#------------------------------------------------------------------------------
#$Date: 2023-12-07 04:52:34 +0200 (Thu, 07 Dec 2023) $
#$Revision: 288111 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/31/23/2312365.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2312365
loop_
_publ_author_name
'Whittington, Abigail A.'
'Keimowitz, Alison R.'
'Tanski, Joseph M.'
_publ_section_title
;
Crystal structures of three uranyl-acetate-bipyridine complexes
crystallized from hydraulic fracking fluid.
;
_journal_coeditor_code EQ3014
_journal_issue 1
_journal_name_full
'Acta crystallographica. Section C, Structural chemistry'
_journal_paper_doi 10.1107/S2053229623010288
_journal_volume 80
_journal_year 2024
_chemical_formula_iupac '[U (C2 H3 O2)2 O2 (C10 H8 N2)]'
_chemical_formula_moiety 'C14 H14 N2 O6 U'
_chemical_formula_sum 'C14 H14 N2 O6 U'
_chemical_formula_weight 544.30
_chemical_name_systematic
Bis(acetato-\k^2^O,O')(2,2'-bipyridine-\k^2^N,N')dioxidouranium(VI)
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_Hall '-P 2yn'
_space_group_name_H-M_alt 'P 1 21/n 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary dual
_atom_sites_solution_secondary difmap
_cell_angle_alpha 90
_cell_angle_beta 96.106(2)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 7.7340(8)
_cell_length_b 19.010(2)
_cell_length_c 10.6154(11)
_cell_measurement_reflns_used 9880
_cell_measurement_temperature 125.(2)
_cell_measurement_theta_max 30.5391
_cell_measurement_theta_min 2.2079
_cell_volume 1551.9(3)
_computing_cell_refinement
;
SAINT (Bruker, 2013)
;
_computing_data_collection
;
APEX3 (Bruker, 2013)
;
_computing_data_reduction
;
SAINT (Bruker, 2013)
;
_computing_molecular_graphics
;
SHELXTL2014 (Sheldrick, 2008)
;
_computing_publication_material
;
SHELXTL2014 (Sheldrick, 2008),
OLEX2 (Dolomanov et al., 2009), and
Mercury (Macrae et al., 2020)
;
_computing_structure_refinement
;
SHELXL2017 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2018 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 125.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device 'three-circle diffractometer'
_diffrn_measurement_device_type 'Bruker APEXII CCD'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_probe x-ray
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0277
_diffrn_reflns_av_unetI/netI 0.0160
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_h_min -10
_diffrn_reflns_limit_k_max 26
_diffrn_reflns_limit_k_min -26
_diffrn_reflns_limit_l_max 15
_diffrn_reflns_limit_l_min -15
_diffrn_reflns_number 37906
_diffrn_reflns_theta_full 25.24
_diffrn_reflns_theta_max 30.53
_diffrn_reflns_theta_min 2.14
_diffrn_source 'sealed X-ray tube'
_diffrn_source_current 30.0
_diffrn_source_power 1.50
_diffrn_source_voltage 50
_exptl_absorpt_coefficient_mu 10.492
_exptl_absorpt_correction_T_max 0.42
_exptl_absorpt_correction_T_min 0.28
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(SADABS: Bruker, 2013)
;
_exptl_crystal_colour yellow
_exptl_crystal_density_diffrn 2.330
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 1008
_exptl_crystal_size_max 0.200
_exptl_crystal_size_mid 0.200
_exptl_crystal_size_min 0.100
_refine_diff_density_max 1.061
_refine_diff_density_min -0.556
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.077
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 210
_refine_ls_number_reflns 4720
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.077
_refine_ls_R_factor_all 0.0193
_refine_ls_R_factor_gt 0.0157
_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/[\s^2^(Fo^2^)+(0.0136P)^2^+1.5912P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0337
_refine_ls_wR_factor_ref 0.0346
_reflns_number_gt 4280
_reflns_number_total 4720
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file eq3014sup1.cif
_cod_data_source_block I_AW2829U
_cod_database_code 2312365
_shelx_hkl_file
;
1 0 0 7.20 1.10
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2 2 0 4009.20 84.59
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0 -3 0 3.10 0.70
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0 3 0 4.90 0.70
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3 -3 -7 17.10 3.50
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-1 1 -9 1304.87 38.60
1 1 9 1327.17 31.80
1 1 9 1323.47 36.40
-1 1 -9 1380.66 34.80
-2 -1 -9 468.55 20.90
-2 -1 -9 495.55 18.20
2 -1 9 460.95 15.90
2 -1 9 424.96 18.30
2 -1 9 466.85 18.40
2 1 9 482.95 18.10
-2 1 -9 506.95 18.20
-2 1 -9 431.76 20.10
2 1 9 459.45 15.80
2 1 9 475.95 18.70
3 -1 9 954.40 28.50
3 -1 9 951.20 30.90
-3 -1 -9 1001.30 30.90
3 -1 9 971.90 30.00
-3 -1 -9 968.90 33.70
3 1 9 992.20 29.50
3 1 9 952.30 31.00
-3 1 -9 1005.20 30.60
3 1 9 955.30 28.50
-3 1 -9 968.30 33.40
4 -1 9 272.67 14.60
4 -1 9 270.37 16.10
-4 -1 -9 289.37 16.30
-4 -1 -9 265.27 18.30
4 -1 9 280.57 15.00
-4 1 -9 255.77 15.30
-4 1 -9 290.67 18.60
4 1 9 278.07 16.20
4 1 9 266.37 14.70
-5 -1 -9 550.24 26.50
-5 -1 -9 558.14 24.30
5 -1 9 527.95 23.60
5 -1 9 492.25 22.10
5 1 9 528.35 22.70
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-5 1 -9 535.85 23.30
5 1 9 551.54 24.10
-6 -1 -9 112.99 14.30
-6 -1 -9 73.89 13.30
6 -1 9 121.69 13.80
6 -1 9 107.69 14.50
6 1 9 104.59 13.60
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6 1 9 94.79 13.70
-7 -1 -9 165.98 16.80
7 -1 9 162.38 17.60
7 -1 9 169.08 16.90
-7 -1 -9 179.88 19.80
7 1 9 148.89 17.10
-7 1 -9 185.68 17.90
7 1 9 208.68 18.90
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8 -1 9 34.30 17.30
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-8 -1 -9 37.10 11.50
8 -1 9 40.50 11.10
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9 -2 -9 156.48 18.40
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-9 2 9 161.78 15.90
-9 2 9 187.78 17.60
-8 -2 9 706.83 29.50
8 -2 -9 675.23 29.90
-8 -2 9 762.62 32.70
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8 2 -9 740.13 30.90
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7 -2 -9 110.89 13.40
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7 2 -9 125.09 14.50
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6 -2 -9 934.71 33.00
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-6 2 9 927.81 33.30
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5 -2 -9 327.77 15.00
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5 -2 -9 313.87 17.50
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5 2 -9 351.56 16.80
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-5 2 9 327.07 17.70
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4 2 -9 1128.89 33.10
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3 -2 -9 242.58 11.60
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3 -2 -9 238.48 14.00
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3 2 -9 247.48 12.90
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2 -2 -9 594.44 19.70
2 -2 -9 611.94 20.30
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2 2 -9 587.84 19.20
2 2 -9 606.84 20.80
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1 -2 -9 312.77 14.60
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1 2 -9 326.67 15.50
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1 2 -9 324.87 13.90
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0 -2 9 186.88 7.60
0 -2 -9 192.48 12.40
0 -2 9 198.48 11.80
0 -2 -9 213.08 10.10
0 -2 9 186.38 11.00
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0 2 9 196.48 9.40
0 2 -9 201.68 9.10
0 2 9 196.38 12.60
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1 -2 9 253.77 13.10
1 -2 9 249.68 13.10
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1 -2 9 250.57 9.90
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1 2 9 255.97 12.90
-1 2 -9 247.28 11.30
1 2 9 252.47 9.40
-1 2 -9 235.48 13.80
1 2 9 248.88 12.50
-2 -2 -9 8.30 5.70
2 -2 9 4.80 3.00
2 -2 9 5.10 4.20
2 -2 9 10.70 4.60
-2 -2 -9 5.60 4.00
-2 2 -9 7.40 5.00
2 2 9 10.40 5.00
2 2 9 6.90 3.30
2 2 9 9.50 4.40
-2 2 -9 7.10 4.20
3 -2 9 13.40 4.30
3 -2 9 12.90 5.10
-3 -2 -9 24.70 7.50
-3 -2 -9 17.10 5.90
3 -2 9 9.60 5.00
3 2 9 20.80 5.20
3 2 9 12.40 5.40
-3 2 -9 3.90 5.40
3 2 9 14.90 4.50
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4 -2 9 115.69 12.20
4 -2 9 115.79 10.80
4 -2 9 112.29 10.30
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4 2 9 102.79 10.40
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5 -2 9 51.39 8.50
5 -2 9 43.20 8.30
5 -2 9 26.40 8.10
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5 2 9 49.10 8.40
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6 -2 9 179.98 16.10
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6 -2 9 192.08 16.20
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6 2 9 164.68 15.70
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7 -2 9 84.09 13.40
7 -2 9 129.79 16.00
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7 2 9 105.49 15.50
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8 -2 9 185.48 19.80
8 -2 9 195.58 24.60
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-8 2 -9 215.18 22.80
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9 -3 -9 15.30 9.70
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-8 -3 9 28.40 8.80
-8 -3 9 46.20 11.50
8 -3 -9 26.00 10.20
8 3 -9 29.10 9.10
-8 3 9 41.50 8.70
-8 3 9 44.10 10.60
8 3 -9 27.50 9.70
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-7 -3 9 -2.20 4.50
7 -3 -9 14.60 7.90
7 3 -9 -1.00 5.70
7 3 -9 12.70 7.40
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-6 -3 9 42.70 7.30
6 -3 -9 47.70 9.50
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6 3 -9 51.59 8.70
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5 -3 -9 7.20 5.80
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5 3 -9 0.70 5.60
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5 3 -9 4.30 5.10
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4 -3 -9 522.55 22.20
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4 -3 -9 558.44 19.10
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4 3 -9 531.85 20.80
3 -3 -9 21.60 4.70
3 -3 -9 11.70 5.50
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-3 -3 9 30.80 4.70
-3 -3 9 17.60 5.50
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3 3 -9 20.80 5.60
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-2 -3 9 1086.09 26.90
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2 -3 -9 1085.89 29.90
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2 3 -9 1088.99 31.60
-2 3 9 1046.30 32.90
-2 3 9 1129.99 30.10
2 3 -9 1081.69 29.60
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1 3 -9 3.40 3.60
1 3 -9 1.30 3.60
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0 -3 9 2000.70 50.99
0 -3 9 1960.80 46.80
0 -3 9 1955.50 45.10
0 -3 9 1920.91 50.09
0 -3 -9 2012.80 48.40
0 3 -9 1989.90 50.89
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0 3 9 1961.00 49.10
0 3 9 2036.40 47.10
0 3 9 1974.10 52.39
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1 -3 9 106.09 9.30
1 -3 9 90.49 8.70
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1 -3 9 88.69 6.20
1 3 9 90.19 8.40
1 3 9 89.79 8.20
1 3 9 93.19 5.80
1 3 9 108.09 10.50
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2 -3 9 1437.56 39.80
2 -3 9 1416.46 36.40
2 -3 9 1431.76 39.30
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2 3 9 1395.06 35.90
2 3 9 1384.86 37.60
2 3 9 1324.17 42.40
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3 -3 9 2.30 3.50
3 -3 9 -4.70 3.90
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3 -3 9 2.00 4.50
3 3 9 -1.20 4.30
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3 3 9 5.50 3.70
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4 -3 9 1294.57 39.00
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4 -3 9 1291.77 37.70
4 -3 9 1259.07 36.90
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4 3 9 1233.08 37.20
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5 -3 9 5.10 6.80
5 -3 9 13.50 6.00
-5 -3 -9 6.10 6.40
5 -3 9 -2.60 5.20
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6 -3 9 293.77 25.40
6 -3 9 314.77 20.10
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6 -3 9 301.47 19.20
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7 -3 9 4.80 8.70
7 -3 9 5.30 7.20
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8 -3 9 99.19 18.80
8 -3 9 108.99 17.80
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9 -4 -9 198.48 19.60
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8 4 -9 665.13 28.80
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7 4 -9 198.08 16.00
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-6 -4 9 999.80 32.30
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6 4 -9 1097.39 34.60
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5 -4 -9 353.96 18.90
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5 4 -9 366.66 19.10
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4 -4 -9 1380.66 39.60
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-4 -4 9 1292.77 39.70
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3 -4 -9 313.37 12.90
3 -4 -9 330.87 16.40
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1 4 -9 196.08 11.00
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1 4 -9 186.88 11.30
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0 -4 -9 192.48 10.40
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1 -4 9 71.89 8.70
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7 -4 9 86.49 13.50
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8 -5 -9 29.90 10.50
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5 -5 -9 186.68 14.60
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4 5 -9 179.68 12.60
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3 -5 -9 418.86 14.90
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3 -5 -9 405.66 18.00
3 5 -9 386.46 17.60
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-3 5 9 395.26 17.00
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2 -5 -9 333.67 15.70
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2 -5 -9 337.97 13.00
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2 5 -9 299.27 14.70
2 5 -9 345.77 13.60
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1 5 -9 1236.18 34.30
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1 5 -9 1217.68 33.00
0 -5 -9 860.91 25.30
0 -5 9 811.12 26.50
0 -5 -9 865.51 23.50
0 -5 9 825.72 23.50
0 -5 9 800.02 22.50
0 -5 9 795.32 26.50
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0 5 9 823.22 24.60
0 5 -9 835.92 26.60
1 -5 9 1005.40 28.00
1 -5 9 1134.49 32.60
-1 -5 -9 1064.99 30.50
1 -5 9 1011.90 31.50
-1 -5 -9 1083.19 27.50
1 5 9 1055.59 34.70
1 5 9 1066.39 26.50
1 5 9 1049.89 29.80
1 5 9 1060.69 30.60
-1 5 -9 1027.30 32.60
2 -5 9 361.86 16.60
2 -5 9 341.97 14.20
2 -5 9 336.47 16.20
-2 -5 -9 383.46 16.20
2 5 9 348.47 16.10
2 5 9 354.86 13.80
2 5 9 333.27 18.80
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3 -5 9 1138.59 33.40
3 -5 9 1190.08 35.80
3 -5 9 1187.08 35.50
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3 5 9 1178.88 35.70
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4 -5 9 252.87 15.90
4 -5 9 239.78 14.40
4 -5 9 309.77 16.50
-4 -5 -9 278.97 16.70
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4 5 9 260.67 16.10
-4 5 -9 243.58 17.20
4 5 9 264.07 18.90
-5 -5 -9 549.25 24.40
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3 -9 13 -9.70 8.40
-3 9 -13 1.70 9.10
3 9 13 -3.40 8.20
3 9 13 9.20 8.30
-4 -10 13 49.20 11.70
-4 -10 13 41.70 11.10
-4 -10 13 59.19 9.50
4 -10 -13 38.40 9.70
-4 10 13 51.59 6.60
-4 10 13 51.59 10.80
4 10 -13 67.59 12.10
-3 -10 13 -3.50 7.60
3 -10 -13 2.40 6.70
-3 -10 13 -1.70 4.70
3 10 -13 -9.60 7.30
-3 10 13 2.30 6.70
-3 10 13 0.40 2.80
2 -10 -13 -2.30 6.10
-2 -10 13 2.20 4.90
-2 -10 13 1.10 7.60
-2 10 13 9.30 2.90
2 10 -13 10.20 8.70
-2 10 13 8.60 7.00
-1 -10 13 4.80 5.00
-1 -10 13 8.40 8.30
1 -10 -13 3.80 6.80
-1 10 13 13.80 8.10
-1 10 13 6.60 3.10
1 10 -13 9.20 7.40
0 -10 -13 121.79 14.40
0 -10 13 129.69 15.70
0 -10 13 117.79 11.20
0 10 13 151.68 17.90
0 10 -13 127.29 15.50
0 10 13 125.69 9.10
0 10 -13 108.49 14.10
-1 -10 -13 26.90 9.10
1 -10 13 39.00 10.30
1 -10 13 41.20 7.60
1 10 13 30.80 11.30
1 10 13 37.50 6.50
-1 10 -13 20.30 9.00
-1 10 -13 44.00 10.70
-2 -10 -13 221.98 18.80
2 -10 13 272.77 20.50
2 -10 13 231.08 15.80
-2 10 -13 236.08 20.40
-2 10 -13 238.98 19.00
2 10 13 241.08 14.90
2 10 13 221.68 22.50
4 -11 -13 182.48 16.80
-4 -11 13 235.88 20.30
-4 11 13 179.28 9.80
4 11 -13 191.48 21.80
-4 11 13 229.18 18.30
-3 -11 13 342.87 18.20
-3 -11 13 367.96 23.00
3 -11 -13 326.27 19.10
3 11 -13 335.07 23.00
-3 11 13 345.57 12.40
-3 11 13 382.26 22.10
-2 -11 13 268.17 20.90
-2 -11 13 231.08 15.00
2 -11 -13 223.88 15.90
-2 11 13 209.78 17.20
2 11 -13 247.68 19.30
-2 11 13 229.48 9.50
-1 -11 13 499.95 25.90
-1 -11 13 488.05 21.00
1 -11 -13 506.25 24.20
1 11 -13 458.55 24.70
-1 11 13 541.55 28.30
-1 11 13 477.65 15.40
0 -11 13 253.37 15.30
0 -11 -13 258.17 18.80
0 -11 13 248.78 19.50
0 11 -13 238.38 19.60
0 11 13 247.48 21.50
0 11 13 251.97 12.20
0 11 -13 256.67 19.60
1 -11 13 266.37 16.60
1 -11 13 302.17 21.70
-1 -11 -13 290.87 19.80
1 11 13 268.37 24.00
1 11 13 285.47 14.50
-1 11 -13 238.98 19.20
-1 11 -13 285.27 20.70
2 -11 13 102.49 15.10
-2 -11 -13 92.49 13.70
2 11 13 118.69 19.50
-2 11 -13 83.79 14.60
2 11 13 88.99 11.50
3 -12 -13 16.00 8.10
-3 -12 13 9.90 6.50
-3 -12 13 19.20 12.00
-3 12 13 12.80 4.10
-3 12 13 14.10 8.30
3 12 -13 11.50 10.40
-2 -12 13 9.70 9.00
2 -12 -13 3.00 6.60
-2 -12 13 9.60 5.90
2 12 -13 4.00 8.10
-2 12 13 -4.40 7.20
-2 12 13 5.00 3.60
-1 -12 13 33.70 10.20
-1 -12 13 34.10 7.50
1 -12 -13 47.80 10.20
1 12 -13 39.30 10.70
-1 12 13 32.70 5.00
-1 12 13 47.00 11.60
0 -12 -13 -4.40 7.20
0 -12 13 3.10 5.50
0 -12 13 -6.10 7.60
0 12 13 5.40 9.10
0 12 -13 -4.40 7.50
0 12 13 -5.60 3.90
1 -12 13 142.09 17.70
1 -12 13 133.69 13.70
-1 -12 -13 139.29 15.50
1 12 13 135.69 11.50
-1 12 -13 95.59 15.50
1 12 13 123.09 20.20
-1 12 -13 103.69 16.30
3 -13 -13 453.85 22.90
-3 13 13 446.56 25.00
-3 13 13 408.96 16.10
-2 -13 13 47.90 13.10
2 -13 -13 44.00 10.80
2 -13 -13 32.30 9.40
-2 13 13 44.50 10.60
-2 13 13 38.60 5.50
-1 -13 13 390.26 21.50
-1 -13 13 404.26 30.60
1 -13 -13 428.76 23.40
-1 13 13 394.16 14.90
1 13 -13 478.25 32.40
-1 13 13 371.16 25.50
0 -13 -13 89.59 13.00
0 -13 13 68.29 12.40
0 13 13 35.10 11.70
0 13 13 71.79 9.10
-1 -13 -13 196.08 18.70
-1 13 -13 215.08 19.30
1 13 13 186.38 22.80
5 0 -14 -1.20 8.60
-5 0 14 5.40 5.10
-5 0 14 5.00 9.30
-4 0 14 358.96 21.80
4 0 -14 315.57 22.60
-4 0 14 315.67 14.60
-3 0 14 -2.30 3.30
3 0 -14 5.60 7.90
3 0 -14 1.50 6.30
-2 0 14 128.59 7.20
2 0 -14 127.89 13.70
-2 0 14 103.09 15.30
1 0 -14 6.30 6.40
-1 0 14 -2.60 7.60
-1 0 14 2.00 2.60
0 0 -14 6.10 6.90
0 0 -14 9.90 7.60
0 0 14 7.80 7.80
1 0 14 4.00 7.00
1 0 14 1.80 3.40
-1 0 -14 -3.90 7.50
-2 0 -14 28.30 10.00
2 0 14 28.40 5.80
2 0 14 27.30 10.20
-3 0 -14 -11.30 12.50
5 -1 -14 37.70 11.20
-5 -1 14 11.80 6.80
-5 -1 14 15.70 10.00
-5 1 14 12.60 5.50
5 1 -14 21.20 10.60
-5 1 14 14.50 9.80
-4 -1 14 184.68 17.50
4 -1 -14 172.78 18.90
-4 -1 14 170.08 11.40
4 1 -14 164.68 18.30
-4 1 14 196.28 17.50
-4 1 14 159.08 10.40
3 -1 -14 125.99 16.10
-3 -1 14 133.79 16.10
-3 -1 14 119.79 8.80
3 1 -14 116.39 14.00
-3 1 14 117.69 8.00
-2 -1 14 301.37 21.60
-2 -1 14 331.27 12.10
2 -1 -14 355.46 19.20
-2 1 14 282.87 20.70
2 1 -14 265.07 17.90
1 -1 -14 182.18 15.10
-1 -1 14 184.38 8.80
-1 -1 14 202.88 17.90
-1 1 14 197.18 17.80
1 1 -14 168.98 14.70
0 -1 14 466.45 24.70
0 -1 -14 483.25 23.00
0 -1 -14 446.46 23.80
0 1 14 494.25 23.50
0 1 -14 472.75 24.00
0 1 14 462.75 14.30
0 1 -14 459.55 23.10
1 -1 14 252.87 18.00
-1 -1 -14 222.38 19.10
1 -1 14 213.48 11.10
-1 1 -14 222.68 18.70
1 1 14 211.58 17.00
1 1 14 221.68 10.60
2 -1 14 327.07 15.30
2 -1 14 310.97 21.10
-2 -1 -14 317.17 22.40
-2 1 -14 343.57 23.10
2 1 14 307.57 14.40
2 1 14 332.27 21.70
-3 -1 -14 114.39 20.20
-3 1 -14 68.59 16.80
-5 -2 14 524.05 28.30
5 -2 -14 493.35 27.20
-5 2 14 483.65 19.60
-5 2 14 533.45 27.50
-4 -2 14 105.39 10.20
4 -2 -14 99.79 14.70
-4 -2 14 125.79 15.80
-4 2 14 115.49 15.20
4 2 -14 102.19 14.00
-4 2 14 107.59 8.90
4 2 -14 110.99 17.00
-3 -2 14 163.68 10.20
-3 -2 14 137.29 17.50
3 -2 -14 151.48 17.10
3 2 -14 168.28 15.80
-2 -2 14 51.19 6.30
2 -2 -14 30.70 9.00
2 -2 -14 37.10 9.40
-2 -2 14 30.20 10.20
2 2 -14 28.00 8.50
1 -2 -14 27.80 8.00
-1 -2 14 21.00 4.20
-1 -2 14 28.40 9.30
1 2 -14 16.30 7.50
0 -2 14 9.10 8.00
0 -2 14 6.50 3.60
0 -2 -14 7.50 8.00
0 2 -14 -0.90 6.80
0 2 14 13.70 7.50
0 2 -14 16.50 7.80
-1 -2 -14 11.70 8.40
1 -2 14 22.90 9.10
1 -2 14 13.70 4.60
1 -2 14 19.80 9.10
-1 2 -14 14.10 8.60
1 2 14 13.70 3.90
1 2 14 10.50 7.80
-2 -2 -14 -0.30 8.50
2 -2 14 5.30 8.50
2 -2 14 -2.30 4.20
2 2 14 6.40 8.20
-2 2 -14 -11.40 7.20
2 2 14 1.30 4.00
-3 2 -14 80.09 20.80
5 -3 -14 266.97 21.70
-5 -3 14 242.48 21.30
-5 3 14 258.77 20.50
5 3 -14 257.47 24.40
-5 3 14 258.07 14.40
4 -3 -14 17.60 9.10
-4 -3 14 -2.50 4.50
-4 -3 14 2.90 7.60
4 3 -14 -4.10 6.70
4 3 -14 2.60 8.20
-4 3 14 -0.50 7.30
-4 3 14 0.80 3.70
3 -3 -14 308.07 21.90
-3 -3 14 383.76 15.40
-3 -3 14 392.56 24.70
3 3 -14 350.86 20.80
-3 3 14 360.86 25.20
2 -3 -14 9.00 7.70
-2 -3 14 4.70 8.40
-2 -3 14 3.40 3.50
2 3 -14 2.20 6.40
1 -3 -14 858.21 30.60
-1 -3 14 803.12 33.60
-1 -3 14 817.62 23.70
1 3 -14 822.02 31.60
0 -3 14 4.50 3.50
0 -3 14 5.70 7.80
0 -3 -14 0.10 7.00
0 3 -14 -4.20 6.50
0 3 -14 12.00 7.50
0 3 14 7.80 6.90
-1 -3 -14 528.75 27.00
1 -3 14 606.24 28.50
1 -3 14 539.85 26.70
1 -3 14 510.45 19.10
-1 3 -14 555.24 26.20
1 3 14 558.24 25.80
1 3 14 542.25 17.00
-1 3 -14 557.14 27.10
-2 -3 -14 -4.50 7.50
2 -3 14 -2.20 7.80
2 -3 14 0.10 4.70
2 3 14 2.80 4.20
-2 3 -14 -2.40 7.70
2 3 14 4.50 7.30
-4 -4 14 105.19 15.50
4 -4 -14 80.19 13.20
-4 -4 14 93.79 15.00
-4 -4 14 100.09 10.60
4 4 -14 102.49 14.00
-4 4 14 79.59 12.20
-4 4 14 93.19 7.70
-3 -4 14 245.08 20.90
-3 -4 14 254.27 12.90
3 -4 -14 217.88 19.00
-3 4 14 233.58 17.20
3 4 -14 228.98 18.10
-2 -4 14 6.40 4.00
-2 -4 14 -4.10 6.70
2 4 -14 17.60 7.70
-1 -4 14 104.49 8.40
-1 -4 14 115.09 15.10
1 4 -14 99.59 13.70
0 -4 14 8.30 8.20
0 -4 -14 0.00 7.10
0 -4 14 8.80 4.20
0 4 14 -2.90 6.10
0 4 -14 3.20 10.70
0 4 -14 -4.20 6.90
-1 -4 -14 1.20 7.70
1 -4 14 -2.00 7.40
1 4 14 -5.60 6.10
-1 4 -14 -3.60 7.00
1 4 14 0.70 3.20
-1 4 -14 -4.30 6.90
2 -4 14 2.60 4.90
-2 -4 -14 5.00 8.80
2 -4 14 9.50 8.40
2 -4 14 7.50 8.50
2 4 14 17.90 8.60
2 4 14 10.50 4.60
-2 4 -14 -7.20 7.30
-4 -5 14 266.17 20.30
-4 -5 14 254.47 15.00
4 -5 -14 250.67 19.80
-4 -5 14 228.48 21.00
-4 5 14 262.07 19.50
-4 5 14 283.27 10.80
4 5 -14 278.47 20.40
-3 -5 14 154.08 11.00
-3 -5 14 154.18 17.50
3 -5 -14 148.89 14.50
3 5 -14 145.79 16.40
-2 -5 14 352.36 15.20
-2 -5 14 340.87 22.90
2 5 -14 352.56 20.80
-1 -5 14 182.58 10.70
-1 -5 14 170.88 17.70
1 5 -14 136.99 15.00
0 -5 -14 624.94 28.80
0 -5 14 601.14 21.00
0 -5 14 633.94 29.90
0 5 -14 619.74 27.50
-1 -5 -14 176.68 17.60
1 -5 14 193.48 18.70
1 5 14 183.98 16.50
-1 5 -14 199.28 18.20
-1 5 -14 136.29 15.90
1 5 14 174.48 9.20
2 -5 14 289.97 26.30
-2 -5 -14 258.57 21.30
2 -5 14 274.07 21.30
2 -5 14 247.98 17.20
2 5 14 252.87 13.10
-2 5 -14 235.68 20.10
2 5 14 275.87 19.50
-4 -6 14 309.17 29.40
-4 -6 14 284.47 23.40
-4 -6 14 324.87 21.80
4 -6 -14 278.67 26.20
4 -6 -14 277.17 19.40
4 6 -14 267.77 20.40
-4 6 14 272.47 10.60
3 -6 -14 16.00 7.60
-3 -6 14 8.10 4.80
-3 -6 14 19.10 9.70
3 6 -14 13.40 8.60
-2 -6 14 153.48 17.80
-2 -6 14 144.29 10.80
2 6 -14 132.29 15.10
-1 -6 14 -4.20 7.00
-1 -6 14 1.90 4.10
1 6 -14 5.40 7.10
0 -6 14 15.50 9.20
0 -6 -14 7.40 7.50
0 -6 14 7.40 4.60
0 6 -14 8.20 7.70
1 -6 14 -0.20 8.50
1 -6 14 -3.40 4.40
-1 -6 -14 6.10 8.30
1 6 14 -0.40 3.40
1 6 14 -2.30 6.50
-1 6 -14 -6.10 7.60
-1 6 -14 -0.80 7.40
-2 -6 -14 37.50 11.60
2 -6 14 7.60 9.10
2 6 14 7.40 7.70
-2 6 -14 23.10 10.10
2 6 14 24.00 5.70
-4 -7 14 253.57 25.90
4 -7 -14 241.38 17.60
-4 7 14 248.38 9.80
4 7 -14 268.77 19.90
-3 -7 14 105.99 10.70
-3 -7 14 118.09 17.60
3 -7 -14 121.49 14.10
3 7 -14 92.89 13.80
-2 -7 14 459.35 25.40
-2 -7 14 420.66 18.00
2 7 -14 419.06 23.50
-1 -7 14 110.59 10.10
-1 -7 14 159.48 17.30
1 7 -14 110.19 15.30
0 -7 14 419.46 25.00
0 -7 -14 403.56 24.20
0 -7 14 417.76 17.80
0 7 -14 417.26 23.20
-1 -7 -14 122.59 16.60
1 -7 14 155.08 18.10
1 -7 14 111.29 11.20
-1 7 -14 118.19 15.60
-1 7 -14 94.09 15.70
1 7 14 108.89 8.40
2 -7 14 369.46 24.20
-2 -7 -14 291.07 25.30
2 7 14 320.77 17.10
2 7 14 349.57 21.30
-2 7 -14 350.86 23.40
-3 -8 14 89.29 17.30
3 -8 -14 123.59 14.20
-3 -8 14 118.99 17.70
3 8 -14 114.79 15.80
-2 -8 14 57.69 9.40
-2 -8 14 49.90 11.80
2 8 -14 44.30 11.00
-1 -8 14 16.20 9.30
-1 -8 14 7.70 4.90
1 8 -14 18.40 9.40
0 -8 14 8.10 8.50
0 -8 14 2.80 4.70
0 -8 -14 1.10 7.70
0 8 -14 6.60 7.60
-1 -8 -14 7.20 8.60
1 -8 14 13.30 9.30
1 8 14 4.40 4.40
-1 8 -14 -4.00 7.40
3 -9 -14 339.97 19.70
-2 -9 14 7.40 10.20
2 9 -14 -1.40 8.10
1 -9 -14 595.64 38.70
-1 -9 14 628.94 26.10
-1 -9 14 594.84 30.20
1 9 -14 585.74 30.00
0 -9 -14 -5.00 7.50
0 -9 14 -11.70 7.60
0 9 14 5.70 9.00
-1 -9 -14 434.46 24.50
-1 -9 -14 417.06 26.70
1 -9 14 451.45 37.40
-1 9 -14 452.15 25.50
1 9 14 402.96 16.30
2 -10 -14 9.80 8.20
1 -10 -14 90.59 13.70
0 -10 -14 8.90 7.90
0 10 14 -5.70 8.80
2 0 -15 -6.90 6.00
-2 0 15 8.40 8.30
1 0 -15 352.36 21.10
-1 0 15 361.86 12.40
-1 0 15 405.96 27.20
0 0 15 -3.40 2.90
0 0 -15 2.30 7.40
2 -1 -15 30.70 9.60
-2 -1 15 36.30 11.00
-2 -1 15 26.30 4.60
-2 1 15 4.80 8.80
2 1 -15 27.30 9.10
-1 -1 15 278.87 11.20
1 -1 -15 286.87 19.00
-1 -1 15 286.87 22.30
1 1 -15 246.88 18.70
0 -1 15 149.09 8.80
0 -1 -15 154.48 16.10
0 1 15 137.89 7.70
0 1 -15 164.68 16.80
-2 -2 15 343.17 24.00
-2 -2 15 287.47 12.60
2 2 -15 311.47 20.40
-1 -2 15 111.69 16.60
1 -2 -15 126.59 14.50
-1 -2 15 108.49 8.10
1 2 -15 86.59 12.60
0 -2 -15 158.38 16.60
0 -2 15 177.58 18.80
0 -2 15 173.08 10.20
0 2 -15 179.38 17.60
-2 -3 15 183.48 19.90
-2 -3 15 182.88 11.30
2 3 -15 191.88 17.40
-1 -3 15 5.90 4.00
-1 -3 15 0.70 7.70
1 3 -15 10.40 8.30
0 0 0 0.00 0.00
_computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)'
;
_shelx_hkl_checksum 83767
_shelx_res_file
;
TITL AW2829U_a.res in P2(1)/n
AW2829U_a.res
created by SHELXL-2017/1 at 11:21:02 on 08-Nov-2023
REM Old TITL AW2829U in P2(1)/n
REM SHELXT solution in P2(1)/n: R1 0.058, Rweak 0.002, Alpha 0.029
REM 1.577 for 114 systematic absences, Orientation as input
REM Formula found by SHELXT: C17 N O4 U
CELL 0.71073 7.7340 19.0096 10.6154 90.000 96.106 90.000
ZERR 4.000 0.0008 0.0020 0.0011 0.000 0.002 0.000
LATT 1
SYMM 1/2-X, 1/2+Y, 1/2-Z
SFAC C H N O U
UNIT 56 56 8 24 4
TEMP -148
SIZE 0.2 0.2 0.1
REM yellow block
L.S. 16
ACTA
BOND $H
CONF
MPLA 6 N1 C1 C2 C3 C4 C5
MPLA 6 N2 C6 C7 C8 C9 C10
HTAB
EQIV $1 x+1/2, -y+1/2, z+1/2
HTAB C2 O4_$1
EQIV $2 -x+2, -y+1, -z+1
EQIV $3 -x+1, -y+1, -z+1
HTAB C7 O1_$3
HTAB C10 O5
HTAB C12 O1_$1
EQIV $4 x-1/2, -y+1/2, z-1/2
HTAB C14 O2_$4
EQIV $5 x+1/2, -y+1/2, z-1/2
HTAB C14 O1_$5
LIST 4
FMAP 2
PLAN 20
REM EXTI 0.000000
WGHT 0.013600 1.591200
FVAR 0.27338 0.50539
U 5 0.722040 0.331219 0.340352 11.00000 0.01680 0.00834 =
0.01466 -0.00027 0.00377 -0.00089
O1 4 0.491529 0.334811 0.330622 11.00000 0.01740 0.01748 =
0.02180 0.00147 0.00265 -0.00304
O2 4 0.951994 0.327747 0.347412 11.00000 0.01758 0.01890 =
0.02363 -0.00008 0.00499 0.00153
O3 4 0.693789 0.274553 0.545516 11.00000 0.02745 0.01371 =
0.01771 0.00081 0.00511 -0.00304
O4 4 0.728400 0.205011 0.386400 11.00000 0.03803 0.01137 =
0.01893 0.00083 0.00785 -0.00075
O5 4 0.735649 0.370580 0.119789 11.00000 0.02814 0.01224 =
0.01734 -0.00030 0.00554 0.00131
O6 4 0.696627 0.258085 0.150217 11.00000 0.04191 0.01252 =
0.01778 -0.00074 0.00640 -0.00497
N1 3 0.820077 0.413113 0.533142 11.00000 0.01575 0.01053 =
0.01898 -0.00070 0.00338 -0.00112
N2 3 0.656992 0.467725 0.320617 11.00000 0.01691 0.01119 =
0.01879 0.00010 0.00290 0.00012
C1 1 0.922402 0.385359 0.630570 11.00000 0.01851 0.01395 =
0.02184 0.00159 0.00227 0.00094
AFIX 43
H1A 2 0.951625 0.336899 0.627365 11.00000 -1.20000
AFIX 0
C2 1 0.987408 0.424080 0.735604 11.00000 0.01624 0.02117 =
0.01910 0.00022 0.00227 -0.00261
AFIX 43
H2A 2 1.060631 0.402727 0.802378 11.00000 -1.20000
AFIX 0
C3 1 0.943571 0.494444 0.741308 11.00000 0.02131 0.02184 =
0.01893 -0.00570 0.00372 -0.00386
AFIX 43
H3A 2 0.983732 0.521905 0.813299 11.00000 -1.20000
AFIX 0
C4 1 0.840093 0.524491 0.640490 11.00000 0.02004 0.01346 =
0.02301 -0.00431 0.00512 -0.00097
AFIX 43
H4A 2 0.808733 0.572768 0.642401 11.00000 -1.20000
AFIX 0
C5 1 0.782935 0.482570 0.536300 11.00000 0.01331 0.01225 =
0.01870 -0.00141 0.00651 -0.00183
C6 1 0.685015 0.512143 0.420727 11.00000 0.01292 0.01211 =
0.01945 -0.00079 0.00637 -0.00199
C7 1 0.629565 0.581920 0.413462 11.00000 0.02260 0.01211 =
0.02266 -0.00139 0.00781 0.00098
AFIX 43
H7A 2 0.650676 0.611892 0.485057 11.00000 -1.20000
AFIX 0
C8 1 0.543700 0.607471 0.301779 11.00000 0.02641 0.01141 =
0.02703 0.00179 0.00780 0.00427
AFIX 43
H8A 2 0.506159 0.655037 0.295151 11.00000 -1.20000
AFIX 0
C9 1 0.513797 0.561843 0.199660 11.00000 0.02457 0.01865 =
0.02242 0.00294 0.00210 0.00495
AFIX 43
H9A 2 0.454847 0.577536 0.121638 11.00000 -1.20000
AFIX 0
C10 1 0.571603 0.492888 0.213654 11.00000 0.02183 0.01603 =
0.02062 -0.00063 0.00095 0.00125
AFIX 43
H10A 2 0.549433 0.461869 0.143631 11.00000 -1.20000
AFIX 0
C11 1 0.705047 0.212938 0.501375 11.00000 0.01617 0.01390 =
0.02028 0.00207 0.00086 -0.00218
C12 1 0.691397 0.149931 0.585373 11.00000 0.02808 0.01661 =
0.02110 0.00579 0.00104 -0.00298
AFIX 123
H12A 2 0.673526 0.165610 0.670976 21.00000 -1.50000
H12B 2 0.592892 0.120736 0.551336 21.00000 -1.50000
H12C 2 0.798875 0.122381 0.588556 21.00000 -1.50000
H12D 2 0.703336 0.106874 0.536269 -21.00000 -1.50000
H12E 2 0.783970 0.151749 0.655909 -21.00000 -1.50000
H12F 2 0.577987 0.150104 0.618689 -21.00000 -1.50000
AFIX 0
C13 1 0.723778 0.307849 0.076200 11.00000 0.01631 0.01572 =
0.01770 0.00061 0.00225 0.00146
C14 1 0.742562 0.293605 -0.060178 11.00000 0.02501 0.01611 =
0.01793 -0.00077 0.00446 0.00241
AFIX 137
H14A 2 0.785960 0.335912 -0.099174 11.00000 -1.50000
H14B 2 0.629206 0.280683 -0.104230 11.00000 -1.50000
H14C 2 0.824834 0.254881 -0.066527 11.00000 -1.50000
AFIX 0
HKLF 4
REM AW2829U_a.res in P2(1)/n
REM R1 = 0.0157 for 4280 Fo > 4sig(Fo) and 0.0193 for all 4720 data
REM 210 parameters refined using 0 restraints
END
WGHT 0.0136 1.5913
REM Instructions for potential hydrogen bonds
HTAB C1 O6_$1
HTAB C2 O4_$1
HTAB C4 O2_$2
HTAB C7 O1_$3
HTAB C10 O5
HTAB C12 O1_$1
HTAB C14 O2_$4
HTAB C14 O1_$5
REM Highest difference peak 1.061, deepest hole -0.556, 1-sigma level 0.103
Q1 1 0.6086 0.3313 0.3206 11.00000 0.05 1.06
Q2 1 0.8355 0.3284 0.3602 11.00000 0.05 1.06
Q3 1 0.6687 0.3365 0.3991 11.00000 0.05 0.97
Q4 1 0.7776 0.3287 0.2774 11.00000 0.05 0.94
Q5 1 0.7530 0.3206 0.4174 11.00000 0.05 0.69
Q6 1 0.9115 0.3283 0.4025 11.00000 0.05 0.48
Q7 1 0.6866 0.2913 0.4797 11.00000 0.05 0.47
Q8 1 0.7954 0.4984 0.5998 11.00000 0.05 0.47
Q9 1 0.5327 0.3197 0.3822 11.00000 0.05 0.45
Q10 1 0.6461 0.5467 0.4131 11.00000 0.05 0.44
Q11 1 0.6717 0.2880 0.1176 11.00000 0.05 0.43
Q12 1 0.6747 0.4895 0.3720 11.00000 0.05 0.41
Q13 1 1.0185 0.3178 0.3247 11.00000 0.05 0.41
Q14 1 0.9809 0.4074 0.6732 11.00000 0.05 0.40
Q15 1 0.6734 0.2723 0.2159 11.00000 0.05 0.40
Q16 1 0.5435 0.3559 0.3794 11.00000 0.05 0.40
Q17 1 0.5059 0.5810 0.2554 11.00000 0.05 0.40
Q18 1 0.7265 0.3063 0.0025 11.00000 0.05 0.39
Q19 1 0.9160 0.3335 0.2983 11.00000 0.05 0.39
Q20 1 0.5711 0.5369 0.2026 11.00000 0.05 0.39
;
_shelx_res_checksum 27048
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U U 0.72204(2) 0.33122(2) 0.34035(2) 0.01312(3) Uani d 1.0 . .
O O1 0.4915(2) 0.33481(8) 0.33062(15) 0.0189(3) Uani d 1.0 . .
O O2 0.9520(2) 0.32775(8) 0.34741(16) 0.0198(3) Uani d 1.0 . .
O O3 0.6938(2) 0.27455(8) 0.54552(14) 0.0194(3) Uani d 1.0 . .
O O4 0.7284(2) 0.20501(8) 0.38640(15) 0.0224(3) Uani d 1.0 . .
O O5 0.7356(2) 0.37058(8) 0.11979(15) 0.0190(3) Uani d 1.0 . .
O O6 0.6966(2) 0.25809(8) 0.15022(15) 0.0238(4) Uani d 1.0 . .
N N1 0.8201(2) 0.41311(9) 0.53314(17) 0.0150(3) Uani d 1.0 . .
N N2 0.6570(2) 0.46772(9) 0.32062(17) 0.0156(3) Uani d 1.0 . .
C C1 0.9224(3) 0.38536(12) 0.6306(2) 0.0181(4) Uani d 1.0 . .
H H1A 0.951625 0.336899 0.627365 0.022 Uiso calc 1.0 . .
C C2 0.9874(3) 0.42408(12) 0.7356(2) 0.0188(4) Uani d 1.0 . .
H H2A 1.060631 0.402727 0.802378 0.023 Uiso calc 1.0 . .
C C3 0.9436(3) 0.49444(12) 0.7413(2) 0.0206(4) Uani d 1.0 . .
H H3A 0.983732 0.521905 0.813299 0.025 Uiso calc 1.0 . .
C C4 0.8401(3) 0.52449(12) 0.6405(2) 0.0186(4) Uani d 1.0 . .
H H4A 0.808733 0.572768 0.642401 0.022 Uiso calc 1.0 . .
C C5 0.7829(3) 0.48257(11) 0.5363(2) 0.0144(4) Uani d 1.0 . .
C C6 0.6850(3) 0.51214(11) 0.4207(2) 0.0145(4) Uani d 1.0 . .
C C7 0.6296(3) 0.58192(11) 0.4135(2) 0.0187(4) Uani d 1.0 . .
H H7A 0.650676 0.611892 0.485057 0.022 Uiso calc 1.0 . .
C C8 0.5437(3) 0.60747(12) 0.3018(2) 0.0213(5) Uani d 1.0 . .
H H8A 0.506159 0.655037 0.295151 0.026 Uiso calc 1.0 . .
C C9 0.5138(3) 0.56184(12) 0.1997(2) 0.0219(5) Uani d 1.0 . .
H H9A 0.454847 0.577536 0.121638 0.026 Uiso calc 1.0 . .
C C10 0.5716(3) 0.49289(12) 0.2137(2) 0.0196(4) Uani d 1.0 . .
H H10A 0.549433 0.461869 0.143631 0.024 Uiso calc 1.0 . .
C C11 0.7050(3) 0.21294(11) 0.5014(2) 0.0169(4) Uani d 1.0 . .
C C12 0.6914(3) 0.14993(12) 0.5854(2) 0.0220(5) Uani d 1.0 . .
H H12A 0.673526 0.16561 0.670976 0.033 Uiso calc 0.51(3) . .
H H12B 0.592892 0.120736 0.551336 0.033 Uiso calc 0.51(3) . .
H H12C 0.798875 0.122381 0.588556 0.033 Uiso calc 0.51(3) . .
H H12D 0.703336 0.106874 0.536269 0.033 Uiso calc 0.49(3) . .
H H12E 0.78397 0.151749 0.655909 0.033 Uiso calc 0.49(3) . .
H H12F 0.577987 0.150104 0.618689 0.033 Uiso calc 0.49(3) . .
C C13 0.7238(3) 0.30785(12) 0.0762(2) 0.0165(4) Uani d 1.0 . .
C C14 0.7426(3) 0.29360(12) -0.0602(2) 0.0195(4) Uani d 1.0 . .
H H14A 0.78596 0.335912 -0.099174 0.029 Uiso calc 1.0 . .
H H14B 0.629206 0.280683 -0.10423 0.029 Uiso calc 1.0 . .
H H14C 0.824834 0.254881 -0.066527 0.029 Uiso calc 1.0 . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
U 0.01680(4) 0.00834(4) 0.01466(4) -0.00089(3) 0.00377(3) -0.00027(3)
O1 0.0174(8) 0.0175(8) 0.0218(8) -0.0030(6) 0.0027(6) 0.0015(6)
O2 0.0176(8) 0.0189(8) 0.0236(8) 0.0015(6) 0.0050(6) -0.0001(6)
O3 0.0275(9) 0.0137(7) 0.0177(7) -0.0030(6) 0.0051(6) 0.0008(6)
O4 0.0380(10) 0.0114(7) 0.0189(7) -0.0007(7) 0.0079(7) 0.0008(6)
O5 0.0281(9) 0.0122(7) 0.0173(7) 0.0013(6) 0.0055(6) -0.0003(6)
O6 0.0419(11) 0.0125(7) 0.0178(8) -0.0050(7) 0.0064(7) -0.0007(6)
N1 0.0158(9) 0.0105(8) 0.0190(8) -0.0011(7) 0.0034(7) -0.0007(6)
N2 0.0169(9) 0.0112(8) 0.0188(8) 0.0001(7) 0.0029(7) 0.0001(6)
C1 0.0185(11) 0.0140(10) 0.0218(10) 0.0009(8) 0.0023(8) 0.0016(8)
C2 0.0162(11) 0.0212(11) 0.0191(10) -0.0026(8) 0.0023(8) 0.0002(8)
C3 0.0213(11) 0.0218(11) 0.0189(10) -0.0039(9) 0.0037(8) -0.0057(8)
C4 0.0200(11) 0.0135(10) 0.0230(10) -0.0010(8) 0.0051(8) -0.0043(8)
C5 0.0133(9) 0.0123(9) 0.0187(9) -0.0018(7) 0.0065(7) -0.0014(7)
C6 0.0129(9) 0.0121(9) 0.0195(9) -0.0020(7) 0.0064(7) -0.0008(7)
C7 0.0226(11) 0.0121(10) 0.0227(10) 0.0010(8) 0.0078(9) -0.0014(8)
C8 0.0264(12) 0.0114(10) 0.0270(11) 0.0043(9) 0.0078(9) 0.0018(8)
C9 0.0246(12) 0.0186(11) 0.0224(11) 0.0049(9) 0.0021(9) 0.0029(8)
C10 0.0218(11) 0.0160(10) 0.0206(10) 0.0012(8) 0.0010(8) -0.0006(8)
C11 0.0162(10) 0.0139(10) 0.0203(10) -0.0022(8) 0.0009(8) 0.0021(8)
C12 0.0281(13) 0.0166(10) 0.0211(11) -0.0030(9) 0.0010(9) 0.0058(8)
C13 0.0163(10) 0.0157(10) 0.0177(10) 0.0015(8) 0.0022(8) 0.0006(8)
C14 0.0250(12) 0.0161(10) 0.0179(10) 0.0024(9) 0.0045(9) -0.0008(8)
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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O2 U O1 . . 179.09(7) ?
O2 U O6 . . 90.34(7) ?
O1 U O6 . . 88.96(7) ?
O2 U O4 . . 87.50(7) ?
O1 U O4 . . 92.75(6) ?
O6 U O4 . . 66.74(5) ?
O2 U O3 . . 97.43(7) ?
O1 U O3 . . 83.41(6) ?
O6 U O3 . . 118.40(5) ?
O4 U O3 . . 52.83(5) ?
O2 U O5 . . 84.70(7) ?
O1 U O5 . . 94.41(7) ?
O6 U O5 . . 52.91(5) ?
O4 U O5 . . 118.95(5) ?
O3 U O5 . . 171.18(5) ?
O2 U N1 . . 77.49(7) ?
O1 U N1 . . 103.18(6) ?
O6 U N1 . . 167.37(6) ?
O4 U N1 . . 115.38(6) ?
O3 U N1 . . 67.30(5) ?
O5 U N1 . . 121.51(5) ?
O2 U N2 . . 102.77(6) ?
O1 U N2 . . 77.09(6) ?
O6 U N2 . . 119.66(5) ?
O4 U N2 . . 167.45(6) ?
O3 U N2 . . 117.72(5) ?
O5 U N2 . . 69.82(5) ?
N1 U N2 . . 61.04(6) ?
O2 U C11 . . 93.19(7) ?
O1 U C11 . . 87.42(7) ?
O6 U C11 . . 92.41(6) ?
O4 U C11 . . 26.34(6) ?
O3 U C11 . . 26.50(6) ?
O5 U C11 . . 145.15(6) ?
N1 U C11 . . 91.63(6) ?
N2 U C11 . . 143.54(6) ?
O2 U C13 . . 85.75(7) ?
O1 U C13 . . 93.37(7) ?
O6 U C13 . . 26.27(6) ?
O4 U C13 . . 92.39(6) ?
O3 U C13 . . 144.65(6) ?
O5 U C13 . . 26.72(6) ?
N1 U C13 . . 146.42(6) ?
N2 U C13 . . 95.51(6) ?
C11 U C13 . . 118.45(6) ?
C11 O3 U . . 93.51(13) ?
C11 O4 U . . 94.26(13) ?
C13 O5 U . . 92.97(12) ?
C13 O6 U . . 94.81(13) ?
C1 N1 C5 . . 118.31(19) ?
C1 N1 U . . 117.82(14) ?
C5 N1 U . . 123.72(14) ?
C10 N2 C6 . . 117.71(19) ?
C10 N2 U . . 119.31(14) ?
C6 N2 U . . 122.34(14) ?
N1 C1 C2 . . 123.1(2) ?
N1 C1 H1A . . 118.5 ?
C2 C1 H1A . . 118.5 ?
C3 C2 C1 . . 118.7(2) ?
C3 C2 H2A . . 120.7 ?
C1 C2 H2A . . 120.7 ?
C2 C3 C4 . . 119.2(2) ?
C2 C3 H3A . . 120.4 ?
C4 C3 H3A . . 120.4 ?
C3 C4 C5 . . 118.9(2) ?
C3 C4 H4A . . 120.5 ?
C5 C4 H4A . . 120.5 ?
N1 C5 C4 . . 121.8(2) ?
N1 C5 C6 . . 116.16(18) ?
C4 C5 C6 . . 122.00(19) ?
N2 C6 C7 . . 121.8(2) ?
N2 C6 C5 . . 115.93(18) ?
C7 C6 C5 . . 122.27(19) ?
C8 C7 C6 . . 119.9(2) ?
C8 C7 H7A . . 120.1 ?
C6 C7 H7A . . 120.1 ?
C7 C8 C9 . . 118.3(2) ?
C7 C8 H8A . . 120.8 ?
C9 C8 H8A . . 120.8 ?
C10 C9 C8 . . 118.8(2) ?
C10 C9 H9A . . 120.6 ?
C8 C9 H9A . . 120.6 ?
N2 C10 C9 . . 123.5(2) ?
N2 C10 H10A . . 118.2 ?
C9 C10 H10A . . 118.2 ?
O4 C11 O3 . . 119.36(19) ?
O4 C11 C12 . . 120.3(2) ?
O3 C11 C12 . . 120.3(2) ?
O4 C11 U . . 59.41(11) ?
O3 C11 U . . 59.98(11) ?
C12 C11 U . . 178.56(16) ?
C11 C12 H12A . . 109.5 ?
C11 C12 H12B . . 109.5 ?
H12A C12 H12B . . 109.5 ?
C11 C12 H12C . . 109.5 ?
H12A C12 H12C . . 109.5 ?
H12B C12 H12C . . 109.5 ?
H12D C12 H12E . . 109.5 ?
H12D C12 H12F . . 109.5 ?
H12E C12 H12F . . 109.5 ?
O6 C13 O5 . . 118.96(19) ?
O6 C13 C14 . . 120.5(2) ?
O5 C13 C14 . . 120.57(19) ?
O6 C13 U . . 58.93(11) ?
O5 C13 U . . 60.31(11) ?
C14 C13 U . . 174.52(16) ?
C13 C14 H14A . . 109.5 ?
C13 C14 H14B . . 109.5 ?
H14A C14 H14B . . 109.5 ?
C13 C14 H14C . . 109.5 ?
H14A C14 H14C . . 109.5 ?
H14B C14 H14C . . 109.5 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
U O2 . 1.7733(16) y
U O1 . 1.7761(16) y
U O6 . 2.4415(16) y
U O4 . 2.4479(16) y
U O3 . 2.4602(15) y
U O5 . 2.4709(15) y
U N1 . 2.6185(18) y
U N2 . 2.6473(18) y
U C11 . 2.836(2) ?
U C13 . 2.840(2) ?
O3 C11 . 1.268(3) ?
O4 C11 . 1.262(3) ?
O5 C13 . 1.279(3) ?
O6 C13 . 1.262(3) ?
N1 C1 . 1.342(3) ?
N1 C5 . 1.352(3) ?
N2 C10 . 1.340(3) ?
N2 C6 . 1.357(3) ?
C1 C2 . 1.385(3) ?
C1 H1A . 0.95 ?
C2 C3 . 1.383(3) ?
C2 H2A . 0.95 ?
C3 C4 . 1.389(3) ?
C3 H3A . 0.95 ?
C4 C5 . 1.396(3) ?
C4 H4A . 0.95 ?
C5 C6 . 1.482(3) ?
C6 C7 . 1.394(3) ?
C7 C8 . 1.384(3) ?
C7 H7A . 0.95 ?
C8 C9 . 1.388(3) ?
C8 H8A . 0.95 ?
C9 C10 . 1.388(3) ?
C9 H9A . 0.95 ?
C10 H10A . 0.95 ?
C11 C12 . 1.504(3) ?
C12 H12A . 0.98 ?
C12 H12B . 0.98 ?
C12 H12C . 0.98 ?
C12 H12D . 0.98 ?
C12 H12E . 0.98 ?
C12 H12F . 0.98 ?
C13 C14 . 1.495(3) ?
C14 H14A . 0.98 ?
C14 H14B . 0.98 ?
C14 H14C . 0.98 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
C2 H2A O4 4_666 0.95 2.54 3.380(3) 148.2 y
C7 H7A O1 3_666 0.95 2.55 3.362(3) 143.1 y
C10 H10A O5 . 0.95 2.29 2.877(3) 119.6 ?
C12 H12E O1 4_666 0.98 2.33 3.311(3) 174.7 y
C14 H14B O2 4_565 0.98 2.50 3.296(3) 138.4 y
C14 H14C O1 4_665 0.98 2.46 3.389(3) 157.7 y
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
C5 N1 C1 C2 . . . . 1.9(3) ?
U N1 C1 C2 . . . . 177.67(17) ?
N1 C1 C2 C3 . . . . 0.7(3) ?
C1 C2 C3 C4 . . . . -1.7(3) ?
C2 C3 C4 C5 . . . . 0.2(3) ?
C1 N1 C5 C4 . . . . -3.6(3) ?
U N1 C5 C4 . . . . -179.05(15) ?
C1 N1 C5 C6 . . . . 173.81(18) ?
U N1 C5 C6 . . . . -1.7(2) ?
C3 C4 C5 N1 . . . . 2.6(3) ?
C3 C4 C5 C6 . . . . -174.7(2) ?
C10 N2 C6 C7 . . . . -0.8(3) ?
U N2 C6 C7 . . . . -171.52(15) ?
C10 N2 C6 C5 . . . . -178.84(19) ?
U N2 C6 C5 . . . . 10.4(2) ?
N1 C5 C6 N2 . . . . -5.6(3) ?
C4 C5 C6 N2 . . . . 171.74(19) ?
N1 C5 C6 C7 . . . . 176.32(19) ?
C4 C5 C6 C7 . . . . -6.3(3) ?
N2 C6 C7 C8 . . . . -0.1(3) ?
C5 C6 C7 C8 . . . . 177.8(2) ?
C6 C7 C8 C9 . . . . 0.6(3) ?
C7 C8 C9 C10 . . . . -0.2(3) ?
C6 N2 C10 C9 . . . . 1.2(3) ?
U N2 C10 C9 . . . . 172.24(18) ?
C8 C9 C10 N2 . . . . -0.7(4) ?
U O4 C11 O3 . . . . -1.9(2) ?
U O4 C11 C12 . . . . 178.36(19) ?
U O3 C11 O4 . . . . 1.9(2) ?
U O3 C11 C12 . . . . -178.37(19) ?
U O6 C13 O5 . . . . -6.1(2) ?
U O6 C13 C14 . . . . 173.66(19) ?
U O5 C13 O6 . . . . 6.0(2) ?
U O5 C13 C14 . . . . -173.75(19) ?
_cod_database_fobs_code 2312365