#------------------------------------------------------------------------------
#$Date: 2016-03-23 22:00:51 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179462 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/59/4335925.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_4335925
loop_
_publ_author_name
'Daniel K. Unruh'
'Kyle Gojdas'
'Erin Flores'
'Anna Libo'
'Tori Z. Forbes'
_publ_contact_author_address
;Department of Chemistry
W374 Chemistry Building
The University of Iowa
Iowa City, IA 52242-1294
USA
;
_publ_contact_author_fax         1-319-335-1270
_publ_contact_author_name        'Forbes, Tori M.'
_publ_contact_author_phone       1-319-384-1908
_publ_section_title
;
 Synthesis and Structural Characterization of Hydrolysis Products within
 the Uranyl Iminodiacetate and Malate Systems
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10191
_journal_page_last               10198
_journal_paper_doi               10.1021/ic401705j
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C12 H9 K O24 U3, 2(C4 H12 N2), 4(O)'
_chemical_formula_sum            'C20 H31 K N4 O28 U3'
_chemical_formula_weight         1528.68
_chemical_name_systematic
;
 ?
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-07-01T08:26:53-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 112.596(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.7851(15)
_cell_length_b                   20.5105(12)
_cell_length_c                   16.5578(9)
_cell_measurement_reflns_used    9814
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.06
_cell_measurement_theta_min      2.39
_cell_volume                     7771.1(8)
_computing_cell_refinement       'APEX2 (Bruker AXS, 2006)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'APEX2 (Bruker AXS, 2006)'
_computing_molecular_graphics    'CrystalMaker v2.5.0'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.034
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            66506
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         1.333
_exptl_absorpt_coefficient_mu    12.682
_exptl_absorpt_correction_T_max  0.522
_exptl_absorpt_correction_T_min  0.183
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.613
_exptl_crystal_description       plate
_exptl_crystal_F_000             5584
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.217
_refine_diff_density_min         -1.171
_refine_diff_density_rms         0.148
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     534
_refine_ls_number_reflns         6845
_refine_ls_number_restraints     46
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0484
_refine_ls_R_factor_gt           0.0381
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[σ²(Fo²)+(0.0543P)²+137.6764P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1039
_refine_ls_wR_factor_ref         0.1111
_reflns_number_gt                5905
_reflns_number_total             6845
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic401705j_si_003.cif
_cod_data_source_block           c2c
_cod_database_code               4335925
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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
U1A U 0.2796(3) -0.0382(2) 0.2202(3) 0.0312(6) Uani 0.612(10) d A .
U2A U 0.18679(11) 0.11371(10) 0.14042(16) 0.0291(3) Uani 0.612(10) d A .
U3A U 0.34934(14) 0.12855(17) 0.26754(17) 0.0288(4) Uani 0.612(10) d A .
U1B U 0.2718(4) -0.0350(3) 0.2119(5) 0.0351(13) Uani 0.388(10) d A .
U2B U 0.2005(2) 0.1291(3) 0.1519(3) 0.0415(8) Uani 0.388(10) d A .
U3B U 0.3629(3) 0.1200(3) 0.2737(3) 0.0375(9) Uani 0.388(10) d A .
K1 K 0.29203(11) 0.06225(11) -0.00407(14) 0.0484(5) Uani 1 d . .
O1 O 0.2712(3) 0.0700(3) 0.2339(4) 0.0378(14) Uani 1 d . .
O2 O 0.3573(3) 0.1132(3) 0.1646(4) 0.0429(16) Uani 1 d . .
O3 O 0.2908(3) -0.0268(3) 0.1201(4) 0.0428(15) Uani 1 d . .
O4 O 0.3699(3) 0.0105(3) 0.3002(5) 0.0461(16) Uani 1 d . .
O5 O 0.2093(3) -0.1194(3) 0.1394(4) 0.0439(16) Uani 1 d . .
O6 O 0.1794(3) 0.0023(4) 0.1439(4) 0.0518(18) Uani 1 d . .
O7 O 0.2639(3) -0.0538(4) 0.3145(4) 0.0505(18) Uani 1 d . .
O8 O 0.2696(4) 0.1928(3) 0.2011(5) 0.059(2) Uani 1 d . .
O9 O 0.2091(3) 0.1089(4) 0.0498(5) 0.058(2) Uani 1 d . .
O10 O 0.3521(4) -0.1147(3) 0.2574(6) 0.061(2) Uani 1 d . .
O11 O 0.3912(4) 0.3393(4) 0.2575(5) 0.060(2) Uani 1 d . .
O12 O 0.1630(4) 0.2268(4) 0.1004(6) 0.065(2) Uani 1 d . .
O13 O 0.3533(4) 0.1415(4) 0.3758(5) 0.068(2) Uani 1 d . .
O14 O 0.3861(3) 0.2339(4) 0.2678(5) 0.0571(19) Uani 1 d . .
O15 O 0.1671(4) 0.1293(4) 0.2326(5) 0.069(2) Uani 1 d . .
O16 O 0.4566(3) 0.1055(4) 0.3350(5) 0.064(2) Uani 1 d . .
O17 O 0.1807(4) 0.3176(4) 0.0452(5) 0.064(2) Uani 1 d . .
O18 O 0.0933(3) 0.0928(5) 0.0523(6) 0.072(3) Uani 1 d . .
O19 O 0.3758(4) -0.0201(5) -0.0125(6) 0.070(2) Uani 1 d . .
O20 O 0.1267(4) -0.1551(5) 0.0434(6) 0.079(3) Uani 1 d . .
O21 O 0.5397(4) 0.0665(5) 0.4271(6) 0.084(3) Uani 1 d . .
O22A O 0.4377(11) -0.1521(12) 0.3227(17) 0.097(7) Uiso 0.5 d . .
O22B O 0.4449(9) -0.1370(10) 0.2894(14) 0.076(6) Uiso 0.5 d . .
O23 O 0.0268(6) 0.0540(7) -0.0631(10) 0.153(7) Uani 1 d . .
O24A O 0.2381(9) -0.0631(9) -0.0922(12) 0.067(5) Uiso 0.5 d A .
O24B O 0.2089(10) -0.0447(11) -0.0993(14) 0.086(6) Uiso 0.5 d A .
O25 O 0.3663(6) 0.4673(7) 0.2105(12) 0.163(7) Uani 1 d . .
O26 O 0.1477(4) 0.3689(5) 0.4374(7) 0.086(3) Uani 1 d . .
O27 O 0.0456(4) 0.2892(5) 0.3675(6) 0.082(3) Uani 1 d . .
O28 O 0.0954(5) 0.2353(5) 0.2355(8) 0.100(3) Uani 1 d . .
C1 C 0.3637(5) 0.2874(6) 0.2434(7) 0.051(3) Uani 1 d . .
C2 C 0.1979(5) 0.2696(7) 0.0931(8) 0.060(3) Uani 1 d . .
C3A C 0.2616(9) 0.2457(12) 0.1428(15) 0.072(3) Uani 0.612(10) d A 2
H3A H 0.2762 0.2309 0.0973 0.086 Uiso 0.612(10) calc A 2
C4A C 0.2985(9) 0.3015(12) 0.1883(15) 0.072(3) Uani 0.612(10) d A 2
H4A1 H 0.2811 0.3212 0.2272 0.086 Uiso 0.612(10) calc A 2
H4A2 H 0.2966 0.3346 0.1437 0.086 Uiso 0.612(10) calc A 2
C3B C 0.2988(14) 0.2534(12) 0.214(2) 0.072(3) Uani 0.388(10) d A 1
H3B H 0.2814 0.2775 0.2504 0.086 Uiso 0.388(10) calc A 1
C4B C 0.2734(14) 0.287(2) 0.130(2) 0.072(3) Uani 0.388(10) d A 1
H4B1 H 0.29 0.2708 0.0883 0.086 Uiso 0.388(10) calc A 1
H4B2 H 0.2804 0.3348 0.1377 0.086 Uiso 0.388(10) calc A 1
C5 C 0.4886(6) 0.0583(7) 0.3704(9) 0.066(3) Uani 1 d . .
C6 C 0.4032(6) -0.1007(6) 0.2879(11) 0.077(4) Uani 1 d . .
C7 C 0.4171(6) -0.0252(9) 0.2966(13) 0.101(5) Uani 1 d . .
H7 H 0.4195 -0.0125 0.2398 0.121 Uiso 1 calc . .
C8 C 0.4734(7) -0.0133(9) 0.3603(13) 0.112(6) Uani 1 d . .
H8A H 0.5025 -0.0368 0.3438 0.135 Uiso 1 calc . .
H8B H 0.4757 -0.0308 0.4172 0.135 Uiso 1 calc . .
C9 C 0.1573(6) -0.1119(6) 0.0881(8) 0.060(3) Uani 1 d . .
C10 C 0.0690(9) 0.0459(8) -0.0007(14) 0.103(6) Uani 1 d . .
C11A C 0.0844(9) -0.0271(11) 0.0368(15) 0.072(3) Uani 0.612(10) d A 2
H11A H 0.0689 -0.0351 0.0828 0.086 Uiso 0.612(10) calc A 2
H11B H 0.0669 -0.0593 -0.0106 0.086 Uiso 0.612(10) calc A 2
C12A C 0.1436(10) -0.0322(12) 0.0706(16) 0.072(3) Uani 0.612(10) d A 2
H12A H 0.1564 -0.02 0.0223 0.086 Uiso 0.612(10) calc A 2
C11B C 0.1081(15) -0.0129(18) 0.001(2) 0.072(3) Uani 0.388(10) d A 1
H11C H 0.1407 0.0012 -0.0155 0.086 Uiso 0.388(10) calc A 1
H11D H 0.085 -0.0462 -0.0417 0.086 Uiso 0.388(10) calc A 1
C12B C 0.1339(14) -0.0440(16) 0.100(2) 0.072(3) Uani 0.388(10) d A 1
H12B H 0.1038 -0.0466 0.1265 0.086 Uiso 0.388(10) calc A 1
N1 N 0.3024(4) 0.2509(5) 0.4821(6) 0.057(2) Uani 1 d . .
H1A H 0.3201 0.2079 0.504 0.068 Uiso 1 calc . .
H1B H 0.3285 0.2741 0.4589 0.068 Uiso 1 calc . .
C13 C 0.2982(5) 0.2888(7) 0.5552(8) 0.069(3) Uani 1 d . .
H13A H 0.2855 0.3337 0.5352 0.083 Uiso 1 calc . .
H13B H 0.3374 0.2913 0.603 0.083 Uiso 1 calc . .
C14 C 0.2442(6) 0.2411(7) 0.4099(8) 0.065(3) Uani 1 d . .
H14A H 0.2484 0.2121 0.3649 0.079 Uiso 1 calc . .
H14B H 0.2288 0.2836 0.3821 0.079 Uiso 1 calc . .
N2 N 0.4419(4) 0.1958(5) 0.0394(6) 0.059(2) Uani 1 d . .
H2A H 0.4057 0.212 -0.0072 0.071 Uiso 1 calc B 1
H2B H 0.4392 0.1478 0.0429 0.071 Uiso 1 calc B 1
N3 N 0.5015(4) 0.3175(5) 0.0915(6) 0.072(3) Uani 1 d . .
H3C H 0.5038 0.3654 0.087 0.086 Uiso 1 calc C 1
H3D H 0.5381 0.3019 0.1379 0.086 Uiso 1 calc C 1
C15A C 0.4495(7) 0.2264(7) 0.1258(8) 0.0524(19) Uani 0.747(11) d D 1
H15A H 0.4171 0.2132 0.1434 0.063 Uiso 0.747(11) calc D 1
H15B H 0.4868 0.2123 0.1718 0.063 Uiso 0.747(11) calc D 1
C16A C 0.4492(6) 0.2990(7) 0.1136(9) 0.0524(19) Uani 0.747(11) d D 1
H16A H 0.4517 0.3213 0.1679 0.063 Uiso 0.747(11) calc D 1
H16B H 0.4125 0.3126 0.0657 0.063 Uiso 0.747(11) calc D 1
C17A C 0.4936(7) 0.2863(7) 0.0063(8) 0.0524(19) Uani 0.747(11) d D 1
H17A H 0.5256 0.2996 -0.0122 0.063 Uiso 0.747(11) calc D 1
H17B H 0.456 0.3001 -0.0395 0.063 Uiso 0.747(11) calc D 1
C18A C 0.4943(6) 0.2140(7) 0.0186(9) 0.0524(19) Uani 0.747(11) d D 1
H18A H 0.5308 0.2006 0.0672 0.063 Uiso 0.747(11) calc D 1
H18B H 0.4924 0.1915 -0.0353 0.063 Uiso 0.747(11) calc D 1
C15B C 0.4228(14) 0.2461(18) 0.091(2) 0.0524(19) Uani 0.253(11) d D 2
H15C H 0.3955 0.2779 0.0512 0.063 Uiso 0.253(11) calc D 2
H15D H 0.4034 0.2245 0.1261 0.063 Uiso 0.253(11) calc D 2
C16B C 0.4786(15) 0.279(2) 0.150(2) 0.0524(19) Uani 0.253(11) d D 2
H16C H 0.5077 0.2465 0.1841 0.063 Uiso 0.253(11) calc D 2
H16D H 0.4706 0.309 0.1911 0.063 Uiso 0.253(11) calc D 2
C17B C 0.5203(15) 0.2647(18) 0.040(2) 0.0524(19) Uani 0.253(11) d D 2
H17C H 0.5419 0.2848 0.007 0.063 Uiso 0.253(11) calc D 2
H17D H 0.5458 0.2317 0.0806 0.063 Uiso 0.253(11) calc D 2
C18B C 0.4639(15) 0.234(2) -0.022(2) 0.0524(19) Uani 0.253(11) d D 2
H18C H 0.4713 0.2038 -0.0637 0.063 Uiso 0.253(11) calc D 2
H18D H 0.4353 0.2672 -0.0552 0.063 Uiso 0.253(11) calc D 2
N4 N 0 0.1724(8) 0.25 0.082(4) Uani 1 d . .
H4A H 0.0296 0.2012 0.242 0.099 Uiso 0.5 calc . .
H4B H -0.0296 0.2012 0.258 0.099 Uiso 0.5 calc . .
N5 N -0.0444(14) 0.0493(18) 0.254(2) 0.131(11) Uani 0.5 d . .
H5A H -0.0749 0.02 0.2581 0.157 Uiso 0.5 calc . .
H5B H -0.0134 0.0224 0.2467 0.157 Uiso 0.5 calc . .
C19 C 0.0296(8) 0.1365(9) 0.3338(10) 0.097(5) Uani 1 d . .
C20 C 0.0702(16) 0.096(2) 0.322(3) 0.114(10) Uani 0.5 d . .
H20A H 0.0896 0.0699 0.3762 0.137 Uiso 0.5 calc . .
H20B H 0.1005 0.1224 0.3126 0.137 Uiso 0.5 calc . .
C21 C -0.0228(16) 0.0862(19) 0.323(2) 0.103(8) Uani 0.5 d . .
H21A H -0.009 0.0569 0.3748 0.124 Uiso 0.5 calc . .
H21B H -0.0555 0.1119 0.3271 0.124 Uiso 0.5 calc . .
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 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
O7 U1A O3 175.5(4) . .
O7 U1A O1 91.6(3) . .
O3 U1A O1 91.0(3) . .
O7 U1A O10 93.2(4) . .
O3 U1A O10 87.3(4) . .
O1 U1A O10 138.0(4) . .
O7 U1A O4 93.6(4) . .
O3 U1A O4 90.7(3) . .
O1 U1A O4 68.1(2) . .
O10 U1A O4 70.0(3) . .
O7 U1A O5 90.5(3) . .
O3 U1A O5 85.0(3) . .
O1 U1A O5 131.6(4) . .
O10 U1A O5 90.1(3) . .
O4 U1A O5 159.8(4) . .
O7 U1A O6 89.6(4) . .
O3 U1A O6 88.1(4) . .
O1 U1A O6 66.7(3) . .
O10 U1A O6 154.9(3) . .
O4 U1A O6 134.7(3) . .
O5 U1A O6 64.9(3) . .
O7 U1A U3B 103.5(3) . .
O3 U1A U3B 80.8(3) . .
O1 U1A U3B 35.78(19) . .
O10 U1A U3B 103.0(3) . .
O4 U1A U3B 34.96(19) . .
O5 U1A U3B 160.2(3) . .
O6 U1A U3B 100.6(3) . .
O7 U1A U3A 102.5(3) . .
O3 U1A U3A 81.5(3) . .
O1 U1A U3A 30.41(17) . .
O10 U1A U3A 108.4(3) . .
O4 U1A U3A 40.03(18) . .
O5 U1A U3A 156.5(3) . .
O6 U1A U3A 95.3(2) . .
U3B U1A U3A 5.43(10) . .
O7 U1A U2A 98.3(3) . .
O3 U1A U2A 82.0(3) . .
O1 U1A U2A 32.64(18) . .
O10 U1A U2A 165.0(3) . .
O4 U1A U2A 99.6(2) . .
O5 U1A U2A 99.4(3) . .
O6 U1A U2A 35.6(2) . .
U3B U1A U2A 65.07(10) . .
U3A U1A U2A 59.77(8) . .
O7 U1A U2B 99.0(3) . .
O3 U1A U2B 81.8(3) . .
O1 U1A U2B 26.46(19) . .
O10 U1A U2B 159.8(3) . .
O4 U1A U2B 93.0(2) . .
O5 U1A U2B 105.8(3) . .
O6 U1A U2B 42.1(2) . .
U3B U1A U2B 58.57(9) . .
U3A U1A U2B 53.26(10) . .
U2A U1A U2B 6.52(7) . .
O7 U1A K1 160.8(3) . .
O3 U1A K1 21.1(2) . .
O1 U1A K1 70.0(2) . .
O10 U1A K1 104.4(3) . .
O4 U1A K1 85.1(2) . .
O5 U1A K1 97.3(2) . .
O6 U1A K1 77.9(2) . .
U3B U1A K1 65.25(10) . .
U3A U1A K1 64.67(8) . .
U2A U1A K1 63.09(9) . .
U2B U1A K1 61.92(10) . .
O9 U2A O15 172.7(4) . .
O9 U2A O18 91.1(4) . .
O15 U2A O18 92.1(4) . .
O9 U2A O1 92.8(3) . .
O15 U2A O1 88.3(3) . .
O18 U2A O1 145.1(3) . .
O9 U2A O6 91.1(3) . .
O15 U2A O6 96.0(3) . .
O18 U2A O6 75.8(3) . .
O1 U2A O6 69.5(2) . .
O9 U2A O12 86.9(3) . .
O15 U2A O12 86.9(3) . .
O18 U2A O12 85.6(3) . .
O1 U2A O12 129.2(3) . .
O6 U2A O12 161.2(3) . .
O9 U2A O8 84.4(3) . .
O15 U2A O8 89.6(4) . .
O18 U2A O8 149.7(3) . .
O1 U2A O8 65.2(2) . .
O6 U2A O8 134.1(3) . .
O12 U2A O8 64.2(3) . .
O9 U2A U1B 84.2(3) . .
O15 U2A U1B 100.6(3) . .
O18 U2A U1B 111.9(3) . .
O1 U2A U1B 34.4(2) . .
O6 U2A U1B 36.7(2) . .
O12 U2A U1B 160.4(3) . .
O8 U2A U1B 97.5(2) . .
O9 U2A U3A 82.2(3) . .
O15 U2A U3A 95.2(3) . .
O18 U2A U3A 171.1(3) . .
O1 U2A U3A 30.57(17) . .
O6 U2A U3A 98.34(18) . .
O12 U2A U3A 99.8(2) . .
O8 U2A U3A 35.79(19) . .
U1B U2A U3A 61.66(13) . .
O9 U2A U1A 84.6(2) . .
O15 U2A U1A 100.1(3) . .
O18 U2A U1A 113.8(3) . .
O1 U2A U1A 32.55(17) . .
O6 U2A U1A 38.52(18) . .
O12 U2A U1A 158.8(2) . .
O8 U2A U1A 95.7(2) . .
U1B U2A U1A 1.87(19) . .
U3A U2A U1A 59.86(9) . .
O9 U2A U3B 81.0(3) . .
O15 U2A U3B 96.8(3) . .
O18 U2A U3B 168.3(3) . .
O1 U2A U3B 28.46(18) . .
O6 U2A U3B 95.62(19) . .
O12 U2A U3B 102.5(2) . .
O8 U2A U3B 38.6(2) . .
U1B U2A U3B 58.90(14) . .
U3A U2A U3B 2.98(11) . .
U1A U2A U3B 57.11(10) . .
O9 U2A K1 21.6(2) . .
O15 U2A K1 159.4(3) . .
O18 U2A K1 106.6(3) . .
O1 U2A K1 71.48(18) . .
O6 U2A K1 80.85(19) . .
O12 U2A K1 102.7(2) . .
O8 U2A K1 78.63(17) . .
U1B U2A K1 64.88(11) . .
U3A U2A K1 65.39(6) . .
U1A U2A K1 64.88(7) . .
U3B U2A K1 63.59(8) . .
O13 U3A O2 171.2(4) . .
O13 U3A O1 92.3(3) . .
O2 U3A O1 94.1(3) . .
O13 U3A O8 95.9(4) . .
O2 U3A O8 91.9(3) . .
O1 U3A O8 70.8(3) . .
O13 U3A O14 89.4(3) . .
O2 U3A O14 88.8(3) . .
O1 U3A O14 145.2(3) . .
O8 U3A O14 74.5(3) . .
O13 U3A O4 89.9(4) . .
O2 U3A O4 87.1(3) . .
O1 U3A O4 66.7(2) . .
O8 U3A O4 137.3(3) . .
O14 U3A O4 148.0(3) . .
O13 U3A O16 86.6(4) . .
O2 U3A O16 84.6(3) . .
O1 U3A O16 134.7(3) . .
O8 U3A O16 154.4(3) . .
O14 U3A O16 80.1(3) . .
O4 U3A O16 68.0(3) . .
O13 U3A C3B 91.6(9) . .
O2 U3A C3B 93.2(8) . .
O1 U3A C3B 100.2(5) . .
O8 U3A C3B 29.5(5) . .
O14 U3A C3B 45.1(5) . .
O4 U3A C3B 166.8(5) . .
O16 U3A C3B 125.1(5) . .
O13 U3A U2B 101.1(3) . .
O2 U3A U2B 87.6(2) . .
O1 U3A U2B 36.47(18) . .
O8 U3A U2B 35.3(2) . .
O14 U3A U2B 109.3(3) . .
O4 U3A U2B 102.1(2) . .
O16 U3A U2B 167.7(3) . .
C3B U3A U2B 64.7(5) . .
O13 U3A U2A 102.0(3) . .
O2 U3A U2A 86.6(2) . .
O1 U3A U2A 32.07(16) . .
O8 U3A U2A 40.1(2) . .
O14 U3A U2A 114.0(2) . .
O4 U3A U2A 97.38(18) . .
O16 U3A U2A 163.3(2) . .
C3B U3A U2A 69.5(5) . .
U2B U3A U2A 4.82(11) . .
O13 U3A U1A 100.9(3) . .
O2 U3A U1A 81.7(2) . .
O1 U3A U1A 31.80(19) . .
O8 U3A U1A 100.4(2) . .
O14 U3A U1A 169.0(2) . .
O4 U3A U1A 37.24(19) . .
O16 U3A U1A 104.2(3) . .
C3B U3A U1A 129.8(5) . .
U2B U3A U1A 65.17(14) . .
U2A U3A U1A 60.37(11) . .
O13 U3A U1B 101.7(3) . .
O17 K1 O9 93.2(3) 7 .
O17 K1 O19 106.4(3) 7 .
O9 K1 O19 157.8(3) . .
O17 K1 O3 149.8(2) 7 .
O9 K1 O3 76.2(2) . .
O19 K1 O3 81.6(3) . .
O17 K1 O7 76.8(2) 7 6
O9 K1 O7 117.7(2) . 6
O19 K1 O7 77.8(2) . 6
O3 K1 O7 133.2(2) . 6
O17 K1 O2 79.0(2) 7 .
O9 K1 O2 76.3(2) . .
O19 K1 O2 97.0(2) . .
O3 K1 O2 71.1(2) . .
O7 K1 O2 152.5(2) 6 .
O17 K1 O24A 139.8(4) 7 .
O9 K1 O24A 102.1(4) . .
O19 K1 O24A 69.5(4) . .
O3 K1 O24A 70.4(4) . .
O7 K1 O24A 63.1(4) 6 .
O2 K1 O24A 140.6(4) . .
O17 K1 O24B 135.9(5) 7 .
O9 K1 O24B 88.7(5) . .
O19 K1 O24B 84.4(5) . .
O3 K1 O24B 72.9(4) . .
O7 K1 O24B 63.7(4) 6 .
O2 K1 O24B 143.3(4) . .
O24A K1 O24B 15.0(4) . .
O17 K1 U2A 100.37(19) 7 .
O9 K1 U2A 14.04(15) . .
O19 K1 U2A 145.1(2) . .
O3 K1 U2A 64.20(14) . .
O7 K1 U2A 130.93(17) 6 .
O2 K1 U2A 66.41(15) . .
O24A K1 U2A 103.2(4) . .
O24B K1 U2A 91.8(4) . .
U2B K1 U2A 6.01(7) . .
U1B K1 U2A 50.14(13) . .
O17 K1 U1A 138.6(2) 7 .
O9 K1 U1A 64.87(17) . .
O19 K1 U1A 93.2(2) . .
O3 K1 U1A 13.56(15) . .
O7 K1 U1A 144.06(18) 6 .
O2 K1 U1A 62.36(15) . .
O24A K1 U1A 81.1(4) . .
O24B K1 U1A 81.0(4) . .
U2A K1 U1A 52.03(8) . .
U3A O1 U1A 117.8(3) . .
U3A O1 U2A 117.4(3) . .
U1A O1 U2A 114.8(3) . .
U3A O2 K1 139.5(3) . .
U1A O3 K1 145.4(4) . .
C7 O4 U1A 112.6(8) . .
C7 O4 U3A 127.1(9) . .
U1A O4 U3A 102.7(3) . .
C9 O5 U1A 128.8(7) . .
C12A O6 U2A 121.0(11) . .
C12B O6 U2A 134.4(17) . .
C12A O6 U1A 117.1(12) . .
C12B O6 U1A 118.5(17) . .
U2A O6 U1A 105.9(3) . .
U1A O7 K1 154.2(4) . 6_556
C3B O8 U3A 97.9(15) . .
C3A O8 U3A 130.0(10) . .
C3B O8 U2A 157.5(14) . .
C3A O8 U2A 110.1(9) . .
U3A O8 U2A 104.2(3) . .
U2A O9 K1 144.4(4) . .
C6 O10 U1A 122.8(8) . .
C2 O12 U2A 125.8(7) . .
C1 O14 U3A 134.2(7) . .
C5 O16 U3A 137.1(7) . .
C2 O17 K1 146.0(8) . 7
C10 O18 U2A 132.8(11) . .
O22B O22A C6 68(3) . .
O22A O22B C6 80(3) . .
O24B O24A K1 83(2) . .
O24A O24B K1 82(2) . .
O14 C1 O11 124.1(10) . .
O14 C1 C4A 126.9(12) . .
O11 C1 C4A 109.0(13) . .
O14 C1 C3B 89.2(13) . .
O11 C1 C3B 145.7(16) . .
O17 C2 O12 122.2(10) . .
O17 C2 C3A 128.5(14) . .
O12 C2 C3A 108.8(12) . .
O17 C2 C4B 96.7(15) . .
O12 C2 C4B 141.0(15) . .
O8 C3A C4A 110.4(17) . .
O8 C3A C2 116.9(16) . .
C4A C3A C2 109.2(19) . .
O8 C3A H3A 106.6 . .
C4A C3A H3A 106.6 . .
C2 C3A H3A 106.6 . .
C3A C4A C1 117.3(19) . .
C3A C4A H4A1 108 . .
C1 C4A H4A1 108 . .
C3A C4A H4A2 108 . .
C1 C4A H4A2 108 . .
H4A1 C4A H4A2 107.2 . .
O8 C3B C4B 106(2) . .
O8 C3B C1 144(3) . .
C4B C3B C1 96(2) . .
O8 C3B U3A 52.6(11) . .
C4B C3B U3A 135(3) . .
C1 C3B U3A 91.5(15) . .
O8 C3B H3B 102.1 . .
C4B C3B H3B 102.1 . .
C1 C3B H3B 102.1 . .
U3A C3B H3B 119.9 . .
C3B C4B C2 104(2) . .
C3B C4B H4B1 110.9 . .
C2 C4B H4B1 110.9 . .
C3B C4B H4B2 110.9 . .
C2 C4B H4B2 110.9 . .
H4B1 C4B H4B2 108.9 . .
O16 C5 O21 121.4(12) . .
O16 C5 C8 128.2(12) . .
O21 C5 C8 110.3(14) . .
O10 C6 O22B 126.0(15) . .
O10 C6 O22A 112.7(16) . .
O22B C6 O22A 31.6(13) . .
O10 C6 C7 115.3(11) . .
O22B C6 C7 115.3(16) . .
O22A C6 C7 130.7(16) . .
O4 C7 C8 118.7(16) . .
O4 C7 C6 111.2(12) . .
C8 C7 C6 110.8(14) . .
O4 C7 H7 105 . .
C8 C7 H7 105 . .
C6 C7 H7 105 . .
C7 C8 C5 112.5(15) . .
C7 C8 H8A 109.1 . .
C5 C8 H8A 109.1 . .
C7 C8 H8B 109.1 . .
C5 C8 H8B 109.1 . .
H8A C8 H8B 107.8 . .
O20 C9 O5 124.2(12) . .
O20 C9 C12B 123.9(14) . .
O5 C9 C12B 111.3(13) . .
O20 C9 C12A 124.7(13) . .
O5 C9 C12A 109.1(11) . .
O23 C10 O18 121.6(16) . .
O23 C10 C11B 118(2) . .
O18 C10 C11B 117(2) . .
O23 C10 C11A 118.2(19) . .
O18 C10 C11A 117.0(16) . .
C12A C11A C10 107(2) . .
C12A C11A H11A 110.4 . .
C10 C11A H11A 110.4 . .
C12A C11A H11B 110.4 . .
C10 C11A H11B 110.4 . .
H11A C11A H11B 108.6 . .
C11A C12A O6 123(2) . .
C11A C12A C9 105.2(18) . .
O6 C12A C9 109.1(15) . .
C11A C12A H12A 106.1 . .
O6 C12A H12A 106.1 . .
C9 C12A H12A 106.1 . .
C10 C11B C12B 109(3) . .
C10 C11B H11C 109.9 . .
C12B C11B H11C 109.9 . .
C10 C11B H11D 109.9 . .
C12B C11B H11D 109.9 . .
H11C C11B H11D 108.3 . .
O6 C12B C9 113(3) . .
O6 C12B C11B 100(2) . .
C9 C12B C11B 104(3) . .
O6 C12B H12B 112.8 . .
C9 C12B H12B 112.8 . .
C11B C12B H12B 112.8 . .
C13 N1 C14 112.1(9) . .
C13 N1 H1A 109.2 . .
C14 N1 H1A 109.2 . .
C13 N1 H1B 109.2 . .
C14 N1 H1B 109.2 . .
H1A N1 H1B 107.9 . .
N1 C13 C14 112.3(10) . 7_556
N1 C13 H13A 109.1 . .
C14 C13 H13A 109.1 7_556 .
N1 C13 H13B 109.1 . .
C14 C13 H13B 109.1 7_556 .
H13A C13 H13B 107.9 . .
N1 C14 C13 110.5(10) . 7_556
N1 C14 H14A 109.5 . .
C13 C14 H14A 109.5 7_556 .
N1 C14 H14B 109.5 . .
C13 C14 H14B 109.5 7_556 .
H14A C14 H14B 108.1 . .
C15A N2 C18A 108.1(10) . .
C15B N2 C18B 107(2) . .
C15A N2 H2A 110.1 . .
C18A N2 H2A 110.1 . .
C15A N2 H2B 110.1 . .
C18A N2 H2B 110.1 . .
H2A N2 H2B 108.4 . .
C17A N3 C16A 107.8(10) . .
C16B N3 C17B 105(3) . .
C17A N3 H3C 110.1 . .
C16A N3 H3C 110.1 . .
C17A N3 H3D 110.1 . .
C16A N3 H3D 110.1 . .
H3C N3 H3D 108.5 . .
C16A C15A N2 107.0(10) . .
C16A C15A H15A 110.3 . .
N2 C15A H15A 110.3 . .
C16A C15A H15B 110.3 . .
N2 C15A H15B 110.3 . .
H15A C15A H15B 108.6 . .
C15A C16A N3 108.6(11) . .
C15A C16A H16A 110 . .
N3 C16A H16A 110 . .
C15A C16A H16B 110 . .
N3 C16A H16B 110 . .
H16A C16A H16B 108.4 . .
N3 C17A C18A 107.7(11) . .
N3 C17A H17A 110.2 . .
C18A C17A H17A 110.2 . .
N3 C17A H17B 110.2 . .
C18A C17A H17B 110.2 . .
H17A C17A H17B 108.5 . .
C17A C18A N2 108.0(11) . .
C17A C18A H18A 110.1 . .
N2 C18A H18A 110.1 . .
C17A C18A H18B 110.1 . .
N2 C18A H18B 110.1 . .
H18A C18A H18B 108.4 . .
C16B C15B N2 105(3) . .
C16B C15B H15C 110.7 . .
N2 C15B H15C 110.7 . .
C16B C15B H15D 110.7 . .
N2 C15B H15D 110.7 . .
H15C C15B H15D 108.8 . .
C15B C16B N3 107(3) . .
C15B C16B H16C 110.3 . .
N3 C16B H16C 110.3 . .
C15B C16B H16D 110.3 . .
N3 C16B H16D 110.3 . .
H16C C16B H16D 108.5 . .
C18B C17B N3 106(3) . .
C18B C17B H17C 110.6 . .
N3 C17B H17C 110.6 . .
C18B C17B H17D 110.6 . .
N3 C17B H17D 110.6 . .
H17C C17B H17D 108.7 . .
C17B C18B N2 103(3) . .
C17B C18B H18C 111.1 . .
C17B C18B H18D 111.1 . .
N2 C18B H18D 111.1 . .
H18C C18B H18D 109 . .
C19 N4 C19 120.8(19) . 2
C19 N4 H4A 107.1 . .
C19 N4 H4A 107.1 2 .
C19 N4 H4B 107.1 . .
C19 N4 H4B 107.1 2 .
H4A N4 H4B 106.8 . .
C21 N5 C20 106(3) . 2
C21 N5 H5A 110.6 . .
C20 N5 H5A 110.6 2 .
C21 N5 H5B 110.6 . .
C20 N5 H5B 110.6 2 .
H5A N5 H5B 108.8 . .
C20 C19 N4 107(2) . .
C20 C19 C21 101(3) . .
N4 C19 C21 97.3(15) . .
C19 C20 N5 114(3) . 2
C19 C20 H20A 108.8 . .
N5 C20 H20A 108.8 2 .
N5 C20 H20B 108.8 2 .
H20A C20 H20B 107.7 . .
N5 C21 C19 120(2) . .
N5 C21 H21A 107.2 . .
C19 C21 H21A 107.2 . .
N5 C21 H21B 107.2 . .
C19 C21 H21B 107.2 . .
H21A C21 H21B 106.9 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1A O7 1.777(8) .
U1A O3 1.798(7) .
U1A O1 2.250(8) .
U1A O10 2.286(10) .
U1A O4 2.343(9) .
U1A O5 2.410(8) .
U1A O6 2.458(9) .
U2A O9 1.789(8) .
U2A O15 1.800(8) .
U2A O18 2.256(9) .
U2A O1 2.256(6) .
U2A O6 2.296(8) .
U2A O12 2.423(8) .
U2A O8 2.504(8) .
U3A O13 1.778(8) .
U3A O2 1.818(7) .
U3A O1 2.161(7) .
U3A O8 2.276(9) .
U3A O14 2.346(8) .
U3A O4 2.490(8) .
U3A O16 2.501(9) .
K1 O17 2.710(8) 7
K1 O9 2.711(8) .
K1 O19 2.722(8) .
K1 O3 2.759(7) .
K1 O7 2.816(7) 6
K1 O2 2.835(7) .
K1 O24A 3.004(18) .
K1 O24B 3.01(2) .
O4 C7 1.400(16) .
O5 C9 1.252(14) .
O6 C12A 1.39(2) .
O6 C12B 1.438(18) .
O8 C3B 1.412(18) .
O8 C3A 1.41(2) .
O10 C6 1.204(15) .
O11 C1 1.237(13) .
O12 C2 1.270(15) .
O14 C1 1.226(14) .
O16 C5 1.245(16) .
O17 C2 1.233(14) .
O17 K1 2.710(8) 7
O18 C10 1.28(2) .
O20 C9 1.216(14) .
O21 C5 1.266(15) .
O22A O22B 0.71(3) .
O22A C6 1.34(3) .
O22B C6 1.27(2) .
O23 C10 1.17(2) .
O24A O24B 0.78(2) .
C1 C4A 1.55(2) .
C1 C3B 1.65(3) .
C2 C3A 1.55(2) .
C2 C4B 1.77(3) .
C3A C4A 1.48(3) .
C3A H3A 1 .
C4A H4A1 0.99 .
C4A H4A2 0.99 .
C3B C4B 1.46(5) .
C3B H3B 1 .
C4B H4B1 0.99 .
C4B H4B2 0.99 .
C5 C8 1.51(2) .
C6 C7 1.58(2) .
C7 C8 1.41(2) .
C7 H7 1 .
C8 H8A 0.99 .
C8 H8B 0.99 .
C9 C12B 1.55(4) .
C9 C12A 1.67(3) .
C10 C11B 1.54(4) .
C10 C11A 1.61(3) .
C11A C12A 1.36(3) .
C11A H11A 0.99 .
C11A H11B 0.99 .
C12A H12A 1 .
C11B C12B 1.65(5) .
C11B H11C 0.99 .
C11B H11D 0.99 .
C12B H12B 1 .
N1 C13 1.475(15) .
N1 C14 1.493(15) .
N1 H1A 0.99 .
N1 H1B 0.99 .
C13 C14 1.510(16) 7_556
C13 H13A 0.99 .
C13 H13B 0.99 .
C14 H14A 0.99 .
C14 H14B 0.99 .
N2 C15A 1.507(13) .
N2 C18A 1.512(13) .
N2 C15B 1.526(19) .
N2 C18B 1.533(19) .
N2 H2A 0.99 .
N2 H2B 0.99 .
N3 C17A 1.491(13) .
N3 C16B 1.514(19) .
N3 C16A 1.525(13) .
N3 C17B 1.554(19) .
N3 H3C 0.99 .
N3 H3D 0.99 .
C15A C16A 1.502(15) .
C15A H15A 0.99 .
C15A H15B 0.99 .
C16A H16A 0.99 .
C16A H16B 0.99 .
C17A C18A 1.498(15) .
C17A H17A 0.99 .
C17A H17B 0.99 .
C18A H18A 0.99 .
C18A H18B 0.99 .
C15B C16B 1.51(2) .
C15B H15C 0.99 .
C15B H15D 0.99 .
C16B H16C 0.99 .
C16B H16D 0.99 .
C17B C18B 1.52(2) .
C17B H17C 0.99 .
C17B H17D 0.99 .
C18B H18C 0.99 .
C18B H18D 0.99 .
N4 C19 1.491(16) .
N4 C19 1.491(16) 2
N4 H4A 0.99 .
N4 H4B 0.99 .
N5 C21 1.31(5) .
N5 C20 1.51(5) 2
N5 H5A 0.99 .
N5 H5B 0.99 .
C19 C20 1.38(4) .
C19 C21 1.62(4) .
C20 N5 1.51(5) 2
C20 H20A 0.99 .
C20 H20B 0.99 .
C21 H21A 0.99 .
C21 H21B 0.99 .
