#------------------------------------------------------------------------------
#$Date: 2024-07-09 05:05:59 +0300 (Tue, 09 Jul 2024) $
#$Revision: 293328 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/31/2023187.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_2023187
loop_
_publ_author_name
'Rangarajan, Shalini'
'Sheokand, Sonu'
'Blair, Victoria L.'
'Deacon, Glen B.'
'Balakrishna, Maravanji S.'
_publ_section_title
;
Synthesis, structural studies and Hirshfeld surface analysis of
2-[(4-phenyl-1H-1,2,3-triazol-1-yl)methyl]pyridin-1-ium
hexakis(nitrato-\k2 O,O′)thorate(IV)
;
_journal_coeditor_code JW2006
_journal_issue 8
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_paper_doi 10.1107/S2056989024006352
_journal_volume 80
_journal_year 2024
_chemical_formula_iupac '(C14 H13 N4)2 [Th (N O3)6]'
_chemical_formula_moiety '2(C14 H13 N4 +), N6 O18 Th 2-'
_chemical_formula_sum 'C28 H26 N14 O18 Th'
_chemical_formula_weight 1078.67
_chemical_name_systematic
;
2-[(4-Phenyl-1H-1,2,3-triazol-1-yl)methyl]pyridin-1-ium
hexakis(nitrato-\k^2^O,O')thorate(IV)
;
_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 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 117.8460(10)
_cell_angle_gamma 90
_cell_formula_units_Z 2
_cell_length_a 14.5386(3)
_cell_length_b 9.3464(2)
_cell_length_c 15.4213(4)
_cell_measurement_reflns_used 9957
_cell_measurement_temperature 150.00
_cell_measurement_theta_max 28.45
_cell_measurement_theta_min 3.85
_cell_volume 1852.86(8)
_computing_cell_refinement
;
SAINT V8.40A (Bruker, 2019)
;
_computing_data_collection
;
APEX4 (Bruker, 2019)
;
_computing_data_reduction
;
SAINT V8.40A (Bruker, 2019)
;
_computing_molecular_graphics
;
Olex2 1.5 (Dolomanov et al., 2009)
;
_computing_publication_material
;
Olex2 1.5 (Dolomanov et al., 2009)
;
_computing_structure_refinement
;
SHELXL2019/3 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2014/5 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 150.00
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type 'Bruker APEXII CCD'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0231
_diffrn_reflns_av_unetI/netI 0.0158
_diffrn_reflns_limit_h_max 19
_diffrn_reflns_limit_h_min -19
_diffrn_reflns_limit_k_max 12
_diffrn_reflns_limit_k_min -12
_diffrn_reflns_limit_l_max 20
_diffrn_reflns_limit_l_min -20
_diffrn_reflns_number 27737
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 28.569
_diffrn_reflns_theta_min 2.698
_exptl_absorpt_coefficient_mu 4.123
_exptl_absorpt_correction_T_max 0.7457
_exptl_absorpt_correction_T_min 0.5124
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause et al., 2015)
;
_exptl_crystal_colour yellow
_exptl_crystal_density_diffrn 1.933
_exptl_crystal_description block
_exptl_crystal_F_000 1052
_exptl_crystal_size_max 0.094
_exptl_crystal_size_mid 0.072
_exptl_crystal_size_min 0.056
_refine_diff_density_max 0.724
_refine_diff_density_min -0.327
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.048
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 281
_refine_ls_number_reflns 4658
_refine_ls_number_restraints 1
_refine_ls_restrained_S_all 1.048
_refine_ls_R_factor_all 0.0197
_refine_ls_R_factor_gt 0.0147
_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^)+(0.0109P)^2^+1.5954P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0327
_refine_ls_wR_factor_ref 0.0346
_reflns_number_gt 3944
_reflns_number_total 4658
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file jw2006.cif
_cod_data_source_block I
_cod_original_cell_volume 1852.85(7)
_cod_database_code 2023187
_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 0.698
_shelx_estimated_absorpt_t_max 0.802
_shelx_hkl_file
;
-3 0 0 0.30 1.10
3 0 0 0.60 1.00
3 0 0 1.20 1.30
-3 0 0 0.20 0.90
-3 0 0 -1.20 0.90
-5 0 0 4.00 2.00
5 0 0 1.40 1.80
-5 0 0 0.30 1.70
5 0 0 0.60 2.10
-5 0 0 0.60 1.50
6 0 0 7622.64 179.38
-6 0 0 7513.15 178.18
-6 0 0 7718.93 179.08
-7 0 0 1.90 2.20
-7 0 0 0.50 1.80
7 0 0 0.90 2.90
7 0 0 4.40 2.50
-7 0 0 2.90 2.40
-8 0 0 2611.64 67.89
-8 0 0 2616.54 67.19
-8 0 0 2651.83 66.29
8 0 0 2840.12 67.89
8 0 0 2675.03 68.79
-8 0 0 2644.94 67.09
9 0 0 6.10 3.90
-9 0 0 -1.00 2.90
-9 0 0 0.30 2.80
-9 0 0 -0.20 3.30
-9 0 0 -1.40 2.00
9 0 0 1.00 2.70
-10 0 0 2615.54 67.59
-10 0 0 2614.74 66.29
10 0 0 2556.74 69.59
-10 0 0 2644.84 67.79
10 0 0 2652.33 68.19
-10 0 0 2608.54 68.59
-11 0 0 4.90 4.50
11 0 0 9.60 4.70
-11 0 0 6.30 4.40
11 0 0 1.10 5.00
-11 0 0 4.40 3.80
-11 0 0 0.90 2.90
-12 0 0 3552.34 93.89
-12 0 0 3563.64 92.69
-12 0 0 3808.52 93.39
12 0 0 3701.03 95.99
-12 0 0 3573.54 91.19
12 0 0 3652.03 93.59
-13 0 0 0.40 4.00
-13 0 0 1.30 4.80
13 0 0 -2.80 5.60
13 0 0 7.80 5.10
14 0 0 460.35 23.30
-14 0 0 484.35 21.20
-14 0 0 464.45 20.90
15 0 0 -3.30 7.30
-15 0 0 -3.20 5.40
-15 0 0 -1.70 5.30
-16 0 0 1140.09 38.60
-16 0 0 1128.39 38.70
16 0 0 1066.49 41.70
17 0 0 -13.00 7.40
-17 0 0 6.90 7.40
-17 0 0 -6.90 6.40
0 -1 0 -0.10 0.30
0 1 0 0.40 0.30
-2 -1 0 99.79 3.80
2 -1 0 110.49 4.20
-2 -1 0 106.09 4.10
2 -1 0 105.99 3.80
-2 -1 0 107.39 4.00
2 -1 0 102.29 3.70
2 1 0 108.49 4.20
-2 1 0 102.39 3.80
-2 1 0 108.99 4.20
-2 1 0 109.19 3.70
2 1 0 104.59 3.90
-3 -1 0 4589.44 104.89
3 -1 0 4563.44 105.29
-3 -1 0 4452.95 105.19
-3 1 0 4274.17 104.99
3 1 0 4490.55 104.89
3 1 0 4582.64 105.39
-4 -1 0 650.43 17.80
-4 -1 0 660.43 18.30
4 -1 0 649.54 17.90
4 -1 0 652.33 18.70
-4 -1 0 673.23 18.70
4 1 0 686.83 18.40
-4 1 0 673.13 18.60
4 1 0 647.14 18.80
-4 1 0 663.83 18.10
-4 1 0 647.74 17.90
-5 -1 0 5973.70 143.09
5 -1 0 6165.48 142.79
-5 -1 0 5949.60 142.59
-5 -1 0 6313.47 143.79
5 -1 0 5972.00 143.79
5 1 0 6265.57 144.09
-5 1 0 6153.28 143.59
5 1 0 6187.88 143.29
-5 1 0 5949.10 142.69
6 -1 0 121.39 6.30
6 -1 0 126.59 6.60
6 -1 0 112.59 7.30
-6 -1 0 129.29 6.90
-6 -1 0 117.69 7.00
-6 1 0 110.39 6.80
-6 1 0 123.59 6.60
6 1 0 121.89 7.50
6 1 0 114.69 6.70
-6 1 0 114.99 6.30
-7 -1 0 2448.26 62.99
7 -1 0 2564.94 62.49
-7 -1 0 2460.15 61.69
-7 -1 0 2521.75 62.29
-7 -1 0 2464.65 62.39
7 -1 0 2492.75 65.69
7 -1 0 2517.45 62.09
7 1 0 2570.84 62.79
-7 1 0 2513.65 62.99
-7 1 0 2518.35 62.29
-7 1 0 2379.66 61.89
7 1 0 2427.16 63.49
8 -1 0 7.50 4.00
-8 -1 0 5.60 3.20
-8 -1 0 2.80 2.40
-8 -1 0 4.70 3.00
-8 -1 0 12.10 3.30
8 -1 0 1.40 2.60
-8 1 0 4.10 3.40
-8 1 0 7.30 3.20
8 1 0 3.20 3.40
-8 1 0 2.30 2.70
-8 1 0 0.80 2.10
8 1 0 3.00 2.50
-9 -1 0 3532.65 85.19
-9 -1 0 3468.95 84.19
-9 -1 0 3288.57 84.79
9 -1 0 3390.26 86.79
9 -1 0 3437.16 85.19
-9 -1 0 3378.26 85.89
9 1 0 3408.76 86.99
9 1 0 3439.36 85.49
-9 1 0 3434.56 83.59
-9 1 0 3388.26 84.79
-9 1 0 3432.66 85.89
-9 1 0 3327.27 87.69
10 -1 0 125.09 10.30
-10 -1 0 120.09 8.10
10 -1 0 138.19 9.50
-10 -1 0 114.99 9.00
-10 -1 0 128.39 9.10
-10 -1 0 109.89 9.20
10 1 0 110.59 10.20
-10 1 0 118.79 9.30
-10 1 0 117.09 7.80
-10 1 0 116.29 8.80
-10 1 0 124.39 9.10
10 1 0 135.89 9.40
11 -1 0 933.71 32.00
-11 -1 0 942.31 31.10
11 -1 0 953.30 30.30
-11 -1 0 956.60 30.20
-11 -1 0 946.81 30.00
-11 -1 0 916.41 28.70
-11 1 0 1003.60 40.00
-11 1 0 887.61 28.00
-11 1 0 931.21 30.00
11 1 0 971.70 30.90
-11 1 0 968.10 30.10
11 1 0 943.01 32.00
12 -1 0 -3.60 5.10
-12 -1 0 0.60 4.30
12 -1 0 2.60 4.10
-12 -1 0 5.50 3.50
-12 -1 0 7.50 8.60
-12 -1 0 2.30 4.30
-12 1 0 1.00 4.10
-12 1 0 5.40 4.50
-12 1 0 0.90 3.20
-12 1 0 -5.90 3.90
12 1 0 -3.50 4.00
12 1 0 1.20 4.70
-13 -1 0 1901.31 53.29
13 -1 0 1855.21 55.69
-13 -1 0 1811.72 53.69
-13 1 0 1871.01 52.99
-13 1 0 1900.51 53.09
13 1 0 1859.41 53.59
-13 1 0 1793.22 50.49
13 1 0 1821.22 55.79
-14 -1 0 -4.10 5.30
14 -1 0 -6.90 4.40
-14 -1 0 3.80 4.90
14 -1 0 5.00 6.60
-14 1 0 -7.70 4.70
-14 1 0 -0.20 4.60
14 1 0 -2.00 7.10
15 -1 0 476.05 25.10
-15 -1 0 531.55 23.20
-15 -1 0 483.35 22.80
-15 1 0 542.95 23.60
-15 1 0 525.45 23.40
15 1 0 501.15 25.10
16 -1 0 4.40 7.80
-16 -1 0 6.00 6.90
-16 -1 0 -6.30 5.40
-16 1 0 6.20 6.50
16 1 0 -0.40 6.90
-16 1 0 2.70 6.50
17 -1 0 1126.49 44.10
-17 -1 0 1132.59 40.50
-17 -1 0 1180.48 40.50
-17 1 0 1141.09 40.40
17 1 0 1161.78 44.40
-17 1 0 1190.98 40.60
1 -2 0 122.39 4.30
-1 -2 0 131.79 4.50
-1 -2 0 124.39 4.30
-1 -2 0 134.19 4.60
1 -2 0 128.59 3.90
-1 2 0 130.59 3.80
1 2 0 128.69 4.30
-1 2 0 123.19 4.50
2 -2 0 1791.02 45.00
-2 -2 0 1905.01 45.40
-2 -2 0 1929.81 45.10
-2 -2 0 1859.41 45.20
2 -2 0 1878.21 44.50
2 -2 0 1886.11 44.90
-2 2 0 1935.71 45.00
2 2 0 1983.70 45.70
-2 2 0 1914.71 44.10
2 2 0 1846.12 45.10
-2 2 0 1811.62 45.30
3 -2 0 308.27 9.30
-3 -2 0 314.57 10.00
3 -2 0 306.37 9.80
-3 -2 0 289.07 9.60
-3 -2 0 303.07 9.50
3 -2 0 309.67 9.40
3 2 0 331.67 10.40
-3 2 0 307.97 9.90
-3 2 0 311.47 8.80
-3 2 0 301.77 9.40
3 2 0 311.17 9.80
4 -2 0 2586.74 61.79
-4 -2 0 2527.55 62.09
-4 -2 0 2546.45 61.79
4 -2 0 2693.63 61.79
4 -2 0 2576.14 62.59
-4 -2 0 2499.65 62.49
-4 2 0 2593.14 61.19
4 2 0 2555.54 62.19
4 2 0 2634.94 62.99
-4 2 0 2510.15 62.29
-4 2 0 2544.55 61.79
5 -2 0 6.80 2.00
5 -2 0 2.80 1.70
-5 -2 0 5.00 2.40
-5 -2 0 5.00 1.80
-5 -2 0 6.60 2.30
5 -2 0 7.40 2.80
-5 2 0 3.70 2.30
-5 2 0 4.50 1.90
-5 2 0 7.40 2.10
5 2 0 3.70 2.10
5 2 0 5.60 2.40
-6 -2 0 2376.26 60.79
-6 -2 0 2329.47 60.19
6 -2 0 2540.85 59.89
6 -2 0 2402.16 61.09
6 -2 0 2372.26 59.89
-6 -2 0 2380.26 59.69
-6 2 0 2379.66 59.89
6 2 0 2426.96 60.49
-6 2 0 2469.25 60.79
-6 2 0 2473.25 59.59
6 2 0 2489.25 61.59
7 -2 0 443.16 15.30
-7 -2 0 448.76 16.00
-7 -2 0 442.76 15.60
7 -2 0 439.16 15.00
7 -2 0 450.15 16.50
-7 -2 0 458.65 15.10
-7 2 0 472.05 16.10
7 2 0 440.26 15.60
7 2 0 438.16 16.70
-7 2 0 458.95 15.10
-7 2 0 459.95 15.50
-8 -2 0 796.52 24.60
-8 -2 0 801.42 23.90
8 -2 0 816.12 24.10
-8 -2 0 784.12 25.10
8 -2 0 819.02 25.90
8 -2 0 795.52 24.30
-8 2 0 804.42 24.90
8 2 0 792.32 25.90
-8 2 0 791.72 22.90
8 2 0 800.32 24.80
-8 2 0 765.52 24.10
-8 2 0 820.42 25.80
9 -2 0 153.48 8.80
9 -2 0 165.78 9.60
-9 -2 0 149.39 9.30
9 -2 0 152.28 10.50
-9 -2 0 150.58 9.50
-9 -2 0 158.58 9.40
-9 -2 0 155.68 8.70
-9 2 0 147.39 9.20
-9 2 0 140.29 9.50
-9 2 0 158.48 8.10
9 2 0 162.88 9.70
-9 2 0 135.59 8.70
9 2 0 150.98 10.80
-10 -2 0 1088.49 31.70
-10 -2 0 1029.10 33.10
10 -2 0 1119.29 32.70
-10 -2 0 1115.69 32.60
-10 -2 0 1031.90 32.40
10 -2 0 1049.59 34.00
-10 2 0 1106.69 32.50
10 2 0 1091.29 34.80
-10 2 0 1060.59 30.40
-10 2 0 1069.19 33.10
-10 2 0 1030.60 31.70
10 2 0 1113.09 33.20
-11 -2 0 190.58 11.90
-11 -2 0 188.98 11.60
11 -2 0 196.48 13.00
-11 -2 0 196.08 10.80
-11 -2 0 194.58 12.00
11 -2 0 180.88 11.60
11 2 0 174.68 15.50
-11 2 0 181.48 11.10
-11 2 0 171.48 11.20
11 2 0 167.98 13.10
-11 2 0 182.78 9.80
-11 2 0 183.28 11.90
-12 -2 0 1600.64 47.30
12 -2 0 1627.54 47.60
-12 -2 0 1726.03 47.80
12 -2 0 1683.23 50.09
-12 -2 0 1609.84 48.40
-12 2 0 1661.23 47.20
-12 2 0 1658.13 45.40
-12 2 0 1720.33 47.80
12 2 0 1633.44 50.09
12 2 0 1617.04 48.10
-13 -2 0 64.39 8.80
13 -2 0 66.79 10.50
-13 -2 0 56.49 9.10
13 -2 0 48.50 7.70
-13 -2 0 63.69 8.90
-13 2 0 55.19 8.20
-13 2 0 81.09 7.70
-13 2 0 64.69 8.30
13 2 0 80.09 11.90
-14 -2 0 510.15 22.20
14 -2 0 527.85 24.80
-14 -2 0 534.35 22.80
14 -2 0 524.75 22.60
-14 2 0 515.95 22.00
14 2 0 512.45 25.50
-14 2 0 538.95 22.60
-15 -2 0 4.70 6.40
-15 -2 0 0.30 5.50
15 -2 0 10.20 7.60
-15 2 0 8.80 6.20
-15 2 0 1.60 6.10
15 2 0 2.70 7.60
-16 -2 0 737.53 29.40
16 -2 0 715.53 32.10
-16 -2 0 733.03 29.60
-16 2 0 771.42 29.70
16 2 0 747.83 33.70
-16 2 0 737.53 29.10
-17 2 0 6.30 7.40
0 -3 0 0.70 0.80
0 3 0 0.00 0.80
-1 -3 0 1047.60 26.50
1 -3 0 1121.79 26.10
-1 -3 0 1129.79 26.80
-1 3 0 1013.70 26.80
1 3 0 1077.69 26.40
-1 3 0 1070.29 25.70
2 -3 0 27.20 2.70
2 -3 0 30.20 2.20
2 -3 0 26.20 2.60
-2 -3 0 27.50 2.80
-2 -3 0 22.90 2.50
-2 -3 0 29.60 2.50
-2 3 0 27.50 1.70
-2 3 0 31.00 3.00
2 3 0 29.40 3.00
3 -3 0 4515.25 111.09
-3 -3 0 4849.41 111.19
3 -3 0 4757.72 110.99
-3 -3 0 4815.42 111.79
-3 -3 0 4652.43 111.39
3 -3 0 4711.23 110.49
3 3 0 4924.31 112.19
-3 3 0 4753.12 110.99
-3 3 0 4629.94 111.59
-3 3 0 4927.11 109.59
3 3 0 4620.04 111.29
4 -3 0 35.90 3.70
4 -3 0 38.80 3.60
-4 -3 0 51.69 4.30
4 -3 0 48.60 3.70
-4 -3 0 44.60 3.70
-4 -3 0 41.90 4.00
-4 3 0 44.80 4.10
4 3 0 41.30 4.40
4 3 0 49.00 4.10
-4 3 0 43.90 3.80
-4 3 0 43.60 2.90
-5 -3 0 4045.70 96.79
5 -3 0 4098.79 95.69
5 -3 0 4031.50 96.49
-5 -3 0 3947.51 96.29
-5 -3 0 3830.72 95.89
5 -3 0 3985.40 95.69
-5 3 0 3977.00 96.49
-5 3 0 4032.00 94.39
-5 3 0 4036.00 95.79
5 3 0 4028.10 96.39
5 3 0 4172.18 97.59
6 -3 0 59.79 4.60
-6 -3 0 43.70 5.00
6 -3 0 60.39 5.60
6 -3 0 53.19 4.80
-6 -3 0 63.29 4.90
-6 -3 0 58.39 5.40
6 3 0 52.59 4.80
-6 3 0 48.60 4.10
-6 3 0 43.60 4.50
-6 3 0 56.69 5.20
6 3 0 51.59 5.80
7 -3 0 1654.73 43.40
-7 -3 0 1657.43 43.40
-7 -3 0 1708.23 44.80
7 -3 0 1670.43 43.30
-7 -3 0 1672.63 44.10
7 -3 0 1655.23 44.70
-7 3 0 1589.14 43.30
7 3 0 1677.63 44.20
7 3 0 1645.64 45.30
-7 3 0 1667.03 44.30
-7 3 0 1660.03 42.30
-8 -3 0 32.40 5.20
-8 -3 0 24.10 4.00
8 -3 0 33.40 5.70
8 -3 0 40.90 5.00
-8 -3 0 33.70 5.50
8 -3 0 36.60 5.00
-8 3 0 28.90 4.10
-8 3 0 34.70 4.00
8 3 0 35.40 5.40
-8 3 0 26.20 4.90
-8 3 0 28.30 4.60
8 3 0 29.70 5.80
9 -3 0 2450.25 62.79
9 -3 0 2522.85 63.29
-9 -3 0 2445.86 62.69
9 -3 0 2446.56 64.79
-9 -3 0 2428.66 63.59
-9 -3 0 2449.16 64.39
-9 3 0 2465.95 61.89
-9 3 0 2499.25 60.99
-9 3 0 2470.35 63.89
9 3 0 2303.17 68.19
-9 3 0 2438.86 63.09
9 3 0 2387.26 63.69
10 -3 0 9.40 3.70
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11 -1 -9 36.10 4.80
11 -1 -9 46.20 5.90
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11 1 -9 49.70 5.70
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10 -1 -9 770.12 23.40
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10 1 -9 759.52 23.60
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9 1 -9 2.50 3.20
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4 1 -9 2645.04 67.39
4 1 -9 2654.23 67.89
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3 -1 -9 0.60 2.10
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3 1 -9 0.90 2.40
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1 -1 -9 38.10 5.00
1 -1 -9 49.00 6.40
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19 -2 -9 577.54 27.10
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18 -2 -9 8.40 6.90
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13 -2 -9 1557.44 41.60
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12 -2 -9 35.20 4.90
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3 -2 -9 496.25 16.60
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11 -3 -9 9.50 3.60
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1 -3 -9 6.30 2.80
1 -3 -9 8.40 3.30
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1 -3 -9 5.90 2.90
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6 2 -19 26.60 10.20
5 -2 -19 414.26 23.90
5 -2 -19 428.66 20.90
5 2 -19 499.35 27.10
5 2 -19 463.85 22.70
4 -2 -19 -4.50 6.10
4 -2 -19 -1.00 9.10
4 2 -19 -18.40 6.60
4 2 -19 -13.90 10.70
3 -2 -19 343.97 19.80
3 2 -19 332.67 20.00
13 -3 -19 7.90 5.90
-13 -3 19 2.10 7.70
13 -3 -19 4.40 5.10
13 3 -19 9.90 8.60
13 3 -19 12.70 9.00
12 -3 -19 537.65 20.50
12 -3 -19 529.15 21.30
-12 -3 19 479.15 24.10
12 -3 -19 535.05 21.40
12 3 -19 516.45 28.90
11 -3 -19 2.00 6.80
11 -3 -19 -1.50 4.60
11 -3 -19 5.80 5.80
11 3 -19 6.00 7.80
11 3 -19 -3.70 5.70
-11 3 19 -7.50 3.30
10 -3 -19 429.16 19.00
10 -3 -19 437.66 25.00
10 -3 -19 403.16 17.80
10 3 -19 428.06 21.90
10 3 -19 399.86 22.40
9 -3 -19 18.60 6.50
9 -3 -19 18.50 7.90
9 3 -19 15.60 8.40
9 3 -19 7.80 6.40
8 -3 -19 566.84 25.10
8 -3 -19 568.24 22.60
8 3 -19 552.74 26.70
8 3 -19 543.85 25.20
7 -3 -19 -0.10 5.80
7 -3 -19 1.60 7.90
7 3 -19 0.80 9.00
7 3 -19 0.90 6.30
6 -3 -19 329.37 17.90
6 -3 -19 345.07 20.00
6 3 -19 361.16 24.40
6 3 -19 361.06 22.90
5 -3 -19 -2.90 5.90
5 -3 -19 -1.20 7.70
5 3 -19 9.60 11.10
5 3 -19 -0.70 8.30
4 -3 -19 433.46 23.80
4 -3 -19 443.46 21.40
4 3 -19 449.95 23.50
-12 -4 19 22.20 8.50
12 -4 -19 22.50 6.70
12 -4 -19 30.50 5.20
12 4 -19 19.20 10.00
12 4 -19 12.90 7.60
11 -4 -19 315.87 13.50
11 -4 -19 268.37 14.90
11 4 -19 265.47 18.30
10 -4 -19 -7.10 6.30
10 -4 -19 1.80 4.40
10 4 -19 3.60 7.10
9 -4 -19 496.65 21.10
9 -4 -19 514.75 21.00
9 4 -19 506.35 28.10
9 4 -19 500.05 25.70
8 -4 -19 1.60 5.50
8 -4 -19 7.60 7.20
8 4 -19 -4.70 6.40
8 4 -19 -3.90 9.60
7 -4 -19 284.57 16.40
7 -4 -19 300.37 18.90
7 4 -19 324.07 25.70
7 4 -19 312.77 19.80
6 -4 -19 27.50 8.50
6 -4 -19 31.80 7.70
6 4 -19 18.60 7.60
5 -4 -19 528.55 22.90
5 -4 -19 508.55 24.20
5 4 -19 537.95 25.80
-13 0 20 2.30 4.40
13 0 -20 3.00 7.10
13 0 -20 5.80 6.80
12 0 -20 183.78 15.20
12 0 -20 203.08 15.20
11 0 -20 -2.00 5.90
11 0 -20 2.60 7.00
-11 0 20 0.20 5.90
10 0 -20 389.36 20.70
10 0 -20 408.26 20.60
9 0 -20 -5.30 5.40
9 0 -20 -5.60 7.90
8 0 -20 148.49 13.80
8 0 -20 144.19 14.90
7 0 -20 -1.90 6.50
7 0 -20 -7.80 9.90
6 0 -20 301.27 18.60
5 0 -20 -0.30 6.90
12 -1 -20 11.30 7.00
12 -1 -20 6.90 6.10
-12 -1 20 3.60 6.00
12 -1 -20 -1.80 6.20
12 1 -20 8.40 7.70
-12 1 20 -1.00 4.70
12 1 -20 -0.80 5.60
11 -1 -20 371.96 19.20
11 -1 -20 333.67 19.00
11 -1 -20 388.06 19.50
11 1 -20 369.86 20.30
10 -1 -20 16.00 7.90
10 -1 -20 -4.10 5.80
-10 -1 20 -7.60 6.30
10 1 -20 -0.50 6.30
10 1 -20 11.30 13.40
9 -1 -20 427.56 21.20
-9 -1 20 453.75 17.00
9 -1 -20 453.45 23.20
9 1 -20 480.75 22.90
9 1 -20 462.15 27.60
8 -1 -20 3.70 6.10
-8 -1 20 -3.30 4.70
8 -1 -20 -4.50 8.60
8 1 -20 5.10 13.60
8 1 -20 -2.10 5.90
7 -1 -20 346.57 18.70
-7 -1 20 306.07 16.40
7 -1 -20 334.07 21.80
7 1 -20 301.37 19.00
6 -1 -20 21.10 7.80
-6 -1 20 5.90 6.20
6 1 -20 33.80 10.60
5 -1 -20 394.66 21.00
5 1 -20 385.16 22.50
12 -2 -20 426.46 20.50
12 -2 -20 425.46 19.90
12 -2 -20 437.16 20.70
-12 -2 20 420.06 21.90
12 2 -20 425.66 23.80
11 -2 -20 -12.00 5.20
11 -2 -20 -6.40 5.70
11 -2 -20 16.30 8.50
-11 2 20 -4.70 4.00
10 -2 -20 676.73 26.40
-10 -2 20 680.13 23.50
10 -2 -20 685.43 28.00
10 2 -20 674.63 30.20
9 -2 -20 46.50 10.10
9 -2 -20 47.20 8.70
9 2 -20 19.50 9.50
8 -2 -20 463.45 21.80
8 -2 -20 498.85 25.10
7 -2 -20 23.70 9.90
7 -2 -20 0.00 6.30
7 2 -20 11.00 8.40
6 -2 -20 309.57 18.30
6 2 -20 319.87 19.90
9 -3 -20 538.25 22.80
9 -3 -20 549.05 25.20
9 3 -20 544.35 25.80
8 -3 -20 -1.70 5.80
8 -3 -20 -22.60 8.10
8 3 -20 -4.70 6.50
0 0 0 0.00 0.00
_computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)'
;
_shelx_hkl_checksum 19730
_shelx_res_file
;
TITL MSB_SR_492_0m_a.res in P2(1)/n
comp_1.res
created by SHELXL-2019/3 at 22:08:35 on 10-Mar-2024
CELL 0.71073 14.5386 9.3464 15.4213 90 117.846 90
ZERR 2 0.0003 0.0002 0.0004 0 0.001 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC C H N O Th
UNIT 56 52 28 36 2
DFIX 0.89 N4 H4
L.S. 30
PLAN 5 0 0
SIZE 0.056 0.072 0.094
TEMP -123.15
CONF
MORE -1
BOND $H
fmap 2
acta
OMIT -16 6 2
REM
REM
REM
WGHT 0.010900 1.595400
FVAR 0.43807
TH1 5 0.500000 0.500000 0.500000 10.50000 0.01291 0.01679 =
0.01779 -0.00091 0.00818 0.00037
O3 4 0.535420 0.859628 0.352236 11.00000 0.03970 0.03229 =
0.03970 0.01307 0.02062 -0.00271
O8 4 0.827012 0.472158 0.649694 11.00000 0.01410 0.05792 =
0.04145 -0.01430 0.00806 0.00311
O7 4 0.681224 0.546500 0.639855 11.00000 0.01938 0.02589 =
0.02587 -0.00214 0.01169 0.00101
O4 4 0.502787 0.541608 0.665178 11.00000 0.02562 0.02762 =
0.02732 -0.00201 0.01511 -0.00114
O9 4 0.678963 0.408350 0.526777 11.00000 0.02041 0.02824 =
0.02542 -0.00406 0.01085 0.00011
O1 4 0.604495 0.689886 0.461030 11.00000 0.02022 0.02707 =
0.02801 0.00124 0.01103 -0.00040
O2 4 0.437503 0.717239 0.385572 11.00000 0.01976 0.02627 =
0.02904 0.00059 0.01160 0.00024
O5 4 0.509414 0.733361 0.590046 11.00000 0.02535 0.02489 =
0.02820 -0.00189 0.01358 0.00020
N5 3 0.732676 0.475761 0.606833 11.00000 0.01684 0.02584 =
0.02487 -0.00130 0.01005 0.00073
N3 3 0.626349 0.658441 1.027260 11.00000 0.01959 0.02497 =
0.02169 -0.00099 0.01126 -0.00161
N4 3 0.668155 0.409686 0.930129 11.00000 0.01887 0.02248 =
0.02601 0.00538 0.01105 -0.00096
N1 3 0.480111 0.691910 1.023565 11.00000 0.02333 0.02003 =
0.02740 -0.00300 0.01504 -0.00437
N2 3 0.565537 0.615127 1.066243 11.00000 0.02437 0.02300 =
0.02721 -0.00208 0.01494 -0.00398
C9 1 0.403841 0.887849 0.899611 11.00000 0.02093 0.02031 =
0.02108 -0.00587 0.01109 -0.00291
N6 3 0.526281 0.759630 0.397677 11.00000 0.02371 0.02196 =
0.02361 -0.00010 0.01258 -0.00125
N7 3 0.503926 0.678636 0.663424 11.00000 0.02698 0.02954 =
0.02711 -0.00731 0.01415 -0.00178
C10 1 0.421923 0.993176 0.845489 11.00000 0.02241 0.02669 =
0.02503 -0.00423 0.01254 -0.00369
AFIX 43
H10 2 0.487167 0.996946 0.845381 11.00000 -1.20000
AFIX 0
O6 4 0.497166 0.750149 0.725312 11.00000 0.08974 0.04461 =
0.04502 -0.02082 0.04387 -0.00584
C2 1 0.580954 0.762984 0.960643 11.00000 0.02321 0.02568 =
0.02292 0.00019 0.01364 -0.00219
AFIX 43
H2 2 0.608517 0.811145 0.923638 11.00000 -1.20000
AFIX 0
C1 1 0.485973 0.784974 0.957763 11.00000 0.02133 0.01893 =
0.02154 -0.00548 0.01210 -0.00524
C3 1 0.728246 0.592703 1.058978 11.00000 0.01989 0.03474 =
0.02389 0.00106 0.00902 0.00247
AFIX 23
H3A 2 0.741548 0.523286 1.112040 11.00000 -1.20000
H3B 2 0.782565 0.667624 1.085923 11.00000 -1.20000
AFIX 0
C11 1 0.345506 1.092676 0.791716 11.00000 0.03007 0.02743 =
0.02213 -0.00055 0.01198 -0.00163
AFIX 43
H11 2 0.359140 1.165092 0.756012 11.00000 -1.20000
AFIX 0
C14 1 0.306615 0.883542 0.897729 11.00000 0.02602 0.02955 =
0.03267 0.00215 0.01927 0.00074
AFIX 43
H14 2 0.293076 0.812659 0.934452 11.00000 -1.20000
AFIX 0
C4 1 0.670306 0.334187 0.857247 11.00000 0.02295 0.02010 =
0.02800 0.00129 0.00818 -0.00127
AFIX 43
H4A 2 0.620849 0.260215 0.826229 11.00000 -1.20000
AFIX 0
C8 1 0.735788 0.516954 0.976260 11.00000 0.01821 0.02068 =
0.02122 0.00454 0.00779 0.00260
C5 1 0.743628 0.363102 0.827083 11.00000 0.02723 0.02322 =
0.02389 0.00430 0.01186 0.00511
AFIX 43
H5 2 0.746028 0.308832 0.776090 11.00000 -1.20000
AFIX 0
C6 1 0.813632 0.472341 0.872209 11.00000 0.02327 0.02710 =
0.03127 0.00598 0.01620 0.00333
AFIX 43
H6 2 0.864548 0.494561 0.852061 11.00000 -1.20000
AFIX 0
C7 1 0.809554 0.549866 0.947224 11.00000 0.02006 0.02107 =
0.03086 0.00176 0.01229 -0.00150
AFIX 43
H7 2 0.857548 0.625368 0.978375 11.00000 -1.20000
AFIX 0
C12 1 0.249314 1.086769 0.789914 11.00000 0.02905 0.03241 =
0.02423 -0.00039 0.01124 0.00650
AFIX 43
H12 2 0.196841 1.154400 0.752611 11.00000 -1.20000
AFIX 0
C13 1 0.230141 0.981631 0.842848 11.00000 0.02589 0.03830 =
0.03625 0.00056 0.01899 0.00458
AFIX 43
H13 2 0.164176 0.976926 0.841424 11.00000 -1.20000
AFIX 0
H4 2 0.624024 0.384993 0.950069 11.00000 0.04333
HKLF 4
REM MSB_SR_492_0m_a.res in P2(1)/n
REM wR2 = 0.0346, GooF = S = 1.048, Restrained GooF = 1.048 for all data
REM R1 = 0.0147 for 3944 Fo > 4sig(Fo) and 0.0197 for all 4658 data
REM 281 parameters refined using 1 restraints
END
WGHT 0.0109 1.5955
REM Highest difference peak 0.724, deepest hole -0.327, 1-sigma level 0.064
Q1 1 0.6044 0.4972 0.6004 11.00000 0.05 0.72
Q2 1 0.4260 0.6493 0.5882 11.00000 0.05 0.52
Q3 1 0.5024 0.7687 0.4682 11.00000 0.05 0.49
Q4 1 0.5996 0.6252 0.6721 11.00000 0.05 0.48
Q5 1 0.5007 0.6373 0.3517 11.00000 0.05 0.47
;
_shelx_res_checksum 57791
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
Th Th1 0.500000 0.500000 0.500000 0.01543(3) Uani d 1 . .
O O3 0.53542(12) 0.85963(17) 0.35224(11) 0.0364(3) Uani d 1 . .
O O8 0.82701(10) 0.47216(19) 0.64969(12) 0.0398(4) Uani d 1 . .
O O7 0.68122(10) 0.54650(15) 0.63986(10) 0.0233(3) Uani d 1 . .
O O4 0.50279(10) 0.54161(15) 0.66518(10) 0.0258(3) Uani d 1 . .
O O9 0.67896(10) 0.40835(15) 0.52678(10) 0.0246(3) Uani d 1 . .
O O1 0.60450(10) 0.68989(15) 0.46103(10) 0.0252(3) Uani d 1 . .
O O2 0.43750(10) 0.71724(15) 0.38557(10) 0.0249(3) Uani d 1 . .
O O5 0.50941(10) 0.73336(15) 0.59005(10) 0.0257(3) Uani d 1 . .
N N5 0.73268(11) 0.47576(17) 0.60683(12) 0.0224(3) Uani d 1 . .
N N3 0.62635(11) 0.65844(17) 1.02726(11) 0.0214(3) Uani d 1 . .
N N4 0.66816(12) 0.40969(17) 0.93013(12) 0.0222(3) Uani d 1 . .
N N1 0.48011(12) 0.69191(17) 1.02356(12) 0.0223(3) Uani d 1 . .
N N2 0.56554(12) 0.61513(17) 1.06624(12) 0.0237(3) Uani d 1 . .
C C9 0.40384(13) 0.8878(2) 0.89961(13) 0.0203(4) Uani d 1 . .
N N6 0.52628(12) 0.75963(17) 0.39768(11) 0.0225(3) Uani d 1 . .
N N7 0.50393(13) 0.67864(19) 0.66342(12) 0.0273(4) Uani d 1 . .
C C10 0.42192(14) 0.9932(2) 0.84549(14) 0.0241(4) Uani d 1 . .
H H10 0.487167 0.996946 0.845381 0.029 Uiso calc 1 . .
O O6 0.49717(17) 0.7501(2) 0.72531(13) 0.0549(5) Uani d 1 . .
C C2 0.58095(14) 0.7630(2) 0.96064(13) 0.0228(4) Uani d 1 . .
H H2 0.608517 0.811145 0.923638 0.027 Uiso calc 1 . .
C C1 0.48597(13) 0.7850(2) 0.95776(13) 0.0198(3) Uani d 1 . .
C C3 0.72825(14) 0.5927(2) 1.05898(14) 0.0267(4) Uani d 1 . .
H H3A 0.741548 0.523286 1.112040 0.032 Uiso calc 1 . .
H H3B 0.782565 0.667624 1.085923 0.032 Uiso calc 1 . .
C C11 0.34551(15) 1.0927(2) 0.79172(14) 0.0266(4) Uani d 1 . .
H H11 0.359140 1.165092 0.756012 0.032 Uiso calc 1 . .
C C14 0.30661(15) 0.8835(2) 0.89773(15) 0.0272(4) Uani d 1 . .
H H14 0.293076 0.812659 0.934452 0.033 Uiso calc 1 . .
C C4 0.67031(14) 0.3342(2) 0.85725(14) 0.0252(4) Uani d 1 . .
H H4A 0.620849 0.260215 0.826229 0.030 Uiso calc 1 . .
C C8 0.73579(13) 0.51695(19) 0.97626(13) 0.0206(4) Uani d 1 . .
C C5 0.74363(14) 0.3631(2) 0.82708(14) 0.0248(4) Uani d 1 . .
H H5 0.746028 0.308832 0.776090 0.030 Uiso calc 1 . .
C C6 0.81363(15) 0.4723(2) 0.87221(15) 0.0258(4) Uani d 1 . .
H H6 0.864548 0.494561 0.852061 0.031 Uiso calc 1 . .
C C7 0.80955(14) 0.5499(2) 0.94722(15) 0.0238(4) Uani d 1 . .
H H7 0.857548 0.625368 0.978375 0.029 Uiso calc 1 . .
C C12 0.24931(16) 1.0868(2) 0.78991(14) 0.0290(4) Uani d 1 . .
H H12 0.196841 1.154400 0.752611 0.035 Uiso calc 1 . .
C C13 0.23014(16) 0.9816(2) 0.84285(16) 0.0317(5) Uani d 1 . .
H H13 0.164176 0.976926 0.841424 0.038 Uiso calc 1 . .
H H4 0.6240(17) 0.385(3) 0.9501(18) 0.043(7) Uiso d 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
Th1 0.01291(4) 0.01679(5) 0.01779(4) 0.00037(3) 0.00818(3) -0.00091(4)
O3 0.0397(8) 0.0323(8) 0.0397(8) -0.0027(7) 0.0206(7) 0.0131(7)
O8 0.0141(6) 0.0579(11) 0.0414(9) 0.0031(6) 0.0081(6) -0.0143(8)
O7 0.0194(6) 0.0259(6) 0.0259(7) 0.0010(5) 0.0117(5) -0.0021(6)
O4 0.0256(7) 0.0276(7) 0.0273(7) -0.0011(5) 0.0151(6) -0.0020(6)
O9 0.0204(6) 0.0282(7) 0.0254(7) 0.0001(5) 0.0109(5) -0.0041(6)
O1 0.0202(6) 0.0271(7) 0.0280(7) -0.0004(5) 0.0110(5) 0.0012(6)
O2 0.0198(6) 0.0263(7) 0.0290(7) 0.0002(5) 0.0116(5) 0.0006(6)
O5 0.0254(7) 0.0249(7) 0.0282(7) 0.0002(5) 0.0136(6) -0.0019(6)
N5 0.0168(7) 0.0258(9) 0.0249(8) 0.0007(6) 0.0100(6) -0.0013(6)
N3 0.0196(7) 0.0250(8) 0.0217(7) -0.0016(6) 0.0113(6) -0.0010(6)
N4 0.0189(7) 0.0225(8) 0.0260(8) -0.0010(6) 0.0110(6) 0.0054(6)
N1 0.0233(7) 0.0200(8) 0.0274(8) -0.0044(6) 0.0150(7) -0.0030(6)
N2 0.0244(8) 0.0230(8) 0.0272(8) -0.0040(6) 0.0149(7) -0.0021(7)
C9 0.0209(8) 0.0203(9) 0.0211(9) -0.0029(7) 0.0111(7) -0.0059(7)
N6 0.0237(7) 0.0220(8) 0.0236(8) -0.0012(6) 0.0126(6) -0.0001(6)
N7 0.0270(8) 0.0295(9) 0.0271(8) -0.0018(7) 0.0141(7) -0.0073(7)
C10 0.0224(8) 0.0267(9) 0.0250(9) -0.0037(8) 0.0125(7) -0.0042(8)
O6 0.0897(14) 0.0446(10) 0.0450(10) -0.0058(10) 0.0439(10) -0.0208(8)
C2 0.0232(8) 0.0257(10) 0.0229(9) -0.0022(7) 0.0136(7) 0.0002(7)
C1 0.0213(8) 0.0189(9) 0.0215(8) -0.0052(7) 0.0121(7) -0.0055(7)
C3 0.0199(8) 0.0347(11) 0.0239(9) 0.0025(8) 0.0090(7) 0.0011(8)
C11 0.0301(10) 0.0274(10) 0.0221(9) -0.0016(8) 0.0120(8) -0.0006(8)
C14 0.0260(9) 0.0295(10) 0.0327(10) 0.0007(8) 0.0193(8) 0.0022(8)
C4 0.0229(9) 0.0201(9) 0.0280(10) -0.0013(7) 0.0082(8) 0.0013(8)
C8 0.0182(8) 0.0207(9) 0.0212(8) 0.0026(7) 0.0078(7) 0.0045(7)
C5 0.0272(9) 0.0232(9) 0.0239(9) 0.0051(7) 0.0119(8) 0.0043(8)
C6 0.0233(9) 0.0271(10) 0.0313(10) 0.0033(7) 0.0162(8) 0.0060(8)
C7 0.0201(8) 0.0211(8) 0.0309(10) -0.0015(7) 0.0123(8) 0.0018(8)
C12 0.0291(10) 0.0324(11) 0.0242(9) 0.0065(8) 0.0112(8) -0.0004(8)
C13 0.0259(9) 0.0383(12) 0.0363(11) 0.0046(8) 0.0190(8) 0.0006(9)
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'
Th Th -7.2400 8.8979 '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
O7 Th1 O7 3_666 . 180.00(6) ?
O7 Th1 O4 . 3_666 113.48(4) yes
O7 Th1 O4 . . 66.52(4) yes
O7 Th1 O4 3_666 3_666 66.52(4) no
O7 Th1 O4 3_666 . 113.48(4) ?
O7 Th1 O9 3_666 . 130.23(4) yes
O7 Th1 O9 . 3_666 130.23(4) ?
O7 Th1 O9 3_666 3_666 49.77(4) no
O7 Th1 O9 . . 49.77(4) yes
O7 Th1 O1 3_666 3_666 65.87(4) yes
O7 Th1 O1 . 3_666 114.13(4) ?
O7 Th1 O1 3_666 . 114.13(4) ?
O7 Th1 O1 . . 65.87(4) ?
O7 Th1 O2 3_666 . 69.99(4) ?
O7 Th1 O2 . . 110.01(4) ?
O7 Th1 O2 . 3_666 69.99(4) yes
O7 Th1 O2 3_666 3_666 110.01(4) ?
O7 Th1 O5 . . 67.79(4) ?
O7 Th1 O5 . 3_666 112.20(4) ?
O7 Th1 O5 3_666 3_666 67.80(4) yes
O7 Th1 O5 3_666 . 112.21(4) ?
O4 Th1 O4 3_666 . 180.0 ?
O4 Th1 O9 3_666 3_666 110.18(4) yes
O4 Th1 O9 3_666 . 69.82(4) ?
O4 Th1 O9 . 3_666 69.82(4) ?
O4 Th1 O9 . . 110.18(4) ?
O4 Th1 O1 3_666 3_666 112.94(4) yes
O4 Th1 O1 . . 112.94(4) ?
O4 Th1 O1 3_666 . 67.06(4) ?
O4 Th1 O1 . 3_666 67.06(4) ?
O4 Th1 O2 . . 113.63(4) ?
O4 Th1 O2 3_666 3_666 113.64(4) yes
O4 Th1 O2 . 3_666 66.36(4) ?
O4 Th1 O2 3_666 . 66.37(4) ?
O9 Th1 O9 . 3_666 180.0 yes
O9 Th1 O1 . . 66.86(4) ?
O9 Th1 O1 3_666 . 113.14(4) ?
O9 Th1 O1 3_666 3_666 66.86(4) yes
O9 Th1 O1 . 3_666 113.14(4) ?
O1 Th1 O1 3_666 . 180.0 ?
O2 Th1 O9 . 3_666 67.69(4) ?
O2 Th1 O9 . . 112.31(4) ?
O2 Th1 O9 3_666 3_666 112.31(4) yes
O2 Th1 O9 3_666 . 67.69(4) ?
O2 Th1 O1 3_666 3_666 49.70(4) yes
O2 Th1 O1 3_666 . 130.30(4) yes
O2 Th1 O1 . . 49.70(4) yes
O2 Th1 O1 . 3_666 130.30(4) ?
O2 Th1 O2 . 3_666 180.0 ?
O5 Th1 O4 3_666 . 130.01(4) yes
O5 Th1 O4 . . 49.99(4) yes
O5 Th1 O4 3_666 3_666 49.99(4) no
O5 Th1 O4 . 3_666 130.01(4) ?
O5 Th1 O9 . 3_666 66.29(4) ?
O5 Th1 O9 3_666 . 66.29(4) yes
O5 Th1 O9 . . 113.71(4) ?
O5 Th1 O9 3_666 3_666 113.71(4) yes
O5 Th1 O1 3_666 3_666 69.63(4) yes
O5 Th1 O1 . 3_666 110.37(4) ?
O5 Th1 O1 3_666 . 110.37(4) ?
O5 Th1 O1 . . 69.63(4) ?
O5 Th1 O2 3_666 3_666 67.02(4) yes
O5 Th1 O2 . . 67.02(4) ?
O5 Th1 O2 . 3_666 112.98(4) ?
O5 Th1 O2 3_666 . 112.98(4) ?
O5 Th1 O5 . 3_666 180.0 ?
N5 O7 Th1 . . 98.16(10) ?
N7 O4 Th1 . . 97.20(11) ?
N5 O9 Th1 . . 96.11(9) ?
N6 O1 Th1 . . 96.79(10) ?
N6 O2 Th1 . . 97.82(10) ?
N7 O5 Th1 . . 97.47(11) ?
O8 N5 Th1 . . 177.24(14) ?
O8 N5 O7 . . 121.59(16) ?
O8 N5 O9 . . 122.56(16) ?
O7 N5 Th1 . . 57.08(8) ?
O7 N5 O9 . . 115.85(14) ?
O9 N5 Th1 . . 58.86(8) ?
N2 N3 C2 . . 111.70(15) ?
N2 N3 C3 . . 120.00(15) ?
C2 N3 C3 . . 128.30(16) ?
C4 N4 C8 . . 122.43(16) ?
C4 N4 H4 . . 118.1(18) ?
C8 N4 H4 . . 119.4(18) ?
N2 N1 C1 . . 110.29(15) ?
N1 N2 N3 . . 106.08(15) ?
C10 C9 C1 . . 120.12(16) ?
C10 C9 C14 . . 118.62(17) ?
C14 C9 C1 . . 121.26(17) ?
O3 N6 Th1 . . 176.58(13) ?
O3 N6 O1 . . 122.44(15) ?
O3 N6 O2 . . 122.05(16) ?
O1 N6 Th1 . . 58.30(8) ?
O2 N6 Th1 . . 57.35(9) ?
O2 N6 O1 . . 115.51(15) ?
O4 N7 Th1 . . 57.75(9) ?
O5 N7 Th1 . . 57.56(9) ?
O5 N7 O4 . . 115.19(15) ?
O6 N7 Th1 . . 174.91(15) ?
O6 N7 O4 . . 122.04(18) ?
O6 N7 O5 . . 122.74(18) ?
C9 C10 H10 . . 119.7 ?
C11 C10 C9 . . 120.61(17) ?
C11 C10 H10 . . 119.7 ?
N3 C2 H2 . . 127.5 ?
N3 C2 C1 . . 105.06(16) ?
C1 C2 H2 . . 127.5 ?
N1 C1 C9 . . 123.68(16) ?
N1 C1 C2 . . 106.87(16) ?
C2 C1 C9 . . 129.44(17) ?
N3 C3 H3A . . 109.2 ?
N3 C3 H3B . . 109.2 ?
N3 C3 C8 . . 112.18(15) ?
H3A C3 H3B . . 107.9 ?
C8 C3 H3A . . 109.2 ?
C8 C3 H3B . . 109.2 ?
C10 C11 H11 . . 119.9 ?
C12 C11 C10 . . 120.24(19) ?
C12 C11 H11 . . 119.9 ?
C9 C14 H14 . . 119.7 ?
C13 C14 C9 . . 120.56(19) ?
C13 C14 H14 . . 119.7 ?
N4 C4 H4A . . 119.8 ?
N4 C4 C5 . . 120.40(18) ?
C5 C4 H4A . . 119.8 ?
N4 C8 C3 . . 118.14(16) ?
N4 C8 C7 . . 118.73(17) ?
C7 C8 C3 . . 123.11(17) ?
C4 C5 H5 . . 120.6 ?
C4 C5 C6 . . 118.76(19) ?
C6 C5 H5 . . 120.6 ?
C5 C6 H6 . . 120.1 ?
C5 C6 C7 . . 119.86(18) ?
C7 C6 H6 . . 120.1 ?
C8 C7 C6 . . 119.81(18) ?
C8 C7 H7 . . 120.1 ?
C6 C7 H7 . . 120.1 ?
C11 C12 H12 . . 120.2 ?
C13 C12 C11 . . 119.64(19) ?
C13 C12 H12 . . 120.2 ?
C14 C13 C12 . . 120.31(18) ?
C14 C13 H13 . . 119.8 ?
C12 C13 H13 . . 119.8 ?
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
Th1 O1 . 2.5830(13) yes
Th1 O2 . 2.5621(14) yes
Th1 O4 3_666 2.5582(13) no
Th1 O4 . 2.5583(13) yes
Th1 O5 . 2.5547(14) yes
Th1 O7 3_666 2.5444(13) no
Th1 O7 . 2.5444(13) yes
Th1 O9 3_666 2.5827(12) no
Th1 O9 . 2.5827(12) yes
Th1 O1 3_666 2.5830(13) no
Th1 O2 3_666 2.5621(13) no
Th1 O5 3_666 2.5547(14) no
O3 N6 . 1.212(2) no
O8 N5 . 1.213(2) no
O7 N5 . 1.270(2) no
O4 N7 . 1.281(2) no
O9 N5 . 1.277(2) no
O1 N6 . 1.279(2) no
O2 N6 . 1.2778(19) no
O5 N7 . 1.278(2) no
N1 C1 . 1.369(2) yes
N1 N2 . 1.314(2) yes
N3 N2 . 1.343(2) yes
N3 C2 . 1.346(2) yes
N3 C3 . 1.461(2) yes
N4 C4 . 1.340(3) yes
N4 C8 . 1.351(2) yes
N4 H4 . 0.862(16) yes
C9 C10 . 1.393(3) no
C9 C1 . 1.468(3) no
C9 C14 . 1.401(2) no
N7 O6 . 1.206(2) no
C10 H10 . 0.9500 no
C10 C11 . 1.388(3) no
C2 H2 . 0.9500 no
C2 C1 . 1.376(2) no
C3 H3A . 0.9900 no
C3 H3B . 0.9900 no
C3 C8 . 1.507(3) no
C11 H11 . 0.9500 no
C11 C12 . 1.387(3) no
C14 H14 . 0.9500 no
C14 C13 . 1.383(3) no
C4 H4A . 0.9500 no
C4 C5 . 1.374(3) no
C8 C7 . 1.376(2) no
C5 H5 . 0.9500 no
C5 C6 . 1.379(3) no
C6 H6 . 0.9500 no
C6 C7 . 1.390(3) no
C7 H7 . 0.9500 no
C12 H12 . 0.9500 no
C12 C13 . 1.386(3) no
C13 H13 . 0.9500 no
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
N4 H4 N1 3_667 0.86(3) 1.88(3) 2.738(3) 170(3) yes
C2 H2 O8 2_656 0.95 2.33 3.261(3) 168 yes
C7 H7 O5 4_565 0.95 2.46 3.379(3) 164 yes
C13 H13 O4 2_556 0.95 2.46 3.377(3) 163 yes
N4 H4 N2 3_667 0.86 2.65(3) 3.432(3) 151 yes
C10 H10 O8 2_656 0.95 2.68 3.621(3) 173 yes
C5 H5 O2 3_666 0.95 2.68 3.191(2) 114 yes
C7 H7 O2 2_656 0.95 2.67 3.279(3) 123 yes
C7 H7 O9 2_656 0.95 2.69 3.369(2) 129 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
Th1 O7 N5 O8 . . . . 177.14(16) ?
Th1 O7 N5 O9 . . . . -3.46(16) ?
Th1 O4 N7 O5 . . . . -3.92(16) ?
Th1 O4 N7 O6 . . . . 173.99(18) ?
Th1 O9 N5 O8 . . . . -177.22(17) ?
Th1 O9 N5 O7 . . . . 3.39(16) ?
Th1 O1 N6 O3 . . . . -176.06(16) ?
Th1 O1 N6 O2 . . . . 4.18(15) ?
Th1 O2 N6 O3 . . . . 176.02(15) ?
Th1 O2 N6 O1 . . . . -4.23(16) ?
Th1 O5 N7 O4 . . . . 3.92(16) ?
Th1 O5 N7 O6 . . . . -173.96(18) ?
N3 C2 C1 N1 . . . . 0.2(2) ?
N3 C2 C1 C9 . . . . 178.82(18) ?
N3 C3 C8 N4 . . . . -59.3(2) ?
N3 C3 C8 C7 . . . . 122.20(19) ?
N4 C4 C5 C6 . . . . -0.9(3) ?
N4 C8 C7 C6 . . . . -0.5(3) ?
N2 N3 C2 C1 . . . . -0.4(2) ?
N2 N3 C3 C8 . . . . 117.63(18) ?
N2 N1 C1 C9 . . . . -178.62(16) ?
N2 N1 C1 C2 . . . . 0.1(2) ?
C9 C10 C11 C12 . . . . -1.1(3) ?
C9 C14 C13 C12 . . . . -0.8(3) ?
C10 C9 C1 N1 . . . . 170.29(17) ?
C10 C9 C1 C2 . . . . -8.1(3) ?
C10 C9 C14 C13 . . . . 0.3(3) ?
C10 C11 C12 C13 . . . . 0.6(3) ?
C2 N3 N2 N1 . . . . 0.5(2) ?
C2 N3 C3 C8 . . . . -62.5(3) ?
C1 N1 N2 N3 . . . . -0.4(2) ?
C1 C9 C10 C11 . . . . -178.78(17) ?
C1 C9 C14 C13 . . . . 179.74(19) ?
C3 N3 N2 N1 . . . . -179.63(16) ?
C3 N3 C2 C1 . . . . 179.72(18) ?
C3 C8 C7 C6 . . . . 178.06(17) ?
C11 C12 C13 C14 . . . . 0.4(3) ?
C14 C9 C10 C11 . . . . 0.7(3) ?
C14 C9 C1 N1 . . . . -9.2(3) ?
C14 C9 C1 C2 . . . . 172.4(2) ?
C4 N4 C8 C3 . . . . -178.54(16) ?
C4 N4 C8 C7 . . . . 0.0(3) ?
C4 C5 C6 C7 . . . . 0.5(3) ?
C8 N4 C4 C5 . . . . 0.7(3) ?
C5 C6 C7 C8 . . . . 0.2(3) ?