#------------------------------------------------------------------------------
#$Date: 2023-12-07 04:52:34 +0200 (Thu, 07 Dec 2023) $
#$Revision: 288111 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/31/23/2312367.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_2312367
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)2]'
_chemical_formula_moiety 'C24 H22 N4 O6 U'
_chemical_formula_sum 'C24 H22 N4 O6 U'
_chemical_formula_weight 700.48
_chemical_name_systematic
;
Bis(acetato-\k^2^O,O')(2,4'-bipyridine-\
\kN^1'^)dioxidouranium(VI)
;
_space_group_crystal_system triclinic
_space_group_IT_number 2
_space_group_name_Hall '-P 1'
_space_group_name_H-M_alt 'P -1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary dual
_atom_sites_solution_secondary difmap
_cell_angle_alpha 78.274(5)
_cell_angle_beta 84.648(5)
_cell_angle_gamma 74.814(5)
_cell_formula_units_Z 1
_cell_length_a 8.006(3)
_cell_length_b 8.786(3)
_cell_length_c 8.833(3)
_cell_measurement_reflns_used 4878
_cell_measurement_temperature 125.(2)
_cell_measurement_theta_max 30.4308
_cell_measurement_theta_min 2.3566
_cell_volume 586.6(4)
_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 0.979
_diffrn_measured_fraction_theta_max 0.979
_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 0.0266
_diffrn_reflns_av_unetI/netI 0.0345
_diffrn_reflns_limit_h_max 9
_diffrn_reflns_limit_h_min -9
_diffrn_reflns_limit_k_max 10
_diffrn_reflns_limit_k_min -10
_diffrn_reflns_limit_l_max 10
_diffrn_reflns_limit_l_min -10
_diffrn_reflns_number 5760
_diffrn_reflns_theta_full 25.24
_diffrn_reflns_theta_max 26.00
_diffrn_reflns_theta_min 2.36
_diffrn_source 'sealed X-ray tube'
_diffrn_source_current 30.0
_diffrn_source_power 1.50
_diffrn_source_voltage 50
_exptl_absorpt_coefficient_mu 6.966
_exptl_absorpt_correction_T_max 0.72
_exptl_absorpt_correction_T_min 0.35
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(SADABS: Bruker, 2013)
;
_exptl_crystal_colour yellow
_exptl_crystal_density_diffrn 1.983
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 334
_exptl_crystal_size_max 0.240
_exptl_crystal_size_mid 0.140
_exptl_crystal_size_min 0.050
_refine_diff_density_max 2.263
_refine_diff_density_min -2.631
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.082
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 161
_refine_ls_number_reflns 2260
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.082
_refine_ls_R_factor_all 0.0266
_refine_ls_R_factor_gt 0.0266
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0285P)^2^+1.9118P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0613
_refine_ls_wR_factor_ref 0.0613
_reflns_number_gt 2260
_reflns_number_total 2260
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file eq3014sup1.cif
_cod_data_source_block III_AW2913U
_cod_original_cell_volume 586.6(3)
_cod_database_code 2312367
_shelx_hkl_file
;
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-2 -1 11 9.62 1.57
1 1 -11 26.87 2.10
-1 -1 11 25.77 2.32
0 1 -11 22.48 1.96
0 -1 11 16.88 1.76
-1 1 -11 11.05 1.42
1 -1 11 10.25 1.50
-2 1 -11 16.30 1.57
2 -1 11 12.16 2.12
2 -1 11 11.92 1.57
-3 1 -11 8.21 1.42
3 -1 11 10.86 2.23
-4 1 -11 9.82 1.41
4 -1 11 10.94 2.39
4 0 -11 17.02 2.54
-4 0 11 15.91 1.80
3 0 -11 14.52 1.64
3 0 -11 11.37 2.22
2 0 -11 28.07 2.19
-2 0 11 28.62 2.24
1 0 -11 35.20 2.21
-1 0 11 29.89 2.27
0 0 11 16.56 1.66
-1 0 -11 12.94 1.48
1 0 11 9.83 1.45
-2 0 -11 13.65 1.49
2 0 11 11.61 2.29
2 0 11 10.23 1.51
-3 0 -11 18.57 1.64
3 0 11 12.38 1.58
3 0 11 12.12 2.38
-4 0 -11 16.11 1.60
-4 0 -11 15.09 2.57
4 0 11 15.33 2.61
-5 0 -11 3.91 2.69
-5 0 -11 9.46 1.45
5 0 11 11.91 3.11
4 -1 -11 15.22 2.51
-4 1 11 15.30 1.77
3 -1 -11 15.54 1.70
3 -1 -11 18.99 2.46
-3 1 11 14.95 1.73
2 -1 -11 8.78 1.97
2 -1 -11 7.78 1.35
-2 1 11 7.00 1.40
1 -1 -11 18.82 1.61
-1 1 11 15.70 1.62
0 -1 -11 50.96 2.37
0 1 11 44.78 2.45
-1 -1 -11 28.03 2.00
1 1 11 27.76 2.05
-2 -1 -11 27.09 2.01
2 1 11 25.54 2.82
2 1 11 27.18 2.08
-3 -1 -11 10.46 1.39
3 1 11 11.30 2.21
3 1 11 9.96 1.43
-4 -1 -11 10.04 1.43
-4 -1 -11 13.05 2.25
4 1 11 9.15 2.32
-5 -1 -11 21.57 2.83
-5 -1 -11 22.86 2.08
5 1 11 18.03 2.88
4 -2 -11 18.83 2.63
-4 2 11 17.89 1.91
3 -2 -11 24.23 2.64
3 -2 -11 18.92 1.76
-3 2 11 20.80 1.86
2 -2 -11 18.37 2.30
2 -2 -11 17.32 1.66
-2 2 11 15.50 1.69
1 -2 -11 20.29 1.87
1 -2 -11 20.31 2.28
-1 2 11 22.38 1.96
0 -2 -11 23.01 1.85
0 2 11 26.09 1.98
-1 -2 -11 26.98 2.08
-1 -2 -11 27.55 1.92
1 2 11 24.81 1.96
-2 -2 -11 23.31 2.14
-2 -2 -11 20.98 1.85
2 2 11 18.41 1.81
-3 -2 -11 26.50 2.31
-3 -2 -11 25.06 1.89
3 2 11 21.77 2.66
3 2 11 21.66 1.93
-4 -2 -11 31.10 2.08
-4 -2 -11 32.83 2.70
4 2 11 23.42 2.97
4 2 11 28.62 2.15
-5 -2 -11 14.51 1.58
-5 -2 -11 16.93 2.42
5 2 11 11.26 2.46
-6 -2 -11 6.62 2.38
4 -3 -11 14.28 2.21
3 -3 -11 29.86 2.43
3 -3 -11 25.76 2.08
3 -3 -11 29.42 3.37
-3 3 11 24.22 2.25
2 -3 -11 31.48 2.15
2 -3 -11 33.25 3.14
2 -3 -11 33.40 2.32
-2 3 11 34.41 2.29
1 -3 -11 26.31 2.04
1 -3 -11 22.56 1.88
1 -3 -11 23.68 2.69
-1 3 11 24.30 2.02
0 -3 -11 28.45 2.61
0 -3 -11 24.62 2.02
0 -3 -11 25.82 1.82
0 3 11 28.00 2.00
-1 -3 -11 29.49 2.10
-1 -3 -11 29.09 1.91
1 3 11 29.66 1.94
-2 -3 -11 17.27 1.94
-2 -3 -11 17.99 1.55
2 3 11 16.73 1.98
2 3 11 18.28 1.70
-3 -3 -11 17.89 1.70
-3 -3 -11 19.61 2.17
3 3 11 16.36 1.53
3 3 11 15.54 2.08
-4 -3 -11 18.28 1.79
-4 -3 -11 20.49 2.14
4 3 11 13.50 1.47
4 3 11 11.47 2.11
-5 -3 -11 18.78 2.31
-5 -3 -11 15.01 1.56
5 3 11 13.80 2.47
6 3 11 6.67 2.94
3 -4 -11 22.11 2.22
3 -4 -11 19.82 1.87
3 -4 -11 19.38 2.54
-3 4 11 17.81 1.85
2 -4 -11 15.12 2.17
2 -4 -11 12.32 1.45
2 -4 -11 15.60 1.89
-2 4 11 15.21 1.68
1 -4 -11 36.61 2.11
1 -4 -11 39.44 2.32
1 -4 -11 33.40 2.84
-1 4 11 37.11 2.30
0 -4 -11 45.88 2.46
0 -4 -11 44.64 2.21
0 -4 -11 45.92 2.93
0 4 11 47.28 2.39
-1 -4 -11 25.61 1.79
-1 -4 -11 26.86 2.04
-1 -4 -11 30.29 2.57
1 4 11 25.02 1.91
-2 -4 -11 14.03 1.35
-2 -4 -11 17.77 1.83
2 4 11 17.27 1.52
-3 -4 -11 22.31 2.03
-3 -4 -11 20.44 1.69
3 4 11 19.77 2.14
-4 -4 -11 15.49 1.94
-4 -4 -11 11.42 1.33
4 4 11 12.18 2.02
-5 -4 -11 18.24 2.54
-5 -4 -11 15.31 1.57
5 4 11 12.78 2.28
-6 -4 -11 8.68 1.62
6 4 11 7.57 2.83
3 -5 -11 12.61 1.87
2 -5 -11 20.26 2.08
2 -5 -11 17.43 2.35
2 -5 -11 15.42 1.51
-2 5 11 16.59 1.83
1 -5 -11 17.58 1.70
1 -5 -11 21.29 2.26
1 -5 -11 20.65 2.08
-1 5 11 21.92 1.88
0 -5 -11 22.27 2.20
0 -5 -11 19.97 1.88
0 -5 -11 16.36 1.60
0 5 11 19.10 1.89
-1 -5 -11 27.96 2.09
-1 -5 -11 28.61 2.31
-1 -5 -11 27.49 1.74
1 5 11 25.54 1.98
-2 -5 -11 26.62 2.08
-2 -5 -11 41.92 3.11
-2 -5 -11 29.84 1.76
-3 -5 -11 16.73 1.57
-3 -5 -11 19.90 1.89
3 5 11 18.59 2.09
-4 -5 -11 11.06 1.29
4 5 11 10.74 1.84
-5 -5 -11 19.00 1.82
5 5 11 17.55 2.38
-6 -5 -11 7.68 1.53
2 -6 -11 15.02 3.59
1 -6 -11 22.25 2.39
-1 6 11 18.23 1.89
0 -6 -11 14.34 1.87
0 6 11 15.88 1.67
-1 -6 -11 15.27 1.35
-1 -6 -11 13.08 1.82
-2 -6 -11 15.11 1.47
-2 -6 -11 18.81 2.07
-3 -6 -11 19.99 1.58
3 6 11 21.82 2.13
-4 -6 -11 26.35 1.77
4 6 11 29.17 2.54
-5 -6 -11 11.40 1.30
5 6 11 12.77 2.11
-6 -6 -11 10.52 1.90
0 -7 -11 32.45 2.88
0 7 11 30.40 2.34
-1 -7 -11 29.25 2.58
-2 -7 -11 12.03 1.71
-3 -7 -11 17.87 2.05
3 7 11 19.05 2.03
4 7 11 22.32 2.41
-5 -7 -11 16.45 1.57
-2 -8 -11 15.81 1.95
-3 -8 -11 21.20 2.33
1 0 -12 13.11 1.98
-1 0 12 11.68 2.33
0 0 -12 28.60 2.18
0 0 12 23.63 2.30
-1 0 -12 14.28 1.54
1 0 12 11.86 1.84
-2 0 -12 5.71 1.54
3 0 12 5.06 2.09
1 -1 -12 16.08 1.66
-1 1 12 15.96 1.72
0 -1 -12 12.25 1.53
0 1 12 9.85 1.52
-1 -1 -12 10.90 1.44
1 1 12 7.37 1.44
-2 -1 -12 17.00 1.65
2 1 12 14.01 1.65
-3 -1 -12 16.10 2.19
3 1 12 11.81 2.31
3 1 12 12.95 1.66
2 -2 -12 17.97 2.63
1 -2 -12 20.00 1.74
-1 2 12 14.87 1.75
0 -2 -12 16.80 1.65
0 2 12 17.16 1.65
-1 -2 -12 14.45 1.89
-1 -2 -12 13.79 1.47
1 2 12 13.98 1.61
-2 -2 -12 11.64 1.47
-2 -2 -12 15.07 1.97
2 2 12 9.60 1.44
2 2 12 7.34 1.79
-3 -2 -12 13.52 1.57
-3 -2 -12 21.77 2.34
3 2 12 6.44 1.94
3 2 12 12.24 1.54
-4 -2 -12 23.12 2.72
4 2 12 14.88 2.62
4 2 12 14.11 1.70
2 -3 -12 12.70 2.31
1 -3 -12 24.50 2.93
1 -3 -12 22.44 2.13
1 -3 -12 24.48 2.06
-1 3 12 21.54 1.97
0 -3 -12 31.19 2.12
0 -3 -12 32.16 2.29
0 3 12 29.25 2.23
-1 -3 -12 19.78 1.83
-1 -3 -12 18.64 2.09
1 3 12 18.09 1.68
-2 -3 -12 19.85 2.01
-2 -3 -12 15.55 1.57
2 3 12 14.46 1.59
-3 -3 -12 12.33 1.49
-3 -3 -12 19.07 2.12
3 3 12 13.00 1.51
3 3 12 11.63 1.97
-4 -3 -12 20.56 2.29
4 3 12 11.80 2.23
1 -4 -12 27.53 2.59
1 -4 -12 25.46 2.04
1 -4 -12 26.53 2.26
0 -4 -12 13.09 1.49
0 -4 -12 22.89 3.14
0 -4 -12 13.37 1.76
0 4 12 14.37 1.68
-1 -4 -12 23.07 1.86
-1 -4 -12 20.65 2.08
1 4 12 20.75 1.99
-2 -4 -12 30.74 2.29
-2 -4 -12 28.11 1.99
2 4 12 30.73 2.05
-3 -4 -12 17.61 2.09
-3 -4 -12 18.80 1.83
-4 -4 -12 9.80 1.78
4 4 12 8.37 1.85
0 -5 -12 20.20 2.07
0 -5 -12 20.04 1.63
0 -5 -12 19.97 2.31
0 5 12 22.57 2.22
-1 -5 -12 14.31 1.79
-1 -5 -12 13.66 1.40
1 5 12 12.70 1.54
-2 -5 -12 11.55 1.67
-2 -5 -12 11.46 1.34
-3 -5 -12 23.70 2.21
-3 -5 -12 22.86 1.86
3 5 12 23.38 2.34
4 5 12 13.85 2.05
-1 -6 -12 15.34 2.00
-1 -6 -12 15.54 1.45
1 6 12 16.45 2.36
-2 -6 -12 6.21 1.11
-3 -6 -12 14.64 1.43
3 6 12 15.14 1.89
0 0 0 0.00 0.00
;
_shelx_hkl_checksum 80438
_shelx_res_file
;
TITL AW2913U_a.res in P-1
AW2913U_a.res
created by SHELXL-2017/1 at 11:54:32 on 08-Nov-2023
REM Old TITL AW2913U in P1
REM SHELXT solution in P-1: R1 0.045, Rweak 0.299, Alpha 0.042
REM 0.000 for 0 systematic absences, Orientation as input
REM Formula found by SHELXT: C26 N2 O6 U
CELL 0.71073 8.00630 8.78640 8.83310 78.2745 84.6484 74.8141
ZERR 1.00 0.00270 0.00290 0.00290 0.0050 0.0045 0.0047
LATT 1
SFAC C H N O U
UNIT 24 22 4 6 1
TEMP -148
SIZE 0.24 0.14 0.05
REM light yellow block
L.S. 16
CONF
BOND $H
HTAB
EQIV $2 -x+1, -y+2, -z+1
HTAB C4 O2_$2
HTAB C12 N2_$2
MPLA 6 N1 C1 C2 C3 C4 C5
MPLA 6 N2 C6 C7 C8 C9 C10
ACTA
OMIT 0 52
LIST 4
FMAP 2
PLAN 20
REM EXTI 0.000955
WGHT 0.028500 1.911800
FVAR 0.18033
U 5 0.500000 1.000000 1.000000 10.50000 0.01675 0.01482 =
0.01439 -0.00708 0.00165 -0.00319
O1 4 0.437405 0.841643 1.132843 11.00000 0.02321 0.01557 =
0.02251 -0.00543 0.00029 -0.00715
O2 4 0.284262 1.002652 0.817760 11.00000 0.02100 0.02527 =
0.02345 -0.01312 -0.00081 -0.00234
O3 4 0.192304 1.154237 0.991652 11.00000 0.02182 0.02410 =
0.02019 -0.00948 -0.00086 -0.00152
N1 3 0.600001 0.806833 0.807861 11.00000 0.02184 0.01933 =
0.01613 -0.00794 -0.00049 -0.00365
N2 3 0.825602 0.559392 0.342277 11.00000 0.03908 0.02649 =
0.02413 -0.01264 0.00612 -0.00929
C1 1 0.609522 0.648682 0.849034 11.00000 0.02847 0.02166 =
0.02027 -0.00890 -0.00041 -0.00218
AFIX 43
H1B 2 0.583062 0.607259 0.953926 11.00000 -1.20000
AFIX 0
C2 1 0.656163 0.542839 0.745696 11.00000 0.02624 0.01716 =
0.02334 -0.00917 -0.00086 -0.00039
AFIX 43
H2B 2 0.659233 0.432421 0.779693 11.00000 -1.20000
AFIX 0
C3 1 0.698380 0.600614 0.591599 11.00000 0.01898 0.02074 =
0.02190 -0.00957 -0.00028 -0.00380
C4 1 0.689461 0.764144 0.549356 11.00000 0.03423 0.02251 =
0.01766 -0.00707 0.00434 -0.00998
AFIX 43
H4A 2 0.717602 0.808646 0.445814 11.00000 -1.20000
AFIX 0
C5 1 0.639203 0.861606 0.659503 11.00000 0.03050 0.02010 =
0.02495 -0.00824 0.00085 -0.00580
AFIX 43
H5A 2 0.632250 0.973022 0.627986 11.00000 -1.20000
AFIX 0
C6 1 0.750600 0.495202 0.473171 11.00000 0.02035 0.02198 =
0.02031 -0.00885 -0.00059 -0.00310
C7 1 0.723565 0.341260 0.498509 11.00000 0.02581 0.02368 =
0.01784 -0.00629 -0.00117 -0.00824
AFIX 43
H7A 2 0.668701 0.299732 0.592049 11.00000 -1.20000
AFIX 0
C8 1 0.779066 0.250217 0.383197 11.00000 0.03232 0.02173 =
0.02907 -0.01288 -0.00199 -0.00393
AFIX 43
H8A 2 0.762534 0.144998 0.396903 11.00000 -1.20000
AFIX 0
C9 1 0.858265 0.314066 0.248871 11.00000 0.03244 0.03049 =
0.02688 -0.01856 0.00262 -0.00426
AFIX 43
H9A 2 0.898205 0.253572 0.169094 11.00000 -1.20000
AFIX 0
C10 1 0.878179 0.468003 0.232998 11.00000 0.04247 0.03371 =
0.02379 -0.01558 0.00791 -0.00752
AFIX 43
H10A 2 0.931921 0.511925 0.139886 11.00000 -1.20000
AFIX 0
C11 1 0.162099 1.099754 0.877632 11.00000 0.02128 0.02042 =
0.02118 -0.00431 -0.00132 -0.00751
C12 1 -0.014739 1.149094 0.812769 11.00000 0.02080 0.02477 =
0.02923 -0.00569 -0.00610 -0.00238
AFIX 137
H12A 2 -0.039326 1.057500 0.779774 11.00000 -1.50000
H12B 2 -0.019017 1.237007 0.723752 11.00000 -1.50000
H12C 2 -0.101419 1.185014 0.892399 11.00000 -1.50000
AFIX 0
HKLF 4
REM AW2913U_a.res in P-1
REM R1 = 0.0266 for 2260 Fo > 4sig(Fo) and 0.0266 for all 2260 data
REM 161 parameters refined using 0 restraints
END
WGHT 0.0285 1.9118
REM Instructions for potential hydrogen bonds
HTAB C4 O2_$2
HTAB C12 N2_$2
REM Highest difference peak 2.263, deepest hole -2.631, 1-sigma level 0.156
Q1 1 0.4803 0.9606 1.1003 11.00000 0.05 2.26
Q2 1 0.3913 1.0309 0.9559 11.00000 0.05 1.70
Q3 1 0.5038 1.0761 1.0133 11.00000 0.05 0.93
Q4 1 0.3258 1.0545 1.0220 11.00000 0.05 0.88
Q5 1 0.3301 0.9815 1.0589 11.00000 0.05 0.85
Q6 1 0.3589 0.9401 1.0743 11.00000 0.05 0.80
Q7 1 0.4990 0.8256 1.0677 11.00000 0.05 0.79
Q8 1 0.6069 0.8394 1.0705 11.00000 0.05 0.79
Q9 1 0.0755 1.1184 0.8484 11.00000 0.05 0.62
Q10 1 0.4656 0.8435 1.1822 11.00000 0.05 0.57
Q11 1 0.3903 0.7982 1.1248 11.00000 0.05 0.48
Q12 1 0.3329 1.0979 1.0928 11.00000 0.05 0.47
Q13 1 0.2831 1.0281 0.9196 11.00000 0.05 0.44
Q14 1 0.2018 1.1079 1.0754 11.00000 0.05 0.39
Q15 1 0.2456 0.9243 1.1408 11.00000 0.05 0.35
Q16 1 0.2794 1.0933 0.7743 11.00000 0.05 0.35
Q17 1 0.2484 1.1971 0.9852 11.00000 0.05 0.34
Q18 1 0.5631 0.7941 1.1896 11.00000 0.05 0.33
Q19 1 0.4416 0.9019 0.6844 11.00000 0.05 0.33
Q20 1 0.1668 1.0780 0.9977 11.00000 0.05 0.33
;
_shelx_res_checksum 958
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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 0.5 1.0 1.0 0.01498(9) Uani d 1 . .
O O1 0.4374(4) 0.8416(4) 1.1328(4) 0.0198(7) Uani d 1 . .
O O2 0.2843(4) 1.0027(4) 0.8178(4) 0.0227(7) Uani d 1 . .
O O3 0.1923(4) 1.1542(4) 0.9917(4) 0.0221(7) Uani d 1 . .
N N1 0.6000(5) 0.8068(5) 0.8079(4) 0.0187(8) Uani d 1 . .
N N2 0.8256(6) 0.5594(5) 0.3423(5) 0.0290(10) Uani d 1 . .
C C1 0.6095(7) 0.6487(6) 0.8490(6) 0.0236(10) Uani d 1 . .
H H1B 0.583062 0.607259 0.953926 0.028 Uiso calc 1 . .
C C2 0.6562(6) 0.5428(6) 0.7457(5) 0.0224(10) Uani d 1 . .
H H2B 0.659233 0.432421 0.779693 0.027 Uiso calc 1 . .
C C3 0.6984(6) 0.6006(6) 0.5916(5) 0.0200(10) Uani d 1 . .
C C4 0.6895(7) 0.7641(6) 0.5494(5) 0.0241(10) Uani d 1 . .
H H4A 0.717602 0.808646 0.445814 0.029 Uiso calc 1 . .
C C5 0.6392(7) 0.8616(6) 0.6595(6) 0.0248(11) Uani d 1 . .
H H5A 0.63225 0.973022 0.627986 0.03 Uiso calc 1 . .
C C6 0.7506(6) 0.4952(6) 0.4732(5) 0.0206(10) Uani d 1 . .
C C7 0.7236(6) 0.3413(6) 0.4985(5) 0.0217(10) Uani d 1 . .
H H7A 0.668701 0.299732 0.592049 0.026 Uiso calc 1 . .
C C8 0.7791(7) 0.2502(6) 0.3832(6) 0.0270(11) Uani d 1 . .
H H8A 0.762534 0.144998 0.396903 0.032 Uiso calc 1 . .
C C9 0.8583(7) 0.3141(7) 0.2489(6) 0.0289(12) Uani d 1 . .
H H9A 0.898205 0.253572 0.169094 0.035 Uiso calc 1 . .
C C10 0.8782(8) 0.4680(7) 0.2330(6) 0.0328(13) Uani d 1 . .
H H10A 0.931921 0.511925 0.139886 0.039 Uiso calc 1 . .
C C11 0.1621(6) 1.0998(6) 0.8776(5) 0.0204(10) Uani d 1 . .
C C12 -0.0147(6) 1.1491(6) 0.8128(6) 0.0251(11) Uani d 1 . .
H H12A -0.039326 1.0575 0.779774 0.038 Uiso calc 1 . .
H H12B -0.019017 1.237007 0.723752 0.038 Uiso calc 1 . .
H H12C -0.101419 1.185014 0.892399 0.038 Uiso calc 1 . .
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 0.01675(14) 0.01482(13) 0.01439(13) -0.00319(9) 0.00165(8) -0.00708(9)
O1 0.0232(17) 0.0156(16) 0.0225(16) -0.0071(14) 0.0003(13) -0.0054(14)
O2 0.0210(17) 0.0253(18) 0.0235(17) -0.0023(14) -0.0008(13) -0.0131(15)
O3 0.0218(18) 0.0241(18) 0.0202(16) -0.0015(14) -0.0009(13) -0.0095(14)
N1 0.022(2) 0.019(2) 0.0161(18) -0.0036(16) -0.0005(15) -0.0079(16)
N2 0.039(3) 0.026(2) 0.024(2) -0.009(2) 0.0061(19) -0.0126(19)
C1 0.028(3) 0.022(3) 0.020(2) -0.002(2) -0.0004(19) -0.009(2)
C2 0.026(3) 0.017(2) 0.023(2) 0.000(2) -0.0009(19) -0.009(2)
C3 0.019(2) 0.021(2) 0.022(2) -0.0038(19) -0.0003(18) -0.010(2)
C4 0.034(3) 0.023(3) 0.018(2) -0.010(2) 0.004(2) -0.007(2)
C5 0.031(3) 0.020(3) 0.025(2) -0.006(2) 0.001(2) -0.008(2)
C6 0.020(2) 0.022(2) 0.020(2) -0.0031(19) -0.0006(18) -0.009(2)
C7 0.026(3) 0.024(3) 0.018(2) -0.008(2) -0.0012(18) -0.006(2)
C8 0.032(3) 0.022(3) 0.029(3) -0.004(2) -0.002(2) -0.013(2)
C9 0.032(3) 0.030(3) 0.027(3) -0.004(2) 0.003(2) -0.019(2)
C10 0.042(3) 0.034(3) 0.024(3) -0.008(3) 0.008(2) -0.016(2)
C11 0.021(2) 0.020(2) 0.021(2) -0.008(2) -0.0013(18) -0.004(2)
C12 0.021(3) 0.025(3) 0.029(3) -0.002(2) -0.006(2) -0.006(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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 U O1 2_677 . 180.0 ?
O1 U O2 2_677 . 88.92(13) ?
O1 U O2 . . 91.08(13) ?
O1 U O2 2_677 2_677 91.08(13) ?
O1 U O2 . 2_677 88.92(13) ?
O2 U O2 . 2_677 180.0 ?
O1 U O3 2_677 2_677 89.22(14) ?
O1 U O3 . 2_677 90.78(14) ?
O2 U O3 . 2_677 127.48(10) ?
O2 U O3 2_677 2_677 52.52(10) ?
O1 U O3 2_677 . 90.78(14) ?
O1 U O3 . . 89.22(14) ?
O2 U O3 . . 52.52(10) ?
O2 U O3 2_677 . 127.48(10) ?
O3 U O3 2_677 . 180.0 ?
O1 U N1 2_677 . 91.78(13) ?
O1 U N1 . . 88.22(13) ?
O2 U N1 . . 63.91(11) ?
O2 U N1 2_677 . 116.09(11) ?
O3 U N1 2_677 . 63.70(11) ?
O3 U N1 . . 116.30(11) ?
O1 U N1 2_677 2_677 88.22(13) ?
O1 U N1 . 2_677 91.78(13) ?
O2 U N1 . 2_677 116.10(11) ?
O2 U N1 2_677 2_677 63.90(11) ?
O3 U N1 2_677 2_677 116.30(11) ?
O3 U N1 . 2_677 63.70(11) ?
N1 U N1 . 2_677 180.0 ?
O1 U C11 2_677 2_677 89.91(15) ?
O1 U C11 . 2_677 90.09(14) ?
O2 U C11 . 2_677 153.71(12) ?
O2 U C11 2_677 2_677 26.29(12) ?
O3 U C11 2_677 2_677 26.23(12) ?
O3 U C11 . 2_677 153.77(12) ?
N1 U C11 . 2_677 89.89(13) ?
N1 U C11 2_677 2_677 90.11(13) ?
O1 U C11 2_677 . 90.09(14) ?
O1 U C11 . . 89.91(15) ?
O2 U C11 . . 26.29(12) ?
O2 U C11 2_677 . 153.71(12) ?
O3 U C11 2_677 . 153.77(12) ?
O3 U C11 . . 26.23(12) ?
N1 U C11 . . 90.11(13) ?
N1 U C11 2_677 . 89.89(13) ?
C11 U C11 2_677 . 180.0(3) ?
C11 O2 U . . 94.6(3) ?
C11 O3 U . . 93.8(3) ?
C5 N1 C1 . . 117.0(4) ?
C5 N1 U . . 120.7(3) ?
C1 N1 U . . 122.2(3) ?
C6 N2 C10 . . 117.4(5) ?
N1 C1 C2 . . 123.3(5) ?
N1 C1 H1B . . 118.3 ?
C2 C1 H1B . . 118.3 ?
C1 C2 C3 . . 119.3(5) ?
C1 C2 H2B . . 120.3 ?
C3 C2 H2B . . 120.3 ?
C4 C3 C2 . . 117.3(4) ?
C4 C3 C6 . . 119.9(4) ?
C2 C3 C6 . . 122.8(4) ?
C5 C4 C3 . . 119.6(5) ?
C5 C4 H4A . . 120.2 ?
C3 C4 H4A . . 120.2 ?
N1 C5 C4 . . 123.5(5) ?
N1 C5 H5A . . 118.3 ?
C4 C5 H5A . . 118.3 ?
N2 C6 C7 . . 122.9(4) ?
N2 C6 C3 . . 115.0(4) ?
C7 C6 C3 . . 122.1(4) ?
C8 C7 C6 . . 118.3(5) ?
C8 C7 H7A . . 120.9 ?
C6 C7 H7A . . 120.9 ?
C9 C8 C7 . . 119.4(5) ?
C9 C8 H8A . . 120.3 ?
C7 C8 H8A . . 120.3 ?
C8 C9 C10 . . 118.4(4) ?
C8 C9 H9A . . 120.8 ?
C10 C9 H9A . . 120.8 ?
N2 C10 C9 . . 123.6(5) ?
N2 C10 H10A . . 118.2 ?
C9 C10 H10A . . 118.2 ?
O3 C11 O2 . . 119.1(4) ?
O3 C11 C12 . . 120.9(4) ?
O2 C11 C12 . . 120.0(4) ?
O3 C11 U . . 60.0(2) ?
O2 C11 U . . 59.1(2) ?
C12 C11 U . . 179.0(3) ?
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 ?
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 O1 2_677 1.777(3) ?
U O1 . 1.777(3) y
U O2 . 2.461(3) y
U O2 2_677 2.461(3) ?
U O3 2_677 2.481(3) ?
U O3 . 2.481(3) y
U N1 . 2.571(4) y
U N1 2_677 2.571(4) ?
U C11 2_677 2.859(5) ?
U C11 . 2.859(5) ?
O2 C11 . 1.270(6) ?
O3 C11 . 1.267(5) ?
N1 C5 . 1.339(6) ?
N1 C1 . 1.347(6) ?
N2 C6 . 1.341(7) ?
N2 C10 . 1.348(6) ?
C1 C2 . 1.392(6) ?
C1 H1B . 0.95 ?
C2 C3 . 1.396(7) ?
C2 H2B . 0.95 ?
C3 C4 . 1.394(7) ?
C3 C6 . 1.495(6) ?
C4 C5 . 1.388(6) ?
C4 H4A . 0.95 ?
C5 H5A . 0.95 ?
C6 C7 . 1.396(7) ?
C7 C8 . 1.391(6) ?
C7 H7A . 0.95 ?
C8 C9 . 1.378(8) ?
C8 H8A . 0.95 ?
C9 C10 . 1.381(8) ?
C9 H9A . 0.95 ?
C10 H10A . 0.95 ?
C11 C12 . 1.500(7) ?
C12 H12A . 0.98 ?
C12 H12B . 0.98 ?
C12 H12C . 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
C4 H4A O2 2_676 0.95 2.57 3.487(6) 162.7 y
C12 H12B N2 2_676 0.98 2.61 3.309(7) 128.6 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 . . . . -0.5(7) ?
U N1 C1 C2 . . . . 177.2(4) ?
N1 C1 C2 C3 . . . . 1.1(8) ?
C1 C2 C3 C4 . . . . -0.6(7) ?
C1 C2 C3 C6 . . . . 179.7(4) ?
C2 C3 C4 C5 . . . . -0.3(7) ?
C6 C3 C4 C5 . . . . 179.4(5) ?
C1 N1 C5 C4 . . . . -0.6(7) ?
U N1 C5 C4 . . . . -178.2(4) ?
C3 C4 C5 N1 . . . . 0.9(8) ?
C10 N2 C6 C7 . . . . -0.9(8) ?
C10 N2 C6 C3 . . . . 178.7(5) ?
C4 C3 C6 N2 . . . . 15.5(7) ?
C2 C3 C6 N2 . . . . -164.8(5) ?
C4 C3 C6 C7 . . . . -164.8(5) ?
C2 C3 C6 C7 . . . . 14.8(7) ?
N2 C6 C7 C8 . . . . 0.8(7) ?
C3 C6 C7 C8 . . . . -178.8(4) ?
C6 C7 C8 C9 . . . . 0.0(7) ?
C7 C8 C9 C10 . . . . -0.6(8) ?
C6 N2 C10 C9 . . . . 0.2(8) ?
C8 C9 C10 N2 . . . . 0.5(9) ?
U O3 C11 O2 . . . . -1.0(5) ?
U O3 C11 C12 . . . . 179.3(4) ?
U O2 C11 O3 . . . . 1.0(5) ?
U O2 C11 C12 . . . . -179.3(4) ?
_cod_database_fobs_code 2312367