#------------------------------------------------------------------------------
#$Date: 2018-09-21 01:06:52 +0300 (Fri, 21 Sep 2018) $
#$Revision: 211092 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/23/7122364.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_7122364
loop_
_publ_author_name
'Chaudhry, Mohammad'
'Lelj, Francesco'
'MacLachlan, Mark'
_publ_section_title
;
 Expanded Campestarene Hosts for Tetra- and Dinuclear Uranyl(VI) Complexes
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C8CC07269H
_journal_year                    2018
_chemical_formula_moiety         'C42 H49 N2 O5 U'
_chemical_formula_sum            'C42 H49 N2 O5 U'
_chemical_formula_weight         899.86
_chemical_name_systematic        'UO2 4 tOct Ph'
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a'
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-03-27
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-08-16 deposited with the CCDC.
2018-09-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   29.7978(13)
_cell_length_b                   29.7978(13)
_cell_length_c                   21.0965(10)
_cell_measurement_reflns_used    9986
_cell_measurement_temperature    90
_cell_measurement_theta_max      25.369
_cell_measurement_theta_min      2.27
_cell_volume                     18731.8(15)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      90.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0632
_diffrn_reflns_av_unetI/netI     0.0608
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            33974
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.371
_diffrn_reflns_theta_min         1.808
_exptl_absorpt_coefficient_mu    3.503
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5683
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1286 before and 0.0528 after correction. The Ratio of minimum to maximum transmission is 0.7626. The λ/2 correction factor is Not present.'
_exptl_crystal_colour            'metallic dark red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.276
_exptl_crystal_description       plate
_exptl_crystal_F_000             7152
_exptl_crystal_preparation
'UO2 salt mixed with my monomer in ethanol and refluxed.'
_exptl_crystal_recrystallization_method
'Vapour diffusion of pentane into acetone'
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.18
_refine_diff_density_max         3.584
_refine_diff_density_min         -1.347
_refine_diff_density_rms         0.148
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     548
_refine_ls_number_reflns         8591
_refine_ls_number_restraints     1222
_refine_ls_restrained_S_all      0.972
_refine_ls_R_factor_all          0.0898
_refine_ls_R_factor_gt           0.0520
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0629P)²+204.7400P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1240
_refine_ls_wR_factor_ref         0.1479
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5569
_reflns_number_total             8591
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8cc07269h2.cif
_cod_data_source_block           mm391_sq
_cod_original_cell_volume        18731.8(19)
_cod_database_code               7122364
_shelx_shelxl_version_number     2017/1
_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.
;
_shelx_estimated_absorpt_t_max   0.571
_shelx_estimated_absorpt_t_min   0.249
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C27-C51 = C28-C51 = C29-C51 = C29-C31 = C32-C31 = C30-C31 = C31-C33
 1.54 with sigma of 0.02
 C52-C51 = C53-C51 = C54-C51 = C54-C55 = C55-C57 = C58-C55 = C55-C56
 1.54 with sigma of 0.02
 C7-C5 = C6-C5 = C8-C5 = C9-C8 = C9-C10 = C9-C12 = C9-C11
 1.54 with sigma of 0.02
 C43-C44 = C43-C45 = C46-C43 = C46-C47 = C50-C47 = C49-C47 = C47-C48
 1.54 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
Uanis(C39) = Uanis(C37)
Uanis(C50) = Uanis(C47)
Uanis(C37) = Uanis(C38) = Uanis(C39)
Uanis(C12) = Uanis(C9) = Uanis(C10) = Uanis(C11)
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C52)=Sof(H52A)=Sof(H52B)=Sof(H52C)=Sof(C53)=Sof(H53A)=Sof(H53B)=Sof(H53C)=
 Sof(C54)=Sof(H54A)=Sof(H54B)=Sof(C55)=Sof(C56)=Sof(H56A)=Sof(H56B)=Sof(H56C)=
 Sof(C57)=Sof(H57A)=Sof(H57B)=Sof(H57C)=Sof(C58)=Sof(H58A)=Sof(H58B)=Sof(H58C)=
 1-FVAR(1)
 Sof(C27)=Sof(H27A)=Sof(H27B)=Sof(H27C)=Sof(C28)=Sof(H28A)=Sof(H28B)=Sof(H28C)=
 Sof(C29)=Sof(H29A)=Sof(H29B)=Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(H30C)=Sof(C31)=
 Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(H32C)=Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(H33C)=
 FVAR(1)
 Sof(C43)=Sof(C44)=Sof(H44A)=Sof(H44B)=Sof(H44C)=Sof(C45)=Sof(H45A)=Sof(H45B)=
 Sof(H45C)=Sof(C46)=Sof(H46A)=Sof(H46B)=Sof(C47)=Sof(C48)=Sof(H48A)=Sof(H48B)=
 Sof(H48C)=Sof(C49)=Sof(H49A)=Sof(H49B)=Sof(H49C)=Sof(C50)=Sof(H50A)=Sof(H50B)=
 Sof(H50C)=1-FVAR(2)
 Sof(C5)=Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(H6C)=Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(H7C)=
 Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(C9)=Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(H10C)=
 Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(H11C)=Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(H12C)=
 FVAR(2)
6.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C29(H29A,H29B), C46(H46A,H46B), C54(H54A,H54B)
6.b Aromatic/amide H refined with riding coordinates:
 N2(H2), C3(H3), C19(H19), C15(H15), C16(H16), C17(H17), C18(H18), C21(H21),
 C23(H23), C40(H40), C39(H39), C38(H38), C37(H37), C36(H36), C42(H42)
6.c Fitted hexagon refined as free rotating group:
 C19(C14,C15,C16,C17,C18), C35(C40,C39,C38,C37,C36)
6.d Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C),
 C12(H12A,H12B,H12C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C30(H30A,H30B,
 H30C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C44(H44A,H44B,H44C), C45(H45A,
 H45B,H45C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C), C50(H50A,H50B,H50C),
 C52(H52A,H52B,H52C), C53(H53A,H53B,H53C), C56(H56A,H56B,H56C), C57(H57A,H57B,
 H57C), C58(H58A,H58B,H58C)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.59468(2) 0.71103(2) 0.62830(2) 0.02878(12) Uani 1 1 d . U . . .
O1 O 0.60655(17) 0.64122(18) 0.6773(2) 0.0343(12) Uani 1 1 d . U . . .
O2 O 0.64959(17) 0.75873(18) 0.5764(2) 0.0359(12) Uani 1 1 d . U . . .
O3 O 0.55621(17) 0.77228(17) 0.5882(3) 0.0341(13) Uani 1 1 d . U . . .
O4 O 0.60244(17) 0.73805(17) 0.7027(3) 0.0341(12) Uani 1 1 d . U . . .
O5 O 0.58888(17) 0.68313(17) 0.5548(3) 0.0348(12) Uani 1 1 d . U . . .
N1 N 0.6789(2) 0.6888(2) 0.6373(3) 0.0348(14) Uani 1 1 d . U . . .
N2 N 0.6548(2) 0.8153(2) 0.4853(3) 0.0356(15) Uani 1 1 d . U . . .
H2 H 0.643891 0.803839 0.520521 0.043 Uiso 1 1 calc R . . . .
C1 C 0.6263(3) 0.6389(3) 0.7313(4) 0.0348(18) Uani 1 1 d . U . . .
C2 C 0.6705(3) 0.6579(3) 0.7420(4) 0.0381(18) Uani 1 1 d . U . . .
C3 C 0.6869(3) 0.6573(3) 0.8038(4) 0.046(2) Uani 1 1 d . U . . .
H3 H 0.715403 0.670564 0.811076 0.055 Uiso 1 1 calc R . . . .
C4 C 0.6649(3) 0.6390(3) 0.8556(5) 0.055(2) Uani 1 1 d . U . . .
C5 C 0.6904(9) 0.6408(11) 0.9217(17) 0.058(5) Uani 0.52(3) 1 d D U P A 1
C6 C 0.6629(10) 0.6141(12) 0.9698(18) 0.062(7) Uani 0.52(3) 1 d D U P A 1
H6A H 0.633077 0.627560 0.973980 0.093 Uiso 0.52(3) 1 calc GR . P A 1
H6B H 0.678142 0.614640 1.010989 0.093 Uiso 0.52(3) 1 calc GR . P A 1
H6C H 0.659980 0.582993 0.955328 0.093 Uiso 0.52(3) 1 calc GR . P A 1
C7 C 0.6939(15) 0.6909(12) 0.939(3) 0.066(8) Uani 0.52(3) 1 d D U P A 1
H7A H 0.718021 0.704881 0.914785 0.099 Uiso 0.52(3) 1 calc GR . P A 1
H7B H 0.700537 0.693684 0.984746 0.099 Uiso 0.52(3) 1 calc GR . P A 1
H7C H 0.665415 0.705869 0.929999 0.099 Uiso 0.52(3) 1 calc GR . P A 1
C8 C 0.7402(9) 0.6266(9) 0.9183(18) 0.060(5) Uani 0.52(3) 1 d D U P A 1
H8A H 0.754046 0.643607 0.883020 0.071 Uiso 0.52(3) 1 calc R . P A 1
H8B H 0.754742 0.637052 0.957789 0.071 Uiso 0.52(3) 1 calc R . P A 1
C9 C 0.7533(7) 0.5772(8) 0.9094(11) 0.069(4) Uani 0.52(3) 1 d D U P A 1
C10 C 0.7203(11) 0.5527(18) 0.8656(18) 0.069(4) Uani 0.52(3) 1 d D U P A 1
H10A H 0.689662 0.562415 0.875102 0.104 Uiso 0.52(3) 1 calc GR . P A 1
H10B H 0.722859 0.520241 0.872385 0.104 Uiso 0.52(3) 1 calc GR . P A 1
H10C H 0.727452 0.559701 0.821337 0.104 Uiso 0.52(3) 1 calc GR . P A 1
C11 C 0.7517(9) 0.5517(9) 0.9730(11) 0.069(4) Uani 0.52(3) 1 d D U P A 1
H11A H 0.779055 0.558061 0.997253 0.104 Uiso 0.52(3) 1 calc GR . P A 1
H11B H 0.749653 0.519415 0.964849 0.104 Uiso 0.52(3) 1 calc GR . P A 1
H11C H 0.725459 0.561501 0.997298 0.104 Uiso 0.52(3) 1 calc GR . P A 1
C12 C 0.8012(7) 0.5725(9) 0.8862(15) 0.069(4) Uani 0.52(3) 1 d D U P A 1
H12A H 0.801322 0.558531 0.844189 0.104 Uiso 0.52(3) 1 calc GR . P A 1
H12B H 0.818231 0.553764 0.915873 0.104 Uiso 0.52(3) 1 calc GR . P A 1
H12C H 0.815169 0.602275 0.883613 0.104 Uiso 0.52(3) 1 calc GR . P A 1
C13 C 0.6975(3) 0.6748(3) 0.6896(4) 0.0374(17) Uani 1 1 d . U . . .
C19 C 0.76937(17) 0.71668(15) 0.6959(3) 0.0399(19) Uani 1 1 d . U . . .
H19 H 0.753636 0.742653 0.682218 0.048 Uiso 1 1 calc R . . . .
C14 C 0.74724(13) 0.67571(18) 0.7000(3) 0.0411(19) Uani 1 1 d G U . . .
C15 C 0.77026(18) 0.63771(15) 0.7200(3) 0.051(2) Uani 1 1 d G U . . .
H15 H 0.755136 0.609712 0.722787 0.062 Uiso 1 1 calc R . . . .
C16 C 0.81541(18) 0.64067(17) 0.7360(3) 0.063(3) Uani 1 1 d G U . . .
H16 H 0.831146 0.614694 0.749751 0.076 Uiso 1 1 calc R . . . .
C17 C 0.83754(13) 0.6816(2) 0.7320(3) 0.055(2) Uani 1 1 d G U . . .
H17 H 0.868402 0.683655 0.742948 0.066 Uiso 1 1 calc R . . . .
C18 C 0.81452(17) 0.71964(16) 0.7119(3) 0.048(2) Uani 1 1 d G U . . .
H18 H 0.829647 0.747635 0.709182 0.057 Uiso 1 1 calc R . . . .
C20 C 0.7029(3) 0.7015(3) 0.5831(4) 0.0370(17) Uani 1 1 d . U . . .
C21 C 0.7393(3) 0.6788(3) 0.5577(4) 0.0419(19) Uani 1 1 d . U . . .
H21 H 0.750806 0.653448 0.579584 0.050 Uiso 1 1 calc R . . . .
C22 C 0.7595(3) 0.6920(3) 0.5010(5) 0.052(2) Uani 1 1 d . U . . .
C23 C 0.7418(3) 0.7297(3) 0.4701(4) 0.046(2) Uani 1 1 d . U . . .
H23 H 0.755569 0.739540 0.431921 0.055 Uiso 1 1 calc R . . . .
C24 C 0.7047(3) 0.7534(3) 0.4932(4) 0.0406(19) Uani 1 1 d . U . . .
C25 C 0.6840(3) 0.7394(3) 0.5513(4) 0.0344(17) Uani 1 1 d . U . . .
C27 C 0.8206(6) 0.6330(7) 0.5198(9) 0.075(6) Uani 0.595(13) 1 d D U P B 1
H27A H 0.832038 0.648531 0.557393 0.113 Uiso 0.595(13) 1 calc GR . P B 1
H27B H 0.845398 0.617286 0.498649 0.113 Uiso 0.595(13) 1 calc GR . P B 1
H27C H 0.797729 0.611156 0.532505 0.113 Uiso 0.595(13) 1 calc GR . P B 1
C28 C 0.8379(7) 0.7007(8) 0.4573(15) 0.098(8) Uani 0.595(13) 1 d D U P B 1
H28A H 0.826594 0.722173 0.425973 0.147 Uiso 0.595(13) 1 calc GR . P B 1
H28B H 0.863520 0.684373 0.439521 0.147 Uiso 0.595(13) 1 calc GR . P B 1
H28C H 0.847312 0.716756 0.495540 0.147 Uiso 0.595(13) 1 calc GR . P B 1
C29 C 0.7854(6) 0.6414(6) 0.4131(8) 0.076(4) Uani 0.595(13) 1 d D U P B 1
H29A H 0.782018 0.664645 0.379930 0.091 Uiso 0.595(13) 1 calc R . P B 1
H29B H 0.811517 0.622879 0.400441 0.091 Uiso 0.595(13) 1 calc R . P B 1
C30 C 0.7479(10) 0.5833(7) 0.3447(9) 0.092(7) Uani 0.595(13) 1 d D U P B 1
H30A H 0.748984 0.604025 0.308596 0.139 Uiso 0.595(13) 1 calc GR . P B 1
H30B H 0.721901 0.563466 0.340362 0.139 Uiso 0.595(13) 1 calc GR . P B 1
H30C H 0.775442 0.565356 0.345674 0.139 Uiso 0.595(13) 1 calc GR . P B 1
C31 C 0.7439(7) 0.6105(6) 0.4071(9) 0.077(5) Uani 0.595(13) 1 d D U P B 1
C32 C 0.7382(9) 0.5783(7) 0.4628(9) 0.077(6) Uani 0.595(13) 1 d D U P B 1
H32A H 0.765049 0.559533 0.466729 0.116 Uiso 0.595(13) 1 calc GR . P B 1
H32B H 0.711934 0.559164 0.455515 0.116 Uiso 0.595(13) 1 calc GR . P B 1
H32C H 0.733923 0.595509 0.501932 0.116 Uiso 0.595(13) 1 calc GR . P B 1
C33 C 0.7004(9) 0.6393(10) 0.3994(17) 0.087(7) Uani 0.595(13) 1 d D U P B 1
H33A H 0.692500 0.652797 0.440246 0.131 Uiso 0.595(13) 1 calc GR . P B 1
H33B H 0.675778 0.620147 0.384840 0.131 Uiso 0.595(13) 1 calc GR . P B 1
H33C H 0.705747 0.663128 0.368194 0.131 Uiso 0.595(13) 1 calc GR . P B 1
C34 C 0.6873(3) 0.7912(3) 0.4605(4) 0.0402(19) Uani 1 1 d . U . . .
C35 C 0.7072(2) 0.8044(2) 0.3977(3) 0.054(2) Uani 1 1 d . U . . .
C40 C 0.6959(3) 0.7799(2) 0.3441(3) 0.085(3) Uani 1 1 d G U . . .
H40 H 0.674583 0.756221 0.347056 0.103 Uiso 1 1 calc R . . . .
C39 C 0.7157(3) 0.7898(3) 0.2861(3) 0.112(3) Uani 1 1 d G U . . .
H39 H 0.707921 0.773013 0.249471 0.134 Uiso 1 1 calc R . . . .
C38 C 0.7469(3) 0.8244(3) 0.2818(3) 0.112(3) Uani 1 1 d G U . . .
H38 H 0.760385 0.831217 0.242172 0.134 Uiso 1 1 calc R . . . .
C37 C 0.7582(3) 0.8490(3) 0.3354(4) 0.112(3) Uani 1 1 d G U . . .
H37 H 0.779512 0.872628 0.332460 0.134 Uiso 1 1 calc R . . . .
C36 C 0.7384(3) 0.8390(2) 0.3934(3) 0.079(3) Uani 1 1 d G U . . .
H36 H 0.746174 0.855836 0.430047 0.094 Uiso 1 1 calc R . . . .
C41 C 0.6337(3) 0.8561(3) 0.4671(4) 0.0392(19) Uani 1 1 d . U . . .
C42 C 0.6318(3) 0.8741(3) 0.4065(4) 0.049(2) Uani 1 1 d . U . . .
H42 H 0.645098 0.858106 0.372319 0.059 Uiso 1 1 calc R . . . .
C43 C 0.6793(10) 0.6467(12) 0.9216(18) 0.062(5) Uani 0.48(3) 1 d D U P A 2
C44 C 0.6800(17) 0.6971(13) 0.937(3) 0.071(9) Uani 0.48(3) 1 d D U P A 2
H44A H 0.700254 0.712630 0.907924 0.106 Uiso 0.48(3) 1 calc GR . P A 2
H44B H 0.690446 0.701466 0.980820 0.106 Uiso 0.48(3) 1 calc GR . P A 2
H44C H 0.649625 0.709454 0.932833 0.106 Uiso 0.48(3) 1 calc GR . P A 2
C45 C 0.6464(12) 0.6299(15) 0.9723(19) 0.081(9) Uani 0.48(3) 1 d D U P A 2
H45A H 0.618846 0.647842 0.970552 0.121 Uiso 0.48(3) 1 calc GR . P A 2
H45B H 0.660153 0.632961 1.014239 0.121 Uiso 0.48(3) 1 calc GR . P A 2
H45C H 0.639219 0.598344 0.964345 0.121 Uiso 0.48(3) 1 calc GR . P A 2
C46 C 0.7270(11) 0.6272(11) 0.929(2) 0.076(6) Uani 0.48(3) 1 d D U P A 2
H46A H 0.746089 0.642775 0.897755 0.091 Uiso 0.48(3) 1 calc R . P A 2
H46B H 0.737720 0.636689 0.971523 0.091 Uiso 0.48(3) 1 calc R . P A 2
C47 C 0.7377(9) 0.5770(10) 0.9234(12) 0.085(6) Uani 0.48(3) 1 d D U P A 2
C48 C 0.7232(14) 0.5510(10) 0.9831(13) 0.098(10) Uani 0.48(3) 1 d D U P A 2
H48A H 0.737710 0.564132 1.020438 0.148 Uiso 0.48(3) 1 calc GR . P A 2
H48B H 0.732057 0.519510 0.978984 0.148 Uiso 0.48(3) 1 calc GR . P A 2
H48C H 0.690516 0.552967 0.987847 0.148 Uiso 0.48(3) 1 calc GR . P A 2
C49 C 0.7895(9) 0.5796(10) 0.929(2) 0.098(9) Uani 0.48(3) 1 d D U P A 2
H49A H 0.801769 0.593886 0.890781 0.148 Uiso 0.48(3) 1 calc GR . P A 2
H49B H 0.801750 0.549183 0.932824 0.148 Uiso 0.48(3) 1 calc GR . P A 2
H49C H 0.797627 0.597211 0.966267 0.148 Uiso 0.48(3) 1 calc GR . P A 2
C50 C 0.7283(15) 0.554(2) 0.8594(18) 0.085(6) Uani 0.48(3) 1 d D U P A 2
H50A H 0.696132 0.547081 0.855951 0.127 Uiso 0.48(3) 1 calc GR . P A 2
H50B H 0.745396 0.525705 0.856956 0.127 Uiso 0.48(3) 1 calc GR . P A 2
H50C H 0.737228 0.573586 0.824592 0.127 Uiso 0.48(3) 1 calc GR . P A 2
C51 C 0.8002(4) 0.6669(3) 0.4745(5) 0.068(3) Uani 1 1 d D U . . .
C52 C 0.8376(8) 0.6735(13) 0.5268(13) 0.093(8) Uani 0.405(13) 1 d D U P B 2
H52A H 0.844712 0.705483 0.530813 0.140 Uiso 0.405(13) 1 calc GR . P B 2
H52B H 0.864667 0.656969 0.514550 0.140 Uiso 0.405(13) 1 calc GR . P B 2
H52C H 0.826596 0.662131 0.567556 0.140 Uiso 0.405(13) 1 calc GR . P B 2
C53 C 0.8237(12) 0.6904(11) 0.4187(14) 0.073(8) Uani 0.405(13) 1 d D U P B 2
H53A H 0.803082 0.692291 0.382654 0.110 Uiso 0.405(13) 1 calc GR . P B 2
H53B H 0.850363 0.673196 0.406470 0.110 Uiso 0.405(13) 1 calc GR . P B 2
H53C H 0.832711 0.720706 0.431563 0.110 Uiso 0.405(13) 1 calc GR . P B 2
C54 C 0.7921(11) 0.6169(6) 0.4688(15) 0.085(6) Uani 0.405(13) 1 d D U P B 2
H54A H 0.780003 0.605851 0.509624 0.102 Uiso 0.405(13) 1 calc R . P B 2
H54B H 0.821307 0.601903 0.461771 0.102 Uiso 0.405(13) 1 calc R . P B 2
C55 C 0.7601(12) 0.6026(12) 0.4161(15) 0.096(8) Uani 0.405(13) 1 d D U P B 2
C56 C 0.7424(18) 0.5566(12) 0.438(2) 0.126(12) Uani 0.405(13) 1 d D U P B 2
H56A H 0.766992 0.534814 0.438228 0.189 Uiso 0.405(13) 1 calc GR . P B 2
H56B H 0.718812 0.546417 0.408992 0.189 Uiso 0.405(13) 1 calc GR . P B 2
H56C H 0.729980 0.559333 0.480913 0.189 Uiso 0.405(13) 1 calc GR . P B 2
C57 C 0.7172(15) 0.6288(17) 0.404(2) 0.106(11) Uani 0.405(13) 1 d D U P B 2
H57A H 0.699992 0.631071 0.443668 0.159 Uiso 0.405(13) 1 calc GR . P B 2
H57B H 0.699111 0.613346 0.372072 0.159 Uiso 0.405(13) 1 calc GR . P B 2
H57C H 0.724681 0.659016 0.389075 0.159 Uiso 0.405(13) 1 calc GR . P B 2
C58 C 0.7841(16) 0.5986(17) 0.3516(17) 0.124(12) Uani 0.405(13) 1 d D U P B 2
H58A H 0.794974 0.628199 0.338526 0.186 Uiso 0.405(13) 1 calc GR . P B 2
H58B H 0.762958 0.587158 0.319844 0.186 Uiso 0.405(13) 1 calc GR . P B 2
H58C H 0.809468 0.577891 0.355446 0.186 Uiso 0.405(13) 1 calc GR . P B 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'
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
O1 U1 O2 127.97(18) . .
O1 U1 N1 66.29(19) . .
O2 U1 N1 62.08(19) . .
O3 U1 O1 158.93(18) . .
O3 U1 O1 79.07(18) 15_566 .
O3 U1 O2 152.95(18) 15_566 .
O3 U1 O2 72.99(18) . .
O3 U1 O3 80.0(3) . 15_566
O3 U1 N1 144.66(19) 15_566 .
O3 U1 N1 134.78(19) . .
O4 U1 O1 89.6(2) . .
O4 U1 O2 92.6(2) . .
O4 U1 O3 91.7(2) . .
O4 U1 O3 87.3(2) . 15_566
O4 U1 N1 85.7(2) . .
O5 U1 O1 89.1(2) . .
O5 U1 O2 86.9(2) . .
O5 U1 O3 90.1(2) . .
O5 U1 O3 94.1(2) . 15_566
O5 U1 O4 177.9(2) . .
O5 U1 N1 92.2(2) . .
C1 O1 U1 120.5(5) . .
C25 O2 U1 117.3(5) . .
U1 O3 U1 136.8(3) . 12_767
U1 O3 O3 50.19(19) . 15_566
U1 O3 O3 119.6(3) 12_767 15_566
U1 O3 O3 49.83(18) 12_767 12_767
U1 O3 O3 117.7(3) . 12_767
O3 O3 O3 74.28(18) 15_566 12_767
C13 N1 U1 123.6(5) . .
C13 N1 C20 124.1(7) . .
C20 N1 U1 111.4(5) . .
C34 N2 C41 133.3(7) . .
O1 C1 C2 122.2(7) . .
O1 C1 C41 120.9(7) . 15_566
C41 C1 C2 116.9(7) 15_566 .
C1 C2 C13 121.2(7) . .
C3 C2 C1 117.3(8) . .
C3 C2 C13 121.4(8) . .
C4 C3 C2 125.3(8) . .
C3 C4 C5 116.9(13) . .
C3 C4 C42 116.4(8) . 15_566
C3 C4 C43 123.1(15) . .
C42 C4 C5 126.5(13) 15_566 .
C42 C4 C43 119.8(15) 15_566 .
C6 C5 C4 108(2) . .
C6 C5 C7 112(3) . .
C6 C5 C8 114(2) . .
C7 C5 C4 106(3) . .
C7 C5 C8 102(2) . .
C8 C5 C4 114(2) . .
C9 C8 C5 121(2) . .
C8 C9 C10 112(3) . .
C8 C9 C11 111(2) . .
C10 C9 C11 106(3) . .
C12 C9 C8 111.6(18) . .
C12 C9 C10 111(2) . .
C12 C9 C11 105.3(18) . .
N1 C13 C2 121.3(7) . .
N1 C13 C14 122.5(7) . .
C2 C13 C14 116.2(7) . .
C14 C19 C18 120.0 . .
C19 C14 C13 118.5(5) . .
C15 C14 C13 121.1(5) . .
C15 C14 C19 120.0 . .
C14 C15 C16 120.0 . .
C17 C16 C15 120.0 . .
C16 C17 C18 120.0 . .
C17 C18 C19 120.0 . .
N1 C20 C25 113.2(7) . .
C21 C20 N1 125.7(8) . .
C21 C20 C25 120.9(8) . .
C20 C21 C22 122.1(8) . .
C21 C22 C23 117.5(8) . .
C21 C22 C51 121.2(8) . .
C23 C22 C51 121.2(8) . .
C24 C23 C22 122.6(8) . .
C23 C24 C25 119.4(8) . .
C23 C24 C34 121.3(8) . .
C34 C24 C25 119.2(8) . .
O2 C25 C20 118.3(7) . .
O2 C25 C24 124.2(7) . .
C20 C25 C24 117.4(7) . .
C31 C29 C51 125.5(15) . .
C29 C31 C30 108.5(17) . .
C29 C31 C33 110.2(18) . .
C30 C31 C33 105.3(19) . .
C32 C31 C29 113.5(18) . .
C32 C31 C30 109.5(16) . .
C32 C31 C33 109.5(19) . .
N2 C34 C24 120.6(8) . .
N2 C34 C35 119.9(7) . .
C24 C34 C35 119.4(7) . .
C40 C35 C34 118.8(6) . .
C40 C35 C36 120.0 . .
C36 C35 C34 121.1(6) . .
C35 C40 C39 120.0 . .
C38 C39 C40 120.0 . .
C37 C38 C39 120.0 . .
C38 C37 C36 120.0 . .
C37 C36 C35 120.0 . .
C1 C41 N2 111.5(7) 12_767 .
C42 C41 N2 126.8(8) . .
C42 C41 C1 121.6(8) . 12_767
C4 C42 C41 121.7(9) 12_767 .
C4 C43 C44 111(3) . .
C4 C43 C45 115(3) . .
C4 C43 C46 108(3) . .
C44 C43 C46 109(2) . .
C45 C43 C44 100(4) . .
C45 C43 C46 113(2) . .
C47 C46 C43 123(3) . .
C46 C47 C48 111(3) . .
C46 C47 C49 99(2) . .
C46 C47 C50 118(4) . .
C48 C47 C49 104(2) . .
C48 C47 C50 116(3) . .
C50 C47 C49 106(3) . .
C22 C51 C28 110.1(12) . .
C22 C51 C29 108.5(10) . .
C22 C51 C52 104.1(14) . .
C22 C51 C53 114.8(15) . .
C27 C51 C22 114.4(10) . .
C27 C51 C28 106.7(15) . .
C27 C51 C29 108.1(13) . .
C28 C51 C29 109.0(15) . .
C53 C51 C52 99(2) . .
C54 C51 C22 112.5(14) . .
C54 C51 C52 106.9(19) . .
C54 C51 C53 117.4(19) . .
C51 C54 C55 116(2) . .
C54 C55 C56 104(3) . .
C54 C55 C58 112(3) . .
C56 C55 C58 111(3) . .
C57 C55 C54 120(3) . .
C57 C55 C56 103(4) . .
C57 C55 C58 106(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 O1 2.350(5) .
U1 O2 2.428(5) .
U1 O3 2.315(5) .
U1 O3 2.328(5) 15_566
U1 O4 1.779(5) .
U1 O5 1.768(5) .
U1 N1 2.602(6) .
O1 C1 1.284(9) .
O2 C25 1.290(9) .
O3 O3 2.984(8) 15_566
O3 O3 2.984(8) 12_767
N1 C13 1.304(10) .
N1 C20 1.401(10) .
N2 C34 1.313(10) .
N2 C41 1.420(10) .
C1 C2 1.451(11) .
C1 C41 1.414(11) 15_566
C2 C3 1.392(11) .
C2 C13 1.458(12) .
C3 C4 1.385(12) .
C4 C5 1.59(4) .
C4 C42 1.388(12) 15_566
C4 C43 1.47(4) .
C5 C6 1.527(17) .
C5 C7 1.542(18) .
C5 C8 1.546(17) .
C8 C9 1.533(17) .
C9 C10 1.535(18) .
C9 C11 1.543(17) .
C9 C12 1.515(17) .
C13 C14 1.499(9) .
C19 C14 1.3900 .
C19 C18 1.3900 .
C14 C15 1.3900 .
C15 C16 1.3900 .
C16 C17 1.3900 .
C17 C18 1.3900 .
C20 C21 1.385(11) .
C20 C25 1.428(11) .
C21 C22 1.395(12) .
C22 C23 1.402(12) .
C22 C51 1.530(13) .
C23 C24 1.399(12) .
C24 C25 1.434(11) .
C24 C34 1.421(12) .
C27 C51 1.520(15) .
C28 C51 1.551(16) .
C29 C31 1.548(17) .
C29 C51 1.563(15) .
C30 C31 1.550(17) .
C31 C32 1.528(17) .
C31 C33 1.561(17) .
C34 C35 1.504(10) .
C35 C40 1.3900 .
C35 C36 1.3900 .
C40 C39 1.3900 .
C39 C38 1.3900 .
C38 C37 1.3900 .
C37 C36 1.3900 .
C41 C42 1.389(11) .
C43 C44 1.540(18) .
C43 C45 1.533(18) .
C43 C46 1.543(18) .
C46 C47 1.534(18) .
C47 C48 1.541(18) .
C47 C49 1.548(18) .
C47 C50 1.544(19) .
C51 C52 1.583(18) .
C51 C53 1.538(17) .
C51 C54 1.515(17) .
C54 C55 1.524(19) .
C55 C56 1.539(19) .
C55 C57 1.521(19) .
C55 C58 1.541(19) .
