?
C50 C51 H51C 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
C12 C13 C14 121.9(5) . . ?
C12 C13 H13 119.1 . . ?
C14 C13 H13 119.1 . . ?
C53 C54 H54A 109.5 . . ?
C53 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C53 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C5 C8 H8A 109.5 . . ?
C5 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C5 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C47 C49 H49A 109.5 . . ?
C47 C49 H49B 109.5 . . ?
H49A C49 H49B 109.5 . . ?
C47 C49 H49C 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
C9 C10 C11 118.9(4) . . ?
C9 C10 C15 123.4(4) . . ?
C11 C10 C15 117.7(4) . . ?
C11 C12 C13 119.9(4) . . ?
C11 C12 H12 120.1 . . ?
C13 C12 H12 120.1 . . ?
C67 C66 C62 111.8(4) . . ?
C67 C66 C68 107.8(4) . . ?
C62 C66 C68 111.6(4) . . ?
C67 C66 H66 108.5 . . ?
C62 C66 H66 108.5 . . ?
C68 C66 H66 108.5 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C37 C40 H40A 109.5 . . ?
C37 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C37 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C53 C55 H55A 109.5 . . ?
C53 C55 H55B 109.5 . . ?
H55A C55 H55B 109.5 . . ?
C53 C55 H55C 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
C12 C11 C10 121.0(4) . . ?
C12 C11 H11 119.5 . . ?
C10 C11 H11 119.5 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C20 C18 C14 112.2(4) . . ?
C20 C18 C19 109.1(4) . . ?
C14 C18 C19 111.6(4) . . ?
C20 C18 H18 107.9 . . ?
C14 C18 H18 107.9 . . ?
C19 C18 H18 107.9 . . ?
C50 C52 H52A 109.5 . . ?
C50 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C50 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C53 C56 H56A 109.5 . . ?
C53 C56 H56B 109.5 . . ?
H56A C56 H56B 109.5 . . ?
C53 C56 H56C 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C66 C68 H68A 109.5 . . ?
C66 C68 H68B 109.5 . . ?
H68A C68 H68B 109.5 . . ?
C66 C68 H68C 109.5 . . ?
H68A C68 H68C 109.5 . . ?
H68B C68 H68C 109.5 . . ?
C66 C67 H67A 109.5 . . ?
C66 C67 H67B 109.5 . . ?
H67A C67 H67B 109.5 . . ?
C66 C67 H67C 109.5 . . ?
H67A C67 H67C 109.5 . . ?
H67B C67 H67C 109.5 . . ?
C10 C15 C17 108.7(5) . . ?
C10 C15 C16 113.5(5) . . ?
C17 C15 C16 108.6(5) . . ?
C10 C15 H15 108.7 . . ?
C17 C15 H15 108.7 . . ?
C16 C15 H15 108.7 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C63 C64 H64A 109.5 . . ?
C63 C64 H64B 109.5 . . ?
H64A C64 H64B 109.5 . . ?
C63 C64 H64C 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C64 C63 C58 112.6(5) . . ?
C64 C63 C65 106.7(4) . . ?
C58 C63 C65 109.2(7) . . ?
C64 C63 H63 109.4 . . ?
C58 C63 H63 109.4 . . ?
C65 C63 H63 109.4 . . ?
C63 C65 H65A 109.5 . . ?
C63 C65 H65B 109.5 . . ?
H65A C65 H65B 109.5 . . ?
C63 C65 H65C 109.5 . . ?
H65A C65 H65C 109.5 . . ?
H65B C65 H65C 109.5 . . ?

_refine_diff_density_max         2.863
_refine_diff_density_min         -0.999
_refine_diff_density_rms         0.084



