# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_1

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H58 O29 U4'
_chemical_formula_weight         1834.88

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'
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   'P 21'

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

_cell_length_a                   15.4579(16)
_cell_length_b                   19.1439(17)
_cell_length_c                   17.1090(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 105.241(6)
_cell_angle_gamma                90.00
_cell_volume                     4884.9(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    147323
_cell_measurement_theta_min      2.32
_cell_measurement_theta_max      25.68

_exptl_crystal_description       parallelepiped
_exptl_crystal_colour            'translucent light yellow'
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.495
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3352
_exptl_absorpt_coefficient_mu    13.308
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.205
_exptl_absorpt_correction_T_max  0.345
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_special_details           'crystal-to-detector distance 30 mm'
_diffrn_ambient_temperature      150(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 area-detector diffractometer'
_diffrn_measurement_method       
'two φ and six ω scans with 2° steps (473 frames)'
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            147323
_diffrn_reflns_av_R_equivalents  0.0554
_diffrn_reflns_av_unetI/netI     0.0643
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.32
_diffrn_reflns_theta_max         25.68
_reflns_number_total             18496
_reflns_number_gt                12679
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  
'SHELXTL (Sheldrick, 2008); PLATON (Spek, 2003)'

_refine_special_details          
;
 Structure solved by direct methods and subsequent Fourier-difference
 synthesis. PLATON/ADDSYM suggests the space group P21/c with 92% fit,
 which is impossible since a pure enantiomeric form of camphoric acid
 was used. However, the structure is close to being centrosymmetric and
 refinement was quite unstable. All non-hydrogen atoms were refined with
 anisotropic displacement parameters, with many restraints on bond lengths
 and displacement parameters:
DFIX 1.52 0.01 C2 C3
DFIX 1.52 0.01 C4 C5
DFIX 1.52 0.01 C3 C7
DFIX 1.52 0.01 C2 C8
DFIX 1.52 0.01 C11 C16
DFIX 1.52 0.01 C22 C23
DFIX 2.45 0.01 C22 C24
DFIX 1.52 0.01 C23 C24
DFIX 1.52 0.01 C23 C30
DFIX 1.52 0.01 C32 C38
DFIX 1.52 0.01 C32 C39
DFIX 1.52 0.01 C33 C40
DFIX 1.52 0.01 C42 C48
DFIX 1.52 0.01 C43 C47
DFIX 1.52 0.01 C44 C45
DFIX 1.52 0.01 C52 C58
DFIX 1.52 0.01 C53 C57
DFIX 1.52 0.01 C53 C60
DFIX 1.52 0.01 C54 C55
DFIX 2.45 0.01 C54 C60
DFIX 2.45 0.01 C52 C60
DFIX -2.1 H28B H30C
DFIX -2.1 H38B H40B
DFIX -2.1 H41 H50D
DFIX -2.1 H44B H50C
DFIX -2.1 H48C H49E
DFIX -2.1 H49C H50D
ISOR 0.01 O5 O10 O11 O13 O18 O33 O50
ISOR 0.03 O6 O8 O9 O16 O22 O36 O49 O53 C15 C16 C18 C34 C38
ISOR 0.03 C5 C8 C10 C17 C22 C24 C25 C28 C30 C32 C35
ISOR 0.03 C39 > C42 C44 C45 C49 C50 C55
SIMU 0.001 0.01 C1 > C10
SIMU 0.005 0.01 C21 C22 C23 C24 C25 C28 C29 C30
SIMU .001 .001 1.6 C32 C33 C38 > C40
SIMU .001 .001 1.6 C41 > C49
SIMU 0.005 0.01 C51 > C55 C58 C59
 The H atoms bound to O atoms were found on a Fourier-difference map 
 for the hydroxide groups and seven water molecules (four coordinated 
 and three free), but not for the other water molecules. The C-bound H
 atoms were introduced at calculated positions. All H atoms were treated
 as riding atoms with an isotropic displacement parameter equal to 1.2 
 times that of the parent atom (1.5 for CH₃). 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.0851P)²+68.8343P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_chemical_absolute_configuration syn
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.137(17)
_refine_ls_number_reflns         18496
_refine_ls_number_parameters     1150
_refine_ls_number_restraints     509
_refine_ls_R_factor_all          0.1108
_refine_ls_R_factor_gt           0.0714
_refine_ls_wR_factor_ref         0.1863
_refine_ls_wR_factor_gt          0.1705
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_restrained_S_all      1.016
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.001
_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.68
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         2.667
_refine_diff_density_min         -2.206
_refine_diff_density_rms         0.234

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
U1 U 0.34546(6) -0.03718(6) 0.36200(5) 0.0437(3) Uani 1 1 d . . .
U2 U 0.46000(7) -0.04940(6) 0.16498(6) 0.0500(3) Uani 1 1 d . . .
U3 U 0.40095(7) 0.45162(6) 0.13385(5) 0.0500(3) Uani 1 1 d . . .
U4 U 0.32555(7) 0.46379(6) 0.35399(6) 0.0520(3) Uani 1 1 d . . .
U5 U 0.08893(7) 0.47235(9) 0.86721(6) 0.0673(4) Uani 1 1 d . . .
U6 U 0.17222(6) 0.46985(5) 0.65183(5) 0.0444(2) Uani 1 1 d . . .
U7 U 0.15933(7) 0.96989(6) 0.63444(6) 0.0476(3) Uani 1 1 d . . .
U8 U 0.05117(7) 0.97232(7) 0.83542(6) 0.0522(3) Uani 1 1 d . . .
O1 O 0.4051(14) -0.0918(9) 0.4441(12) 0.067(6) Uani 1 1 d . . .
O2 O 0.2873(13) 0.0182(9) 0.2892(10) 0.050(5) Uani 1 1 d . . .
O3 O 0.5546(14) -0.1028(11) 0.1836(12) 0.065(6) Uani 1 1 d . . .
O4 O 0.3601(14) 0.0052(12) 0.1324(9) 0.071(6) Uani 1 1 d . . .
O5 O 0.5006(11) 0.5087(9) 0.1426(9) 0.058(4) Uani 1 1 d U . .
O6 O 0.3071(17) 0.3913(13) 0.1198(13) 0.062(4) Uani 1 1 d U . .
O7 O 0.4022(16) 0.5195(10) 0.4270(13) 0.078(7) Uani 1 1 d . . .
O8 O 0.2528(11) 0.4098(10) 0.2833(8) 0.047(5) Uani 1 1 d U . .
O9 O 0.0031(18) 0.4219(14) 0.8550(15) 0.111(9) Uani 1 1 d U . .
O10 O 0.1884(14) 0.5240(13) 0.8864(12) 0.070(6) Uani 1 1 d U . .
O11 O 0.1100(13) 0.4120(10) 0.5849(9) 0.055(5) Uani 1 1 d U . .
O12 O 0.2425(14) 0.5296(10) 0.7167(13) 0.064(6) Uani 1 1 d . . .
O13 O 0.0945(11) 1.0200(9) 0.5550(8) 0.046(4) Uani 1 1 d U . .
O14 O 0.2256(11) 0.9231(10) 0.7144(9) 0.050(5) Uani 1 1 d . . .
O15 O -0.0516(13) 1.0230(12) 0.8097(10) 0.064(6) Uani 1 1 d . . .
O16 O 0.1404(12) 0.9253(10) 0.8529(10) 0.062(6) Uani 1 1 d U . .
O17 O 0.4607(10) -0.0473(8) 0.3015(9) 0.046(4) Uani 1 1 d . . .
H17 H 0.5176 -0.0379 0.3296 0.055 Uiso 1 1 d R . .
O18 O 0.4141(10) 0.4605(9) 0.2683(8) 0.045(4) Uani 1 1 d U . .
H18 H 0.4611 0.4303 0.2870 0.054 Uiso 1 1 d R . .
O19 O 0.2980(13) -0.1346(9) 0.2714(11) 0.059(6) Uani 1 1 d . . .
O20 O 0.3703(14) -0.1438(10) 0.1766(10) 0.061(5) Uani 1 1 d . . .
O21 O 0.3018(18) -0.4582(12) 0.1435(14) 0.090(8) Uani 1 1 d . . .
O22 O 0.2735(15) -0.4435(10) 0.2591(13) 0.073(6) Uani 1 1 d U . .
O23 O 0.3321(11) 0.0510(9) 0.4660(9) 0.042(4) Uani 1 1 d . . .
O24 O 0.4417(12) 0.0627(9) 0.4124(12) 0.056(5) Uani 1 1 d . . .
O25 O 0.3309(15) 0.3805(12) 0.4739(11) 0.072(6) Uani 1 1 d . . .
O26 O 0.4303(11) 0.3632(9) 0.4012(8) 0.043(4) Uani 1 1 d . . .
O27 O 0.5388(13) 0.0353(10) 0.0967(11) 0.059(5) Uani 1 1 d . . .
O28 O 0.5417(12) 0.0541(10) 0.2211(8) 0.050(5) Uani 1 1 d . . .
O29 O 0.4746(13) 0.3596(9) 0.0673(10) 0.055(5) Uani 1 1 d . . .
O30 O 0.5025(12) 0.3580(10) 0.1970(9) 0.052(5) Uani 1 1 d . . .
O31 O 0.2062(12) -0.0626(10) 0.3950(9) 0.054(5) Uani 1 1 d . . .
O32 O 0.4288(12) -0.0902(10) 0.0310(8) 0.053(5) Uani 1 1 d . . .
H32A H 0.4143 -0.1294 0.0379 0.064 Uiso 1 1 d R . .
H32B H 0.3816 -0.0614 -0.0050 0.064 Uiso 1 1 d R . .
O33 O 0.3573(13) 0.4855(14) -0.0096(11) 0.084(6) Uani 1 1 d U . .
H33A H 0.4051 0.4904 -0.0262 0.100 Uiso 1 1 d R . .
H33B H 0.3397 0.4381 -0.0286 0.100 Uiso 1 1 d R . .
O34 O 0.1998(15) 0.4969(13) 0.4047(12) 0.090(8) Uani 1 1 d . . .
O35 O 0.0721(11) 0.4607(8) 0.7302(7) 0.044(4) Uani 1 1 d . . .
H35 H 0.0130 0.4741 0.6943 0.053 Uiso 1 1 d R . .
O36 O 0.0458(12) 0.9728(11) 0.7031(10) 0.069(5) Uani 1 1 d U . .
H36 H -0.0086 0.9594 0.6756 0.082 Uiso 1 1 d R . .
O37 O 0.1823(16) 0.3759(14) 0.8564(12) 0.092(8) Uani 1 1 d . . .
O38 O 0.2246(13) 0.3776(9) 0.7411(10) 0.055(5) Uani 1 1 d . . .
O39 O 0.2002(14) 0.0678(11) 0.7187(11) 0.062(5) Uani 1 1 d . . .
O40 O 0.1436(13) 0.0658(11) 0.8248(11) 0.060(5) Uani 1 1 d . . .
O41 O 0.0203(15) 0.5572(15) 0.9369(11) 0.093(9) Uani 1 1 d . . .
O42 O -0.0167(14) 0.5616(12) 0.8024(10) 0.067(6) Uani 1 1 d . . .
O43 O -0.0220(14) 0.8914(11) 0.9102(10) 0.062(5) Uani 1 1 d . . .
O44 O -0.0344(15) 0.8662(10) 0.7815(13) 0.071(6) Uani 1 1 d . . .
O45 O 0.1697(11) 0.5479(8) 0.5399(8) 0.034(4) Uani 1 1 d . . .
O46 O 0.0664(13) 0.5657(10) 0.5993(11) 0.057(5) Uani 1 1 d . . .
O47 O 0.1745(12) 0.8812(9) 0.5333(10) 0.047(4) Uani 1 1 d . . .
O48 O 0.0628(11) 0.8694(10) 0.5909(9) 0.051(5) Uani 1 1 d . . .
O49 O 0.1348(15) 0.443(2) 1.0078(13) 0.128(10) Uani 1 1 d U . .
O50 O 0.2980(11) 0.4426(10) 0.6013(9) 0.056(4) Uani 1 1 d U . .
H50A H 0.3191 0.4168 0.5713 0.068 Uiso 1 1 d R . .
H50B H 0.3435 0.4629 0.6161 0.068 Uiso 1 1 d R . .
O51 O 0.2953(12) 0.9983(11) 0.5956(10) 0.057(5) Uani 1 1 d . . .
O52 O 0.0859(13) 1.0106(11) 0.9756(13) 0.082(7) Uani 1 1 d . . .
H52A H 0.1359 0.9849 1.0116 0.098 Uiso 1 1 d R . .
H52B H 0.1129 1.0501 0.9936 0.098 Uiso 1 1 d R . .
O53 O 0.6160(12) 0.0569(10) 0.3878(10) 0.059(5) Uani 1 1 d U . .
H53A H 0.5679 0.0579 0.4020 0.071 Uiso 1 1 d R . .
H53B H 0.6058 0.0652 0.3347 0.071 Uiso 1 1 d R . .
O54 O 0.5884(12) 0.3926(13) 0.3627(9) 0.075(7) Uani 1 1 d . . .
H54A H 0.5436 0.3750 0.3886 0.090 Uiso 1 1 d R . .
H54B H 0.6421 0.3756 0.3839 0.090 Uiso 1 1 d R . .
O55 O -0.0953(13) 0.5354(13) 0.6400(12) 0.080(7) Uani 1 1 d . . .
O56 O -0.1070(13) 0.8772(13) 0.6125(11) 0.081(7) Uani 1 1 d . . .
H56A H -0.1648 0.8652 0.5735 0.098 Uiso 1 1 d R . .
H56B H -0.0646 0.8741 0.5994 0.098 Uiso 1 1 d R . .
O57 O 0.1822(13) -0.0415(16) 0.1100(12) 0.096(8) Uani 1 1 d . . .
O58 O 0.6661(12) 0.4693(18) 0.1024(11) 0.101(8) Uani 1 1 d . . .
C1 C 0.252(2) -0.2254(18) 0.179(2) 0.077(3) Uani 1 1 d U . .
C2 C 0.3052(19) -0.2951(13) 0.1896(16) 0.077(3) Uani 1 1 d DU . .
C3 C 0.2315(18) -0.3496(13) 0.170(2) 0.077(3) Uani 1 1 d DU . .
H3 H 0.2049 -0.3511 0.1101 0.093 Uiso 1 1 calc R . .
C4 C 0.161(2) -0.3276(11) 0.2105(18) 0.077(3) Uani 1 1 d DU . .
H4A H 0.1676 -0.3525 0.2624 0.093 Uiso 1 1 calc R . .
H4B H 0.1002 -0.3352 0.1750 0.093 Uiso 1 1 calc R . .
C5 C 0.183(2) -0.2502(11) 0.2238(18) 0.077(3) Uani 1 1 d DU . .
H5A H 0.2065 -0.2412 0.2825 0.093 Uiso 1 1 calc R . .
H5B H 0.1268 -0.2228 0.2044 0.093 Uiso 1 1 calc R . .
C6 C 0.311(2) -0.1658(19) 0.213(2) 0.077(3) Uani 1 1 d U . .
C7 C 0.276(2) -0.4194(15) 0.198(2) 0.077(3) Uani 1 1 d DU . .
C8 C 0.351(2) -0.3011(16) 0.1210(18) 0.093(6) Uani 1 1 d DU . .
H8A H 0.3746 -0.2560 0.1109 0.140 Uiso 1 1 calc R . .
H8B H 0.3074 -0.3178 0.0716 0.140 Uiso 1 1 calc RD . .
H8C H 0.4003 -0.3353 0.1363 0.140 Uiso 1 1 calc R . .
C9 C 0.381(2) -0.3000(17) 0.2609(18) 0.083(6) Uani 1 1 d U . .
H9A H 0.3595 -0.3044 0.3095 0.124 Uiso 1 1 calc R . .
H9B H 0.4182 -0.2579 0.2650 0.124 Uiso 1 1 calc R . .
H9C H 0.4174 -0.3411 0.2561 0.124 Uiso 1 1 calc R . .
C10 C 0.215(2) -0.2104(17) 0.087(2) 0.096(6) Uani 1 1 d U . .
H10A H 0.2024 -0.1604 0.0786 0.145 Uiso 1 1 calc R . .
H10B H 0.1599 -0.2372 0.0656 0.145 Uiso 1 1 calc R . .
H10C H 0.2599 -0.2243 0.0585 0.145 Uiso 1 1 calc R . .
C11 C 0.4249(15) 0.1552(10) 0.5061(12) 0.039(5) Uani 1 1 d D . .
H11 H 0.4175 0.1488 0.5620 0.047 Uiso 1 1 calc R . .
C12 C 0.3694(16) 0.2152(13) 0.4685(12) 0.048(6) Uani 1 1 d . . .
C13 C 0.4198(17) 0.2778(13) 0.5025(13) 0.047(6) Uani 1 1 d . . .
C14 C 0.5154(17) 0.2571(14) 0.4999(15) 0.056(7) Uani 1 1 d . . .
H14A H 0.5602 0.2819 0.5430 0.067 Uiso 1 1 calc R . .
H14B H 0.5254 0.2699 0.4469 0.067 Uiso 1 1 calc R . .
C15 C 0.526(2) 0.1749(16) 0.513(2) 0.072(9) Uani 1 1 d U . .
H15A H 0.5483 0.1520 0.4708 0.087 Uiso 1 1 calc R . .
H15B H 0.5650 0.1631 0.5673 0.087 Uiso 1 1 calc R . .
C16 C 0.3990(17) 0.0873(10) 0.4597(12) 0.044(6) Uani 1 1 d DU . .
C17 C 0.3925(19) 0.3449(12) 0.4555(16) 0.049(7) Uani 1 1 d U . .
C18 C 0.284(2) 0.216(2) 0.487(2) 0.118(14) Uani 1 1 d U . .
H18A H 0.2478 0.1760 0.4616 0.177 Uiso 1 1 calc R . .
H18B H 0.2518 0.2595 0.4667 0.177 Uiso 1 1 calc R . .
H18C H 0.2927 0.2136 0.5461 0.177 Uiso 1 1 calc R . .
C19 C 0.355(3) 0.2123(18) 0.3718(16) 0.100(13) Uani 1 1 d . . .
H19A H 0.4100 0.2261 0.3584 0.150 Uiso 1 1 calc R . .
H19B H 0.3061 0.2443 0.3457 0.150 Uiso 1 1 calc R . .
H19C H 0.3384 0.1646 0.3525 0.150 Uiso 1 1 calc R . .
C20 C 0.4195(18) 0.2907(12) 0.5913(12) 0.057(7) Uani 1 1 d . . .
H20A H 0.3600 0.3068 0.5934 0.086 Uiso 1 1 calc R . .
H20B H 0.4643 0.3264 0.6148 0.086 Uiso 1 1 calc R . .
H20C H 0.4342 0.2472 0.6221 0.086 Uiso 1 1 calc R . .
C21 C 0.597(2) 0.1452(17) 0.1500(19) 0.080(4) Uani 1 1 d U . .
H21 H 0.6551 0.1451 0.1926 0.096 Uiso 1 1 calc R . .
C22 C 0.542(2) 0.2069(14) 0.1769(15) 0.083(4) Uani 1 1 d DU . .
C23 C 0.5794(17) 0.2673(12) 0.1371(13) 0.081(4) Uani 1 1 d DU . .
C24 C 0.582(2) 0.2411(15) 0.0534(14) 0.083(4) Uani 1 1 d DU . .
H24A H 0.5191 0.2346 0.0226 0.100 Uiso 1 1 d R . .
H24B H 0.6141 0.2682 0.0201 0.100 Uiso 1 1 d R . .
C25 C 0.623(2) 0.1643(17) 0.0717(17) 0.083(4) Uani 1 1 d U . .
H25A H 0.5963 0.1316 0.0271 0.099 Uiso 1 1 calc R . .
H25B H 0.6893 0.1644 0.0806 0.099 Uiso 1 1 calc R . .
C26 C 0.5577(15) 0.0756(12) 0.1585(13) 0.041(5) Uani 1 1 d . . .
C27 C 0.5156(14) 0.3330(12) 0.1307(12) 0.036(5) Uani 1 1 d . . .
C28 C 0.561(3) 0.2070(18) 0.269(2) 0.099(6) Uani 1 1 d U . .
H28A H 0.5401 0.2509 0.2874 0.148 Uiso 1 1 calc R . .
H28B H 0.6259 0.2023 0.2935 0.148 Uiso 1 1 calc RD . .
H28C H 0.5300 0.1677 0.2867 0.148 Uiso 1 1 calc R . .
C29 C 0.443(2) 0.1973(16) 0.1373(17) 0.074(6) Uani 1 1 d U . .
H29A H 0.4190 0.1608 0.1656 0.111 Uiso 1 1 d R . .
H29B H 0.4352 0.1837 0.0806 0.111 Uiso 1 1 d R . .
H29C H 0.4114 0.2413 0.1395 0.111 Uiso 1 1 d R . .
C30 C 0.6708(18) 0.2818(17) 0.1950(18) 0.093(6) Uani 1 1 d DU . .
H30A H 0.6629 0.3063 0.2429 0.140 Uiso 1 1 calc R . .
H30B H 0.7062 0.3109 0.1677 0.140 Uiso 1 1 calc R . .
H30C H 0.7022 0.2376 0.2115 0.140 Uiso 1 1 calc RD . .
C31 C 0.2628(17) 0.2807(10) 0.8322(12) 0.045(6) Uani 1 1 d . . .
H31 H 0.3261 0.2823 0.8280 0.054 Uiso 1 1 calc R . .
C32 C 0.2180(16) 0.2213(17) 0.7784(14) 0.082(4) Uani 1 1 d DU . .
C33 C 0.2527(18) 0.153(2) 0.821(2) 0.082(4) Uani 1 1 d DU . .
C34 C 0.254(3) 0.1772(17) 0.9121(18) 0.092(10) Uani 1 1 d U . .
H34C H 0.1965 0.1644 0.9237 0.110 Uiso 1 1 calc R . .
H34D H 0.3030 0.1531 0.9517 0.110 Uiso 1 1 calc R . .
C35 C 0.268(2) 0.2578(14) 0.9200(15) 0.085(9) Uani 1 1 d U . .
H35A H 0.2199 0.2802 0.9399 0.102 Uiso 1 1 calc R . .
H35B H 0.3268 0.2694 0.9571 0.102 Uiso 1 1 calc R . .
C36 C 0.2264(15) 0.3527(13) 0.8144(15) 0.045(6) Uani 1 1 d . . .
C37 C 0.1938(19) 0.0906(14) 0.7865(14) 0.053(6) Uani 1 1 d . . .
C38 C 0.2410(19) 0.2240(16) 0.6970(14) 0.082(4) Uani 1 1 d DU . .
H38A H 0.2089 0.1866 0.6619 0.122 Uiso 1 1 calc R . .
H38B H 0.3057 0.2176 0.7055 0.122 Uiso 1 1 calc RD . .
H38C H 0.2231 0.2693 0.6713 0.122 Uiso 1 1 calc R . .
C39 C 0.1171(15) 0.2287(19) 0.7602(18) 0.082(4) Uani 1 1 d DU . .
H39A H 0.0979 0.2703 0.7266 0.122 Uiso 1 1 calc R . .
H39B H 0.0997 0.2335 0.8110 0.122 Uiso 1 1 calc R . .
H39C H 0.0883 0.1872 0.7310 0.122 Uiso 1 1 calc R . .
C40 C 0.3467(18) 0.1430(16) 0.8119(18) 0.082(4) Uani 1 1 d DU . .
H40A H 0.3766 0.1884 0.8136 0.123 Uiso 1 1 d R . .
H40B H 0.3436 0.1202 0.7599 0.123 Uiso 1 1 d RD . .
H40C H 0.3808 0.1136 0.8562 0.123 Uiso 1 1 d R . .
C41 C -0.0739(18) 0.6498(13) 0.8671(15) 0.110(5) Uani 1 1 d DU . .
H41 H -0.1348 0.6402 0.8306 0.132 Uiso 1 1 calc RD . .
C42 C -0.0335(12) 0.7182(12) 0.8325(11) 0.079(4) Uani 1 1 d DU . .
C43 C -0.0875(14) 0.7782(10) 0.8551(13) 0.079(4) Uani 1 1 d DU . .
C44 C -0.078(2) 0.7552(11) 0.9463(14) 0.110(5) Uani 1 1 d DU . .
H44A H -0.0186 0.7703 0.9806 0.132 Uiso 1 1 calc R . .
H44B H -0.1249 0.7780 0.9668 0.132 Uiso 1 1 calc RD . .
C45 C -0.086(3) 0.6760(11) 0.9511(18) 0.110(5) Uani 1 1 d DU . .
H45A H -0.1457 0.6626 0.9578 0.132 Uiso 1 1 calc R . .
H45B H -0.0390 0.6566 0.9968 0.132 Uiso 1 1 calc R . .
C46 C -0.018(3) 0.5883(15) 0.867(2) 0.110(5) Uani 1 1 d DU . .
C47 C -0.048(2) 0.8500(11) 0.8502(18) 0.079(4) Uani 1 1 d DU . .
C48 C 0.0654(13) 0.7270(15) 0.8756(14) 0.079(4) Uani 1 1 d DU . .
H48A H 0.0877 0.7670 0.8517 0.137 Uiso 1 1 d R . .
H48B H 0.0715 0.7323 0.9296 0.137 Uiso 1 1 d R . .
H48C H 0.0971 0.6859 0.8636 0.137 Uiso 1 1 d RD . .
C49 C -0.0419(18) 0.7073(13) 0.7414(12) 0.080(4) Uani 1 1 d DU . .
H49C H -0.1032 0.7061 0.7063 0.119 Uiso 1 1 d RD . .
H49D H -0.0105 0.6643 0.7340 0.119 Uiso 1 1 d R . .
H49E H -0.0102 0.7477 0.7272 0.119 Uiso 1 1 d RD . .
C50 C -0.1834(14) 0.7728(15) 0.8091(19) 0.158(18) Uani 1 1 d DU . .
H50C H -0.2208 0.7688 0.8471 0.238 Uiso 1 1 calc RD . .
H50D H -0.1919 0.7315 0.7742 0.238 Uiso 1 1 calc RD . .
H50E H -0.2007 0.8147 0.7757 0.238 Uiso 1 1 calc R . .
C51 C 0.0753(15) 0.6501(12) 0.4992(14) 0.058(4) Uani 1 1 d DU . .
H51 H 0.0861 0.6418 0.4448 0.070 Uiso 1 1 calc R . .
C52 C 0.1351(11) 0.7172(11) 0.5379(11) 0.058(3) Uani 1 1 d DU . .
C53 C 0.0825(14) 0.7799(9) 0.4960(10) 0.058(4) Uani 1 1 d DU . .
C54 C -0.0159(14) 0.7550(10) 0.4922(15) 0.060(4) Uani 1 1 d DU . .
H54C H -0.0316 0.7698 0.5422 0.072 Uiso 1 1 calc R . .
H54D H -0.0585 0.7775 0.4456 0.072 Uiso 1 1 calc R . .
C55 C -0.0247(15) 0.6760(10) 0.4837(16) 0.061(4) Uani 1 1 d DU . .
H55C H -0.0605 0.6627 0.4288 0.073 Uiso 1 1 calc R . .
H55D H -0.0532 0.6561 0.5242 0.073 Uiso 1 1 calc R . .
C56 C 0.1027(16) 0.5868(13) 0.5465(13) 0.054(8) Uani 1 1 d D . .
C57 C 0.1056(17) 0.8485(9) 0.5408(14) 0.048(7) Uani 1 1 d D . .
C58 C 0.2273(11) 0.7132(12) 0.5215(13) 0.062(5) Uani 1 1 d DU . .
H58C H 0.2433 0.7591 0.5043 0.093 Uiso 1 1 calc R . .
H58D H 0.2259 0.6789 0.4787 0.093 Uiso 1 1 calc R . .
H58E H 0.2718 0.6989 0.5711 0.093 Uiso 1 1 calc R . .
C59 C 0.1501(16) 0.7157(13) 0.6307(11) 0.056(5) Uani 1 1 d DU . .
H59A H 0.1707 0.6692 0.6513 0.085 Uiso 1 1 calc R . .
H59B H 0.0937 0.7265 0.6441 0.085 Uiso 1 1 calc R . .
H59C H 0.1955 0.7505 0.6557 0.085 Uiso 1 1 calc R . .
C60 C 0.0885(15) 0.7831(12) 0.4100(9) 0.081(9) Uani 1 1 d D . .
H60A H 0.1477 0.8006 0.4088 0.121 Uiso 1 1 calc R . .
H60B H 0.0420 0.8145 0.3789 0.121 Uiso 1 1 calc R . .
H60C H 0.0797 0.7362 0.3862 0.121 Uiso 1 1 calc R . .


_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 O2 1.701(18) . ?
U1 O1 1.80(2) . ?
U1 O17 2.291(13) . ?
U1 O19 2.413(15) . ?
U1 O31 2.414(16) . ?
U1 O24 2.437(16) . ?
U1 O23 2.501(17) . ?
U2 O3 1.74(2) . ?
U2 O4 1.83(2) . ?
U2 O20 2.318(18) . ?
U2 O17 2.334(14) . ?
U2 O32 2.348(14) . ?
U2 O28 2.410(15) . ?
U2 O27 2.496(17) . ?
U3 O6 1.82(2) . ?
U3 O5 1.862(14) . ?
U3 O18 2.262(13) . ?
U3 O21 2.343(19) 1_565 ?
U3 O30 2.440(18) . ?
U3 O33 2.456(18) . ?
U3 O29 2.525(16) . ?
U4 O8 1.756(16) . ?
U4 O7 1.82(2) . ?
U4 O18 2.254(13) . ?
U4 O22 2.40(2) 1_565 ?
U4 O34 2.413(18) . ?
U4 O26 2.508(16) . ?
U4 O25 2.582(19) . ?
U5 O9 1.61(3) . ?
U5 O10 1.78(2) . ?
U5 O35 2.301(12) . ?
U5 O37 2.38(2) . ?
U5 O49 2.39(2) . ?
U5 O41 2.42(3) . ?
U5 O42 2.42(2) . ?
U6 O11 1.698(18) . ?
U6 O12 1.76(2) . ?
U6 O35 2.305(14) . ?
U6 O38 2.336(17) . ?
U6 O50 2.384(16) . ?
U6 O45 2.420(13) . ?
U6 O46 2.47(2) . ?
U7 O14 1.729(18) . ?
U7 O13 1.748(14) . ?
U7 O39 2.35(2) 1_565 ?
U7 O36 2.354(15) . ?
U7 O51 2.426(16) . ?
U7 O48 2.43(2) . ?
U7 O47 2.478(16) . ?
U8 O16 1.61(2) . ?
U8 O15 1.814(18) . ?
U8 O36 2.244(15) . ?
U8 O40 2.327(19) 1_565 ?
U8 O52 2.43(2) . ?
U8 O43 2.466(18) . ?
U8 O44 2.47(2) . ?
O17 H17 0.9030 . ?
O18 H18 0.9179 . ?
O19 C6 1.23(4) . ?
O20 C6 1.30(3) . ?
O21 C7 1.34(4) . ?
O21 U3 2.343(19) 1_545 ?
O22 C7 1.15(3) . ?
O22 U4 2.40(2) 1_545 ?
O23 C16 1.27(3) . ?
O24 C16 1.26(3) . ?
O25 C17 1.28(3) . ?
O26 C17 1.27(3) . ?
O27 C26 1.28(3) . ?
O28 C26 1.23(3) . ?
O29 C27 1.21(3) . ?
O30 C27 1.30(2) . ?
O32 H32A 0.8021 . ?
O32 H32B 0.9901 . ?
O33 H33A 0.8631 . ?
O33 H33B 0.9778 . ?
O35 H35 0.9909 . ?
O36 H36 0.8871 . ?
O37 C36 1.20(3) . ?
O38 C36 1.33(3) . ?
O39 C37 1.27(3) . ?
O39 U7 2.35(2) 1_545 ?
O40 C37 1.23(3) . ?
O40 U8 2.327(19) 1_545 ?
O41 C46 1.33(4) . ?
O42 C46 1.22(4) . ?
O43 C47 1.27(3) . ?
O44 C47 1.28(3) . ?
O45 C56 1.31(3) . ?
O46 C56 1.25(3) . ?
O47 C57 1.27(3) . ?
O48 C57 1.28(3) . ?
O50 H50A 0.8374 . ?
O50 H50B 0.7841 . ?
O52 H52A 0.9844 . ?
O52 H52B 0.8784 . ?
O53 H53A 0.8415 . ?
O53 H53B 0.8958 . ?
O54 H54A 0.9762 . ?
O54 H54B 0.8759 . ?
O56 H56A 0.9910 . ?
O56 H56B 0.7498 . ?
C1 C6 1.48(5) . ?
C1 C10 1.55(4) . ?
C1 C5 1.55(4) . ?
C1 C2 1.55(4) . ?
C2 C9 1.46(4) . ?
C2 C3 1.516(10) . ?
C2 C8 1.525(10) . ?
C3 C4 1.49(4) . ?
C3 C7 1.524(10) . ?
C3 H3 1.0000 . ?
C4 C5 1.523(10) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C12 1.48(3) . ?
C11 C16 1.521(10) . ?
C11 C15 1.57(3) . ?
C11 H11 1.0000 . ?
C12 C18 1.45(4) . ?
C12 C13 1.46(3) . ?
C12 C19 1.61(3) . ?
C13 C17 1.52(3) . ?
C13 C20 1.54(3) . ?
C13 C14 1.54(3) . ?
C14 C15 1.59(4) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C26 1.49(4) . ?
C21 C25 1.55(4) . ?
C21 C22 1.59(4) . ?
C21 H21 1.0000 . ?
C22 C29 1.51(4) . ?
C22 C28 1.53(4) . ?
C22 C23 1.531(10) . ?
C23 C30 1.522(10) . ?
C23 C24 1.530(10) . ?
C23 C27 1.58(3) . ?
C24 C25 1.60(4) . ?
C24 H24A 0.9899 . ?
C24 H24B 0.9896 . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9798 . ?
C29 H29B 0.9801 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 C36 1.49(3) . ?
C31 C32 1.51(3) . ?
C31 C35 1.55(3) . ?
C31 H31 1.0000 . ?
C32 C39 1.516(10) . ?
C32 C33 1.52(4) . ?
C32 C38 1.526(10) . ?
C33 C40 1.515(10) . ?
C33 C37 1.53(4) . ?
C33 C34 1.62(4) . ?
C34 C35 1.56(4) . ?
C34 H34C 0.9900 . ?
C34 H34D 0.9900 . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 H40A 0.9801 . ?
C40 H40B 0.9801 . ?
C40 H40C 0.9800 . ?
C41 C46 1.46(3) . ?
C41 C45 1.58(3) . ?
C41 C42 1.63(3) . ?
C41 H41 1.0000 . ?
C42 C43 1.53(2) . ?
C42 C48 1.523(8) . ?
C42 C49 1.54(2) . ?
C43 C50 1.487(13) . ?
C43 C47 1.519(8) . ?
C43 C44 1.59(3) . ?
C44 C45 1.526(8) . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C48 H48A 0.9700 . ?
C48 H48B 0.9100 . ?
C48 H48C 0.9799 . ?
C49 H49C 0.9800 . ?
C49 H49D 0.9794 . ?
C49 H49E 0.9802 . ?
C50 H50C 0.9800 . ?
C50 H50D 0.9800 . ?
C50 H50E 0.9800 . ?
C51 C56 1.46(3) . ?
C51 C55 1.58(3) . ?
C51 C52 1.62(3) . ?
C51 H51 1.0000 . ?
C52 C53 1.52(2) . ?
C52 C58 1.525(8) . ?
C52 C59 1.54(2) . ?
C53 C60 1.499(9) . ?
C53 C57 1.515(8) . ?
C53 C54 1.58(2) . ?
C54 C55 1.523(8) . ?
C54 H54C 0.9900 . ?
C54 H54D 0.9900 . ?
C55 H55C 0.9900 . ?
C55 H55D 0.9900 . ?
C58 H58C 0.9800 . ?
C58 H58D 0.9800 . ?
C58 H58E 0.9800 . ?
C59 H59A 0.9800 . ?
C59 H59B 0.9800 . ?
C59 H59C 0.9800 . ?
C60 H60A 0.9800 . ?
C60 H60B 0.9800 . ?
C60 H60C 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
O2 U1 O1 176.0(8) . . ?
O2 U1 O17 92.7(6) . . ?
O1 U1 O17 90.2(6) . . ?
O2 U1 O19 89.9(8) . . ?
O1 U1 O19 93.4(8) . . ?
O17 U1 O19 77.6(6) . . ?
O2 U1 O31 88.0(7) . . ?
O1 U1 O31 90.3(7) . . ?
O17 U1 O31 159.3(6) . . ?
O19 U1 O31 81.7(6) . . ?
O2 U1 O24 85.8(8) . . ?
O1 U1 O24 92.3(8) . . ?
O17 U1 O24 75.6(6) . . ?
O19 U1 O24 152.6(5) . . ?
O31 U1 O24 125.0(6) . . ?
O2 U1 O23 88.5(7) . . ?
O1 U1 O23 87.6(6) . . ?
O17 U1 O23 126.7(6) . . ?
O19 U1 O23 155.7(5) . . ?
O31 U1 O23 74.0(5) . . ?
O24 U1 O23 51.3(5) . . ?
O3 U2 O4 173.0(8) . . ?
O3 U2 O20 91.1(8) . . ?
O4 U2 O20 89.7(8) . . ?
O3 U2 O17 92.5(7) . . ?
O4 U2 O17 94.4(6) . . ?
O20 U2 O17 76.9(6) . . ?
O3 U2 O32 86.0(8) . . ?
O4 U2 O32 87.3(7) . . ?
O20 U2 O32 81.4(6) . . ?
O17 U2 O32 158.2(6) . . ?
O3 U2 O28 94.8(8) . . ?
O4 U2 O28 87.9(8) . . ?
O20 U2 O28 150.4(5) . . ?
O17 U2 O28 73.9(5) . . ?
O32 U2 O28 127.9(5) . . ?
O3 U2 O27 88.7(8) . . ?
O4 U2 O27 87.9(7) . . ?
O20 U2 O27 157.4(6) . . ?
O17 U2 O27 125.7(6) . . ?
O32 U2 O27 76.1(6) . . ?
O28 U2 O27 51.9(5) . . ?
O6 U3 O5 175.3(8) . . ?
O6 U3 O18 92.2(7) . . ?
O5 U3 O18 91.3(6) . . ?
O6 U3 O21 87.9(10) . 1_565 ?
O5 U3 O21 96.0(9) . 1_565 ?
O18 U3 O21 76.0(7) . 1_565 ?
O6 U3 O30 89.4(10) . . ?
O5 U3 O30 88.5(7) . . ?
O18 U3 O30 74.3(6) . . ?
O21 U3 O30 150.1(6) 1_565 . ?
O6 U3 O33 92.0(9) . . ?
O5 U3 O33 86.0(7) . . ?
O18 U3 O33 157.6(7) . . ?
O21 U3 O33 82.1(7) 1_565 . ?
O30 U3 O33 127.8(6) . . ?
O6 U3 O29 86.3(8) . . ?
O5 U3 O29 89.1(7) . . ?
O18 U3 O29 125.5(6) . . ?
O21 U3 O29 157.9(7) 1_565 . ?
O30 U3 O29 51.2(5) . . ?
O33 U3 O29 76.8(6) . . ?
O8 U4 O7 179.4(9) . . ?
O8 U4 O18 85.7(6) . . ?
O7 U4 O18 93.8(8) . . ?
O8 U4 O22 85.9(8) . 1_565 ?
O7 U4 O22 94.2(9) . 1_565 ?
O18 U4 O22 74.5(6) . 1_565 ?
O8 U4 O34 88.4(8) . . ?
O7 U4 O34 92.2(9) . . ?
O18 U4 O34 157.8(7) . . ?
O22 U4 O34 83.7(7) 1_565 . ?
O8 U4 O26 90.7(7) . . ?
O7 U4 O26 88.9(7) . . ?
O18 U4 O26 74.8(6) . . ?
O22 U4 O26 149.3(6) 1_565 . ?
O34 U4 O26 126.8(6) . . ?
O8 U4 O25 93.7(7) . . ?
O7 U4 O25 86.4(8) . . ?
O18 U4 O25 127.0(7) . . ?
O22 U4 O25 158.4(7) 1_565 . ?
O34 U4 O25 74.8(7) . . ?
O26 U4 O25 52.2(6) . . ?
O9 U5 O10 175.8(12) . . ?
O9 U5 O35 86.6(9) . . ?
O10 U5 O35 95.9(7) . . ?
O9 U5 O37 91.2(10) . . ?
O10 U5 O37 86.2(9) . . ?
O35 U5 O37 75.8(6) . . ?
O9 U5 O49 90.4(12) . . ?
O10 U5 O49 86.0(10) . . ?
O35 U5 O49 158.1(9) . . ?
O37 U5 O49 82.7(9) . . ?
O9 U5 O41 90.8(9) . . ?
O10 U5 O41 90.3(9) . . ?
O35 U5 O41 128.4(7) . . ?
O37 U5 O41 155.9(7) . . ?
O49 U5 O41 73.3(9) . . ?
O9 U5 O42 86.0(10) . . ?
O10 U5 O42 97.9(9) . . ?
O35 U5 O42 73.8(6) . . ?
O37 U5 O42 149.5(6) . . ?
O49 U5 O42 127.7(9) . . ?
O41 U5 O42 54.6(7) . . ?
O9 U5 C46 90.5(10) . . ?
O11 U6 O12 175.7(9) . . ?
O11 U6 O35 89.7(7) . . ?
O12 U6 O35 94.6(7) . . ?
O11 U6 O38 89.1(8) . . ?
O12 U6 O38 91.6(7) . . ?
O35 U6 O38 74.5(6) . . ?
O11 U6 O50 89.1(7) . . ?
O12 U6 O50 86.8(7) . . ?
O35 U6 O50 158.5(6) . . ?
O38 U6 O50 84.0(7) . . ?
O11 U6 O45 88.9(7) . . ?
O12 U6 O45 88.7(7) . . ?
O35 U6 O45 129.3(5) . . ?
O38 U6 O45 156.1(6) . . ?
O50 U6 O45 72.1(6) . . ?
O11 U6 O46 92.1(8) . . ?
O12 U6 O46 89.2(8) . . ?
O35 U6 O46 77.7(5) . . ?
O38 U6 O46 152.1(6) . . ?
O50 U6 O46 123.9(5) . . ?
O45 U6 O46 51.8(5) . . ?
O14 U7 O13 177.9(8) . . ?
O14 U7 O39 85.4(7) . 1_565 ?
O13 U7 O39 92.6(7) . 1_565 ?
O14 U7 O36 88.9(8) . . ?
O13 U7 O36 91.4(8) . . ?
O39 U7 O36 77.9(6) 1_565 . ?
O14 U7 O51 87.6(7) . . ?
O13 U7 O51 91.4(7) . . ?
O39 U7 O51 82.9(7) 1_565 . ?
O36 U7 O51 160.7(6) . . ?
O14 U7 O48 91.2(7) . . ?
O13 U7 O48 90.9(7) . . ?
O39 U7 O48 149.9(6) 1_565 . ?
O36 U7 O48 72.1(5) . . ?
O51 U7 O48 126.9(6) . . ?
O14 U7 O47 93.0(7) . . ?
O13 U7 O47 88.5(7) . . ?
O39 U7 O47 156.3(6) 1_565 . ?
O36 U7 O47 125.7(6) . . ?
O51 U7 O47 73.4(6) . . ?
O48 U7 O47 53.6(5) . . ?
O16 U8 O15 176.5(8) . . ?
O16 U8 O36 89.5(8) . . ?
O15 U8 O36 87.5(7) . . ?
O16 U8 O40 86.0(8) . 1_565 ?
O15 U8 O40 94.9(9) . 1_565 ?
O36 U8 O40 77.2(6) . 1_565 ?
O16 U8 O52 91.7(8) . . ?
O15 U8 O52 91.7(8) . . ?
O36 U8 O52 159.2(7) . . ?
O40 U8 O52 82.2(6) 1_565 . ?
O16 U8 O43 92.3(8) . . ?
O15 U8 O43 88.3(8) . . ?
O36 U8 O43 128.7(6) . . ?
O40 U8 O43 154.0(6) 1_565 . ?
O52 U8 O43 71.9(6) . . ?
O16 U8 O44 87.6(7) . . ?
O15 U8 O44 90.0(8) . . ?
O36 U8 O44 75.6(6) . . ?
O40 U8 O44 152.1(6) 1_565 . ?
O52 U8 O44 125.1(6) . . ?
O43 U8 O44 53.3(6) . . ?
U1 O17 U2 130.8(7) . . ?
U1 O17 H17 120.5 . . ?
U2 O17 H17 106.4 . . ?
U4 O18 U3 139.1(7) . . ?
U4 O18 H18 110.6 . . ?
U3 O18 H18 99.1 . . ?
C6 O19 U1 144(2) . . ?
C6 O20 U2 144(2) . . ?
C7 O21 U3 141(2) . 1_545 ?
C7 O22 U4 146(2) . 1_545 ?
C16 O23 U1 95.0(13) . . ?
C16 O24 U1 98.4(13) . . ?
C17 O25 U4 90.3(15) . . ?
C17 O26 U4 93.8(15) . . ?
C26 O27 U2 92.1(14) . . ?
C26 O28 U2 97.5(13) . . ?
C27 O29 U3 94.7(13) . . ?
C27 O30 U3 96.5(13) . . ?
U2 O32 H32A 99.3 . . ?
U2 O32 H32B 110.5 . . ?
H32A O32 H32B 115.0 . . ?
U3 O33 H33A 108.8 . . ?
U3 O33 H33B 93.7 . . ?
H33A O33 H33B 100.4 . . ?
U5 O35 U6 132.2(7) . . ?
U5 O35 H35 116.4 . . ?
U6 O35 H35 105.6 . . ?
U8 O36 U7 131.9(8) . . ?
U8 O36 H36 108.1 . . ?
U7 O36 H36 117.2 . . ?
C36 O37 U5 141.8(19) . . ?
C36 O38 U6 143.3(17) . . ?
C37 O39 U7 139.9(18) . 1_545 ?
C37 O40 U8 145.3(18) . 1_545 ?
C46 O41 U5 90.3(17) . . ?
C46 O42 U5 93(2) . . ?
C47 O43 U8 93.5(13) . . ?
C47 O44 U8 93.2(16) . . ?
C56 O45 U6 97.6(14) . . ?
C56 O46 U6 97.1(15) . . ?
C57 O47 U7 91.8(11) . . ?
C57 O48 U7 93.9(13) . . ?
U6 O50 H50A 146.8 . . ?
U6 O50 H50B 121.5 . . ?
H50A O50 H50B 91.7 . . ?
U8 O52 H52A 113.5 . . ?
U8 O52 H52B 124.5 . . ?
H52A O52 H52B 89.4 . . ?
H53A O53 H53B 110.9 . . ?
H54A O54 H54B 113.0 . . ?
H56A O56 H56B 118.9 . . ?
C6 C1 C10 106(3) . . ?
C6 C1 C5 119(3) . . ?
C10 C1 C5 116(3) . . ?
C6 C1 C2 111(3) . . ?
C10 C1 C2 109(3) . . ?
C5 C1 C2 95(2) . . ?
C9 C2 C3 122(3) . . ?
C9 C2 C8 102(2) . . ?
C3 C2 C8 105(2) . . ?
C9 C2 C1 116(3) . . ?
C3 C2 C1 103(2) . . ?
C8 C2 C1 108(2) . . ?
C4 C3 C2 107(2) . . ?
C4 C3 C7 115(2) . . ?
C2 C3 C7 106(2) . . ?
C4 C3 H3 109.3 . . ?
C2 C3 H3 109.3 . . ?
C7 C3 H3 109.3 . . ?
C3 C4 C5 101(2) . . ?
C3 C4 H4A 111.6 . . ?
C5 C4 H4A 111.6 . . ?
C3 C4 H4B 111.6 . . ?
C5 C4 H4B 111.6 . . ?
H4A C4 H4B 109.4 . . ?
C4 C5 C1 112(2) . . ?
C4 C5 H5A 109.2 . . ?
C1 C5 H5A 109.2 . . ?
C4 C5 H5B 109.2 . . ?
C1 C5 H5B 109.2 . . ?
H5A C5 H5B 107.9 . . ?
O19 C6 O20 121(3) . . ?
O19 C6 C1 118(3) . . ?
O20 C6 C1 120(3) . . ?
O22 C7 O21 120(3) . . ?
O22 C7 C3 121(3) . . ?
O21 C7 C3 117(3) . . ?
C2 C8 H8A 109.5 . . ?
C2 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C2 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C2 C9 H9A 109.5 . . ?
C2 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C2 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C1 C10 H10A 109.5 . . ?
C1 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C1 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C12 C11 C16 113.3(18) . . ?
C12 C11 C15 107(2) . . ?
C16 C11 C15 111.3(19) . . ?
C12 C11 H11 108.3 . . ?
C16 C11 H11 108.3 . . ?
C15 C11 H11 108.3 . . ?
C18 C12 C13 109(2) . . ?
C18 C12 C11 112(2) . . ?
C13 C12 C11 106.1(17) . . ?
C18 C12 C19 110(2) . . ?
C13 C12 C19 111(2) . . ?
C11 C12 C19 109(2) . . ?
C12 C13 C17 116(2) . . ?
C12 C13 C20 112.6(19) . . ?
C17 C13 C20 108.3(19) . . ?
C12 C13 C14 101(2) . . ?
C17 C13 C14 109.7(19) . . ?
C20 C13 C14 109(2) . . ?
C13 C14 C15 108(2) . . ?
C13 C14 H14A 110.1 . . ?
C15 C14 H14A 110.1 . . ?
C13 C14 H14B 110.1 . . ?
C15 C14 H14B 110.1 . . ?
H14A C14 H14B 108.4 . . ?
C11 C15 C14 100(2) . . ?
C11 C15 H15A 111.8 . . ?
C14 C15 H15A 111.8 . . ?
C11 C15 H15B 111.8 . . ?
C14 C15 H15B 111.8 . . ?
H15A C15 H15B 109.6 . . ?
O24 C16 O23 115.1(17) . . ?
O24 C16 C11 123(2) . . ?
O23 C16 C11 122(2) . . ?
O26 C17 O25 123(2) . . ?
O26 C17 C13 120(2) . . ?
O25 C17 C13 116(2) . . ?
C12 C18 H18A 109.5 . . ?
C12 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C12 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C12 C19 H19A 109.5 . . ?
C12 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C12 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C13 C20 H20A 109.5 . . ?
C13 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C13 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C26 C21 C25 120(3) . . ?
C26 C21 C22 112(2) . . ?
C25 C21 C22 111(2) . . ?
C26 C21 H21 103.8 . . ?
C25 C21 H21 103.8 . . ?
C22 C21 H21 103.8 . . ?
C29 C22 C28 111(2) . . ?
C29 C22 C23 110(2) . . ?
C28 C22 C23 118(2) . . ?
C29 C22 C21 109(3) . . ?
C28 C22 C21 109(2) . . ?
C23 C22 C21 98.0(19) . . ?
C30 C23 C22 104(2) . . ?
C30 C23 C24 115(2) . . ?
C22 C23 C24 106.1(9) . . ?
C30 C23 C27 110.8(19) . . ?
C22 C23 C27 109(2) . . ?
C24 C23 C27 111(2) . . ?
C23 C24 C25 103.0(19) . . ?
C23 C24 H24A 105.7 . . ?
C25 C24 H24A 105.8 . . ?
C23 C24 H24B 120.6 . . ?
C25 C24 H24B 111.4 . . ?
H24A C24 H24B 109.3 . . ?
C21 C25 C24 102(2) . . ?
C21 C25 H25A 111.4 . . ?
C24 C25 H25A 111.4 . . ?
C21 C25 H25B 111.4 . . ?
C24 C25 H25B 111.4 . . ?
H25A C25 H25B 109.3 . . ?
O28 C26 O27 118(2) . . ?
O28 C26 C21 124(2) . . ?
O27 C26 C21 118(2) . . ?
O29 C27 O30 117(2) . . ?
O29 C27 C23 124.4(18) . . ?
O30 C27 C23 118.0(18) . . ?
C22 C28 H28A 109.5 . . ?
C22 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C22 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C22 C29 H29A 109.8 . . ?
C22 C29 H29B 109.0 . . ?
H29A C29 H29B 109.5 . . ?
C22 C29 H29C 109.6 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C23 C30 H30A 109.5 . . ?
C23 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C23 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C36 C31 C32 119(2) . . ?
C36 C31 C35 112(2) . . ?
C32 C31 C35 106(2) . . ?
C36 C31 H31 106.2 . . ?
C32 C31 H31 106.2 . . ?
C35 C31 H31 106.2 . . ?
C31 C32 C39 110(2) . . ?
C31 C32 C33 108(2) . . ?
C39 C32 C33 113(2) . . ?
C31 C32 C38 111(2) . . ?
C39 C32 C38 106(2) . . ?
C33 C32 C38 109(2) . . ?
C40 C33 C32 107(2) . . ?
C40 C33 C37 111(3) . . ?
C32 C33 C37 113(2) . . ?
C40 C33 C34 112(3) . . ?
C32 C33 C34 97(2) . . ?
C37 C33 C34 117(3) . . ?
C35 C34 C33 109(2) . . ?
C35 C34 H34C 109.8 . . ?
C33 C34 H34C 109.8 . . ?
C35 C34 H34D 109.8 . . ?
C33 C34 H34D 109.8 . . ?
H34C C34 H34D 108.3 . . ?
C31 C35 C34 103(2) . . ?
C31 C35 H35A 111.1 . . ?
C34 C35 H35A 111.1 . . ?
C31 C35 H35B 111.1 . . ?
C34 C35 H35B 111.1 . . ?
H35A C35 H35B 109.1 . . ?
O37 C36 O38 124(2) . . ?
O37 C36 C31 118(2) . . ?
O38 C36 C31 116(2) . . ?
O40 C37 O39 124(3) . . ?
O40 C37 C33 119(2) . . ?
O39 C37 C33 116(3) . . ?
C32 C38 H38A 109.5 . . ?
C32 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C32 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C32 C39 H39A 109.5 . . ?
C32 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C32 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C33 C40 H40A 109.9 . . ?
C33 C40 H40B 109.3 . . ?
H40A C40 H40B 109.5 . . ?
C33 C40 H40C 109.2 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C46 C41 C45 118(2) . . ?
C46 C41 C42 111(2) . . ?
C45 C41 C42 103.0(14) . . ?
C46 C41 H41 107.9 . . ?
C45 C41 H41 107.9 . . ?
C42 C41 H41 107.9 . . ?
C43 C42 C48 109.9(15) . . ?
C43 C42 C49 116.8(15) . . ?
C48 C42 C49 108.1(13) . . ?
C43 C42 C41 103.0(14) . . ?
C48 C42 C41 110.2(15) . . ?
C49 C42 C41 108.7(15) . . ?
C50 C43 C42 110.4(13) . . ?
C50 C43 C47 113.3(18) . . ?
C42 C43 C47 114.2(17) . . ?
C50 C43 C44 109.0(17) . . ?
C42 C43 C44 97.0(14) . . ?
C47 C43 C44 111.7(16) . . ?
C45 C44 C43 110.0(17) . . ?
C45 C44 H44A 109.7 . . ?
C43 C44 H44A 109.7 . . ?
C45 C44 H44B 109.7 . . ?
C43 C44 H44B 109.7 . . ?
H44A C44 H44B 108.2 . . ?
C44 C45 C41 103.5(17) . . ?
C44 C45 H45A 111.1 . . ?
C41 C45 H45A 111.1 . . ?
C44 C45 H45B 111.1 . . ?
C41 C45 H45B 111.1 . . ?
H45A C45 H45B 109.0 . . ?
O42 C46 O41 121(3) . . ?
O42 C46 C41 120(3) . . ?
O41 C46 C41 119(3) . . ?
O43 C47 O44 120(2) . . ?
O43 C47 C43 124(2) . . ?
O44 C47 C43 116(2) . . ?
C42 C48 H48A 108.0 . . ?
C42 C48 H48B 109.0 . . ?
H48A C48 H48B 113.0 . . ?
C42 C48 H48C 108.0 . . ?
H48A C48 H48C 107.0 . . ?
H48B C48 H48C 112.0 . . ?
C42 C49 H49C 115.6 . . ?
C42 C49 H49D 109.4 . . ?
H49C C49 H49D 109.5 . . ?
C42 C49 H49E 103.2 . . ?
H49C C49 H49E 109.5 . . ?
H49D C49 H49E 109.5 . . ?
C43 C50 H50C 109.5 . . ?
C43 C50 H50D 109.5 . . ?
H50C C50 H50D 109.5 . . ?
C43 C50 H50E 109.5 . . ?
H50C C50 H50E 109.5 . . ?
H50D C50 H50E 109.5 . . ?
C56 C51 C55 119.0(19) . . ?
C56 C51 C52 112.4(18) . . ?
C55 C51 C52 104.3(14) . . ?
C56 C51 H51 106.8 . . ?
C55 C51 H51 106.8 . . ?
C52 C51 H51 106.8 . . ?
C53 C52 C58 111.3(14) . . ?
C53 C52 C59 114.6(14) . . ?
C58 C52 C59 107.0(14) . . ?
C53 C52 C51 104.9(14) . . ?
C58 C52 C51 110.2(15) . . ?
C59 C52 C51 108.8(14) . . ?
C60 C53 C52 109.3(12) . . ?
C60 C53 C57 113.2(16) . . ?
C52 C53 C57 114.9(16) . . ?
C60 C53 C54 106.2(13) . . ?
C52 C53 C54 99.8(13) . . ?
C57 C53 C54 112.3(15) . . ?
C55 C54 C53 111.4(16) . . ?
C55 C54 H54C 109.3 . . ?
C53 C54 H54C 109.3 . . ?
C55 C54 H54D 109.3 . . ?
C53 C54 H54D 109.3 . . ?
H54C C54 H54D 108.0 . . ?
C54 C55 C51 103.7(17) . . ?
C54 C55 H55C 111.0 . . ?
C51 C55 H55C 111.0 . . ?
C54 C55 H55D 111.0 . . ?
C51 C55 H55D 111.0 . . ?
H55C C55 H55D 109.0 . . ?
O46 C56 O45 113(2) . . ?
O46 C56 C51 123(2) . . ?
O45 C56 C51 123(2) . . ?
O47 C57 O48 120.6(18) . . ?
O47 C57 C53 118.0(19) . . ?
O48 C57 C53 121.0(19) . . ?
C52 C58 H58C 109.5 . . ?
C52 C58 H58D 109.5 . . ?
H58C C58 H58D 109.5 . . ?
C52 C58 H58E 109.5 . . ?
H58C C58 H58E 109.5 . . ?
H58D C58 H58E 109.5 . . ?
C52 C59 H59A 109.5 . . ?
C52 C59 H59B 109.5 . . ?
H59A C59 H59B 109.5 . . ?
C52 C59 H59C 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
C53 C60 H60A 109.5 . . ?
C53 C60 H60B 109.5 . . ?
H60A C60 H60B 109.5 . . ?
C53 C60 H60C 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O17 H17 O53 0.90 2.41 3.17(3) 142.3 .
O18 H18 O54 0.92 2.17 3.04(3) 157.8 .
O32 H32A O20 0.80 2.65 3.04(2) 112.1 .
O32 H32B O58 0.99 1.74 2.63(3) 147.3 2_645
O33 H33A O27 0.86 1.87 2.64(3) 147.5 2_655
O35 H35 O55 0.99 2.06 3.00(3) 159.4 .
O36 H36 O56 0.89 2.26 3.07(3) 151.8 .
O50 H50A O25 0.84 1.86 2.65(2) 156.3 .
O50 H50B O53 0.78 1.91 2.54(3) 136.8 2_656
O52 H52A O57 0.98 1.72 2.59(3) 144.5 1_566
O53 H53A O24 0.84 2.01 2.84(2) 168.7 .
O53 H53B O28 0.90 1.95 2.78(2) 154.5 .
O54 H54A O26 0.98 1.83 2.75(2) 155.5 .
O56 H56A O25 0.99 2.50 3.39(3) 149.1 2_556
O56 H56B O48 0.75 2.01 2.75(2) 167.0 .
_database_code_depnum_ccdc_archive 'CCDC 978146'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_2

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C120 H194 K8 O77 U8'
_chemical_formula_weight         5085.79

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'R 3'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'

_cell_length_a                   21.3657(7)
_cell_length_b                   21.3657(7)
_cell_length_c                   38.4108(14)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     15185.1(13)
_cell_formula_units_Z            3
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    137837
_cell_measurement_theta_min      2.96
_cell_measurement_theta_max      25.68

_exptl_crystal_description       parallelepiped
_exptl_crystal_colour            'translucent light yellow'
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.668
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             7254
_exptl_absorpt_coefficient_mu    6.614
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.351
_exptl_absorpt_correction_T_max  0.483
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_special_details           'crystal-to-detector distance 35 mm'
_diffrn_ambient_temperature      150(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 area-detector diffractometer'
_diffrn_measurement_method       
'two φ and six ω scans with 2° steps (481 frames)'
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            137837
_diffrn_reflns_av_R_equivalents  0.0924
_diffrn_reflns_av_unetI/netI     0.0852
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_theta_min         2.96
_diffrn_reflns_theta_max         25.68
_reflns_number_total             12834
_reflns_number_gt                8979
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  
'SHELXTL (Sheldrick, 2008); PLATON (Spek, 2003)'

_refine_special_details          
;
 Structure solved by direct methods and subsequent Fourier-difference
 synthesis. For charge equilibrium and in order to retain acceptable 
 displacement parameters, two K atoms were given occupancy parameters
 of 1/3. All non-hydrogen atoms were refined with anisotropic displacement
 parameters, with many restraints on bond lengths and/or displacement
 parameters:
DFIX 1.52 0.01 C2 C1
DFIX 1.52 0.01 C2 C3
DFIX 1.52 0.01 C2 C8
DFIX 1.52 0.01 C2 C9
DFIX 2.40 0.01 C2 C5
DFIX 1.52 0.01 C3 C4
DFIX 1.52 0.01 C4 C5
DFIX 1.52 0.01 C12 C18
DFIX 1.52 0.01 C22 C23
DFIX 1.52 0.01 C22 C28
DFIX 1.52 0.01 C24 C25
ISOR 0.003 C2 C5 C8
ISOR 0.01 O26 O27 O29 C10 C14 C20 C30 C35
SIMU .01 .01 1.6 C1 C2 C3 C5 C8 C9
SIMU .01 .01 4 O7 O8
SIMU .001 .001 3.3 K2 O26
SIMU .01 .01 1.7 C22 > C25 C28
 The H atoms bound to water O atoms were not found, nor introduced. The
 C-bound H atoms were introduced at calculated positions and were treated
 as riding atoms with an isotropic displacement parameter equal to 1.2 times
 that of the parent atom (1.5 for CH₃). Large voids in the lattice likely
 indicate the presence of other, disordered water solvent molecules.
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.0895P)²+18.7238P] where P=(Fo²+2Fc²)/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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_chemical_absolute_configuration syn
_refine_ls_abs_structure_Flack   0.070(13)
_refine_ls_number_reflns         12834
_refine_ls_number_parameters     664
_refine_ls_number_restraints     144
_refine_ls_R_factor_all          0.0961
_refine_ls_R_factor_gt           0.0630
_refine_ls_wR_factor_ref         0.1692
_refine_ls_wR_factor_gt          0.1569
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_restrained_S_all      1.055
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.68
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         2.214
_refine_diff_density_min         -1.530
_refine_diff_density_rms         0.164

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
U1 U 0.59243(3) 0.66398(3) -0.074230(12) 0.04781(17) Uani 1 1 d . . .
U2 U 0.27428(3) 0.26883(3) 0.069883(15) 0.05238(18) Uani 1 1 d . . .
U3 U 0.6667 0.3333 -0.21354(2) 0.0438(3) Uani 1 3 d S . .
U4 U 0.6667 0.3333 0.21395(2) 0.0469(3) Uani 1 3 d S . .
K1 K 0.8037(3) 0.7848(3) -0.12507(14) 0.0917(14) Uani 1 1 d . . .
K2 K 0.3670(3) 0.4796(3) 0.12014(15) 0.0930(14) Uani 1 1 d U . .
K3 K 0.8590(14) 0.8042(15) 0.1292(5) 0.158(9) Uani 0.34 1 d P . .
K4 K 0.3993(9) 0.5720(15) -0.1421(5) 0.160(10) Uani 0.33 1 d P . .
O1 O 0.6050(5) 0.5904(6) -0.0612(3) 0.057(3) Uani 1 1 d . . .
O2 O 0.5799(6) 0.7368(6) -0.0880(3) 0.058(3) Uani 1 1 d . . .
O3 O 0.3621(6) 0.2865(6) 0.0600(4) 0.077(4) Uani 1 1 d . . .
O4 O 0.1866(5) 0.2509(5) 0.0815(3) 0.055(3) Uani 1 1 d . . .
O5 O 0.6667 0.3333 -0.1680(5) 0.057(5) Uani 1 3 d S . .
O6 O 0.6667 0.3333 -0.2593(5) 0.052(4) Uani 1 3 d S . .
O7 O 0.6667 0.3333 0.1684(5) 0.064(4) Uani 1 3 d SU . .
O8 O 0.6667 0.3333 0.2589(4) 0.051(4) Uani 1 3 d SU . .
O9 O 0.5075(6) 0.6406(6) -0.0268(3) 0.062(3) Uani 1 1 d . . .
O10 O 0.4621(6) 0.5851(7) -0.0747(3) 0.060(3) Uani 1 1 d . . .
O11 O 0.3085(6) 0.3967(6) 0.0632(3) 0.056(3) Uani 1 1 d . . .
O12 O 0.2668(8) 0.3255(7) 0.0171(3) 0.071(4) Uani 1 1 d . . .
O13 O 0.5460(6) 0.6053(6) -0.1306(3) 0.055(3) Uani 1 1 d . . .
O14 O 0.6636(5) 0.6791(6) -0.1285(2) 0.048(3) Uani 1 1 d . . .
O15 O 0.7073(6) 0.4627(5) -0.2140(3) 0.054(3) Uani 1 1 d . . .
O16 O 0.5917(5) 0.3934(5) -0.2144(3) 0.046(2) Uani 1 1 d . . .
O17 O 0.7250(5) 0.7483(6) -0.0678(3) 0.051(3) Uani 1 1 d . . .
O18 O 0.6582(6) 0.7318(7) -0.0213(3) 0.065(3) Uani 1 1 d . . .
O19 O 0.9616(6) 0.7770(7) 0.0218(3) 0.065(3) Uani 1 1 d . . .
O20 O 0.9106(6) 0.7736(7) 0.0693(4) 0.072(4) Uani 1 1 d . . .
O21 O 0.2880(7) 0.2231(6) 0.1266(3) 0.066(3) Uani 1 1 d . . .
O22 O 0.3252(6) 0.3382(6) 0.1233(3) 0.064(3) Uani 1 1 d . . .
O23 O 0.5803(6) 0.3817(6) 0.2145(3) 0.054(3) Uani 1 1 d . . .
O24 O 0.5326(6) 0.2623(7) 0.2134(3) 0.066(3) Uani 1 1 d . . .
O25 O 0.8327(14) 0.8188(13) -0.2013(5) 0.181(9) Uani 1 1 d . . .
O26 O 0.5044(8) 0.5131(7) 0.0782(4) 0.0960(16) Uani 1 1 d U . .
O27 O 0.8590(11) 0.9346(11) 0.1219(5) 0.142(7) Uani 1 1 d U . .
O28 O 0.9201(8) 0.8521(9) 0.1966(4) 0.109(5) Uani 1 1 d . . .
O29 O 0.0000 0.0000 0.1150(4) 0.065(5) Uani 1 3 d SU . .
C1 C 0.3784(10) 0.5536(9) -0.0254(5) 0.069(4) Uani 1 1 d DU . .
C2 C 0.3576(8) 0.4738(8) -0.0187(4) 0.095(4) Uani 1 1 d DU . .
C3 C 0.2987(10) 0.4499(9) 0.0084(5) 0.070(4) Uani 1 1 d DU . .
H3 H 0.2530 0.4288 -0.0054 0.084 Uiso 1 1 calc R . .
C4 C 0.3006(13) 0.5122(9) 0.0275(5) 0.115(9) Uani 1 1 d D . .
H4A H 0.3069 0.5092 0.0529 0.138 Uiso 1 1 calc R . .
H4B H 0.2563 0.5149 0.0232 0.138 Uiso 1 1 calc R . .
C5 C 0.3672(11) 0.5763(9) 0.0111(6) 0.096(5) Uani 1 1 d DU . .
H5A H 0.4104 0.5900 0.0257 0.116 Uiso 1 1 calc R . .
H5B H 0.3600 0.6184 0.0093 0.116 Uiso 1 1 calc R . .
C6 C 0.4517(9) 0.5973(9) -0.0441(4) 0.055(4) Uani 1 1 d . . .
C7 C 0.2906(8) 0.3886(10) 0.0303(5) 0.063(5) Uani 1 1 d . . .
C8 C 0.3181(13) 0.4218(13) -0.0492(5) 0.114(5) Uani 1 1 d DU . .
H8A H 0.3070 0.3729 -0.0428 0.171 Uiso 1 1 calc R . .
H8B H 0.3491 0.4377 -0.0699 0.171 Uiso 1 1 calc R . .
H8C H 0.2731 0.4217 -0.0542 0.171 Uiso 1 1 calc R . .
C9 C 0.4225(10) 0.4720(12) -0.0035(5) 0.074(4) Uani 1 1 d DU . .
H9A H 0.4332 0.4940 0.0197 0.111 Uiso 1 1 calc R . .
H9B H 0.4645 0.4991 -0.0187 0.111 Uiso 1 1 calc R . .
H9C H 0.4117 0.4218 -0.0018 0.111 Uiso 1 1 calc R . .
C10 C 0.3217(13) 0.5473(14) -0.0518(6) 0.119(8) Uani 1 1 d U . .
H10A H 0.3270 0.5260 -0.0735 0.179 Uiso 1 1 calc R . .
H10B H 0.3287 0.5954 -0.0567 0.179 Uiso 1 1 calc R . .
H10C H 0.2732 0.5164 -0.0423 0.179 Uiso 1 1 calc R . .
C11 C 0.6153(8) 0.6064(8) -0.1800(3) 0.046(4) Uani 1 1 d . . .
C12 C 0.6527(9) 0.5589(10) -0.1769(5) 0.069(5) Uani 1 1 d D . .
C13 C 0.6379(9) 0.5234(9) -0.2121(4) 0.058(4) Uani 1 1 d . . .
H13 H 0.6759 0.5588 -0.2282 0.069 Uiso 1 1 calc R . .
C14 C 0.5650(11) 0.5136(11) -0.2249(6) 0.084(6) Uani 1 1 d U . .
H14A H 0.5272 0.4619 -0.2246 0.101 Uiso 1 1 calc R . .
H14B H 0.5696 0.5321 -0.2489 0.101 Uiso 1 1 calc R . .
C15 C 0.5451(10) 0.5575(11) -0.1994(5) 0.075(5) Uani 1 1 d . . .
H15A H 0.5283 0.5865 -0.2123 0.090 Uiso 1 1 calc R . .
H15B H 0.5067 0.5250 -0.1830 0.090 Uiso 1 1 calc R . .
C16 C 0.6088(9) 0.6334(8) -0.1455(4) 0.046(4) Uani 1 1 d . . .
C17 C 0.6438(8) 0.4562(8) -0.2128(4) 0.045(4) Uani 1 1 d . . .
C18 C 0.7325(9) 0.5986(12) -0.1659(5) 0.092(7) Uani 1 1 d D . .
H18A H 0.7398 0.6328 -0.1472 0.138 Uiso 1 1 calc R . .
H18B H 0.7628 0.6249 -0.1859 0.138 Uiso 1 1 calc R . .
H18C H 0.7457 0.5635 -0.1575 0.138 Uiso 1 1 calc R . .
C19 C 0.6203(10) 0.5032(11) -0.1496(5) 0.065(5) Uani 1 1 d . . .
H19A H 0.5676 0.4773 -0.1520 0.097 Uiso 1 1 calc R . .
H19B H 0.6336 0.5263 -0.1267 0.097 Uiso 1 1 calc R . .
H19C H 0.6380 0.4691 -0.1520 0.097 Uiso 1 1 calc R . .
C20 C 0.6705(10) 0.6737(11) -0.2016(5) 0.089(6) Uani 1 1 d U . .
H20A H 0.7046 0.7113 -0.1858 0.134 Uiso 1 1 calc R . .
H20B H 0.6444 0.6924 -0.2151 0.134 Uiso 1 1 calc R . .
H20C H 0.6971 0.6595 -0.2176 0.134 Uiso 1 1 calc R . .
C21 C 0.7858(7) 0.8124(8) -0.0154(4) 0.043(4) Uani 1 1 d . . .
C22 C 0.8033(7) 0.7744(10) 0.0132(4) 0.078(4) Uani 1 1 d DU . .
C23 C 0.8827(7) 0.8264(9) 0.0227(5) 0.064(4) Uani 1 1 d DU . .
H23 H 0.8834 0.8609 0.0404 0.077 Uiso 1 1 calc R . .
C24 C 0.9166(9) 0.8691(11) -0.0103(5) 0.080(4) Uani 1 1 d DU . .
H24A H 0.9547 0.8595 -0.0188 0.097 Uiso 1 1 calc R . .
H24B H 0.9387 0.9215 -0.0056 0.097 Uiso 1 1 calc R . .
C25 C 0.8567(9) 0.8455(11) -0.0375(5) 0.081(5) Uani 1 1 d DU . .
H25A H 0.8564 0.8090 -0.0534 0.097 Uiso 1 1 calc R . .
H25B H 0.8627 0.8872 -0.0513 0.097 Uiso 1 1 calc R . .
C26 C 0.7202(8) 0.7617(8) -0.0365(5) 0.054(4) Uani 1 1 d . . .
C27 C 0.9215(9) 0.7916(9) 0.0379(4) 0.053(4) Uani 1 1 d . . .
C28 C 0.7584(11) 0.7541(12) 0.0468(5) 0.090(5) Uani 1 1 d DU . .
H28A H 0.7093 0.7149 0.0420 0.135 Uiso 1 1 calc R . .
H28B H 0.7567 0.7963 0.0556 0.135 Uiso 1 1 calc R . .
H28C H 0.7808 0.7381 0.0644 0.135 Uiso 1 1 calc R . .
C29 C 0.7918(13) 0.6994(10) -0.0006(7) 0.092(7) Uani 1 1 d . . .
H29A H 0.7426 0.6704 -0.0096 0.138 Uiso 1 1 calc R . .
H29B H 0.7992 0.6735 0.0186 0.138 Uiso 1 1 calc R . .
H29C H 0.8266 0.7081 -0.0192 0.138 Uiso 1 1 calc R . .
C30 C 0.7712(13) 0.8703(14) -0.0011(7) 0.114(8) Uani 1 1 d U . .
H30A H 0.7359 0.8740 -0.0161 0.171 Uiso 1 1 calc R . .
H30B H 0.8163 0.9169 -0.0008 0.171 Uiso 1 1 calc R . .
H30C H 0.7519 0.8574 0.0226 0.171 Uiso 1 1 calc R . .
C31 C 0.3514(10) 0.2958(10) 0.1766(5) 0.065(5) Uani 1 1 d . . .
H31 H 0.3391 0.3296 0.1888 0.078 Uiso 1 1 calc R . .
C32 C 0.4319(11) 0.3307(13) 0.1764(5) 0.090(7) Uani 1 1 d . . .
C33 C 0.4498(8) 0.3126(9) 0.2128(4) 0.054(4) Uani 1 1 d . . .
C34 C 0.3923(11) 0.2353(12) 0.2190(6) 0.092(7) Uani 1 1 d . . .
H34A H 0.3824 0.2254 0.2442 0.110 Uiso 1 1 calc R . .
H34B H 0.4067 0.2016 0.2092 0.110 Uiso 1 1 calc R . .
C35 C 0.3228(11) 0.2282(11) 0.1990(6) 0.084(6) Uani 1 1 d U . .
H35A H 0.3000 0.1842 0.1844 0.101 Uiso 1 1 calc R . .
H35B H 0.2866 0.2258 0.2159 0.101 Uiso 1 1 calc R . .
C36 C 0.3175(9) 0.2824(9) 0.1397(5) 0.056(4) Uani 1 1 d . . .
C37 C 0.5259(9) 0.3188(10) 0.2145(4) 0.057(4) Uani 1 1 d . . .
C38 C 0.4743(12) 0.4109(10) 0.1687(5) 0.081(6) Uani 1 1 d . . .
H38A H 0.5259 0.4287 0.1720 0.121 Uiso 1 1 calc R . .
H38B H 0.4588 0.4365 0.1846 0.121 Uiso 1 1 calc R . .
H38C H 0.4654 0.4195 0.1446 0.121 Uiso 1 1 calc R . .
C39 C 0.4499(12) 0.2886(14) 0.1467(5) 0.089(7) Uani 1 1 d . . .
H39A H 0.4450 0.3054 0.1237 0.133 Uiso 1 1 calc R . .
H39B H 0.4162 0.2365 0.1486 0.133 Uiso 1 1 calc R . .
H39C H 0.4995 0.2982 0.1497 0.133 Uiso 1 1 calc R . .
C40 C 0.4468(12) 0.3625(14) 0.2386(7) 0.119(9) Uani 1 1 d . . .
H40A H 0.4320 0.3384 0.2613 0.179 Uiso 1 1 calc R . .
H40B H 0.4117 0.3765 0.2310 0.179 Uiso 1 1 calc R . .
H40C H 0.4946 0.4058 0.2407 0.179 Uiso 1 1 calc R . .


_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 O2 1.787(11) . ?
U1 O1 1.794(10) . ?
U1 O10 2.430(11) . ?
U1 O9 2.440(11) . ?
U1 O13 2.451(10) . ?
U1 O18 2.484(11) . ?
U1 O17 2.496(9) . ?
U1 O14 2.505(10) . ?
U2 O3 1.761(12) . ?
U2 O4 1.771(11) . ?
U2 O12 2.409(12) . ?
U2 O19 2.425(11) 2_655 ?
U2 O22 2.445(12) . ?
U2 O11 2.464(11) . ?
U2 O21 2.466(11) . ?
U2 O20 2.470(12) 2_655 ?
U3 O5 1.749(18) . ?
U3 O6 1.757(18) . ?
U3 O15 2.449(10) 3_665 ?
U3 O15 2.449(10) 2_655 ?
U3 O15 2.449(10) . ?
U3 O16 2.504(10) 2_655 ?
U3 O16 2.504(10) 3_665 ?
U3 O16 2.504(10) . ?
U4 O8 1.726(17) . ?
U4 O7 1.751(19) . ?
U4 O24 2.482(11) 2_655 ?
U4 O24 2.482(11) 3_665 ?
U4 O24 2.482(11) . ?
U4 O23 2.527(11) 2_655 ?
U4 O23 2.527(11) 3_665 ?
U4 O23 2.527(11) . ?
K1 O17 2.638(12) . ?
K1 O24 2.683(14) 7_554 ?
K1 O14 2.705(11) . ?
K1 O23 2.751(11) 8_654 ?
K1 O25 3.00(2) . ?
K2 O22 2.691(12) . ?
K2 O11 2.696(13) . ?
K2 O16 2.735(11) 5 ?
K2 O15 2.738(12) 6_565 ?
K2 O26 3.103(16) . ?
K3 O20 2.77(2) . ?
K3 O27 2.80(3) . ?
K3 O28 2.85(3) . ?
K3 O21 3.12(2) 3_665 ?
K4 O27 2.70(3) 8_654 ?
K4 O28 2.74(2) 7_444 ?
K4 O10 2.86(2) . ?
K4 O13 2.88(2) . ?
K4 O28 3.02(3) 8_654 ?
O9 C6 1.272(18) . ?
O10 C6 1.250(18) . ?
O11 C7 1.30(2) . ?
O12 C7 1.28(2) . ?
O13 C16 1.297(19) . ?
O14 C16 1.267(18) . ?
O15 C17 1.292(17) . ?
O15 K2 2.738(12) 8_654 ?
O16 C17 1.244(17) . ?
O16 K2 2.735(11) 9_554 ?
O17 C26 1.253(19) . ?
O18 C26 1.29(2) . ?
O19 C27 1.216(18) . ?
O19 U2 2.425(11) 3_665 ?
O20 C27 1.254(18) . ?
O20 U2 2.470(12) 3_665 ?
O21 C36 1.208(19) . ?
O21 K3 3.12(2) 2_655 ?
O22 C36 1.284(19) . ?
O23 C37 1.263(19) . ?
O23 K1 2.751(11) 6_565 ?
O24 C37 1.29(2) . ?
O24 K1 2.683(14) 4_445 ?
O27 K4 2.70(3) 6_565 ?
O28 K4 2.74(2) 4 ?
O28 K4 3.02(3) 6_565 ?
C1 C10 1.53(3) . ?
C1 C5 1.54(2) . ?
C1 C6 1.54(2) . ?
C1 C2 1.552(9) . ?
C2 C3 1.513(10) . ?
C2 C9 1.524(10) . ?
C2 C8 1.541(10) . ?
C3 C7 1.49(2) . ?
C3 C4 1.502(10) . ?
C3 H3 1.0000 . ?
C4 C5 1.533(10) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C16 1.48(2) . ?
C11 C15 1.53(2) . ?
C11 C20 1.57(2) . ?
C11 C12 1.58(2) . ?
C12 C19 1.47(2) . ?
C12 C13 1.50(2) . ?
C12 C18 1.535(10) . ?
C13 C17 1.50(2) . ?
C13 C14 1.55(2) . ?
C13 H13 1.0000 . ?
C14 C15 1.56(3) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C26 1.509(18) . ?
C21 C22 1.52(2) . ?
C21 C30 1.52(3) . ?
C21 C25 1.56(2) . ?
C22 C28 1.536(10) . ?
C22 C23 1.537(10) . ?
C22 C29 1.59(3) . ?
C23 C27 1.48(2) . ?
C23 C24 1.52(2) . ?
C23 H23 1.0000 . ?
C24 C25 1.529(9) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 C32 1.49(3) . ?
C31 C35 1.52(3) . ?
C31 C36 1.55(2) . ?
C31 H31 1.0000 . ?
C32 C38 1.51(3) . ?
C32 C33 1.55(2) . ?
C32 C39 1.61(3) . ?
C33 C40 1.48(3) . ?
C33 C34 1.50(2) . ?
C33 C37 1.57(2) . ?
C34 C35 1.61(3) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 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
O2 U1 O1 179.0(5) . . ?
O2 U1 O10 89.0(5) . . ?
O1 U1 O10 90.9(4) . . ?
O2 U1 O9 88.8(5) . . ?
O1 U1 O9 91.9(4) . . ?
O10 U1 O9 52.2(3) . . ?
O2 U1 O13 89.2(4) . . ?
O1 U1 O13 89.9(4) . . ?
O10 U1 O13 66.9(3) . . ?
O9 U1 O13 119.1(4) . . ?
O2 U1 O18 91.2(4) . . ?
O1 U1 O18 89.6(5) . . ?
O10 U1 O18 121.9(4) . . ?
O9 U1 O18 69.8(4) . . ?
O13 U1 O18 171.1(4) . . ?
O2 U1 O17 90.6(4) . . ?
O1 U1 O17 89.5(4) . . ?
O10 U1 O17 174.4(3) . . ?
O9 U1 O17 122.2(4) . . ?
O13 U1 O17 118.7(4) . . ?
O18 U1 O17 52.5(4) . . ?
O2 U1 O14 89.3(4) . . ?
O1 U1 O14 89.9(4) . . ?
O10 U1 O14 119.6(3) . . ?
O9 U1 O14 171.6(4) . . ?
O13 U1 O14 52.7(3) . . ?
O18 U1 O14 118.4(4) . . ?
O17 U1 O14 66.0(3) . . ?
O3 U2 O4 177.9(5) . . ?
O3 U2 O12 92.4(5) . . ?
O4 U2 O12 89.5(5) . . ?
O3 U2 O19 91.8(5) . 2_655 ?
O4 U2 O19 89.7(4) . 2_655 ?
O12 U2 O19 67.2(4) . 2_655 ?
O3 U2 O22 87.0(5) . . ?
O4 U2 O22 91.2(4) . . ?
O12 U2 O22 121.6(4) . . ?
O19 U2 O22 171.2(4) 2_655 . ?
O3 U2 O11 92.7(5) . . ?
O4 U2 O11 87.8(4) . . ?
O12 U2 O11 54.0(4) . . ?
O19 U2 O11 121.2(4) 2_655 . ?
O22 U2 O11 67.7(4) . . ?
O3 U2 O21 87.2(5) . . ?
O4 U2 O21 90.8(5) . . ?
O12 U2 O21 174.2(4) . . ?
O19 U2 O21 118.6(4) 2_655 . ?
O22 U2 O21 52.6(4) . . ?
O11 U2 O21 120.3(4) . . ?
O3 U2 O20 91.8(5) . 2_655 ?
O4 U2 O20 88.0(4) . 2_655 ?
O12 U2 O20 118.2(4) . 2_655 ?
O19 U2 O20 51.0(4) 2_655 2_655 ?
O22 U2 O20 120.2(4) . 2_655 ?
O11 U2 O20 171.1(4) . 2_655 ?
O21 U2 O20 67.6(4) . 2_655 ?
O5 U3 O6 180 . . ?
O5 U3 O15 90.4(3) . 3_665 ?
O6 U3 O15 89.6(3) . 3_665 ?
O5 U3 O15 90.4(3) . 2_655 ?
O6 U3 O15 89.6(3) . 2_655 ?
O15 U3 O15 119.992(8) 3_665 2_655 ?
O5 U3 O15 90.4(3) . . ?
O6 U3 O15 89.6(3) . . ?
O15 U3 O15 119.995(7) 3_665 . ?
O15 U3 O15 119.997(7) 2_655 . ?
O5 U3 O16 90.7(2) . 2_655 ?
O6 U3 O16 89.3(2) . 2_655 ?
O15 U3 O16 68.5(3) 3_665 2_655 ?
O15 U3 O16 51.5(3) 2_655 2_655 ?
O15 U3 O16 171.4(3) . 2_655 ?
O5 U3 O16 90.7(2) . 3_665 ?
O6 U3 O16 89.3(2) . 3_665 ?
O15 U3 O16 51.5(3) 3_665 3_665 ?
O15 U3 O16 171.4(3) 2_655 3_665 ?
O15 U3 O16 68.5(3) . 3_665 ?
O16 U3 O16 119.987(11) 2_655 3_665 ?
O5 U3 O16 90.7(2) . . ?
O6 U3 O16 89.3(2) . . ?
O15 U3 O16 171.4(3) 3_665 . ?
O15 U3 O16 68.5(3) 2_655 . ?
O15 U3 O16 51.5(3) . . ?
O16 U3 O16 119.981(11) 2_655 . ?
O16 U3 O16 119.982(11) 3_665 . ?
O8 U4 O7 180 . . ?
O8 U4 O24 90.5(3) . 2_655 ?
O7 U4 O24 89.5(3) . 2_655 ?
O8 U4 O24 90.5(3) . 3_665 ?
O7 U4 O24 89.5(3) . 3_665 ?
O24 U4 O24 119.992(11) 2_655 3_665 ?
O8 U4 O24 90.5(3) . . ?
O7 U4 O24 89.5(3) . . ?
O24 U4 O24 119.992(10) 2_655 . ?
O24 U4 O24 119.991(9) 3_665 . ?
O8 U4 O23 89.5(3) . 2_655 ?
O7 U4 O23 90.5(3) . 2_655 ?
O24 U4 O23 52.8(4) 2_655 2_655 ?
O24 U4 O23 172.8(4) 3_665 2_655 ?
O24 U4 O23 67.3(4) . 2_655 ?
O8 U4 O23 89.5(3) . 3_665 ?
O7 U4 O23 90.5(3) . 3_665 ?
O24 U4 O23 67.3(4) 2_655 3_665 ?
O24 U4 O23 52.8(4) 3_665 3_665 ?
O24 U4 O23 172.8(4) . 3_665 ?
O23 U4 O23 119.993(9) 2_655 3_665 ?
O8 U4 O23 89.5(3) . . ?
O7 U4 O23 90.5(3) . . ?
O24 U4 O23 172.8(4) 2_655 . ?
O24 U4 O23 67.3(4) 3_665 . ?
O24 U4 O23 52.8(4) . . ?
O23 U4 O23 119.993(9) 2_655 . ?
O23 U4 O23 119.994(9) 3_665 . ?
O17 K1 O24 98.9(4) . 7_554 ?
O17 K1 O14 61.2(3) . . ?
O24 K1 O14 132.0(4) 7_554 . ?
O17 K1 O23 118.4(4) . 8_654 ?
O24 K1 O23 61.4(3) 7_554 8_654 ?
O14 K1 O23 166.4(4) . 8_654 ?
O17 K1 O25 155.2(6) . . ?
O24 K1 O25 82.5(5) 7_554 . ?
O14 K1 O25 99.4(6) . . ?
O23 K1 O25 84.2(6) 8_654 . ?
O22 K2 O11 61.0(4) . . ?
O22 K2 O16 123.9(4) . 5 ?
O11 K2 O16 93.4(3) . 5 ?
O22 K2 O15 174.5(4) . 6_565 ?
O11 K2 O15 122.3(4) . 6_565 ?
O16 K2 O15 61.2(3) 5 6_565 ?
O22 K2 O26 91.6(4) . . ?
O11 K2 O26 78.8(4) . . ?
O16 K2 O26 134.3(4) 5 . ?
O15 K2 O26 85.0(4) 6_565 . ?
O20 K3 O27 110.5(10) . . ?
O20 K3 O28 132.5(9) . . ?
O27 K3 O28 87.8(8) . . ?
O20 K3 O21 55.2(5) . 3_665 ?
O27 K3 O21 152.1(12) . 3_665 ?
O28 K3 O21 88.1(6) . 3_665 ?
O27 K4 O28 92.7(7) 8_654 7_444 ?
O27 K4 O10 156.3(8) 8_654 . ?
O28 K4 O10 110.7(7) 7_444 . ?
O27 K4 O13 101.5(8) 8_654 . ?
O28 K4 O13 164.4(10) 7_444 . ?
O10 K4 O13 55.9(4) . . ?
O27 K4 O28 86.4(8) 8_654 8_654 ?
O28 K4 O28 111.0(11) 7_444 8_654 ?
O10 K4 O28 81.5(7) . 8_654 ?
O13 K4 O28 76.8(6) . 8_654 ?
C6 O9 U1 95.2(10) . . ?
C6 O10 U1 96.3(10) . . ?
C6 O10 K4 138.5(12) . . ?
U1 O10 K4 113.2(5) . . ?
C7 O11 U2 92.8(10) . . ?
C7 O11 K2 151.8(11) . . ?
U2 O11 K2 115.3(4) . . ?
C7 O12 U2 95.8(11) . . ?
C16 O13 U1 95.2(9) . . ?
C16 O13 K4 142.5(10) . . ?
U1 O13 K4 111.9(6) . . ?
C16 O14 U1 93.5(9) . . ?
C16 O14 K1 151.5(10) . . ?
U1 O14 K1 114.4(4) . . ?
C17 O15 U3 96.7(9) . . ?
C17 O15 K2 147.2(9) . 8_654 ?
U3 O15 K2 116.0(4) . 8_654 ?
C17 O16 U3 95.4(9) . . ?
C17 O16 K2 150.0(9) . 9_554 ?
U3 O16 K2 114.2(4) . 9_554 ?
C26 O17 U1 93.8(9) . . ?
C26 O17 K1 147.8(9) . . ?
U1 O17 K1 117.1(4) . . ?
C26 O18 U1 93.5(9) . . ?
C27 O19 U2 97.5(10) . 3_665 ?
C27 O20 U2 94.2(10) . 3_665 ?
C27 O20 K3 139.8(12) . . ?
U2 O20 K3 123.3(6) 3_665 . ?
C36 O21 U2 93.1(10) . . ?
C36 O21 K3 153.4(12) . 2_655 ?
U2 O21 K3 110.7(6) . 2_655 ?
C36 O22 U2 92.2(10) . . ?
C36 O22 K2 151.7(11) . . ?
U2 O22 K2 116.1(4) . . ?
C37 O23 U4 92.1(9) . . ?
C37 O23 K1 153.9(11) . 6_565 ?
U4 O23 K1 113.5(4) . 6_565 ?
C37 O24 U4 93.6(10) . . ?
C37 O24 K1 148.9(10) . 4_445 ?
U4 O24 K1 117.5(5) . 4_445 ?
K4 O27 K3 88.5(8) 6_565 . ?
K4 O28 K3 107.7(8) 4 . ?
K4 O28 K4 128.0(10) 4 6_565 ?
K3 O28 K4 81.7(7) . 6_565 ?
C10 C1 C5 112.9(17) . . ?
C10 C1 C6 105.4(16) . . ?
C5 C1 C6 120.1(15) . . ?
C10 C1 C2 103.5(16) . . ?
C5 C1 C2 101.0(11) . . ?
C6 C1 C2 113.0(13) . . ?
C3 C2 C9 110.0(15) . . ?
C3 C2 C8 102.5(15) . . ?
C9 C2 C8 116.7(16) . . ?
C3 C2 C1 102.7(12) . . ?
C9 C2 C1 109.0(14) . . ?
C8 C2 C1 114.8(16) . . ?
C7 C3 C4 116.3(15) . . ?
C7 C3 C2 113.4(13) . . ?
C4 C3 C2 112.8(15) . . ?
C7 C3 H3 104.2 . . ?
C4 C3 H3 104.2 . . ?
C2 C3 H3 104.2 . . ?
C3 C4 C5 101.0(15) . . ?
C3 C4 H4A 111.6 . . ?
C5 C4 H4A 111.6 . . ?
C3 C4 H4B 111.6 . . ?
C5 C4 H4B 111.6 . . ?
H4A C4 H4B 109.4 . . ?
C4 C5 C1 108.4(12) . . ?
C4 C5 H5A 110.0 . . ?
C1 C5 H5A 110.0 . . ?
C4 C5 H5B 110.0 . . ?
C1 C5 H5B 110.0 . . ?
H5A C5 H5B 108.4 . . ?
O10 C6 O9 116.4(15) . . ?
O10 C6 C1 122.9(15) . . ?
O9 C6 C1 119.9(14) . . ?
O12 C7 O11 117.4(16) . . ?
O12 C7 C3 120.5(17) . . ?
O11 C7 C3 122.0(17) . . ?
C2 C8 H8A 109.5 . . ?
C2 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C2 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C2 C9 H9A 109.5 . . ?
C2 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C2 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C1 C10 H10A 109.5 . . ?
C1 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C1 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C16 C11 C15 116.8(14) . . ?
C16 C11 C20 106.9(13) . . ?
C15 C11 C20 113.6(14) . . ?
C16 C11 C12 111.1(13) . . ?
C15 C11 C12 103.8(13) . . ?
C20 C11 C12 103.9(14) . . ?
C19 C12 C13 109.7(15) . . ?
C19 C12 C18 101.2(15) . . ?
C13 C12 C18 115.1(16) . . ?
C19 C12 C11 112.8(15) . . ?
C13 C12 C11 102.1(13) . . ?
C18 C12 C11 116.3(15) . . ?
C12 C13 C17 113.6(14) . . ?
C12 C13 C14 107.4(15) . . ?
C17 C13 C14 115.2(14) . . ?
C12 C13 H13 106.7 . . ?
C17 C13 H13 106.7 . . ?
C14 C13 H13 106.7 . . ?
C13 C14 C15 106.2(16) . . ?
C13 C14 H14A 110.5 . . ?
C15 C14 H14A 110.5 . . ?
C13 C14 H14B 110.5 . . ?
C15 C14 H14B 110.5 . . ?
H14A C14 H14B 108.7 . . ?
C11 C15 C14 104.3(14) . . ?
C11 C15 H15A 110.9 . . ?
C14 C15 H15A 110.9 . . ?
C11 C15 H15B 110.9 . . ?
C14 C15 H15B 110.9 . . ?
H15A C15 H15B 108.9 . . ?
O14 C16 O13 118.3(13) . . ?
O14 C16 C11 122.0(15) . . ?
O13 C16 C11 119.4(14) . . ?
O16 C17 O15 116.1(14) . . ?
O16 C17 C13 124.9(14) . . ?
O15 C17 C13 118.8(14) . . ?
C12 C18 H18A 109.5 . . ?
C12 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C12 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C12 C19 H19A 109.5 . . ?
C12 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C12 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C11 C20 H20A 109.5 . . ?
C11 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C11 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C26 C21 C22 113.2(13) . . ?
C26 C21 C30 106.4(14) . . ?
C22 C21 C30 112.3(15) . . ?
C26 C21 C25 112.1(13) . . ?
C22 C21 C25 101.1(12) . . ?
C30 C21 C25 112.0(15) . . ?
C21 C22 C28 118.3(15) . . ?
C21 C22 C23 105.3(13) . . ?
C28 C22 C23 108.2(15) . . ?
C21 C22 C29 110.0(15) . . ?
C28 C22 C29 103.7(17) . . ?
C23 C22 C29 111.4(16) . . ?
C27 C23 C24 114.4(14) . . ?
C27 C23 C22 115.1(15) . . ?
C24 C23 C22 105.0(13) . . ?
C27 C23 H23 107.3 . . ?
C24 C23 H23 107.3 . . ?
C22 C23 H23 107.3 . . ?
C23 C24 C25 107.7(14) . . ?
C23 C24 H24A 110.2 . . ?
C25 C24 H24A 110.2 . . ?
C23 C24 H24B 110.2 . . ?
C25 C24 H24B 110.2 . . ?
H24A C24 H24B 108.5 . . ?
C24 C25 C21 103.9(14) . . ?
C24 C25 H25A 111.0 . . ?
C21 C25 H25A 111.0 . . ?
C24 C25 H25B 111.0 . . ?
C21 C25 H25B 111.0 . . ?
H25A C25 H25B 109.0 . . ?
O17 C26 O18 120.2(12) . . ?
O17 C26 C21 121.7(14) . . ?
O18 C26 C21 118.0(14) . . ?
O19 C27 O20 117.2(16) . . ?
O19 C27 C23 124.8(15) . . ?
O20 C27 C23 117.9(16) . . ?
C22 C28 H28A 109.5 . . ?
C22 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C22 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C22 C29 H29A 109.5 . . ?
C22 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C22 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C21 C30 H30A 109.5 . . ?
C21 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C21 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C32 C31 C35 107.0(16) . . ?
C32 C31 C36 113.8(16) . . ?
C35 C31 C36 114.4(15) . . ?
C32 C31 H31 107.1 . . ?
C35 C31 H31 107.1 . . ?
C36 C31 H31 107.1 . . ?
C31 C32 C38 116.9(18) . . ?
C31 C32 C33 103.7(14) . . ?
C38 C32 C33 112.0(17) . . ?
C31 C32 C39 105.2(18) . . ?
C38 C32 C39 108.7(16) . . ?
C33 C32 C39 110.1(18) . . ?
C40 C33 C34 112.3(17) . . ?
C40 C33 C32 108.8(18) . . ?
C34 C33 C32 104.4(15) . . ?
C40 C33 C37 109.2(14) . . ?
C34 C33 C37 109.2(15) . . ?
C32 C33 C37 113.0(14) . . ?
C33 C34 C35 103.7(15) . . ?
C33 C34 H34A 111.0 . . ?
C35 C34 H34A 111.0 . . ?
C33 C34 H34B 111.0 . . ?
C35 C34 H34B 111.0 . . ?
H34A C34 H34B 109.0 . . ?
C31 C35 C34 105.5(16) . . ?
C31 C35 H35A 110.6 . . ?
C34 C35 H35A 110.6 . . ?
C31 C35 H35B 110.6 . . ?
C34 C35 H35B 110.6 . . ?
H35A C35 H35B 108.8 . . ?
O21 C36 O22 121.8(16) . . ?
O21 C36 C31 121.6(15) . . ?
O22 C36 C31 116.5(15) . . ?
O23 C37 O24 121.6(15) . . ?
O23 C37 C33 117.0(15) . . ?
O24 C37 C33 121.3(15) . . ?
C32 C38 H38A 109.5 . . ?
C32 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C32 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C32 C39 H39A 109.5 . . ?
C32 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C32 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C33 C40 H40A 109.5 . . ?
C33 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C33 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
_database_code_depnum_ccdc_archive 'CCDC 978147'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_3

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C15 H23 N O7 U'
_chemical_formula_weight         567.37

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   'P 21'

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

_cell_length_a                   9.2051(2)
_cell_length_b                   19.3999(3)
_cell_length_c                   10.3663(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.9411(7)
_cell_angle_gamma                90.00
_cell_volume                     1833.44(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    116055
_cell_measurement_theta_min      3.36
_cell_measurement_theta_max      30.51

_exptl_crystal_description       parallelepiped
_exptl_crystal_colour            'translucent light yellow'
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.14
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.055
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1072
_exptl_absorpt_coefficient_mu    8.887
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.191
_exptl_absorpt_correction_T_max  0.288
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_special_details           'crystal-to-detector distance 30 mm'
_diffrn_ambient_temperature      150(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 area-detector diffractometer'
_diffrn_measurement_method       
'2 φ and 15 ω scans with 1° steps (1643 frames)'
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            116055
_diffrn_reflns_av_R_equivalents  0.0226
_diffrn_reflns_av_unetI/netI     0.0210
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.36
_diffrn_reflns_theta_max         30.51
_reflns_number_total             11154
_reflns_number_gt                10445
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  
'SHELXTL (Sheldrick, 2008); PLATON (Spek, 2003)'

_refine_special_details          
;
 Structure solved by direct methods and subsequent Fourier-difference
 synthesis. One N-methylpyrrolidone molecule is disordered over two
 positions sharing the atoms O14 and C29, which have been refined with
 occupancy parameters constrained to sum to unity. All non-hydrogen atoms 
 were refined with anisotropic displacement parameters, with restraints 
 on some bond lengths, angles and displacement parameters, particularly
 for the atoms of the disordered part:
DFIX 2.27 0.01 O14 N2A
DFIX 2.49 0.01 O14 C27A
DFIX 1.35 0.01 N2A C26
DFIX 1.44 0.01 N2A C29
DFIX 2.17 0.01 N2A C27A
DFIX 1.52 0.01 C26 C27A
DFIX 1.52 0.01 C27A C28A
DFIX 1.52 0.01 C28A C29
DFIX 2.45 0.01 C26 C28A
DFIX 2.27 0.01 O14 N2B
DFIX 2.49 0.01 O14 C27B
DFIX 1.35 0.01 N2B C26
DFIX 1.44 0.01 N2B C29
DFIX 2.17 0.01 N2B C27B
DFIX 1.52 0.01 C26 C27B
DFIX 1.52 0.01 C27B C28B
DFIX 1.52 0.01 C28B C29
DFIX 1.44 0.01 N2A C30A
DFIX 1.44 0.01 N2B C30B
ISOR 0.01 O8 N2B C27B
SIMU .005 .005 2.5 C26 C27A C27B
 The H atoms were introduced at calculated positions and were treated as 
 riding atoms with an isotropic displacement parameter equal to 1.2 times 
 that of the parent atom (1.5 for CH₃). 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.0625P)²+4.1477P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_chemical_absolute_configuration ad
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.023(8)
_refine_ls_number_reflns         11154
_refine_ls_number_parameters     478
_refine_ls_number_restraints     50
_refine_ls_R_factor_all          0.0408
_refine_ls_R_factor_gt           0.0379
_refine_ls_wR_factor_ref         0.1009
_refine_ls_wR_factor_gt          0.0992
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_restrained_S_all      1.079
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        30.51
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         2.490
_refine_diff_density_min         -1.657
_refine_diff_density_rms         0.122

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
U1 U 0.03344(2) 0.426796(13) 0.54850(2) 0.03692(6) Uani 1 1 d . . .
U2 U 0.44385(3) 0.559454(13) 0.91467(3) 0.04215(7) Uani 1 1 d . . .
O1 O 0.1349(7) 0.4780(3) 0.4506(7) 0.0520(13) Uani 1 1 d . . .
O2 O -0.0722(7) 0.3763(3) 0.6410(7) 0.0536(14) Uani 1 1 d . . .
O3 O 0.5000(10) 0.6038(3) 0.7796(9) 0.076(2) Uani 1 1 d . . .
O4 O 0.3894(8) 0.5146(4) 1.0469(7) 0.0609(17) Uani 1 1 d . . .
O5 O 0.2342(6) 0.4148(3) 0.7051(6) 0.0532(14) Uani 1 1 d . . .
O6 O 0.4452(7) 0.4544(3) 0.8038(7) 0.0506(14) Uani 1 1 d . . .
O7 O 0.6495(7) 0.1651(3) 0.9945(8) 0.0621(17) Uani 1 1 d . . .
O8 O 0.4209(8) 0.1409(4) 0.9404(10) 0.083(2) Uani 1 1 d U . .
O9 O 0.0160(6) 0.5228(3) 0.6849(6) 0.0487(13) Uani 1 1 d . . .
O10 O 0.2009(7) 0.5672(3) 0.8164(6) 0.0537(14) Uani 1 1 d . . .
O11 O 0.0394(6) 0.8541(3) 0.6478(6) 0.0501(12) Uani 1 1 d . . .
O12 O -0.1563(7) 0.8240(3) 0.5154(6) 0.0496(13) Uani 1 1 d . . .
O13 O -0.1804(6) 0.4763(3) 0.4377(7) 0.0559(15) Uani 1 1 d . . .
O14 O 0.6872(6) 0.5194(4) 0.9679(8) 0.070(2) Uani 1 1 d D . .
N1 N -0.4166(10) 0.4491(8) 0.3672(12) 0.096(4) Uani 1 1 d . . .
N2A N 0.9285(10) 0.4810(7) 1.0190(12) 0.058(4) Uani 0.500(18) 1 d PD . .
N2B N 0.9153(10) 0.5231(7) 1.1032(12) 0.051(4) Uani 0.500(18) 1 d PDU A .
C1 C 0.3986(8) 0.2843(4) 0.8298(8) 0.0447(16) Uani 1 1 d . . .
C2 C 0.4362(8) 0.3373(3) 0.7241(7) 0.0375(13) Uani 1 1 d . . .
H2 H 0.3920 0.3202 0.6387 0.045 Uiso 1 1 calc R . .
C3 C 0.6027(9) 0.3361(4) 0.7271(10) 0.0520(19) Uani 1 1 d . . .
H3A H 0.6470 0.3761 0.7731 0.062 Uiso 1 1 calc R . .
H3B H 0.6278 0.3363 0.6392 0.062 Uiso 1 1 calc R . .
C4 C 0.6577(9) 0.2687(4) 0.7989(11) 0.055(2) Uani 1 1 d . . .
H4A H 0.7218 0.2433 0.7492 0.066 Uiso 1 1 calc R . .
H4B H 0.7105 0.2789 0.8844 0.066 Uiso 1 1 calc R . .
C5 C 0.5169(9) 0.2272(4) 0.8104(9) 0.0491(18) Uani 1 1 d . . .
C6 C 0.3697(8) 0.4069(3) 0.7443(7) 0.0367(13) Uani 1 1 d . . .
C7 C 0.5346(10) 0.1757(4) 0.9219(11) 0.058(2) Uani 1 1 d . . .
C8 C 0.4372(10) 0.3138(5) 0.9723(7) 0.052(2) Uani 1 1 d . . .
H8A H 0.3789 0.3541 0.9816 0.079 Uiso 1 1 calc R . .
H8B H 0.5393 0.3258 0.9878 0.079 Uiso 1 1 calc R . .
H8C H 0.4167 0.2795 1.0341 0.079 Uiso 1 1 calc R . .
C9 C 0.2397(9) 0.2620(5) 0.8096(10) 0.0535(19) Uani 1 1 d . . .
H9A H 0.2211 0.2329 0.8804 0.080 Uiso 1 1 calc R . .
H9B H 0.2193 0.2371 0.7292 0.080 Uiso 1 1 calc R . .
H9C H 0.1778 0.3020 0.8064 0.080 Uiso 1 1 calc R . .
C10 C 0.4692(13) 0.1852(5) 0.6882(12) 0.071(3) Uani 1 1 d . . .
H10A H 0.5395 0.1493 0.6811 0.107 Uiso 1 1 calc R . .
H10B H 0.4632 0.2146 0.6133 0.107 Uiso 1 1 calc R . .
H10C H 0.3749 0.1651 0.6931 0.107 Uiso 1 1 calc R . .
C11 C -0.0211(9) 0.6337(4) 0.7623(7) 0.0436(15) Uani 1 1 d . . .
H11 H -0.1226 0.6171 0.7519 0.052 Uiso 1 1 calc R . .
C12 C -0.0127(10) 0.6837(4) 0.6489(8) 0.0494(17) Uani 1 1 d . . .
C13 C -0.0875(8) 0.7498(4) 0.6992(8) 0.0431(15) Uani 1 1 d . . .
C14 C -0.0165(11) 0.7522(4) 0.8423(9) 0.0547(19) Uani 1 1 d . . .
H14A H -0.0780 0.7778 0.8942 0.066 Uiso 1 1 calc R . .
H14B H 0.0786 0.7745 0.8496 0.066 Uiso 1 1 calc R . .
C15 C 0.0009(9) 0.6740(4) 0.8913(8) 0.0477(16) Uani 1 1 d . . .
H15A H 0.0974 0.6657 0.9394 0.057 Uiso 1 1 calc R . .
H15B H -0.0731 0.6620 0.9455 0.057 Uiso 1 1 calc R . .
C16 C 0.0732(8) 0.5698(4) 0.7561(7) 0.0395(14) Uani 1 1 d . . .
C17 C -0.0656(7) 0.8135(4) 0.6186(7) 0.0389(14) Uani 1 1 d . . .
C18 C -0.0918(17) 0.6567(6) 0.5170(11) 0.082(4) Uani 1 1 d . . .
H18A H -0.0420 0.6164 0.4916 0.123 Uiso 1 1 calc R . .
H18B H -0.0910 0.6918 0.4518 0.123 Uiso 1 1 calc R . .
H18C H -0.1913 0.6450 0.5258 0.123 Uiso 1 1 calc R . .
C19 C 0.1501(12) 0.6997(6) 0.6372(13) 0.074(3) Uani 1 1 d . . .
H19A H 0.2015 0.7108 0.7216 0.111 Uiso 1 1 calc R . .
H19B H 0.1551 0.7381 0.5796 0.111 Uiso 1 1 calc R . .
H19C H 0.1945 0.6601 0.6031 0.111 Uiso 1 1 calc R . .
C20 C -0.2518(12) 0.7372(6) 0.6965(12) 0.074(3) Uani 1 1 d . . .
H20A H -0.2968 0.7777 0.7266 0.110 Uiso 1 1 calc R . .
H20B H -0.2664 0.6990 0.7520 0.110 Uiso 1 1 calc R . .
H20C H -0.2953 0.7271 0.6090 0.110 Uiso 1 1 calc R . .
C21 C -0.3189(10) 0.4770(6) 0.4425(13) 0.073(3) Uani 1 1 d . . .
C22 C -0.3892(13) 0.5182(6) 0.5457(12) 0.073(3) Uani 1 1 d . . .
H22A H -0.3728 0.4956 0.6299 0.087 Uiso 1 1 calc R . .
H22B H -0.3507 0.5647 0.5543 0.087 Uiso 1 1 calc R . .
C23 C -0.5464(13) 0.5181(7) 0.4920(15) 0.077(3) Uani 1 1 d . . .
H23A H -0.5745 0.5618 0.4505 0.092 Uiso 1 1 calc R . .
H23B H -0.6066 0.5098 0.5602 0.092 Uiso 1 1 calc R . .
C24 C -0.5642(10) 0.4563(7) 0.3869(11) 0.072(3) Uani 1 1 d . . .
H24A H -0.6018 0.4147 0.4221 0.087 Uiso 1 1 calc R . .
H24B H -0.6266 0.4693 0.3075 0.087 Uiso 1 1 calc R . .
C25 C -0.3824(14) 0.4050(9) 0.2617(13) 0.091(5) Uani 1 1 d . . .
H25A H -0.2850 0.4148 0.2437 0.136 Uiso 1 1 calc R . .
H25B H -0.4513 0.4135 0.1851 0.136 Uiso 1 1 calc R . .
H25C H -0.3884 0.3576 0.2868 0.136 Uiso 1 1 calc R . .
C26 C 0.8045(8) 0.5065(6) 1.0263(10) 0.082(3) Uani 1 1 d DU A .
C27A C 0.8544(15) 0.5521(14) 1.1556(17) 0.086(4) Uani 0.500(18) 1 d PDU A 1
H27A H 0.8087 0.5363 1.2280 0.103 Uiso 0.500(18) 1 d PR A 1
H27B H 0.8242 0.5988 1.1367 0.103 Uiso 0.500(18) 1 d PR A 1
C28A C 1.0176(15) 0.5550(7) 1.1745(17) 0.079(7) Uani 0.500(18) 1 d PD A 1
H28A H 1.0386 0.5543 1.2678 0.095 Uiso 0.500(18) 1 d PR A 1
H28B H 1.0659 0.5935 1.1406 0.095 Uiso 0.500(18) 1 d PR A 1
C30A C 0.899(3) 0.4267(8) 0.9280(12) 0.059(5) Uani 0.500(18) 1 d PD A 1
H30A H 0.8089 0.4354 0.8726 0.089 Uiso 0.500(18) 1 d PR A 1
H30B H 0.9779 0.4237 0.8761 0.089 Uiso 0.500(18) 1 d PR A 1
H30C H 0.8922 0.3840 0.9736 0.089 Uiso 0.500(18) 1 d PR A 1
C27B C 0.8784(14) 0.4363(8) 0.975(2) 0.084(4) Uani 0.500(18) 1 d PDU A 2
H27C H 0.8577 0.4375 0.8821 0.101 Uiso 0.500(18) 1 d PR A 2
H27D H 0.8321 0.3961 1.0052 0.101 Uiso 0.500(18) 1 d PR A 2
C28B C 1.0427(14) 0.4356(9) 1.0028(15) 0.057(4) Uani 0.500(18) 1 d PD A 2
H28C H 1.0957 0.4508 0.9345 0.069 Uiso 0.500(18) 1 d PR A 2
H28D H 1.0723 0.3895 1.0277 0.069 Uiso 0.500(18) 1 d PR A 2
C30B C 0.881(3) 0.5767(8) 1.187(2) 0.062(6) Uani 0.500(18) 1 d PD A 2
H30D H 0.7812 0.5875 1.1540 0.093 Uiso 0.500(18) 1 d PR A 2
H30E H 0.8887 0.5654 1.2777 0.093 Uiso 0.500(18) 1 d PR A 2
H30F H 0.9423 0.6157 1.1757 0.093 Uiso 0.500(18) 1 d PR A 2
C29 C 1.0509(10) 0.4852(6) 1.1190(9) 0.067(3) Uani 1 1 d D A .
H29A H 1.1414 0.4879 1.0831 0.080 Uiso 0.500(18) 1 d PR . .
H29B H 1.0560 0.4479 1.1804 0.080 Uiso 0.500(18) 1 d PR . .
H29C H 1.0689 0.4606 1.2001 0.080 Uiso 0.500(18) 1 d PR . .
H29D H 1.1295 0.5171 1.1133 0.080 Uiso 0.500(18) 1 d PR . .


_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 O2 1.756(6) . ?
U1 O1 1.775(6) . ?
U1 O5 2.297(6) . ?
U1 O13 2.343(6) . ?
U1 O9 2.357(6) . ?
U1 O12 2.429(6) 2_546 ?
U1 O11 2.490(6) 2_546 ?
U2 O4 1.755(7) . ?
U2 O3 1.780(8) . ?
U2 O10 2.330(6) . ?
U2 O6 2.341(6) . ?
U2 O14 2.363(6) . ?
U2 O8 2.406(7) 2_657 ?
U2 O7 2.460(6) 2_657 ?
O5 C6 1.267(9) . ?
O6 C6 1.262(8) . ?
O7 C7 1.228(11) . ?
O7 U2 2.460(6) 2_647 ?
O8 C7 1.281(11) . ?
O8 U2 2.406(7) 2_647 ?
O9 C16 1.244(9) . ?
O10 C16 1.254(9) . ?
O11 C17 1.251(9) . ?
O11 U1 2.491(6) 2_556 ?
O12 C17 1.280(9) . ?
O12 U1 2.429(6) 2_556 ?
O13 C21 1.283(11) . ?
O14 C26 1.189(8) . ?
N1 C21 1.232(16) . ?
N1 C24 1.409(13) . ?
N1 C25 1.457(18) . ?
N2A C26 1.257(8) . ?
N2A C30A 1.414(9) . ?
N2A C29 1.424(8) . ?
N2B C26 1.247(8) . ?
N2B C30B 1.416(10) . ?
N2B C29 1.439(9) . ?
C1 C9 1.512(11) . ?
C1 C2 1.576(10) . ?
C1 C8 1.579(11) . ?
C1 C5 1.584(11) . ?
C2 C6 1.509(9) . ?
C2 C3 1.529(11) . ?
C2 H2 0.9800 . ?
C3 C4 1.555(12) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 C5 1.544(11) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C10 1.519(15) . ?
C5 C7 1.520(11) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 C16 1.518(10) . ?
C11 C12 1.534(11) . ?
C11 C15 1.538(10) . ?
C11 H11 0.9800 . ?
C12 C18 1.548(14) . ?
C12 C19 1.552(13) . ?
C12 C13 1.580(10) . ?
C13 C17 1.521(10) . ?
C13 C20 1.528(13) . ?
C13 C14 1.536(12) . ?
C14 C15 1.602(12) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 C22 1.546(18) . ?
C22 C23 1.477(17) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C23 C24 1.613(19) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 C27A 1.619(8) . ?
C26 C27B 1.642(9) . ?
C27A C28A 1.489(10) . ?
C27A H27A 0.9600 . ?
C27A H27B 0.9601 . ?
C28A C29 1.519(10) . ?
C28A H28A 0.9599 . ?
C28A H28B 0.9599 . ?
C30A H30A 0.9600 . ?
C30A H30B 0.9601 . ?
C30A H30C 0.9599 . ?
C27B C28B 1.500(10) . ?
C27B H27C 0.9600 . ?
C27B H27D 0.9598 . ?
C28B C29 1.536(10) . ?
C28B H28C 0.9600 . ?
C28B H28D 0.9601 . ?
C30B H30D 0.9600 . ?
C30B H30E 0.9600 . ?
C30B H30F 0.9599 . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9601 . ?
C29 H29C 0.9600 . ?
C29 H29D 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
O2 U1 O1 178.0(3) . . ?
O2 U1 O5 90.6(3) . . ?
O1 U1 O5 91.4(3) . . ?
O2 U1 O13 90.3(3) . . ?
O1 U1 O13 87.9(3) . . ?
O5 U1 O13 158.0(2) . . ?
O2 U1 O9 91.4(3) . . ?
O1 U1 O9 89.1(3) . . ?
O5 U1 O9 76.8(2) . . ?
O13 U1 O9 81.3(2) . . ?
O2 U1 O12 90.3(3) . 2_546 ?
O1 U1 O12 90.1(3) . 2_546 ?
O5 U1 O12 75.52(19) . 2_546 ?
O13 U1 O12 126.4(2) . 2_546 ?
O9 U1 O12 152.2(2) . 2_546 ?
O2 U1 O11 91.3(3) . 2_546 ?
O1 U1 O11 87.4(3) . 2_546 ?
O5 U1 O11 128.30(19) . 2_546 ?
O13 U1 O11 73.6(2) . 2_546 ?
O9 U1 O11 154.8(2) . 2_546 ?
O12 U1 O11 52.81(19) 2_546 2_546 ?
O4 U2 O3 179.1(3) . . ?
O4 U2 O10 90.7(3) . . ?
O3 U2 O10 89.4(4) . . ?
O4 U2 O6 88.4(3) . . ?
O3 U2 O6 90.7(3) . . ?
O10 U2 O6 84.9(2) . . ?
O4 U2 O14 91.1(3) . . ?
O3 U2 O14 88.5(4) . . ?
O10 U2 O14 160.9(2) . . ?
O6 U2 O14 76.1(2) . . ?
O4 U2 O8 91.0(4) . 2_657 ?
O3 U2 O8 89.6(4) . 2_657 ?
O10 U2 O8 127.8(2) . 2_657 ?
O6 U2 O8 147.3(2) . 2_657 ?
O14 U2 O8 71.2(2) . 2_657 ?
O4 U2 O7 87.8(3) . 2_657 ?
O3 U2 O7 93.1(3) . 2_657 ?
O10 U2 O7 75.4(2) . 2_657 ?
O6 U2 O7 160.0(2) . 2_657 ?
O14 U2 O7 123.7(2) . 2_657 ?
O8 U2 O7 52.5(2) 2_657 2_657 ?
C6 O5 U1 154.1(6) . . ?
C6 O6 U2 146.6(5) . . ?
C7 O7 U2 93.3(5) . 2_647 ?
C7 O8 U2 94.4(5) . 2_647 ?
C16 O9 U1 151.3(5) . . ?
C16 O10 U2 175.9(6) . . ?
C17 O11 U1 92.7(5) . 2_556 ?
C17 O12 U1 94.8(4) . 2_556 ?
C21 O13 U1 139.3(7) . . ?
C26 O14 U2 162.3(7) . . ?
C21 N1 C24 119.9(14) . . ?
C21 N1 C25 121.3(11) . . ?
C24 N1 C25 118.7(11) . . ?
C26 N2A C30A 104.1(12) . . ?
C26 N2A C29 124.6(9) . . ?
C30A N2A C29 125.9(11) . . ?
C26 N2B C30B 110.5(12) . . ?
C26 N2B C29 124.1(8) . . ?
C30B N2B C29 124.5(12) . . ?
C9 C1 C2 113.1(6) . . ?
C9 C1 C8 108.7(8) . . ?
C2 C1 C8 111.8(6) . . ?
C9 C1 C5 116.9(7) . . ?
C2 C1 C5 98.5(6) . . ?
C8 C1 C5 107.6(6) . . ?
C6 C2 C3 115.8(6) . . ?
C6 C2 C1 110.8(6) . . ?
C3 C2 C1 107.0(6) . . ?
C6 C2 H2 107.6 . . ?
C3 C2 H2 107.6 . . ?
C1 C2 H2 107.6 . . ?
C2 C3 C4 106.4(6) . . ?
C2 C3 H3A 110.5 . . ?
C4 C3 H3A 110.5 . . ?
C2 C3 H3B 110.5 . . ?
C4 C3 H3B 110.5 . . ?
H3A C3 H3B 108.6 . . ?
C5 C4 C3 104.7(6) . . ?
C5 C4 H4A 110.8 . . ?
C3 C4 H4A 110.8 . . ?
C5 C4 H4B 110.8 . . ?
C3 C4 H4B 110.8 . . ?
H4A C4 H4B 108.9 . . ?
C10 C5 C7 105.6(8) . . ?
C10 C5 C4 111.3(9) . . ?
C7 C5 C4 113.5(7) . . ?
C10 C5 C1 110.9(7) . . ?
C7 C5 C1 111.5(7) . . ?
C4 C5 C1 104.1(6) . . ?
O6 C6 O5 121.4(6) . . ?
O6 C6 C2 120.9(6) . . ?
O5 C6 C2 117.6(6) . . ?
O7 C7 O8 118.2(8) . . ?
O7 C7 C5 124.7(8) . . ?
O8 C7 C5 117.1(8) . . ?
C1 C8 H8A 109.5 . . ?
C1 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C1 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C1 C9 H9A 109.5 . . ?
C1 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C1 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C5 C10 H10A 109.5 . . ?
C5 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C5 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C16 C11 C12 113.2(6) . . ?
C16 C11 C15 116.4(6) . . ?
C12 C11 C15 109.3(6) . . ?
C16 C11 H11 105.7 . . ?
C12 C11 H11 105.7 . . ?
C15 C11 H11 105.7 . . ?
C11 C12 C18 113.3(8) . . ?
C11 C12 C19 109.7(8) . . ?
C18 C12 C19 109.9(9) . . ?
C11 C12 C13 101.0(6) . . ?
C18 C12 C13 113.2(8) . . ?
C19 C12 C13 109.5(8) . . ?
C17 C13 C20 109.0(6) . . ?
C17 C13 C14 115.8(7) . . ?
C20 C13 C14 108.1(7) . . ?
C17 C13 C12 112.4(6) . . ?
C20 C13 C12 109.8(8) . . ?
C14 C13 C12 101.3(6) . . ?
C13 C14 C15 106.7(7) . . ?
C13 C14 H14A 110.4 . . ?
C15 C14 H14A 110.4 . . ?
C13 C14 H14B 110.4 . . ?
C15 C14 H14B 110.4 . . ?
H14A C14 H14B 108.6 . . ?
C11 C15 C14 102.2(6) . . ?
C11 C15 H15A 111.3 . . ?
C14 C15 H15A 111.3 . . ?
C11 C15 H15B 111.3 . . ?
C14 C15 H15B 111.3 . . ?
H15A C15 H15B 109.2 . . ?
O9 C16 O10 123.8(7) . . ?
O9 C16 C11 115.2(6) . . ?
O10 C16 C11 120.9(7) . . ?
O11 C17 O12 119.7(7) . . ?
O11 C17 C13 122.3(7) . . ?
O12 C17 C13 117.9(6) . . ?
C12 C18 H18A 109.5 . . ?
C12 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C12 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C12 C19 H19A 109.5 . . ?
C12 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C12 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C13 C20 H20A 109.5 . . ?
C13 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C13 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
N1 C21 O13 127.8(14) . . ?
N1 C21 C22 109.0(10) . . ?
O13 C21 C22 123.1(11) . . ?
C23 C22 C21 102.8(10) . . ?
C23 C22 H22A 111.2 . . ?
C21 C22 H22A 111.2 . . ?
C23 C22 H22B 111.2 . . ?
C21 C22 H22B 111.2 . . ?
H22A C22 H22B 109.1 . . ?
C22 C23 C24 105.0(9) . . ?
C22 C23 H23A 110.8 . . ?
C24 C23 H23A 110.8 . . ?
C22 C23 H23B 110.8 . . ?
C24 C23 H23B 110.8 . . ?
H23A C23 H23B 108.8 . . ?
N1 C24 C23 99.3(10) . . ?
N1 C24 H24A 111.9 . . ?
C23 C24 H24A 111.9 . . ?
N1 C24 H24B 111.9 . . ?
C23 C24 H24B 111.9 . . ?
H24A C24 H24B 109.6 . . ?
N1 C25 H25A 109.5 . . ?
N1 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
N1 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
O14 C26 N2B 151.1(9) . . ?
O14 C26 N2A 145.2(9) . . ?
O14 C26 C27A 116.1(8) . . ?
N2A C26 C27A 96.3(6) . . ?
O14 C26 C27B 113.5(7) . . ?
N2B C26 C27B 94.7(7) . . ?
C28A C27A C26 107.2(7) . . ?
C28A C27A H27A 116.9 . . ?
C26 C27A H27A 111.6 . . ?
C28A C27A H27B 104.5 . . ?
C26 C27A H27B 107.8 . . ?
H27A C27A H27B 108.4 . . ?
C27A C28A C29 99.7(10) . . ?
C27A C28A H28A 101.0 . . ?
C29 C28A H28A 110.2 . . ?
C27A C28A H28B 119.4 . . ?
C29 C28A H28B 115.3 . . ?
H28A C28A H28B 109.9 . . ?
N2A C30A H30A 109.6 . . ?
N2A C30A H30B 109.4 . . ?
H30A C30A H30B 109.5 . . ?
N2A C30A H30C 109.5 . . ?
H30A C30A H30C 109.5 . . ?
H30B C30A H30C 109.4 . . ?
C28B C27B C26 113.5(9) . . ?
C28B C27B H27C 104.2 . . ?
C26 C27B H27C 105.6 . . ?
C28B C27B H27D 114.4 . . ?
C26 C27B H27D 110.4 . . ?
H27C C27B H27D 108.0 . . ?
C27B C28B C29 94.7(9) . . ?
C27B C28B H28C 117.4 . . ?
C29 C28B H28C 114.3 . . ?
C27B C28B H28D 107.5 . . ?
C29 C28B H28D 113.0 . . ?
H28C C28B H28D 109.3 . . ?
N2B C30B H30D 103.1 . . ?
N2B C30B H30E 116.3 . . ?
H30D C30B H30E 109.5 . . ?
N2B C30B H30F 108.8 . . ?
H30D C30B H30F 109.5 . . ?
H30E C30B H30F 109.5 . . ?
N2A C29 C28A 98.4(8) . . ?
N2B C29 C28B 106.4(8) . . ?
N2A C29 H29A 111.2 . . ?
C28A C29 H29A 109.2 . . ?
N2A C29 H29B 113.6 . . ?
C28A C29 H29B 114.6 . . ?
H29A C29 H29B 109.5 . . ?
N2B C29 H29C 113.3 . . ?
C28B C29 H29C 111.1 . . ?
N2B C29 H29D 108.2 . . ?
H29C C29 H29D 109.5 . . ?
_database_code_depnum_ccdc_archive 'CCDC 978148'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_4

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40 H60 Cu N2 O18 U2'
_chemical_formula_weight         1396.50

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2'

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

_cell_length_a                   19.5109(15)
_cell_length_b                   18.8200(10)
_cell_length_c                   13.9091(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 109.813(4)
_cell_angle_gamma                90.00
_cell_volume                     4805.0(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    79699
_cell_measurement_theta_min      3.11
_cell_measurement_theta_max      28.70

_exptl_crystal_description       platelet
_exptl_crystal_colour            'translucent light green'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.930
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2684
_exptl_absorpt_coefficient_mu    7.234
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.440
_exptl_absorpt_correction_T_max  0.805
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_special_details           'crystal-to-detector distance 30 mm'
_diffrn_ambient_temperature      150(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 area-detector diffractometer'
_diffrn_measurement_method       
'two φ and five ω scans with 2° steps (451 frames)'
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            79699
_diffrn_reflns_av_R_equivalents  0.0336
_diffrn_reflns_av_unetI/netI     0.0473
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.11
_diffrn_reflns_theta_max         28.70
_reflns_number_total             12387
_reflns_number_gt                8355
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  
'SHELXTL (Sheldrick, 2008); PLATON (Spek, 2003)'

_refine_special_details          
;
 Structure solved by direct methods and subsequent Fourier-difference
 synthesis. The two half-camphorate ligands in the asymmetric unit, both
 with the other half generated by a twofold rotation axis, are highly 
 disordered, with an occupancy of 0.5 for the different components. Due
 to the disorder and the quite low crystal quality, the use of many restraints
 was necessary:
DFIX 1.52 0.01 C11 C15
DFIX 2.38 0.01 C12 C15
DFIX 1.52 0.01 C12 C18
DFIX 1.52 0.01 C12 C19
DFIX 1.52 0.01 C14 C15
DFIX 1.52 0.01 C21 C23
DFIX 1.52 0.01 C22 C26A
DFIX 1.52 0.01 C22 C26B
DFIX 2.55 0.01 C26A C26B
DFIX 1.52 0.01 C23 C24
DFIX 1.52 0.01 C29 C30
DFIX 1.52 0.01 C28 C32
DFIX 1.52 0.01 C28 C33
DFIX 1.52 0.01 N2 C43
ISOR 0.01 O2 O9 C5 C8 C12 C14 C18 C19 C20 C22 C25
ISOR 0.01 C27 C30 C32 C33 C38 C41
SIMU .005 .005 3. C11 C13 C14 C15 C18 C20
SIMU .01 .01 3. C21 C22 C23 C24 C26A C26B
SIMU .01 .01 3. C27 C29 C30
SIMU .01 .01 3. C35 C36 C37 
 ADDSYM suggests C2/m as a possible space group with 91% fit, but
 a chiral space group is necessary, a pure enantiomeric form of the
 ligand having been used. The Flack parameter deviates from 0, but
 it gives nevertheless the right enantiomer. All non-hydrogen atoms were 
 refined with anisotropic displacement parameters. The H atoms were 
 introduced at calculated positions and were treated as riding atoms with 
 an isotropic displacement parameter equal to 1.2 times that of the parent 
 atom (1.5 for CH₃). 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.1009P)²+37.8832P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_chemical_absolute_configuration ad
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.117(16)
_refine_ls_number_reflns         12387
_refine_ls_number_parameters     609
_refine_ls_number_restraints     291
_refine_ls_R_factor_all          0.1013
_refine_ls_R_factor_gt           0.0678
_refine_ls_wR_factor_ref         0.1941
_refine_ls_wR_factor_gt          0.1787
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_restrained_S_all      1.042
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        28.70
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.581
_refine_diff_density_min         -1.825
_refine_diff_density_rms         0.149

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
U1 U 0.727682(18) 0.471379(12) 0.73013(3) 0.04663(14) Uani 1 1 d . . .
U2 U 0.77202(2) 0.47104(3) 1.27943(3) 0.05199(15) Uani 1 1 d . . .
Cu Cu 0.75143(7) 0.4684(2) 1.00705(15) 0.0647(5) Uani 1 1 d . . .
O1 O 0.7195(4) 0.5308(5) 0.8257(7) 0.051(2) Uani 1 1 d . . .
O2 O 0.7328(5) 0.4136(5) 0.6340(8) 0.056(2) Uani 1 1 d U . .
O3 O 0.7851(5) 0.4154(5) 1.1831(7) 0.049(2) Uani 1 1 d . . .
O4 O 0.7596(6) 0.5248(7) 1.3775(9) 0.072(3) Uani 1 1 d . . .
O5 O 0.7033(4) 0.5694(4) 0.6095(6) 0.0412(18) Uani 1 1 d . . .
O6 O 0.8195(4) 0.5496(5) 0.7030(7) 0.053(2) Uani 1 1 d . . .
O7 O 0.8163(4) 0.8861(5) 0.6989(7) 0.052(2) Uani 1 1 d . . .
O8 O 0.7028(4) 0.8705(5) 0.6047(7) 0.049(2) Uani 1 1 d . . .
O9 O 0.6896(5) 0.3758(5) 0.8048(7) 0.054(2) Uani 1 1 d U . .
O10 O 0.6915(5) 0.3821(6) 0.9668(8) 0.064(3) Uani 1 1 d . . .
O11 O 0.6900(6) 0.0680(5) 0.7955(8) 0.060(3) Uani 1 1 d . . .
O12 O 0.6870(5) 0.0517(5) 0.9499(8) 0.059(3) Uani 1 1 d . . .
O13 O 0.8347(4) 0.4158(5) 1.0032(8) 0.058(3) Uani 1 1 d . . .
O14 O 0.8368(4) 0.4267(6) 0.8441(9) 0.064(3) Uani 1 1 d . . .
O15 O 0.6583(5) 0.5119(6) 1.1630(8) 0.069(3) Uani 1 1 d . . .
O16 O 0.6653(5) 0.5198(6) 1.0079(9) 0.066(3) Uani 1 1 d . . .
O17 O 0.5985(4) 0.4799(7) 0.6534(6) 0.054(3) Uani 1 1 d . . .
O18 O 0.9020(4) 0.4754(8) 1.3627(6) 0.0515(19) Uani 1 1 d . . .
N1 N 0.4818(9) 0.5080(13) 0.6225(14) 0.110(7) Uani 1 1 d . . .
N2 N 1.0211(5) 0.4580(7) 1.3834(8) 0.061(4) Uani 1 1 d D . .
C1 C 0.7912(7) 0.6554(7) 0.5920(10) 0.048(3) Uani 1 1 d . . .
H1 H 0.8410 0.6483 0.5922 0.058 Uiso 1 1 calc R . .
C2 C 0.7920(9) 0.7174(9) 0.6592(12) 0.075(4) Uani 1 1 d . . .
C3 C 0.7868(6) 0.7853(7) 0.5878(10) 0.044(3) Uani 1 1 d . . .
C4 C 0.7238(10) 0.7537(8) 0.4910(14) 0.074(5) Uani 1 1 d . . .
H4A H 0.7225 0.7777 0.4287 0.089 Uiso 1 1 calc R . .
H4B H 0.6766 0.7582 0.4992 0.089 Uiso 1 1 calc R . .
C5 C 0.7461(8) 0.6719(9) 0.4891(11) 0.067(5) Uani 1 1 d U . .
H5A H 0.7031 0.6420 0.4678 0.080 Uiso 1 1 calc R . .
H5B H 0.7727 0.6649 0.4423 0.080 Uiso 1 1 calc R . .
C6 C 0.7688(6) 0.5882(7) 0.6363(10) 0.046(3) Uani 1 1 d . . .
C7 C 0.7717(7) 0.8514(8) 0.6348(11) 0.053(3) Uani 1 1 d . . .
C8 C 0.8700(8) 0.7156(11) 0.7507(12) 0.081(4) Uani 1 1 d U . .
H8A H 0.8684 0.6815 0.8012 0.122 Uiso 1 1 calc R . .
H8B H 0.8806 0.7618 0.7815 0.122 Uiso 1 1 calc R . .
H8C H 0.9074 0.7024 0.7236 0.122 Uiso 1 1 calc R . .
C9 C 0.7380(7) 0.7201(9) 0.7126(10) 0.058(3) Uani 1 1 d . . .
H9A H 0.6903 0.7278 0.6636 0.087 Uiso 1 1 calc R . .
H9B H 0.7500 0.7583 0.7612 0.087 Uiso 1 1 calc R . .
H9C H 0.7387 0.6759 0.7475 0.087 Uiso 1 1 calc R . .
C10 C 0.8563(8) 0.7920(8) 0.5575(15) 0.080(5) Uani 1 1 d . . .
H10A H 0.8565 0.8374 0.5260 0.120 Uiso 1 1 calc R . .
H10B H 0.8566 0.7549 0.5103 0.120 Uiso 1 1 calc R . .
H10C H 0.8988 0.7879 0.6175 0.120 Uiso 1 1 calc R . .
C11 C 0.6325(9) 0.2849(9) 0.8692(12) 0.072(2) Uani 1 1 d DU . .
C12 C 0.6718(6) 0.2231(11) 0.8413(10) 0.086(5) Uani 1 1 d DU . .
C13 C 0.6295(9) 0.1555(9) 0.8597(14) 0.071(2) Uani 1 1 d U . .
H13 H 0.5863 0.1504 0.7984 0.086 Uiso 1 1 calc R . .
C14 C 0.6031(10) 0.1728(7) 0.9432(14) 0.079(2) Uani 1 1 d DU . .
H14A H 0.6305 0.1470 1.0046 0.094 Uiso 1 1 calc R . .
H14B H 0.5519 0.1607 0.9252 0.094 Uiso 1 1 calc R . .
C15 C 0.6144(10) 0.2538(7) 0.9600(12) 0.080(2) Uani 1 1 d DU . .
H15A H 0.5705 0.2756 0.9643 0.096 Uiso 1 1 calc R . .
H15B H 0.6540 0.2630 1.0233 0.096 Uiso 1 1 calc R . .
C16 C 0.6756(6) 0.3555(7) 0.8822(11) 0.049(3) Uani 1 1 d . . .
C17 C 0.6721(5) 0.0863(7) 0.8708(11) 0.044(3) Uani 1 1 d . . .
C18 C 0.6702(9) 0.2277(10) 0.7300(10) 0.081(2) Uani 1 1 d DU . .
H18A H 0.6894 0.2728 0.7191 0.122 Uiso 1 1 calc R . .
H18B H 0.6209 0.2230 0.6845 0.122 Uiso 1 1 calc R . .
H18C H 0.6993 0.1902 0.7172 0.122 Uiso 1 1 calc R . .
C19 C 0.7516(6) 0.2206(11) 0.8949(15) 0.090(5) Uani 1 1 d DU . .
H19A H 0.7614 0.2168 0.9672 0.136 Uiso 1 1 calc R . .
H19B H 0.7734 0.2632 0.8807 0.136 Uiso 1 1 calc R . .
H19C H 0.7716 0.1801 0.8717 0.136 Uiso 1 1 calc R . .
C20 C 0.5583(9) 0.2928(9) 0.7851(14) 0.081(2) Uani 1 1 d U . .
H20A H 0.5377 0.3381 0.7914 0.121 Uiso 1 1 calc R . .
H20B H 0.5264 0.2557 0.7917 0.121 Uiso 1 1 calc R . .
H20C H 0.5642 0.2894 0.7195 0.121 Uiso 1 1 calc R . .
C21 C 0.9356(6) 0.3673(7) 0.9685(10) 0.048(2) Uani 1 1 d DU . .
H21 H 0.9387 0.3382 0.9135 0.058 Uiso 0.50 1 d PR . .
C22 C 1.0000 0.4204(9) 1.0000 0.061(3) Uani 1 2 d SDU . .
C23 C 0.9687(8) 0.3287(13) 1.0697(15) 0.055(4) Uani 0.50 1 d PDU . .
H23A H 0.9488 0.2815 1.0590 0.066 Uiso 0.50 1 d PR . .
H23B H 0.9529 0.3509 1.1206 0.066 Uiso 0.50 1 d PR . .
C24 C 1.0527(7) 0.3191(8) 1.1122(12) 0.065(3) Uani 1 1 d DU . .
H24A H 1.0694 0.2717 1.1078 0.078 Uiso 0.50 1 d PR . .
H24B H 1.0746 0.3372 1.1803 0.078 Uiso 0.50 1 d PR . .
H24D H 1.0923 0.2860 1.1363 0.097 Uiso 0.50 1 d PR . .
H24E H 1.0500 0.3473 1.1684 0.097 Uiso 0.50 1 d PR . .
H24F H 1.0079 0.2936 1.0825 0.097 Uiso 0.50 1 d PR . .
C25 C 0.8634(6) 0.4061(6) 0.9356(9) 0.040(3) Uani 1 1 d U . .
C26A C 0.9970(14) 0.4880(11) 1.0568(15) 0.057(4) Uani 0.50 1 d PDU . .
H26A H 1.0419 0.5135 1.0702 0.086 Uiso 0.50 1 d PR . .
H26B H 0.9571 0.5173 1.0171 0.086 Uiso 0.50 1 d PR . .
H26C H 0.9906 0.4759 1.1203 0.086 Uiso 0.50 1 d PR . .
C26B C 1.0088(16) 0.4361(13) 0.8948(12) 0.062(4) Uani 0.50 1 d PDU . .
H26D H 0.9639 0.4616 0.8814 0.092 Uiso 0.50 1 d PR . .
H26E H 1.0486 0.4654 0.9344 0.092 Uiso 0.50 1 d PR . .
H26F H 1.0151 0.4239 0.8313 0.092 Uiso 0.50 1 d PR . .
C27 C 0.5662(6) 0.5712(7) 1.0346(10) 0.043(2) Uani 1 1 d U . .
H27 H 0.5691 0.6022 1.0907 0.051 Uiso 0.50 1 d PR . .
C28 C 0.4987(13) 0.5192(9) 1.0273(12) 0.030(5) Uani 0.50 1 d PD . .
C29 C 0.5578(8) 0.6196(8) 0.9503(12) 0.072(3) Uani 1 1 d DU . .
H29A H 0.5827 0.6039 0.9054 0.086 Uiso 0.50 1 d PR . .
H29B H 0.5726 0.6673 0.9720 0.086 Uiso 0.50 1 d PR . .
H29D H 0.6008 0.6481 0.9634 0.107 Uiso 0.50 1 d PR . .
H29E H 0.5499 0.5923 0.8891 0.107 Uiso 0.50 1 d PR . .
H29F H 0.5166 0.6499 0.9418 0.107 Uiso 0.50 1 d PR . .
C30 C 0.4740(9) 0.6121(15) 0.898(2) 0.059(4) Uani 0.50 1 d PDU . .
H30A H 0.4627 0.5885 0.8337 0.071 Uiso 0.50 1 d PR . .
H30B H 0.4535 0.6589 0.8867 0.071 Uiso 0.50 1 d PR . .
C31 C 0.6356(6) 0.5301(8) 1.0713(13) 0.055(4) Uani 1 1 d . . .
C32 C 0.4987(12) 0.4572(10) 0.9569(17) 0.044(6) Uani 0.50 1 d PDU . .
H32A H 0.4594 0.4251 0.9520 0.066 Uiso 0.50 1 d PR . .
H32B H 0.4933 0.4755 0.8903 0.066 Uiso 0.50 1 d PR . .
H32C H 0.5442 0.4324 0.9837 0.066 Uiso 0.50 1 d PR . .
C33 C 0.4976(13) 0.4891(13) 1.1285(14) 0.052(6) Uani 0.50 1 d PDU . .
H33A H 0.4569 0.4576 1.1171 0.077 Uiso 0.50 1 d PR . .
H33B H 0.5419 0.4644 1.1651 0.077 Uiso 0.50 1 d PR . .
H33C H 0.4921 0.5292 1.1678 0.077 Uiso 0.50 1 d PR . .
C34 C 0.5478(6) 0.5240(9) 0.6468(9) 0.057(4) Uani 1 1 d . . .
C35 C 0.5629(8) 0.6022(10) 0.6687(13) 0.073(3) Uani 1 1 d U . .
H35A H 0.5917 0.6106 0.7398 0.088 Uiso 1 1 calc R . .
H35B H 0.5872 0.6230 0.6251 0.088 Uiso 1 1 calc R . .
C36 C 0.4894(9) 0.6286(11) 0.6441(15) 0.090(4) Uani 1 1 d U . .
H36A H 0.4788 0.6617 0.5875 0.108 Uiso 1 1 calc R . .
H36B H 0.4850 0.6540 0.7025 0.108 Uiso 1 1 calc R . .
C37 C 0.4349(8) 0.5687(10) 0.6160(13) 0.077(4) Uani 1 1 d U . .
H37A H 0.4088 0.5649 0.6639 0.092 Uiso 1 1 calc R . .
H37B H 0.4003 0.5746 0.5474 0.092 Uiso 1 1 calc R . .
C38 C 0.4579(12) 0.4336(11) 0.6022(17) 0.085(6) Uani 1 1 d U . .
H38A H 0.4973 0.4025 0.6380 0.127 Uiso 1 1 calc R . .
H38B H 0.4434 0.4244 0.5301 0.127 Uiso 1 1 calc R . .
H38C H 0.4174 0.4253 0.6251 0.127 Uiso 1 1 calc R . .
C39 C 0.9519(7) 0.4366(7) 1.3621(10) 0.047(3) Uani 1 1 d . . .
C40 C 0.9551(8) 0.3583(10) 1.3444(11) 0.073(5) Uani 1 1 d . . .
H40A H 0.9308 0.3472 1.2727 0.088 Uiso 1 1 calc R . .
H40B H 0.9313 0.3322 1.3844 0.088 Uiso 1 1 calc R . .
C41 C 1.0354(9) 0.3382(10) 1.3770(15) 0.079(5) Uani 1 1 d U . .
H41A H 1.0513 0.3155 1.4435 0.095 Uiso 1 1 calc R . .
H41B H 1.0445 0.3064 1.3278 0.095 Uiso 1 1 calc R . .
C42 C 1.0734(8) 0.4073(11) 1.3809(12) 0.076(5) Uani 1 1 d . . .
H42A H 1.1164 0.4105 1.4416 0.091 Uiso 1 1 calc R . .
H42B H 1.0875 0.4136 1.3210 0.091 Uiso 1 1 calc R . .
C43 C 1.0419(9) 0.5356(8) 1.3968(13) 0.075(5) Uani 1 1 d D . .
H43A H 1.0668 0.5482 1.3504 0.113 Uiso 1 1 calc R . .
H43B H 1.0734 0.5438 1.4658 0.113 Uiso 1 1 calc R . .
H43C H 0.9988 0.5640 1.3828 0.113 Uiso 1 1 calc R . .


_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 O2 1.753(10) . ?
U1 O1 1.785(10) . ?
U1 O9 2.321(9) . ?
U1 O14 2.338(9) . ?
U1 O17 2.386(7) . ?
U1 O5 2.430(8) . ?
U1 O6 2.445(9) . ?
U2 O4 1.780(11) . ?
U2 O3 1.785(10) . ?
U2 O11 2.342(11) 4_657 ?
U2 O15 2.387(8) . ?
U2 O18 2.406(7) . ?
U2 O8 2.425(10) 4_647 ?
U2 O7 2.444(9) 4_647 ?
Cu O13 1.918(8) . ?
Cu O12 1.941(10) 4_657 ?
Cu O16 1.942(9) . ?
Cu O10 1.968(9) . ?
Cu O3 2.517(10) . ?
Cu O1 2.657(10) . ?
O5 C6 1.254(13) . ?
O6 C6 1.321(14) . ?
O7 C7 1.205(16) . ?
O7 U2 2.444(9) 4_657 ?
O8 C7 1.315(14) . ?
O8 U2 2.425(10) 4_657 ?
O9 C16 1.256(16) . ?
O10 C16 1.219(16) . ?
O11 C17 1.259(16) . ?
O11 U2 2.342(11) 4_647 ?
O12 C17 1.227(15) . ?
O12 Cu 1.941(10) 4_647 ?
O13 C25 1.260(15) . ?
O14 C25 1.261(15) . ?
O15 C31 1.247(17) . ?
O16 C31 1.224(16) . ?
O17 C34 1.271(17) . ?
O18 C39 1.219(16) . ?
N1 C34 1.25(2) . ?
N1 C37 1.45(2) . ?
N1 C38 1.47(3) . ?
N2 C39 1.343(16) . ?
N2 C42 1.405(19) . ?
N2 C43 1.510(9) . ?
C1 C5 1.438(18) . ?
C1 C2 1.49(2) . ?
C1 C6 1.533(18) . ?
C1 H1 0.9800 . ?
C2 C9 1.482(17) . ?
C2 C3 1.60(2) . ?
C2 C8 1.62(2) . ?
C3 C7 1.481(19) . ?
C3 C10 1.556(16) . ?
C3 C4 1.598(18) . ?
C4 C5 1.60(2) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 C12 1.52(2) . ?
C11 C20 1.53(2) . ?
C11 C15 1.537(9) . ?
C11 C16 1.55(2) . ?
C12 C19 1.481(9) . ?
C12 C18 1.539(9) . ?
C12 C13 1.58(3) . ?
C13 C14 1.46(2) . ?
C13 C17 1.52(2) . ?
C13 H13 0.9800 . ?
C14 C15 1.547(9) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 C25 1.514(16) . ?
C21 C23 1.520(10) . ?
C21 C24 1.520(19) 2_757 ?
C21 C22 1.548(16) . ?
C21 H21 0.9601 . ?
C22 C26A 1.509(10) . ?
C22 C26B 1.558(10) . ?
C23 C24 1.552(10) . ?
C23 H23A 0.9597 . ?
C23 H23B 0.9601 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9601 . ?
C24 H24D 0.9600 . ?
C24 H24E 0.9601 . ?
C24 H24F 0.9600 . ?
C26A H26A 0.9601 . ?
C26A H26B 0.9600 . ?
C26A H26C 0.9600 . ?
C26B H26D 0.9596 . ?
C26B H26E 0.9601 . ?
C26B H26F 0.9600 . ?
C27 C29 1.449(19) . ?
C27 C31 1.492(16) . ?
C27 C28 1.62(2) . ?
C27 H27 0.9599 . ?
C28 C33 1.524(10) . ?
C28 C32 1.525(10) . ?
C29 C30 1.552(10) . ?
C29 H29A 0.9601 . ?
C29 H29B 0.9600 . ?
C29 H29D 0.9600 . ?
C29 H29E 0.9601 . ?
C29 H29F 0.9600 . ?
C30 H30A 0.9599 . ?
C30 H30B 0.9602 . ?
C32 H32A 0.9598 . ?
C32 H32B 0.9599 . ?
C32 H32C 0.9602 . ?
C33 H33A 0.9599 . ?
C33 H33B 0.9601 . ?
C33 H33C 0.9602 . ?
C34 C35 1.51(2) . ?
C35 C36 1.44(2) . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
C36 C37 1.51(3) . ?
C36 H36A 0.9700 . ?
C36 H36B 0.9700 . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?
C39 C40 1.50(2) . ?
C40 C41 1.52(2) . ?
C40 H40A 0.9700 . ?
C40 H40B 0.9700 . ?
C41 C42 1.49(2) . ?
C41 H41A 0.9700 . ?
C41 H41B 0.9700 . ?
C42 H42A 0.9700 . ?
C42 H42B 0.9700 . ?
C43 H43A 0.9600 . ?
C43 H43B 0.9600 . ?
C43 H43C 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
O2 U1 O1 178.2(4) . . ?
O2 U1 O9 88.3(4) . . ?
O1 U1 O9 91.6(4) . . ?
O2 U1 O14 91.1(4) . . ?
O1 U1 O14 90.6(4) . . ?
O9 U1 O14 76.9(3) . . ?
O2 U1 O17 91.5(4) . . ?
O1 U1 O17 86.7(4) . . ?
O9 U1 O17 78.6(4) . . ?
O14 U1 O17 155.3(4) . . ?
O2 U1 O5 89.6(4) . . ?
O1 U1 O5 89.6(4) . . ?
O9 U1 O5 151.6(3) . . ?
O14 U1 O5 131.4(3) . . ?
O17 U1 O5 73.2(3) . . ?
O2 U1 O6 91.2(4) . . ?
O1 U1 O6 89.6(4) . . ?
O9 U1 O6 153.9(3) . . ?
O14 U1 O6 77.0(3) . . ?
O17 U1 O6 127.5(4) . . ?
O5 U1 O6 54.4(3) . . ?
O4 U2 O3 178.7(5) . . ?
O4 U2 O11 92.5(5) . 4_657 ?
O3 U2 O11 88.6(4) . 4_657 ?
O4 U2 O15 90.0(5) . . ?
O3 U2 O15 90.9(4) . . ?
O11 U2 O15 79.0(4) 4_657 . ?
O4 U2 O18 90.4(4) . . ?
O3 U2 O18 89.2(4) . . ?
O11 U2 O18 75.3(4) 4_657 . ?
O15 U2 O18 154.3(4) . . ?
O4 U2 O8 89.1(5) . 4_647 ?
O3 U2 O8 89.6(4) . 4_647 ?
O11 U2 O8 151.6(3) 4_657 4_647 ?
O15 U2 O8 129.4(3) . 4_647 ?
O18 U2 O8 76.3(4) . 4_647 ?
O4 U2 O7 89.6(5) . 4_647 ?
O3 U2 O7 89.7(4) . 4_647 ?
O11 U2 O7 155.1(3) 4_657 4_647 ?
O15 U2 O7 76.3(3) . 4_647 ?
O18 U2 O7 129.4(4) . 4_647 ?
O8 U2 O7 53.1(3) 4_647 4_647 ?
O13 Cu O12 89.1(4) . 4_657 ?
O13 Cu O16 178.2(5) . . ?
O12 Cu O16 92.5(4) 4_657 . ?
O13 Cu O10 89.6(4) . . ?
O12 Cu O10 178.1(5) 4_657 . ?
O16 Cu O10 88.9(4) . . ?
O13 Cu O3 83.0(4) . . ?
O12 Cu O3 95.1(4) 4_657 . ?
O16 Cu O3 97.6(4) . . ?
O10 Cu O3 83.3(4) . . ?
O13 Cu O1 97.5(4) . . ?
O12 Cu O1 81.8(4) 4_657 . ?
O16 Cu O1 82.0(4) . . ?
O10 Cu O1 99.7(4) . . ?
O3 Cu O1 176.9(4) . . ?
U1 O1 Cu 112.3(4) . . ?
U2 O3 Cu 116.2(5) . . ?
C6 O5 U1 93.9(7) . . ?
C6 O6 U1 91.4(7) . . ?
C7 O7 U2 94.7(8) . 4_657 ?
C7 O8 U2 92.7(8) . 4_657 ?
C16 O9 U1 144.6(9) . . ?
C16 O10 Cu 123.1(9) . . ?
C17 O11 U2 143.3(9) . 4_647 ?
C17 O12 Cu 129.7(9) . 4_647 ?
C25 O13 Cu 133.6(10) . . ?
C25 O14 U1 139.7(8) . . ?
C31 O15 U2 135.1(9) . . ?
C31 O16 Cu 134.8(11) . . ?
C34 O17 U1 139.0(10) . . ?
C39 O18 U2 133.7(11) . . ?
C34 N1 C37 113(2) . . ?
C34 N1 C38 120.7(19) . . ?
C37 N1 C38 125.9(19) . . ?
C39 N2 C42 118.3(13) . . ?
C39 N2 C43 121.7(11) . . ?
C42 N2 C43 119.5(12) . . ?
C5 C1 C2 109.1(14) . . ?
C5 C1 C6 114.6(11) . . ?
C2 C1 C6 109.8(10) . . ?
C5 C1 H1 107.7 . . ?
C2 C1 H1 107.7 . . ?
C6 C1 H1 107.7 . . ?
C9 C2 C1 118.8(13) . . ?
C9 C2 C3 112.2(14) . . ?
C1 C2 C3 104.5(11) . . ?
C9 C2 C8 104.3(12) . . ?
C1 C2 C8 106.5(14) . . ?
C3 C2 C8 110.5(12) . . ?
C7 C3 C10 111.9(11) . . ?
C7 C3 C4 118.3(11) . . ?
C10 C3 C4 107.1(12) . . ?
C7 C3 C2 112.2(11) . . ?
C10 C3 C2 110.8(11) . . ?
C4 C3 C2 95.4(11) . . ?
C3 C4 C5 103.7(14) . . ?
C3 C4 H4A 111.0 . . ?
C5 C4 H4A 111.0 . . ?
C3 C4 H4B 111.0 . . ?
C5 C4 H4B 111.0 . . ?
H4A C4 H4B 109.0 . . ?
C1 C5 C4 105.6(14) . . ?
C1 C5 H5A 110.6 . . ?
C4 C5 H5A 110.6 . . ?
C1 C5 H5B 110.6 . . ?
C4 C5 H5B 110.6 . . ?
H5A C5 H5B 108.8 . . ?
O5 C6 O6 120.0(11) . . ?
O5 C6 C1 120.9(10) . . ?
O6 C6 C1 119.2(10) . . ?
O5 C6 U1 59.7(6) . . ?
O6 C6 U1 60.5(6) . . ?
C1 C6 U1 175.6(9) . . ?
O7 C7 O8 119.5(13) . . ?
O7 C7 C3 125.4(11) . . ?
O8 C7 C3 115.1(12) . . ?
C2 C8 H8A 109.5 . . ?
C2 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C2 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C2 C9 H9A 109.5 . . ?
C2 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C2 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C3 C10 H10A 109.5 . . ?
C3 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C3 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C12 C11 C20 108.0(14) . . ?
C12 C11 C15 101.3(11) . . ?
C20 C11 C15 104.1(14) . . ?
C12 C11 C16 112.7(12) . . ?
C20 C11 C16 110.0(12) . . ?
C15 C11 C16 119.9(13) . . ?
C19 C12 C11 115.6(15) . . ?
C19 C12 C18 99.7(12) . . ?
C11 C12 C18 112.0(14) . . ?
C19 C12 C13 114.2(16) . . ?
C11 C12 C13 103.7(9) . . ?
C18 C12 C13 111.9(13) . . ?
C14 C13 C17 115.9(14) . . ?
C14 C13 C12 107.2(13) . . ?
C17 C13 C12 114.0(12) . . ?
C14 C13 H13 106.4 . . ?
C17 C13 H13 106.4 . . ?
C12 C13 H13 106.4 . . ?
C13 C14 C15 105.6(12) . . ?
C13 C14 H14A 110.6 . . ?
C15 C14 H14A 110.6 . . ?
C13 C14 H14B 110.6 . . ?
C15 C14 H14B 110.6 . . ?
H14A C14 H14B 108.8 . . ?
C11 C15 C14 108.2(11) . . ?
C11 C15 H15A 110.1 . . ?
C14 C15 H15A 110.1 . . ?
C11 C15 H15B 110.1 . . ?
C14 C15 H15B 110.1 . . ?
H15A C15 H15B 108.4 . . ?
O10 C16 O9 130.1(13) . . ?
O10 C16 C11 114.5(13) . . ?
O9 C16 C11 115.4(12) . . ?
O12 C17 O11 123.5(13) . . ?
O12 C17 C13 120.1(13) . . ?
O11 C17 C13 116.4(12) . . ?
C12 C18 H18A 109.5 . . ?
C12 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C12 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C12 C19 H19A 109.5 . . ?
C12 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C12 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C11 C20 H20A 109.5 . . ?
C11 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C11 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C25 C21 C23 124.9(12) . . ?
C23 C21 C24 106.0(14) . 2_757 ?
C25 C21 C22 111.0(10) . . ?
C25 C21 H21 109.7 . . ?
C23 C21 H21 110.1 . . ?
C22 C21 H21 109.3 . . ?
C26A C22 C21 124.6(11) . 2_757 ?
C26A C22 C21 121.3(11) . . ?
C21 C22 C21 99.6(13) 2_757 . ?
C26A C22 C26B 111.6(9) . . ?
C21 C22 C26B 101.2(11) . . ?
C21 C23 C24 118.1(14) . . ?
C21 C23 H23A 106.0 . . ?
C24 C23 H23A 105.8 . . ?
C21 C23 H23B 109.4 . . ?
C24 C23 H23B 109.4 . . ?
H23A C23 H23B 107.6 . . ?
C21 C23 H24F 123.5 . . ?
C24 C23 H24F 36.4 . . ?
H23A C23 H24F 69.8 . . ?
H23B C23 H24F 125.9 . . ?
C21 C24 C23 93.0(11) 2_757 . ?
C21 C24 H24A 111.6 2_757 . ?
C23 C24 H24A 114.9 . . ?
C21 C24 H24B 113.0 2_757 . ?
C23 C24 H24B 113.2 . . ?
H24A C24 H24B 110.2 . . ?
C21 C24 H24D 109.9 2_757 . ?
C21 C24 H24E 109.6 2_757 . ?
H24D C24 H24E 109.5 . . ?
C21 C24 H24F 108.9 2_757 . ?
H24D C24 H24F 109.5 . . ?
H24E C24 H24F 109.5 . . ?
O13 C25 O14 125.0(12) . . ?
O13 C25 C21 116.6(11) . . ?
O14 C25 C21 118.4(11) . . ?
C22 C26A H26A 109.1 . . ?
C22 C26A H26B 110.6 . . ?
H26A C26A H26B 109.5 . . ?
C22 C26A H26C 108.7 . . ?
H26A C26A H26C 109.5 . . ?
H26B C26A H26C 109.5 . . ?
H26D C26B H26E 109.5 . . ?
H26D C26B H26F 109.5 . . ?
H26E C26B H26F 109.5 . . ?
C29 C27 C31 116.4(11) . . ?
C29 C27 C28 95.5(11) . 2_657 ?
C31 C27 C28 109.1(11) . 2_657 ?
C29 C27 C30 103.0(14) . 2_657 ?
C31 C27 C30 128.1(13) . 2_657 ?
C28 C27 C30 98.7(11) 2_657 2_657 ?
C29 C27 C28 117.5(11) . . ?
C31 C27 C28 109.4(11) . . ?
C29 C27 H27 103.6 . . ?
C31 C27 H27 103.9 . . ?
C28 C27 H27 103.9 . . ?
C33 C28 C32 108.1(18) . . ?
C33 C28 C27 117.9(16) . 2_657 ?
C32 C28 C27 107.1(14) . 2_657 ?
C33 C28 C27 115.7(17) . . ?
C32 C28 C27 109.1(14) . . ?
C28 C28 C30 114.1(15) 2_657 2_657 ?
C27 C29 H29A 112.9 . . ?
C30 C29 H29A 110.8 . . ?
C27 C29 H29B 113.1 . . ?
C30 C29 H29B 113.0 . . ?
H29A C29 H29B 109.1 . . ?
C27 C29 H29D 110.1 . . ?
C27 C29 H29E 108.8 . . ?
H29D C29 H29E 109.5 . . ?
C27 C29 H29F 109.5 . . ?
H29D C29 H29F 109.5 . . ?
H29E C29 H29F 109.5 . . ?
C29 C30 C27 114.8(17) . 2_657 ?
C29 C30 H30A 110.4 . . ?
C27 C30 H30A 108.8 2_657 . ?
C28 C30 H30A 91.0 2_657 . ?
C29 C30 H30B 108.0 . . ?
C27 C30 H30B 106.3 2_657 . ?
H30A C30 H30B 108.3 . . ?
O16 C31 O15 127.1(12) . . ?
O16 C31 C27 115.6(14) . . ?
O15 C31 C27 117.3(12) . . ?
C33 C32 C28 103.6(18) 2_657 . ?
C28 C32 H32A 110.7 . . ?
C28 C32 H32B 108.8 . . ?
H32A C32 H32B 109.5 . . ?
C33 C32 H32C 103.8 2_657 . ?
C28 C32 H32C 108.9 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C28 C33 H33A 110.3 . . ?
C28 C33 H33B 112.2 . . ?
H33A C33 H33B 109.5 . . ?
C28 C33 H33C 105.8 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
N1 C34 C35 113.7(15) . . ?
O17 C34 C35 121.9(12) . . ?
C36 C35 C34 100.2(13) . . ?
C36 C35 H35A 111.7 . . ?
C34 C35 H35A 111.7 . . ?
C36 C35 H35B 111.7 . . ?
C34 C35 H35B 111.7 . . ?
H35A C35 H35B 109.5 . . ?
C35 C36 C37 111.1(16) . . ?
C35 C36 H36A 109.4 . . ?
C37 C36 H36A 109.4 . . ?
C35 C36 H36B 109.4 . . ?
C37 C36 H36B 109.4 . . ?
H36A C36 H36B 108.0 . . ?
N1 C37 C36 101.5(15) . . ?
N1 C37 H37A 111.5 . . ?
C36 C37 H37A 111.5 . . ?
N1 C37 H37B 111.5 . . ?
C36 C37 H37B 111.5 . . ?
H37A C37 H37B 109.3 . . ?
N1 C38 H38A 109.5 . . ?
N1 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
N1 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
O18 C39 N2 124.4(13) . . ?
O18 C39 C40 131.9(13) . . ?
N2 C39 C40 103.7(11) . . ?
C39 C40 C41 106.9(14) . . ?
C39 C40 H40A 110.3 . . ?
C41 C40 H40A 110.3 . . ?
C39 C40 H40B 110.3 . . ?
C41 C40 H40B 110.3 . . ?
H40A C40 H40B 108.6 . . ?
C42 C41 C40 104.1(14) . . ?
C42 C41 H41A 110.9 . . ?
C40 C41 H41A 110.9 . . ?
C42 C41 H41B 110.9 . . ?
C40 C41 H41B 110.9 . . ?
H41A C41 H41B 109.0 . . ?
N2 C42 C41 103.8(11) . . ?
N2 C42 H42A 111.0 . . ?
C41 C42 H42A 111.0 . . ?
N2 C42 H42B 111.0 . . ?
C41 C42 H42B 111.0 . . ?
H42A C42 H42B 109.0 . . ?
N2 C43 H43A 109.5 . . ?
N2 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
N2 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?

_database_code_depnum_ccdc_archive 'CCDC 978149'
