#------------------------------------------------------------------------------
#$Date: 2015-09-06 00:34:46 +0300 (Sun, 06 Sep 2015) $
#$Revision: 154600 $
#$URL: svn://www.crystallography.net/cod/cif/4/34/34/4343413.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_4343413
loop_
_publ_author_name
'Thuéry, Pierre'
'Harrowfield, Jack'
_publ_section_title
;
 Uranyl Ion Complexes with 1,1'-Biphenyl-2,2',6,6'-tetracarboxylic Acid:
 Structural and Spectroscopic Studies of One- to Three-Dimensional
 Assemblies.
;
_journal_issue                   13
_journal_name_full               'Inorganic chemistry'
_journal_page_first              6296
_journal_page_last               6305
_journal_paper_doi               10.1021/acs.inorgchem.5b00596
_journal_volume                  54
_journal_year                    2015
_chemical_formula_sum            'C96 H74 Dy I O80 U8'
_chemical_formula_weight         4701.19
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 107.986(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   30.5301(7)
_cell_length_b                   15.9030(7)
_cell_length_c                   29.9686(10)
_cell_measurement_reflns_used    245741
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      2.93
_cell_volume                     13839.3(8)
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material
'SHELXTL (Sheldrick, 2008); PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type
'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method
'two φ and seven ω scans with 2° steps (548 frames)'
_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  0.0337
_diffrn_reflns_av_unetI/netI     0.0448
_diffrn_reflns_laue_measured_fraction_full 0.997
_diffrn_reflns_laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            245741
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.681
_diffrn_reflns_theta_min         2.933
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    10.182
_exptl_absorpt_correction_T_max  0.665
_exptl_absorpt_correction_T_min  0.456
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            'translucent light yellow'
_exptl_crystal_density_diffrn    2.256
_exptl_crystal_description       needle
_exptl_crystal_F_000             8580
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.858
_refine_diff_density_min         -3.931
_refine_diff_density_rms         0.300
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     901
_refine_ls_number_reflns         13110
_refine_ls_number_restraints     95
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0668
_refine_ls_R_factor_gt           0.0488
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0832P)²+278.5143P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1383
_refine_ls_wR_factor_ref         0.1471
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10363
_reflns_number_total             13110
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic5b00596_si_002.cif
_cod_data_source_block           6
_cod_depositor_comments
'Adding full bibliography for 4343408--4343413.cif.'
_cod_database_code               4343413
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelxl_version_number           2014-3
loop_
_space_group_symop_operation_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'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
U1 U 0.22628(2) 0.73009(3) 0.77263(2) 0.03278(13) Uani 1 1 d . . .
U2 U 0.23849(2) 0.67059(3) 0.57186(2) 0.02535(12) Uani 1 1 d . . .
U3 U 0.42283(2) 0.66355(3) 0.76361(2) 0.02583(12) Uani 1 1 d . . .
U4 U 0.47956(2) 0.97535(3) 0.57560(2) 0.02818(12) Uani 1 1 d . . .
Dy1 Dy -0.01467(4) 0.66536(7) 0.73986(4) 0.0342(3) Uani 0.5 1 d . . P
I1 I 0.26116(12) 0.7979(2) 1.01493(11) 0.1070(10) Uani 0.5 1 d . . P
O1 O 0.2043(3) 0.6428(7) 0.7954(3) 0.052(2) Uani 1 1 d . . .
O2 O 0.2478(3) 0.8183(5) 0.7514(3) 0.046(2) Uani 1 1 d . . .
O3 O 0.2325(2) 0.7507(5) 0.6097(2) 0.0295(17) Uani 1 1 d . . .
O4 O 0.2452(3) 0.5907(5) 0.5340(3) 0.0377(19) Uani 1 1 d . . .
O5 O 0.3932(3) 0.7550(5) 0.7701(3) 0.0329(17) Uani 1 1 d . . .
O6 O 0.4531(3) 0.5712(5) 0.7576(3) 0.0357(18) Uani 1 1 d . . .
O7 O 0.4468(3) 1.0600(5) 0.5428(3) 0.0361(18) Uani 1 1 d . . .
O8 O 0.5127(3) 0.8930(6) 0.6081(3) 0.039(2) Uani 1 1 d . . .
O9 O 0.1461(3) 0.7736(6) 0.7207(3) 0.042(2) Uani 1 1 d . . .
O10 O 0.1856(3) 0.6845(5) 0.6931(3) 0.0371(19) Uani 1 1 d . . .
O11 O 0.0363(3) 0.6030(5) 0.4938(2) 0.0313(17) Uani 1 1 d . . .
O12 O 0.0433(2) 0.5220(5) 0.5558(2) 0.0275(16) Uani 1 1 d . . .
O13 O 0.1662(3) 0.6094(5) 0.5740(3) 0.0339(18) Uani 1 1 d . . .
O14 O 0.2276(2) 0.5681(5) 0.6302(3) 0.0331(18) Uani 1 1 d . . .
O15 O 0.0490(3) 0.6211(6) 0.7071(3) 0.049(2) Uani 1 1 d . . .
O16 O 0.0109(3) 0.5760(6) 0.6353(3) 0.044(2) Uani 1 1 d . . .
O17 O 0.2931(2) 0.7537(5) 0.5525(3) 0.0338(19) Uani 1 1 d . . .
O18 O 0.3155(2) 0.7593(6) 0.4886(3) 0.0360(19) Uani 1 1 d . . .
O19 O 0.4468(2) 0.7326(5) 0.7060(2) 0.0310(17) Uani 1 1 d . . .
O20 O 0.5094(3) 0.7163(6) 0.6852(3) 0.040(2) Uani 1 1 d . . .
O21 O 0.3102(2) 0.6231(5) 0.6252(3) 0.0307(17) Uani 1 1 d . . .
O22 O 0.3675(2) 0.6210(5) 0.6905(2) 0.0307(17) Uani 1 1 d . . .
O23 O 0.4331(3) 0.9783(6) 0.6292(3) 0.043(2) Uani 1 1 d . . .
O24 O 0.4100(3) 0.8934(5) 0.5703(3) 0.0362(19) Uani 1 1 d . . .
O25 O 0.4147(2) 0.6110(6) 0.8375(2) 0.0356(19) Uani 1 1 d . . .
O26 O 0.3596(2) 0.5784(5) 0.7733(2) 0.0292(17) Uani 1 1 d . . .
O27 O 0.3114(6) 0.4884(9) 0.9852(5) 0.116(4) Uani 1 1 d D U .
O28 O 0.3543(6) 0.5992(11) 0.9889(6) 0.137(5) Uani 1 1 d D U .
O29 O 0.3038(3) 0.6887(6) 0.8162(3) 0.042(2) Uani 1 1 d . . .
O30 O 0.2741(3) 0.7727(6) 0.8558(3) 0.048(2) Uani 1 1 d . . .
O31 O 0.4742(5) 0.5778(10) 1.0024(6) 0.114(5) Uani 1 1 d . U .
O32 O 0.4463(6) 0.5212(11) 0.9397(7) 0.129(5) Uani 1 1 d D U .
O33 O 0.2685(3) 0.6372(6) 0.7309(3) 0.041(2) Uani 1 1 d . . .
H33A H 0.2513 0.6025 0.7050 0.050 Uiso 1 1 d R U .
H33B H 0.2915 0.6119 0.7489 0.050 Uiso 1 1 d R U .
O34 O 0.1864(4) 0.8204(8) 0.8116(4) 0.081(4) Uani 1 1 d . . .
H34A H 0.2020 0.8733 0.8208 0.098 Uiso 1 1 d R U .
H34B H 0.1835 0.8110 0.8407 0.098 Uiso 1 1 d R U .
O35 O 0.0120(8) 0.7788(14) 0.8016(8) 0.076(6) Uani 0.5 1 d . U P
O36 O -0.0704(9) 0.7649(15) 0.7421(10) 0.084(8) Uani 0.5 1 d . . P
O37 O -0.0314(6) 0.5243(11) 0.7220(6) 0.040(4) Uani 0.5 1 d . . P
O38 O -0.0447(6) 0.5994(13) 0.7015(6) 0.053(5) Uani 0.5 1 d . . P
O39 O 0.3459(8) 1.0446(18) 0.4940(8) 0.090(8) Uani 0.5 1 d . U P
O40 O 0.0721(8) 0.8823(15) 0.7107(8) 0.078(7) Uani 0.5 1 d . . P
H40A H 0.0731 0.9062 0.7409 0.094 Uiso 0.5 1 d R U P
H40B H 0.0411 0.9010 0.6931 0.094 Uiso 0.5 1 d R U P
O41 O 0.3017(9) 0.4735(17) 0.6854(9) 0.089(8) Uani 0.5 1 d . . P
O42 O 0.2851(10) 0.4315(14) 0.6145(8) 0.082(7) Uani 0.5 1 d . U P
O43 O 0.3267(10) 0.4720(16) 0.5784(7) 0.089(8) Uani 0.5 1 d . U P
O44 O 0.3872(9) 0.4342(16) 0.7046(9) 0.088(8) Uani 0.5 1 d . U P
O45 O 0.4825(9) 0.4519(17) 0.8691(9) 0.087(7) Uani 0.5 1 d . U P
O46 O 0.1481(9) 0.726(2) 0.8778(8) 0.099(9) Uani 0.5 1 d . . P
C1 C 0.0980(3) 0.6546(7) 0.6148(4) 0.025(2) Uani 1 1 d . . .
C2 C 0.1131(3) 0.7294(7) 0.6400(4) 0.029(2) Uani 1 1 d . . .
C3 C 0.0989(4) 0.8074(8) 0.6213(5) 0.046(3) Uani 1 1 d . . .
H3 H 0.1075 0.8565 0.6400 0.055 Uiso 1 1 calc R U .
C4 C 0.0717(5) 0.8131(9) 0.5745(5) 0.051(4) Uani 1 1 d . . .
H4 H 0.0623 0.8669 0.5613 0.061 Uiso 1 1 calc R U .
C5 C 0.0584(4) 0.7435(8) 0.5476(4) 0.036(3) Uani 1 1 d . . .
H5 H 0.0421 0.7488 0.5152 0.043 Uiso 1 1 calc R U .
C6 C 0.0689(3) 0.6637(7) 0.5680(3) 0.026(2) Uani 1 1 d . . .
C7 C 0.1491(4) 0.7274(7) 0.6870(4) 0.032(3) Uani 1 1 d . . .
C8 C 0.0492(3) 0.5908(7) 0.5377(4) 0.027(2) Uani 1 1 d . . .
C9 C 0.1127(3) 0.5730(7) 0.6386(3) 0.024(2) Uani 1 1 d . . .
C10 C 0.1541(4) 0.5351(7) 0.6384(3) 0.028(2) Uani 1 1 d . . .
C11 C 0.1705(4) 0.4633(8) 0.6671(4) 0.037(3) Uani 1 1 d . . .
H11 H 0.1991 0.4388 0.6678 0.044 Uiso 1 1 calc R U .
C12 C 0.1456(4) 0.4289(8) 0.6936(4) 0.041(3) Uani 1 1 d . . .
H12 H 0.1558 0.3790 0.7112 0.049 Uiso 1 1 calc R U .
C13 C 0.1057(4) 0.4681(9) 0.6943(4) 0.044(3) Uani 1 1 d . . .
H13 H 0.0886 0.4456 0.7132 0.053 Uiso 1 1 calc R U .
C14 C 0.0896(4) 0.5407(8) 0.6675(3) 0.032(3) Uani 1 1 d . . .
C15 C 0.1834(3) 0.5716(7) 0.6130(3) 0.024(2) Uani 1 1 d . . .
C16 C 0.0465(4) 0.5822(7) 0.6700(4) 0.031(3) Uani 1 1 d . . .
C17 C 0.3933(3) 0.7330(7) 0.6050(3) 0.023(2) Uani 1 1 d . . .
C18 C 0.3710(3) 0.7125(7) 0.5580(4) 0.025(2) Uani 1 1 d . . .
C19 C 0.3925(4) 0.6639(8) 0.5325(4) 0.033(3) Uani 1 1 d . . .
H19 H 0.3769 0.6508 0.5006 0.040 Uiso 1 1 calc R U .
C20 C 0.4363(5) 0.6347(9) 0.5535(4) 0.048(3) Uani 1 1 d . . .
H20 H 0.4509 0.6013 0.5360 0.057 Uiso 1 1 calc R U .
C21 C 0.4589(4) 0.6530(8) 0.5988(4) 0.037(3) Uani 1 1 d . . .
H21 H 0.4890 0.6315 0.6130 0.044 Uiso 1 1 calc R U .
C22 C 0.4381(4) 0.7034(8) 0.6250(4) 0.029(2) Uani 1 1 d . . .
C23 C 0.3238(3) 0.7440(7) 0.5315(4) 0.028(2) Uani 1 1 d . . .
C24 C 0.4663(3) 0.7188(7) 0.6757(4) 0.029(2) Uani 1 1 d . . .
C25 C 0.3709(3) 0.7903(7) 0.6316(3) 0.023(2) Uani 1 1 d . . .
C26 C 0.3439(3) 0.7559(7) 0.6560(3) 0.024(2) Uani 1 1 d . . .
C27 C 0.3221(4) 0.8054(9) 0.6816(4) 0.035(3) Uani 1 1 d . . .
H27 H 0.3042 0.7801 0.6989 0.042 Uiso 1 1 calc R U .
C28 C 0.3273(4) 0.8935(7) 0.6812(4) 0.030(2) Uani 1 1 d . . .
H28 H 0.3117 0.9287 0.6969 0.037 Uiso 1 1 calc R U .
C29 C 0.3549(4) 0.9276(8) 0.6580(4) 0.033(3) Uani 1 1 d . . .
H29 H 0.3592 0.9868 0.6587 0.040 Uiso 1 1 calc R U .
C30 C 0.3775(3) 0.8770(7) 0.6330(3) 0.028(2) Uani 1 1 d . . .
C31 C 0.3397(3) 0.6615(7) 0.6576(3) 0.024(2) Uani 1 1 d . . .
C32 C 0.4085(3) 0.9179(8) 0.6098(4) 0.030(2) Uani 1 1 d . . .
C33 C 0.3504(4) 0.5660(7) 0.8900(4) 0.030(2) Uani 1 1 d . . .
C34 C 0.3489(3) 0.5346(7) 0.8456(4) 0.027(2) Uani 1 1 d . . .
C35 C 0.3225(4) 0.4667(7) 0.8261(4) 0.032(3) Uani 1 1 d . . .
H35 H 0.3211 0.4487 0.7954 0.039 Uiso 1 1 calc R U .
C36 C 0.2979(4) 0.4238(8) 0.8508(4) 0.038(3) Uani 1 1 d . . .
H36 H 0.2799 0.3761 0.8374 0.046 Uiso 1 1 calc R U .
C37 C 0.2998(5) 0.4514(9) 0.8954(5) 0.046(3) Uani 1 1 d . . .
H37 H 0.2838 0.4213 0.9129 0.056 Uiso 1 1 calc R U .
C38 C 0.3247(6) 0.5221(10) 0.9144(5) 0.061(3) Uani 1 1 d D U .
C39 C 0.3758(4) 0.5773(7) 0.8183(4) 0.029(2) Uani 1 1 d . . .
C40 C 0.3259(7) 0.5472(11) 0.9635(4) 0.093(4) Uani 1 1 d D U .
C41 C 0.3741(3) 0.6475(7) 0.9088(3) 0.024(2) Uani 1 1 d . . .
C42 C 0.3513(4) 0.7235(7) 0.8944(4) 0.031(3) Uani 1 1 d . . .
C43 C 0.3693(5) 0.7979(8) 0.9143(4) 0.044(3) Uani 1 1 d . . .
H43 H 0.3525 0.8484 0.9045 0.052 Uiso 1 1 calc R U .
C44 C 0.4124(5) 0.8012(10) 0.9492(5) 0.058(4) Uani 1 1 d . . .
H44 H 0.4255 0.8534 0.9621 0.070 Uiso 1 1 calc R U .
C45 C 0.4352(5) 0.7269(9) 0.9643(4) 0.048(3) Uani 1 1 d . . .
H45 H 0.4639 0.7276 0.9885 0.058 Uiso 1 1 calc R U .
C46 C 0.4166(4) 0.6511(8) 0.9446(4) 0.032(3) Uani 1 1 d . . .
C47 C 0.3065(4) 0.7275(8) 0.8544(4) 0.035(3) Uani 1 1 d . . .
C48 C 0.4432(7) 0.5822(14) 0.9647(7) 0.099(5) Uani 1 1 d 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'
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'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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
O2 U1 O1 178.3(4) . .
O2 U1 O34 90.0(5) . .
O1 U1 O34 88.4(5) . .
O2 U1 O29 90.0(4) . .
O1 U1 O29 90.2(4) . .
O34 U1 O29 117.3(3) . .
O2 U1 O10 91.1(4) . .
O1 U1 O10 90.2(3) . .
O34 U1 O10 118.2(3) . .
O29 U1 O10 124.5(3) . .
O2 U1 O33 89.1(4) . .
O1 U1 O33 92.5(4) . .
O34 U1 O33 179.1(4) . .
O29 U1 O33 62.9(3) . .
O10 U1 O33 61.7(3) . .
O2 U1 O30 88.6(4) . .
O1 U1 O30 90.2(4) . .
O34 U1 O30 65.8(3) . .
O29 U1 O30 51.5(3) . .
O10 U1 O30 176.0(3) . .
O33 U1 O30 114.3(3) . .
O2 U1 O9 87.6(3) . .
O1 U1 O9 92.3(4) . .
O34 U1 O9 66.5(3) . .
O29 U1 O9 175.5(3) . .
O10 U1 O9 51.8(3) . .
O33 U1 O9 113.3(2) . .
O30 U1 O9 132.2(3) . .
O3 U2 O4 179.2(4) . .
O3 U2 O18 88.0(3) . 7_566
O4 U2 O18 92.2(3) . 7_566
O3 U2 O17 88.6(3) . .
O4 U2 O17 90.7(3) . .
O18 U2 O17 85.6(3) 7_566 .
O3 U2 O21 93.1(3) . .
O4 U2 O21 86.5(3) . .
O18 U2 O21 162.2(3) 7_566 .
O17 U2 O21 76.7(3) . .
O3 U2 O13 89.8(3) . .
O4 U2 O13 90.9(3) . .
O18 U2 O13 77.4(3) 7_566 .
O17 U2 O13 163.0(3) . .
O21 U2 O13 120.3(3) . .
O3 U2 O14 87.6(3) . .
O4 U2 O14 92.8(3) . .
O18 U2 O14 130.3(2) 7_566 .
O17 U2 O14 143.7(2) . .
O21 U2 O14 67.5(2) . .
O13 U2 O14 53.1(2) . .
O5 U3 O6 179.5(4) . .
O5 U3 O20 90.7(3) . 2_656
O6 U3 O20 88.9(3) . 2_656
O5 U3 O19 89.0(3) . .
O6 U3 O19 91.3(3) . .
O20 U3 O19 84.2(3) 2_656 .
O5 U3 O22 95.3(3) . .
O6 U3 O22 85.1(3) . .
O20 U3 O22 158.9(3) 2_656 .
O19 U3 O22 75.7(3) . .
O5 U3 O26 89.5(3) . .
O6 U3 O26 90.5(3) . .
O20 U3 O26 134.2(3) 2_656 .
O19 U3 O26 141.6(2) . .
O22 U3 O26 66.2(2) . .
O5 U3 O25 89.0(3) . .
O6 U3 O25 90.6(3) . .
O20 U3 O25 81.0(3) 2_656 .
O19 U3 O25 165.1(3) . .
O22 U3 O25 119.2(3) . .
O26 U3 O25 53.2(2) . .
O8 U4 O7 179.0(4) . .
O8 U4 O12 89.7(3) . 3
O7 U4 O12 89.4(3) . 3
O8 U4 O11 91.2(3) . 7_566
O7 U4 O11 89.2(3) . 7_566
O12 U4 O11 84.4(2) 3 7_566
O8 U4 O16 93.2(4) . 3
O7 U4 O16 86.1(4) . 3
O12 U4 O16 78.6(3) 3 3
O11 U4 O16 162.4(3) 7_566 3
O8 U4 O23 90.1(4) . .
O7 U4 O23 90.3(3) . .
O12 U4 O23 149.5(3) 3 .
O11 U4 O23 126.1(3) 7_566 .
O16 U4 O23 70.9(3) 3 .
O8 U4 O24 88.8(3) . .
O7 U4 O24 92.2(3) . .
O12 U4 O24 158.2(2) 3 .
O11 U4 O24 73.9(2) 7_566 .
O16 U4 O24 123.2(3) 3 .
O23 U4 O24 52.3(3) . .
O38 Dy1 O35 104.0(9) . 2_556
O38 Dy1 O15 90.7(7) . 2_556
O35 Dy1 O15 138.9(7) 2_556 2_556
O35 Dy1 O37 134.6(7) 2_556 .
O15 Dy1 O37 75.3(5) 2_556 .
O38 Dy1 O36 101.6(10) . .
O35 Dy1 O36 67.5(8) 2_556 .
O15 Dy1 O36 72.1(6) 2_556 .
O37 Dy1 O36 123.3(8) . .
O38 Dy1 O38 112.3(12) . 2_556
O35 Dy1 O38 129.3(8) 2_556 2_556
O15 Dy1 O38 75.8(5) 2_556 2_556
O37 Dy1 O38 78.8(7) . 2_556
O36 Dy1 O38 133.0(9) . 2_556
O38 Dy1 O35 165.0(9) . .
O35 Dy1 O35 76.7(11) 2_556 .
O15 Dy1 O35 79.8(6) 2_556 .
O37 Dy1 O35 148.6(6) . .
O36 Dy1 O35 64.5(10) . .
O38 Dy1 O35 76.8(7) 2_556 .
O38 Dy1 O15 83.1(7) . .
O35 Dy1 O15 80.9(7) 2_556 .
O15 Dy1 O15 139.6(4) 2_556 .
O37 Dy1 O15 77.5(5) . .
O36 Dy1 O15 148.3(6) . .
O38 Dy1 O15 70.0(5) 2_556 .
O35 Dy1 O15 111.7(6) . .
O38 Dy1 O37 82.5(9) . 2_556
O35 Dy1 O37 144.2(7) 2_556 2_556
O15 Dy1 O37 74.9(4) 2_556 2_556
O36 Dy1 O37 146.7(7) . 2_556
O35 Dy1 O37 105.9(6) . 2_556
O15 Dy1 O37 64.7(4) . 2_556
C7 O9 U1 92.1(6) . .
C7 O10 U1 98.1(7) . .
C8 O11 U4 138.8(7) . 7_566
C8 O12 U4 129.1(6) . 3_445
C15 O13 U2 95.3(6) . .
C15 O14 U2 92.4(6) . .
C16 O15 Dy1 149.2(8) . 2_556
C16 O15 Dy1 129.5(7) . .
C16 O16 U4 136.3(8) . 3_445
C23 O17 U2 137.3(8) . .
C23 O18 U2 139.7(7) . 7_566
C24 O19 U3 141.2(7) . .
C24 O20 U3 145.0(8) . 2_656
C31 O21 U2 130.5(7) . .
C31 O22 U3 132.8(7) . .
C32 O23 U4 93.8(7) . .
C32 O24 U4 93.3(6) . .
C39 O25 U3 94.3(6) . .
C39 O26 U3 93.9(6) . .
C47 O29 U1 97.7(7) . .
C47 O30 U1 92.1(7) . .
U1 O33 H33A 119.9 . .
U1 O33 H33B 114.4 . .
H33A O33 H33B 112.3 . .
U1 O34 H34A 112.4 . .
U1 O34 H34B 125.3 . .
H34A O34 H34B 93.1 . .
H40A O40 H40B 97.4 . .
C2 C1 C6 116.5(10) . .
C2 C1 C9 118.8(9) . .
C6 C1 C9 124.7(9) . .
C3 C2 C1 122.3(10) . .
C3 C2 C7 116.7(10) . .
C1 C2 C7 120.7(10) . .
C2 C3 C4 118.9(11) . .
C2 C3 H3 120.6 . .
C4 C3 H3 120.6 . .
C5 C4 C3 121.4(12) . .
C5 C4 H4 119.3 . .
C3 C4 H4 119.3 . .
C4 C5 C6 119.6(11) . .
C4 C5 H5 120.2 . .
C6 C5 H5 120.2 . .
C5 C6 C1 120.8(10) . .
C5 C6 C8 116.6(9) . .
C1 C6 C8 122.7(10) . .
O10 C7 O9 118.0(10) . .
O10 C7 C2 120.2(10) . .
O9 C7 C2 121.5(10) . .
O12 C8 O11 122.7(10) . .
O12 C8 C6 120.0(9) . .
O11 C8 C6 117.0(10) . .
C14 C9 C10 118.8(10) . .
C14 C9 C1 119.5(10) . .
C10 C9 C1 120.9(9) . .
C9 C10 C11 119.4(10) . .
C9 C10 C15 121.9(9) . .
C11 C10 C15 118.4(10) . .
C12 C11 C10 121.0(12) . .
C12 C11 H11 119.5 . .
C10 C11 H11 119.5 . .
C11 C12 C13 118.6(11) . .
C11 C12 H12 120.7 . .
C13 C12 H12 120.7 . .
C12 C13 C14 121.4(11) . .
C12 C13 H13 119.3 . .
C14 C13 H13 119.3 . .
C9 C14 C13 120.6(11) . .
C9 C14 C16 119.9(10) . .
C13 C14 C16 119.5(10) . .
O13 C15 O14 118.1(9) . .
O13 C15 C10 121.3(9) . .
O14 C15 C10 120.6(9) . .
O15 C16 O16 125.1(11) . .
O15 C16 C14 116.6(10) . .
O16 C16 C14 118.3(10) . .
C22 C17 C18 117.4(10) . .
C22 C17 C25 121.6(9) . .
C18 C17 C25 120.9(9) . .
C19 C18 C17 121.2(9) . .
C19 C18 C23 115.9(9) . .
C17 C18 C23 122.9(10) . .
C20 C19 C18 119.8(11) . .
C20 C19 H19 120.1 . .
C18 C19 H19 120.1 . .
C21 C20 C19 120.7(11) . .
C21 C20 H20 119.6 . .
C19 C20 H20 119.6 . .
C20 C21 C22 120.4(11) . .
C20 C21 H21 119.8 . .
C22 C21 H21 119.8 . .
C17 C22 C21 120.4(10) . .
C17 C22 C24 123.6(10) . .
C21 C22 C24 115.9(9) . .
O18 C23 O17 121.9(9) . .
O18 C23 C18 117.6(9) . .
O17 C23 C18 120.5(9) . .
O19 C24 O20 122.7(10) . .
O19 C24 C22 120.4(9) . .
O20 C24 C22 117.0(10) . .
C26 C25 C30 118.9(10) . .
C26 C25 C17 119.1(10) . .
C30 C25 C17 122.0(9) . .
C25 C26 C27 122.2(11) . .
C25 C26 C31 118.9(9) . .
C27 C26 C31 118.8(10) . .
C26 C27 C28 118.5(11) . .
C26 C27 H27 120.8 . .
C28 C27 H27 120.8 . .
C29 C28 C27 119.4(11) . .
C29 C28 H28 120.3 . .
C27 C28 H28 120.3 . .
C28 C29 C30 121.6(11) . .
C28 C29 H29 119.2 . .
C30 C29 H29 119.2 . .
C25 C30 C29 119.3(9) . .
C25 C30 C32 121.8(10) . .
C29 C30 C32 118.9(10) . .
O21 C31 O22 120.2(10) . .
O21 C31 C26 120.4(9) . .
O22 C31 C26 119.3(9) . .
O23 C32 O24 119.0(10) . .
O23 C32 C30 119.8(10) . .
O24 C32 C30 121.2(10) . .
C38 C33 C34 116.9(11) . .
C38 C33 C41 120.8(10) . .
C34 C33 C41 122.0(9) . .
C35 C34 C33 121.9(10) . .
C35 C34 C39 118.5(10) . .
C33 C34 C39 119.6(10) . .
C34 C35 C36 120.3(11) . .
C34 C35 H35 119.8 . .
C36 C35 H35 119.8 . .
C35 C36 C37 119.3(11) . .
C35 C36 H36 120.3 . .
C37 C36 H36 120.3 . .
C38 C37 C36 120.5(11) . .
C38 C37 H37 119.7 . .
C36 C37 H37 119.7 . .
C37 C38 C33 121.0(11) . .
C37 C38 C40 117.3(11) . .
C33 C38 C40 121.6(12) . .
O25 C39 O26 118.5(9) . .
O25 C39 C34 122.7(10) . .
O26 C39 C34 118.8(9) . .
O28 C40 O27 116.6(11) . .
O28 C40 C38 124.0(14) . .
O27 C40 C38 112.9(13) . .
C42 C41 C46 117.2(10) . .
C42 C41 C33 119.5(9) . .
C46 C41 C33 123.0(10) . .
C43 C42 C41 121.3(10) . .
C43 C42 C47 117.0(11) . .
C41 C42 C47 121.7(10) . .
C42 C43 C44 121.1(12) . .
C42 C43 H43 119.5 . .
C44 C43 H43 119.5 . .
C45 C44 C43 118.3(13) . .
C45 C44 H44 120.8 . .
C43 C44 H44 120.8 . .
C44 C45 C46 120.7(12) . .
C44 C45 H45 119.6 . .
C46 C45 H45 119.6 . .
C45 C46 C48 113.4(13) . .
C45 C46 C41 121.3(11) . .
C48 C46 C41 125.3(14) . .
O30 C47 O29 118.6(10) . .
O30 C47 C42 122.4(10) . .
O29 C47 C42 118.7(10) . .
O31 C48 O32 109.1(19) . .
O31 C48 C46 129(2) . .
O32 C48 C46 119.7(19) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 O2 1.749(9) .
U1 O1 1.768(10) .
U1 O34 2.405(10) .
U1 O29 2.414(8) .
U1 O10 2.434(7) .
U1 O33 2.529(8) .
U1 O30 2.559(8) .
U1 O9 2.559(8) .
U2 O3 1.753(8) .
U2 O4 1.758(8) .
U2 O18 2.323(7) 7_566
U2 O17 2.338(7) .
U2 O21 2.399(7) .
U2 O13 2.431(7) .
U2 O14 2.486(7) .
U3 O5 1.756(8) .
U3 O6 1.773(8) .
U3 O20 2.319(8) 2_656
U3 O19 2.347(7) .
U3 O22 2.414(7) .
U3 O26 2.448(7) .
U3 O25 2.451(7) .
U4 O8 1.755(8) .
U4 O7 1.780(8) .
U4 O12 2.326(7) 3
U4 O11 2.343(7) 7_566
U4 O16 2.370(8) 3
U4 O23 2.450(8) .
U4 O24 2.454(7) .
Dy1 O35 2.21(2) 2_556
Dy1 O15 2.270(9) 2_556
Dy1 O37 2.326(16) .
Dy1 O36 2.34(2) .
Dy1 O38 2.346(17) 2_556
Dy1 O35 2.53(2) .
Dy1 O15 2.533(9) .
Dy1 O37 2.706(15) 2_556
O9 C7 1.275(13) .
O10 C7 1.271(13) .
O11 C8 1.266(12) .
O11 U4 2.343(7) 7_566
O12 C8 1.258(13) .
O12 U4 2.326(7) 3_445
O13 C15 1.274(12) .
O14 C15 1.288(12) .
O15 C16 1.252(14) .
O15 Dy1 2.269(9) 2_556
O16 C16 1.256(13) .
O16 U4 2.370(8) 3_445
O17 C23 1.287(13) .
O18 C23 1.256(12) .
O18 U2 2.323(7) 7_566
O19 C24 1.250(13) .
O20 C24 1.257(13) .
O20 U3 2.319(8) 2_656
O21 C31 1.260(13) .
O22 C31 1.262(12) .
O23 C32 1.246(14) .
O24 C32 1.261(13) .
O25 C39 1.267(13) .
O26 C39 1.285(13) .
O27 C40 1.291(9) .
O28 C40 1.268(9) .
O29 C47 1.282(14) .
O30 C47 1.235(14) .
O31 C48 1.23(2) .
O32 C48 1.248(10) .
O33 H33A 0.9650 .
O33 H33B 0.8436 .
O34 H34A 0.9645 .
O34 H34B 0.9160 .
O35 Dy1 2.21(2) 2_556
O37 Dy1 2.706(15) 2_556
O38 Dy1 2.346(17) 2_556
O40 H40A 0.9738 .
O40 H40B 0.9789 .
C1 C2 1.407(15) .
C1 C6 1.417(14) .
C1 C9 1.482(15) .
C2 C3 1.373(17) .
C2 C7 1.496(14) .
C3 C4 1.394(17) .
C3 H3 0.9500 .
C4 C5 1.355(18) .
C4 H4 0.9500 .
C5 C6 1.402(16) .
C5 H5 0.9500 .
C6 C8 1.481(15) .
C9 C14 1.376(14) .
C9 C10 1.403(15) .
C10 C11 1.424(16) .
C10 C15 1.462(15) .
C11 C12 1.373(17) .
C11 H11 0.9500 .
C12 C13 1.375(19) .
C12 H12 0.9500 .
C13 C14 1.405(18) .
C13 H13 0.9500 .
C14 C16 1.494(17) .
C17 C22 1.395(14) .
C17 C18 1.402(14) .
C17 C25 1.506(14) .
C18 C19 1.385(15) .
C18 C23 1.500(14) .
C19 C20 1.371(17) .
C19 H19 0.9500 .
C20 C21 1.351(17) .
C20 H20 0.9500 .
C21 C22 1.403(16) .
C21 H21 0.9500 .
C22 C24 1.518(15) .
C25 C26 1.372(14) .
C25 C30 1.393(16) .
C26 C27 1.403(16) .
C26 C31 1.508(15) .
C27 C28 1.412(17) .
C27 H27 0.9500 .
C28 C29 1.358(16) .
C28 H28 0.9500 .
C29 C30 1.415(16) .
C29 H29 0.9500 .
C30 C32 1.487(14) .
C33 C38 1.410(16) .
C33 C34 1.410(15) .
C33 C41 1.506(15) .
C34 C35 1.366(16) .
C34 C39 1.492(14) .
C35 C36 1.387(16) .
C35 H35 0.9500 .
C36 C37 1.391(17) .
C36 H36 0.9500 .
C37 C38 1.379(18) .
C37 H37 0.9500 .
C38 C40 1.515(9) .
C41 C42 1.396(16) .
C41 C46 1.406(15) .
C42 C43 1.363(17) .
C42 C47 1.514(15) .
C43 C44 1.407(18) .
C43 H43 0.9500 .
C44 C45 1.37(2) .
C44 H44 0.9500 .
C45 C46 1.384(18) .
C45 H45 0.9500 .
C46 C48 1.39(2) .
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
O33 H33A O14 0.97 2.20 3.091(11) 152.7 .
O33 H33B O26 0.84 2.05 2.835(10) 154.7 .
O34 H34A O41 0.96 1.60 2.46(3) 145.3 4_556
O34 H34A O42 0.96 2.07 2.76(2) 126.3 4_556
O34 H34B O46 0.92 2.23 3.00(3) 141.0 .
O40 H40A O44 0.97 1.76 2.59(4) 140.7 4_556
O40 H40B O45 0.98 1.95 2.69(4) 130.6 4_556
