# Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 1999
# CCDC Number: 186/1615


# Article submitted to J. Chem. Soc., Dalton Trans.
# 'An unprecedented trigonal coordination geometry
# for the uranyl ion in its complex with
# p-tert-butylhexahomotrioxacalix[3]arene.'
#
data_global

_publ_contact_author
;
      Pierre Thu\'ery
      CEA / Saclay, SCM (CNRS URA 331)
      B\^at. 125
      91191 Gif-sur-Yvette
      France
;
_publ_contact_author_phone        '16(1)69 08 63 29'
_publ_contact_author_fax             '16(1)69 08 66 40'
_publ_contact_author_email          thuery@drecam.cea.fr
_publ_requested_journal               'J. Chem. Soc., Dalton Trans.'

data_1 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic         ?
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum             'C42 H67 N O11 U' 
_chemical_formula_weight          1000.00 
 
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' 
 
_symmetry_cell_setting            monoclinic 
_symmetry_space_group_name_H-M    P2(1)/c 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, y+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x, -y-1/2, z-1/2' 
 
_cell_length_a                    16.464(3) 
_cell_length_b                    14.203(2) 
_cell_length_c                    19.590(2) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  91.844(9) 
_cell_angle_gamma                 90.00 
_cell_volume                      4579(4) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     270(2) 
_cell_measurement_reflns_used     21286 
_cell_measurement_theta_min       3.49 
_cell_measurement_theta_max       23.25
 
_exptl_crystal_description        platelet 
_exptl_crystal_colour             'translucent dark orange'
_exptl_crystal_size_max           0.32
_exptl_crystal_size_mid           0.25
_exptl_crystal_size_min           0.10
_exptl_crystal_density_meas       'not measured' 
_exptl_crystal_density_diffrn     1.451 
_exptl_crystal_density_method     ? 
_exptl_crystal_F_000              2024 
_exptl_absorpt_coefficient_mu     3.600 
_exptl_absorpt_correction_type    empirical 
_exptl_absorpt_correction_T_min   0.303 
_exptl_absorpt_correction_T_max   0.371
_exptl_absorpt_process_details    'MULABS (Spek, 1997)' 
_exptl_special_details            ?
 
_diffrn_ambient_temperature       270(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   'Nonius Kappa-CCD' 
_diffrn_measurement_method        'area detector' 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_decay_%         none
_diffrn_reflns_number             21286 
_diffrn_reflns_av_R_equivalents   0.085 
_diffrn_reflns_av_sigmaI/netI     0.087 
_diffrn_reflns_limit_h_min        -18 
_diffrn_reflns_limit_h_max        18 
_diffrn_reflns_limit_k_min        -15 
_diffrn_reflns_limit_k_max        14 
_diffrn_reflns_limit_l_min        -21 
_diffrn_reflns_limit_l_max        21 
_diffrn_reflns_theta_min          3.49 
_diffrn_reflns_theta_max          23.25 
_reflns_number_total              6299 
_reflns_number_gt                 3733 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        'Kappa-CCD software (Nonius, 1997)' 
_computing_cell_refinement        'HKL package (Otwinowski & Minor, 1997)' 
_computing_data_reduction         'HKL package (Otwinowski & Minor, 1997)' 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     'SHELXTL (Sheldrick, 1999)' 
_computing_publication_material   'SHELXTL (Sheldrick, 1999)' 
 
_refine_special_details 
;
 Structure solved by direct methods. All non-hydrogen atoms refined 
 anisotropically. One aromatic ring refined as an idealized hexagon.
 Hydrogen atoms introduced at calculated positions
 (except for water molecules and nitrogen atom of triethylammonium
 cation) as riding atoms with a displacement parameter equal to 1.2 
 (CH, CH2) or 1.5 (CH3) times that of the parent atom. Highest residual 
 electron density peaks located near uranium atom. 
 Refinement of F^2^ against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F^2^, conventional R-factors R are based 
 on F, with F set to zero for negative F^2^. The threshold expression of 
 F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F^2^ are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;  
_refine_ls_structure_factor_coef  Fsqd  
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme       calc  
_refine_ls_weighting_details 
 'calc w=1/[\s^2^(Fo^2^)+(0.0716P)^2^+20.3268P] where P=(Fo^2^+2Fc^2^)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     mixed 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          6299 
_refine_ls_number_parameters      496 
_refine_ls_number_restraints      138 
_refine_ls_R_factor_all           0.1384 
_refine_ls_R_factor_gt            0.0816 
_refine_ls_wR_factor_ref          0.2008 
_refine_ls_wR_factor_gt           0.1720 
_refine_ls_goodness_of_fit_ref    1.078 
_refine_ls_restrained_S_all       1.082 
_refine_ls_shift/su_max           0.000 
_refine_ls_shift/su_mean          0.000 
_diffrn_measured_fraction_theta_max    0.959 
_diffrn_reflns_theta_full              23.25 
_diffrn_measured_fraction_theta_full   0.959 
_refine_diff_density_max    3.319 
_refine_diff_density_min   -0.834 
_refine_diff_density_rms    0.111 
 
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_symmetry_multiplicity 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_assembly 
 _atom_site_disorder_group 
U U 0.24129(4) 0.24209(3) 0.21061(3) 0.0824(3) Uani 1 1 d D . . 
O1 O 0.1256(7) 0.1679(7) 0.2307(5) 0.094(3) Uani 1 1 d . . . 
O2 O 0.2488(9) 0.1041(8) 0.3312(7) 0.118(4) Uani 1 1 d . . . 
O3 O 0.3558(6) 0.1705(8) 0.2246(5) 0.111(4) Uani 1 1 d DU . . 
O4 O 0.3965(9) 0.3710(9) 0.2307(7) 0.140(6) Uani 1 1 d U . . 
O5 O 0.2418(8) 0.3728(7) 0.1501(5) 0.105(4) Uani 1 1 d . . . 
O6 O 0.0944(9) 0.3709(10) 0.2331(7) 0.133(5) Uani 1 1 d U . . 
O7 O 0.2345(8) 0.1822(8) 0.1307(5) 0.109(4) Uani 1 1 d . . . 
O8 O 0.2471(5) 0.3002(6) 0.2915(4) 0.065(2) Uani 1 1 d . . . 
C1 C 0.0860(12) 0.1788(11) 0.2897(8) 0.090(5) Uani 1 1 d . . . 
C2 C 0.1051(12) 0.1200(11) 0.3440(9) 0.096(5) Uani 1 1 d . . . 
C3 C 0.0611(13) 0.1320(12) 0.4030(9) 0.100(6) Uani 1 1 d . . . 
H3 H 0.0729 0.0927 0.4400 0.120 Uiso 1 1 calc R . . 
C4 C -0.0001(13) 0.1999(12) 0.4097(9) 0.098(5) Uani 1 1 d . . . 
C5 C -0.0105(11) 0.2608(11) 0.3567(8) 0.095(5) Uani 1 1 d . . . 
H5 H -0.0476 0.3095 0.3617 0.115 Uiso 1 1 calc R . . 
C6 C 0.0301(14) 0.2558(12) 0.2956(9) 0.106(6) Uani 1 1 d . . . 
C7 C -0.0494(13) 0.2041(15) 0.4708(9) 0.133(8) Uani 1 1 d D . . 
C8 C -0.1141(18) 0.279(2) 0.4677(14) 0.193(17) Uani 1 1 d D . . 
H8A H -0.0911 0.3381 0.4823 0.289 Uiso 1 1 calc PR . . 
H8B H -0.1571 0.2620 0.4973 0.289 Uiso 1 1 calc PR . . 
H8C H -0.1354 0.2847 0.4217 0.289 Uiso 1 1 calc PR . . 
C9 C 0.0035(15) 0.226(3) 0.5331(13) 0.194(17) Uani 1 1 d D . . 
H9A H -0.0301 0.2402 0.5708 0.292 Uiso 1 1 calc R . . 
H9B H 0.0377 0.2787 0.5239 0.292 Uiso 1 1 calc R . . 
H9C H 0.0368 0.1720 0.5443 0.292 Uiso 1 1 calc R . . 
C10 C -0.093(2) 0.1137(17) 0.4873(18) 0.23(2) Uani 1 1 d D . . 
H10A H -0.1144 0.0860 0.4458 0.351 Uiso 1 1 calc PR . . 
H10B H -0.1363 0.1268 0.5173 0.351 Uiso 1 1 calc PR . . 
H10C H -0.0552 0.0708 0.5091 0.351 Uiso 1 1 calc PR . . 
C11 C 0.1735(14) 0.0515(13) 0.3406(10) 0.111(6) Uani 1 1 d . . . 
H11A H 0.1776 0.0150 0.3824 0.133 Uiso 1 1 calc R . . 
H11B H 0.1640 0.0084 0.3027 0.133 Uiso 1 1 calc R . . 
C12 C 0.3196(13) 0.0482(12) 0.3373(10) 0.106(6) Uani 1 1 d . . . 
H12A H 0.3227 0.0060 0.2985 0.127 Uiso 1 1 calc R . . 
H12B H 0.3186 0.0106 0.3786 0.127 Uiso 1 1 calc R . . 
C13 C 0.3935(6) 0.1150(7) 0.3399(6) 0.096(6) Uani 1 1 d G . . 
C14 C 0.4047(7) 0.1760(8) 0.2855(4) 0.096(5) Uani 1 1 d GDU . . 
C15 C 0.4637(8) 0.2458(7) 0.2905(4) 0.094(5) Uani 1 1 d G . . 
C16 C 0.5116(6) 0.2547(7) 0.3499(6) 0.101(5) Uani 1 1 d G . . 
H16 H 0.5511 0.3014 0.3532 0.121 Uiso 1 1 calc R . . 
C17 C 0.5004(7) 0.1937(8) 0.4043(4) 0.091(5) Uani 1 1 d G . . 
C18 C 0.4414(7) 0.1238(7) 0.3993(5) 0.096(5) Uani 1 1 d G . . 
H18 H 0.4339 0.0830 0.4357 0.116 Uiso 1 1 calc R . . 
C19 C 0.5597(14) 0.1984(15) 0.4665(10) 0.111(6) Uani 1 1 d . . . 
C20 C 0.512(2) 0.191(3) 0.5292(15) 0.244(16) Uani 1 1 d U . . 
H20A H 0.5451 0.1645 0.5655 0.366 Uiso 1 1 calc R . . 
H20B H 0.4655 0.1514 0.5205 0.366 Uiso 1 1 calc R . . 
H20C H 0.4940 0.2526 0.5424 0.366 Uiso 1 1 calc R . . 
C21 C 0.616(2) 0.274(3) 0.4682(18) 0.231(16) Uani 1 1 d U . . 
H21A H 0.6601 0.2590 0.4393 0.346 Uiso 1 1 calc R . . 
H21B H 0.6363 0.2827 0.5142 0.346 Uiso 1 1 calc R . . 
H21C H 0.5894 0.3300 0.4523 0.346 Uiso 1 1 calc R . . 
C22 C 0.610(2) 0.114(3) 0.475(2) 0.268(19) Uani 1 1 d U . . 
H22A H 0.6656 0.1287 0.4653 0.402 Uiso 1 1 calc R . . 
H22B H 0.5908 0.0658 0.4438 0.402 Uiso 1 1 calc R . . 
H22C H 0.6074 0.0911 0.5209 0.402 Uiso 1 1 calc R . . 
C23 C 0.4728(13) 0.3201(13) 0.2329(9) 0.114(7) Uani 1 1 d U . . 
H23A H 0.5179 0.3623 0.2435 0.137 Uiso 1 1 calc R . . 
H23B H 0.4820 0.2897 0.1895 0.137 Uiso 1 1 calc R . . 
C24 C 0.3945(11) 0.4486(12) 0.1859(9) 0.100(5) Uani 1 1 d U . . 
H24A H 0.3955 0.4273 0.1389 0.120 Uiso 1 1 calc R . . 
H24B H 0.4412 0.4889 0.1948 0.120 Uiso 1 1 calc R . . 
C25 C 0.3189(10) 0.5006(10) 0.1977(8) 0.069(4) Uani 1 1 d . . . 
C26 C 0.2484(15) 0.4614(11) 0.1823(8) 0.095(6) Uani 1 1 d . . . 
C27 C 0.1708(11) 0.5032(11) 0.1991(7) 0.081(4) Uani 1 1 d . . . 
C28 C 0.1750(10) 0.5915(10) 0.2298(8) 0.077(4) Uani 1 1 d . . . 
H28 H 0.1271 0.6224 0.2399 0.092 Uiso 1 1 calc R . . 
C29 C 0.2491(9) 0.6348(9) 0.2459(7) 0.068(4) Uani 1 1 d . . . 
C30 C 0.3200(9) 0.5902(11) 0.2282(7) 0.075(4) Uani 1 1 d . . . 
H30 H 0.3695 0.6201 0.2367 0.090 Uiso 1 1 calc R . . 
C31 C 0.2528(10) 0.7330(10) 0.2780(8) 0.085(4) Uani 1 1 d . . . 
C32 C 0.3292(15) 0.7519(15) 0.3177(16) 0.174(12) Uani 1 1 d . . . 
H32A H 0.3611 0.6954 0.3208 0.261 Uiso 1 1 calc R . . 
H32B H 0.3165 0.7726 0.3628 0.261 Uiso 1 1 calc R . . 
H32C H 0.3594 0.8001 0.2953 0.261 Uiso 1 1 calc R . . 
C33 C 0.1849(18) 0.7483(16) 0.3280(16) 0.194(14) Uani 1 1 d . . . 
H33A H 0.1754 0.6910 0.3524 0.291 Uiso 1 1 calc R . . 
H33B H 0.1362 0.7667 0.3033 0.291 Uiso 1 1 calc R . . 
H33C H 0.2006 0.7970 0.3598 0.291 Uiso 1 1 calc R . . 
C34 C 0.2425(18) 0.8061(13) 0.2231(11) 0.162(10) Uani 1 1 d . . . 
H34A H 0.2225 0.8633 0.2426 0.243 Uiso 1 1 calc R . . 
H34B H 0.2045 0.7839 0.1886 0.243 Uiso 1 1 calc R . . 
H34C H 0.2939 0.8180 0.2031 0.243 Uiso 1 1 calc R . . 
C35 C 0.0935(12) 0.4511(11) 0.1871(9) 0.107(6) Uani 1 1 d . . . 
H35A H 0.0475 0.4915 0.1961 0.128 Uiso 1 1 calc R . . 
H35B H 0.0888 0.4299 0.1401 0.128 Uiso 1 1 calc R . . 
C36 C 0.0211(13) 0.3217(15) 0.2384(9) 0.117(7) Uani 1 1 d . . . 
H36A H 0.0088 0.2877 0.1964 0.141 Uiso 1 1 calc R . . 
H36B H -0.0230 0.3653 0.2463 0.141 Uiso 1 1 calc R . . 
N N 0.2525(13) 0.3826(13) 0.4185(8) 0.141(7) Uani 1 1 d D . . 
C37 C 0.3403(13) 0.374(2) 0.436(2) 0.29(3) Uani 1 1 d D . . 
H37A H 0.3634 0.3169 0.4181 0.348 Uiso 1 1 calc R . . 
H37B H 0.3515 0.3783 0.4847 0.348 Uiso 1 1 calc R . . 
C38 C 0.3701(19) 0.461(2) 0.3987(17) 0.227(15) Uani 1 1 d D . . 
H38A H 0.3270 0.5060 0.3947 0.341 Uiso 1 1 calc R . . 
H38B H 0.3869 0.4429 0.3540 0.341 Uiso 1 1 calc R . . 
H38C H 0.4153 0.4876 0.4240 0.341 Uiso 1 1 calc R . . 
C39 C 0.2083(19) 0.323(2) 0.467(3) 0.31(3) Uani 1 1 d D . . 
H39A H 0.1546 0.3093 0.4475 0.367 Uiso 1 1 calc R . . 
H39B H 0.2013 0.3580 0.5089 0.367 Uiso 1 1 calc R . . 
C40 C 0.251(2) 0.2301(17) 0.4843(12) 0.184(13) Uani 1 1 d D . . 
H40A H 0.2359 0.1837 0.4506 0.276 Uiso 1 1 calc R . . 
H40B H 0.2352 0.2090 0.5285 0.276 Uiso 1 1 calc R . . 
H40C H 0.3088 0.2394 0.4846 0.276 Uiso 1 1 calc R . . 
C41 C 0.2271(18) 0.4809(14) 0.426(3) 0.37(3) Uani 1 1 d DU . . 
H41A H 0.2527 0.5243 0.3955 0.450 Uiso 1 1 calc R . . 
H41B H 0.2307 0.5037 0.4731 0.450 Uiso 1 1 calc R . . 
C42 C 0.142(2) 0.451(3) 0.403(2) 0.21(2) Uani 1 1 d D . . 
H42A H 0.1373 0.4539 0.3542 0.322 Uiso 1 1 calc R . . 
H42B H 0.1029 0.4917 0.4227 0.322 Uiso 1 1 calc R . . 
H42C H 0.1327 0.3872 0.4177 0.322 Uiso 1 1 calc R . . 
O9 O 0.076(2) 0.014(2) 0.1502(18) 0.182(14) Uani 1 1 d D . . 
O10 O 0.412(3) 0.010(2) 0.146(2) 0.208(17) Uani 1 1 d D . . 
O11 O 0.251(4) -0.017(3) 0.098(3) 0.26(2) Uani 1 1 d D . . 
 
loop_ 
 _atom_site_aniso_label 
 _atom_site_aniso_U_11 
 _atom_site_aniso_U_22 
 _atom_site_aniso_U_33 
 _atom_site_aniso_U_23 
 _atom_site_aniso_U_13 
 _atom_site_aniso_U_12 
U 0.1268(6) 0.0677(4) 0.0530(3) -0.0078(3) 0.0072(3) -0.0065(4) 
O1 0.108(9) 0.096(7) 0.077(7) -0.016(6) 0.000(6) -0.036(6) 
O2 0.142(13) 0.074(7) 0.140(11) -0.022(7) 0.012(9) -0.004(8) 
O3 0.116(8) 0.142(8) 0.075(6) -0.039(6) 0.014(6) 0.004(6) 
O4 0.149(12) 0.133(10) 0.141(11) 0.072(9) 0.083(10) 0.060(9) 
O5 0.186(13) 0.072(6) 0.058(6) -0.007(5) 0.026(7) -0.016(7) 
O6 0.126(11) 0.143(11) 0.127(10) 0.065(9) -0.047(8) -0.061(9) 
O7 0.173(12) 0.095(8) 0.059(6) -0.016(6) -0.001(7) -0.006(8) 
O8 0.074(6) 0.079(5) 0.043(5) -0.007(4) -0.006(4) 0.000(5) 
C1 0.131(16) 0.066(10) 0.072(11) 0.000(8) 0.030(10) -0.050(10) 
C2 0.133(17) 0.072(10) 0.085(12) 0.001(9) 0.010(11) -0.003(11) 
C3 0.143(17) 0.086(11) 0.070(11) 0.014(8) -0.002(11) -0.003(11) 
C4 0.138(17) 0.077(10) 0.080(11) 0.008(9) 0.016(11) 0.014(11) 
C5 0.129(14) 0.084(11) 0.074(10) 0.007(9) 0.007(9) 0.009(10) 
C6 0.168(18) 0.075(11) 0.073(11) 0.007(9) -0.007(11) -0.044(13) 
C7 0.16(2) 0.146(18) 0.092(14) 0.022(13) 0.036(15) 0.039(17) 
C8 0.20(3) 0.27(4) 0.12(2) 0.03(2) 0.10(2) 0.08(3) 
C9 0.15(3) 0.35(4) 0.084(19) -0.01(3) 0.028(19) 0.02(3) 
C10 0.30(4) 0.21(3) 0.21(3) -0.02(3) 0.17(3) -0.05(3) 
C11 0.146(19) 0.090(12) 0.098(13) -0.019(10) 0.028(12) -0.022(14) 
C12 0.141(18) 0.071(10) 0.105(14) -0.013(9) 0.001(12) 0.008(12) 
C13 0.160(18) 0.059(9) 0.067(10) 0.004(8) 0.003(11) -0.002(10) 
C14 0.108(14) 0.070(10) 0.110(14) -0.021(10) 0.006(11) 0.038(10) 
C15 0.134(15) 0.078(11) 0.071(10) 0.010(9) 0.019(10) 0.015(11) 
C16 0.122(14) 0.084(11) 0.099(13) 0.014(10) 0.033(11) 0.011(11) 
C17 0.126(15) 0.076(10) 0.071(10) 0.004(8) -0.007(10) 0.010(10) 
C18 0.126(16) 0.070(10) 0.093(13) 0.019(9) 0.009(11) -0.005(10) 
C19 0.125(18) 0.107(14) 0.101(14) -0.001(11) 0.007(13) -0.020(13) 
C20 0.22(3) 0.38(4) 0.12(2) -0.04(3) 0.00(2) -0.05(3) 
C21 0.21(3) 0.27(3) 0.21(3) 0.06(2) -0.07(2) -0.09(3) 
C22 0.27(4) 0.27(4) 0.26(3) -0.04(3) -0.11(3) 0.04(3) 
C23 0.148(18) 0.116(13) 0.080(11) 0.016(10) 0.031(11) 0.058(13) 
C24 0.105(14) 0.098(11) 0.100(12) 0.020(10) 0.035(10) 0.018(10) 
C25 0.065(11) 0.066(9) 0.078(10) 0.005(7) 0.016(8) 0.000(8) 
C26 0.15(2) 0.075(10) 0.062(10) 0.000(8) 0.016(11) 0.008(12) 
C27 0.102(14) 0.081(10) 0.061(9) 0.003(8) -0.002(9) -0.009(10) 
C28 0.066(11) 0.070(9) 0.093(11) 0.003(8) -0.019(8) 0.011(8) 
C29 0.074(11) 0.064(8) 0.066(9) 0.004(6) 0.001(8) 0.002(8) 
C30 0.053(10) 0.089(11) 0.083(10) 0.008(8) -0.002(8) -0.009(8) 
C31 0.095(12) 0.077(9) 0.081(10) -0.003(8) 0.003(9) 0.002(9) 
C32 0.14(2) 0.14(2) 0.23(3) -0.091(19) -0.05(2) 0.003(16) 
C33 0.21(3) 0.135(19) 0.24(3) -0.098(19) 0.13(3) -0.018(18) 
C34 0.29(3) 0.072(11) 0.121(17) -0.004(12) -0.014(19) 0.006(17) 
C35 0.128(16) 0.083(11) 0.106(13) 0.019(10) -0.048(12) -0.022(11) 
C36 0.127(18) 0.145(17) 0.078(12) 0.026(11) -0.020(11) -0.045(14) 
N 0.19(2) 0.148(16) 0.088(12) -0.029(10) -0.010(12) 0.010(14) 
C37 0.30(5) 0.28(5) 0.27(4) -0.13(4) -0.10(4) 0.00(4) 
C38 0.27(4) 0.21(3) 0.20(3) 0.04(2) 0.01(3) 0.00(3) 
C39 0.36(5) 0.34(5) 0.23(4) -0.01(4) 0.09(4) 0.01(4) 
C40 0.30(4) 0.15(2) 0.105(16) -0.045(15) 0.02(2) 0.05(2) 
C41 0.43(5) 0.34(5) 0.36(5) 0.02(4) -0.01(4) 0.02(4) 
C42 0.25(4) 0.23(4) 0.17(3) -0.07(3) 0.02(3) -0.08(3) 
O9 0.26(3) 0.12(2) 0.17(3) -0.045(18) -0.04(2) -0.08(2) 
O10 0.27(4) 0.16(2) 0.20(3) -0.05(2) 0.09(3) 0.08(2) 
O11 0.34(5) 0.21(3) 0.22(4) 0.04(3) 0.00(3) 0.00(3) 
 
_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 
U O8 1.787(8) . ? 
U O7 1.781(10) . ? 
U O3 2.152(8) . ? 
U O5 2.202(10) . ? 
U O1 2.222(11) . ? 
O1 C1 1.354(17) . ? 
O2 C12 1.41(2) . ? 
O2 C11 1.46(2) . ? 
O3 C14 1.419(8) . ? 
O4 C24 1.409(18) . ? 
O4 C23 1.45(2) . ? 
O5 C26 1.411(18) . ? 
O6 C36 1.40(2) . ? 
O6 C35 1.452(18) . ? 
C1 C2 1.38(2) . ? 
C1 C6 1.44(3) . ? 
C2 C3 1.40(2) . ? 
C2 C11 1.49(3) . ? 
C3 C4 1.40(2) . ? 
C4 C5 1.36(2) . ? 
C4 C7 1.47(2) . ? 
C5 C6 1.39(2) . ? 
C6 C36 1.46(2) . ? 
C7 C8 1.505(10) . ? 
C7 C9 1.509(10) . ? 
C7 C10 1.510(10) . ? 
C12 C13 1.54(2) . ? 
C13 C14 1.3900 . ? 
C13 C18 1.3900 . ? 
C14 C15 1.3900 . ? 
C15 C16 1.3900 . ? 
C15 C23 1.556(18) . ? 
C16 C17 1.3900 . ? 
C17 C18 1.3900 . ? 
C17 C19 1.54(2) . ? 
C19 C21 1.41(3) . ? 
C19 C22 1.47(4) . ? 
C19 C20 1.48(3) . ? 
C24 C25 1.47(2) . ? 
C25 C26 1.31(2) . ? 
C25 C30 1.41(2) . ? 
C26 C27 1.46(2) . ? 
C27 C28 1.39(2) . ? 
C27 C35 1.48(2) . ? 
C28 C29 1.393(19) . ? 
C29 C30 1.382(19) . ? 
C29 C31 1.530(19) . ? 
C31 C32 1.48(3) . ? 
C31 C34 1.50(2) . ? 
C31 C33 1.53(3) . ? 
N C41 1.467(10) . ? 
N C37 1.480(10) . ? 
N C39 1.481(10) . ? 
C37 C38 1.513(10) . ? 
C39 C40 1.527(10) . ? 
C41 C42 1.518(10) . ? 
 
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 
O8 U O7 178.9(5) . . ? 
O8 U O3 94.8(4) . . ? 
O7 U O3 85.2(5) . . ? 
O8 U O5 95.0(4) . . ? 
O7 U O5 86.0(4) . . ? 
O3 U O5 116.6(5) . . ? 
O8 U O1 94.8(4) . . ? 
O7 U O1 84.2(5) . . ? 
O3 U O1 120.4(5) . . ? 
O5 U O1 120.8(5) . . ? 
C1 O1 U 122.4(9) . . ? 
C12 O2 C11 113.7(14) . . ? 
C14 O3 U 123.5(7) . . ? 
C24 O4 C23 114.3(13) . . ? 
C26 O5 U 120.9(8) . . ? 
C36 O6 C35 116.4(14) . . ? 
O1 C1 C2 118.9(18) . . ? 
O1 C1 C6 118.9(15) . . ? 
C2 C1 C6 121.9(16) . . ? 
C3 C2 C1 116.9(17) . . ? 
C3 C2 C11 122.0(16) . . ? 
C1 C2 C11 120.9(17) . . ? 
C2 C3 C4 123.7(16) . . ? 
C5 C4 C3 116.1(16) . . ? 
C5 C4 C7 122.5(17) . . ? 
C3 C4 C7 121.4(16) . . ? 
C4 C5 C6 124.9(17) . . ? 
C5 C6 C1 115.8(15) . . ? 
C5 C6 C36 126(2) . . ? 
C1 C6 C36 118.3(17) . . ? 
C4 C7 C8 114.0(16) . . ? 
C4 C7 C9 110.3(19) . . ? 
C8 C7 C9 106.2(9) . . ? 
C4 C7 C10 114.6(19) . . ? 
C8 C7 C10 105.7(9) . . ? 
C9 C7 C10 105.4(9) . . ? 
O2 C11 C2 108.4(15) . . ? 
O2 C12 C13 107.7(13) . . ? 
C14 C13 C18 120.0 . . ? 
C14 C13 C12 118.8(11) . . ? 
C18 C13 C12 120.6(11) . . ? 
C13 C14 C15 120.0 . . ? 
C13 C14 O3 121.7(10) . . ? 
C15 C14 O3 118.3(10) . . ? 
C16 C15 C14 120.0 . . ? 
C16 C15 C23 118.7(12) . . ? 
C14 C15 C23 121.1(12) . . ? 
C17 C16 C15 120.0 . . ? 
C16 C17 C18 120.0 . . ? 
C16 C17 C19 119.0(11) . . ? 
C18 C17 C19 120.8(11) . . ? 
C17 C18 C13 120.0 . . ? 
C21 C19 C22 104(3) . . ? 
C21 C19 C20 113(3) . . ? 
C22 C19 C20 99(3) . . ? 
C21 C19 C17 116.7(19) . . ? 
C22 C19 C17 113(2) . . ? 
C20 C19 C17 108(2) . . ? 
O4 C23 C15 104.9(13) . . ? 
O4 C24 C25 107.3(13) . . ? 
C26 C25 C30 118.7(14) . . ? 
C26 C25 C24 119.8(16) . . ? 
C30 C25 C24 121.4(16) . . ? 
C25 C26 O5 122.4(18) . . ? 
C25 C26 C27 123.4(15) . . ? 
O5 C26 C27 114.1(18) . . ? 
C28 C27 C26 115.6(15) . . ? 
C28 C27 C35 123.3(17) . . ? 
C26 C27 C35 121.0(16) . . ? 
C27 C28 C29 121.8(15) . . ? 
C30 C29 C28 118.8(13) . . ? 
C30 C29 C31 119.9(14) . . ? 
C28 C29 C31 121.2(13) . . ? 
C29 C30 C25 121.5(14) . . ? 
C32 C31 C34 109.0(19) . . ? 
C32 C31 C29 113.8(14) . . ? 
C34 C31 C29 109.6(13) . . ? 
C32 C31 C33 105(2) . . ? 
C34 C31 C33 107.0(19) . . ? 
C29 C31 C33 112.0(14) . . ? 
O6 C35 C27 107.6(13) . . ? 
O6 C36 C6 108.0(15) . . ? 
C41 N C37 109.3(10) . . ? 
C41 N C39 109.2(10) . . ? 
C37 N C39 107.8(9) . . ? 
N C37 C38 99.0(18) . . ? 
N C39 C40 114(2) . . ? 
N C41 C42 88(3) . . ? 
#===END
############################################################

data_2 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic         ?
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum             'C45 H70 N2 O11 U' 
_chemical_formula_weight          1053.06 
 
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' 
 
_symmetry_cell_setting            monoclinic 
_symmetry_space_group_name_H-M    P2(1)/c 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, y+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x, -y-1/2, z-1/2' 
 
_cell_length_a                    16.481(2) 
_cell_length_b                    14.2749(15) 
_cell_length_c                    20.314(2) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.020(3) 
_cell_angle_gamma                 90.00 
_cell_volume                      4779(4) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     270(2) 
_cell_measurement_reflns_used     27083 
_cell_measurement_theta_min       2.75
_cell_measurement_theta_max       26.77 
 
_exptl_crystal_description        platelet 
_exptl_crystal_colour             'translucent light orange' 
_exptl_crystal_size_max           0.30 
_exptl_crystal_size_mid           0.25
_exptl_crystal_size_min           0.10
_exptl_crystal_density_meas       'not measured' 
_exptl_crystal_density_diffrn     1.464 
_exptl_crystal_density_method     ?
_exptl_crystal_F_000              2136 
_exptl_absorpt_coefficient_mu     3.453 
_exptl_absorpt_correction_type    'empirical' 
_exptl_absorpt_correction_T_min   0.354 
_exptl_absorpt_correction_T_max   0.399 
_exptl_absorpt_process_details    'MULABS (Spek, 1997)'  
_exptl_special_details 
; 
 ? 
;  
_diffrn_ambient_temperature       270(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   'Nonius Kappa-CCD'
_diffrn_measurement_method        'area detector' 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_decay_%         none 
_diffrn_reflns_number             27083 
_diffrn_reflns_av_R_equivalents   0.074 
_diffrn_reflns_av_sigmaI/netI     0.090 
_diffrn_reflns_limit_h_min        -19 
_diffrn_reflns_limit_h_max        19 
_diffrn_reflns_limit_k_min        -17 
_diffrn_reflns_limit_k_max        18 
_diffrn_reflns_limit_l_min        -25 
_diffrn_reflns_limit_l_max        24 
_diffrn_reflns_theta_min          2.75 
_diffrn_reflns_theta_max          26.77 
_reflns_number_total              8158 
_reflns_number_gt                 4023 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        'Kappa-CCD software (Nonius, 1997)' 
_computing_cell_refinement        'HKL package (Otwinowski & Minor, 1997)' 
_computing_data_reduction         'HKL package (Otwinowski & Minor, 1997)' 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     'SHELXTL (Sheldrick, 1999)' 
_computing_publication_material   'SHELXTL (Sheldrick, 1999)' 
 
_refine_special_details 
;
 Structure solved by direct methods. Disorder on one tert-butyl group
 modelled with nine terminal carbon atoms with occupancies constrained 
 to sum up to unity. All non-hydrogen atoms refined anisotropically unless
 the disordered ones. Hydrogen atoms (except those of the disordered carbon
 atoms, the oxygen atoms of the methanol molecules and the nitrogen
 atom of DABCO) introduced at calculated positions as riding atoms with
 a displacement factor equal to 1.2 (CH, CH2) or 1.5 (CH3) times that
 of the parent atom.
 Refinement of F^2^ against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F^2^, conventional R-factors R are based 
 on F, with F set to zero for negative F^2^. The threshold expression of 
 F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F^2^ are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;  
_refine_ls_structure_factor_coef  Fsqd  
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme       calc  
_refine_ls_weighting_details 
 'calc w=1/[\s^2^(Fo^2^)+(0.0631P)^2^+15.9634P] where P=(Fo^2^+2Fc^2^)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     mixed 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          8158 
_refine_ls_number_parameters      553 
_refine_ls_number_restraints      73 
_refine_ls_R_factor_all           0.1606 
_refine_ls_R_factor_gt            0.0744 
_refine_ls_wR_factor_ref          0.1891 
_refine_ls_wR_factor_gt           0.1528 
_refine_ls_goodness_of_fit_ref    1.051 
_refine_ls_restrained_S_all       1.049 
_refine_ls_shift/su_max           0.002 
_refine_ls_shift/su_mean          0.000  
_diffrn_measured_fraction_theta_max    0.801 
_diffrn_reflns_theta_full              26.77 
_diffrn_measured_fraction_theta_full   0.801 
_refine_diff_density_max    1.093 
_refine_diff_density_min   -0.873 
_refine_diff_density_rms    0.101 

 
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_symmetry_multiplicity 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_assembly 
 _atom_site_disorder_group 
U U 0.25003(3) 0.74842(4) 0.21538(2) 0.0773(2) Uani 1 1 d . . . 
O1 O 0.1379(6) 0.6663(6) 0.2324(4) 0.085(3) Uani 1 1 d . . . 
O2 O 0.2521(6) 0.6013(6) 0.3394(6) 0.120(4) Uani 1 1 d . . . 
O3 O 0.3622(5) 0.6657(6) 0.2326(4) 0.081(2) Uani 1 1 d . . . 
O4 O 0.3955(5) 0.8657(6) 0.2325(4) 0.086(3) Uani 1 1 d . . . 
O5 O 0.2508(6) 0.8761(6) 0.1533(4) 0.085(2) Uani 1 1 d . . . 
O6 O 0.1047(5) 0.8667(6) 0.2325(4) 0.087(3) Uani 1 1 d . . . 
O7 O 0.2501(7) 0.6963(8) 0.1350(5) 0.120(4) Uani 1 1 d . . . 
O8 O 0.2502(4) 0.7993(5) 0.2954(3) 0.0606(18) Uani 1 1 d . . . 
C1 C 0.0935(8) 0.6759(9) 0.2880(8) 0.081(4) Uani 1 1 d . . . 
C2 C 0.1062(8) 0.6151(8) 0.3408(8) 0.076(4) Uani 1 1 d . . . 
C3 C 0.0587(8) 0.6217(8) 0.3965(7) 0.083(4) Uani 1 1 d . . . 
H3 H 0.0673 0.5804 0.4312 0.099 Uiso 1 1 calc R . . 
C4 C -0.0019(8) 0.6894(10) 0.4016(7) 0.082(4) Uani 1 1 d . . . 
C5 C -0.0091(7) 0.7536(10) 0.3499(7) 0.079(3) Uani 1 1 d . . . 
H5 H -0.0457 0.8030 0.3536 0.095 Uiso 1 1 calc R . . 
C6 C 0.0371(7) 0.7449(10) 0.2932(6) 0.073(3) Uani 1 1 d . . . 
C7 C -0.0585(10) 0.6979(11) 0.4636(8) 0.098(4) Uani 1 1 d . . . 
C8 C -0.077(2) 0.793(3) 0.4761(17) 0.273(16) Uani 1 1 d U . . 
H8A H -0.0707 0.8058 0.5222 0.409 Uiso 1 1 calc R . . 
H8B H -0.1325 0.8051 0.4635 0.409 Uiso 1 1 calc R . . 
H8C H -0.0417 0.8325 0.4511 0.409 Uiso 1 1 calc R . . 
C9 C -0.0079(19) 0.681(2) 0.5244(15) 0.241(13) Uani 1 1 d U . . 
H9A H 0.0463 0.7029 0.5171 0.361 Uiso 1 1 calc R . . 
H9B H -0.0065 0.6146 0.5336 0.361 Uiso 1 1 calc R . . 
H9C H -0.0313 0.7132 0.5610 0.361 Uiso 1 1 calc R . . 
C10 C -0.1123(17) 0.622(2) 0.4633(13) 0.219(12) Uani 1 1 d U . . 
H10A H -0.1095 0.5903 0.5048 0.328 Uiso 1 1 calc R . . 
H10B H -0.0979 0.5799 0.4286 0.328 Uiso 1 1 calc R . . 
H10C H -0.1665 0.6448 0.4563 0.328 Uiso 1 1 calc R . . 
C11 C 0.1756(9) 0.5481(9) 0.3373(8) 0.096(4) Uani 1 1 d . . . 
H11A H 0.1733 0.5048 0.3741 0.115 Uiso 1 1 calc R . . 
H11B H 0.1726 0.5122 0.2968 0.115 Uiso 1 1 calc R . . 
C12 C 0.3236(8) 0.5489(9) 0.3376(8) 0.090(4) Uani 1 1 d . . . 
H12A H 0.3271 0.5144 0.2965 0.108 Uiso 1 1 calc R . . 
H12B H 0.3246 0.5044 0.3737 0.108 Uiso 1 1 calc R . . 
C13 C 0.3927(9) 0.6150(9) 0.3432(8) 0.081(4) Uani 1 1 d . . . 
C14 C 0.4054(8) 0.6762(9) 0.2901(7) 0.075(3) Uani 1 1 d . . . 
C15 C 0.4630(8) 0.7446(11) 0.2931(6) 0.078(3) Uani 1 1 d . . . 
C16 C 0.5105(7) 0.7507(10) 0.3500(7) 0.081(3) Uani 1 1 d . . . 
H16 H 0.5495 0.7976 0.3525 0.097 Uiso 1 1 calc R . . 
C17 C 0.5021(6) 0.6902(9) 0.4024(5) 0.077(3) Uani 1 1 d D . . 
C18 C 0.4417(8) 0.6218(8) 0.3975(7) 0.080(4) Uani 1 1 d . . . 
H18 H 0.4346 0.5798 0.4320 0.096 Uiso 1 1 calc R . . 
C19 C 0.5565(7) 0.6978(8) 0.4653(7) 0.090(4) Uani 1 1 d D . . 
C20A C 0.5022(14) 0.685(3) 0.5256(6) 0.109(13) Uiso 0.52(4) 1 d PD . . 
C20B C 0.572(4) 0.6001(15) 0.492(2) 0.09(2) Uiso 0.26(4) 1 d PD . . 
C20C C 0.519(4) 0.639(6) 0.5195(19) 0.11(3) Uiso 0.22(4) 1 d PD . . 
C21A C 0.602(3) 0.790(2) 0.4639(18) 0.134(15) Uiso 0.52(4) 1 d PD . . 
C21B C 0.555(4) 0.7990(17) 0.489(2) 0.073(18) Uiso 0.26(4) 1 d PD . . 
C21C C 0.519(4) 0.771(5) 0.511(2) 0.10(3) Uiso 0.22(4) 1 d PD . . 
C22A C 0.6183(17) 0.617(2) 0.4620(14) 0.109(13) Uiso 0.52(4) 1 d PD . . 
C22B C 0.637(3) 0.741(8) 0.4450(17) 0.12(2) Uiso 0.26(4) 1 d PD . . 
C22C C 0.6449(7) 0.691(7) 0.4442(14) 0.09(3) Uiso 0.22(4) 1 d PD . . 
C23 C 0.4715(7) 0.8137(9) 0.2378(7) 0.080(4) Uani 1 1 d . . . 
H23A H 0.5160 0.8563 0.2467 0.096 Uiso 1 1 calc R . . 
H23B H 0.4826 0.7811 0.1969 0.096 Uiso 1 1 calc R . . 
C24 C 0.3993(8) 0.9494(9) 0.1924(7) 0.081(4) Uani 1 1 d . . . 
H24A H 0.4048 0.9328 0.1463 0.098 Uiso 1 1 calc R . . 
H24B H 0.4457 0.9871 0.2050 0.098 Uiso 1 1 calc R . . 
C25 C 0.3231(7) 1.0030(8) 0.2029(5) 0.064(3) Uani 1 1 d . . . 
C26 C 0.2505(8) 0.9633(7) 0.1865(6) 0.066(3) Uani 1 1 d . . . 
C27 C 0.1779(7) 1.0034(8) 0.2036(6) 0.065(3) Uani 1 1 d . . . 
C28 C 0.1785(6) 1.0891(7) 0.2353(5) 0.060(3) Uani 1 1 d . . . 
H28 H 0.1295 1.1171 0.2468 0.072 Uiso 1 1 calc R . . 
C29 C 0.2504(6) 1.1339(7) 0.2501(5) 0.058(3) Uani 1 1 d . . . 
C30 C 0.3211(6) 1.0890(7) 0.2344(5) 0.059(3) Uani 1 1 d . . . 
H30 H 0.3700 1.1175 0.2454 0.071 Uiso 1 1 calc R . . 
C31 C 0.2487(7) 1.2299(7) 0.2835(6) 0.070(3) Uani 1 1 d . . . 
C32 C 0.3243(11) 1.2415(12) 0.3270(11) 0.156(9) Uani 1 1 d . . . 
H32A H 0.3526 1.2975 0.3146 0.234 Uiso 1 1 calc R . . 
H32B H 0.3594 1.1884 0.3212 0.234 Uiso 1 1 calc R . . 
H32C H 0.3082 1.2458 0.3723 0.234 Uiso 1 1 calc R . . 
C33 C 0.1798(11) 1.2443(13) 0.3279(11) 0.152(8) Uani 1 1 d . . . 
H33A H 0.1863 1.3028 0.3507 0.228 Uiso 1 1 calc R . . 
H33B H 0.1777 1.1941 0.3593 0.228 Uiso 1 1 calc R . . 
H33C H 0.1304 1.2455 0.3028 0.228 Uiso 1 1 calc R . . 
C34 C 0.2528(13) 1.3031(11) 0.2323(8) 0.146(8) Uani 1 1 d . . . 
H34A H 0.3058 1.3029 0.2126 0.219 Uiso 1 1 calc R . . 
H34B H 0.2426 1.3632 0.2518 0.219 Uiso 1 1 calc R . . 
H34C H 0.2127 1.2907 0.1991 0.219 Uiso 1 1 calc R . . 
C35 C 0.1011(7) 0.9477(9) 0.1920(6) 0.076(3) Uani 1 1 d . . . 
H35A H 0.0539 0.9850 0.2032 0.091 Uiso 1 1 calc R . . 
H35B H 0.0971 0.9297 0.1460 0.091 Uiso 1 1 calc R . . 
C36 C 0.0281(8) 0.8164(10) 0.2382(6) 0.086(4) Uani 1 1 d . . . 
H36A H 0.0155 0.7851 0.1971 0.103 Uiso 1 1 calc R . . 
H36B H -0.0154 0.8597 0.2483 0.103 Uiso 1 1 calc R . . 
N1 N 0.254(2) 1.0042(12) 0.4171(9) 0.166(10) Uani 1 1 d . . . 
N2 N 0.2500(11) 0.8554(9) 0.4789(7) 0.104(4) Uani 1 1 d . . . 
C37 C 0.1869(17) 0.9585(19) 0.3996(12) 0.155(9) Uani 1 1 d . . . 
H37A H 0.1868 0.9496 0.3523 0.186 Uiso 1 1 calc R . . 
H37B H 0.1399 0.9961 0.4109 0.186 Uiso 1 1 calc R . . 
C38 C 0.1799(13) 0.8639(16) 0.4330(11) 0.148(8) Uani 1 1 d . . . 
H38A H 0.1292 0.8596 0.4571 0.178 Uiso 1 1 calc R . . 
H38B H 0.1813 0.8141 0.4005 0.178 Uiso 1 1 calc R . . 
C39 C 0.2509(13) 0.9368(12) 0.5234(8) 0.141(7) Uani 1 1 d . . . 
H39A H 0.2053 0.9323 0.5533 0.169 Uiso 1 1 calc R . . 
H39B H 0.3002 0.9352 0.5495 0.169 Uiso 1 1 calc R . . 
C40 C 0.2468(17) 1.0252(12) 0.4885(9) 0.177(10) Uani 1 1 d . . . 
H40A H 0.2905 1.0660 0.5024 0.213 Uiso 1 1 calc R . . 
H40B H 0.1956 1.0561 0.4975 0.213 Uiso 1 1 calc R . . 
C41 C 0.3167(16) 0.862(2) 0.4363(13) 0.162(10) Uani 1 1 d . . . 
H41A H 0.3148 0.8103 0.4053 0.194 Uiso 1 1 calc R . . 
H41B H 0.3662 0.8558 0.4617 0.194 Uiso 1 1 calc R . . 
C42 C 0.3195(17) 0.947(2) 0.4005(13) 0.164(10) Uani 1 1 d . . . 
H42A H 0.3698 0.9800 0.4103 0.197 Uiso 1 1 calc R . . 
H42B H 0.3184 0.9343 0.3537 0.197 Uiso 1 1 calc R . . 
O9 O 0.0972(12) 0.5072(14) 0.1533(9) 0.206(7) Uani 1 1 d U . . 
O10 O 0.4029(13) 0.5126(14) 0.1512(9) 0.224(8) Uani 1 1 d U . . 
O11 O 0.2484(12) 0.8189(17) 0.0266(9) 0.210(7) Uani 1 1 d U . . 
C43 C 0.0308(16) 0.5406(18) 0.1342(12) 0.188(10) Uani 1 1 d U . . 
H43A H -0.0094 0.5321 0.1679 0.282 Uiso 1 1 calc R . . 
H43B H 0.0138 0.5091 0.0948 0.282 Uiso 1 1 calc R . . 
H43C H 0.0372 0.6062 0.1253 0.282 Uiso 1 1 calc R . . 
C45 C 0.2491(14) 0.8960(17) 0.0005(12) 0.162(8) Uani 1 1 d U . . 
H45A H 0.1976 0.9259 0.0068 0.244 Uiso 1 1 calc R . . 
H45B H 0.2594 0.8890 -0.0457 0.244 Uiso 1 1 calc R . . 
H45C H 0.2911 0.9336 0.0199 0.244 Uiso 1 1 calc R . . 
C44 C 0.4732(15) 0.5329(18) 0.1361(12) 0.182(9) Uani 1 1 d U . . 
H44A H 0.4743 0.5944 0.1169 0.273 Uiso 1 1 calc R . . 
H44B H 0.4933 0.4882 0.1048 0.273 Uiso 1 1 calc R . . 
H44C H 0.5067 0.5320 0.1747 0.273 Uiso 1 1 calc R . . 
 
loop_ 
 _atom_site_aniso_label 
 _atom_site_aniso_U_11 
 _atom_site_aniso_U_22 
 _atom_site_aniso_U_33 
 _atom_site_aniso_U_23 
 _atom_site_aniso_U_13 
 _atom_site_aniso_U_12 
U 0.0890(3) 0.0667(3) 0.0762(3) -0.0180(3) 0.0011(2) 0.0005(3) 
O1 0.086(6) 0.079(6) 0.089(6) -0.032(5) -0.002(5) -0.017(5) 
O2 0.074(6) 0.049(5) 0.236(13) -0.027(6) -0.006(7) 0.000(5) 
O3 0.087(6) 0.065(5) 0.091(6) -0.019(4) 0.012(5) 0.009(4) 
O4 0.067(5) 0.085(6) 0.106(7) 0.020(5) 0.029(5) 0.017(5) 
O5 0.109(7) 0.074(6) 0.073(5) -0.014(5) 0.005(5) 0.001(5) 
O6 0.063(5) 0.084(6) 0.112(7) 0.035(5) -0.031(5) -0.021(5) 
O7 0.158(10) 0.097(7) 0.105(7) -0.047(6) -0.003(7) 0.010(7) 
O8 0.065(4) 0.063(4) 0.054(4) -0.014(3) 0.001(4) -0.007(4) 
C1 0.077(9) 0.050(7) 0.115(12) -0.013(8) 0.000(8) -0.006(7) 
C2 0.066(8) 0.047(7) 0.114(11) -0.011(7) 0.001(8) -0.003(6) 
C3 0.082(9) 0.049(7) 0.118(11) 0.002(7) -0.003(8) -0.016(7) 
C4 0.070(8) 0.086(10) 0.090(10) 0.007(8) -0.006(7) -0.018(8) 
C5 0.065(7) 0.068(7) 0.103(9) -0.008(9) -0.007(6) 0.020(8) 
C6 0.077(7) 0.058(7) 0.083(8) -0.001(8) -0.013(6) -0.022(9) 
C7 0.126(13) 0.068(9) 0.099(11) -0.002(8) -0.003(10) -0.014(9) 
C8 0.275(16) 0.272(16) 0.271(16) 0.000(5) 0.007(5) 0.004(5) 
C9 0.241(14) 0.244(14) 0.238(14) 0.000(5) 0.003(5) 0.002(5) 
C10 0.219(12) 0.220(12) 0.218(12) -0.003(5) 0.007(5) -0.005(5) 
C11 0.099(11) 0.063(8) 0.125(12) -0.004(8) -0.003(9) -0.010(8) 
C12 0.073(9) 0.057(8) 0.140(13) -0.011(8) 0.006(8) 0.011(7) 
C13 0.082(9) 0.056(8) 0.104(11) -0.010(8) 0.005(8) 0.012(7) 
C14 0.075(9) 0.059(8) 0.090(10) -0.013(7) 0.002(8) 0.019(7) 
C15 0.073(8) 0.074(8) 0.089(8) 0.001(9) 0.013(7) 0.028(9) 
C16 0.066(7) 0.073(7) 0.103(9) -0.001(9) 0.007(7) 0.000(8) 
C17 0.064(8) 0.079(9) 0.089(9) -0.001(8) 0.008(7) 0.014(7) 
C18 0.085(9) 0.048(7) 0.108(11) 0.008(7) 0.010(8) 0.013(7) 
C19 0.079(10) 0.080(9) 0.111(12) -0.001(8) 0.001(8) -0.003(8) 
C23 0.062(8) 0.081(9) 0.098(10) 0.022(8) 0.029(7) 0.019(7) 
C24 0.077(9) 0.078(9) 0.089(9) 0.032(7) 0.023(7) 0.020(7) 
C25 0.074(8) 0.062(7) 0.057(7) 0.002(6) 0.015(6) 0.013(6) 
C26 0.082(9) 0.046(6) 0.068(7) -0.003(6) -0.004(7) 0.004(6) 
C27 0.063(8) 0.056(7) 0.074(8) 0.006(6) -0.005(6) -0.006(6) 
C28 0.048(6) 0.056(7) 0.076(8) 0.005(6) 0.008(5) 0.003(5) 
C29 0.053(7) 0.053(6) 0.068(7) 0.003(6) 0.002(5) -0.004(6) 
C30 0.037(6) 0.058(7) 0.082(8) 0.004(6) 0.012(5) -0.002(5) 
C31 0.063(7) 0.051(8) 0.096(8) -0.015(6) -0.007(6) 0.003(6) 
C32 0.132(15) 0.117(14) 0.22(2) -0.066(14) -0.085(15) 0.023(12) 
C33 0.106(12) 0.151(17) 0.20(2) -0.062(15) 0.049(13) -0.010(13) 
C34 0.25(3) 0.058(9) 0.130(14) 0.010(10) 0.007(15) 0.001(13) 
C35 0.066(8) 0.076(8) 0.085(9) 0.018(7) -0.017(6) -0.007(7) 
C36 0.078(9) 0.091(10) 0.089(9) 0.001(8) -0.027(7) -0.029(8) 
N1 0.31(3) 0.083(11) 0.106(14) 0.045(10) -0.032(18) -0.045(16) 
N2 0.123(11) 0.073(8) 0.116(11) 0.007(7) 0.018(11) 0.004(8) 
C37 0.17(2) 0.13(2) 0.16(2) 0.036(17) 0.011(18) 0.076(17) 
C38 0.128(17) 0.16(2) 0.156(18) -0.060(16) 0.044(14) -0.063(15) 
C39 0.23(2) 0.084(12) 0.105(13) 0.023(10) 0.000(14) -0.003(13) 
C40 0.36(3) 0.085(12) 0.083(12) 0.015(10) 0.014(16) 0.002(16) 
C41 0.136(19) 0.18(3) 0.17(2) -0.047(19) -0.084(18) 0.058(18) 
C42 0.15(2) 0.17(3) 0.18(2) 0.02(2) 0.014(18) -0.070(19) 
O9 0.208(8) 0.204(8) 0.207(8) -0.007(5) -0.002(5) -0.005(5) 
O10 0.224(9) 0.221(9) 0.227(9) -0.008(5) 0.001(5) 0.003(5) 
O11 0.224(8) 0.201(8) 0.206(8) 0.001(5) -0.001(5) -0.002(5) 
C43 0.188(11) 0.187(11) 0.189(11) -0.004(5) -0.007(5) 0.001(5) 
C45 0.167(9) 0.161(9) 0.159(9) 0.002(5) -0.001(5) 0.000(5) 
C44 0.182(10) 0.179(10) 0.185(10) -0.004(5) 0.008(5) -0.002(5) 
 
_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 
U O8 1.780(6) . ? 
U O7 1.794(9) . ? 
U O1 2.215(9) . ? 
U O5 2.216(8) . ? 
U O3 2.221(9) . ? 
U O4 2.945(9) . ? 
U O6 2.950(9) . ? 
O1 C1 1.355(15) . ? 
O2 C12 1.397(14) . ? 
O2 C11 1.472(15) . ? 
O3 C14 1.377(15) . ? 
O4 C24 1.448(13) . ? 
O4 C23 1.459(13) . ? 
O5 C26 1.415(13) . ? 
O6 C35 1.421(13) . ? 
O6 C36 1.457(13) . ? 
C1 C6 1.358(17) . ? 
C1 C2 1.396(18) . ? 
C2 C3 1.379(17) . ? 
C2 C11 1.493(17) . ? 
C3 C4 1.394(18) . ? 
C4 C5 1.399(18) . ? 
C4 C7 1.57(2) . ? 
C5 C6 1.386(17) . ? 
C6 C36 1.520(17) . ? 
C7 C10 1.40(3) . ? 
C7 C8 1.41(4) . ? 
C7 C9 1.51(3) . ? 
C12 C13 1.484(18) . ? 
C13 C18 1.369(17) . ? 
C13 C14 1.403(18) . ? 
C14 C15 1.363(18) . ? 
C15 C16 1.398(18) . ? 
C15 C23 1.501(17) . ? 
C16 C17 1.378(17) . ? 
C17 C18 1.398(16) . ? 
C17 C19 1.565(14) . ? 
C19 C21A 1.515(10) . ? 
C19 C20B 1.517(10) . ? 
C19 C20C 1.520(10) . ? 
C19 C21C 1.521(10) . ? 
C19 C21B 1.521(10) . ? 
C19 C22C 1.522(10) . ? 
C19 C22B 1.526(10) . ? 
C19 C20A 1.529(10) . ? 
C19 C22A 1.536(10) . ? 
C20A C20C 0.72(10) . ? 
C20A C21C 1.30(9) . ? 
C20A C20B 1.80(6) . ? 
C20A C21B 2.00(6) . ? 
C20B C22A 1.01(6) . ? 
C20B C20C 1.17(10) . ? 
C20B C22C 2.02(7) . ? 
C20C C21C 1.89(11) . ? 
C20C C22A 2.03(8) . ? 
C21A C21B 0.93(7) . ? 
C21A C22B 0.99(9) . ? 
C21A C22C 1.63(8) . ? 
C21A C21C 1.69(8) . ? 
C21B C21C 0.84(8) . ? 
C21B C22B 1.82(11) . ? 
C22A C22C 1.20(8) . ? 
C22A C22B 1.83(9) . ? 
C22B C22C 0.72(10) . ? 
C24 C25 1.485(15) . ? 
C25 C26 1.365(16) . ? 
C25 C30 1.386(15) . ? 
C26 C27 1.370(16) . ? 
C27 C28 1.383(15) . ? 
C27 C35 1.513(15) . ? 
C28 C29 1.380(14) . ? 
C29 C30 1.368(13) . ? 
C29 C31 1.529(14) . ? 
C31 C33 1.464(19) . ? 
C31 C34 1.477(18) . ? 
C31 C32 1.536(19) . ? 
N1 C37 1.33(3) . ? 
N1 C42 1.39(3) . ? 
N1 C40 1.49(2) . ? 
N2 C41 1.40(3) . ? 
N2 C39 1.47(2) . ? 
N2 C38 1.49(2) . ? 
C37 C38 1.52(3) . ? 
C39 C40 1.45(2) . ? 
C41 C42 1.42(3) . ? 
O9 C43 1.26(2) . ? 
O10 C44 1.23(2) . ? 
O11 C45 1.22(2) . ? 
 
loop_ 
 _geom_angle_atom_site_label_1 
 _geom_angle_atom_site_label_2 
 _geom_angle_atom_site_label_3 
 _geom_angle 
 _geom_angle_site_symmetry_1 
 _geom_angle_site_symmetry_3 
 _geom_angle_publ_flag 
O8 U O7 179.5(4) . . ? 
O8 U O1 94.3(3) . . ? 
O7 U O1 85.6(4) . . ? 
O8 U O5 100.6(3) . . ? 
O7 U O5 79.8(4) . . ? 
O1 U O5 121.9(3) . . ? 
O8 U O3 94.1(3) . . ? 
O7 U O3 85.6(4) . . ? 
O1 U O3 112.8(3) . . ? 
O5 U O3 121.5(3) . . ? 
O8 U O4 70.1(3) . . ? 
O7 U O4 110.0(4) . . ? 
O1 U O4 164.1(3) . . ? 
O5 U O4 66.1(3) . . ? 
O3 U O4 66.8(3) . . ? 
O8 U O6 70.1(3) . . ? 
O7 U O6 110.2(4) . . ? 
O1 U O6 66.9(3) . . ? 
O5 U O6 66.5(3) . . ? 
O3 U O6 164.0(3) . . ? 
O4 U O6 108.8(2) . . ? 
C1 O1 U 121.9(7) . . ? 
C12 O2 C11 116.4(9) . . ? 
C14 O3 U 120.4(7) . . ? 
C24 O4 C23 115.2(8) . . ? 
C24 O4 U 116.0(7) . . ? 
C23 O4 U 114.7(7) . . ? 
C26 O5 U 117.0(7) . . ? 
C35 O6 C36 114.3(9) . . ? 
C35 O6 U 115.6(7) . . ? 
C36 O6 U 115.5(8) . . ? 
O1 C1 C6 120.6(13) . . ? 
O1 C1 C2 119.8(13) . . ? 
C6 C1 C2 119.6(13) . . ? 
C3 C2 C1 120.2(12) . . ? 
C3 C2 C11 121.2(13) . . ? 
C1 C2 C11 118.5(13) . . ? 
C2 C3 C4 121.0(13) . . ? 
C3 C4 C5 117.3(13) . . ? 
C3 C4 C7 122.6(13) . . ? 
C5 C4 C7 120.0(13) . . ? 
C6 C5 C4 121.2(12) . . ? 
C1 C6 C5 120.3(13) . . ? 
C1 C6 C36 119.7(12) . . ? 
C5 C6 C36 119.8(13) . . ? 
C10 C7 C8 127(2) . . ? 
C10 C7 C9 103(2) . . ? 
C8 C7 C9 98(2) . . ? 
C10 C7 C4 108.3(16) . . ? 
C8 C7 C4 110.4(18) . . ? 
C9 C7 C4 108.3(17) . . ? 
O2 C11 C2 108.9(10) . . ? 
O2 C12 C13 107.8(10) . . ? 
C18 C13 C14 119.1(13) . . ? 
C18 C13 C12 124.0(14) . . ? 
C14 C13 C12 116.8(14) . . ? 
C15 C14 O3 118.4(13) . . ? 
C15 C14 C13 121.1(14) . . ? 
O3 C14 C13 120.5(14) . . ? 
C14 C15 C16 118.1(13) . . ? 
C14 C15 C23 120.2(13) . . ? 
C16 C15 C23 121.7(14) . . ? 
C17 C16 C15 122.9(12) . . ? 
C16 C17 C18 117.0(11) . . ? 
C16 C17 C19 122.0(10) . . ? 
C18 C17 C19 120.9(10) . . ? 
C13 C18 C17 121.8(12) . . ? 
C21A C19 C20B 137(2) . . ? 
C21A C19 C20C 134(3) . . ? 
C20B C19 C20C 45(4) . . ? 
C21A C19 C21C 67(4) . . ? 
C20B C19 C21C 119(4) . . ? 
C20C C19 C21C 77(5) . . ? 
C21A C19 C21B 36(3) . . ? 
C20B C19 C21B 140(2) . . ? 
C20C C19 C21B 107(5) . . ? 
C21C C19 C21B 32(3) . . ? 
C21A C19 C22C 65(4) . . ? 
C20B C19 C22C 84(4) . . ? 
C20C C19 C22C 124(4) . . ? 
C21C C19 C22C 127(4) . . ? 
C21B C19 C22C 99(4) . . ? 
C21A C19 C22B 38(4) . . ? 
C20B C19 C22B 109(4) . . ? 
C20C C19 C22B 141(3) . . ? 
C21C C19 C22B 104(5) . . ? 
C21B C19 C22B 74(5) . . ? 
C22C C19 C22B 27(4) . . ? 
C21A C19 C20A 114(2) . . ? 
C20B C19 C20A 72(3) . . ? 
C20C C19 C20A 27(4) . . ? 
C21C C19 C20A 50(4) . . ? 
C21B C19 C20A 82(3) . . ? 
C22C C19 C20A 141(2) . . ? 
C22B C19 C20A 141(2) . . ? 
C21A C19 C22A 109(2) . . ? 
C20B C19 C22A 39(2) . . ? 
C20C C19 C22A 83(4) . . ? 
C21C C19 C22A 143.9(19) . . ? 
C21B C19 C22A 137(2) . . ? 
C22C C19 C22A 46(3) . . ? 
C22B C19 C22A 73(4) . . ? 
C20A C19 C22A 109(2) . . ? 
C21A C19 C17 109.1(10) . . ? 
C20B C19 C17 108.8(10) . . ? 
C20C C19 C17 108.6(11) . . ? 
C21C C19 C17 108.0(11) . . ? 
C21B C19 C17 108.3(10) . . ? 
C22C C19 C17 108.2(10) . . ? 
C22B C19 C17 107.9(10) . . ? 
C20A C19 C17 108.1(9) . . ? 
C22A C19 C17 106.9(9) . . ? 
C20C C20A C21C 138(3) . . ? 
C20C C20A C19 76(2) . . ? 
C21C C20A C19 64.5(19) . . ? 
C20C C20A C20B 23(2) . . ? 
C21C C20A C20B 114(3) . . ? 
C19 C20A C20B 53.5(15) . . ? 
C20C C20A C21B 121(3) . . ? 
C21C C20A C21B 16.9(17) . . ? 
C19 C20A C21B 49.0(15) . . ? 
C20B C20A C21B 97(2) . . ? 
C22A C20B C20C 138(3) . . ? 
C22A C20B C19 71.7(15) . . ? 
C20C C20B C19 67(2) . . ? 
C22A C20B C20A 123.3(18) . . ? 
C20C C20B C20A 14(2) . . ? 
C19 C20B C20A 54.1(16) . . ? 
C22A C20B C22C 25.9(19) . . ? 
C20C C20B C22C 112(3) . . ? 
C19 C20B C22C 48.3(19) . . ? 
C20A C20B C22C 98(2) . . ? 
C20A C20C C20B 142(3) . . ? 
C20A C20C C19 77(2) . . ? 
C20B C20C C19 67(2) . . ? 
C20A C20C C21C 27(2) . . ? 
C20B C20C C21C 115(3) . . ? 
C19 C20C C21C 51(3) . . ? 
C20A C20C C22A 123(2) . . ? 
C20B C20C C22A 19.6(15) . . ? 
C19 C20C C22A 49(2) . . ? 
C21C C20C C22A 95(2) . . ? 
C21B C21A C22B 143(3) . . ? 
C21B C21A C19 72.5(15) . . ? 
C22B C21A C19 72(2) . . ? 
C21B C21A C22C 128(3) . . ? 
C22B C21A C22C 15(2) . . ? 
C19 C21A C22C 57.7(18) . . ? 
C21B C21A C21C 17.3(19) . . ? 
C22B C21A C21C 125(3) . . ? 
C19 C21A C21C 56.5(19) . . ? 
C22C C21A C21C 110(3) . . ? 
C21C C21B C21A 144(3) . . ? 
C21C C21B C19 73.9(17) . . ? 
C21A C21B C19 71.8(15) . . ? 
C21C C21B C22B 124(3) . . ? 
C21A C21B C22B 19(2) . . ? 
C19 C21B C22B 53(2) . . ? 
C21C C21B C20A 26(2) . . ? 
C21A C21B C20A 117(2) . . ? 
C19 C21B C20A 49.3(16) . . ? 
C22B C21B C20A 98(3) . . ? 
C21B C21C C20A 137(3) . . ? 
C21B C21C C19 73.9(18) . . ? 
C20A C21C C19 65.2(19) . . ? 
C21B C21C C21A 19.2(18) . . ? 
C20A C21C C21A 117.5(19) . . ? 
C19 C21C C21A 56.1(19) . . ? 
C21B C21C C20C 122(3) . . ? 
C20A C21C C20C 15(2) . . ? 
C19 C21C C20C 51(3) . . ? 
C21A C21C C20C 103(3) . . ? 
C20B C22A C22C 132(2) . . ? 
C20B C22A C19 69.6(14) . . ? 
C22C C22A C19 66.3(17) . . ? 
C20B C22A C22B 119(3) . . ? 
C22C C22A C22B 14(2) . . ? 
C19 C22A C22B 53(2) . . ? 
C20B C22A C20C 23(2) . . ? 
C22C C22A C20C 110(3) . . ? 
C19 C22A C20C 48(2) . . ? 
C22B C22A C20C 96(3) . . ? 
C22C C22B C21A 144(3) . . ? 
C22C C22B C19 76(2) . . ? 
C21A C22B C19 70.3(19) . . ? 
C22C C22B C21B 126(3) . . ? 
C21A C22B C21B 18.0(16) . . ? 
C19 C22B C21B 53(2) . . ? 
C22C C22B C22A 23(2) . . ? 
C21A C22B C22A 121(2) . . ? 
C19 C22B C22A 54(2) . . ? 
C21B C22B C22A 102.6(19) . . ? 
C22B C22C C22A 143(3) . . ? 
C22B C22C C19 77(2) . . ? 
C22A C22C C19 67.5(18) . . ? 
C22B C22C C21A 21(2) . . ? 
C22A C22C C21A 121.9(18) . . ? 
C19 C22C C21A 57.3(18) . . ? 
C22B C22C C20B 121(3) . . ? 
C22A C22C C20B 21.6(15) . . ? 
C19 C22C C20B 48.1(19) . . ? 
C21A C22C C20B 100(2) . . ? 
O4 C23 C15 108.0(9) . . ? 
O4 C24 C25 108.0(9) . . ? 
C26 C25 C30 117.3(10) . . ? 
C26 C25 C24 119.5(11) . . ? 
C30 C25 C24 122.9(12) . . ? 
C25 C26 C27 122.0(10) . . ? 
C25 C26 O5 118.5(11) . . ? 
C27 C26 O5 119.4(11) . . ? 
C26 C27 C28 118.8(10) . . ? 
C26 C27 C35 118.1(11) . . ? 
C28 C27 C35 122.9(11) . . ? 
C29 C28 C27 121.2(10) . . ? 
C30 C29 C28 117.6(10) . . ? 
C30 C29 C31 122.6(10) . . ? 
C28 C29 C31 119.7(10) . . ? 
C29 C30 C25 122.9(10) . . ? 
C33 C31 C34 111.7(14) . . ? 
C33 C31 C29 114.4(11) . . ? 
C34 C31 C29 108.7(11) . . ? 
C33 C31 C32 105.1(14) . . ? 
C34 C31 C32 106.9(14) . . ? 
C29 C31 C32 109.7(10) . . ? 
O6 C35 C27 107.6(9) . . ? 
O6 C36 C6 107.8(9) . . ? 
C37 N1 C42 107(2) . . ? 
C37 N1 C40 107(3) . . ? 
C42 N1 C40 115(2) . . ? 
C41 N2 C39 108.5(16) . . ? 
C41 N2 C38 102.5(14) . . ? 
C39 N2 C38 109.1(14) . . ? 
N1 C37 C38 112.4(19) . . ? 
N2 C38 C37 107.1(16) . . ? 
C40 C39 N2 112.7(14) . . ? 
C39 C40 N1 107.3(15) . . ? 
N2 C41 C42 114(2) . . ? 
N1 C42 C41 111(2) . . ?