#------------------------------------------------------------------------------
#$Date: 2016-03-21 19:03:03 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178833 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/87/4108789.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_4108789
loop_
_publ_author_name
'Grégory Nocton'
'Pawel Horeglad'
'Jacques Pécaut'
'Marinella Mazzanti'
_publ_contact_author
;
      Dr Marinella Mazzanti
      LCIB (UMR-E 3 CEA-UJF)
      DRFMC, CEA Grenoble
      17, rue des Martyrs
      38054 Grenoble cedex 9
;
_publ_section_title
;
 Polynuclear Cation-Cation Complexes of Pentavalent Uranyl: Relating
 Stability and Magnetic Properties to Structure
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16633
_journal_page_last               16645
_journal_paper_doi               10.1021/ja804766r
_journal_volume                  130
_journal_year                    2008
_chemical_formula_sum            'C138 H115 K4 N9 O24 U4'
_chemical_formula_weight         3391.91
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_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_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 101.202(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   30.537(17)
_cell_length_b                   14.227(8)
_cell_length_c                   31.856(18)
_cell_measurement_reflns_used    971
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      24.69
_cell_measurement_theta_min      2.41
_cell_volume                     13576(13)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.918
_diffrn_measured_fraction_theta_max 0.918
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0469
_diffrn_reflns_av_sigmaI/netI    0.0635
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            28159
_diffrn_reflns_theta_full        24.77
_diffrn_reflns_theta_max         24.77
_diffrn_reflns_theta_min         1.58
_exptl_absorpt_coefficient_mu    4.950
_exptl_absorpt_correction_T_max  0.820
_exptl_absorpt_correction_T_min  0.629
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.659
_exptl_crystal_density_meas      0
_exptl_crystal_description       needle
_exptl_crystal_F_000             6568
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         5.295
_refine_diff_density_min         -1.838
_refine_diff_density_rms         0.253
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     822
_refine_ls_number_reflns         10701
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      1.122
_refine_ls_R_factor_all          0.0838
_refine_ls_R_factor_gt           0.0697
_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)+(0.0528P)²+1137.1892P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1846
_refine_ls_wR_factor_ref         0.1913
_reflns_number_gt                8866
_reflns_number_total             10701
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja804766r_si_001_1.cif
_cod_data_source_block           3
_cod_database_code               4108789
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'
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 0.651503(17) 0.70539(4) -0.000373(16) 0.01624(16) Uani 1 1 d . . .
O11 O 0.7072(3) 0.6910(7) 0.0389(3) 0.024(2) Uani 1 1 d . . .
O14 O 0.5987(3) 0.7177(8) -0.0372(3) 0.026(2) Uani 1 1 d . . .
U2 U 0.775360(17) 0.67973(4) 0.091440(16) 0.01732(16) Uani 1 1 d . . .
O12 O 0.7457(3) 0.6354(8) 0.1321(3) 0.027(2) Uani 1 1 d . . .
O13 O 0.8039(3) 0.7286(7) 0.0472(3) 0.021(2) Uani 1 1 d . . .
K2 K 0.74074(11) 0.8954(2) 0.02171(10) 0.0243(7) Uani 1 1 d . . .
K1 K 0.65976(16) 0.6230(5) 0.12163(19) 0.081(2) Uani 1 1 d . . .
O1 O 0.6678(3) 0.5695(8) -0.0424(3) 0.027(2) Uani 1 1 d . . .
O2 O 0.6250(4) 0.5620(8) 0.0276(3) 0.027(2) Uani 1 1 d . . .
C1 C 0.6757(6) 0.4892(14) -0.1204(6) 0.040(5) Uani 1 1 d . . .
H1 H 0.6893 0.5478 -0.1133 0.048 Uiso 1 1 calc R . .
C2 C 0.6836(9) 0.4403(17) -0.1564(7) 0.068(8) Uani 1 1 d . . .
H2 H 0.7037 0.4651 -0.1724 0.081 Uiso 1 1 calc R . .
C3 C 0.6625(7) 0.3569(14) -0.1688(6) 0.045(5) Uani 1 1 d . . .
H3 H 0.6671 0.3258 -0.1936 0.054 Uiso 1 1 calc R . .
C4 C 0.6343(7) 0.3197(15) -0.1441(6) 0.047(5) Uani 1 1 d . . .
H4 H 0.6197 0.2623 -0.1519 0.056 Uiso 1 1 calc R . .
C5 C 0.6273(6) 0.3670(12) -0.1079(6) 0.038(4) Uani 1 1 d . . .
H5 H 0.6079 0.3406 -0.0915 0.045 Uiso 1 1 calc R . .
C6 C 0.6477(5) 0.4507(12) -0.0952(5) 0.024(3) Uani 1 1 d . . .
C7 C 0.6401(4) 0.5029(9) -0.0566(5) 0.017(3) Uani 1 1 d . . .
C8 C 0.6048(5) 0.4753(12) -0.0369(5) 0.029(4) Uani 1 1 d . . .
H8 H 0.5820 0.4385 -0.0530 0.035 Uiso 1 1 calc R . .
C9 C 0.6012(5) 0.4985(10) 0.0046(5) 0.026(3) Uani 1 1 d . . .
C10 C 0.5686(5) 0.4451(10) 0.0252(5) 0.021(3) Uani 1 1 d . . .
C11 C 0.5765(7) 0.4360(15) 0.0692(6) 0.048(5) Uani 1 1 d . . .
H11 H 0.6029 0.4610 0.0854 0.058 Uiso 1 1 calc R . .
C12 C 0.5471(8) 0.392(2) 0.0900(7) 0.071(8) Uani 1 1 d . . .
H12 H 0.5530 0.3862 0.1200 0.086 Uiso 1 1 calc R . .
C13 C 0.5084(8) 0.3562(14) 0.0654(7) 0.053(6) Uani 1 1 d . . .
H13 H 0.4878 0.3258 0.0792 0.064 Uiso 1 1 calc R . .
C14 C 0.4991(6) 0.3634(12) 0.0221(6) 0.034(4) Uani 1 1 d . . .
H14 H 0.4723 0.3393 0.0062 0.041 Uiso 1 1 calc R . .
C15 C 0.5296(5) 0.4065(12) 0.0018(5) 0.030(4) Uani 1 1 d . . .
H15 H 0.5240 0.4099 -0.0283 0.036 Uiso 1 1 calc R . .
O21 O 0.6164(4) 0.7355(8) 0.0614(3) 0.033(3) Uani 1 1 d . . .
O22 O 0.6479(4) 0.8752(8) 0.0133(3) 0.027(2) Uani 1 1 d . . .
C21 C 0.5429(6) 0.6812(13) 0.0965(5) 0.036(4) Uani 1 1 d . . .
H21 H 0.5546 0.6350 0.0807 0.043 Uiso 1 1 calc R . .
C22 C 0.5130(7) 0.6548(17) 0.1220(6) 0.052(5) Uani 1 1 d . . .
H22 H 0.5046 0.5914 0.1233 0.062 Uiso 1 1 calc R . .
C23 C 0.4963(7) 0.718(2) 0.1443(6) 0.057(6) Uani 1 1 d . . .
H23 H 0.4763 0.7000 0.1618 0.068 Uiso 1 1 calc R . .
C24 C 0.5081(7) 0.815(2) 0.1425(6) 0.058(7) Uani 1 1 d . . .
H24 H 0.4958 0.8599 0.1584 0.070 Uiso 1 1 calc R . .
C25 C 0.5379(6) 0.8411(17) 0.1171(5) 0.048(5) Uani 1 1 d . . .
H25 H 0.5459 0.9046 0.1155 0.057 Uiso 1 1 calc R . .
C26 C 0.5559(5) 0.7738(12) 0.0937(5) 0.028(4) Uani 1 1 d . . .
C27 C 0.5882(5) 0.7953(11) 0.0656(5) 0.025(3) Uani 1 1 d . . .
C28 C 0.5829(6) 0.8830(11) 0.0433(5) 0.030(4) Uani 1 1 d U . .
H28 H 0.5575 0.9191 0.0449 0.035 Uiso 1 1 calc R . .
C29 C 0.6126(5) 0.9189(11) 0.0192(5) 0.026(3) Uani 1 1 d . . .
C30 C 0.6031(5) 1.0129(12) -0.0011(5) 0.031(4) Uani 1 1 d . . .
C31 C 0.6174(6) 1.0331(13) -0.0393(5) 0.036(4) Uani 1 1 d . . .
H31 H 0.6362 0.9910 -0.0502 0.044 Uiso 1 1 calc R . .
C32 C 0.6036(7) 1.1156(14) -0.0611(6) 0.043(5) Uani 1 1 d . . .
H32 H 0.6132 1.1293 -0.0867 0.052 Uiso 1 1 calc R . .
C33 C 0.5762(7) 1.1771(14) -0.0457(6) 0.046(5) Uani 1 1 d . . .
H33 H 0.5658 1.2308 -0.0618 0.055 Uiso 1 1 calc R . .
C34 C 0.5635(8) 1.1614(14) -0.0068(8) 0.058(6) Uani 1 1 d . . .
H34 H 0.5457 1.2052 0.0043 0.069 Uiso 1 1 calc R . .
C35 C 0.5777(7) 1.0799(13) 0.0153(6) 0.046(5) Uani 1 1 d . . .
H35 H 0.5701 1.0694 0.0422 0.055 Uiso 1 1 calc R . .
O61 O 0.7445(4) 0.8358(7) 0.1046(3) 0.025(2) Uani 1 1 d . . .
O62 O 0.8227(3) 0.7623(8) 0.1479(3) 0.029(3) Uani 1 1 d . . .
C61 C 0.6909(7) 0.9986(14) 0.1113(6) 0.042(5) Uani 1 1 d . . .
H61 H 0.7072 1.0032 0.0892 0.050 Uiso 1 1 calc R . .
C62 C 0.6560(8) 1.0592(14) 0.1128(6) 0.052(6) Uani 1 1 d . . .
H62 H 0.6488 1.1050 0.0913 0.063 Uiso 1 1 calc R . .
C63 C 0.6311(7) 1.0551(16) 0.1450(7) 0.050(5) Uani 1 1 d . . .
H63 H 0.6079 1.0979 0.1463 0.059 Uiso 1 1 calc R . .
C64 C 0.6425(7) 0.9843(17) 0.1750(7) 0.056(6) Uani 1 1 d . . .
H64 H 0.6258 0.9785 0.1968 0.068 Uiso 1 1 calc R . .
C65 C 0.6775(7) 0.9210(17) 0.1745(7) 0.055(6) Uani 1 1 d . . .
H65 H 0.6841 0.8735 0.1953 0.066 Uiso 1 1 calc R . .
C66 C 0.7017(5) 0.9297(12) 0.1434(5) 0.028(4) Uani 1 1 d . . .
C67 C 0.7410(6) 0.8642(11) 0.1414(5) 0.026(3) Uani 1 1 d . . .
C68 C 0.7692(6) 0.8443(12) 0.1795(5) 0.034(4) Uani 1 1 d . . .
H68 H 0.7605 0.8609 0.2052 0.040 Uiso 1 1 calc R . .
C69 C 0.8103(6) 0.8000(13) 0.1811(5) 0.034(4) Uani 1 1 d . . .
C70 C 0.8447(6) 0.7942(13) 0.2210(5) 0.033(4) Uani 1 1 d . . .
C71 C 0.8722(7) 0.7161(16) 0.2268(6) 0.050(5) Uani 1 1 d . . .
H71 H 0.8684 0.6686 0.2059 0.059 Uiso 1 1 calc R . .
C72 C 0.9052(8) 0.7070(16) 0.2629(7) 0.056(6) Uani 1 1 d . . .
H72 H 0.9236 0.6536 0.2666 0.067 Uiso 1 1 calc R . .
C73 C 0.9111(8) 0.7769(19) 0.2938(7) 0.066(7) Uani 1 1 d . . .
H73 H 0.9334 0.7709 0.3185 0.079 Uiso 1 1 calc R . .
C74 C 0.8842(8) 0.8550(18) 0.2881(6) 0.061(7) Uani 1 1 d . . .
H74 H 0.8885 0.9037 0.3084 0.073 Uiso 1 1 calc R . .
C75 C 0.8507(8) 0.8611(18) 0.2523(6) 0.059(6) Uani 1 1 d . . .
H75 H 0.8314 0.9132 0.2493 0.071 Uiso 1 1 calc R . .
O41 O 0.7660(3) 0.5235(8) 0.0577(3) 0.023(2) Uani 1 1 d . . .
O42 O 0.8380(4) 0.5794(8) 0.1219(3) 0.032(3) Uani 1 1 d . . .
C41 C 0.7027(6) 0.3763(12) 0.0364(5) 0.032(4) Uani 1 1 d . . .
H41 H 0.6913 0.4376 0.0317 0.039 Uiso 1 1 calc R . .
C42 C 0.6759(6) 0.2996(12) 0.0214(6) 0.041(5) Uani 1 1 d . . .
H42 H 0.6460 0.3090 0.0081 0.049 Uiso 1 1 calc R . .
C43 C 0.6932(6) 0.2109(12) 0.0261(6) 0.039(4) Uani 1 1 d . . .
H43 H 0.6753 0.1594 0.0151 0.047 Uiso 1 1 calc R . .
C44 C 0.7372(7) 0.1960(13) 0.0471(6) 0.044(5) Uani 1 1 d . . .
H44 H 0.7489 0.1347 0.0503 0.053 Uiso 1 1 calc R . .
C45 C 0.7635(6) 0.2714(13) 0.0631(5) 0.035(4) Uani 1 1 d . . .
H45 H 0.7932 0.2615 0.0772 0.042 Uiso 1 1 calc R . .
C46 C 0.7461(5) 0.3631(11) 0.0583(5) 0.024(3) Uani 1 1 d . . .
C47 C 0.7725(4) 0.4442(10) 0.0785(4) 0.017(3) Uani 1 1 d U . .
C48 C 0.8013(6) 0.4308(10) 0.1158(5) 0.034(4) Uani 1 1 d . . .
H48 H 0.7995 0.3739 0.1304 0.040 Uiso 1 1 calc R . .
C49 C 0.8345(5) 0.4971(12) 0.1348(5) 0.027(4) Uani 1 1 d . . .
C50 C 0.8692(6) 0.4662(12) 0.1723(5) 0.030(4) Uani 1 1 d . . .
C51 C 0.9114(6) 0.5052(15) 0.1790(5) 0.041(5) Uani 1 1 d . . .
H51 H 0.9176 0.5522 0.1602 0.049 Uiso 1 1 calc R . .
C52 C 0.9448(8) 0.4773(18) 0.2122(6) 0.060(6) Uani 1 1 d . . .
H52 H 0.9733 0.5043 0.2160 0.072 Uiso 1 1 calc R . .
C53 C 0.9351(8) 0.4076(18) 0.2405(6) 0.059(6) Uani 1 1 d . . .
H53 H 0.9576 0.3876 0.2633 0.071 Uiso 1 1 calc R . .
C54 C 0.8940(8) 0.3690(15) 0.2352(6) 0.053(6) Uani 1 1 d . . .
H54 H 0.8874 0.3230 0.2543 0.063 Uiso 1 1 calc R . .
C55 C 0.8624(7) 0.3982(13) 0.2018(5) 0.038(4) Uani 1 1 d . . .
H55 H 0.8339 0.3706 0.1983 0.046 Uiso 1 1 calc R . .
N1 N 0.5096(7) 0.1090(16) 0.1511(6) 0.073(6) Uani 1 1 d D . .
C81 C 0.4976(7) 0.1075(16) 0.1157(6) 0.052(5) Uani 1 1 d DU . .
C82 C 0.4760(9) 0.110(2) 0.0745(6) 0.080(8) Uani 1 1 d D . .
H82A H 0.4446 0.1231 0.0734 0.120 Uiso 1 1 calc R . .
H82B H 0.4792 0.0500 0.0610 0.120 Uiso 1 1 calc R . .
H82C H 0.4888 0.1593 0.0595 0.120 Uiso 1 1 calc R . .
N2 N 0.6178(11) 0.621(3) 0.1935(9) 0.131(13) Uani 1 1 d . . .
C83 C 0.5945(10) 0.602(2) 0.2162(9) 0.082(8) Uani 1 1 d . . .
C84 C 0.5640(12) 0.586(3) 0.2434(11) 0.123(14) Uani 1 1 d . . .
H84A H 0.5440 0.6389 0.2422 0.184 Uiso 1 1 calc R . .
H84B H 0.5802 0.5773 0.2725 0.184 Uiso 1 1 calc R . .
H84C H 0.5469 0.5293 0.2342 0.184 Uiso 1 1 calc R . .
N3 N 0.6842(8) 0.437(2) 0.1441(9) 0.088(8) Uani 1 1 d . . .
C85 C 0.6924(12) 0.366(3) 0.1502(9) 0.086(10) Uani 1 1 d . . .
C86 C 0.7109(14) 0.270(2) 0.1592(14) 0.135(16) Uani 1 1 d . . .
H86A H 0.7251 0.2500 0.1360 0.203 Uiso 1 1 calc R . .
H86B H 0.6869 0.2269 0.1617 0.203 Uiso 1 1 calc R . .
H86C H 0.7327 0.2705 0.1858 0.203 Uiso 1 1 calc R . .
N4 N 0.9725(13) 0.961(3) 0.1760(10) 0.138(14) Uani 1 1 d . . .
C87 C 0.9511(9) 0.909(2) 0.1605(8) 0.072(8) Uani 1 1 d . . .
C88 C 0.9245(8) 0.833(2) 0.1428(8) 0.074(7) Uani 1 1 d . . .
H88A H 0.9394 0.7748 0.1526 0.111 Uiso 1 1 calc R . .
H88B H 0.9198 0.8363 0.1118 0.111 Uiso 1 1 calc R . .
H88C H 0.8959 0.8362 0.1518 0.111 Uiso 1 1 calc R . .
N5 N 0.7286(18) 0.690(5) 0.2484(17) 0.031(16) Uiso 0.28(6) 1 d PD A 1
C89 C 0.7407(19) 0.620(4) 0.2366(16) 0.022(17) Uiso 0.28(6) 1 d PD A 1
C90 C 0.769(2) 0.554(4) 0.2281(19) 0.034(18) Uiso 0.28(6) 1 d PD A 1
N5B N 0.716(2) 0.727(5) 0.252(2) 0.04(2) Uiso 0.22(6) 1 d PD A 2
C89B C 0.727(2) 0.655(5) 0.241(3) 0.03(2) Uiso 0.22(6) 1 d PD A 2
C90B C 0.756(2) 0.588(5) 0.2340(16) 0.000(18) Uiso 0.22(6) 1 d PD A 2
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'
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
O14 U1 O11 179.3(5) . .
O14 U1 O13 95.8(4) . 7_665
O11 U1 O13 84.8(4) . 7_665
O14 U1 O2 90.1(4) . .
O11 U1 O2 89.3(4) . .
O13 U1 O2 145.8(4) 7_665 .
O14 U1 O21 91.7(4) . .
O11 U1 O21 88.0(4) . .
O13 U1 O21 145.1(4) 7_665 .
O2 U1 O21 67.9(4) . .
O14 U1 O1 88.4(4) . .
O11 U1 O1 91.4(4) . .
O13 U1 O1 76.6(3) 7_665 .
O2 U1 O1 69.9(3) . .
O21 U1 O1 137.8(4) . .
O14 U1 O22 87.4(4) . .
O11 U1 O22 93.1(4) . .
O13 U1 O22 77.1(3) 7_665 .
O2 U1 O22 137.0(3) . .
O21 U1 O22 69.2(4) . .
O1 U1 O22 152.8(3) . .
O14 U1 K2 128.3(3) . 7_665
O11 U1 K2 51.9(3) . 7_665
O13 U1 K2 54.2(3) 7_665 7_665
O2 U1 K2 96.4(3) . 7_665
O21 U1 K2 138.0(3) . 7_665
O1 U1 K2 47.6(2) . 7_665
O22 U1 K2 118.4(2) . 7_665
O14 U1 K2 124.6(3) . .
O11 U1 K2 56.1(3) . .
O13 U1 K2 50.5(2) 7_665 .
O2 U1 K2 143.8(2) . .
O21 U1 K2 97.8(3) . .
O1 U1 K2 116.5(2) . .
O22 U1 K2 47.6(2) . .
K2 U1 K2 71.62(9) 7_665 .
O14 U1 K1 122.4(3) . .
O11 U1 K1 57.1(3) . .
O13 U1 K1 141.2(3) 7_665 .
O2 U1 K1 50.4(3) . .
O21 U1 K1 39.7(3) . .
O1 U1 K1 108.4(3) . .
O22 U1 K1 96.4(3) . .
K2 U1 K1 99.81(9) 7_665 .
K2 U1 K1 96.91(11) . .
U1 O11 U2 176.3(6) . .
U1 O11 K2 97.9(4) . 7_665
U2 O11 K2 85.7(3) . 7_665
U1 O11 K2 93.7(4) . .
U2 O11 K2 85.2(3) . .
K2 O11 K2 92.0(3) 7_665 .
U1 O11 K1 94.5(4) . .
U2 O11 K1 83.3(3) . .
K2 O11 K1 138.2(4) 7_665 .
K2 O11 K1 126.8(3) . .
O12 U2 O13 177.2(5) . .
O12 U2 O62 87.0(4) . .
O13 U2 O62 94.6(4) . .
O12 U2 O11 92.0(4) . .
O13 U2 O11 85.4(4) . .
O62 U2 O11 143.7(4) . .
O12 U2 O42 88.6(4) . .
O13 U2 O42 94.1(4) . .
O62 U2 O42 71.0(4) . .
O11 U2 O42 145.3(4) . .
O12 U2 O41 88.1(4) . .
O13 U2 O41 92.2(4) . .
O62 U2 O41 140.9(4) . .
O11 U2 O41 75.2(3) . .
O42 U2 O41 70.1(3) . .
O12 U2 O61 86.1(4) . .
O13 U2 O61 92.3(4) . .
O62 U2 O61 68.1(4) . .
O11 U2 O61 75.6(3) . .
O42 U2 O61 138.9(4) . .
O41 U2 O61 150.0(3) . .
O12 U2 K2 126.8(3) . 7_665
O13 U2 K2 52.0(3) . 7_665
O62 U2 K2 145.4(3) . 7_665
O11 U2 K2 53.8(2) . 7_665
O42 U2 K2 99.5(3) . 7_665
O41 U2 K2 48.0(2) . 7_665
O61 U2 K2 116.1(2) . 7_665
O12 U2 K2 124.7(3) . .
O13 U2 K2 52.9(3) . .
O62 U2 K2 95.8(3) . .
O11 U2 K2 55.8(2) . .
O42 U2 K2 144.3(3) . .
O41 U2 K2 118.4(2) . .
O61 U2 K2 46.1(2) . .
K2 U2 K2 72.27(9) 7_665 .
O12 U2 K1 33.1(3) . .
O13 U2 K1 144.2(3) . .
O62 U2 K1 111.1(3) . .
O11 U2 K1 59.1(3) . .
O42 U2 K1 117.2(3) . .
O41 U2 K1 83.5(2) . .
O61 U2 K1 75.7(3) . .
K2 U2 K1 102.95(12) 7_665 .
K2 U2 K1 98.49(9) . .
U2 O12 K1 124.2(5) . .
U2 O13 U1 171.6(5) . 7_665
U2 O13 K2 96.9(4) . 7_665
U1 O13 K2 90.4(3) 7_665 7_665
U2 O13 K2 97.1(4) . .
U1 O13 K2 86.3(3) 7_665 .
K2 O13 K2 95.2(3) 7_665 .
O41 K2 O61 172.9(3) 7_665 .
O41 K2 O1 92.0(3) 7_665 7_665
O61 K2 O1 88.6(3) . 7_665
O41 K2 O22 93.5(3) 7_665 .
O61 K2 O22 85.0(3) . .
O1 K2 O22 170.7(3) 7_665 .
O41 K2 O13 67.9(3) 7_665 7_665
O61 K2 O13 117.3(3) . 7_665
O1 K2 O13 125.6(3) 7_665 7_665
O22 K2 O13 63.5(3) . 7_665
O41 K2 O11 62.2(3) 7_665 7_665
O61 K2 O11 124.3(3) . 7_665
O1 K2 O11 66.0(3) 7_665 7_665
O22 K2 O11 123.3(3) . 7_665
O13 K2 O11 59.9(3) 7_665 7_665
O41 K2 O13 119.9(3) 7_665 .
O61 K2 O13 66.5(3) . .
O1 K2 O13 61.7(3) 7_665 .
O22 K2 O13 121.1(3) . .
O13 K2 O13 84.8(3) 7_665 .
O11 K2 O13 57.9(3) 7_665 .
O41 K2 O11 125.1(3) 7_665 .
O61 K2 O11 60.4(3) . .
O1 K2 O11 117.8(3) 7_665 .
O22 K2 O11 64.4(3) . .
O13 K2 O11 57.3(3) 7_665 .
O11 K2 O11 88.0(3) 7_665 .
O13 K2 O11 56.7(3) . .
O41 K2 U2 41.7(2) 7_665 7_665
O61 K2 U2 144.9(2) . 7_665
O1 K2 U2 102.7(2) 7_665 7_665
O22 K2 U2 86.4(2) . 7_665
O13 K2 U2 31.08(18) 7_665 7_665
O11 K2 U2 40.50(19) 7_665 7_665
O13 K2 U2 89.6(2) . 7_665
O11 K2 U2 85.25(19) . 7_665
O41 K2 U1 84.6(2) 7_665 7_665
O61 K2 U1 100.4(2) . 7_665
O1 K2 U1 40.7(2) 7_665 7_665
O22 K2 U1 147.5(3) . 7_665
O13 K2 U1 86.0(2) 7_665 7_665
O11 K2 U1 30.23(19) 7_665 7_665
O13 K2 U1 39.44(18) . 7_665
O11 K2 U1 90.3(2) . 7_665
U2 K2 U1 70.73(6) 7_665 7_665
O41 K2 U1 101.8(2) 7_665 .
O61 K2 U1 81.6(2) . .
O1 K2 U1 145.1(3) 7_665 .
O22 K2 U1 40.2(2) . .
O13 K2 U1 39.09(18) 7_665 .
O11 K2 U1 92.3(2) 7_665 .
O13 K2 U1 83.7(2) . .
O11 K2 U1 30.16(18) . .
U2 K2 U1 70.12(6) 7_665 .
U1 K2 U1 108.38(9) 7_665 .
O41 K2 U2 146.6(2) 7_665 .
O61 K2 U2 40.4(2) . .
O1 K2 U2 81.6(2) 7_665 .
O22 K2 U2 97.7(2) . .
O13 K2 U2 89.3(2) 7_665 .
O11 K2 U2 85.6(2) 7_665 .
O13 K2 U2 30.03(18) . .
O11 K2 U2 39.01(18) . .
U2 K2 U2 107.72(9) 7_665 .
U1 K2 U2 69.29(6) 7_665 .
U1 K2 U2 69.14(7) . .
O12 K1 O21 113.8(4) . .
O12 K1 N3 79.6(6) . .
O21 K1 N3 145.8(7) . .
O12 K1 N2 120.2(7) . .
O21 K1 N2 110.6(8) . .
N3 K1 N2 85.5(10) . .
O12 K1 O2 106.9(4) . .
O21 K1 O2 56.0(3) . .
N3 K1 O2 90.4(7) . .
N2 K1 O2 130.8(7) . .
O12 K1 O11 60.2(3) . .
O21 K1 O11 59.5(3) . .
N3 K1 O11 109.7(6) . .
N2 K1 O11 164.1(9) . .
O2 K1 O11 56.4(3) . .
O12 K1 C27 122.0(4) . .
O21 K1 C27 16.3(3) . .
N3 K1 C27 153.2(7) . .
N2 K1 C27 94.9(8) . .
O2 K1 C27 69.1(3) . .
O11 K1 C27 74.0(3) . .
O12 K1 U2 22.7(2) . .
O21 K1 U2 92.6(3) . .
N3 K1 U2 92.9(5) . .
N2 K1 U2 140.5(7) . .
O2 K1 U2 88.6(2) . .
O11 K1 U2 37.64(17) . .
C27 K1 U2 103.4(3) . .
O12 K1 U1 88.6(3) . .
O21 K1 U1 36.3(2) . .
N3 K1 U1 119.1(6) . .
N2 K1 U1 146.3(7) . .
O2 K1 U1 37.1(2) . .
O11 K1 U1 28.37(17) . .
C27 K1 U1 52.6(3) . .
U2 K1 U1 65.98(8) . .
C7 O1 U1 125.4(9) . .
C7 O1 K2 140.6(9) . 7_665
U1 O1 K2 91.7(3) . 7_665
C9 O2 U1 124.7(9) . .
C9 O2 K1 142.4(9) . .
U1 O2 K1 92.5(3) . .
C6 C1 C2 119.9(17) . .
C3 C2 C1 121.4(18) . .
C2 C3 C4 118.6(18) . .
C3 C4 C5 120.1(17) . .
C6 C5 C4 122.2(15) . .
C5 C6 C1 117.8(15) . .
C5 C6 C7 122.7(13) . .
C1 C6 C7 119.4(14) . .
O1 C7 C8 123.9(13) . .
O1 C7 C6 117.1(12) . .
C8 C7 C6 119.0(13) . .
C9 C8 C7 124.7(15) . .
O2 C9 C8 124.5(15) . .
O2 C9 C10 116.8(13) . .
C8 C9 C10 118.7(14) . .
C11 C10 C15 118.2(14) . .
C11 C10 C9 119.5(13) . .
C15 C10 C9 122.3(14) . .
C12 C11 C10 122.3(18) . .
C11 C12 C13 117.6(19) . .
C14 C13 C12 122.4(17) . .
C13 C14 C15 118.9(16) . .
C14 C15 C10 120.7(16) . .
C27 O21 U1 128.9(10) . .
C27 O21 K1 126.8(10) . .
U1 O21 K1 103.9(4) . .
C29 O22 U1 124.5(10) . .
C29 O22 K2 142.4(10) . .
U1 O22 K2 92.2(4) . .
C26 C21 C22 121.6(19) . .
C23 C22 C21 120(2) . .
C22 C23 C24 121.1(19) . .
C25 C24 C23 119(2) . .
C24 C25 C26 120(2) . .
C21 C26 C25 118.3(17) . .
C21 C26 C27 117.8(15) . .
C25 C26 C27 124.0(16) . .
O21 C27 C28 124.1(15) . .
O21 C27 C26 118.7(14) . .
C28 C27 C26 117.1(13) . .
O21 C27 K1 36.9(7) . .
C28 C27 K1 148.9(11) . .
C26 C27 K1 88.3(9) . .
C29 C28 C27 124.8(15) . .
O22 C29 C28 123.8(15) . .
O22 C29 C30 117.9(14) . .
C28 C29 C30 118.3(14) . .
C35 C30 C31 118.4(17) . .
C35 C30 C29 121.8(15) . .
C31 C30 C29 119.6(15) . .
C32 C31 C30 119.5(17) . .
C33 C32 C31 120.8(18) . .
C32 C33 C34 121.0(18) . .
C35 C34 C33 118.4(18) . .
C34 C35 C30 121.7(18) . .
C67 O61 U2 123.1(10) . .
C67 O61 K2 142.7(10) . .
U2 O61 K2 93.5(3) . .
C69 O62 U2 125.7(10) . .
C62 C61 C66 119.0(17) . .
C61 C62 C63 122.4(19) . .
C64 C63 C62 116.0(18) . .
C63 C64 C65 123.3(19) . .
C66 C65 C64 118(2) . .
C65 C66 C61 120.7(17) . .
C65 C66 C67 121.3(16) . .
C61 C66 C67 118.0(14) . .
O61 C67 C68 127.1(16) . .
O61 C67 C66 116.2(14) . .
C68 C67 C66 116.7(14) . .
C67 C68 C69 121.9(15) . .
O62 C69 C68 123.8(15) . .
O62 C69 C70 113.7(16) . .
C68 C69 C70 122.5(15) . .
C75 C70 C71 118.0(17) . .
C75 C70 C69 124.0(18) . .
C71 C70 C69 118.0(16) . .
C72 C71 C70 120.8(19) . .
C71 C72 C73 120(2) . .
C74 C73 C72 119.7(19) . .
C73 C74 C75 119(2) . .
C70 C75 C74 122(2) . .
C47 O41 U2 124.5(9) . .
C47 O41 K2 143.7(9) . 7_665
U2 O41 K2 90.3(3) . 7_665
C49 O42 U2 124.6(10) . .
C46 C41 C42 120.5(16) . .
C43 C42 C41 119.9(17) . .
C42 C43 C44 120.5(17) . .
C45 C44 C43 119.8(17) . .
C44 C45 C46 120.1(16) . .
C41 C46 C45 119.1(15) . .
C41 C46 C47 120.0(14) . .
C45 C46 C47 120.8(14) . .
O41 C47 C48 125.4(13) . .
O41 C47 C46 115.9(12) . .
C48 C47 C46 118.7(13) . .
C47 C48 C49 124.5(14) . .
O42 C49 C48 125.4(14) . .
O42 C49 C50 116.2(14) . .
C48 C49 C50 118.4(14) . .
C51 C50 C55 115.6(15) . .
C51 C50 C49 119.9(16) . .
C55 C50 C49 124.4(16) . .
C52 C51 C50 122(2) . .
C51 C52 C53 119(2) . .
C54 C53 C52 120.7(18) . .
C53 C54 C55 118(2) . .
C54 C55 C50 124.5(19) . .
N1 C81 C82 170(3) . .
C83 N2 K1 162(3) . .
N2 C83 C84 176(4) . .
C85 N3 K1 176(3) . .
N3 C85 C86 172(4) . .
N4 C87 C88 174(4) . .
N5 C89 C90 159(4) . .
N5B C89B C90B 157(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 O14 1.808(10) .
U1 O11 1.916(10) .
U1 O13 2.400(9) 7_665
U1 O2 2.428(10) .
U1 O21 2.454(11) .
U1 O1 2.458(11) .
U1 O22 2.461(11) .
U1 K2 3.770(4) 7_665
U1 K2 3.805(4) .
U1 K1 4.020(6) .
O11 U2 2.410(10) .
O11 K2 2.994(11) 7_665
O11 K2 3.165(11) .
O11 K1 3.386(11) .
U2 O12 1.830(10) .
U2 O13 1.924(9) .
U2 O62 2.386(10) .
U2 O42 2.432(11) .
U2 O41 2.461(11) .
U2 O61 2.479(11) .
U2 K2 3.700(4) 7_665
U2 K2 3.815(4) .
U2 K1 3.919(5) .
O12 K1 2.586(11) .
O13 U1 2.400(9) 7_665
O13 K2 2.938(10) 7_665
O13 K2 3.065(11) .
K2 O41 2.752(11) 7_665
K2 O61 2.754(10) .
K2 O1 2.787(11) 7_665
K2 O22 2.811(11) .
K2 O13 2.938(10) 7_665
K2 O11 2.994(11) 7_665
K2 U2 3.700(4) 7_665
K2 U1 3.770(4) 7_665
K1 O21 2.647(12) .
K1 N3 2.80(3) .
K1 N2 2.83(3) .
K1 O2 3.101(12) .
K1 C27 3.531(16) .
O1 C7 1.291(17) .
O1 K2 2.787(11) 7_665
O2 C9 1.295(18) .
C1 C6 1.39(2) .
C1 C2 1.40(3) .
C2 C3 1.37(3) .
C3 C4 1.38(3) .
C4 C5 1.39(2) .
C5 C6 1.37(2) .
C6 C7 1.49(2) .
C7 C8 1.40(2) .
C8 C9 1.39(2) .
C9 C10 1.50(2) .
C10 C11 1.38(2) .
C10 C15 1.39(2) .
C11 C12 1.37(3) .
C12 C13 1.38(3) .
C13 C14 1.36(3) .
C14 C15 1.38(2) .
O21 C27 1.237(18) .
O22 C29 1.289(18) .
C21 C26 1.38(2) .
C21 C22 1.39(3) .
C22 C23 1.31(3) .
C23 C24 1.42(3) .
C24 C25 1.38(3) .
C25 C26 1.39(2) .
C26 C27 1.49(2) .
C27 C28 1.43(2) .
C28 C29 1.39(2) .
C29 C30 1.49(2) .
C30 C35 1.39(2) .
C30 C31 1.40(2) .
C31 C32 1.39(3) .
C32 C33 1.37(3) .
C33 C34 1.39(3) .
C34 C35 1.38(3) .
O61 C67 1.264(18) .
O62 C69 1.31(2) .
C61 C62 1.38(3) .
C61 C66 1.41(2) .
C62 C63 1.39(3) .
C63 C64 1.39(3) .
C64 C65 1.40(3) .
C65 C66 1.35(2) .
C66 C67 1.53(2) .
C67 C68 1.37(2) .
C68 C69 1.40(3) .
C69 C70 1.49(2) .
C70 C75 1.36(3) .
C70 C71 1.38(3) .
C71 C72 1.38(3) .
C72 C73 1.38(3) .
C73 C74 1.37(3) .
C74 C75 1.38(3) .
O41 C47 1.305(17) .
O41 K2 2.752(11) 7_665
O42 C49 1.25(2) .
C41 C46 1.38(2) .
C41 C42 1.39(2) .
C42 C43 1.36(3) .
C43 C44 1.40(3) .
C44 C45 1.38(3) .
C45 C46 1.41(2) .
C46 C47 1.48(2) .
C47 C48 1.35(2) .
C48 C49 1.43(2) .
C49 C50 1.50(2) .
C50 C51 1.38(3) .
C50 C55 1.39(3) .
C51 C52 1.38(3) .
C52 C53 1.41(3) .
C53 C54 1.35(3) .
C54 C55 1.36(3) .
N1 C81 1.117(8) .
C81 C82 1.348(8) .
N2 C83 1.14(4) .
C83 C84 1.41(4) .
N3 C85 1.05(4) .
C85 C86 1.48(5) .
N4 C87 1.04(4) .
C87 C88 1.41(4) .
N5 C89 1.146(10) .
C89 C90 1.348(10) .
N5B C89B 1.150(10) .
C89B C90B 1.350(10) .
