#------------------------------------------------------------------------------
#$Date: 2024-06-26 04:46:33 +0300 (Wed, 26 Jun 2024) $
#$Revision: 292597 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/31/2023178.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_2023178
loop_
_publ_author_name
'Mustaphi, Nour El Hoda'
'Chlouchi, Amina'
'El Hafi, Mohamed'
'Mague, Joel T.'
'H\"okelek, Tuncer'
'El Monfalouti, Hanae'
'Haoudi, Amal'
'Mazzah, Ahmed'
_publ_section_title
;
Crystal structure determination and analyses of Hirshfeld surface,
crystal voids, intermolecular interaction energies and energy frameworks
of 1-benzyl-4-(methylsulfanyl)-3a,7a-dihydro-1H-pyrazolo[3,4-d]pyrimidine
;
_journal_coeditor_code WM5721
_journal_issue 7
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_paper_doi 10.1107/S2056989024005954
_journal_volume 80
_journal_year 2024
_chemical_formula_iupac 'C13 H12 N4 S'
_chemical_formula_moiety 'C13 H12 N4 S'
_chemical_formula_sum 'C13 H12 N4 S'
_chemical_formula_weight 256.33
_chemical_name_systematic
1-Benzyl-4-(methylsulfanyl)-3a,7a-dihydro-1H-pyrazolo[3,4-d]pyrimidine
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_Hall '-P 2ybc'
_space_group_name_H-M_alt 'P 1 21/c 1'
_atom_sites_solution_hydrogens difmap
_atom_sites_solution_primary dual
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-2018/3
_cell_angle_alpha 90
_cell_angle_beta 96.0850(10)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 12.4617(5)
_cell_length_b 7.0766(3)
_cell_length_c 13.6500(5)
_cell_measurement_reflns_used 7875
_cell_measurement_temperature 150(2)
_cell_measurement_theta_max 74.7271
_cell_measurement_theta_min 6.2542
_cell_volume 1196.96(8)
_computing_cell_refinement
;
SAINT (Bruker, 2016)
;
_computing_data_collection
;
APEX3 (Bruker, 2016)
;
_computing_data_reduction
;
SAINT (Bruker, 2016)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg & Putz, 2012)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL2018/3 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT/5 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 150(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type 'Bruker D8 VENTURE PHOTON 100 CMOS'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_monochromator mirror
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54178
_diffrn_reflns_av_R_equivalents 0.0261
_diffrn_reflns_av_unetI/netI 0.0248
_diffrn_reflns_limit_h_max 14
_diffrn_reflns_limit_h_min -15
_diffrn_reflns_limit_k_max 8
_diffrn_reflns_limit_k_min -8
_diffrn_reflns_limit_l_max 17
_diffrn_reflns_limit_l_min -15
_diffrn_reflns_number 8877
_diffrn_reflns_theta_full 68.000
_diffrn_reflns_theta_max 74.719
_diffrn_reflns_theta_min 6.522
_diffrn_source 'INCOATEC I\mS micro--focus source'
_exptl_absorpt_coefficient_mu 2.285
_exptl_absorpt_correction_T_max 0.72
_exptl_absorpt_correction_T_min 0.59
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause et al., 2015)
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.422
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 536
_exptl_crystal_size_max 0.257
_exptl_crystal_size_mid 0.218
_exptl_crystal_size_min 0.156
_refine_diff_density_max 0.684
_refine_diff_density_min -0.419
_refine_ls_extinction_coef 0.0175(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2018/3 (Sheldrick, 2015b)
;
_refine_ls_goodness_of_fit_ref 1.100
_refine_ls_hydrogen_treatment refall
_refine_ls_matrix_type full
_refine_ls_number_parameters 212
_refine_ls_number_reflns 2388
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.100
_refine_ls_R_factor_all 0.0498
_refine_ls_R_factor_gt 0.0487
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0792P)^2^+0.9126P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1338
_refine_ls_wR_factor_ref 0.1349
_reflns_number_gt 2292
_reflns_number_total 2388
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file wm5721.cif
_cod_data_source_block I
_cod_original_sg_symbol_H-M 'P 21/c'
_cod_database_code 2023178
_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 0.591
_shelx_estimated_absorpt_t_max 0.717
_shelx_hkl_file
;
2 0 0 208.08 7.50
-2 0 0 225.98 7.50
-3 0 0 1010.60 33.20
3 0 0 981.00 33.20
4 0 0 526.85 18.10
5 0 0 3305.77 110.09
-5 0 0 3419.86 110.19
5 0 0 3258.07 109.39
6 0 0 242.68 8.70
6 0 0 243.68 9.50
-6 0 0 241.08 9.60
7 0 0 614.24 20.70
7 0 0 596.54 21.90
8 0 0 141.79 5.60
8 0 0 130.19 5.40
9 0 0 57.79 3.10
9 0 0 61.89 2.90
10 0 0 150.58 6.00
10 0 0 152.58 6.40
11 0 0 231.48 9.80
11 0 0 246.88 8.90
12 0 0 252.67 10.20
12 0 0 269.77 9.60
13 0 0 440.16 15.80
14 0 0 15.50 1.70
0 -1 0 0.90 0.30
0 1 0 0.70 0.30
1 -1 0 2428.66 76.39
-1 -1 0 2217.28 76.39
-2 -1 0 507.15 17.60
2 -1 0 514.65 17.70
-2 1 0 547.45 17.70
-3 -1 0 1.60 0.50
3 -1 0 1.70 0.60
-3 1 0 1.60 0.70
-4 -1 0 265.27 9.60
4 -1 0 274.67 9.70
-4 1 0 269.27 9.80
4 1 0 251.47 9.60
-5 -1 0 343.17 12.00
5 -1 0 323.67 11.60
5 1 0 315.57 11.30
-5 1 0 325.27 12.10
5 1 0 316.17 11.90
6 -1 0 128.09 5.00
6 -1 0 137.39 5.90
-6 -1 0 120.69 5.80
-6 1 0 122.89 6.00
6 1 0 125.89 5.00
6 1 0 125.79 5.70
7 -1 0 346.27 11.90
7 -1 0 332.97 13.20
7 1 0 326.27 13.20
7 1 0 338.07 12.00
8 -1 0 126.69 4.90
8 -1 0 114.09 4.70
8 1 0 107.09 4.70
8 1 0 115.89 4.90
9 -1 0 101.79 4.60
9 -1 0 101.19 4.40
9 1 0 112.39 4.80
9 1 0 105.59 4.40
10 -1 0 10.70 1.50
10 -1 0 8.90 1.50
10 1 0 10.30 1.70
10 1 0 11.80 1.40
11 -1 0 5.80 1.40
11 -1 0 6.20 1.50
11 1 0 7.40 1.40
11 1 0 5.70 1.50
-11 1 0 4.10 1.20
12 -1 0 212.88 8.50
-12 1 0 219.88 8.00
12 1 0 217.18 8.70
12 1 0 222.08 8.10
13 -1 0 40.90 2.60
13 1 0 40.70 3.10
14 -1 0 73.19 3.50
14 1 0 69.89 3.40
-15 1 0 0.10 0.50
0 -2 0 984.90 33.30
0 2 0 1001.40 33.30
1 -2 0 2651.23 91.29
-1 -2 0 2882.81 91.39
2 -2 0 1657.23 57.19
-2 -2 0 1761.12 57.19
-2 2 0 1742.53 57.39
3 -2 0 944.71 32.00
-3 -2 0 911.71 31.90
-3 -2 0 972.60 31.90
-3 2 0 937.61 32.10
4 -2 0 288.57 10.70
-4 -2 0 285.27 10.60
-4 2 0 280.37 10.90
5 -2 0 463.65 16.50
-5 -2 0 450.35 16.40
5 -2 0 435.36 15.40
-5 2 0 425.86 16.60
5 2 0 479.65 15.60
6 -2 0 36.30 2.20
6 -2 0 42.40 3.20
6 2 0 32.30 2.10
7 -2 0 548.15 18.70
7 -2 0 533.35 18.60
7 2 0 546.95 18.90
8 -2 0 18.20 1.90
8 -2 0 19.30 1.80
8 2 0 16.80 2.00
8 2 0 23.00 1.90
9 -2 0 426.96 14.50
9 -2 0 385.96 15.10
9 2 0 391.16 14.10
9 2 0 414.76 14.70
-9 2 0 399.76 14.10
10 -2 0 700.03 24.20
10 -2 0 707.73 24.00
10 2 0 688.93 23.80
10 2 0 715.13 24.40
-10 2 0 680.83 23.70
11 -2 0 193.88 7.50
11 2 0 183.38 7.00
11 2 0 173.68 7.50
-11 2 0 190.48 7.00
12 -2 0 50.79 3.00
12 2 0 51.19 3.60
12 2 0 46.90 2.90
13 -2 0 72.39 3.80
-13 2 0 82.29 3.90
13 2 0 77.89 3.90
14 2 0 193.98 7.50
-14 2 0 199.78 7.10
-15 2 0 2.50 0.80
0 -3 0 1.50 0.80
0 3 0 2.50 0.90
1 -3 0 523.75 18.00
-1 -3 0 500.25 18.30
-1 3 0 497.85 18.20
2 -3 0 58.59 3.30
-2 -3 0 61.09 3.30
-2 3 0 59.09 3.60
-3 -3 0 664.33 23.00
3 -3 0 638.24 22.80
-3 -3 0 683.33 22.90
-3 3 0 597.44 23.10
-4 -3 0 10.60 2.60
4 -3 0 8.20 1.80
-4 -3 0 5.00 2.20
4 3 0 7.50 1.40
5 -3 0 721.43 26.30
-5 -3 0 736.03 26.30
5 3 0 739.33 24.90
-6 -3 0 8.10 3.90
6 -3 0 7.50 2.00
6 3 0 5.60 1.30
-6 3 0 5.90 1.10
7 -3 0 192.08 7.60
-7 3 0 201.38 7.40
7 3 0 208.18 7.80
8 -3 0 79.89 4.00
-8 3 0 82.69 3.70
8 3 0 87.69 4.10
9 -3 0 51.79 3.20
9 3 0 54.79 3.10
-9 3 0 49.70 2.70
9 3 0 53.29 3.10
10 -3 0 136.99 5.90
10 3 0 131.79 5.40
10 3 0 129.79 5.80
-10 3 0 136.79 5.30
11 3 0 528.25 18.10
11 3 0 499.15 18.70
-11 3 0 552.84 18.20
12 3 0 489.65 17.80
-12 3 0 513.45 17.20
13 3 0 24.40 2.00
-13 3 0 26.60 1.60
-13 3 0 25.10 1.80
-14 3 0 139.29 5.10
0 -4 0 443.56 16.70
1 -4 0 13.60 3.00
-1 -4 0 19.00 2.70
-2 -4 0 140.89 6.70
2 -4 0 124.49 6.60
-3 -4 0 873.71 30.80
3 4 0 853.61 29.10
3 4 0 878.71 29.00
-3 4 0 835.02 28.90
4 4 0 36.50 2.30
-4 4 0 33.30 2.10
-4 4 0 29.40 2.70
4 4 0 33.60 2.80
-5 4 0 1.70 0.80
5 4 0 -0.10 1.40
-5 4 0 3.10 1.50
5 4 0 1.40 1.10
5 4 0 0.90 1.10
-5 4 0 1.70 1.50
-6 4 0 4.20 1.40
-6 4 0 6.30 2.80
6 4 0 4.80 1.30
-6 4 0 6.60 1.30
6 4 0 4.10 1.20
6 4 0 2.40 1.60
7 4 0 8.20 2.10
7 4 0 3.40 1.30
-7 4 0 1.30 0.80
8 4 0 224.48 8.80
-8 4 0 220.18 8.30
-9 4 0 342.77 12.50
9 4 0 348.87 13.00
-9 4 0 365.96 12.70
-10 4 0 75.59 3.50
10 4 0 69.89 3.80
-10 4 0 75.79 3.40
-11 4 0 0.80 0.70
-11 4 0 0.70 0.80
11 4 0 0.20 1.30
-12 4 0 12.50 1.30
12 4 0 7.90 2.10
-12 4 0 11.50 1.20
-13 4 0 -0.80 0.70
-13 4 0 -0.10 0.80
0 5 0 1.20 1.10
0 5 0 3.40 1.20
0 5 0 1.20 1.00
1 5 0 597.84 20.50
-1 5 0 599.04 20.50
-1 5 0 594.94 20.50
1 5 0 613.04 20.60
-1 5 0 564.14 20.60
1 5 0 628.24 20.60
2 5 0 904.21 30.40
-2 5 0 884.11 30.40
2 5 0 921.91 30.60
-2 5 0 920.61 30.50
-2 5 0 840.52 30.40
2 5 0 951.30 30.60
-3 5 0 228.48 8.80
3 5 0 245.18 8.80
-3 5 0 227.88 8.60
3 5 0 244.98 8.70
3 5 0 222.38 8.70
-3 5 0 237.68 8.70
-4 5 0 38.90 3.50
4 5 0 48.10 3.00
-4 5 0 48.30 2.70
-4 5 0 49.70 2.80
4 5 0 49.10 2.70
5 5 0 254.37 9.30
5 5 0 253.67 9.20
-5 5 0 242.38 9.60
-5 5 0 245.28 9.20
6 5 0 2.00 1.20
-6 5 0 0.80 0.80
-6 5 0 2.80 1.40
-6 5 0 2.60 1.60
7 5 0 3.60 1.20
-7 5 0 3.30 1.50
-7 5 0 1.20 0.80
7 5 0 1.00 1.30
-8 5 0 8.80 1.40
-8 5 0 11.00 2.20
8 5 0 7.10 2.00
-9 5 0 8.40 1.30
-9 5 0 6.70 1.30
-10 5 0 6.80 1.10
-10 5 0 7.80 1.60
-11 5 0 501.45 17.10
-11 5 0 501.85 17.10
-12 5 0 231.08 7.90
-12 5 0 225.38 8.00
0 6 0 602.24 21.00
0 6 0 610.14 21.00
0 6 0 615.14 20.90
1 6 0 165.68 6.40
-1 6 0 158.08 6.50
-1 6 0 163.78 6.40
1 6 0 162.58 6.60
1 6 0 167.68 6.40
-1 6 0 159.48 6.40
2 6 0 154.58 6.20
2 6 0 156.48 6.00
-2 6 0 143.69 6.10
-2 6 0 150.38 6.00
-2 6 0 148.49 6.00
2 6 0 155.68 6.20
-3 6 0 151.78 6.10
-3 6 0 153.28 6.30
-3 6 0 149.49 6.10
3 6 0 159.58 6.30
3 6 0 155.18 6.10
4 6 0 54.19 3.10
-4 6 0 51.89 2.80
4 6 0 55.49 2.90
-4 6 0 57.49 2.90
-4 6 0 50.29 3.40
-5 6 0 87.89 4.00
-5 6 0 87.19 4.00
5 6 0 90.59 4.00
5 6 0 90.19 4.20
6 6 0 96.89 4.30
-6 6 0 92.19 4.20
6 6 0 99.19 4.20
-7 6 0 198.88 7.70
7 6 0 179.58 7.00
7 6 0 183.98 7.10
-8 6 0 0.50 0.60
8 6 0 -0.10 1.10
-9 6 0 86.09 3.60
-10 6 0 136.59 5.10
-11 6 0 14.70 1.10
0 7 0 2.10 1.00
0 7 0 0.00 0.90
0 7 0 -0.70 0.70
-1 7 0 70.89 3.40
-1 7 0 73.49 3.60
1 7 0 74.89 3.40
-1 7 0 69.99 3.40
1 7 0 71.89 3.50
1 7 0 66.59 4.10
-2 7 0 54.69 2.90
-2 7 0 59.59 3.10
-2 7 0 54.69 2.90
2 7 0 60.49 3.00
2 7 0 61.89 3.10
-3 7 0 29.10 2.60
-3 7 0 33.50 2.20
-3 7 0 33.80 2.50
3 7 0 39.00 2.40
3 7 0 39.00 2.20
4 7 0 28.80 1.80
-4 7 0 21.80 1.70
4 7 0 25.00 2.00
-4 7 0 20.70 2.60
-4 7 0 22.40 1.70
5 7 0 91.79 3.90
5 7 0 96.29 4.10
-5 7 0 94.49 4.00
-6 7 0 56.79 2.70
6 7 0 59.29 2.70
6 7 0 63.69 2.90
7 7 0 15.50 1.30
-7 7 0 14.90 1.20
7 7 0 16.50 1.70
-8 7 0 1.30 0.60
-9 7 0 3.70 0.70
0 8 0 500.25 16.90
0 8 0 472.35 16.60
-1 8 0 174.18 6.50
-1 8 0 183.98 6.60
-1 8 0 180.78 6.60
1 8 0 181.18 6.70
1 8 0 184.98 6.80
-2 8 0 135.69 5.20
-2 8 0 134.39 5.20
2 8 0 144.99 5.30
2 8 0 138.19 5.40
-2 8 0 137.29 5.10
3 8 0 1.50 0.70
3 8 0 4.60 0.90
-3 8 0 2.90 0.70
-3 8 0 3.10 1.10
4 8 0 387.56 13.20
-4 8 0 372.66 13.20
4 8 0 395.26 13.20
-5 8 0 1.30 0.60
5 8 0 0.80 0.60
5 8 0 1.90 0.70
6 8 0 85.19 3.50
-6 8 0 74.59 3.00
14 0 -1 -1.20 0.90
13 0 -1 0.00 0.90
13 0 -1 0.50 0.60
12 0 -1 -0.60 0.80
12 0 -1 0.80 0.90
11 0 -1 1.30 0.70
10 0 -1 0.10 0.60
10 0 -1 0.60 0.80
9 0 -1 1.10 0.80
9 0 -1 0.00 0.70
9 0 -1 -0.60 1.00
8 0 -1 0.40 0.70
8 0 -1 0.90 0.90
8 0 -1 0.80 1.90
7 0 -1 0.90 1.10
-7 0 1 0.50 2.30
7 0 -1 1.40 0.70
-6 0 1 1.30 0.90
6 0 -1 2.00 0.70
6 0 -1 1.20 0.80
-5 0 1 0.70 0.50
5 0 -1 0.80 0.60
5 0 -1 1.30 0.80
4 0 -1 0.10 0.30
-4 0 1 0.30 0.40
3 0 -1 0.30 0.20
-3 0 1 0.30 0.30
1 0 -1 0.40 0.10
-1 0 1 0.60 0.10
0 0 -1 0.50 0.10
1 0 1 0.10 0.10
-1 0 -1 0.10 0.10
-2 0 -1 1.00 0.40
3 0 1 0.20 0.20
-3 0 -1 0.40 0.30
4 0 1 -0.10 0.30
-4 0 -1 0.90 0.50
5 0 1 1.90 0.70
5 0 1 2.10 1.00
-5 0 -1 2.90 1.20
6 0 1 1.90 0.70
6 0 1 1.00 0.90
-6 0 -1 1.10 1.20
7 0 1 2.70 0.80
7 0 1 1.00 1.30
8 0 1 0.20 0.60
8 0 1 0.90 0.90
9 0 1 -0.80 0.70
9 0 1 0.90 0.80
10 0 1 -0.10 0.90
10 0 1 -0.30 0.80
11 0 1 0.00 0.80
11 0 1 1.20 0.90
12 0 1 0.30 0.90
13 0 1 0.90 0.90
14 0 1 0.00 1.00
-15 0 -1 0.10 0.60
14 -1 -1 374.76 13.20
14 1 -1 364.46 13.20
13 -1 -1 5.20 1.40
13 1 -1 3.40 1.10
-13 1 1 1.50 1.10
13 1 -1 2.10 0.90
12 -1 -1 111.09 4.50
12 -1 -1 100.19 4.80
12 1 -1 93.19 4.70
-12 1 1 110.69 4.40
12 1 -1 105.29 4.40
11 -1 -1 1197.58 38.90
11 -1 -1 1137.69 39.10
11 1 -1 1117.99 39.20
11 1 -1 1157.68 38.70
10 -1 -1 988.00 33.10
10 -1 -1 960.50 32.70
10 1 -1 985.50 33.50
10 1 -1 943.61 32.70
9 -1 -1 218.68 8.40
9 1 -1 230.18 8.50
9 1 -1 223.18 8.10
9 1 -1 205.18 8.00
8 -1 -1 891.61 32.30
8 -1 -1 1009.30 32.60
8 1 -1 1000.10 32.70
8 1 -1 953.60 32.30
7 -1 -1 790.32 28.20
7 -1 -1 798.42 27.00
7 1 -1 802.42 27.10
7 1 -1 805.32 28.20
6 -1 -1 878.81 29.20
-6 -1 1 815.12 28.90
6 -1 -1 858.81 28.20
6 1 -1 856.81 28.30
-6 1 1 786.52 29.10
6 1 -1 839.62 29.00
5 -1 -1 64.59 2.80
-5 -1 1 63.59 3.10
5 -1 -1 65.29 3.20
5 1 -1 60.09 3.10
5 1 -1 61.19 2.80
-5 1 1 66.79 3.30
-4 -1 1 134.89 5.00
4 -1 -1 129.69 5.10
4 1 -1 124.69 5.00
-4 1 1 122.69 5.10
3 -1 -1 3132.09 103.19
-2 -1 1 32.50 1.40
2 -1 -1 28.60 1.50
-2 1 1 29.80 1.50
1 -1 -1 1517.45 47.00
-1 -1 1 1323.67 46.80
0 -1 1 149.49 5.10
0 -1 -1 138.19 5.10
0 1 -1 148.99 5.10
0 1 1 140.09 5.10
1 -1 1 1029.90 35.10
-1 1 -1 1088.59 35.20
3 -1 1 2197.58 71.99
-3 1 -1 2143.19 72.59
3 1 1 2178.88 71.99
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10 2 -9 86.99 3.90
10 2 -9 67.49 3.90
9 -2 -9 36.90 2.50
9 2 -9 40.40 2.30
9 2 -9 40.50 2.20
9 2 -9 36.50 2.90
8 -2 -9 74.59 3.90
8 2 -9 79.69 3.60
8 2 -9 80.29 3.70
7 -2 -9 46.70 2.90
7 2 -9 47.00 2.70
7 2 -9 52.39 3.10
6 -2 -9 175.38 6.90
6 2 -9 163.68 6.60
6 2 -9 169.08 6.50
5 -2 -9 45.10 2.70
5 -2 -9 46.10 2.70
5 2 -9 49.60 2.60
-5 2 9 38.00 3.40
5 2 -9 50.29 2.70
4 -2 -9 60.09 3.10
4 2 -9 57.19 2.90
-4 2 9 55.49 3.30
4 2 -9 58.69 3.00
3 -2 -9 219.98 8.30
3 2 -9 219.08 8.10
-3 2 9 213.18 8.20
3 2 -9 217.38 8.20
3 2 -9 218.28 8.10
2 -2 -9 39.90 2.40
2 2 -9 43.30 2.60
-2 2 9 42.30 2.80
2 2 -9 41.60 2.60
2 2 -9 40.90 2.50
-1 -2 9 3.40 1.50
1 -2 -9 5.50 1.20
-1 2 9 3.20 1.20
1 2 -9 3.50 1.10
1 2 -9 3.40 1.00
1 2 -9 3.50 1.10
-1 2 9 2.30 2.00
0 -2 9 218.48 8.30
0 -2 -9 231.18 8.50
0 2 -9 226.38 8.40
0 2 9 218.88 8.30
0 2 9 228.68 8.40
0 2 -9 223.48 8.30
0 2 -9 205.78 8.30
1 -2 9 36.60 2.50
-1 -2 -9 42.00 2.60
-1 2 -9 42.70 2.70
1 2 9 43.50 2.70
1 2 9 40.90 2.60
2 -2 9 0.80 1.00
-2 2 -9 0.60 1.00
2 2 9 2.10 1.10
2 2 9 1.00 1.00
-3 2 -9 240.38 9.10
3 2 9 259.57 9.60
3 2 9 232.18 9.80
4 -2 9 782.02 26.70
4 2 9 772.52 26.60
-4 2 -9 786.42 26.80
4 2 9 786.12 26.70
5 -2 9 25.40 2.00
5 2 9 29.10 2.60
5 2 9 29.00 2.20
-5 2 -9 26.80 2.30
6 -2 9 235.78 8.90
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6 2 9 241.08 8.90
6 2 9 231.78 9.00
7 -2 9 403.86 14.60
7 2 9 418.76 14.70
-7 2 -9 415.96 14.70
8 -2 9 94.99 4.20
8 2 9 98.99 4.30
-8 2 -9 99.29 4.40
9 -2 9 120.39 4.80
-9 2 -9 122.89 5.00
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10 -2 9 1.10 0.80
-10 2 -9 1.20 0.80
10 2 9 2.10 0.80
11 2 9 4.60 1.20
12 3 -9 0.30 0.50
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12 3 -9 1.10 0.60
11 -3 -9 23.60 1.80
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11 3 -9 23.10 1.40
11 3 -9 20.70 1.30
10 -3 -9 28.00 2.00
10 3 -9 22.90 1.50
-10 3 9 25.30 1.60
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9 -3 -9 2.30 0.90
9 3 -9 2.90 0.80
9 3 -9 3.30 1.10
8 -3 -9 200.78 8.00
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8 3 -9 202.88 7.60
7 -3 -9 27.40 2.20
7 3 -9 26.60 2.00
7 3 -9 30.70 2.00
6 3 -9 18.70 1.70
6 3 -9 23.70 2.30
6 3 -9 18.20 1.80
5 -3 -9 121.49 5.20
5 3 -9 114.89 5.00
5 3 -9 115.69 5.00
5 3 -9 120.59 5.20
-5 3 9 121.59 5.20
4 -3 -9 191.38 7.50
-4 3 9 182.18 7.30
4 3 -9 196.38 7.30
4 3 -9 185.48 7.10
4 3 -9 181.98 7.20
3 -3 -9 2.00 0.80
3 3 -9 0.00 1.00
3 3 -9 0.50 0.80
3 3 -9 0.90 0.70
-3 3 9 3.10 1.20
2 -3 -9 27.00 2.00
2 3 -9 30.40 2.40
2 3 -9 28.40 2.10
2 3 -9 25.40 2.20
1 -3 -9 6.90 1.30
1 3 -9 3.80 1.20
1 3 -9 4.80 1.10
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1 3 -9 7.40 2.30
0 -3 -9 139.29 5.80
0 3 9 131.89 5.60
0 3 -9 134.59 5.80
0 3 -9 134.79 5.70
0 3 -9 135.69 5.50
0 3 9 132.89 5.70
-1 -3 -9 72.69 3.60
1 -3 9 72.09 3.50
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-1 3 -9 66.89 3.50
1 3 9 69.29 3.60
-2 -3 -9 551.34 18.50
2 -3 9 520.05 18.10
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2 3 9 513.45 18.20
2 3 9 520.95 18.10
-2 3 -9 530.95 18.20
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3 -3 9 35.60 2.40
3 3 9 39.30 2.60
3 3 9 41.00 2.50
-3 3 -9 35.30 2.60
4 -3 9 137.49 5.50
4 3 9 132.09 5.50
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4 3 9 125.29 5.50
5 -3 9 4.20 1.00
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5 3 9 5.30 1.40
5 3 9 2.10 1.20
6 -3 9 118.09 5.00
6 3 9 117.19 5.10
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6 3 9 120.49 5.20
7 -3 9 21.40 1.70
7 3 9 20.10 1.80
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8 -3 9 1.20 0.70
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9 -3 9 43.40 2.20
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10 -3 9 4.30 1.10
-10 3 -9 6.10 1.00
10 3 9 6.00 1.30
-11 3 -9 31.80 1.60
12 4 -9 118.89 4.40
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11 4 -9 78.69 3.30
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11 4 -9 79.49 3.00
10 -4 -9 267.57 9.70
10 4 -9 274.07 9.40
-10 4 9 268.17 9.40
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9 -4 -9 116.89 5.00
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8 -4 -9 194.68 7.60
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7 -4 -9 7.90 1.50
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6 -4 -9 96.19 4.60
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6 4 -9 112.29 4.60
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6 4 -9 103.59 4.50
5 -4 -9 236.18 9.20
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-5 4 9 239.68 9.10
5 4 -9 247.18 9.00
4 -4 -9 192.18 7.80
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4 4 -9 189.48 7.40
4 4 -9 202.38 7.60
3 4 -9 382.16 13.90
3 4 -9 391.46 13.80
3 4 -9 391.56 14.00
-3 4 9 401.16 14.00
2 4 -9 91.39 4.00
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2 4 -9 85.69 4.10
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1 -4 -9 37.90 2.50
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1 4 -9 34.90 2.30
1 4 -9 34.90 2.30
1 4 -9 34.10 2.80
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0 -4 -9 144.49 6.00
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0 4 -9 141.79 5.90
0 4 -9 142.29 5.70
0 4 9 138.99 5.90
-1 -4 -9 497.55 18.20
1 4 9 497.45 17.50
-1 4 -9 500.05 17.40
-1 4 -9 497.55 17.50
-1 4 -9 493.05 17.30
1 4 9 496.15 17.40
2 -4 9 269.67 10.10
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-2 4 -9 268.17 9.80
2 4 9 262.07 9.90
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3 -4 9 277.47 10.40
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4 -4 9 40.60 2.40
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-4 4 -9 33.30 2.70
4 4 9 36.80 2.50
5 -4 9 91.29 4.10
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5 4 9 99.09 4.40
5 4 9 96.69 4.30
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6 4 9 392.06 15.30
7 -4 9 434.56 15.20
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8 -4 9 92.59 3.70
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8 4 9 94.49 3.90
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9 -4 9 10.00 1.10
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8 -5 -9 8.80 2.00
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8 5 -9 11.00 1.20
7 -5 -9 10.30 1.80
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-7 5 9 6.90 2.00
6 -5 -9 -0.20 1.00
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5 -5 -9 158.08 6.60
5 5 -9 170.18 6.40
5 5 -9 180.38 7.40
-5 5 9 164.38 6.70
4 -5 -9 219.38 9.00
4 5 -9 239.88 8.90
4 5 -9 250.27 8.90
-4 5 9 246.38 8.90
4 5 -9 235.38 8.70
3 -5 -9 18.30 1.90
3 5 -9 18.30 1.80
-3 5 9 25.30 2.20
3 5 -9 19.60 1.70
3 5 -9 22.80 2.00
2 -5 -9 253.97 10.10
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2 5 -9 273.57 10.00
2 5 -9 270.67 9.90
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1 -5 -9 130.59 5.70
1 5 -9 138.09 5.50
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1 5 -9 133.69 5.60
1 5 -9 136.09 6.30
0 -5 -9 90.59 4.40
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0 5 -9 94.19 4.30
0 5 9 95.39 4.30
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-1 5 -9 56.29 2.90
1 5 9 53.19 2.90
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2 5 9 5.90 1.60
-2 5 -9 9.10 1.60
-2 5 -9 5.40 1.40
-2 5 -9 9.00 1.60
3 -5 9 45.90 2.50
-3 -5 -9 40.90 2.80
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3 5 9 48.10 2.70
3 5 9 43.30 2.70
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4 -5 9 13.80 1.50
-4 -5 -9 17.20 1.90
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4 5 9 17.90 1.60
-4 5 -9 15.60 1.70
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5 -5 9 58.29 2.80
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-5 5 -9 56.59 2.90
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6 -5 9 28.20 1.70
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-6 5 -9 27.10 1.80
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-7 -5 -9 23.60 2.00
7 -5 9 23.00 1.40
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-7 5 -9 21.60 1.60
8 -5 9 2.60 0.80
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6 6 -9 10.10 1.10
5 6 -9 13.70 1.20
5 6 -9 14.90 1.30
5 6 -9 13.00 1.40
4 6 -9 128.19 4.90
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4 6 -9 122.59 4.90
4 6 -9 124.09 5.00
3 -6 -9 21.90 2.50
-3 6 9 21.70 2.00
3 6 -9 23.50 1.70
3 6 -9 23.60 1.60
3 6 -9 27.70 2.30
2 -6 -9 33.50 2.70
2 6 -9 31.30 1.90
-2 6 9 32.80 2.20
2 6 -9 29.80 2.00
2 6 -9 32.10 1.90
1 -6 -9 93.29 4.50
1 6 -9 96.59 4.10
-1 6 9 99.59 4.20
-1 6 9 95.19 4.10
1 6 -9 96.09 4.00
1 6 -9 93.49 4.00
0 -6 -9 198.98 7.90
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0 6 -9 200.78 7.40
0 6 -9 200.68 7.40
0 6 -9 200.48 7.40
-1 -6 -9 639.94 21.50
1 -6 9 619.14 21.20
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1 6 9 597.54 21.20
-1 6 -9 616.14 21.10
-1 6 -9 625.44 21.10
2 -6 9 38.70 2.10
-2 -6 -9 40.90 2.70
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2 6 9 42.00 2.30
-2 6 -9 39.20 2.10
2 6 9 37.70 2.10
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3 -6 9 51.49 2.40
-3 6 -9 49.40 2.50
-3 6 -9 50.79 2.40
3 6 9 52.19 2.60
3 6 9 49.60 2.50
-4 -6 -9 227.68 8.70
4 -6 9 242.38 8.50
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-4 6 -9 232.58 8.40
4 6 9 225.78 8.30
-4 6 -9 233.68 8.20
5 -6 9 69.79 3.00
-5 6 -9 61.59 2.70
-5 6 -9 66.89 2.80
5 6 9 61.39 2.80
5 6 9 62.59 3.30
6 -6 9 108.39 3.90
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-6 6 -9 101.69 4.00
7 -6 9 54.29 2.30
-7 6 -9 61.69 2.40
7 6 9 58.79 2.30
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4 7 -9 120.19 4.40
3 7 -9 3.40 0.80
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3 7 -9 1.50 0.60
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2 7 -9 11.10 1.10
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1 7 -9 2.30 0.80
0 -7 9 8.90 1.20
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1 -7 9 106.29 4.30
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1 7 9 101.29 4.00
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2 -7 9 255.77 8.60
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-2 7 -9 248.78 8.60
2 7 9 253.97 8.60
-2 7 -9 249.97 8.60
3 -7 9 37.80 1.70
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-6 0 10 286.47 10.90
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-5 0 10 238.18 9.20
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-4 0 10 58.09 3.20
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-3 0 10 19.60 2.10
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12 -1 -10 28.20 1.70
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11 -1 -10 6.70 1.70
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10 -1 -10 72.19 3.80
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7 -1 -10 321.77 12.30
7 -1 -10 318.87 12.00
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5 -1 -10 20.50 1.90
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2 -1 -10 4.00 1.30
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-2 1 10 4.00 1.20
1 -1 -10 268.67 9.60
-1 -1 10 242.98 9.40
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-1 -1 -10 71.69 3.50
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2 -2 -15 26.30 2.10
-2 -2 15 28.00 2.00
-2 2 15 24.00 1.70
2 2 -15 21.90 2.10
1 -2 -15 63.09 3.10
-1 -2 15 63.39 3.20
-1 2 15 61.19 2.90
1 2 -15 53.49 4.10
0 -2 -15 3.60 1.30
0 2 15 0.90 0.80
1 -2 15 -0.20 0.60
-1 -2 -15 1.50 1.30
1 2 15 0.60 0.70
2 -2 15 69.09 3.00
2 -2 15 67.59 3.00
2 2 15 77.49 4.00
3 -2 15 -0.10 0.80
3 -2 15 1.00 0.80
3 2 15 0.40 1.00
3 2 15 -0.30 0.70
4 -2 15 5.40 1.00
4 2 15 6.60 1.20
4 2 15 7.90 1.40
5 -2 15 2.70 0.70
6 3 -15 5.10 1.00
-5 -3 15 8.10 1.20
5 3 -15 8.80 1.10
4 3 -15 11.30 1.10
-4 3 15 10.30 1.60
3 -3 -15 101.29 4.40
-3 -3 15 105.79 4.10
3 3 -15 106.39 4.00
-2 -3 15 16.30 1.40
2 -3 -15 14.80 1.70
2 3 -15 16.10 1.30
-2 3 15 15.50 1.30
-1 -3 15 0.50 0.60
1 -3 -15 -1.40 1.10
1 3 -15 0.40 0.70
-1 3 15 0.60 0.60
0 -3 -15 20.00 1.90
0 -3 15 21.20 1.40
0 3 15 23.70 2.00
0 3 -15 20.90 1.50
-1 3 -15 1.80 0.80
1 3 15 1.70 0.60
2 -3 15 35.40 1.80
2 3 15 34.40 1.80
3 3 15 -0.60 0.70
-3 -4 15 7.40 1.00
3 4 -15 8.90 1.00
-2 -4 15 89.59 3.40
2 4 -15 87.29 3.30
-2 4 15 87.29 3.40
-1 -4 15 11.20 1.00
-1 4 15 9.50 1.10
1 4 -15 10.70 1.10
0 -4 15 22.90 1.30
0 4 15 24.40 1.40
0 4 -15 22.30 1.50
-5 0 16 112.69 4.30
-4 0 16 33.40 2.00
-3 0 16 54.49 2.50
-2 0 16 55.29 2.90
-1 0 16 639.04 21.60
0 0 16 1313.57 44.20
1 0 16 54.99 2.50
2 0 16 67.89 2.80
3 0 16 28.50 1.70
-5 -1 16 0.40 0.90
-4 -1 16 8.50 1.20
-4 1 16 9.80 1.40
-3 -1 16 1.80 0.60
-3 1 16 1.20 0.70
-2 -1 16 27.40 1.70
-2 1 16 26.00 2.40
-1 1 16 4.80 1.10
0 -1 16 5.90 1.40
0 1 16 4.20 1.00
1 1 16 111.09 4.50
2 -1 16 10.90 1.30
2 1 16 8.90 1.10
3 1 16 11.00 2.00
-4 -2 16 2.50 0.70
-4 2 16 6.50 1.50
-3 -2 16 1.10 0.60
-3 2 16 0.40 0.70
-2 2 16 4.80 1.00
-1 2 16 40.40 2.40
0 -2 16 16.30 1.30
0 2 16 16.70 1.20
1 -2 16 10.30 1.10
1 2 16 8.90 1.10
2 -2 16 36.00 2.40
2 2 16 28.60 1.60
-2 -3 16 17.60 1.20
-2 3 16 18.00 1.30
-1 -3 16 11.00 1.00
-1 3 16 7.30 1.10
-2 0 17 -0.30 0.60
-1 0 17 0.70 0.60
0 0 0 0.00 0.00
_computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)'
;
_shelx_hkl_checksum 11462
_shelx_res_file
;
TITL jtm1198_0m_a.res in P2(1)/c
jtm1198_0m_a.res
created by SHELXL-2018/3 at 15:50:21 on 31-Dec-2019
REM Old TITL jtm1198_0m in P2(1)/c
REM SHELXT solution in P2(1)/c
REM R1 0.103, Rweak 0.003, Alpha 0.026, Orientation as input
REM Formula found by SHELXT: C14 N3 S
CELL 1.54178 12.4617 7.0766 13.6500 90.000 96.085 90.000
ZERR 4.000 0.0005 0.0003 0.0005 0.000 0.001 0.000
LATT 1
SYMM -X, 1/2+Y, 1/2-Z
SFAC C H N S
UNIT 52 48 16 4
TEMP -123
SIZE 0.156 0.218 0.257
L.S. 5
BOND $H
LIST 4
FMAP 2
PLAN 5
MPLA N1 > C5
MPLA C7 > C12
CONF
EQIV $1 x, y-1, z
HTAB C2 S1_$1
ACTA 136
WGHT 0.079200 0.912600
EXTI 0.017523
FVAR 0.84588
S1 4 0.651899 0.561758 0.632805 11.00000 0.02359 0.02297 =
0.03413 -0.00033 0.00211 0.00000
N1 3 0.602371 0.196645 0.624618 11.00000 0.02252 0.02112 =
0.03267 0.00088 0.00388 0.00114
N2 3 0.425034 0.058013 0.619204 11.00000 0.02587 0.01983 =
0.02955 -0.00025 0.00422 -0.00093
N3 3 0.284644 0.292082 0.620892 11.00000 0.01941 0.02515 =
0.02603 -0.00131 0.00209 -0.00167
N4 3 0.277152 0.485131 0.624267 11.00000 0.02416 0.02509 =
0.02931 -0.00336 0.00243 0.00219
C1 1 0.562833 0.371829 0.628218 11.00000 0.02110 0.02139 =
0.01785 0.00098 0.00060 -0.00224
C2 1 0.530489 0.051913 0.620473 11.00000 0.02813 0.01909 =
0.03873 -0.00115 0.00395 0.00236
H2 2 0.561282 -0.074017 0.617859 11.00000 0.04034
C3 1 0.388196 0.237101 0.622097 11.00000 0.02136 0.02425 =
0.01945 -0.00056 0.00184 -0.00338
C4 1 0.376309 0.552438 0.628050 11.00000 0.02266 0.02422 =
0.02807 -0.00309 0.00227 0.00376
H4 2 0.387187 0.676157 0.632570 11.00000 0.01597
C5 1 0.451911 0.401433 0.626844 11.00000 0.02245 0.01969 =
0.02156 -0.00157 0.00117 -0.00031
C6 1 0.188602 0.171090 0.614040 11.00000 0.02009 0.03198 =
0.02462 0.00020 0.00454 -0.00668
H6A 2 0.213160 0.050482 0.636932 11.00000 0.02411
H6B 2 0.143881 0.215046 0.659384 11.00000 0.02429
C7 1 0.131009 0.162652 0.511104 11.00000 0.01611 0.02001 =
0.02549 0.00097 0.00363 -0.00289
C8 1 0.177187 0.066050 0.437087 11.00000 0.01904 0.02162 =
0.02942 0.00024 0.00473 0.00044
H8 2 0.241524 0.004411 0.450707 11.00000 0.02051
C9 1 0.124223 0.057493 0.342451 11.00000 0.03017 0.02499 =
0.02724 -0.00374 0.00765 -0.00504
H9 2 0.156336 -0.002554 0.295107 11.00000 0.03837
C10 1 0.024995 0.145632 0.321151 11.00000 0.02647 0.03292 =
0.02728 0.00479 -0.00358 -0.00992
H10 2 -0.003928 0.137278 0.263663 11.00000 0.04134
C11 1 -0.021574 0.242330 0.394110 11.00000 0.01635 0.02992 =
0.04002 0.00815 -0.00078 -0.00134
H11 2 -0.082479 0.299439 0.380085 11.00000 0.03265
C12 1 0.031666 0.250639 0.488944 11.00000 0.01871 0.02192 =
0.03367 0.00017 0.00659 -0.00117
H12 2 -0.002536 0.320544 0.538318 11.00000 0.04111
C13 1 0.778785 0.443998 0.631622 11.00000 0.02559 0.02960 =
0.04413 0.00388 -0.00026 -0.00200
H13A 2 0.780893 0.380843 0.570017 11.00000 0.04010
H13B 2 0.786722 0.361071 0.686214 11.00000 0.03578
H13C 2 0.836037 0.547433 0.632827 11.00000 0.06757
HKLF 4
REM jtm1198_0m_a.res in P2(1)/c
REM wR2 = 0.134862, GooF = S = 1.09953, Restrained GooF = 1.09953 for all data
REM R1 = 0.048725 for 2292 Fo > 4sig(Fo) and 0.049755 for all 2388 data
REM 212 parameters refined using 0 restraints
END
WGHT 0.0792 0.9126
REM Highest difference peak 0.684, deepest hole -0.419, 1-sigma level 0.083
Q1 1 0.6659 0.3466 0.6422 11.00000 0.05 0.68
Q2 1 0.7355 0.5253 0.6368 11.00000 0.05 0.42
Q3 1 0.3637 -0.0080 0.6219 11.00000 0.05 0.35
Q4 1 0.0046 0.1901 0.3634 11.00000 0.05 0.34
Q5 1 0.0793 0.0982 0.3408 11.00000 0.05 0.32
;
_shelx_res_checksum 58812
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
S S1 0.65190(4) 0.56176(7) 0.63280(4) 0.0270(2) Uani d 1 . .
N N1 0.60237(13) 0.1966(2) 0.62462(13) 0.0254(4) Uani d 1 . .
N N2 0.42503(15) 0.0580(2) 0.61920(13) 0.0250(4) Uani d 1 . .
N N3 0.28464(13) 0.2921(2) 0.62089(12) 0.0236(4) Uani d 1 . .
N N4 0.27715(14) 0.4851(3) 0.62427(13) 0.0262(4) Uani d 1 . .
C C1 0.56283(15) 0.3718(3) 0.62822(13) 0.0202(4) Uani d 1 . .
C C2 0.53049(18) 0.0519(3) 0.62047(17) 0.0286(5) Uani d 1 . .
H H2 0.561(2) -0.074(4) 0.618(2) 0.040(8) Uiso d 1 . .
C C3 0.38820(15) 0.2371(3) 0.62210(13) 0.0217(4) Uani d 1 . .
C C4 0.37631(17) 0.5524(3) 0.62805(15) 0.0250(4) Uani d 1 . .
H H4 0.3872(18) 0.676(4) 0.6326(16) 0.016(5) Uiso d 1 . .
C C5 0.45191(16) 0.4014(3) 0.62684(14) 0.0213(4) Uani d 1 . .
C C6 0.18860(16) 0.1711(3) 0.61404(14) 0.0254(4) Uani d 1 . .
H H6A 0.213(2) 0.050(4) 0.6369(18) 0.024(6) Uiso d 1 . .
H H6B 0.144(2) 0.215(4) 0.6594(18) 0.024(6) Uiso d 1 . .
C C7 0.13101(14) 0.1627(3) 0.51110(13) 0.0204(4) Uani d 1 . .
C C8 0.17719(16) 0.0661(3) 0.43709(15) 0.0232(4) Uani d 1 . .
H H8 0.242(2) 0.004(4) 0.4507(16) 0.021(5) Uiso d 1 . .
C C9 0.12422(18) 0.0575(3) 0.34245(16) 0.0271(5) Uani d 1 . .
H H9 0.156(2) -0.003(4) 0.295(2) 0.038(7) Uiso d 1 . .
C C10 0.02500(17) 0.1456(3) 0.32115(16) 0.0293(5) Uani d 1 . .
H H10 -0.004(2) 0.137(4) 0.264(2) 0.041(8) Uiso d 1 . .
C C11 -0.02157(16) 0.2423(3) 0.39411(16) 0.0290(5) Uani d 1 . .
H H11 -0.082(2) 0.299(4) 0.3801(19) 0.033(7) Uiso d 1 . .
C C12 0.03167(15) 0.2506(3) 0.48894(15) 0.0245(4) Uani d 1 . .
H H12 -0.003(2) 0.321(4) 0.538(2) 0.041(7) Uiso d 1 . .
C C13 0.77879(19) 0.4440(3) 0.6316(2) 0.0334(5) Uani d 1 . .
H H13A 0.781(2) 0.381(4) 0.570(2) 0.040(7) Uiso d 1 . .
H H13B 0.787(2) 0.361(4) 0.686(2) 0.036(7) Uiso d 1 . .
H H13C 0.836(3) 0.547(5) 0.633(3) 0.068(11) 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
S1 0.0236(3) 0.0230(3) 0.0341(3) 0.00000(17) 0.0021(2) -0.00033(17)
N1 0.0225(8) 0.0211(8) 0.0327(9) 0.0011(6) 0.0039(7) 0.0009(6)
N2 0.0259(9) 0.0198(8) 0.0295(9) -0.0009(6) 0.0042(7) -0.0002(6)
N3 0.0194(8) 0.0252(9) 0.0260(8) -0.0017(6) 0.0021(6) -0.0013(6)
N4 0.0242(9) 0.0251(9) 0.0293(8) 0.0022(7) 0.0024(6) -0.0034(7)
C1 0.0211(9) 0.0214(9) 0.0178(8) -0.0022(7) 0.0006(6) 0.0010(7)
C2 0.0281(11) 0.0191(10) 0.0387(12) 0.0024(8) 0.0039(9) -0.0011(8)
C3 0.0214(9) 0.0242(10) 0.0194(8) -0.0034(7) 0.0018(7) -0.0006(7)
C4 0.0227(10) 0.0242(11) 0.0281(10) 0.0038(7) 0.0023(8) -0.0031(7)
C5 0.0224(10) 0.0197(9) 0.0216(9) -0.0003(7) 0.0012(7) -0.0016(7)
C6 0.0201(9) 0.0320(11) 0.0246(9) -0.0067(8) 0.0045(8) 0.0002(8)
C7 0.0161(8) 0.0200(8) 0.0255(9) -0.0029(7) 0.0036(7) 0.0010(7)
C8 0.0190(10) 0.0216(9) 0.0294(10) 0.0004(7) 0.0047(8) 0.0002(7)
C9 0.0302(11) 0.0250(10) 0.0272(10) -0.0050(8) 0.0076(8) -0.0037(7)
C10 0.0265(10) 0.0329(11) 0.0273(10) -0.0099(8) -0.0036(8) 0.0048(8)
C11 0.0164(9) 0.0299(11) 0.0400(11) -0.0013(8) -0.0008(8) 0.0082(9)
C12 0.0187(9) 0.0219(9) 0.0337(10) -0.0012(7) 0.0066(7) 0.0002(7)
C13 0.0256(11) 0.0296(12) 0.0441(13) -0.0020(8) -0.0003(9) 0.0039(9)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 '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
C1 S1 C13 . . 101.59(10) ?
C1 N1 C2 . . 117.19(17) ?
C2 N2 C3 . . 111.93(17) ?
C3 N3 N4 . . 110.87(16) ?
C3 N3 C6 . . 127.36(18) ?
N4 N3 C6 . . 121.74(16) ?
C4 N4 N3 . . 107.11(16) ?
N1 C1 C5 . . 120.45(17) ?
N1 C1 S1 . . 118.78(15) ?
C5 C1 S1 . . 120.76(15) ?
N2 C2 N1 . . 129.09(19) ?
N2 C2 H2 . . 115.3(18) ?
N1 C2 H2 . . 115.6(18) ?
N3 C3 N2 . . 126.83(18) ?
N3 C3 C5 . . 107.31(18) ?
N2 C3 C5 . . 125.86(18) ?
N4 C4 C5 . . 110.24(18) ?
N4 C4 H4 . . 119.6(15) ?
C5 C4 H4 . . 130.1(15) ?
C1 C5 C3 . . 115.47(18) ?
C1 C5 C4 . . 140.06(19) ?
C3 C5 C4 . . 104.47(17) ?
N3 C6 C7 . . 112.75(15) ?
N3 C6 H6A . . 105.8(16) ?
C7 C6 H6A . . 112.1(15) ?
N3 C6 H6B . . 107.8(15) ?
C7 C6 H6B . . 111.9(15) ?
H6A C6 H6B . . 106(2) ?
C12 C7 C8 . . 119.25(18) ?
C12 C7 C6 . . 120.62(17) ?
C8 C7 C6 . . 120.13(17) ?
C9 C8 C7 . . 120.25(19) ?
C9 C8 H8 . . 119.2(14) ?
C7 C8 H8 . . 120.5(14) ?
C10 C9 C8 . . 120.03(19) ?
C10 C9 H9 . . 121.0(18) ?
C8 C9 H9 . . 119.0(18) ?
C11 C10 C9 . . 120.2(2) ?
C11 C10 H10 . . 123(2) ?
C9 C10 H10 . . 117(2) ?
C10 C11 C12 . . 119.65(19) ?
C10 C11 H11 . . 119.8(18) ?
C12 C11 H11 . . 120.5(18) ?
C7 C12 C11 . . 120.61(19) ?
C7 C12 H12 . . 121.6(17) ?
C11 C12 H12 . . 117.8(17) ?
S1 C13 H13A . . 109.4(17) ?
S1 C13 H13B . . 107.5(17) ?
H13A C13 H13B . . 113(3) ?
S1 C13 H13C . . 106(2) ?
H13A C13 H13C . . 105(3) ?
H13B C13 H13C . . 115(3) ?
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
S1 C1 . 1.7400(19) ?
S1 C13 . 1.789(2) ?
N1 C1 . 1.337(3) ?
N1 C2 . 1.358(3) ?
N2 C2 . 1.313(3) ?
N2 C3 . 1.350(3) ?
N3 C3 . 1.346(3) ?
N3 N4 . 1.370(2) ?
N3 C6 . 1.466(2) ?
N4 C4 . 1.320(3) ?
C1 C5 . 1.396(3) ?
C2 H2 . 0.97(3) ?
C3 C5 . 1.406(3) ?
C4 C5 . 1.426(3) ?
C4 H4 . 0.89(2) ?
C6 C7 . 1.510(3) ?
C6 H6A . 0.95(3) ?
C6 H6B . 0.93(3) ?
C7 C12 . 1.390(3) ?
C7 C8 . 1.394(3) ?
C8 C9 . 1.388(3) ?
C8 H8 . 0.91(2) ?
C9 C10 . 1.388(3) ?
C9 H9 . 0.90(3) ?
C10 C11 . 1.385(3) ?
C10 H10 . 0.83(3) ?
C11 C12 . 1.392(3) ?
C11 H11 . 0.86(3) ?
C12 H12 . 0.97(3) ?
C13 H13A . 0.96(3) ?
C13 H13B . 0.95(3) ?
C13 H13C . 1.02(4) ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
C2 H2 S1 1_545 0.97(3) 2.81(3) 3.781(2) 174(2) yes
C13 H13C Cg3 3_666 1.02(4) 2.49(4) 3.455(2) 157(3) 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
C3 N3 N4 C4 . . . . -0.3(2) ?
C6 N3 N4 C4 . . . . -178.65(17) ?
C2 N1 C1 C5 . . . . -0.5(3) ?
C2 N1 C1 S1 . . . . -179.60(15) ?
C13 S1 C1 N1 . . . . -0.32(18) ?
C13 S1 C1 C5 . . . . -179.38(17) ?
C3 N2 C2 N1 . . . . 0.3(3) ?
C1 N1 C2 N2 . . . . 0.2(3) ?
N4 N3 C3 N2 . . . . -179.71(18) ?
C6 N3 C3 N2 . . . . -1.4(3) ?
N4 N3 C3 C5 . . . . 0.2(2) ?
C6 N3 C3 C5 . . . . 178.49(16) ?
C2 N2 C3 N3 . . . . 179.36(19) ?
C2 N2 C3 C5 . . . . -0.6(3) ?
N3 N4 C4 C5 . . . . 0.2(2) ?
N1 C1 C5 C3 . . . . 0.3(3) ?
S1 C1 C5 C3 . . . . 179.39(13) ?
N1 C1 C5 C4 . . . . -179.1(2) ?
S1 C1 C5 C4 . . . . 0.0(3) ?
N3 C3 C5 C1 . . . . -179.69(16) ?
N2 C3 C5 C1 . . . . 0.2(3) ?
N3 C3 C5 C4 . . . . -0.1(2) ?
N2 C3 C5 C4 . . . . 179.84(18) ?
N4 C4 C5 C1 . . . . 179.4(2) ?
N4 C4 C5 C3 . . . . -0.1(2) ?
C3 N3 C6 C7 . . . . -99.9(2) ?
N4 N3 C6 C7 . . . . 78.2(2) ?
N3 C6 C7 C12 . . . . -108.9(2) ?
N3 C6 C7 C8 . . . . 71.1(2) ?
C12 C7 C8 C9 . . . . -0.2(3) ?
C6 C7 C8 C9 . . . . 179.77(18) ?
C7 C8 C9 C10 . . . . 0.1(3) ?
C8 C9 C10 C11 . . . . 0.0(3) ?
C9 C10 C11 C12 . . . . 0.0(3) ?
C8 C7 C12 C11 . . . . 0.2(3) ?
C6 C7 C12 C11 . . . . -179.80(18) ?
C10 C11 C12 C7 . . . . -0.1(3) ?