# Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2002


data_global

_journal_coden_Cambridge      182


loop_
_publ_author_name
_publ_author_address
'Karsten Meyer'
;    
University of California, San Diego
Department of Chemistry & Biochemistry
9500 Gilman Dr. MC 0358
La Jolla CA, 92093-0358
United States of America
;
'Ingrid Castro-Rodriguez'
;    
University of California, San Diego
Department of Chemistry & Biochemistry
9500 Gilman Dr. MC 0358
La Jolla CA, 92093-0358
United States of America
;
'Kristian Olsen'
;    
University of California, San Diego
Department of Chemistry & Biochemistry
9500 Gilman Dr. MC 0358
La Jolla CA, 92093-0358
United States of America
;

'Peter Gantzel'
;    
University of California, San Diego
Department of Chemistry & Biochemistry
9500 Gilman Dr. MC 0358
La Jolla CA, 92093-0358
United States of America
; 


_publ_contact_author_name     	'Prof Karsten Meyer'  
_publ_contact_author_address 
;
Department of Chemistry & Biochemistry
University of California, San Diego
9500 Gilman Drive, MC0358
La Jolla
California
92093
UNITED STATES OF AMERICA
;

_publ_contact_author_phone        '1 858 822 4247'
_publ_contact_author_fax          '1 858 534 5383'
_publ_contact_author_email        'kmeyer@ucsd.edu'
_publ_requested_journal           'Chemical Communications'
_publ_requested_coeditor_name     ?



_publ_section_title
;
Uranium complexes supported by an aryloxide-functionalized 
triazacyclononane macrocycle: Synthesis and characterization of a 
six-coordinate U(III) species and insights into its reactivity
;



_publ_section_experimental
;
The crystal was obtained from a diluted solution of 
[{((ArO)3tacn)U}2(m-O)] in Et2O/pentane. 
;

_publ_section_acknowledgements
;
This work was supported by the University of California, 
San Diego. ICR thanks the National Institute of Health for a fellowship 
(3 T32 DK07233-2651). We are grateful to the University of Copenhagen 
(Denmark) for granting leave of absence to KO. KO thanks the 
Danish Chemical Society for financial support. 
;

data_oxo
_database_code_CSD                  195391

_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
'C55 H88 N3 O4.50 U'
_chemical_formula_weight          1101.31

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            Triclinic
_symmetry_space_group_name_H-M    P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                    14.8550(17)
_cell_length_b                    15.0174(17)
_cell_length_c                    15.2609(17)
_cell_angle_alpha                 60.832(2)
_cell_angle_beta                  74.682(2)
_cell_angle_gamma                 66.580(2)
_cell_volume                      2717.3(5)
_cell_formula_units_Z             2
_cell_measurement_temperature     296(2)
_cell_measurement_reflns_used     9842
_cell_measurement_theta_min       2.24
_cell_measurement_theta_max       27.14

_exptl_crystal_description        rectangular
_exptl_crystal_colour             'pale blue'
_exptl_crystal_size_max           0.20
_exptl_crystal_size_mid           0.20
_exptl_crystal_size_min           0.13
_exptl_crystal_density_meas       0
_exptl_crystal_density_diffrn     1.346
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              1134
_exptl_absorpt_coefficient_mu     3.032
_exptl_absorpt_correction_type    
'SADABS (BrukerAXS SaintPlus Program Suite)'
_exptl_absorpt_correction_T_min   0.5823
_exptl_absorpt_correction_T_max   0.6940
_exptl_absorpt_process_details    ?

_exptl_special_details
;
?
;

_diffrn_ambient_temperature       296(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   'CCD area detector'
_diffrn_measurement_method        'phi and omega scans'
_diffrn_detector_area_resol_mean  ?
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             22661
_diffrn_reflns_av_R_equivalents   0.0489
_diffrn_reflns_av_sigmaI/netI     0.0891
_diffrn_reflns_limit_h_min        -19
_diffrn_reflns_limit_h_max        19
_diffrn_reflns_limit_k_min        -19
_diffrn_reflns_limit_k_max        19
_diffrn_reflns_limit_l_min        -19
_diffrn_reflns_limit_l_max        19
_diffrn_reflns_theta_min          1.50
_diffrn_reflns_theta_max          27.55
_reflns_number_total              11787
_reflns_number_gt                 8803
_reflns_threshold_expression      >2sigma(I)

_computing_data_collection        'Bruker SMART'
_computing_cell_refinement        'Bruker SMART'
_computing_data_reduction         'Bruker SAINT'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics     'Bruker SHELXTL'
_computing_publication_material   'Bruker SHELXTL'

_refine_special_details
;
Refinement of F^2^ against ALL reflections.  The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
;
calc w=1/[\s^2^(Fo^2^)+(0.0993P)^2^+0.0000P] where 
P=(Fo^2^+2Fc^2^)/3
;
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     mixed
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        ?
_refine_ls_number_reflns          11787
_refine_ls_number_parameters      592
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0938
_refine_ls_R_factor_gt            0.0646
_refine_ls_wR_factor_ref          0.1674
_refine_ls_wR_factor_gt           0.1525
_refine_ls_goodness_of_fit_ref    1.033
_refine_ls_restrained_S_all       1.033
_refine_ls_shift/su_max           0.078
_refine_ls_shift/su_mean          0.002

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 0.65532(2) 0.44849(2) 0.48688(2) 0.03106(11) Uani 1 1 d . . .
O4 O 0.5000 0.5000 0.5000 0.0313(15) Uani 1 2 d S . .
N1 N 0.8177(5) 0.4341(5) 0.3514(5) 0.0356(14) Uani 1 1 d . . .
N2 N 0.8183(5) 0.4735(5) 0.5163(5) 0.0345(14) Uani 1 1 d . . .
N3 N 0.8142(5) 0.2686(5) 0.5549(5) 0.0342(14) Uani 1 1 d . . .
C1 C 0.8941(6) 0.4729(7) 0.3514(6) 0.0409(19) Uani 1 1 d . . .
H1A H 0.9107 0.5204 0.2828 0.049 Uiso 1 1 calc R . .
H1B H 0.9528 0.4121 0.3756 0.049 Uiso 1 1 calc R . .
C2 C 0.8625(6) 0.5324(7) 0.4161(6) 0.0423(19) Uani 1 1 d . . .
H2A H 0.9193 0.5437 0.4239 0.051 Uiso 1 1 calc R . .
H2B H 0.8151 0.6024 0.3826 0.051 Uiso 1 1 calc R . .
C3 C 0.8939(6) 0.3744(6) 0.5753(6) 0.0407(19) Uani 1 1 d . . .
H3A H 0.9098 0.3839 0.6273 0.049 Uiso 1 1 calc R . .
H3B H 0.9534 0.3624 0.5314 0.049 Uiso 1 1 calc R . .
C4 C 0.8598(6) 0.2772(6) 0.6237(6) 0.0389(18) Uani 1 1 d . . .
H4A H 0.9158 0.2129 0.6491 0.047 Uiso 1 1 calc R . .
H4B H 0.8126 0.2802 0.6807 0.047 Uiso 1 1 calc R . .
C5 C 0.8913(6) 0.2443(6) 0.4768(6) 0.0380(18) Uani 1 1 d . . .
H5A H 0.9048 0.1705 0.4894 0.046 Uiso 1 1 calc R . .
H5B H 0.9516 0.2510 0.4822 0.046 Uiso 1 1 calc R . .
C6 C 0.8601(6) 0.3192(6) 0.3703(6) 0.0401(18) Uani 1 1 d . . .
H6A H 0.9169 0.3107 0.3224 0.048 Uiso 1 1 calc R . .
H6B H 0.8117 0.2984 0.3590 0.048 Uiso 1 1 calc R . .
O5 O 0.9423(11) -0.0507(12) 0.2369(12) 0.171(6) Uani 1 1 d . . .
C7 C 0.900(2) 0.055(2) 0.217(2) 0.188(13) Uani 1 1 d . . .
H7A H 0.8292 0.0736 0.2264 0.226 Uiso 1 1 calc R . .
H7B H 0.9190 0.0996 0.1481 0.226 Uiso 1 1 calc R . .
C8 C 0.9362(19) 0.073(2) 0.289(2) 0.209(16) Uani 1 1 d . . .
H8A H 0.9082 0.1478 0.2762 0.313 Uiso 1 1 calc R . .
H8B H 1.0067 0.0540 0.2797 0.313 Uiso 1 1 calc R . .
H8C H 0.9165 0.0297 0.3571 0.313 Uiso 1 1 calc R . .
C9 C 0.914(3) -0.071(3) 0.169(2) 0.26(2) Uani 1 1 d . . .
H9A H 0.9447 -0.0378 0.1024 0.317 Uiso 1 1 calc R . .
H9B H 0.8428 -0.0397 0.1667 0.317 Uiso 1 1 calc R . .
C10 C 0.945(3) -0.192(2) 0.206(2) 0.249(17) Uani 1 1 d . . .
H10A H 0.9255 -0.2071 0.1603 0.374 Uiso 1 1 calc R . .
H10B H 0.9142 -0.2239 0.2719 0.374 Uiso 1 1 calc R . .
H10C H 1.0153 -0.2219 0.2073 0.374 Uiso 1 1 calc R . .
O1A O 0.6498(4) 0.6108(4) 0.3623(4) 0.0372(12) Uani 1 1 d . . .
C1A C 0.6818(6) 0.6687(6) 0.2676(6) 0.0371(17) Uani 1 1 d . . .
C2A C 0.7462(6) 0.6136(6) 0.2115(6) 0.0378(17) Uani 1 1 d . . .
C3A C 0.7815(6) 0.6693(7) 0.1127(6) 0.0420(19) Uani 1 1 d . . .
H3AA H 0.8249 0.6310 0.0772 0.050 Uiso 1 1 calc R . .
C4A C 0.7528(6) 0.7806(7) 0.0667(6) 0.044(2) Uani 1 1 d . . .
C5A C 0.6890(6) 0.8335(7) 0.1233(6) 0.0423(19) Uani 1 1 d . . .
H5AA H 0.6696 0.9083 0.0929 0.051 Uiso 1 1 calc R . .
C6A C 0.6518(6) 0.7832(6) 0.2223(6) 0.0363(17) Uani 1 1 d . . .
C7A C 0.7729(6) 0.4947(6) 0.2536(6) 0.0389(18) Uani 1 1 d . . .
H7AA H 0.8189 0.4710 0.2050 0.047 Uiso 1 1 calc R . .
H7AB H 0.7141 0.4768 0.2628 0.047 Uiso 1 1 calc R . .
C8A C 0.7867(8) 0.8438(8) -0.0431(6) 0.058(3) Uani 1 1 d . . .
C9A C 0.8683(9) 0.7733(9) -0.0871(8) 0.077(3) Uani 1 1 d . . .
H9AA H 0.8896 0.8174 -0.1542 0.115 Uiso 1 1 calc R . .
H9AB H 0.8444 0.7235 -0.0891 0.115 Uiso 1 1 calc R . .
H9AC H 0.9226 0.7341 -0.0461 0.115 Uiso 1 1 calc R . .
C10A C 0.7002(10) 0.9037(13) -0.1054(9) 0.115(6) Uani 1 1 d . . .
H10D H 0.7204 0.9467 -0.1734 0.173 Uiso 1 1 calc R . .
H10E H 0.6493 0.9495 -0.0778 0.173 Uiso 1 1 calc R . .
H10F H 0.6754 0.8533 -0.1047 0.173 Uiso 1 1 calc R . .
C11A C 0.8261(12) 0.9263(11) -0.0509(9) 0.099(5) Uani 1 1 d . . .
H11A H 0.8407 0.9704 -0.1206 0.149 Uiso 1 1 calc R . .
H11B H 0.8850 0.8902 -0.0166 0.149 Uiso 1 1 calc R . .
H11C H 0.7775 0.9706 -0.0205 0.149 Uiso 1 1 calc R . .
C12A C 0.5833(6) 0.8499(7) 0.2781(6) 0.0422(19) Uani 1 1 d . . .
C13A C 0.6336(9) 0.8261(9) 0.3643(8) 0.075(3) Uani 1 1 d . . .
H13A H 0.6525 0.7503 0.4072 0.112 Uiso 1 1 calc R . .
H13B H 0.5893 0.8645 0.4022 0.112 Uiso 1 1 calc R . .
H13C H 0.6912 0.8485 0.3384 0.112 Uiso 1 1 calc R . .
C14A C 0.4868(8) 0.8260(9) 0.3147(9) 0.071(3) Uani 1 1 d . . .
H14A H 0.4987 0.7515 0.3612 0.106 Uiso 1 1 calc R . .
H14B H 0.4567 0.8413 0.2583 0.106 Uiso 1 1 calc R . .
H14C H 0.4436 0.8701 0.3477 0.106 Uiso 1 1 calc R . .
C15A C 0.5590(9) 0.9703(8) 0.2109(8) 0.068(3) Uani 1 1 d . . .
H15A H 0.5144 1.0092 0.2482 0.102 Uiso 1 1 calc R . .
H15B H 0.5288 0.9884 0.1535 0.102 Uiso 1 1 calc R . .
H15C H 0.6184 0.9892 0.1887 0.102 Uiso 1 1 calc R . .
O1B O 0.6475(4) 0.4234(4) 0.6444(4) 0.0363(12) Uani 1 1 d . . .
C1B C 0.6802(6) 0.4333(6) 0.7117(6) 0.0360(17) Uani 1 1 d . . .
C2B C 0.7469(6) 0.4907(6) 0.6776(6) 0.0389(18) Uani 1 1 d . . .
C3B C 0.7877(6) 0.4993(7) 0.7444(6) 0.0421(19) Uani 1 1 d . . .
H3BA H 0.8330 0.5365 0.7194 0.051 Uiso 1 1 calc R . .
C4B C 0.7624(7) 0.4541(7) 0.8468(6) 0.046(2) Uani 1 1 d . . .
C5B C 0.6948(7) 0.3993(7) 0.8792(7) 0.049(2) Uani 1 1 d . . .
H5BA H 0.6766 0.3689 0.9480 0.058 Uiso 1 1 calc R . .
C6B C 0.6517(6) 0.3862(7) 0.8172(6) 0.0400(18) Uani 1 1 d . . .
C7B C 0.7735(6) 0.5461(6) 0.5675(6) 0.0410(19) Uani 1 1 d . . .
H7BA H 0.8196 0.5820 0.5576 0.049 Uiso 1 1 calc R . .
H7BB H 0.7147 0.6010 0.5356 0.049 Uiso 1 1 calc R . .
C8B C 0.8043(8) 0.4628(9) 0.9229(7) 0.062(3) Uani 1 1 d . . .
C9B C 0.8924(10) 0.5021(12) 0.8775(9) 0.091(4) Uani 1 1 d . . .
H9BA H 0.9200 0.4998 0.9292 0.137 Uiso 1 1 calc R . .
H9BB H 0.8723 0.5748 0.8265 0.137 Uiso 1 1 calc R . .
H9BC H 0.9410 0.4569 0.8481 0.137 Uiso 1 1 calc R . .
C10B C 0.7210(11) 0.5381(15) 0.9636(13) 0.120(6) Uani 1 1 d . . .
H10G H 0.7445 0.5423 1.0139 0.180 Uiso 1 1 calc R . .
H10H H 0.6666 0.5104 0.9930 0.180 Uiso 1 1 calc R . .
H10I H 0.6999 0.6085 0.9094 0.180 Uiso 1 1 calc R . .
C11B C 0.8398(11) 0.3526(12) 1.0107(9) 0.100(5) Uani 1 1 d . . .
H11D H 0.8680 0.3589 1.0565 0.151 Uiso 1 1 calc R . .
H11E H 0.8886 0.3034 0.9856 0.151 Uiso 1 1 calc R . .
H11F H 0.7851 0.3262 1.0454 0.151 Uiso 1 1 calc R . .
C12B C 0.5808(7) 0.3213(7) 0.8636(7) 0.048(2) Uani 1 1 d . . .
C13B C 0.6312(11) 0.2140(10) 0.8560(11) 0.093(4) Uani 1 1 d . . .
H13D H 0.6378 0.2266 0.7870 0.140 Uiso 1 1 calc R . .
H13E H 0.5922 0.1672 0.8959 0.140 Uiso 1 1 calc R . .
H13F H 0.6953 0.1811 0.8804 0.140 Uiso 1 1 calc R . .
C14B C 0.4868(8) 0.3805(10) 0.8110(9) 0.080(4) Uani 1 1 d . . .
H14D H 0.5026 0.3977 0.7406 0.120 Uiso 1 1 calc R . .
H14E H 0.4528 0.4456 0.8193 0.120 Uiso 1 1 calc R . .
H14F H 0.4455 0.3356 0.8399 0.120 Uiso 1 1 calc R . .
C15B C 0.5503(10) 0.2951(12) 0.9745(8) 0.087(4) Uani 1 1 d . . .
H15D H 0.5041 0.2562 0.9992 0.131 Uiso 1 1 calc R . .
H15E H 0.5203 0.3606 0.9824 0.131 Uiso 1 1 calc R . .
H15F H 0.6074 0.2518 1.0118 0.131 Uiso 1 1 calc R . .
O1C O 0.6514(4) 0.3223(4) 0.4527(4) 0.0342(11) Uani 1 1 d . . .
C1C C 0.6801(5) 0.2158(6) 0.4759(6) 0.0341(16) Uani 1 1 d . . .
C2C C 0.7408(6) 0.1444(6) 0.5545(6) 0.0365(17) Uani 1 1 d . . .
C3C C 0.7725(6) 0.0345(6) 0.5840(6) 0.0394(18) Uani 1 1 d . . .
H3CA H 0.8135 -0.0113 0.6360 0.047 Uiso 1 1 calc R . .
C4C C 0.7444(6) -0.0080(6) 0.5379(6) 0.0425(19) Uani 1 1 d . . .
C5C C 0.6848(6) 0.0639(7) 0.4592(6) 0.0407(18) Uani 1 1 d . . .
H5CA H 0.6653 0.0358 0.4276 0.049 Uiso 1 1 calc R . .
C6C C 0.6523(6) 0.1758(6) 0.4241(6) 0.0378(17) Uani 1 1 d . . .
C7C C 0.7669(6) 0.1839(6) 0.6140(6) 0.0391(18) Uani 1 1 d . . .

H7CA H 0.7073 0.2115 0.6507 0.047 Uiso 1 1 calc R . .
H7CB H 0.8108 0.1232 0.6633 0.047 Uiso 1 1 calc R . .
C8C C 0.7736(7) -0.1304(7) 0.5717(8) 0.054(2) Uani 1 1 d . . .
C9C C 0.8486(8) -0.1937(8) 0.6459(9) 0.069(3) Uani 1 1 d . . .
H9CA H 0.8738 -0.2670 0.6550 0.104 Uiso 1 1 calc R . .
H9CB H 0.8190 -0.1914 0.7091 0.104 Uiso 1 1 calc R . .
H9CC H 0.9015 -0.1638 0.6215 0.104 Uiso 1 1 calc R . .
C10C C 0.6854(9) -0.1649(9) 0.6106(12) 0.094(5) Uani 1 1 d . . .
H10J H 0.7000 -0.2330 0.6102 0.141 Uiso 1 1 calc R . .
H10K H 0.6329 -0.1123 0.5687 0.141 Uiso 1 1 calc R . .
H10L H 0.6657 -0.1719 0.6782 0.141 Uiso 1 1 calc R . .
C11C C 0.8234(9) -0.1567(9) 0.4809(9) 0.074(3) Uani 1 1 d . . .
H11G H 0.8448 -0.2331 0.5030 0.111 Uiso 1 1 calc R . .
H11H H 0.8791 -0.1311 0.4519 0.111 Uiso 1 1 calc R . .
H11I H 0.7771 -0.1221 0.4314 0.111 Uiso 1 1 calc R . .
C12C C 0.5896(6) 0.2472(7) 0.3349(6) 0.0431(19) Uani 1 1 d . . .
C13C C 0.6461(8) 0.3191(8) 0.2482(7) 0.061(3) Uani 1 1 d . . .
H13G H 0.6578 0.3639 0.2694 0.092 Uiso 1 1 calc R . .
H13H H 0.6078 0.3635 0.1911 0.092 Uiso 1 1 calc R . .
H13I H 0.7079 0.2748 0.2301 0.092 Uiso 1 1 calc R . .
C14C C 0.4917(7) 0.3174(8) 0.3640(8) 0.059(3) Uani 1 1 d . . .
H14G H 0.5036 0.3586 0.3894 0.088 Uiso 1 1 calc R . .
H14H H 0.4545 0.2726 0.4150 0.088 Uiso 1 1 calc R . .
H14I H 0.4552 0.3654 0.3058 0.088 Uiso 1 1 calc R . .
C15C C 0.5681(8) 0.1839(8) 0.2950(8) 0.057(2) Uani 1 1 d . . .
H15G H 0.5259 0.2325 0.2414 0.086 Uiso 1 1 calc R . .
H15H H 0.5360 0.1348 0.3483 0.086 Uiso 1 1 calc R . .
H15I H 0.6287 0.1443 0.2702 0.086 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23

_atom_site_aniso_U_13
_atom_site_aniso_U_12
U1 0.03530(17) 0.03093(16) 0.01881(14) -0.00411(11) -0.00425(10) 
-0.01019(11)
O4 0.032(4) 0.028(4) 0.027(4) -0.006(3) -0.007(3) -0.008(3)
N1 0.039(4) 0.033(3) 0.023(3) -0.004(3) -0.002(3) -0.011(3)
N2 0.038(4) 0.033(3) 0.026(3) -0.007(3) -0.005(3) -0.011(3)
N3 0.038(4) 0.032(3) 0.025(3) -0.007(3) -0.004(3) -0.010(3)
C1 0.037(4) 0.047(5) 0.030(4) -0.012(4) 0.002(3) -0.014(4)
C2 0.045(5) 0.051(5) 0.029(4) -0.010(4) -0.002(3) -0.024(4)
C3 0.047(5) 0.040(4) 0.028(4) -0.003(3) -0.016(3) -0.014(4)
C4 0.039(4) 0.041(4) 0.030(4) -0.011(4) -0.009(3) -0.009(3)
C5 0.035(4) 0.034(4) 0.036(4) -0.012(4) -0.002(3) -0.009(3)
C6 0.039(4) 0.039(4) 0.035(4) -0.014(4) -0.005(3) -0.008(3)
O5 0.175(14) 0.111(11) 0.139(13) -0.016(9) -0.033(10) 0.002(10)
C7 0.15(2) 0.11(2) 0.22(3) -0.03(2) 0.01(2) -0.029(16)
C8 0.16(2) 0.111(17) 0.28(4) -0.08(2) 0.10(3) -0.053(17)
C9 0.39(5) 0.20(3) 0.22(3) -0.07(3) -0.22(4) -0.01(3)
C10 0.38(5) 0.17(3) 0.18(3) -0.03(2) -0.19(3) -0.03(3)
O1A 0.043(3) 0.032(3) 0.022(3) -0.002(2) 0.001(2) -0.012(2)
C1A 0.040(4) 0.041(4) 0.022(4) -0.005(3) 0.000(3) -0.016(3)
C2A 0.046(5) 0.037(4) 0.026(4) -0.006(3) -0.005(3) -0.018(4)
C3A 0.052(5) 0.043(5) 0.026(4) -0.011(4) -0.006(4) -0.014(4)
C4A 0.051(5) 0.046(5) 0.028(4) -0.010(4) -0.005(4) -0.016(4)
C5A 0.054(5) 0.036(4) 0.027(4) -0.003(3) -0.006(4) -0.018(4)
C6A 0.039(4) 0.039(4) 0.026(4) -0.007(3) -0.005(3) -0.016(3)
C7A 0.050(5) 0.040(4) 0.027(4) -0.012(3) -0.002(3) -0.018(4)
C8A 0.078(7) 0.050(5) 0.023(4) 0.001(4) -0.003(4) -0.022(5)
C9A 0.093(9) 0.069(7) 0.035(5) -0.006(5) 0.012(5) -0.027(6)
C10A 0.096(10) 0.149(14) 0.032(6) 0.003(7) -0.020(6) -0.018(9)
C11A 0.154(13) 0.093(10) 0.051(7) -0.019(7) 0.030(8) -0.079(10)
C12A 0.044(5) 0.041(5) 0.037(5) -0.012(4) -0.006(4) -0.013(4)
C13A 0.097(9) 0.073(7) 0.048(6) -0.032(6) -0.022(6) -0.004(6)
C14A 0.058(6) 0.067(7) 0.078(8) -0.032(6) 0.020(6) -0.026(5)
C15A 0.091(8) 0.042(5) 0.058(7) -0.016(5) -0.004(6) -0.019(5)
O1B 0.041(3) 0.045(3) 0.019(2) -0.008(2) -0.003(2) -0.018(2)
C1B 0.042(4) 0.034(4) 0.026(4) -0.008(3) -0.011(3) -0.007(3)
C2B 0.048(5) 0.035(4) 0.027(4) -0.008(3) -0.013(3) -0.009(4)
C3B 0.052(5) 0.040(5) 0.033(4) -0.011(4) -0.008(4) -0.017(4)
C4B 0.053(5) 0.054(5) 0.032(4) -0.018(4) -0.008(4) -0.018(4)
C5B 0.054(5) 0.055(5) 0.032(5) -0.015(4) -0.003(4) -0.019(4)
C6B 0.048(5) 0.040(4) 0.025(4) -0.011(3) -0.006(3) -0.010(4)
C7B 0.052(5) 0.036(4) 0.025(4) -0.003(3) -0.009(3) -0.014(4)

C8B 0.080(7) 0.088(8) 0.030(5) -0.018(5) -0.008(5) -0.045(6)
C9B 0.114(10) 0.144(13) 0.049(7) -0.032(8) -0.011(7) -0.085(10)
C10B 0.126(13) 0.172(17) 0.117(13) -0.108(13) -0.014(10) -0.038(12)
C11B 0.133(12) 0.130(12) 0.043(7) -0.002(7) -0.035(7) -0.076(10)
C12B 0.051(5) 0.054(5) 0.034(5) -0.012(4) 0.000(4) -0.024(4)
C13B 0.119(11) 0.063(8) 0.094(10) -0.032(7) 0.022(8) -0.047(8)
C14B 0.063(7) 0.090(9) 0.070(8) -0.005(7) -0.020(6) -0.036(6)
C15B 0.099(9) 0.137(12) 0.046(6) -0.032(7) 0.013(6) -0.077(9)
O1C 0.039(3) 0.026(3) 0.027(3) -0.004(2) -0.007(2) -0.008(2)
C1C 0.031(4) 0.036(4) 0.026(4) -0.008(3) 0.000(3) -0.010(3)
C2C 0.042(4) 0.037(4) 0.028(4) -0.011(3) 0.000(3) -0.016(3)
C3C 0.040(4) 0.037(4) 0.031(4) -0.007(4) -0.004(3) -0.013(3)
C4C 0.052(5) 0.030(4) 0.037(5) -0.007(4) -0.006(4) -0.013(4)
C5C 0.046(5) 0.040(5) 0.039(5) -0.016(4) -0.003(4) -0.018(4)
C6C 0.039(4) 0.037(4) 0.033(4) -0.012(4) -0.001(3) -0.014(3)
C7C 0.048(5) 0.033(4) 0.030(4) -0.006(3) -0.010(3) -0.013(3)

C8C 0.060(6) 0.041(5) 0.051(6) -0.011(4) -0.013(5) -0.015(4)
C9C 0.079(8) 0.039(5) 0.076(8) -0.018(5) -0.022(6) -0.003(5)
C10C 0.083(9) 0.041(6) 0.130(13) -0.015(7) -0.006(8) -0.024(6)
C11C 0.091(9) 0.056(7) 0.076(8) -0.034(6) -0.018(7) -0.010(6)
C12C 0.053(5) 0.042(5) 0.032(4) -0.008(4) -0.011(4) -0.019(4)
C13C 0.083(7) 0.063(6) 0.029(5) -0.005(4) -0.007(5) -0.034(6)
C14C 0.051(6) 0.055(6) 0.057(6) -0.018(5) -0.016(5) -0.005(4)
C15C 0.064(6) 0.058(6) 0.052(6) -0.019(5) -0.019(5) -0.019(5)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 O4 2.1095(4) . ?
U1 O1B 2.222(5) . ?
U1 O1C 2.222(5) . ?
U1 O1A 2.230(5) . ?
U1 N3 2.727(6) . ?
U1 N1 2.744(6) . ?
U1 N2 2.768(6) . ?
O4 U1 2.1095(4) 2_666 ?
N1 C1 1.466(10) . ?
N1 C6 1.485(10) . ?
N1 C7A 1.489(10) . ?
N2 C2 1.471(10) . ?
N2 C3 1.479(9) . ?
N2 C7B 1.490(10) . ?
N3 C4 1.468(10) . ?
N3 C7C 1.477(10) . ?
N3 C5 1.496(10) . ?
C1 C2 1.509(11) . ?
C3 C4 1.508(11) . ?
C5 C6 1.524(11) . ?
O5 C7 1.36(3) . ?
O5 C9 1.40(3) . ?
C7 C8 1.51(4) . ?
C9 C10 1.53(3) . ?
O1A C1A 1.346(9) . ?
C1A C2A 1.401(11) . ?
C1A C6A 1.424(11) . ?
C2A C3A 1.396(11) . ?
C2A C7A 1.487(11) . ?
C3A C4A 1.384(12) . ?
C4A C5A 1.384(12) . ?
C4A C8A 1.531(12) . ?
C5A C6A 1.392(11) . ?
C6A C12A 1.525(11) . ?
C8A C10A 1.502(15) . ?
C8A C9A 1.511(14) . ?
C8A C11A 1.512(15) . ?
C12A C13A 1.506(13) . ?
C12A C14A 1.512(13) . ?
C12A C15A 1.524(13) . ?
O1B C1B 1.336(9) . ?
C1B C2B 1.401(11) . ?
C1B C6B 1.427(11) . ?
C2B C3B 1.395(11) . ?
C2B C7B 1.489(11) . ?
C3B C4B 1.379(12) . ?
C4B C5B 1.388(12) . ?
C4B C8B 1.532(12) . ?
C5B C6B 1.395(12) . ?
C6B C12B 1.519(12) . ?
C8B C9B 1.510(15) . ?
C8B C11B 1.527(16) . ?
C8B C10B 1.537(17) . ?
C12B C14B 1.514(13) . ?
C12B C15B 1.520(13) . ?
C12B C13B 1.532(15) . ?
O1C C1C 1.360(9) . ?
C1C C2C 1.396(11) . ?
C1C C6C 1.409(11) . ?
C2C C3C 1.386(11) . ?
C2C C7C 1.490(11) . ?
C3C C4C 1.372(11) . ?
C4C C5C 1.389(12) . ?
C4C C8C 1.546(12) . ?
C5C C6C 1.400(11) . ?
C6C C12C 1.525(11) . ?
C8C C10C 1.471(14) . ?
C8C C9C 1.484(14) . ?
C8C C11C 1.544(15) . ?
C12C C15C 1.511(12) . ?
C12C C14C 1.523(13) . ?
C12C C13C 1.536(12) . ?

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
O4 U1 O1B 87.96(13) . . ?
O4 U1 O1C 87.32(13) . . ?
O1B U1 O1C 121.53(19) . . ?
O4 U1 O1A 88.67(13) . . ?
O1B U1 O1A 118.57(19) . . ?
O1C U1 O1A 119.53(19) . . ?
O4 U1 N3 141.52(13) . . ?
O1B U1 N3 79.35(19) . . ?
O1C U1 N3 69.59(18) . . ?
O1A U1 N3 129.28(19) . . ?
O4 U1 N1 142.98(13) . . ?
O1B U1 N1 128.54(19) . . ?
O1C U1 N1 78.66(19) . . ?
O1A U1 N1 69.65(18) . . ?
N3 U1 N1 63.62(18) . . ?
O4 U1 N2 144.34(13) . . ?
O1B U1 N2 69.49(18) . . ?
O1C U1 N2 127.82(18) . . ?
O1A U1 N2 79.19(19) . . ?
N3 U1 N2 62.74(18) . . ?
N1 U1 N2 62.37(19) . . ?
U1 O4 U1 180.000(1) 2_666 . ?
C1 N1 C6 110.3(6) . . ?
C1 N1 C7A 112.6(6) . . ?
C6 N1 C7A 107.1(6) . . ?
C1 N1 U1 117.6(5) . . ?
C6 N1 U1 106.2(4) . . ?
C7A N1 U1 102.2(4) . . ?
C2 N2 C3 110.1(6) . . ?
C2 N2 C7B 108.3(6) . . ?
C3 N2 C7B 111.2(6) . . ?
C2 N2 U1 107.1(4) . . ?
C3 N2 U1 116.9(4) . . ?
C7B N2 U1 102.7(4) . . ?
C4 N3 C7C 108.8(6) . . ?
C4 N3 C5 109.1(6) . . ?
C7C N3 C5 111.8(6) . . ?
C4 N3 U1 108.3(4) . . ?
C7C N3 U1 101.7(4) . . ?
C5 N3 U1 116.8(4) . . ?
N1 C1 C2 112.9(6) . . ?
N2 C2 C1 112.2(7) . . ?
N2 C3 C4 112.1(6) . . ?
N3 C4 C3 113.6(6) . . ?
N3 C5 C6 112.3(6) . . ?
N1 C6 C5 113.0(7) . . ?
C7 O5 C9 110(2) . . ?
O5 C7 C8 108(3) . . ?
O5 C9 C10 108(2) . . ?
C1A O1A U1 147.5(5) . . ?
O1A C1A C2A 118.3(7) . . ?
O1A C1A C6A 122.6(7) . . ?
C2A C1A C6A 119.1(7) . . ?
C3A C2A C1A 120.9(7) . . ?
C3A C2A C7A 118.5(7) . . ?
C1A C2A C7A 120.4(7) . . ?
C4A C3A C2A 121.1(8) . . ?
C5A C4A C3A 117.0(8) . . ?
C5A C4A C8A 120.8(8) . . ?
C3A C4A C8A 122.1(8) . . ?
C4A C5A C6A 124.9(8) . . ?
C5A C6A C1A 116.9(7) . . ?
C5A C6A C12A 120.3(7) . . ?
C1A C6A C12A 122.8(7) . . ?
C2A C7A N1 114.5(6) . . ?
C10A C8A C9A 110.1(10) . . ?
C10A C8A C11A 107.4(11) . . ?
C9A C8A C11A 106.7(10) . . ?
C10A C8A C4A 109.4(9) . . ?
C9A C8A C4A 113.0(8) . . ?
C11A C8A C4A 110.1(8) . . ?
C13A C12A C14A 111.3(9) . . ?
C13A C12A C15A 106.9(8) . . ?
C14A C12A C15A 107.1(8) . . ?
C13A C12A C6A 109.1(7) . . ?
C14A C12A C6A 110.3(7) . . ?
C15A C12A C6A 112.1(7) . . ?
C1B O1B U1 148.8(5) . . ?
O1B C1B C2B 118.6(7) . . ?
O1B C1B C6B 122.8(7) . . ?
C2B C1B C6B 118.6(7) . . ?
C3B C2B C1B 121.4(7) . . ?
C3B C2B C7B 118.7(8) . . ?
C1B C2B C7B 119.8(7) . . ?
C4B C3B C2B 121.5(8) . . ?
C3B C4B C5B 116.3(8) . . ?
C3B C4B C8B 123.3(8) . . ?
C5B C4B C8B 120.4(8) . . ?
C4B C5B C6B 125.5(8) . . ?
C5B C6B C1B 116.7(8) . . ?
C5B C6B C12B 119.7(7) . . ?
C1B C6B C12B 123.6(7) . . ?
C2B C7B N2 114.4(6) . . ?
C9B C8B C11B 106.2(10) . . ?
C9B C8B C4B 112.4(8) . . ?
C11B C8B C4B 110.5(9) . . ?
C9B C8B C10B 111.4(11) . . ?
C11B C8B C10B 108.7(11) . . ?
C4B C8B C10B 107.7(9) . . ?

C14B C12B C6B 111.8(8) . . ?
C14B C12B C15B 106.6(9) . . ?
C6B C12B C15B 113.1(8) . . ?
C14B C12B C13B 109.2(10) . . ?
C6B C12B C13B 108.9(8) . . ?
C15B C12B C13B 107.1(9) . . ?
C1C O1C U1 147.6(5) . . ?
O1C C1C C2C 117.2(7) . . ?
O1C C1C C6C 123.2(7) . . ?
C2C C1C C6C 119.6(7) . . ?
C3C C2C C1C 121.1(7) . . ?
C3C C2C C7C 118.1(7) . . ?
C1C C2C C7C 120.7(7) . . ?
C4C C3C C2C 121.2(8) . . ?
C3C C4C C5C 117.2(7) . . ?
C3C C4C C8C 123.0(8) . . ?
C5C C4C C8C 119.8(8) . . ?
C4C C5C C6C 124.5(8) . . ?
C5C C6C C1C 116.5(7) . . ?
C5C C6C C12C 119.9(7) . . ?
C1C C6C C12C 123.7(7) . . ?
N3 C7C C2C 115.5(6) . . ?
C10C C8C C9C 111.7(10) . . ?
C10C C8C C11C 108.0(10) . . ?
C9C C8C C11C 104.8(9) . . ?
C10C C8C C4C 110.2(8) . . ?
C9C C8C C4C 112.2(8) . . ?
C11C C8C C4C 109.7(8) . . ?
C15C C12C C14C 108.1(8) . . ?
C15C C12C C6C 113.0(7) . . ?
C14C C12C C6C 110.6(7) . . ?
C15C C12C C13C 106.9(8) . . ?
C14C C12C C13C 109.5(8) . . ?
C6C C12C C13C 108.7(7) . . ?

_diffrn_measured_fraction_theta_max    0.940
_diffrn_reflns_theta_full              27.55
_diffrn_measured_fraction_theta_full   0.940
_refine_diff_density_max    5.185
_refine_diff_density_min   -3.406
_refine_diff_density_rms    0.223
#===========================================================================

#_eof 

data_aryloxide
_database_code_CSD                  195392

_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
'C65 H99 N3 O4 U'
_chemical_formula_weight          1224.50

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'
'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    C2/c

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

_cell_length_a                    35.737(3)
_cell_length_b                    15.0416(12)
_cell_length_c                    26.266(2)
_cell_angle_alpha                 90.00
_cell_angle_beta                  90.188(2)
_cell_angle_gamma                 90.00
_cell_volume                      14119(2)
_cell_formula_units_Z             8
_cell_measurement_temperature     228(2)
_cell_measurement_reflns_used     ?
_cell_measurement_theta_min       ?
_cell_measurement_theta_max       ?

_exptl_crystal_description        recatangular
_exptl_crystal_colour             colorless
_exptl_crystal_size_max           0.25
_exptl_crystal_size_mid           0.25
_exptl_crystal_size_min           0.10
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.152
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              5072
_exptl_absorpt_coefficient_mu     2.340
_exptl_absorpt_correction_type    
'SADABS (BrukerAXS SaintPlus Program Suite)'
_exptl_absorpt_correction_T_min   0.5923
_exptl_absorpt_correction_T_max   0.7997
_exptl_absorpt_process_details    ?

_exptl_special_details
;
?
;

_diffrn_ambient_temperature       228(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   'CCD area detector'
_diffrn_measurement_method        'phi and omega scans'
_diffrn_detector_area_resol_mean  ?
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             58665
_diffrn_reflns_av_R_equivalents   0.0730
_diffrn_reflns_av_sigmaI/netI     0.0869
_diffrn_reflns_limit_h_min        -46
_diffrn_reflns_limit_h_max        46
_diffrn_reflns_limit_k_min        -19
_diffrn_reflns_limit_k_max        19
_diffrn_reflns_limit_l_min        -33
_diffrn_reflns_limit_l_max        32
_diffrn_reflns_theta_min          1.14
_diffrn_reflns_theta_max          27.57
_reflns_number_total              15962
_reflns_number_gt                 10202
_reflns_threshold_expression      >2sigma(I)

_computing_data_collection        'Bruker SMART'
_computing_cell_refinement        'Bruker SMART'
_computing_data_reduction         'Bruker SHELXTL'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics     'Bruker SHELXTL'
_computing_publication_material   'Bruker SHELXTL'

_refine_special_details
;
Refinement of F^2^ against ALL reflections.  The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
;
calc w=1/[\s^2^(Fo^2^)+(0.0721P)^2^+0.0000P] where 
P=(Fo^2^+2Fc^2^)/3
;
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     mixed
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        ?
_refine_ls_number_reflns          15962
_refine_ls_number_parameters      658
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0672
_refine_ls_R_factor_gt            0.0422
_refine_ls_wR_factor_ref          0.1380
_refine_ls_wR_factor_gt           0.1334
_refine_ls_goodness_of_fit_ref    1.017
_refine_ls_restrained_S_all       1.017
_refine_ls_shift/su_max           0.514
_refine_ls_shift/su_mean          0.048

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 0.191570(6) 0.325121(13) 0.317885(7) 0.03071(8) Uani 1 1 d . . .
O4 O 0.18642(11) 0.2017(2) 0.35970(13) 0.0378(9) Uani 1 1 d . . .
C1D C 0.16165(17) 0.1548(4) 0.3881(2) 0.0373(13) Uani 1 1 d . . .
C2D C 0.12345(17) 0.1631(4) 0.3773(2) 0.0444(15) Uani 1 1 d . . .
H2DA H 0.1157 0.1972 0.3492 0.053 Uiso 1 1 calc R . .
C3D C 0.09692(18) 0.1220(4) 0.4072(2) 0.0501(16) Uani 1 1 d . . .
H3DA H 0.0715 0.1275 0.3986 0.060 Uiso 1 1 calc R . .
C4D C 0.10712(18) 0.0727(4) 0.4498(2) 0.0484(16) Uani 1 1 d . . .
C5D C 0.14452(17) 0.0622(4) 0.4589(2) 0.0420(14) Uani 1 1 d . . .
H5DA H 0.1517 0.0270 0.4868 0.050 Uiso 1 1 calc R . .
C6D C 0.17295(16) 0.1007(4) 0.4291(2) 0.0365(13) Uani 1 1 d . . .
C8D C 0.21448(16) 0.0837(4) 0.4412(2) 0.0374(13) Uani 1 1 d . . .
C9D C 0.23344(18) 0.1696(4) 0.4560(2) 0.0463(15) Uani 1 1 d . . .
H9DA H 0.2307 0.2124 0.4285 0.069 Uiso 1 1 calc R . .
H9DB H 0.2598 0.1587 0.4623 0.069 Uiso 1 1 calc R . .
H9DC H 0.2220 0.1931 0.4866 0.069 Uiso 1 1 calc R . .
C10 C 0.23281(17) 0.0418(4) 0.3941(2) 0.0464(15) Uani 1 1 d . . .
H10A H 0.2299 0.0813 0.3652 0.070 Uiso 1 1 calc R . .
H10B H 0.2209 -0.0147 0.3867 0.070 Uiso 1 1 calc R . .
H10C H 0.2592 0.0324 0.4007 0.070 Uiso 1 1 calc R . .
C11 C 0.21967(19) 0.0191(5) 0.4853(2) 0.0584(18) Uani 1 1 d . . .
H11A H 0.2083 0.0436 0.5157 0.088 Uiso 1 1 calc R . .
H11B H 0.2462 0.0096 0.4912 0.088 Uiso 1 1 calc R . .
H11C H 0.2078 -0.0371 0.4769 0.088 Uiso 1 1 calc R . .
C12 C 0.07756(19) 0.0333(5) 0.4856(3) 0.0606(19) Uani 1 1 d . . .
C13 C 0.0611(4) 0.1061(8) 0.5158(5) 0.193(8) Uani 1 1 d . . .
H13A H 0.0425 0.0822 0.5387 0.289 Uiso 1 1 calc R . .
H13B H 0.0495 0.1489 0.4931 0.289 Uiso 1 1 calc R . .
H13C H 0.0807 0.1352 0.5354 0.289 Uiso 1 1 calc R . .
C14 C 0.0494(3) -0.0190(10) 0.4558(4) 0.187(8) Uani 1 1 d . . .
H14A H 0.0308 -0.0432 0.4788 0.280 Uiso 1 1 calc R . .
H14B H 0.0618 -0.0671 0.4381 0.280 Uiso 1 1 calc R . .
H14C H 0.0372 0.0196 0.4312 0.280 Uiso 1 1 calc R . .
C15 C 0.0944(3) -0.0266(11) 0.5248(6) 0.225(10) Uani 1 1 d . . .
H15A H 0.0748 -0.0495 0.5467 0.338 Uiso 1 1 calc R . .
H15B H 0.1123 0.0064 0.5451 0.338 Uiso 1 1 calc R . .
H15C H 0.1069 -0.0757 0.5081 0.338 Uiso 1 1 calc R . .
N1 N 0.21473(12) 0.3949(3) 0.22904(16) 0.0360(11) Uani 1 1 d . . .
N2 N 0.21419(13) 0.4976(3) 0.32182(17) 0.0359(11) Uani 1 1 d . . .
N3 N 0.14500(13) 0.4447(3) 0.27469(16) 0.0359(11) Uani 1 1 d . . .
C1 C 0.23617(17) 0.4783(4) 0.2324(2) 0.0444(14) Uani 1 1 d . . .
H1A H 0.2216 0.5263 0.2167 0.053 Uiso 1 1 calc R . .
H1B H 0.2594 0.4719 0.2131 0.053 Uiso 1 1 calc R . .
C2 C 0.24557(17) 0.5038(4) 0.2872(2) 0.0440(15) Uani 1 1 d . . .
H2A H 0.2657 0.4649 0.2996 0.053 Uiso 1 1 calc R . .
H2B H 0.2550 0.5649 0.2876 0.053 Uiso 1 1 calc R . .
C3 C 0.18519(16) 0.5641(4) 0.3090(2) 0.0439(15) Uani 1 1 d . . .
H3A H 0.1911 0.5906 0.2758 0.053 Uiso 1 1 calc R . .
H3B H 0.1858 0.6117 0.3344 0.053 Uiso 1 1 calc R . .
C4 C 0.14613(17) 0.5252(4) 0.3068(2) 0.0445(14) Uani 1 1 d . . .
H4A H 0.1380 0.5102 0.3414 0.053 Uiso 1 1 calc R . .
H4B H 0.1288 0.5696 0.2931 0.053 Uiso 1 1 calc R . .
C5 C 0.15228(17) 0.4672(4) 0.2206(2) 0.0431(14) Uani 1 1 d . . .
H5A H 0.1606 0.5291 0.2186 0.052 Uiso 1 1 calc R . .
H5B H 0.1288 0.4622 0.2014 0.052 Uiso 1 1 calc R . .
C6 C 0.18099(16) 0.4091(4) 0.1963(2) 0.0430(15) Uani 1 1 d . . .
H6A H 0.1697 0.3513 0.1885 0.052 Uiso 1 1 calc R . .
H6B H 0.1888 0.4360 0.1641 0.052 Uiso 1 1 calc R . .
O1A O 0.25147(11) 0.2940(3) 0.30902(13) 0.0382(9) Uani 1 1 d . . .
C1A C 0.28208(16) 0.2955(4) 0.2785(2) 0.0360(13) Uani 1 1 d . . .
C2A C 0.27615(16) 0.3104(4) 0.2257(2) 0.0396(14) Uani 1 1 d . . .
C3A C 0.30564(16) 0.3166(4) 0.1928(2) 0.0420(15) Uani 1 1 d . . .
H3AA H 0.3008 0.3265 0.1581 0.050 Uiso 1 1 calc R . .
C4A C 0.34239(18) 0.3085(4) 0.2091(2) 0.0419(15) Uani 1 1 d . . .
C5A C 0.34780(17) 0.2926(4) 0.2619(2) 0.0405(14) Uani 1 1 d . . .
H5AA H 0.3725 0.2865 0.2740 0.049 Uiso 1 1 calc R . .
C6A C 0.31915(16) 0.2854(4) 0.2964(2) 0.0362(13) Uani 1 1 d . . .
C7A C 0.23729(17) 0.3215(4) 0.2060(2) 0.0423(14) Uani 1 1 d . . .
H7AA H 0.2238 0.2655 0.2113 0.051 Uiso 1 1 calc R . .
H7AB H 0.2386 0.3316 0.1692 0.051 Uiso 1 1 calc R . .
C8A C 0.37534(18) 0.3188(4) 0.1721(2) 0.0463(15) Uani 1 1 d . . .
C9A C 0.3752(3) 0.2449(6) 0.1341(3) 0.104(3) Uani 1 1 d . . .
H9AA H 0.3791 0.1888 0.1515 0.156 Uiso 1 1 calc R . .
H9AB H 0.3951 0.2543 0.1097 0.156 Uiso 1 1 calc R . .
H9AC H 0.3513 0.2437 0.1165 0.156 Uiso 1 1 calc R . .
C10A C 0.3693(3) 0.4014(6) 0.1391(5) 0.168(7) Uani 1 1 d . . .
H10D H 0.3901 0.4078 0.1157 0.253 Uiso 1 1 calc R . .
H10E H 0.3679 0.4536 0.1607 0.253 Uiso 1 1 calc R . .
H10F H 0.3462 0.3952 0.1200 0.253 Uiso 1 1 calc R . .
C11A C 0.4118(2) 0.3132(10) 0.1979(4) 0.169(7) Uani 1 1 d . . .
H11D H 0.4129 0.2590 0.2179 0.253 Uiso 1 1 calc R . .
H11E H 0.4149 0.3642 0.2202 0.253 Uiso 1 1 calc R . .
H11F H 0.4316 0.3127 0.1728 0.253 Uiso 1 1 calc R . .
C12A C 0.32813(16) 0.2652(4) 0.3521(2) 0.0381(13) Uani 1 1 d . . .
C13A C 0.31020(19) 0.1750(4) 0.3652(2) 0.0481(15) Uani 1 1 d . . .
H13D H 0.3204 0.1293 0.3432 0.072 Uiso 1 1 calc R . .
H13E H 0.2833 0.1786 0.3603 0.072 Uiso 1 1 calc R . .
H13F H 0.3156 0.1602 0.4004 0.072 Uiso 1 1 calc R . .
C14A C 0.31179(19) 0.3356(4) 0.3878(2) 0.0474(15) Uani 1 1 d . . .
H14D H 0.3228 0.3930 0.3801 0.071 Uiso 1 1 calc R . .
H14E H 0.3174 0.3198 0.4228 0.071 Uiso 1 1 calc R . .
H14F H 0.2849 0.3385 0.3831 0.071 Uiso 1 1 calc R . .
C15A C 0.36930(17) 0.2615(5) 0.3632(2) 0.0522(17) Uani 1 1 d . . .
H15D H 0.3809 0.2169 0.3418 0.078 Uiso 1 1 calc R . .
H15E H 0.3732 0.2463 0.3987 0.078 Uiso 1 1 calc R . .
H15F H 0.3804 0.3191 0.3563 0.078 Uiso 1 1 calc R . .
O1B O 0.17212(11) 0.3862(2) 0.38896(13) 0.0388(9) Uani 1 1 d . . .
C1B C 0.17220(16) 0.4552(4) 0.4220(2) 0.0374(13) Uani 1 1 d . . .
C2B C 0.19869(16) 0.5226(4) 0.4150(2) 0.0395(13) Uani 1 1 d . . .
C3B C 0.19894(17) 0.5963(4) 0.4463(2) 0.0434(14) Uani 1 1 d . . .
H3BA H 0.2170 0.6408 0.4410 0.052 Uiso 1 1 calc R . .
C4B C 0.17373(17) 0.6064(4) 0.4849(2) 0.0434(14) Uani 1 1 d . . .
C5B C 0.14849(18) 0.5385(4) 0.4911(2) 0.0448(15) Uani 1 1 d . . .
H5BA H 0.1312 0.5438 0.5179 0.054 Uiso 1 1 calc R . .
C6B C 0.14639(16) 0.4627(4) 0.4613(2) 0.0393(13) Uani 1 1 d . . .
C7B C 0.22831(16) 0.5112(4) 0.3747(2) 0.0390(13) Uani 1 1 d . . .
H7BA H 0.2444 0.5639 0.3750 0.047 Uiso 1 1 calc R . .
H7BB H 0.2439 0.4601 0.3839 0.047 Uiso 1 1 calc R . .
C8B C 0.1750(2) 0.6878(4) 0.5209(3) 0.0557(18) Uani 1 1 d . . .
C9B C 0.2079(4) 0.6772(6) 0.5559(4) 0.136(5) Uani 1 1 d . . .
H9BA H 0.2307 0.6741 0.5360 0.204 Uiso 1 1 calc R . .
H9BB H 0.2052 0.6231 0.5756 0.204 Uiso 1 1 calc R . .
H9BC H 0.2093 0.7278 0.5788 0.204 Uiso 1 1 calc R . .
C10B C 0.1396(4) 0.6934(9) 0.5554(6) 0.213(9) Uani 1 1 d . . .
H10G H 0.1415 0.7451 0.5773 0.320 Uiso 1 1 calc R . .
H10H H 0.1378 0.6401 0.5760 0.320 Uiso 1 1 calc R . .
H10I H 0.1174 0.6986 0.5341 0.320 Uiso 1 1 calc R . .
C11B C 0.1808(3) 0.7732(5) 0.4928(4) 0.120(4) Uani 1 1 d . . .
H11G H 0.2029 0.7684 0.4716 0.180 Uiso 1 1 calc R . .
H11H H 0.1841 0.8213 0.5171 0.180 Uiso 1 1 calc R . .
H11I H 0.1591 0.7853 0.4716 0.180 Uiso 1 1 calc R . .
C12B C 0.11894(18) 0.3873(4) 0.4740(2) 0.0476(15) Uani 1 1 d . . .
C13B C 0.1417(2) 0.3015(4) 0.4859(2) 0.0513(17) Uani 1 1 d . . .
H13G H 0.1573 0.2868 0.4569 0.077 Uiso 1 1 calc R . .
H13H H 0.1246 0.2528 0.4925 0.077 Uiso 1 1 calc R . .
H13I H 0.1573 0.3114 0.5156 0.077 Uiso 1 1 calc R . .
C14B C 0.09183(19) 0.3718(5) 0.4288(2) 0.0555(17) Uani 1 1 d . . .
H14G H 0.1061 0.3577 0.3985 0.083 Uiso 1 1 calc R . .
H14H H 0.0772 0.4252 0.4229 0.083 Uiso 1 1 calc R . .
H14I H 0.0752 0.3228 0.4367 0.083 Uiso 1 1 calc R . .
C15B C 0.0934(2) 0.4097(5) 0.5210(3) 0.068(2) Uani 1 1 d . . .
H15G H 0.0791 0.4632 0.5139 0.102 Uiso 1 1 calc R . .
H15H H 0.1089 0.4190 0.5508 0.102 Uiso 1 1 calc R . .
H15I H 0.0764 0.3606 0.5271 0.102 Uiso 1 1 calc R . .
O1C O 0.15363(11) 0.2580(3) 0.26496(13) 0.0401(9) Uani 1 1 d . . .
C1C C 0.12152(16) 0.2586(4) 0.2378(2) 0.0392(13) Uani 1 1 d . . .
C2C C 0.09815(16) 0.3318(4) 0.2429(2) 0.0401(13) Uani 1 1 d . . .
C3C C 0.06675(18) 0.3396(5) 0.2125(2) 0.0527(17) Uani 1 1 d . . .
H3CA H 0.0515 0.3902 0.2158 0.063 Uiso 1 1 calc R . .
C4C C 0.0570(2) 0.2750(5) 0.1773(3) 0.064(2) Uani 1 1 d . . .
C5C C 0.0790(2) 0.2005(5) 0.1765(3) 0.065(2) Uani 1 1 d . . .
H5CA H 0.0715 0.1536 0.1551 0.078 Uiso 1 1 calc R . .
C6C C 0.11160(19) 0.1890(4) 0.2050(2) 0.0478(16) Uani 1 1 d . . .
C7C C 0.10743(16) 0.4036(4) 0.2808(2) 0.0418(14) Uani 1 1 d . . .
H7CA H 0.0885 0.4505 0.2780 0.050 Uiso 1 1 calc R . .
H7CB H 0.1057 0.3785 0.3151 0.050 Uiso 1 1 calc R . .
C8C C 0.0230(2) 0.2879(7) 0.1416(4) 0.093(3) Uani 1 1 d . . .
C9C C 0.0183(3) 0.2170(9) 0.1031(4) 0.142(5) Uani 1 1 d . . .
H9CA H 0.0152 0.1602 0.1201 0.213 Uiso 1 1 calc R . .
H9CB H 0.0403 0.2148 0.0816 0.213 Uiso 1 1 calc R . .
H9CC H -0.0036 0.2294 0.0824 0.213 Uiso 1 1 calc R . .
C10C C -0.0087(3) 0.3013(16) 0.1676(5) 0.313(16) Uani 1 1 d . . .
H10J H -0.0142 0.2493 0.1881 0.470 Uiso 1 1 calc R . .
H10K H -0.0291 0.3118 0.1440 0.470 Uiso 1 1 calc R . .
H10L H -0.0057 0.3526 0.1897 0.470 Uiso 1 1 calc R . .
C11C C 0.0278(4) 0.3777(10) 0.1095(5) 0.170(6) Uani 1 1 d . . .
H11J H 0.0065 0.3852 0.0870 0.254 Uiso 1 1 calc R . .
H11K H 0.0506 0.3743 0.0895 0.254 Uiso 1 1 calc R . .
H11L H 0.0294 0.4279 0.1326 0.254 Uiso 1 1 calc R . .
C12C C 0.13502(19) 0.1023(4) 0.1985(2) 0.0503(16) Uani 1 1 d . . .
C13C C 0.1110(2) 0.0244(5) 0.1783(4) 0.103(3) Uani 1 1 d . . .
H13J H 0.1266 -0.0280 0.1746 0.154 Uiso 1 1 calc R . .
H13K H 0.1004 0.0403 0.1455 0.154 Uiso 1 1 calc R . .
H13L H 0.0910 0.0121 0.2021 0.154 Uiso 1 1 calc R . .
C14C C 0.1656(2) 0.1179(5) 0.1611(3) 0.084(3) Uani 1 1 d . . .
H14J H 0.1813 0.1662 0.1729 0.126 Uiso 1 1 calc R . .
H14K H 0.1548 0.1332 0.1283 0.126 Uiso 1 1 calc R . .
H14L H 0.1805 0.0643 0.1577 0.126 Uiso 1 1 calc R . .
C15C C 0.1540(3) 0.0700(5) 0.2476(3) 0.119(4) Uani 1 1 d . . .
H15J H 0.1695 0.1171 0.2614 0.179 Uiso 1 1 calc R . .
H15K H 0.1694 0.0186 0.2401 0.179 Uiso 1 1 calc R . .
H15L H 0.1350 0.0539 0.2723 0.179 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
U1 0.03342(12) 0.03238(12) 0.02632(11) 0.00304(9) -0.00169(7) -0.00008(10)
O4 0.044(2) 0.037(2) 0.033(2) 0.0054(16) -0.0023(18) -0.0011(18)
C1D 0.050(4) 0.033(3) 0.029(3) 0.000(2) 0.000(3) -0.001(3)
C2D 0.044(4) 0.051(4) 0.037(3) 0.001(3) -0.002(3) 0.001(3)
C3D 0.045(4) 0.054(4) 0.052(4) -0.003(3) -0.004(3) -0.001(3)
C4D 0.047(4) 0.044(4) 0.055(4) 0.001(3) 0.008(3) -0.002(3)
C5D 0.048(4) 0.040(3) 0.038(3) 0.005(3) 0.002(3) -0.002(3)
C6D 0.045(3) 0.032(3) 0.032(3) -0.006(2) 0.000(3) 0.000(3)
C8D 0.038(3) 0.039(3) 0.035(3) 0.001(2) 0.000(2) -0.001(3)
C9D 0.047(4) 0.045(4) 0.047(3) -0.010(3) -0.003(3) -0.001(3)
C10 0.050(4) 0.038(4) 0.052(4) -0.007(3) 0.006(3) -0.001(3)
C11 0.055(4) 0.068(5) 0.052(4) 0.018(3) -0.003(3) 0.016(4)
C12 0.048(4) 0.070(5) 0.064(4) 0.006(4) 0.012(3) -0.013(4)
C13 0.243(15) 0.139(11) 0.197(13) -0.082(10) 0.181(12) -0.090(11)
C14 0.165(12) 0.258(17) 0.137(10) -0.074(11) 0.084(9) -0.153(12)
C15 0.097(9) 0.297(19) 0.283(18) 0.239(16) 0.092(10) 0.042(10)
N1 0.034(3) 0.045(3) 0.029(2) 0.005(2) -0.001(2) -0.001(2)
N2 0.035(3) 0.035(3) 0.038(3) 0.002(2) 0.001(2) -0.004(2)
N3 0.042(3) 0.034(3) 0.032(2) 0.0016(19) -0.004(2) 0.003(2)
C1 0.043(4) 0.050(4) 0.040(3) 0.012(3) 0.004(3) 0.002(3)
C2 0.047(4) 0.039(4) 0.045(3) 0.009(3) 0.001(3) -0.008(3)
C3 0.052(4) 0.034(3) 0.046(4) 0.002(3) -0.003(3) 0.003(3)
C4 0.052(4) 0.036(3) 0.046(3) 0.008(3) -0.009(3) 0.005(3)
C5 0.046(4) 0.047(4) 0.036(3) 0.011(3) -0.005(3) 0.008(3)
C6 0.044(4) 0.054(4) 0.030(3) 0.011(3) -0.006(3) 0.002(3)
O1A 0.036(2) 0.051(2) 0.0274(19) 0.0047(17) 0.0007(17) 0.0038(18)
C1A 0.041(3) 0.037(3) 0.030(3) 0.003(2) 0.003(2) 0.000(3)
C2A 0.036(3) 0.052(4) 0.031(3) 0.005(3) 0.000(2) 0.003(3)
C3A 0.047(4) 0.050(4) 0.028(3) 0.003(2) 0.004(3) 0.006(3)
C4A 0.049(4) 0.039(4) 0.038(3) 0.002(2) 0.010(3) -0.001(3)
C5A 0.037(3) 0.047(3) 0.038(3) 0.002(3) 0.000(3) 0.001(3)
C6A 0.037(3) 0.039(3) 0.033(3) 0.002(2) 0.001(2) -0.001(3)
C7A 0.043(3) 0.056(4) 0.028(3) 0.003(3) -0.002(2) 0.002(3)
C8A 0.045(4) 0.053(4) 0.040(3) 0.003(3) 0.013(3) -0.004(3)
C9A 0.111(8) 0.105(7) 0.096(6) -0.032(6) 0.070(6) -0.034(6)
C10A 0.185(12) 0.074(7) 0.247(14) 0.075(8) 0.172(11) 0.041(7)
C11A 0.049(6) 0.40(2) 0.056(5) -0.009(9) 0.019(4) -0.048(9)
C12A 0.040(3) 0.044(3) 0.030(3) 0.002(2) 0.002(2) 0.000(3)
C13A 0.065(4) 0.042(4) 0.037(3) 0.004(3) -0.003(3) 0.000(3)
C14A 0.056(4) 0.049(4) 0.037(3) -0.001(3) -0.007(3) 0.001(3)
C15A 0.046(4) 0.069(5) 0.041(4) 0.008(3) -0.005(3) 0.002(3)
O1B 0.049(2) 0.033(2) 0.035(2) -0.0038(17) 0.0037(18) -0.0014(18)
C1B 0.043(3) 0.035(3) 0.034(3) 0.000(2) -0.005(3) 0.001(3)
C2B 0.044(4) 0.038(3) 0.036(3) 0.000(3) -0.009(3) 0.003(3)
C3B 0.047(4) 0.037(3) 0.046(3) -0.002(3) -0.009(3) -0.003(3)
C4B 0.048(4) 0.041(4) 0.040(3) -0.007(3) -0.005(3) 0.004(3)
C5B 0.055(4) 0.041(4) 0.038(3) -0.004(3) 0.003(3) 0.006(3)
C6B 0.046(4) 0.040(3) 0.032(3) -0.003(2) -0.001(3) 0.002(3)
C7B 0.040(3) 0.036(3) 0.040(3) 0.001(2) -0.004(3) -0.006(3)
C8B 0.068(5) 0.046(4) 0.053(4) -0.016(3) 0.001(3) 0.003(3)
C9B 0.204(13) 0.114(9) 0.090(7) -0.060(6) -0.078(8) 0.055(8)
C10B 0.171(13) 0.185(13) 0.285(18) -0.196(14) 0.115(13) -0.085(11)
C11B 0.222(13) 0.047(5) 0.092(7) -0.019(5) 0.011(7) -0.002(7)
C12B 0.058(4) 0.048(4) 0.037(3) -0.005(3) 0.002(3) -0.002(3)
C13B 0.067(5) 0.046(4) 0.041(4) 0.001(3) 0.001(3) -0.005(3)
C14B 0.054(4) 0.056(4) 0.056(4) 0.000(3) -0.003(3) -0.009(3)
C15B 0.081(6) 0.070(5) 0.053(4) -0.008(4) 0.024(4) -0.012(4)
O1C 0.041(2) 0.042(2) 0.038(2) 0.0046(17) -0.0112(18) -0.0033(18)
C1C 0.040(3) 0.043(3) 0.034(3) 0.003(3) -0.006(3) -0.004(3)
C2C 0.036(3) 0.047(4) 0.036(3) 0.002(3) -0.003(2) 0.000(3)
C3C 0.040(4) 0.065(5) 0.053(4) -0.008(3) -0.011(3) 0.011(3)
C4C 0.050(4) 0.078(5) 0.064(5) -0.016(4) -0.021(4) 0.009(4)
C5C 0.062(5) 0.067(5) 0.066(5) -0.024(4) -0.025(4) 0.008(4)
C6C 0.053(4) 0.052(4) 0.038(3) -0.005(3) -0.009(3) 0.002(3)
C7C 0.037(3) 0.050(4) 0.039(3) -0.001(3) -0.007(3) 0.006(3)
C8C 0.058(6) 0.126(8) 0.093(7) -0.030(6) -0.035(5) 0.014(5)
C9C 0.128(10) 0.193(12) 0.105(8) -0.059(8) -0.073(7) 0.039(9)
C10C 0.045(7) 0.81(5) 0.089(9) -0.126(17) -0.032(6) 0.040(14)
C11C 0.190(14) 0.162(13) 0.156(12) 0.021(11) -0.095(11) 0.026(11)
C12C 0.057(4) 0.048(4) 0.045(4) -0.008(3) -0.013(3) 0.001(3)
C13C 0.087(7) 0.062(5) 0.159(9) -0.044(6) -0.031(6) 0.003(5)
C14C 0.078(6) 0.064(5) 0.111(7) 0.024(5) 0.033(5) 0.022(5)
C15C 0.242(13) 0.051(5) 0.065(5) -0.011(4) -0.040(7) 0.051(7)

_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 O4 2.165(4) . ?
U1 O1C 2.185(4) . ?
U1 O1B 2.195(3) . ?
U1 O1A 2.204(4) . ?
U1 N1 2.691(4) . ?
U1 N3 2.698(4) . ?
U1 N2 2.719(4) . ?
O4 C1D 1.358(7) . ?
C1D C2D 1.399(8) . ?
C1D C6D 1.408(7) . ?
C2D C3D 1.378(8) . ?
C3D C4D 1.391(8) . ?
C4D C5D 1.366(8) . ?
C4D C12 1.536(9) . ?
C5D C6D 1.409(8) . ?
C6D C8D 1.538(8) . ?
C8D C9D 1.509(8) . ?
C8D C11 1.522(8) . ?
C8D C10 1.538(8) . ?
C12 C13 1.475(12) . ?
C12 C15 1.492(12) . ?
C12 C14 1.498(12) . ?
N1 C1 1.473(7) . ?
N1 C6 1.493(7) . ?
N1 C7A 1.495(7) . ?
N2 C2 1.449(7) . ?
N2 C3 1.479(7) . ?
N2 C7B 1.490(7) . ?
N3 C4 1.477(7) . ?
N3 C5 1.484(6) . ?
N3 C7C 1.487(7) . ?
C1 C2 1.527(8) . ?
C3 C4 1.515(8) . ?
C5 C6 1.493(8) . ?
O1A C1A 1.359(6) . ?
C1A C6A 1.412(8) . ?
C1A C2A 1.420(7) . ?
C2A C3A 1.367(8) . ?
C2A C7A 1.489(8) . ?
C3A C4A 1.386(8) . ?
C4A C5A 1.420(8) . ?
C4A C8A 1.537(8) . ?
C5A C6A 1.373(8) . ?
C6A C12A 1.528(7) . ?
C8A C11A 1.469(11) . ?
C8A C9A 1.494(10) . ?
C8A C10A 1.530(11) . ?
C12A C15A 1.500(8) . ?
C12A C14A 1.531(8) . ?
C12A C13A 1.540(8) . ?
O1B C1B 1.353(6) . ?
C1B C6B 1.391(8) . ?
C1B C2B 1.399(8) . ?
C2B C3B 1.381(8) . ?
C2B C7B 1.510(8) . ?
C3B C4B 1.367(8) . ?
C4B C5B 1.373(8) . ?
C4B C8B 1.547(8) . ?
C5B C6B 1.385(8) . ?
C6B C12B 1.537(8) . ?
C8B C11B 1.497(11) . ?
C8B C9B 1.501(12) . ?
C8B C10B 1.559(13) . ?
C12B C14B 1.547(8) . ?
C12B C13B 1.557(9) . ?
C12B C15B 1.574(8) . ?
O1C C1C 1.349(6) . ?
C1C C2C 1.389(8) . ?
C1C C6C 1.402(8) . ?
C2C C3C 1.380(8) . ?
C2C C7C 1.505(8) . ?
C3C C4C 1.384(9) . ?
C4C C5C 1.368(9) . ?
C4C C8C 1.544(10) . ?
C5C C6C 1.394(9) . ?
C6C C12C 1.559(9) . ?
C8C C10C 1.342(14) . ?
C8C C9C 1.478(13) . ?
C8C C11C 1.601(16) . ?
C12C C14C 1.491(9) . ?
C12C C15C 1.533(9) . ?
C12C C13C 1.545(9) . ?

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
O4 U1 O1C 82.72(14) . . ?
O4 U1 O1B 84.23(13) . . ?
O1C U1 O1B 122.45(14) . . ?
O4 U1 O1A 87.44(14) . . ?
O1C U1 O1A 115.80(14) . . ?
O1B U1 O1A 119.27(14) . . ?
O4 U1 N1 143.22(14) . . ?
O1C U1 N1 79.65(14) . . ?
O1B U1 N1 132.34(14) . . ?
O1A U1 N1 71.93(13) . . ?
O4 U1 N3 137.01(14) . . ?
O1C U1 N3 70.10(14) . . ?
O1B U1 N3 83.24(13) . . ?
O1A U1 N3 134.05(13) . . ?
N1 U1 N3 64.32(14) . . ?
O4 U1 N2 145.53(13) . . ?
O1C U1 N2 130.42(13) . . ?
O1B U1 N2 70.34(13) . . ?
O1A U1 N2 85.31(14) . . ?
N1 U1 N2 64.47(14) . . ?
N3 U1 N2 64.09(14) . . ?
C1D O4 U1 141.4(4) . . ?
O4 C1D C2D 118.7(5) . . ?
O4 C1D C6D 122.4(5) . . ?
C2D C1D C6D 118.9(5) . . ?
C3D C2D C1D 121.2(6) . . ?
C2D C3D C4D 121.2(6) . . ?
C5D C4D C3D 117.1(6) . . ?
C5D C4D C12 121.5(6) . . ?
C3D C4D C12 121.3(6) . . ?
C4D C5D C6D 124.2(6) . . ?
C1D C6D C5D 117.2(5) . . ?
C1D C6D C8D 121.9(5) . . ?
C5D C6D C8D 121.0(5) . . ?
C9D C8D C11 107.4(5) . . ?
C9D C8D C10 111.5(5) . . ?
C11 C8D C10 107.4(5) . . ?
C9D C8D C6D 110.1(5) . . ?
C11 C8D C6D 112.2(5) . . ?
C10 C8D C6D 108.4(5) . . ?
C13 C12 C15 103.8(10) . . ?
C13 C12 C14 113.7(9) . . ?
C15 C12 C14 108.2(10) . . ?
C13 C12 C4D 108.5(7) . . ?
C15 C12 C4D 112.3(6) . . ?
C14 C12 C4D 110.2(6) . . ?
C1 N1 C6 109.3(4) . . ?
C1 N1 C7A 111.8(4) . . ?
C6 N1 C7A 108.0(4) . . ?
C1 N1 U1 116.2(3) . . ?
C6 N1 U1 107.7(3) . . ?
C7A N1 U1 103.3(3) . . ?
C2 N2 C3 110.9(4) . . ?
C2 N2 C7B 108.4(4) . . ?
C3 N2 C7B 110.8(4) . . ?
C2 N2 U1 105.6(3) . . ?
C3 N2 U1 115.4(3) . . ?
C7B N2 U1 105.4(3) . . ?
C4 N3 C5 110.8(4) . . ?
C4 N3 C7C 107.6(4) . . ?
C5 N3 C7C 111.0(4) . . ?
C4 N3 U1 106.9(3) . . ?
C5 N3 U1 116.4(3) . . ?
C7C N3 U1 103.6(3) . . ?
N1 C1 C2 112.5(4) . . ?
N2 C2 C1 114.0(5) . . ?
N2 C3 C4 113.1(5) . . ?
N3 C4 C3 111.2(5) . . ?
N3 C5 C6 113.5(4) . . ?
N1 C6 C5 113.1(5) . . ?
C1A O1A U1 147.4(3) . . ?
O1A C1A C6A 123.9(5) . . ?
O1A C1A C2A 117.5(5) . . ?
C6A C1A C2A 118.6(5) . . ?
C3A C2A C1A 120.9(5) . . ?
C3A C2A C7A 119.6(5) . . ?
C1A C2A C7A 119.5(5) . . ?
C2A C3A C4A 122.0(5) . . ?
C3A C4A C5A 116.3(5) . . ?
C3A C4A C8A 121.5(5) . . ?
C5A C4A C8A 122.2(6) . . ?
C6A C5A C4A 123.9(6) . . ?
C5A C6A C1A 118.2(5) . . ?
C5A C6A C12A 119.5(5) . . ?
C1A C6A C12A 122.3(5) . . ?
C2A C7A N1 116.5(5) . . ?
C11A C8A C9A 105.5(8) . . ?
C11A C8A C10A 115.5(8) . . ?
C9A C8A C10A 103.0(8) . . ?
C11A C8A C4A 112.5(6) . . ?
C9A C8A C4A 110.3(5) . . ?
C10A C8A C4A 109.5(6) . . ?
C15A C12A C6A 113.3(5) . . ?
C15A C12A C14A 106.4(5) . . ?
C6A C12A C14A 111.7(5) . . ?
C15A C12A C13A 109.5(5) . . ?
C6A C12A C13A 107.7(5) . . ?
C14A C12A C13A 108.2(5) . . ?
C1B O1B U1 150.0(3) . . ?
O1B C1B C6B 122.6(5) . . ?
O1B C1B C2B 118.1(5) . . ?
C6B C1B C2B 119.3(5) . . ?
C3B C2B C1B 120.4(5) . . ?
C3B C2B C7B 120.4(5) . . ?
C1B C2B C7B 119.1(5) . . ?
C4B C3B C2B 121.9(6) . . ?
C3B C4B C5B 116.2(5) . . ?
C3B C4B C8B 121.6(6) . . ?
C5B C4B C8B 122.2(6) . . ?
C4B C5B C6B 125.4(6) . . ?
C5B C6B C1B 116.9(5) . . ?
C5B C6B C12B 121.2(5) . . ?
C1B C6B C12B 121.8(5) . . ?
N2 C7B C2B 115.7(5) . . ?
C11B C8B C9B 106.4(8) . . ?
C11B C8B C4B 112.5(6) . . ?
C9B C8B C4B 108.1(6) . . ?
C11B C8B C10B 110.7(9) . . ?
C9B C8B C10B 106.7(9) . . ?
C4B C8B C10B 112.1(6) . . ?
C6B C12B C14B 110.1(5) . . ?
C6B C12B C13B 108.8(5) . . ?
C14B C12B C13B 110.7(5) . . ?
C6B C12B C15B 112.6(5) . . ?
C14B C12B C15B 105.7(5) . . ?
C13B C12B C15B 108.9(5) . . ?
C1C O1C U1 149.1(4) . . ?
O1C C1C C2C 117.7(5) . . ?
O1C C1C C6C 122.2(6) . . ?
C2C C1C C6C 120.1(5) . . ?
C3C C2C C1C 119.9(6) . . ?
C3C C2C C7C 120.0(5) . . ?
C1C C2C C7C 120.1(5) . . ?
C2C C3C C4C 122.0(6) . . ?
C5C C4C C3C 116.2(6) . . ?
C5C C4C C8C 122.9(7) . . ?
C3C C4C C8C 120.9(7) . . ?
C4C C5C C6C 125.0(6) . . ?
C5C C6C C1C 116.5(6) . . ?
C5C C6C C12C 119.7(5) . . ?
C1C C6C C12C 123.8(5) . . ?
N3 C7C C2C 115.1(5) . . ?
C10C C8C C9C 111.3(11) . . ?
C10C C8C C4C 111.9(9) . . ?
C9C C8C C4C 114.3(8) . . ?
C10C C8C C11C 103.5(13) . . ?
C9C C8C C11C 105.1(10) . . ?
C4C C8C C11C 109.9(8) . . ?
C14C C12C C15C 106.4(7) . . ?
C14C C12C C13C 107.4(7) . . ?
C15C C12C C13C 107.0(7) . . ?
C14C C12C C6C 109.5(6) . . ?
C15C C12C C6C 114.2(5) . . ?
C13C C12C C6C 112.0(6) . . ?

_diffrn_measured_fraction_theta_max    0.977
_diffrn_reflns_theta_full              27.57
_diffrn_measured_fraction_theta_full   0.977
_refine_diff_density_max    1.918
_refine_diff_density_min   -0.748
_refine_diff_density_rms    0.266
#========================================================

#_eof