#------------------------------------------------------------------------------
#$Date: 2016-03-25 23:59:21 +0200 (Fri, 25 Mar 2016) $
#$Revision: 180054 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/00/7050050.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7050050
loop_
_publ_author_name
'Bernardo Masci'
'Pierre Thuéry'
_publ_section_title
;
 Synthesis of homooxacalixarenes with 5 and 10 phenol units and crystal
 structure of their complexes with uranyl ions
;
_journal_issue                   3
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              493
_journal_paper_doi               10.1039/b413827a
_journal_volume                  29
_journal_year                    2005
_chemical_formula_sum            'C178 H244 N20 O28 U4'
_chemical_formula_weight         4064.05
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                117.130(6)
_cell_angle_beta                 102.485(7)
_cell_angle_gamma                96.117(7)
_cell_formula_units_Z            1
_cell_length_a                   13.4500(14)
_cell_length_b                   19.1428(16)
_cell_length_c                   20.2899(18)
_cell_measurement_reflns_used    23830
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      2.98
_cell_volume                     4411.0(8)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'Kappa-CCD software (Nonius B.V., 1998)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1999)'
_computing_publication_material  'SHELXTL (Sheldrick, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.860
_diffrn_measured_fraction_theta_max 0.860
_diffrn_measurement_device_type  'Nonius Kappa-CCD'
_diffrn_measurement_method       'φ scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0920
_diffrn_reflns_av_sigmaI/netI    0.1087
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            23830
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         2.98
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    3.734
_exptl_absorpt_correction_T_max  0.688
_exptl_absorpt_correction_T_min  0.466
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details   'program DELABS from PLATON (Spek, 2000)'
_exptl_crystal_colour            'translucent dark orange'
_exptl_crystal_density_diffrn    1.530
_exptl_crystal_density_meas      ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2044
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.066
_refine_diff_density_min         -1.123
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.913
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1049
_refine_ls_number_reflns         14405
_refine_ls_number_restraints     380
_refine_ls_restrained_S_all      0.905
_refine_ls_R_factor_all          0.2695
_refine_ls_R_factor_gt           0.0886
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0548P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1589
_refine_ls_wR_factor_ref         0.2386
_reflns_number_gt                4660
_reflns_number_total             14405
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b413827a.txt
_cod_data_source_block           19
_cod_original_cell_volume        4411.0(7)
_cod_database_code               7050050
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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 0.63602(7) 0.84798(6) 0.27396(5) 0.0614(3) Uani 1 1 d . . .
U2 U 0.93984(7) 0.88817(6) 0.49212(6) 0.0634(4) Uani 1 1 d . . .
O1 O 0.6187(11) 0.9392(9) 0.2319(8) 0.071(5) Uani 1 1 d . . .
O2 O 0.5002(11) 0.7845(9) 0.1716(9) 0.068(5) Uani 1 1 d . . .
O3 O 0.5973(10) 0.7270(8) 0.2745(8) 0.055(4) Uani 1 1 d . . .
O4 O 0.8332(10) 0.7801(9) 0.4587(9) 0.064(4) Uani 1 1 d . . .
O5 O 1.0405(11) 0.8477(9) 0.5605(9) 0.068(4) Uani 1 1 d . . .
O6 O 1.1846(11) 0.9587(8) 0.7859(8) 0.067(5) Uani 1 1 d . . .
O7 O 0.7233(10) 0.8068(9) 0.2194(10) 0.074(5) Uani 1 1 d . . .
O8 O 0.5582(10) 0.8907(8) 0.3345(9) 0.057(4) Uani 1 1 d . . .
O9 O 0.9918(10) 0.8433(9) 0.4123(8) 0.069(5) Uani 1 1 d . . .
O10 O 0.8848(10) 0.9415(10) 0.5693(9) 0.075(5) Uani 1 1 d . . .
O11 O 0.7826(12) 0.8816(9) 0.3937(9) 0.072(5) Uani 1 1 d . . .
O12 O 0.7741(14) 0.9750(10) 0.3537(10) 0.075(6) Uani 1 1 d . . .
O13 O 0.9186(12) 0.9922(10) 0.4521(9) 0.081(6) Uani 1 1 d . . .
N1 N 0.827(2) 0.9551(14) 0.3975(15) 0.064(7) Uani 1 1 d . . .
C1 C 0.6690(19) 0.9284(13) 0.1220(15) 0.074(7) Uani 1 1 d . . .
C2 C 0.5916(17) 0.9256(12) 0.1567(14) 0.059(7) Uani 1 1 d . . .
C3 C 0.4826(16) 0.8976(12) 0.1097(13) 0.059(7) Uani 1 1 d . . .
C4 C 0.461(2) 0.8734(13) 0.0303(12) 0.072(8) Uani 1 1 d . . .
H4A H 0.3912 0.8531 0.0001 0.087 Uiso 1 1 calc R . .
C5 C 0.5352(18) 0.8772(13) -0.0068(14) 0.068(7) Uani 1 1 d . . .
C6 C 0.6388(18) 0.9073(14) 0.0420(16) 0.071(7) Uani 1 1 d . . .
H6 H 0.6915 0.9140 0.0209 0.085 Uiso 1 1 calc R . .
C7 C 0.504(2) 0.8489(15) -0.0908(13) 0.070(8) Uani 1 1 d D . .
C8 C 0.494(5) 0.7583(18) -0.135(3) 0.13(3) Uani 1 1 d DU . .
H8A H 0.5571 0.7457 -0.1162 0.197 Uiso 1 1 calc R . .
H8B H 0.4809 0.7408 -0.1894 0.197 Uiso 1 1 calc R . .
H8C H 0.4362 0.7312 -0.1280 0.197 Uiso 1 1 calc R . .
C9 C 0.405(2) 0.8760(19) -0.1172(18) 0.112(11) Uani 1 1 d U . .
H9A H 0.3457 0.8493 -0.1114 0.168 Uiso 1 1 calc R . .
H9B H 0.3924 0.8620 -0.1707 0.168 Uiso 1 1 calc R . .
H9C H 0.4161 0.9334 -0.0858 0.168 Uiso 1 1 calc R . .
C10 C 0.582(2) 0.8915(18) -0.1122(17) 0.116(11) Uani 1 1 d U . .
H10A H 0.5566 0.8741 -0.1665 0.174 Uiso 1 1 calc R . .
H10B H 0.6482 0.8788 -0.1009 0.174 Uiso 1 1 calc R . .
H10C H 0.5894 0.9488 -0.0826 0.174 Uiso 1 1 calc R . .
C11 C 0.3983(16) 0.8912(12) 0.1436(12) 0.055(6) Uani 1 1 d . . .
H11A H 0.3478 0.9198 0.1322 0.066 Uiso 1 1 calc R . .
H11B H 0.4278 0.9176 0.1996 0.066 Uiso 1 1 calc R . .
C12 C 0.3418(17) 0.8051(14) 0.1142(14) 0.061(7) Uani 1 1 d . . .
C13 C 0.3963(15) 0.7571(17) 0.1320(13) 0.065(7) Uani 1 1 d . . .
C14 C 0.3471(17) 0.6783(16) 0.1140(13) 0.063(7) Uani 1 1 d . . .
C15 C 0.2441(16) 0.6494(14) 0.0757(13) 0.061(7) Uani 1 1 d . . .
H15 H 0.2115 0.5964 0.0592 0.073 Uiso 1 1 calc R . .
C16 C 0.1816(17) 0.7047(17) 0.0601(15) 0.071(7) Uani 1 1 d . . .
C17 C 0.2351(19) 0.7803(15) 0.0810(13) 0.074(8) Uani 1 1 d . . .
H17 H 0.1984 0.8155 0.0726 0.088 Uiso 1 1 calc R . .
C18 C 0.0588(19) 0.6721(16) 0.0204(16) 0.071(7) Uani 1 1 d U . .
C19 C 0.036(2) 0.6656(17) -0.0592(16) 0.110(10) Uani 1 1 d U . .
H19A H 0.0664 0.6243 -0.0913 0.166 Uiso 1 1 calc R . .
H19B H 0.0666 0.7164 -0.0538 0.166 Uiso 1 1 calc R . .
H19C H -0.0380 0.6519 -0.0829 0.166 Uiso 1 1 calc R . .
C20 C 0.018(2) 0.5876(17) 0.0042(17) 0.107(10) Uani 1 1 d U . .
H20A H -0.0570 0.5736 -0.0146 0.160 Uiso 1 1 calc R . .
H20B H 0.0402 0.5850 0.0512 0.160 Uiso 1 1 calc R . .
H20C H 0.0454 0.5504 -0.0342 0.160 Uiso 1 1 calc R . .
C21 C 0.012(2) 0.7304(19) 0.0740(18) 0.118(11) Uani 1 1 d U . .
H21A H 0.0072 0.7735 0.0625 0.178 Uiso 1 1 calc R . .
H21B H 0.0559 0.7520 0.1264 0.178 Uiso 1 1 calc R . .
H21C H -0.0562 0.7039 0.0682 0.178 Uiso 1 1 calc R . .
C22 C 0.4093(17) 0.6316(14) 0.1362(13) 0.067(7) Uani 1 1 d . . .
H22A H 0.4786 0.6438 0.1317 0.080 Uiso 1 1 calc R . .
H22B H 0.3782 0.5748 0.0995 0.080 Uiso 1 1 calc R . .
C23 C 0.4215(17) 0.6448(12) 0.2175(15) 0.060(7) Uani 1 1 d . . .
C24 C 0.5089(17) 0.6927(14) 0.2818(14) 0.066(7) Uani 1 1 d . . .
C25 C 0.5065(16) 0.6985(13) 0.3526(13) 0.051(6) Uani 1 1 d . . .
C26 C 0.4211(16) 0.6649(13) 0.3623(14) 0.068(7) Uani 1 1 d . . .
H26 H 0.4215 0.6741 0.4115 0.081 Uiso 1 1 calc R . .
C27 C 0.3265(16) 0.6134(14) 0.2950(13) 0.054(6) Uani 1 1 d . . .
C28 C 0.3359(15) 0.6086(13) 0.2284(13) 0.061(7) Uani 1 1 d . . .
H28 H 0.2784 0.5775 0.1846 0.073 Uiso 1 1 calc R . .
C29 C 0.235(2) 0.5700(17) 0.3051(14) 0.083(9) Uani 1 1 d . . .
C30 C 0.201(3) 0.627(2) 0.371(2) 0.138(13) Uani 1 1 d U . .
H30A H 0.1458 0.5975 0.3783 0.208 Uiso 1 1 calc R . .
H30B H 0.1767 0.6670 0.3605 0.208 Uiso 1 1 calc R . .
H30C H 0.2596 0.6530 0.4179 0.208 Uiso 1 1 calc R . .
C31 C 0.1439(17) 0.5276(14) 0.2327(14) 0.078(7) Uani 1 1 d U . .
H31A H 0.1536 0.4758 0.1986 0.117 Uiso 1 1 calc R . .
H31B H 0.1389 0.5594 0.2073 0.117 Uiso 1 1 calc R . .
H31C H 0.0805 0.5205 0.2459 0.117 Uiso 1 1 calc R . .
C32 C 0.268(2) 0.5094(18) 0.3277(17) 0.101(10) Uani 1 1 d U . .
H32A H 0.2079 0.4771 0.3270 0.152 Uiso 1 1 calc R . .
H32B H 0.3171 0.5373 0.3790 0.152 Uiso 1 1 calc R . .
H32C H 0.3010 0.4752 0.2916 0.152 Uiso 1 1 calc R . .
C33 C 0.6058(15) 0.7387(12) 0.4193(12) 0.056(6) Uani 1 1 d . . .
H33A H 0.5875 0.7628 0.4674 0.067 Uiso 1 1 calc R . .
H33B H 0.6448 0.7820 0.4160 0.067 Uiso 1 1 calc R . .
C34 C 0.6789(16) 0.6810(14) 0.4229(14) 0.061(7) Uani 1 1 d . . .
C35 C 0.7873(13) 0.7038(12) 0.4421(11) 0.042(5) Uani 1 1 d U . .
C36 C 0.8450(14) 0.6491(11) 0.4447(13) 0.047(5) Uani 1 1 d . . .
C37 C 0.7972(15) 0.5764(12) 0.4283(12) 0.056(6) Uani 1 1 d . . .
H37 H 0.8400 0.5429 0.4332 0.068 Uiso 1 1 calc R . .
C38 C 0.6878(17) 0.5444(11) 0.4040(13) 0.066(7) Uani 1 1 d D . .
C39 C 0.634(2) 0.6016(16) 0.4068(14) 0.072(8) Uani 1 1 d . . .
H39 H 0.5623 0.5879 0.3974 0.086 Uiso 1 1 calc R . .
C40 C 0.6470(16) 0.4588(12) 0.3797(13) 0.098(13) Uani 1 1 d DU . .
C41 C 0.682(3) 0.4456(19) 0.4462(18) 0.158(19) Uani 1 1 d DU . .
H41A H 0.6299 0.4532 0.4731 0.236 Uiso 1 1 calc R . .
H41B H 0.7470 0.4835 0.4808 0.236 Uiso 1 1 calc R . .
H41C H 0.6912 0.3916 0.4279 0.236 Uiso 1 1 calc R . .
C42 C 0.5323(15) 0.4377(18) 0.3501(19) 0.108(14) Uani 1 1 d DU . .
H42A H 0.5053 0.3866 0.3454 0.162 Uiso 1 1 calc R . .
H42B H 0.5112 0.4342 0.3001 0.162 Uiso 1 1 calc R . .
H42C H 0.5051 0.4786 0.3854 0.162 Uiso 1 1 calc R . .
C43 C 0.689(3) 0.4073(16) 0.3170(18) 0.105(19) Uani 1 1 d DU . .
H43A H 0.6697 0.4177 0.2745 0.158 Uiso 1 1 calc R . .
H43B H 0.6609 0.3514 0.2995 0.158 Uiso 1 1 calc R . .
H43C H 0.7641 0.4194 0.3365 0.158 Uiso 1 1 calc R . .
C44 C 0.9660(16) 0.6767(14) 0.4699(13) 0.065(7) Uani 1 1 d . . .
H44A H 0.9955 0.6300 0.4490 0.078 Uiso 1 1 calc R . .
H44B H 0.9859 0.7113 0.4495 0.078 Uiso 1 1 calc R . .
C45 C 1.0094(15) 0.7232(16) 0.5593(15) 0.072(8) Uani 1 1 d . . .
C46 C 1.0355(14) 0.8041(14) 0.5962(14) 0.052(6) Uani 1 1 d . . .
C47 C 1.0672(17) 0.8427(13) 0.6787(15) 0.063(7) Uani 1 1 d . . .
C48 C 1.0635(19) 0.7972(15) 0.7201(17) 0.081(8) Uani 1 1 d . . .
H48 H 1.0765 0.8235 0.7737 0.097 Uiso 1 1 calc R . .
C49 C 1.0401(19) 0.7144(17) 0.6771(18) 0.081(8) Uani 1 1 d . . .
C50 C 1.0085(15) 0.6762(13) 0.5948(16) 0.065(7) Uani 1 1 d . . .
H50 H 0.9875 0.6202 0.5650 0.078 Uiso 1 1 calc R . .
C51 C 1.0416(18) 0.6640(15) 0.7199(13) 0.066(7) Uani 1 1 d D . .
C52 C 1.147(2) 0.6989(16) 0.7853(16) 0.104(9) Uani 1 1 d U . .
H52A H 1.1372 0.6957 0.8293 0.156 Uiso 1 1 calc R . .
H52B H 1.1736 0.7543 0.8001 0.156 Uiso 1 1 calc R . .
H52C H 1.1971 0.6683 0.7668 0.156 Uiso 1 1 calc R . .
C53 C 0.960(2) 0.6842(19) 0.7626(17) 0.122(12) Uani 1 1 d DU . .
H53A H 0.9687 0.6639 0.7984 0.183 Uiso 1 1 calc R . .
H53B H 0.8916 0.6598 0.7260 0.183 Uiso 1 1 calc R . .
H53C H 0.9695 0.7417 0.7906 0.183 Uiso 1 1 calc R . .
C54 C 1.0189(19) 0.5756(15) 0.6658(15) 0.091(9) Uani 1 1 d U . .
H54A H 1.0706 0.5642 0.6386 0.136 Uiso 1 1 calc R . .
H54B H 0.9506 0.5582 0.6292 0.136 Uiso 1 1 calc R . .
H54C H 1.0210 0.5474 0.6947 0.136 Uiso 1 1 calc R . .
C55 C 1.0928(18) 0.9351(11) 0.7279(13) 0.066(7) Uani 1 1 d . . .
H55A H 1.1007 0.9594 0.6960 0.079 Uiso 1 1 calc R . .
H55B H 1.0367 0.9522 0.7499 0.079 Uiso 1 1 calc R . .
C56 C 1.2165(16) 1.0430(12) 0.8309(13) 0.060(7) Uani 1 1 d . . .
H56A H 1.1741 1.0621 0.8658 0.071 Uiso 1 1 calc R . .
H56B H 1.2046 1.0663 0.7971 0.071 Uiso 1 1 calc R . .
N2 N 0.6191(18) 1.0865(13) 0.3359(14) 0.084(7) Uani 1 1 d U . .
H2 H 0.6186 1.0348 0.3021 0.101 Uiso 1 1 calc R . .
N3 N 0.622(2) 1.2282(15) 0.4301(15) 0.092(7) Uani 1 1 d U . .
C57 C 0.711(2) 1.1348(18) 0.3456(18) 0.108(10) Uani 1 1 d U . .
H57A H 0.7092 1.1352 0.2977 0.130 Uiso 1 1 calc R . .
H57B H 0.7701 1.1143 0.3594 0.130 Uiso 1 1 calc R . .
C58 C 0.721(2) 1.2260(18) 0.4147(18) 0.103(10) Uani 1 1 d U . .
H58A H 0.7760 1.2387 0.4610 0.124 Uiso 1 1 calc R . .
H58B H 0.7383 1.2651 0.3986 0.124 Uiso 1 1 calc R . .
C59 C 0.529(3) 1.104(2) 0.303(2) 0.133(13) Uani 1 1 d U . .
H59A H 0.4665 1.0708 0.3005 0.159 Uiso 1 1 calc R . .
H59B H 0.5255 1.0930 0.2511 0.159 Uiso 1 1 calc R . .
C60 C 0.534(3) 1.196(2) 0.356(2) 0.145(14) Uani 1 1 d U . .
H60A H 0.5464 1.2255 0.3296 0.174 Uiso 1 1 calc R . .
H60B H 0.4683 1.2021 0.3678 0.174 Uiso 1 1 calc R . .
C61 C 0.600(3) 1.087(2) 0.408(2) 0.118(11) Uani 1 1 d U . .
H61A H 0.6566 1.0723 0.4336 0.142 Uiso 1 1 calc R . .
H61B H 0.5343 1.0499 0.3941 0.142 Uiso 1 1 calc R . .
C62 C 0.597(3) 1.177(2) 0.459(2) 0.142(14) Uani 1 1 d U . .
H62A H 0.5268 1.1784 0.4645 0.170 Uiso 1 1 calc R . .
H62B H 0.6450 1.1982 0.5105 0.170 Uiso 1 1 calc R . .
N4 N 0.7225(13) 0.6302(11) 0.2194(10) 0.061(5) Uani 1 1 d U . .
H4 H 0.6790 0.6624 0.2383 0.073 Uiso 1 1 calc R . .
N5 N 0.852(2) 0.5479(17) 0.1713(17) 0.108(8) Uani 1 1 d U . .
C63 C 0.706(2) 0.5619(15) 0.2340(15) 0.075(8) Uani 1 1 d U . .
H63A H 0.6348 0.5291 0.2071 0.090 Uiso 1 1 calc R . .
H63B H 0.7204 0.5805 0.2891 0.090 Uiso 1 1 calc R . .
C64 C 0.783(3) 0.5158(19) 0.2021(18) 0.104(10) Uani 1 1 d U . .
H64A H 0.8272 0.5098 0.2431 0.124 Uiso 1 1 calc R . .
H64B H 0.7444 0.4620 0.1612 0.124 Uiso 1 1 calc R . .
C65 C 0.7030(18) 0.6056(15) 0.1347(14) 0.073(7) Uani 1 1 d U . .
H65A H 0.7116 0.6530 0.1284 0.088 Uiso 1 1 calc R . .
H65B H 0.6325 0.5727 0.1047 0.088 Uiso 1 1 calc R . .
C66 C 0.787(2) 0.5557(18) 0.1070(18) 0.093(9) Uani 1 1 d U . .
H66A H 0.7510 0.5025 0.0636 0.112 Uiso 1 1 calc R . .
H66B H 0.8312 0.5828 0.0897 0.112 Uiso 1 1 calc R . .
C67 C 0.8329(16) 0.6791(15) 0.2592(14) 0.074(7) Uani 1 1 d U . .
H67A H 0.8454 0.7050 0.3149 0.089 Uiso 1 1 calc R . .
H67B H 0.8427 0.7213 0.2456 0.089 Uiso 1 1 calc R . .
C68 C 0.913(2) 0.6280(16) 0.2373(16) 0.083(8) Uani 1 1 d U . .
H68A H 0.9637 0.6528 0.2223 0.099 Uiso 1 1 calc R . .
H68B H 0.9496 0.6226 0.2809 0.099 Uiso 1 1 calc R . .
N6 N 0.2275(18) 0.9000(15) 0.3028(14) 0.095(7) Uani 1 1 d U . .
N7 N 0.321(2) 0.8977(18) 0.4285(17) 0.111(9) Uani 1 1 d U . .
C69 C 0.295(2) 0.840(2) 0.2864(17) 0.109(10) Uani 1 1 d U . .
H69A H 0.3535 0.8588 0.2727 0.131 Uiso 1 1 calc R . .
H69B H 0.2547 0.7886 0.2424 0.131 Uiso 1 1 calc R . .
C70 C 0.337(2) 0.829(2) 0.3541(19) 0.108(10) Uani 1 1 d U . .
H70A H 0.4105 0.8301 0.3620 0.130 Uiso 1 1 calc R . .
H70B H 0.3002 0.7773 0.3442 0.130 Uiso 1 1 calc R . .
C71 C 0.149(2) 0.8800(18) 0.3391(16) 0.101(9) Uani 1 1 d DU . .
H71A H 0.1051 0.9184 0.3507 0.122 Uiso 1 1 calc R . .
H71B H 0.1050 0.8261 0.3044 0.122 Uiso 1 1 calc R . .
C72 C 0.216(3) 0.886(2) 0.4135(17) 0.127(12) Uani 1 1 d DU . .
H72A H 0.2016 0.9294 0.4568 0.152 Uiso 1 1 calc R . .
H72B H 0.1902 0.8362 0.4133 0.152 Uiso 1 1 calc R . .
C73 C 0.292(2) 0.9797(18) 0.3667(18) 0.098(10) Uani 1 1 d U . .
H73A H 0.2461 1.0144 0.3878 0.118 Uiso 1 1 calc R . .
H73B H 0.3345 1.0048 0.3470 0.118 Uiso 1 1 calc R . .
C74 C 0.363(2) 0.970(2) 0.4312(19) 0.112(11) Uani 1 1 d U . .
H74A H 0.4320 0.9699 0.4250 0.135 Uiso 1 1 calc R . .
H74B H 0.3687 1.0154 0.4814 0.135 Uiso 1 1 calc R . .
N8 N 0.213(2) 1.1196(18) 0.2873(18) 0.116(9) Uani 1 1 d U . .
C75 C 0.209(2) 1.185(2) 0.354(2) 0.095(9) Uani 1 1 d U . .
H75 H 0.1745 1.1699 0.3821 0.114 Uiso 1 1 calc R . .
C76 C 0.243(2) 1.264(2) 0.3863(18) 0.092(9) Uani 1 1 d U . .
H76 H 0.2413 1.3023 0.4349 0.110 Uiso 1 1 calc R . .
C77 C 0.282(2) 1.281(2) 0.335(2) 0.117(11) Uani 1 1 d U . .
H77 H 0.3096 1.3352 0.3526 0.140 Uiso 1 1 calc R . .
C78 C 0.285(2) 1.2263(18) 0.2623(19) 0.097(9) Uani 1 1 d DU . .
H78 H 0.3085 1.2408 0.2294 0.116 Uiso 1 1 calc R . .
C79 C 0.247(2) 1.1476(18) 0.2438(19) 0.106(10) Uani 1 1 d DU . .
H79 H 0.2457 1.1082 0.1946 0.127 Uiso 1 1 calc R . .
N9 N 0.098(2) 0.9234(14) 0.0508(14) 0.096(7) Uani 1 1 d U . .
C80 C 0.164(2) 0.9352(16) 0.0133(17) 0.087(8) Uani 1 1 d U . .
H80 H 0.2356 0.9488 0.0369 0.105 Uiso 1 1 calc R . .
C81 C 0.124(3) 0.9269(18) -0.064(2) 0.104(10) Uani 1 1 d U . .
H81 H 0.1694 0.9346 -0.0898 0.125 Uiso 1 1 calc R . .
C82 C 0.013(3) 0.9062(18) -0.0962(19) 0.105(10) Uani 1 1 d U . .
H82 H -0.0189 0.9016 -0.1439 0.126 Uiso 1 1 calc R . .
C83 C -0.045(3) 0.8933(19) -0.051(2) 0.103(10) Uani 1 1 d U . .
H83 H -0.1176 0.8790 -0.0710 0.124 Uiso 1 1 calc R . .
C84 C -0.006(2) 0.8998(17) 0.0154(19) 0.087(9) Uani 1 1 d U . .
H84 H -0.0503 0.8878 0.0398 0.105 Uiso 1 1 calc R . .
N10 N 0.5036(18) 0.5795(15) -0.0926(15) 0.089(7) Uani 1 1 d U . .
C85 C 0.513(2) 0.6451(19) -0.0261(19) 0.094(9) Uani 1 1 d U . .
H85 H 0.4527 0.6491 -0.0103 0.113 Uiso 1 1 calc R . .
C86 C 0.595(2) 0.7051(18) 0.0205(17) 0.090(9) Uani 1 1 d U . .
H86 H 0.5932 0.7501 0.0652 0.108 Uiso 1 1 calc R . .
C87 C 0.688(2) 0.6946(18) -0.0038(18) 0.084(9) Uani 1 1 d U . .
H87 H 0.7514 0.7318 0.0286 0.101 Uiso 1 1 calc R . .
C88 C 0.686(2) 0.636(2) -0.068(2) 0.111(11) Uani 1 1 d U . .
H88 H 0.7447 0.6328 -0.0857 0.134 Uiso 1 1 calc R . .
C89 C 0.590(2) 0.5758(18) -0.1128(17) 0.088(9) Uani 1 1 d U . .
H89 H 0.5887 0.5312 -0.1588 0.106 Uiso 1 1 calc R . .
O14 O 0.1468(17) 0.9602(14) 0.2047(13) 0.138(8) Uani 1 1 d U . .
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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O8 U1 O7 175.4(6) . . ?
O8 U1 O2 92.1(6) . . ?
O7 U1 O2 92.4(6) . . ?
O8 U1 O1 89.3(6) . . ?
O7 U1 O1 92.9(6) . . ?
O2 U1 O1 76.8(5) . . ?
O8 U1 O3 91.6(5) . . ?
O7 U1 O3 87.8(6) . . ?
O2 U1 O3 80.8(5) . . ?
O1 U1 O3 157.7(5) . . ?
O8 U1 O12 89.4(6) . . ?
O7 U1 O12 87.8(6) . . ?
O2 U1 O12 143.5(5) . . ?
O1 U1 O12 66.7(5) . . ?
O3 U1 O12 135.6(5) . . ?
O8 U1 O11 88.7(6) . . ?
O7 U1 O11 86.7(6) . . ?
O2 U1 O11 162.4(5) . . ?
O1 U1 O11 120.8(5) . . ?
O3 U1 O11 81.6(5) . . ?
O12 U1 O11 54.1(5) . . ?
O8 U1 N1 91.4(6) . . ?
O7 U1 N1 84.5(6) . . ?
O2 U1 N1 167.8(6) . . ?
O1 U1 N1 91.6(7) . . ?
O3 U1 N1 110.7(6) . . ?
O12 U1 N1 24.9(5) . . ?
O11 U1 N1 29.4(6) . . ?
O9 U2 O10 173.7(8) . . ?
O9 U2 O4 94.5(6) . . ?
O10 U2 O4 89.2(6) . . ?
O9 U2 O5 93.2(7) . . ?
O10 U2 O5 92.3(7) . . ?
O4 U2 O5 82.6(5) . . ?
O9 U2 O13 87.9(6) . 2_776 ?
O10 U2 O13 89.3(6) . 2_776 ?
O4 U2 O13 169.7(5) . 2_776 ?
O5 U2 O13 87.3(5) . 2_776 ?
O9 U2 O13 84.8(7) . . ?
O10 U2 O13 88.9(7) . . ?
O4 U2 O13 129.7(5) . . ?
O5 U2 O13 147.7(5) . . ?
O13 U2 O13 60.5(6) 2_776 . ?
O9 U2 O11 85.3(6) . . ?
O10 U2 O11 90.7(6) . . ?
O4 U2 O11 75.7(5) . . ?
O5 U2 O11 158.1(5) . . ?
O13 U2 O11 114.5(5) 2_776 . ?
O13 U2 O11 54.0(5) . . ?
O12 N1 O13 131(2) . . ?
O12 N1 O11 117(2) . . ?
O13 N1 O11 111(2) . . ?
C2 C1 C6 119(2) . . ?
C2 C1 C56 120(2) . 2_776 ?
C6 C1 C56 121(2) . 2_776 ?
O1 C2 C1 120(2) . . ?
O1 C2 C3 120.7(18) . . ?
C1 C2 C3 119(2) . . ?
C4 C3 C2 118(2) . . ?
C4 C3 C11 121.5(19) . . ?
C2 C3 C11 120.6(19) . . ?
C5 C4 C3 126(2) . . ?
C4 C5 C6 114(2) . . ?
C4 C5 C7 121(2) . . ?
C6 C5 C7 125(3) . . ?
C5 C6 C1 125(2) . . ?
C5 C7 C10 112(2) . . ?
C5 C7 C8 109(3) . . ?
C10 C7 C8 110(4) . . ?
C5 C7 C9 112(3) . . ?
C10 C7 C9 99(2) . . ?
C8 C7 C9 114(3) . . ?
C3 C11 C12 114(2) . . ?
C13 C12 C17 121(2) . . ?
C13 C12 C11 118(2) . . ?
C17 C12 C11 120(2) . . ?
C12 C13 O2 121(2) . . ?
C12 C13 C14 122.1(19) . . ?
O2 C13 C14 117(2) . . ?
C15 C14 C13 119(2) . . ?
C15 C14 C22 122(2) . . ?
C13 C14 C22 119(2) . . ?
C14 C15 C16 119(2) . . ?
C17 C16 C15 118(2) . . ?
C17 C16 C18 124(2) . . ?
C15 C16 C18 119(2) . . ?
C12 C17 C16 121(2) . . ?
C21 C18 C19 115(3) . . ?
C21 C18 C20 112(2) . . ?
C19 C18 C20 105(2) . . ?
C21 C18 C16 105(2) . . ?
C19 C18 C16 107(2) . . ?
C20 C18 C16 114(2) . . ?
C14 C22 C23 116(2) . . ?
C24 C23 C28 118(2) . . ?
C24 C23 C22 125.3(19) . . ?
C28 C23 C22 117(2) . . ?
O3 C24 C23 121(2) . . ?
O3 C24 C25 121.0(19) . . ?
C23 C24 C25 118(2) . . ?
C26 C25 C24 123(2) . . ?
C26 C25 C33 118.5(19) . . ?
C24 C25 C33 118.3(19) . . ?
C25 C26 C27 121(2) . . ?
C28 C27 C26 112.8(18) . . ?
C28 C27 C29 127(2) . . ?
C26 C27 C29 120.2(19) . . ?
C27 C28 C23 128(2) . . ?
C30 C29 C31 110(3) . . ?
C30 C29 C32 104(2) . . ?
C31 C29 C32 109(2) . . ?
C30 C29 C27 111(2) . . ?
C31 C29 C27 112(2) . . ?
C32 C29 C27 110(3) . . ?
C25 C33 C34 114.7(17) . . ?
C35 C34 C39 117(2) . . ?
C35 C34 C33 122.7(19) . . ?
C39 C34 C33 119.9(19) . . ?
O4 C35 C36 122.6(16) . . ?
O4 C35 C34 119.1(19) . . ?
C36 C35 C34 118.4(19) . . ?
C37 C36 C35 120.3(18) . . ?
C37 C36 C44 121.8(19) . . ?
C35 C36 C44 117.9(17) . . ?
C36 C37 C38 127(2) . . ?
C39 C38 C37 110.9(18) . . ?
C39 C38 C40 129.3(18) . . ?
C37 C38 C40 119.8(17) . . ?
C38 C39 C34 126(2) . . ?
C42 C40 C41 111(3) . . ?
C42 C40 C38 110(2) . . ?
C41 C40 C38 109(2) . . ?
C42 C40 C43 109(2) . . ?
C41 C40 C43 109(3) . . ?
C38 C40 C43 109(2) . . ?
C45 C44 C36 109.9(18) . . ?
C46 C45 C50 125(2) . . ?
C46 C45 C44 119(2) . . ?
C50 C45 C44 116(2) . . ?
O5 C46 C45 124(2) . . ?
O5 C46 C47 120(2) . . ?
C45 C46 C47 115(2) . . ?
C46 C47 C48 122(2) . . ?
C46 C47 C55 121(2) . . ?
C48 C47 C55 117(2) . . ?
C49 C48 C47 118(3) . . ?
C48 C49 C50 119(3) . . ?
C48 C49 C51 119(3) . . ?
C50 C49 C51 121(2) . . ?
C45 C50 C49 119(2) . . ?
C54 C51 C53 111(2) . . ?
C54 C51 C52 115(2) . . ?
C53 C51 C52 104(2) . . ?
C54 C51 C49 113(2) . . ?
C53 C51 C49 107(2) . . ?
C52 C51 C49 107(2) . . ?
O6 C55 C47 107.7(19) . . ?
O6 C56 C1 112.1(19) . 2_776 ?
C57 N2 C59 113(2) . . ?
C57 N2 C61 118(3) . . ?
C59 N2 C61 104(3) . . ?
C62 N3 C58 113(3) . . ?
C62 N3 C60 103(3) . . ?
C58 N3 C60 111(3) . . ?
N2 C57 C58 108(2) . . ?
N3 C58 C57 107(2) . . ?
N2 C59 C60 108(3) . . ?
N3 C60 C59 109(3) . . ?
N2 C61 C62 102(3) . . ?
N3 C62 C61 115(3) . . ?
C63 N4 C67 111.0(18) . . ?
C63 N4 C65 114.2(18) . . ?
C67 N4 C65 105.7(17) . . ?
C64 N5 C68 105(2) . . ?
C64 N5 C66 109(2) . . ?
C68 N5 C66 111(3) . . ?
N4 C63 C64 103(2) . . ?
N5 C64 C63 119(3) . . ?
N4 C65 C66 106(2) . . ?
N5 C66 C65 111(2) . . ?
N4 C67 C68 112(2) . . ?
N5 C68 C67 106(2) . . ?
C73 N6 C69 109(2) . . ?
C73 N6 C71 102(2) . . ?
C69 N6 C71 109(2) . . ?
C72 N7 C74 110(3) . . ?
C72 N7 C70 104(3) . . ?
C74 N7 C70 105(3) . . ?
N6 C69 C70 112(3) . . ?
C69 C70 N7 111(3) . . ?
C72 C71 N6 105(2) . . ?
N7 C72 C71 119(3) . . ?
N6 C73 C74 110(2) . . ?
N7 C74 C73 111(2) . . ?
C79 N8 C75 108(3) . . ?
C76 C75 N8 134(3) . . ?
C75 C76 C77 109(3) . . ?
C78 C77 C76 127(3) . . ?
C79 C78 C77 112(3) . . ?
N8 C79 C78 129(3) . . ?
C80 N9 C84 119(3) . . ?
N9 C80 C81 121(3) . . ?
C82 C81 C80 116(3) . . ?
C83 C82 C81 115(3) . . ?
C84 C83 C82 125(3) . . ?
C83 C84 N9 122(3) . . ?
C89 N10 C85 114(3) . . ?
N10 C85 C86 129(3) . . ?
C85 C86 C87 114(3) . . ?
C88 C87 C86 122(3) . . ?
C87 C88 C89 117(3) . . ?
N10 C89 C88 124(3) . . ?
N8 O14 N9 105.5(11) . . ?
N8 O14 N6 106.6(11) . . ?
N9 O14 N6 141.6(12) . . ?
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 O8 1.759(15) . ?
U1 O7 1.785(17) . ?
U1 O2 2.170(14) . ?
U1 O1 2.278(17) . ?
U1 O3 2.325(14) . ?
U1 O12 2.476(15) . ?
U1 O11 2.537(16) . ?
U1 N1 2.91(3) . ?
U1 U2 5.0287(14) . ?
U1 U2 6.3930(15) 2_776 ?
U1 U1 10.687(2) 2_776 ?
U2 O9 1.788(14) . ?
U2 O10 1.801(17) . ?
U2 O4 2.113(13) . ?
U2 O5 2.179(15) . ?
U2 O13 2.434(13) 2_776 ?
U2 O13 2.491(16) . ?
U2 O11 2.523(16) . ?
U2 U2 4.2549(18) 2_776 ?
O1 C2 1.38(2) . ?
O1 O2 2.77(2) . ?
O1 O6 11.96(2) . ?
O2 C13 1.36(2) . ?
O2 O3 2.92(2) . ?
O2 O2 15.00(3) 2_776 ?
O3 C24 1.37(2) . ?
O3 O4 3.973(18) . ?
O3 O3 12.49(2) 2_776 ?
O4 C35 1.38(2) . ?
O4 O5 2.832(18) . ?
O5 C46 1.34(2) . ?
O5 O6 3.95(2) . ?
O5 O1 5.233(19) 2_776 ?
O5 O5 7.38(3) 2_776 ?
O6 C55 1.37(2) . ?
O6 C56 1.40(2) . ?
O11 N1 1.43(3) . ?
O12 N1 1.24(3) . ?
O13 N1 1.33(3) . ?
O13 U2 2.434(13) 2_776 ?
C1 C2 1.39(3) . ?
C1 C6 1.43(3) . ?
C1 C56 1.51(3) 2_776 ?
C2 C3 1.45(3) . ?
C3 C4 1.41(3) . ?
C3 C11 1.47(3) . ?
C4 C5 1.39(3) . ?
C5 C6 1.40(3) . ?
C5 C7 1.48(3) . ?
C7 C10 1.51(3) . ?
C7 C8 1.52(6) . ?
C7 C9 1.56(3) . ?
C11 C12 1.51(3) . ?
C12 C13 1.36(3) . ?
C12 C17 1.37(3) . ?
C13 C14 1.42(3) . ?
C14 C15 1.35(3) . ?
C14 C22 1.44(3) . ?
C15 C16 1.52(3) . ?
C16 C17 1.37(3) . ?
C16 C18 1.58(3) . ?
C18 C21 1.47(4) . ?
C18 C19 1.52(3) . ?
C18 C20 1.51(3) . ?
C22 C23 1.52(3) . ?
C23 C24 1.39(3) . ?
C23 C28 1.39(3) . ?
C24 C25 1.40(3) . ?
C25 C26 1.35(3) . ?
C25 C33 1.50(3) . ?
C26 C27 1.49(3) . ?
C27 C28 1.35(3) . ?
C27 C29 1.51(3) . ?
C29 C30 1.50(4) . ?
C29 C31 1.50(3) . ?
C29 C32 1.50(4) . ?
C33 C34 1.57(3) . ?
C34 C35 1.39(2) . ?
C34 C39 1.43(3) . ?
C35 C36 1.38(3) . ?
C36 C37 1.32(2) . ?
C36 C44 1.55(3) . ?
C37 C38 1.42(3) . ?
C38 C39 1.36(3) . ?
C38 C40 1.48(4) . ?
C40 C42 1.47(3) . ?
C40 C41 1.47(4) . ?
C40 C43 1.48(4) . ?
C44 C45 1.54(3) . ?
C45 C46 1.34(3) . ?
C45 C50 1.38(3) . ?
C46 C47 1.42(3) . ?
C47 C48 1.46(3) . ?
C47 C55 1.54(3) . ?
C48 C49 1.37(3) . ?
C49 C50 1.42(3) . ?
C49 C51 1.56(4) . ?
C51 C54 1.49(3) . ?
C51 C53 1.52(4) . ?
C51 C52 1.55(3) . ?
C56 C1 1.51(3) 2_776 ?
N2 C57 1.38(3) . ?
N2 C59 1.40(3) . ?
N2 C61 1.53(3) . ?
N3 C62 1.40(4) . ?
N3 C58 1.44(3) . ?
N3 C60 1.50(4) . ?
C57 C58 1.63(4) . ?
C59 C60 1.57(4) . ?
C61 C62 1.57(4) . ?
N4 C63 1.47(3) . ?
N4 C67 1.49(2) . ?
N4 C65 1.51(3) . ?
N5 C64 1.45(3) . ?
N5 C68 1.48(3) . ?
N5 C66 1.49(3) . ?
C63 C64 1.50(3) . ?
C65 C66 1.58(3) . ?
C67 C68 1.53(3) . ?
N6 C73 1.48(3) . ?
N6 C69 1.50(3) . ?
N6 C71 1.52(3) . ?
N6 O14 2.81(3) . ?
N7 C72 1.36(3) . ?
N7 C74 1.41(3) . ?
N7 C70 1.56(4) . ?
C69 C70 1.48(3) . ?
C71 C72 1.53(4) . ?
C73 C74 1.54(4) . ?
N8 C79 1.35(3) . ?
N8 C75 1.37(4) . ?
N8 O14 2.65(4) . ?
C75 C76 1.33(4) . ?
C76 C77 1.40(4) . ?
C77 C78 1.38(4) . ?
C78 C79 1.38(5) . ?
N9 C80 1.35(3) . ?
N9 C84 1.34(3) . ?
N9 O14 2.77(3) . ?
C80 C81 1.46(4) . ?
C81 C82 1.43(4) . ?
C82 C83 1.41(4) . ?
C83 C84 1.28(4) . ?
N10 C89 1.31(3) . ?
N10 C85 1.33(3) . ?
C85 C86 1.31(3) . ?
C86 C87 1.45(4) . ?
C87 C88 1.26(4) . ?
C88 C89 1.43(4) . ?
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
N2 H2 O1 0.91 1.73 2.64(3) 175.4 .
N4 H4 O3 0.91 1.76 2.67(2) 178.6 .
