#------------------------------------------------------------------------------
#$Date: 2024-07-13 05:00:09 +0300 (Sat, 13 Jul 2024) $
#$Revision: 293407 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/31/2023198.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_2023198
loop_
_publ_author_name
'Vashchenko, Oleksandr V.'
'Khomenko, Dmytro M.'
'Doroshchuk, Roman O.'
'Stoica, Alexandru-Constantin'
'Vassilyeva, Olga Yu.'
'Lampeka, Rostyslav D.'
_publ_section_title
;
Crystal structure of
catena-poly[[methanoldioxidouranium(VI)]-\m-2-[5-(2-oxidophenyl)-1H-1,2,4-triazol-3-yl]acetato-\k2
O:O′]
;
_journal_coeditor_code EJ2005
_journal_issue 8
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_paper_doi 10.1107/S2056989024006637
_journal_volume 80
_journal_year 2024
_chemical_formula_iupac '[U (C10 H7 N3 O3) O2 (C H4 O)]'
_chemical_formula_moiety 'C11 H11 N3 O6 U'
_chemical_formula_sum 'C11 H11 N3 O6 U'
_chemical_formula_weight 519.26
_chemical_name_systematic
catena-Poly[[methanoldioxidouranium(VI)]-\m-2-[5-(2-oxidophenyl)-1H-1,2,4-triazol-3-yl]acetato-\k^2^O:O']
_space_group_crystal_system orthorhombic
_space_group_IT_number 61
_space_group_name_Hall '-P 2ac 2ab'
_space_group_name_H-M_alt 'P b c a'
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary dual
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 8
_cell_length_a 10.9966(6)
_cell_length_b 13.7147(10)
_cell_length_c 17.9345(9)
_cell_measurement_reflns_used 2366
_cell_measurement_temperature 200.00(10)
_cell_measurement_theta_max 30.7120
_cell_measurement_theta_min 2.6210
_cell_volume 2704.8(3)
_computing_cell_refinement
;
CrysAlisPro (Rigaku OD, 2023)
;
_computing_data_collection
;
CrysAlisPro (Rigaku OD, 2023)
;
_computing_data_reduction
;
CrysAlisPro (Rigaku OD, 2023)
;
_computing_molecular_graphics
;
Mercury (Macrae et al., 2020)
;
_computing_publication_material
;
Olex2 1.5 (Dolomanov et al., 2009)
;
_computing_structure_refinement
;
SHELXL2018/3 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2014/5 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 200.00(10)
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean 8.0797
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'Xcalibur, Eos'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_probe x-ray
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0404
_diffrn_reflns_av_unetI/netI 0.0496
_diffrn_reflns_limit_h_max 7
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_k_max 14
_diffrn_reflns_limit_k_min -16
_diffrn_reflns_limit_l_max 21
_diffrn_reflns_limit_l_min -11
_diffrn_reflns_number 6980
_diffrn_reflns_theta_full 25.027
_diffrn_reflns_theta_max 25.027
_diffrn_reflns_theta_min 2.271
_diffrn_source 'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu 12.034
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.50319
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2023)
;
_exptl_crystal_colour 'clear light red'
_exptl_crystal_density_diffrn 2.550
_exptl_crystal_description prism
_exptl_crystal_F_000 1904
_exptl_crystal_size_max 0.15
_exptl_crystal_size_mid 0.1
_exptl_crystal_size_min 0.1
_refine_diff_density_max 1.077
_refine_diff_density_min -0.816
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.047
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 194
_refine_ls_number_reflns 2380
_refine_ls_number_restraints 1
_refine_ls_restrained_S_all 1.047
_refine_ls_R_factor_all 0.0481
_refine_ls_R_factor_gt 0.0331
_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/[\s^2^(Fo^2^)+(0.0147P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0522
_refine_ls_wR_factor_ref 0.0561
_reflns_number_gt 1904
_reflns_number_total 2380
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file ej2005.cif
_cod_data_source_block I
_cod_database_code 2023198
_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_min 0.265
_shelx_estimated_absorpt_t_max 0.379
_shelx_hkl_file
;
0 0 2 3686.90 27.47
0 0 3 1.33 1.38
0 0 4 3141.65 36.63
0 0 5 -0.71 1.74
0 0 6 14.54 3.04
0 0 7 -0.19 1.69
0 0 8 867.96 27.44
0 0 9 0.92 2.28
0 0 10 1425.66 40.38
0 0 11 1.04 3.91
0 0 12 1119.95 39.94
0 0 13 13.71 5.51
0 0 13 2.68 3.91
0 0 14 1291.43 43.94
0 0 14 1285.29 47.49
0 0 15 3.33 5.68
0 0 15 4.95 4.76
0 0 16 1041.84 44.59
0 0 16 1058.18 46.83
0 0 17 7.46 6.19
0 0 17 4.44 6.76
0 0 18 376.73 30.50
0 0 19 4.91 5.90
0 0 20 105.32 18.11
0 0 21 -8.24 7.56
0 0 22 25.25 10.69
0 0 23 13.15 9.24
0 0 24 127.22 22.26
0 0 25 23.54 12.74
0 0 26 224.15 31.38
0 0 27 8.16 9.38
0 -1 1 6.01 1.66
0 1 -1 5.18 1.51
0 1 -2 2.96 0.91
0 -1 2 4.00 1.16
0 -1 2 7.04 1.98
0 1 -2 2.47 1.46
0 -1 3 1.29 0.98
0 1 -3 1.18 0.97
0 -1 3 1.70 1.62
0 -1 4 5.07 2.57
0 -1 4 2.01 1.51
0 1 -4 3.18 1.59
0 1 -5 2.19 1.85
0 -1 5 1.77 1.43
0 -1 6 4.73 2.34
0 -1 7 5.15 2.90
0 -1 8 1.17 2.27
0 -1 9 2.40 2.80
0 1 9 0.56 2.66
0 -1 9 -4.07 2.95
0 -1 10 8.74 3.80
0 1 10 8.12 3.90
0 -1 10 13.45 5.31
0 1 11 3.89 4.15
0 -1 11 5.18 3.73
0 -1 11 3.67 4.40
0 -1 12 4.29 4.61
0 -1 12 3.70 3.74
0 1 12 8.21 4.14
0 -1 13 -2.72 3.04
0 1 13 1.27 3.80
0 -1 13 -5.38 3.90
0 1 14 13.40 7.20
0 -1 14 4.71 5.44
0 -1 14 12.22 7.24
0 1 15 6.41 5.79
0 -1 15 2.87 5.46
0 -1 15 2.09 3.79
0 1 15 3.79 4.92
0 -1 16 18.22 8.74
0 1 16 13.70 8.38
0 1 16 17.31 7.62
0 -1 16 12.23 7.56
0 -1 17 4.81 4.49
0 -1 17 5.62 6.44
0 1 17 -0.52 5.23
0 -1 18 9.51 6.54
0 -1 18 2.33 6.35
0 1 18 8.97 8.22
0 -1 19 13.03 8.14
0 1 19 6.73 5.13
0 -1 20 -1.98 6.70
0 1 20 13.37 8.46
0 1 21 1.16 6.46
0 -1 21 -9.94 7.62
0 1 22 20.19 9.75
0 -1 22 -1.00 6.28
0 -1 23 4.16 6.49
0 1 23 3.11 8.41
0 -1 24 14.23 9.99
0 1 24 8.92 9.18
0 -1 25 13.46 9.16
0 1 25 20.05 13.36
0 1 26 15.14 13.20
0 -1 26 6.94 8.14
0 -1 27 24.73 14.98
0 2 0 9999.00 83.27
0 -2 0 9990.08 80.51
0 -2 -1 8.72 2.52
0 2 -1 12.27 3.34
0 2 1 9.52 2.58
0 -2 1 8.18 2.53
0 -2 2 4138.46 52.88
0 2 2 4070.91 40.52
0 2 -2 4256.36 36.97
0 2 -2 4330.68 53.45
0 -2 3 7.68 3.19
0 -2 3 10.53 2.22
0 2 -3 11.11 3.25
0 2 -3 10.72 2.15
0 -2 4 2351.83 42.50
0 -2 4 2301.09 31.75
0 2 -4 2301.34 31.78
0 -2 5 60.35 5.65
0 -2 5 52.73 6.99
0 2 -5 64.23 5.80
0 -2 6 134.24 11.39
0 -2 6 170.70 10.33
0 -2 7 511.46 23.38
0 -2 7 482.27 18.56
0 -2 8 289.29 18.35
0 -2 8 326.73 16.39
0 -2 9 232.63 14.79
0 -2 9 213.53 16.59
0 -2 10 890.45 35.40
0 -2 10 896.39 30.84
0 -2 11 380.28 21.45
0 -2 11 414.40 25.25
0 2 12 1479.58 48.64
0 -2 12 1429.61 48.93
0 -2 12 1537.46 45.16
0 2 13 111.29 14.33
0 -2 13 128.41 14.38
0 -2 13 118.76 15.17
0 -2 14 1451.18 48.64
0 2 14 1459.04 52.42
0 -2 14 1460.57 54.60
0 -2 15 3.70 5.25
0 -2 15 5.38 5.13
0 2 15 1.67 6.49
0 2 16 1334.50 43.46
0 -2 16 1337.97 57.36
0 -2 16 1379.44 51.47
0 2 16 1340.12 54.72
0 -2 17 57.18 11.78
0 -2 17 70.33 14.06
0 2 17 67.09 14.19
0 -2 18 204.20 22.04
0 2 18 208.39 23.17
0 -2 18 194.53 24.36
0 -2 19 93.00 16.10
0 2 19 121.55 18.94
0 2 20 46.70 13.11
0 -2 20 64.37 14.56
0 -2 21 56.87 13.85
0 2 21 70.75 16.94
0 -2 22 26.24 11.43
0 2 22 1.37 8.46
0 -2 23 60.52 15.76
0 2 23 73.05 18.29
0 -2 24 99.20 20.16
0 2 24 144.33 24.32
0 2 25 18.03 11.34
0 -2 25 23.47 10.80
0 -2 26 257.99 33.17
0 2 26 257.04 34.39
0 -3 0 8.66 3.76
0 3 0 10.08 4.48
0 -3 1 4.19 3.17
0 -3 -1 1.81 2.48
0 3 1 4.37 3.52
0 3 -1 4.09 2.93
0 -3 -2 7.80 3.29
0 3 -2 3.58 2.94
0 -3 2 -1.44 2.23
0 3 2 1.89 1.63
0 3 3 0.41 1.27
0 -3 3 -0.28 3.07
0 3 -3 1.37 1.66
0 3 -3 -0.77 2.44
0 3 4 0.10 1.47
0 -3 4 2.90 2.71
0 3 -4 2.46 1.70
0 -3 5 -0.49 1.58
0 -3 5 -0.41 2.68
0 3 -5 1.68 1.83
0 -3 6 -1.22 1.64
0 -3 6 -0.61 3.36
0 -3 7 3.06 3.59
0 -3 7 3.66 1.94
0 -3 8 5.32 5.09
0 -3 8 -0.61 2.42
0 -3 9 2.37 3.20
0 -3 9 7.29 5.04
0 -3 10 6.45 3.47
0 -3 10 3.76 4.55
0 -3 11 7.29 5.93
0 -3 11 5.19 4.08
0 -3 12 12.25 5.86
0 -3 12 2.87 6.21
0 -3 13 -2.36 3.45
0 -3 13 2.68 3.87
0 -3 14 16.01 7.02
0 -3 14 16.55 9.12
0 3 14 16.44 8.76
0 -3 15 10.98 8.24
0 3 15 -4.58 5.43
0 -3 15 3.32 4.85
0 -3 16 22.59 9.95
0 -3 16 3.40 7.23
0 3 16 17.80 9.55
0 -3 17 -4.39 6.84
0 3 17 0.90 4.67
0 -3 17 8.49 7.19
0 -3 18 -4.12 6.47
0 -3 18 5.37 7.53
0 3 18 -2.00 6.38
0 -3 19 5.43 5.65
0 -3 19 2.53 5.53
0 3 19 7.96 9.06
0 3 20 -4.71 7.00
0 -3 20 0.59 4.81
0 -3 21 21.94 11.45
0 3 21 -11.78 10.64
0 -3 22 -0.08 6.42
0 3 22 9.63 11.58
0 3 23 7.98 12.61
0 -3 23 14.18 9.80
0 3 24 8.21 11.32
0 -3 24 21.27 12.33
0 3 25 -0.90 8.34
0 -3 25 15.26 10.47
0 3 26 28.57 17.13
0 4 0 894.52 34.60
0 -4 0 804.30 31.64
0 4 1 2.92 2.69
0 -4 -1 3.93 3.70
0 -4 1 -2.01 4.82
0 4 2 3078.08 58.68
0 -4 2 2931.13 63.24
0 -4 -2 2865.79 53.62
0 -4 3 641.75 29.64
0 -4 -3 686.12 24.21
0 4 3 663.92 25.22
0 -4 4 935.24 36.07
0 4 4 872.76 27.46
0 4 -4 855.90 23.76
0 -4 5 479.34 26.32
0 4 5 456.79 18.83
0 4 6 110.40 9.07
0 -4 6 106.30 13.06
0 4 7 1166.29 28.94
0 -4 7 1157.79 31.02
0 -4 7 1088.40 42.16
0 -4 8 3.68 3.10
0 -4 8 4.95 2.01
0 -4 9 1176.03 34.37
0 -4 9 1147.81 45.79
0 -4 10 585.43 25.57
0 -4 10 583.08 33.95
0 -4 11 670.52 28.83
0 -4 11 772.19 40.23
0 -4 12 1498.81 58.22
0 -4 12 1389.79 43.62
0 -4 13 126.82 14.14
0 -4 13 130.18 18.54
0 -4 14 1288.38 58.46
0 -4 14 1261.78 45.76
0 4 15 23.82 9.39
0 -4 15 25.63 8.09
0 -4 15 2.45 6.31
0 4 16 1183.47 53.91
0 -4 16 1059.78 58.31
0 -4 16 1110.48 46.51
0 -4 17 129.34 21.48
0 4 17 141.89 20.28
0 -4 17 148.08 18.24
0 -4 18 123.58 20.91
0 -4 18 116.39 17.16
0 4 18 164.64 22.10
0 -4 19 253.88 25.20
0 4 19 219.22 27.07
0 -4 19 236.09 30.81
0 -4 20 26.32 10.86
0 4 20 14.29 9.28
0 4 21 225.09 28.63
0 -4 21 233.00 26.38
0 4 22 33.62 13.15
0 -4 22 50.00 13.80
0 4 23 127.60 23.45
0 -4 23 121.56 20.58
0 4 24 62.54 18.31
0 -4 24 57.34 15.55
0 4 25 43.86 16.90
0 -5 0 1.95 4.74
0 -5 1 5.02 5.25
0 -5 -1 7.44 4.92
0 -5 -2 -2.80 2.49
0 -5 2 6.43 5.29
0 -5 -3 4.50 4.68
0 -5 3 3.28 3.27
0 -5 4 6.73 4.32
0 -5 5 0.05 4.38
0 5 5 3.05 2.74
0 -5 6 -2.52 4.94
0 5 6 1.24 3.16
0 -5 6 1.14 0.89
0 5 7 4.37 3.32
0 -5 7 -0.96 4.28
0 -5 8 -7.21 6.89
0 5 8 -0.70 2.28
0 -5 9 6.43 6.71
0 -5 9 5.89 3.80
0 5 9 5.15 3.18
0 5 10 2.20 1.91
0 -5 10 -3.71 5.80
0 -5 10 0.85 2.45
0 -5 11 -1.88 5.25
0 -5 11 3.99 4.05
0 -5 12 2.08 4.98
0 -5 12 -0.96 5.32
0 -5 13 -4.59 4.04
0 -5 13 0.32 5.67
0 -5 14 -1.38 5.28
0 -5 14 -2.96 4.01
0 -5 15 -0.73 4.00
0 -5 15 -6.15 7.30
0 -5 16 8.97 9.55
0 -5 16 6.72 6.81
0 -5 17 3.59 6.70
0 -5 17 14.89 10.01
0 5 17 -6.29 7.74
0 -5 18 1.09 6.07
0 5 18 -3.45 7.36
0 -5 18 9.10 10.24
0 5 19 7.06 8.28
0 -5 19 14.16 12.46
0 -5 19 14.21 8.45
0 -5 20 21.88 10.36
0 5 20 13.43 10.31
0 -5 20 5.17 8.72
0 5 21 1.89 9.08
0 -5 21 1.19 7.81
0 5 22 1.35 9.52
0 -5 22 21.29 10.65
0 5 23 -2.35 9.16
0 -5 23 -4.39 7.09
0 5 24 5.70 12.34
0 5 25 34.54 15.72
0 -6 0 824.33 38.16
0 -6 1 91.25 13.84
0 -6 -1 82.22 12.43
0 -6 -2 672.44 33.08
0 -6 2 681.92 36.61
0 -6 3 589.04 34.31
0 -6 -3 573.89 29.28
0 -6 4 235.20 22.36
0 -6 -4 232.59 17.86
0 -6 5 1830.27 62.40
0 -6 6 12.21 5.92
0 -6 7 1357.05 55.41
0 -6 7 1241.70 17.62
0 -6 8 1.25 1.35
0 -6 8 -7.75 6.59
0 -6 9 1569.23 62.75
0 -6 10 339.96 30.29
0 -6 11 623.04 41.27
0 -6 12 564.08 41.54
0 -6 13 143.72 15.37
0 -6 13 161.92 23.13
0 -6 14 608.91 32.89
0 -6 14 641.04 46.52
0 -6 15 66.96 16.02
0 -6 15 66.79 11.79
0 -6 16 313.59 24.93
0 -6 16 333.13 36.19
0 -6 17 180.15 20.38
0 -6 17 202.01 28.96
0 -6 18 172.73 27.84
0 6 18 147.56 22.27
0 -6 18 150.60 19.75
0 6 19 440.55 38.29
0 -6 19 432.45 32.88
0 -6 19 386.41 43.20
0 -6 20 12.77 9.70
0 -6 20 1.02 5.44
0 6 20 7.53 9.13
0 -6 21 385.14 33.06
0 6 21 443.32 41.48
0 6 22 2.99 8.79
0 -6 22 20.05 9.92
0 6 23 198.18 29.47
0 6 24 49.92 17.35
0 6 25 109.77 24.69
0 -7 0 8.60 7.04
0 -7 1 -1.06 4.93
0 -7 -1 0.23 4.15
0 -7 2 3.69 6.30
0 -7 -2 2.80 3.60
0 -7 -3 1.15 3.78
0 -7 3 4.74 4.33
0 -7 -4 2.60 4.05
0 -7 4 -3.52 4.53
0 -7 5 -0.24 5.43
0 -7 6 5.14 5.30
0 -7 7 17.99 9.46
0 -7 8 1.92 6.56
0 -7 9 2.95 7.89
0 -7 9 2.01 1.34
0 -7 10 1.50 6.30
0 -7 11 -0.48 6.50
0 -7 12 12.00 8.13
0 -7 13 -7.89 6.17
0 -7 14 -5.92 6.06
0 -7 15 13.51 14.30
0 -7 16 -10.25 8.50
0 -7 17 -10.99 7.83
0 -7 18 4.80 10.01
0 7 19 3.08 8.14
0 -7 19 11.16 7.87
0 7 20 15.02 13.91
0 -7 20 22.72 13.41
0 7 21 -8.60 9.90
0 7 22 8.46 8.68
0 7 23 36.52 16.33
0 7 24 22.46 14.25
0 -8 0 196.58 21.63
0 -8 1 300.96 26.80
0 -8 -1 297.15 25.92
0 -8 2 234.94 24.24
0 -8 -2 177.50 20.03
0 -8 -3 1240.60 50.47
0 -8 3 1393.98 59.12
0 -8 -4 37.28 9.45
0 -8 4 76.10 14.85
0 -8 5 2366.31 80.78
0 -8 6 9.19 6.58
0 -8 7 1479.93 66.15
0 -8 8 25.97 9.69
0 -8 9 812.06 50.53
0 -8 10 40.13 13.13
0 -8 11 367.97 35.69
0 -8 12 66.56 15.39
0 -8 13 134.33 23.00
0 -8 14 171.14 25.60
0 -8 15 25.96 12.35
0 -8 16 15.08 12.89
0 -8 17 154.30 27.41
0 -8 18 36.84 15.47
0 -8 19 429.66 47.64
0 8 20 3.58 8.51
0 -8 20 -0.19 9.43
0 8 21 470.88 44.45
0 -8 21 446.57 50.54
0 8 22 0.04 8.62
0 8 23 324.38 39.18
0 -9 0 6.31 5.98
0 -9 1 -3.50 4.03
0 -9 -1 5.50 6.20
0 -9 2 11.82 7.87
0 -9 -2 1.01 3.91
0 -9 -3 -2.16 3.68
0 -9 3 1.45 6.47
0 -9 4 -3.75 6.09
0 -9 -4 8.33 6.17
0 -9 5 2.44 6.43
0 -9 6 2.47 5.23
0 -9 7 1.10 6.38
0 -9 8 8.76 8.11
0 -9 9 0.56 6.43
0 -9 10 4.90 8.19
0 -9 11 4.29 6.82
0 -9 12 -14.20 11.79
0 -9 13 -2.73 6.58
0 -9 14 -1.83 7.92
0 -9 15 -0.71 8.60
0 -9 16 0.83 7.53
0 -9 17 -16.53 11.89
0 -9 18 28.29 15.21
0 -9 19 22.68 14.21
0 -9 20 6.22 9.27
0 9 21 15.30 11.52
0 -9 21 39.35 17.59
0 9 22 5.05 10.93
0 9 23 13.17 14.23
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-13 3 6 498.99 46.70
-13 -3 7 15.91 10.93
-13 3 7 22.34 12.96
-13 -3 8 447.73 39.93
-13 3 8 458.24 44.92
-13 -3 9 37.30 14.00
-13 3 9 4.50 7.66
-13 -3 10 252.47 30.53
-13 3 10 209.89 32.54
-13 3 11 28.10 11.92
-13 -3 11 70.05 17.66
-13 3 11 96.58 24.23
-13 3 12 131.99 24.74
-13 -3 12 97.96 20.91
-13 3 12 100.46 25.43
-13 3 13 109.36 23.27
-13 -3 13 91.30 19.85
-13 3 13 123.61 28.25
-13 3 14 -4.27 7.73
-13 -3 14 -7.79 7.32
-13 3 14 -0.20 13.37
-13 3 15 89.72 23.23
-13 -3 15 60.84 17.34
-13 4 0 -8.43 10.56
-13 4 -1 3.11 9.86
-13 4 1 2.01 9.03
-13 -4 2 1.53 8.68
-13 4 -2 13.85 13.06
-13 4 2 6.47 8.39
-13 -4 3 6.08 8.52
-13 4 -3 13.41 13.07
-13 4 3 12.76 11.43
-13 4 -4 4.19 10.77
-13 -4 4 2.08 6.66
-13 4 4 1.98 8.61
-13 -4 5 21.53 8.15
-13 4 5 5.96 10.05
-13 -4 6 8.10 6.27
-13 4 6 12.79 13.81
-13 -4 7 -4.25 7.17
-13 4 7 -6.96 7.96
-13 -4 8 34.43 13.28
-13 4 8 9.56 10.27
-13 4 9 8.57 9.44
-13 -4 9 17.41 10.63
-13 4 9 7.79 7.87
-13 4 10 6.43 9.74
-13 -4 10 5.78 7.95
-13 4 10 7.91 10.95
-13 4 11 9.42 7.53
-13 -4 11 1.85 6.74
-13 4 12 12.00 12.43
-13 -4 12 19.07 11.19
-13 4 12 -18.06 14.29
-13 4 13 1.53 9.09
-13 -4 13 19.56 12.99
-13 4 13 16.40 13.90
-13 4 14 10.90 11.70
-13 4 15 13.26 12.70
-13 5 0 11.15 12.69
-13 5 -1 390.96 41.26
-13 5 1 409.43 41.80
-13 5 -2 71.80 19.22
-13 5 2 60.80 18.07
-13 5 3 269.16 35.73
-13 -5 3 245.38 28.73
-13 5 -3 251.01 33.53
-13 5 -4 134.69 24.64
-13 -5 4 183.58 24.51
-13 5 4 184.27 30.58
-13 -5 5 70.70 17.78
-13 5 5 32.50 13.69
-13 -5 6 281.19 31.30
-13 5 6 279.05 37.09
-13 -5 7 -4.95 7.76
-13 5 7 5.91 11.76
-13 -5 8 311.54 32.55
-13 5 8 281.81 37.64
-13 -5 9 75.47 17.97
-13 5 9 47.79 17.65
-13 -5 10 151.16 23.37
-13 5 10 129.76 26.54
-13 5 11 176.01 27.66
-13 -5 11 143.91 23.43
-13 5 11 175.70 31.93
-13 5 12 103.86 22.02
-13 5 12 66.11 22.23
-13 5 13 202.05 30.74
-13 5 14 11.18 13.44
-13 5 15 181.97 31.71
-13 6 0 3.49 8.45
-13 6 -1 8.56 11.30
-13 6 1 11.32 9.15
-13 6 -2 13.75 12.51
-13 6 2 6.18 8.68
-13 6 -3 33.72 14.66
-13 6 3 26.70 16.02
-13 6 -4 19.36 13.60
-13 6 4 4.45 8.87
-13 -6 5 -10.26 8.51
-13 6 5 17.09 10.94
-13 -6 6 9.28 8.47
-13 6 6 -1.27 11.08
-13 -6 7 2.67 7.57
-13 6 7 -1.23 9.42
-13 -6 8 13.59 8.45
-13 6 8 9.76 10.56
-13 -6 9 -2.24 7.01
-13 6 9 2.54 9.70
-13 6 10 15.77 13.47
-13 6 11 15.13 13.99
-13 6 12 16.74 14.03
-13 6 13 24.64 15.29
-13 6 14 24.01 15.37
-13 6 15 18.71 13.91
-13 7 0 18.34 13.95
-13 7 -1 421.84 44.27
-13 7 1 502.38 47.68
-13 7 -2 74.34 20.08
-13 7 2 51.91 18.69
-13 7 -3 341.73 40.27
-13 7 3 360.05 42.03
-13 7 -4 68.48 21.34
-13 7 4 49.32 18.08
-13 7 -5 82.00 19.96
-13 7 5 55.29 16.29
-13 7 6 84.26 21.94
-13 -7 7 1.52 6.69
-13 7 7 -1.43 10.85
-13 7 8 161.78 29.70
-13 7 9 98.25 24.84
-13 7 10 25.65 15.75
-13 7 11 262.30 39.01
-13 8 0 -8.70 9.25
-13 8 -1 42.78 16.04
-13 8 1 24.05 12.61
-13 8 -2 0.71 8.52
-13 8 2 -0.51 12.24
-13 8 -3 -4.31 8.02
-13 8 3 23.71 16.05
-13 8 -4 0.29 10.98
-13 8 4 32.47 15.41
-13 8 -5 15.16 14.07
-13 8 5 -0.21 10.91
-13 8 6 -8.13 11.12
-13 8 7 7.25 12.10
-13 8 8 10.07 13.81
-13 8 9 -4.93 11.10
-13 9 0 16.93 16.07
-13 9 -1 495.10 49.42
-13 9 1 408.10 45.35
-13 9 -2 29.95 15.03
-13 9 2 11.84 11.93
-13 9 -3 234.30 35.26
-13 9 3 198.46 31.88
-13 9 -4 8.91 12.86
-13 9 4 21.76 16.37
-13 9 -5 108.61 23.44
-13 9 5 124.69 25.97
-13 9 6 29.40 18.54
-13 9 7 -14.68 12.36
-13 9 8 12.89 14.89
-13 -10 0 12.91 11.27
-13 10 0 0.77 10.21
-13 -10 1 12.93 10.13
-13 10 -1 22.48 14.53
-13 10 1 -1.44 9.82
-13 10 -2 1.17 12.88
-13 10 2 -0.25 11.28
-13 10 -3 -2.05 12.33
-13 10 3 19.57 13.46
-13 10 -4 -0.43 12.03
-13 10 4 -2.16 9.69
-13 10 -5 4.87 10.74
-13 10 5 3.33 9.98
-13 10 6 14.28 11.27
-13 10 7 27.27 14.57
-13 -11 0 16.76 12.50
-13 11 0 15.59 11.88
-13 11 -1 423.03 47.16
-13 11 1 381.36 45.15
-13 -11 1 353.72 40.86
-13 -11 2 7.89 10.09
-13 11 -2 1.13 11.73
-13 11 2 15.64 14.04
-13 -11 3 126.91 24.67
-13 11 -3 182.63 31.29
-13 11 3 190.37 33.56
-13 -11 4 28.89 15.47
-13 11 -4 -4.21 10.92
-13 11 4 9.12 9.52
-13 -11 5 77.57 22.52
-13 11 5 106.76 25.35
-13 -11 6 35.43 17.26
-13 12 0 5.09 9.81
-13 -12 1 4.73 12.78
-13 12 -1 9.56 11.68
-13 12 1 2.62 9.90
-13 -12 2 30.34 16.99
-13 12 -2 -20.18 13.64
-13 12 2 34.49 17.91
-13 -12 3 38.92 16.79
-13 12 -3 22.20 16.01
-13 -12 4 16.34 12.22
-13 12 -4 2.13 9.15
-13 13 -2 6.39 9.98
-14 0 0 67.38 18.50
-14 0 -1 11.25 11.90
-14 0 1 -9.44 8.27
-14 0 2 74.69 18.57
-14 0 3 -2.09 9.46
-14 0 4 19.33 9.45
-14 0 5 -2.32 11.39
-14 0 6 -11.19 9.74
-14 0 7 -19.52 12.76
-14 0 8 17.21 13.67
-14 0 9 -0.49 10.80
-14 0 10 40.44 17.90
-14 0 11 6.77 10.29
-14 0 12 34.89 17.90
-14 0 13 11.73 12.18
-14 -1 0 602.45 49.45
-14 1 0 476.97 44.91
-14 1 -1 3.59 7.05
-14 -1 1 -2.53 7.72
-14 1 1 -0.43 8.96
-14 1 -2 508.21 46.34
-14 -1 2 574.92 48.13
-14 1 2 543.14 47.71
-14 -1 3 -0.27 8.73
-14 1 3 -5.54 9.17
-14 -1 4 204.09 30.33
-14 1 4 221.74 30.64
-14 -1 5 25.60 12.01
-14 1 5 3.67 8.01
-14 -1 6 45.36 15.86
-14 1 6 58.26 19.09
-14 -1 7 32.82 14.55
-14 1 7 34.62 14.10
-14 -1 8 32.23 15.82
-14 1 8 34.72 14.84
-14 -1 9 14.73 12.24
-14 1 9 15.15 14.77
-14 -1 10 217.21 31.75
-14 1 10 200.40 33.01
-14 -1 11 -0.47 7.75
-14 1 11 18.75 16.64
-14 -1 12 333.03 39.84
-14 1 12 345.46 42.06
-14 -1 13 13.30 13.83
-14 2 0 42.12 15.56
-14 -2 1 5.09 6.95
-14 2 -1 21.25 15.52
-14 2 1 18.03 12.22
-14 2 -2 61.73 18.68
-14 -2 2 40.37 14.32
-14 2 2 38.41 16.57
-14 -2 3 -6.64 6.68
-14 2 3 10.69 13.61
-14 -2 4 16.92 9.41
-14 2 4 7.02 11.30
-14 -2 5 -13.90 12.38
-14 2 5 3.54 11.22
-14 -2 6 -5.34 10.41
-14 2 6 3.25 10.00
-14 -2 7 12.84 10.62
-14 2 7 30.11 14.61
-14 -2 8 1.01 9.55
-14 2 8 24.57 13.94
-14 -2 9 7.00 7.86
-14 2 9 31.15 17.50
-14 -2 10 32.08 14.92
-14 2 10 5.30 8.90
-14 -2 11 11.17 11.70
-14 2 11 32.97 15.39
-14 -2 12 31.93 16.54
-14 2 12 47.11 18.58
-14 -2 13 -11.29 11.32
-14 3 0 509.30 48.04
-14 3 -1 18.46 14.44
-14 3 1 27.96 13.80
-14 -3 2 385.36 38.85
-14 3 -2 449.36 44.24
-14 3 2 355.65 40.46
-14 3 -3 30.04 11.76
-14 -3 3 13.81 9.58
-14 3 3 55.31 17.58
-14 -3 4 224.32 29.55
-14 3 4 215.24 32.70
-14 -3 5 90.89 19.53
-14 3 5 75.35 21.06
-14 -3 6 36.03 15.51
-14 3 6 4.31 11.28
-14 -3 7 158.69 26.51
-14 3 7 153.14 27.65
-14 -3 8 37.97 14.66
-14 3 8 34.27 16.49
-14 -3 9 63.42 18.36
-14 3 9 83.80 21.27
-14 -3 10 135.31 23.47
-14 3 10 166.50 29.67
-14 -3 11 71.93 20.51
-14 3 11 36.99 18.00
-14 -3 12 236.62 31.98
-14 -3 13 23.46 13.32
-14 -3 14 255.65 33.86
-14 4 0 10.04 11.94
-14 4 -1 13.07 14.59
-14 4 1 -0.50 10.39
-14 4 -2 33.03 15.28
-14 4 2 43.96 16.10
-14 -4 3 4.89 9.49
-14 4 -3 -5.33 9.12
-14 4 3 0.25 9.03
-14 -4 4 -4.37 6.76
-14 4 4 15.34 13.17
-14 -4 5 13.78 10.91
-14 4 5 16.38 11.33
-14 -4 6 3.95 8.50
-14 4 6 17.59 12.66
-14 -4 7 18.06 9.34
-14 4 7 33.82 14.60
-14 -4 8 13.31 11.72
-14 4 8 -6.81 8.91
-14 -4 9 9.37 10.68
-14 4 9 8.58 13.38
-14 -4 10 10.30 10.89
-14 4 10 24.51 11.40
-14 -4 11 9.68 9.26
-14 -4 12 37.36 16.41
-14 5 0 268.95 36.90
-14 5 -1 37.50 16.20
-14 5 1 70.35 21.17
-14 5 -2 264.48 37.00
-14 5 2 269.54 36.32
-14 5 -3 95.90 21.75
-14 5 3 88.37 23.23
-14 5 -4 104.90 24.07
-14 -5 4 152.36 24.77
-14 5 4 90.75 23.48
-14 -5 5 196.15 28.79
-14 5 5 227.71 34.86
-14 -5 6 25.70 12.09
-14 5 6 33.56 16.87
-14 5 7 323.73 41.27
-14 -5 7 261.81 31.57
-14 -5 8 -1.91 8.28
-14 5 8 23.49 16.27
-14 -5 9 222.44 29.10
-14 5 9 213.53 34.63
-14 -5 10 78.00 18.56
-14 6 0 2.13 10.51
-14 6 -1 14.13 13.65
-14 6 1 31.29 17.81
-14 6 -2 7.68 13.93
-14 6 2 2.18 9.57
-14 6 -3 19.09 14.74
-14 6 3 10.95 11.86
-14 6 -4 3.89 10.77
-14 6 4 0.79 10.56
-14 6 5 9.00 11.93
-14 -6 6 19.51 10.75
-14 6 6 29.99 15.65
-14 -6 7 13.97 9.18
-14 6 7 31.16 17.22
-14 -6 8 -3.48 7.61
-14 6 8 24.68 16.28
-14 7 0 88.08 23.37
-14 7 -1 -2.62 10.33
-14 7 1 11.54 12.46
-14 7 -2 121.33 26.46
-14 7 2 82.94 21.72
-14 7 -3 159.96 29.71
-14 7 3 144.31 29.80
-14 7 -4 47.19 19.04
-14 7 4 49.10 19.07
-14 7 5 251.33 37.68
-14 7 6 3.16 10.25
-14 7 7 378.17 46.41
-14 8 0 36.88 14.74
-14 8 -1 18.18 15.57
-14 8 1 12.53 11.96
-14 8 -2 25.90 16.66
-14 8 2 -1.65 9.71
-14 8 -3 22.12 15.93
-14 8 3 43.14 20.65
-14 8 -4 20.82 13.88
-14 8 4 -3.89 13.46
-14 8 5 2.64 13.02
-14 9 0 7.76 8.84
-14 9 -1 -3.64 9.83
-14 9 1 -1.09 11.46
-14 9 -2 21.34 13.58
-14 9 2 21.80 17.09
-14 9 -3 78.65 22.59
-14 9 3 109.02 27.70
-14 9 -4 36.38 16.67
-14 -10 1 -24.59 13.06
-14 10 -1 19.77 14.72
-14 10 -2 20.74 15.03
-14 10 -3 37.60 18.93
-14 10 -4 -12.30 14.15
-14 -11 2 19.24 13.28
-15 0 0 9.78 11.92
-15 0 1 5.36 10.96
-15 0 2 22.28 14.35
-15 0 3 6.29 14.89
-15 0 4 47.57 17.09
-15 0 5 -8.63 12.00
-15 0 6 171.25 28.66
-15 0 7 7.25 9.07
-15 0 8 170.77 30.45
-15 0 9 15.38 13.48
-15 1 0 1.90 8.07
-15 1 -1 14.28 16.39
-15 -1 1 15.21 11.22
-15 1 1 14.47 9.64
-15 -1 2 95.53 21.62
-15 1 2 45.76 21.64
-15 -1 3 22.47 14.26
-15 1 3 6.27 9.60
-15 -1 4 249.14 34.65
-15 1 4 208.24 31.62
-15 -1 5 -13.09 10.32
-15 1 5 16.17 13.03
-15 -1 6 380.91 41.72
-15 1 6 322.99 40.45
-15 -1 7 7.05 11.03
-15 1 7 84.68 24.38
-15 -1 8 269.44 36.37
-15 1 8 222.36 33.60
-15 -1 9 14.55 15.80
-15 2 0 -8.97 8.43
-15 2 -1 27.86 15.23
-15 2 1 2.02 11.39
-15 -2 2 25.62 12.50
-15 2 2 9.90 13.18
-15 -2 3 39.60 16.89
-15 2 3 32.10 15.05
-15 -2 4 73.00 20.52
-15 2 4 98.14 21.72
-15 -2 5 -11.11 9.73
-15 2 5 6.82 13.79
-15 -2 6 135.71 23.66
-15 2 6 160.18 29.35
-15 -2 7 -5.73 11.32
-15 2 7 15.34 12.48
-15 -2 8 130.98 25.06
-15 -2 9 19.24 12.45
-15 3 0 4.98 10.06
-15 3 -1 121.66 25.47
-15 3 1 109.85 25.33
-15 3 -2 75.48 20.38
-15 3 2 97.50 23.96
-15 -3 3 69.05 18.64
-15 3 3 102.40 24.06
-15 -3 4 226.94 31.45
-15 3 4 205.42 33.70
-15 -3 5 37.33 17.42
-15 3 5 46.11 19.00
-15 -3 6 257.34 33.40
-15 3 6 279.60 37.94
-15 -3 7 -6.39 7.56
-15 -3 8 248.16 33.63
-15 -3 9 18.65 12.33
-15 -3 10 141.73 27.30
-15 4 0 14.00 13.94
-15 4 -1 60.85 19.80
-15 4 1 54.59 20.03
-15 4 -2 23.65 14.81
-15 4 2 44.59 17.31
-15 4 3 64.50 22.43
-15 -4 4 103.61 21.92
-15 4 4 48.24 16.90
-15 -4 5 26.37 14.14
-15 4 5 4.54 8.82
-15 -4 6 90.10 21.20
-15 -4 7 -0.36 8.97
-15 -4 8 63.31 18.36
-15 -4 9 21.10 12.38
-15 -4 10 82.19 21.55
-15 5 0 3.83 10.27
-15 5 -1 235.78 35.86
-15 5 1 208.79 34.26
-15 5 -2 36.21 15.06
-15 5 2 36.05 18.13
-15 5 -3 87.60 24.97
-15 5 3 59.92 19.88
-15 -5 6 124.48 24.50
-15 -5 7 22.20 12.49
-15 -5 8 182.74 28.25
-15 -5 9 14.77 11.42
-15 6 0 42.44 19.80
-15 6 -1 108.59 26.77
-15 6 -2 25.14 18.66
0 0 0 0.00 0.00
TITL shI_3654_YaLa in Pbca
REM Pbca (#61 in standard setting)
CELL 0.71073 10.996556 13.714678 17.934471 90.0000 90.0000 90.0000
ZERR 4.00 0.000555 0.000984 0.000896 0.0000 0.0000 0.0000
LATT 1
SYMM -x+1/2,-y, z+1/2
SYMM -x, y+1/2,-z+1/2
SYMM x+1/2,-y+1/2,-z
SFAC C H N O U
UNIT 120.00 120.00 24.00 16.00 4.00
TREF
HKLF 4
END
_computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)'
;
_shelx_hkl_checksum 76498
_shelx_res_file
;
TITL shi_3654_yala_a.res in Pbca
shi_3654_yala.res
created by SHELXL-2018/3 at 15:42:42 on 01-Jul-2024
REM Old TITL shI_3654_YaLa in Pbca #61
REM SHELXT solution in Pbca
REM R1 0.145, Rweak 0.010, Alpha 0.062, Orientation as input
REM Formula found by SHELXT: C6 N3 O1 I
CELL 0.71073 10.996556 13.714678 17.934471 90 90 90
ZERR 8 0.000555 0.000984 0.000896 0 0 0
LATT 1
SYMM 0.5-X,-Y,0.5+Z
SYMM -X,0.5+Y,0.5-Z
SYMM 0.5+X,0.5-Y,-Z
SFAC C H N O U
UNIT 88 88 24 48 8
EQIV $1 0.5+X,0.5-Y,1-Z
EQIV $2 +X,0.5-Y,0.5+Z
EQIV $3 -0.5+X,+Y,1.5-Z
EQIV $4 1.5-X,-0.5+Y,+Z
EQIV $5 +X,0.5-Y,-0.5+Z
DFIX 0.85 0.01 O6 H6
L.S. 20
PLAN 5
SIZE 0.1 0.1 0.15
TEMP -73
CONF
HTAB O6 O3_$1
HTAB N3 O6_$2
HTAB N3 O4_$3
HTAB C10 O2_$4
HTAB C11 N2_$5
htab
BOND $H
list 4
MORE -1
fmap 2
acta
SHEL 99 0.84
OMIT 0 2 0
OMIT 0 2 1
OMIT 8 11 7
REM
REM
REM
WGHT 0.014700
FVAR 0.12714
U1 5 0.693910 0.275796 0.535123 11.00000 0.01371 0.02400 =
0.01753 -0.00098 -0.00102 0.00033
O1 4 0.670590 0.161213 0.492737 11.00000 0.02974 0.02832 =
0.02968 0.00165 -0.00256 0.00034
O2 4 0.719411 0.390237 0.576342 11.00000 0.01545 0.03042 =
0.02513 -0.00218 -0.00088 0.00295
O3 4 0.517498 0.270036 0.599183 11.00000 0.01891 0.03834 =
0.01752 -0.00397 -0.00167 0.00059
O4 4 1.073356 0.148201 0.561289 11.00000 0.01411 0.03761 =
0.03061 0.01067 0.01071 0.00700
O5 4 0.900706 0.230225 0.553706 11.00000 0.01956 0.03543 =
0.02230 0.01767 0.00580 -0.00255
O6 4 0.824122 0.335522 0.432332 11.00000 0.01787 0.02588 =
0.02683 0.00161 0.00295 0.00320
H6 2 0.875390 0.290219 0.425218 11.00000 -1.50000
N1 3 0.727610 0.201111 0.660836 11.00000 0.01078 0.02719 =
0.02557 0.00191 0.00175 -0.00586
N2 3 0.816277 0.126303 0.756626 11.00000 0.02920 0.03234 =
0.02838 0.00641 -0.00145 -0.00433
N3 3 0.719471 0.179721 0.780371 11.00000 0.02696 0.03934 =
0.01719 0.00553 0.00078 0.00279
AFIX 43
H3 2 0.694586 0.183100 0.826934 11.00000 -1.20000
AFIX 0
C1 1 0.494033 0.311731 0.665399 11.00000 0.01838 0.02023 =
0.02930 0.00263 0.00441 -0.00620
C2 1 0.394357 0.373551 0.672689 11.00000 0.02178 0.02452 =
0.03913 -0.00079 0.00208 -0.00187
AFIX 43
H2 2 0.343935 0.386412 0.630816 11.00000 -1.20000
AFIX 0
C3 1 0.368578 0.416174 0.740487 11.00000 0.02357 0.02536 =
0.05917 0.00377 0.01551 -0.00212
AFIX 43
H3A 2 0.299727 0.457636 0.744780 11.00000 -1.20000
AFIX 0
C4 1 0.440067 0.400043 0.801777 11.00000 0.03033 0.03442 =
0.04171 -0.00516 0.01894 -0.01282
AFIX 43
H4 2 0.421840 0.430771 0.847916 11.00000 -1.20000
AFIX 0
C5 1 0.538276 0.338984 0.795704 11.00000 0.03164 0.03258 =
0.02429 -0.00012 0.00230 -0.01202
AFIX 43
H5 2 0.588149 0.327390 0.838037 11.00000 -1.20000
AFIX 0
C6 1 0.565799 0.293859 0.728469 11.00000 0.01921 0.02443 =
0.01969 -0.00288 0.00701 -0.00568
C7 1 0.667420 0.226308 0.723322 11.00000 0.01775 0.02855 =
0.02349 0.00709 -0.00173 -0.00760
C8 1 0.817996 0.138839 0.684871 11.00000 0.01579 0.02264 =
0.02293 0.00533 0.00219 -0.00560
C9 1 0.964784 0.162010 0.579674 11.00000 0.02427 0.01883 =
0.02012 -0.00034 -0.00103 -0.00399
C10 1 0.908987 0.093902 0.634661 11.00000 0.01544 0.02524 =
0.04441 0.00915 -0.00034 -0.00429
AFIX 23
H10A 2 0.869498 0.039972 0.607091 11.00000 -1.20000
H10B 2 0.974574 0.065223 0.665466 11.00000 -1.20000
AFIX 0
C11 1 0.862004 0.435205 0.430325 11.00000 0.05122 0.03832 =
0.03735 -0.00125 0.00644 -0.01248
AFIX 137
H11A 2 0.902753 0.448521 0.382807 11.00000 -1.50000
H11B 2 0.918432 0.447745 0.471518 11.00000 -1.50000
H11C 2 0.790796 0.477681 0.435274 11.00000 -1.50000
AFIX 0
HKLF 4
REM shi_3654_yala_a.res in Pbca
REM wR2 = 0.0561, GooF = S = 1.047, Restrained GooF = 1.047 for all data
REM R1 = 0.0331 for 1904 Fo > 4sig(Fo) and 0.0481 for all 2380 data
REM 194 parameters refined using 1 restraints
END
WGHT 0.0147 0.0000
REM Instructions for potential hydrogen bonds
HTAB O6 O3_$1
HTAB N3 O4_$3
HTAB N3 O6_$2
HTAB C10 O2_$4
HTAB C11 N2_$5
REM Highest difference peak 1.077, deepest hole -0.816, 1-sigma level 0.160
Q1 1 0.6910 0.2066 0.5315 11.00000 0.05 1.08
Q2 1 0.7341 0.3497 0.5261 11.00000 0.05 0.97
Q3 1 0.6291 0.2794 0.4975 11.00000 0.05 0.64
Q4 1 0.6988 0.2363 0.6003 11.00000 0.05 0.60
Q5 1 0.4569 0.2656 0.5354 11.00000 0.05 0.56
;
_shelx_res_checksum 32205
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, 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 U1 0.69391(2) 0.27580(2) 0.53512(2) 0.01841(9) Uani d 1 . .
O O1 0.6706(4) 0.1612(4) 0.4927(2) 0.0292(13) Uani d 1 . .
O O2 0.7194(4) 0.3902(4) 0.5763(2) 0.0237(12) Uani d 1 . .
O O3 0.5175(4) 0.2700(4) 0.5992(2) 0.0249(12) Uani d 1 . .
O O4 1.0734(4) 0.1482(4) 0.5613(2) 0.0274(13) Uani d 1 . .
O O5 0.9007(4) 0.2302(4) 0.5537(2) 0.0258(12) Uani d 1 . .
O O6 0.8241(4) 0.3355(4) 0.4323(3) 0.0235(12) Uani d 1 . .
H H6 0.875(5) 0.290(4) 0.425(4) 0.035 Uiso d 1 . .
N N1 0.7276(5) 0.2011(4) 0.6608(3) 0.0212(15) Uani d 1 . .
N N2 0.8163(5) 0.1263(5) 0.7566(3) 0.0300(15) Uani d 1 . .
N N3 0.7195(5) 0.1797(5) 0.7804(3) 0.0278(15) Uani d 1 . .
H H3 0.694586 0.183100 0.826934 0.033 Uiso calc 1 . .
C C1 0.4940(6) 0.3117(5) 0.6654(4) 0.0226(17) Uani d 1 . .
C C2 0.3944(6) 0.3736(5) 0.6727(4) 0.0285(19) Uani d 1 . .
H H2 0.343935 0.386412 0.630816 0.034 Uiso calc 1 . .
C C3 0.3686(7) 0.4162(6) 0.7405(5) 0.036(2) Uani d 1 . .
H H3A 0.299727 0.457636 0.744780 0.043 Uiso calc 1 . .
C C4 0.4401(6) 0.4000(6) 0.8018(4) 0.035(2) Uani d 1 . .
H H4 0.421840 0.430771 0.847916 0.043 Uiso calc 1 . .
C C5 0.5383(7) 0.3390(6) 0.7957(4) 0.0295(19) Uani d 1 . .
H H5 0.588149 0.327390 0.838037 0.035 Uiso calc 1 . .
C C6 0.5658(6) 0.2939(5) 0.7285(3) 0.0211(17) Uani d 1 . .
C C7 0.6674(6) 0.2263(5) 0.7233(4) 0.0233(17) Uani d 1 . .
C C8 0.8180(6) 0.1388(5) 0.6849(4) 0.0205(16) Uani d 1 . .
C C9 0.9648(6) 0.1620(5) 0.5797(4) 0.0211(17) Uani d 1 . .
C C10 0.9090(6) 0.0939(5) 0.6347(4) 0.0284(19) Uani d 1 . .
H H10A 0.869498 0.039972 0.607091 0.034 Uiso calc 1 . .
H H10B 0.974574 0.065223 0.665466 0.034 Uiso calc 1 . .
C C11 0.8620(7) 0.4352(6) 0.4303(4) 0.042(2) Uani d 1 . .
H H11A 0.902753 0.448521 0.382807 0.063 Uiso calc 1 . .
H H11B 0.918432 0.447745 0.471518 0.063 Uiso calc 1 . .
H H11C 0.790796 0.477681 0.435274 0.063 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
U1 0.01371(14) 0.02400(17) 0.01753(13) 0.00033(12) -0.00102(12) -0.00098(14)
O1 0.030(3) 0.028(3) 0.030(3) 0.000(2) -0.003(2) 0.002(3)
O2 0.015(3) 0.030(3) 0.025(3) 0.003(2) -0.001(2) -0.002(2)
O3 0.019(2) 0.038(3) 0.018(2) 0.001(2) -0.002(2) -0.004(3)
O4 0.014(3) 0.038(4) 0.031(3) 0.007(2) 0.011(2) 0.011(3)
O5 0.020(3) 0.035(3) 0.022(2) -0.003(2) 0.006(2) 0.018(3)
O6 0.018(3) 0.026(3) 0.027(2) 0.003(2) 0.003(2) 0.002(3)
N1 0.011(3) 0.027(4) 0.026(3) -0.006(2) 0.002(3) 0.002(3)
N2 0.029(4) 0.032(4) 0.028(3) -0.004(3) -0.001(3) 0.006(3)
N3 0.027(4) 0.039(4) 0.017(3) 0.003(3) 0.001(3) 0.006(3)
C1 0.018(4) 0.020(5) 0.029(4) -0.006(3) 0.004(3) 0.003(4)
C2 0.022(4) 0.025(5) 0.039(4) -0.002(3) 0.002(4) -0.001(4)
C3 0.024(4) 0.025(5) 0.059(6) -0.002(4) 0.016(4) 0.004(5)
C4 0.030(5) 0.034(5) 0.042(5) -0.013(4) 0.019(4) -0.005(5)
C5 0.032(5) 0.033(5) 0.024(4) -0.012(4) 0.002(4) 0.000(4)
C6 0.019(4) 0.024(5) 0.020(3) -0.006(3) 0.007(3) -0.003(3)
C7 0.018(4) 0.029(5) 0.023(4) -0.008(3) -0.002(3) 0.007(4)
C8 0.016(4) 0.023(4) 0.023(4) -0.006(3) 0.002(3) 0.005(4)
C9 0.024(4) 0.019(5) 0.020(4) -0.004(3) -0.001(3) 0.000(4)
C10 0.015(4) 0.025(5) 0.044(5) -0.004(3) 0.000(4) 0.009(4)
C11 0.051(5) 0.038(6) 0.037(5) -0.012(5) 0.006(4) -0.001(5)
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 U1 O3 . . 93.63(19) y
O1 U1 O4 . 4_456 89.78(19) y
O1 U1 O5 . . 88.01(19) y
O1 U1 O6 . . 93.32(19) y
O1 U1 N1 . . 92.6(2) y
O2 U1 O1 . . 179.0(2) y
O2 U1 O3 . . 87.38(18) y
O2 U1 O4 . 4_456 90.19(18) y
O2 U1 O5 . . 91.33(18) y
O2 U1 O6 . . 85.72(19) y
O2 U1 N1 . . 87.88(19) y
O3 U1 O4 . 4_456 84.70(15) y
O3 U1 O5 . . 137.78(15) y
O3 U1 O6 . . 152.73(16) y
O3 U1 N1 . . 69.78(16) y
O4 U1 O6 4_456 . 68.98(15) y
O4 U1 N1 4_456 . 154.47(16) y
O5 U1 O4 . 4_456 137.52(15) y
O5 U1 O6 . . 68.81(14) y
O5 U1 N1 . . 68.00(15) y
O6 U1 N1 . . 136.12(15) y
C1 O3 U1 . . 126.9(4) ?
C9 O4 U1 . 4_556 130.3(4) ?
C9 O5 U1 . . 141.3(4) ?
U1 O6 H6 . . 105(5) ?
C11 O6 U1 . . 120.3(4) ?
C11 O6 H6 . . 120(5) ?
C7 N1 U1 . . 124.9(4) ?
C7 N1 C8 . . 104.7(6) ?
C8 N1 U1 . . 129.9(4) ?
C8 N2 N3 . . 104.5(6) ?
N2 N3 H3 . . 124.7 ?
C7 N3 N2 . . 110.7(6) ?
C7 N3 H3 . . 124.7 ?
O3 C1 C2 . . 119.6(7) ?
O3 C1 C6 . . 122.1(6) ?
C2 C1 C6 . . 118.3(7) ?
C1 C2 H2 . . 119.9 ?
C3 C2 C1 . . 120.2(7) ?
C3 C2 H2 . . 119.9 ?
C2 C3 H3A . . 119.3 ?
C4 C3 C2 . . 121.4(7) ?
C4 C3 H3A . . 119.3 ?
C3 C4 H4 . . 120.4 ?
C3 C4 C5 . . 119.2(8) ?
C5 C4 H4 . . 120.4 ?
C4 C5 H5 . . 119.6 ?
C4 C5 C6 . . 120.9(7) ?
C6 C5 H5 . . 119.6 ?
C1 C6 C7 . . 119.5(6) ?
C5 C6 C1 . . 120.0(6) ?
C5 C6 C7 . . 120.4(6) ?
N1 C7 C6 . . 126.4(6) ?
N3 C7 N1 . . 107.7(6) ?
N3 C7 C6 . . 125.8(6) ?
N1 C8 C10 . . 123.7(6) ?
N2 C8 N1 . . 112.4(6) ?
N2 C8 C10 . . 123.9(7) ?
O4 C9 O5 . . 123.2(6) ?
O4 C9 C10 . . 118.1(6) ?
O5 C9 C10 . . 118.7(6) ?
C8 C10 C9 . . 114.8(6) ?
C8 C10 H10A . . 108.6 ?
C8 C10 H10B . . 108.6 ?
C9 C10 H10A . . 108.6 ?
C9 C10 H10B . . 108.6 ?
H10A C10 H10B . . 107.5 ?
O6 C11 H11A . . 109.5 ?
O6 C11 H11B . . 109.5 ?
O6 C11 H11C . . 109.5 ?
H11A C11 H11B . . 109.5 ?
H11A C11 H11C . . 109.5 ?
H11B C11 H11C . . 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
U1 O1 . 1.764(5) y
U1 O2 . 1.757(5) y
U1 O3 . 2.256(4) y
U1 O4 4_456 2.415(4) y
U1 O5 . 2.382(5) y
U1 O6 . 2.474(5) y
U1 N1 . 2.504(5) y
O3 C1 . 1.343(8) ?
O4 C9 . 1.253(7) ?
O5 C9 . 1.260(8) ?
O6 H6 . 0.849(10) ?
O6 C11 . 1.430(8) ?
N1 C7 . 1.347(8) ?
N1 C8 . 1.380(8) ?
N2 N3 . 1.361(8) ?
N2 C8 . 1.298(8) ?
N3 H3 . 0.8800 ?
N3 C7 . 1.335(8) ?
C1 C2 . 1.392(9) ?
C1 C6 . 1.401(9) ?
C2 H2 . 0.9500 ?
C2 C3 . 1.379(10) ?
C3 H3A . 0.9500 ?
C3 C4 . 1.369(10) ?
C4 H4 . 0.9500 ?
C4 C5 . 1.371(10) ?
C5 H5 . 0.9500 ?
C5 C6 . 1.389(9) ?
C6 C7 . 1.454(9) ?
C8 C10 . 1.481(9) ?
C9 C10 . 1.490(9) ?
C10 H10A . 0.9900 ?
C10 H10B . 0.9900 ?
C11 H11A . 0.9800 ?
C11 H11B . 0.9800 ?
C11 H11C . 0.9800 ?
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
O6 H6 O3 4_556 0.849(10) 1.82(3) 2.634(6) 160(7) yes
N3 H3 O4 6_557 0.88 2.45 3.291(7) 159.0 yes
N3 H3 O6 7_566 0.88 2.38 2.966(7) 124.2 yes
C10 H10A O2 8_755 0.99 2.34 3.300(8) 163.0 yes
C11 H11A N2 7_565 0.98 2.66 3.266(10) 120.3 yes
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
U1 O3 C1 C2 . . . . 125.8(6) ?
U1 O3 C1 C6 . . . . -55.2(9) ?
U1 O4 C9 O5 4_556 . . . -8.3(10) ?
U1 O4 C9 C10 4_556 . . . 171.3(4) ?
U1 O5 C9 O4 . . . . 158.0(5) ?
U1 O5 C9 C10 . . . . -21.7(11) ?
U1 N1 C7 N3 . . . . -172.7(4) ?
U1 N1 C7 C6 . . . . 5.9(10) ?
U1 N1 C8 N2 . . . . 170.6(4) ?
U1 N1 C8 C10 . . . . -7.6(10) ?
O3 C1 C2 C3 . . . . 179.4(6) ?
O3 C1 C6 C5 . . . . 179.7(6) ?
O3 C1 C6 C7 . . . . -1.6(10) ?
O4 C9 C10 C8 . . . . 146.7(6) ?
O5 C9 C10 C8 . . . . -33.6(9) ?
N1 C8 C10 C9 . . . . 45.3(9) ?
N2 N3 C7 N1 . . . . 2.0(8) ?
N2 N3 C7 C6 . . . . -176.6(6) ?
N2 C8 C10 C9 . . . . -132.7(7) ?
N3 N2 C8 N1 . . . . 1.8(8) ?
N3 N2 C8 C10 . . . . 180.0(6) ?
C1 C2 C3 C4 . . . . 0.7(11) ?
C1 C6 C7 N1 . . . . 23.3(11) ?
C1 C6 C7 N3 . . . . -158.3(7) ?
C2 C1 C6 C5 . . . . -1.3(10) ?
C2 C1 C6 C7 . . . . 177.4(6) ?
C2 C3 C4 C5 . . . . -1.0(11) ?
C3 C4 C5 C6 . . . . 0.1(11) ?
C4 C5 C6 C1 . . . . 1.1(11) ?
C4 C5 C6 C7 . . . . -177.6(7) ?
C5 C6 C7 N1 . . . . -158.0(7) ?
C5 C6 C7 N3 . . . . 20.4(11) ?
C6 C1 C2 C3 . . . . 0.5(11) ?
C7 N1 C8 N2 . . . . -0.6(8) ?
C7 N1 C8 C10 . . . . -178.8(6) ?
C8 N1 C7 N3 . . . . -0.9(8) ?
C8 N1 C7 C6 . . . . 177.8(7) ?
C8 N2 N3 C7 . . . . -2.3(8) ?