#------------------------------------------------------------------------------
#$Date: 2023-06-06 07:31:40 +0200 (Tue, 06 Jun 2023) $
#$Revision: 284373 $
#$URL: svn://www.crystallography.net/cod/cif/2/02/27/2022756.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_2022756
loop_
_publ_author_name
'Aliyeva, Vusala A.'
'Aliyeva, Fargana S.'
'Akkurt, Mehmet'
'Yıldırım, Sema Öztürk'
'Bhattarai, Ajaya'
_publ_section_title
;
Synthesis and crystal structure of
catena-poly[[[aqua-{2-[(E)-(1-cyano-2-imino-2-meth-oxy-ethyl-idene)hydrazin-yl]benzene-sulfonato}-sodium]-di-μ-aqua]
dihydrate].
;
_journal_coeditor_code WM5680
_journal_issue 'Pt 5'
_journal_name_full
'Acta crystallographica. Section E, Crystallographic communications'
_journal_page_first 508
_journal_page_last 511
_journal_paper_doi 10.1107/S2056989023003602
_journal_volume 79
_journal_year 2023
_chemical_formula_iupac '[Na (C10 H9 N4 O4 S) (H2 O)3], 2H2 O'
_chemical_formula_moiety 'C10 H15 N4 Na O7 S, 2(H2 O)'
_chemical_formula_sum 'C10 H19 N4 Na O9 S'
_chemical_formula_weight 394.34
_chemical_name_systematic
'catena-Poly[[[aqua{2-[(E)-(1-cyano-2-imino-2-methoxyethylidene)hydrazinyl]benzenesulfonato}sodium]-di-\m-aqua] dihydrate]'
_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 mixed
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-2019/1
_cell_angle_alpha 90
_cell_angle_beta 106.6810(10)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 13.3305(5)
_cell_length_b 6.8212(3)
_cell_length_c 20.9547(8)
_cell_measurement_reflns_used 9914
_cell_measurement_temperature 150(2)
_cell_measurement_theta_max 26.49
_cell_measurement_theta_min 3.15
_cell_volume 1825.23(13)
_computing_cell_refinement
;
SAINT (Bruker, 2007)
;
_computing_data_collection
;
APEX2 (Bruker, 2007)
;
_computing_data_reduction
;
SAINT (Bruker, 2007)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012)
;
_computing_publication_material
;
PLATON (Spek, 2020)
;
_computing_structure_refinement
;
SHELXL2019 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS (Sheldrick, 2008)
;
_diffrn_ambient_temperature 150(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.987
_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 0.0206
_diffrn_reflns_av_unetI/netI 0.0115
_diffrn_reflns_limit_h_max 16
_diffrn_reflns_limit_h_min -16
_diffrn_reflns_limit_k_max 7
_diffrn_reflns_limit_k_min -8
_diffrn_reflns_limit_l_max 26
_diffrn_reflns_limit_l_min -26
_diffrn_reflns_number 27710
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 26.528
_diffrn_reflns_theta_min 2.192
_exptl_absorpt_coefficient_mu 0.251
_exptl_absorpt_correction_T_max 0.967
_exptl_absorpt_correction_T_min 0.926
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause et al., 2015)
;
_exptl_crystal_colour yellow
_exptl_crystal_density_diffrn 1.435
_exptl_crystal_description needle
_exptl_crystal_F_000 824
_exptl_crystal_size_max 0.270
_exptl_crystal_size_mid 0.210
_exptl_crystal_size_min 0.100
_refine_diff_density_max 0.346
_refine_diff_density_min -0.362
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.066
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 227
_refine_ls_number_reflns 3748
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.066
_refine_ls_R_factor_all 0.0321
_refine_ls_R_factor_gt 0.0280
_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^)+(0.0397P)^2^+0.8377P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0771
_refine_ls_wR_factor_ref 0.0808
_reflns_number_gt 3389
_reflns_number_total 3748
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file wm5680sup1.cif
_cod_data_source_block I
_cod_depositor_comments 'Adding full bibliography for 2022756.cif.'
_cod_original_sg_symbol_H-M 'P 21/c'
_cod_database_code 2022756
_cod_database_fobs_code 2022756
_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 0.935
_shelx_estimated_absorpt_t_max 0.975
_shelx_hkl_file
;
3 0 0 53.99 3.00
-3 0 0 52.19 2.60
5 0 0 4377.16 68.89
-5 0 0 4305.97 69.09
-5 0 0 4189.48 68.69
5 0 0 4454.25 69.29
6 0 0 882.61 15.80
6 0 0 870.11 16.20
-6 0 0 848.92 15.50
-6 0 0 866.81 16.10
7 0 0 422.36 9.70
-7 0 0 430.56 9.10
7 0 0 417.36 9.20
-7 0 0 410.26 11.50
8 0 0 319.97 8.40
-8 0 0 293.27 7.50
8 0 0 303.97 7.70
-8 0 0 299.37 8.20
-8 0 0 314.87 9.90
-9 0 0 574.34 12.80
-9 0 0 592.54 12.20
9 0 0 586.94 13.10
9 0 0 573.04 12.40
-9 0 0 570.54 15.20
-10 0 0 9999.00 155.78
10 0 0 9856.51 156.88
-10 0 0 9978.90 156.58
10 0 0 9819.32 156.18
-10 0 0 9528.35 159.18
11 0 0 1082.89 22.60
-11 0 0 1176.88 21.60
11 0 0 1124.89 22.00
-11 0 0 1155.08 25.90
-11 0 0 1124.19 22.30
-12 0 0 65.19 5.80
12 0 0 61.89 5.70
12 0 0 54.89 5.00
-13 0 0 994.80 24.70
13 0 0 1042.40 21.50
-13 0 0 1040.70 21.70
-13 0 0 1057.99 20.90
13 0 0 1064.79 22.50
14 0 0 441.86 12.50
-14 0 0 458.15 12.00
14 0 0 422.06 13.10
-14 0 0 449.86 12.80
-14 0 0 439.86 16.10
-15 0 0 163.98 11.50
15 0 0 158.98 8.00
-15 0 0 179.38 8.60
-15 0 0 167.08 7.90
15 0 0 170.28 8.80
0 -1 0 2.30 1.20
0 1 0 1.40 1.10
-1 -1 0 2680.73 41.10
-1 -1 0 2598.14 41.10
2 -1 0 87.49 2.90
-2 -1 0 98.49 2.90
2 -1 0 92.99 2.60
-2 -1 0 96.79 2.60
2 1 0 91.19 2.70
2 1 0 95.99 2.60
-2 1 0 91.59 3.00
-2 1 0 87.19 2.20
-2 1 0 92.29 2.40
-3 -1 0 2123.79 34.50
3 -1 0 2136.89 34.40
-3 -1 0 2174.08 34.40
3 -1 0 2183.98 35.10
3 1 0 2173.38 34.30
-3 1 0 2116.99 34.20
3 1 0 2143.89 34.40
-3 1 0 2136.49 34.00
-3 1 0 2085.69 34.70
4 -1 0 131.79 3.80
4 -1 0 136.39 4.20
4 -1 0 131.09 4.80
-4 -1 0 134.49 3.90
4 1 0 130.89 3.90
-4 1 0 127.29 4.00
-4 1 0 130.29 3.60
-4 1 0 129.79 4.30
4 1 0 134.99 4.20
5 -1 0 730.73 13.70
-5 -1 0 735.93 13.80
5 -1 0 732.53 13.20
-5 -1 0 738.63 13.40
-5 1 0 721.33 14.10
5 1 0 746.13 13.40
-5 1 0 730.13 12.90
-5 1 0 723.33 13.40
5 1 0 741.03 13.70
6 -1 0 1492.45 25.00
-6 -1 0 1451.05 25.50
-6 -1 0 1435.16 25.00
6 -1 0 1469.05 25.50
-6 1 0 1468.85 25.10
6 1 0 1476.55 25.10
-6 1 0 1473.25 24.60
6 1 0 1478.85 25.40
7 -1 0 478.05 10.10
7 -1 0 483.75 10.70
-7 -1 0 480.45 10.80
-7 -1 0 487.75 10.30
7 1 0 496.95 10.70
-7 1 0 497.35 9.80
-7 1 0 480.25 10.30
7 1 0 483.95 10.30
8 -1 0 352.06 9.10
-8 -1 0 335.17 8.90
8 -1 0 355.86 8.40
-8 -1 0 358.86 8.50
8 1 0 358.36 8.50
-8 1 0 358.86 8.00
8 1 0 342.97 8.90
-8 1 0 350.16 8.60
-8 1 0 336.97 9.70
9 -1 0 1354.76 25.50
9 -1 0 1393.96 24.90
-9 -1 0 1381.46 24.80
-9 -1 0 1393.06 25.40
-9 1 0 1359.06 24.20
-9 1 0 1380.46 24.90
9 1 0 1394.76 25.50
-9 1 0 1365.66 26.50
9 1 0 1389.46 25.00
-10 -1 0 34.40 3.80
10 -1 0 24.40 3.30
10 -1 0 26.50 3.10
-10 -1 0 22.30 3.00
-10 1 0 28.20 3.00
10 1 0 21.00 3.00
-10 1 0 24.00 3.30
10 1 0 33.00 3.80
11 -1 0 123.59 6.00
-11 -1 0 111.09 6.60
-11 -1 0 125.99 6.20
11 -1 0 125.59 6.50
-11 1 0 124.79 5.60
-11 1 0 141.19 8.80
11 1 0 115.79 5.80
11 1 0 115.99 6.40
-11 1 0 120.29 6.20
-12 -1 0 131.09 10.80
-12 -1 0 148.99 6.80
12 -1 0 150.28 7.30
12 -1 0 146.79 6.70
-12 -1 0 152.28 7.50
-12 1 0 147.49 6.30
12 1 0 133.49 7.20
12 1 0 135.19 6.50
-12 1 0 146.49 6.90
-13 -1 0 542.95 14.30
13 -1 0 563.24 13.90
13 -1 0 575.84 14.70
-13 -1 0 549.95 17.80
-13 -1 0 575.64 13.70
-13 1 0 541.35 15.80
13 1 0 543.65 13.80
-13 1 0 574.44 13.10
-13 1 0 550.34 13.70
13 1 0 544.55 14.40
-14 -1 0 479.75 12.70
-14 -1 0 459.25 17.40
14 -1 0 460.65 13.70
14 -1 0 464.05 13.00
-14 -1 0 461.35 13.30
-14 1 0 471.35 12.10
-14 1 0 474.25 15.30
14 1 0 456.55 12.70
14 1 0 471.65 13.50
-14 1 0 474.85 12.70
-15 -1 0 11.50 5.60
-15 -1 0 14.30 4.20
15 -1 0 8.50 3.90
15 -1 0 11.70 3.60
-15 1 0 13.40 3.60
-15 1 0 10.70 3.30
-15 1 0 16.10 5.10
15 1 0 10.90 3.50
15 1 0 13.40 4.00
0 -2 0 1665.03 28.30
2 -2 0 57.89 3.20
-2 -2 0 58.39 2.10
-2 -2 0 56.99 2.30
-2 2 0 57.29 3.70
-3 -2 0 5500.15 86.09
-3 -2 0 5632.34 86.09
3 -2 0 5454.35 85.79
3 -2 0 5307.07 85.59
3 2 0 5399.46 85.49
3 2 0 5595.04 85.49
-4 -2 0 776.32 13.70
4 -2 0 774.22 13.20
4 -2 0 770.62 14.30
-4 -2 0 763.82 13.80
4 -2 0 791.82 13.60
-4 2 0 751.32 12.60
4 2 0 762.52 13.30
-4 2 0 752.22 12.80
-4 2 0 744.03 14.40
4 2 0 775.32 13.30
5 -2 0 881.11 16.10
-5 -2 0 850.71 16.20
5 -2 0 953.10 17.40
-5 -2 0 886.31 16.00
-5 2 0 877.21 15.00
-5 2 0 900.81 16.80
5 2 0 941.31 15.90
5 2 0 888.21 15.70
-5 2 0 882.31 15.30
6 -2 0 640.04 12.80
6 -2 0 636.84 12.30
-6 -2 0 660.73 12.70
-6 -2 0 649.14 13.00
6 -2 0 670.13 14.30
6 2 0 654.83 12.60
-6 2 0 678.93 11.80
6 2 0 654.53 12.40
-6 2 0 676.53 13.40
-6 2 0 642.84 12.10
-7 -2 0 3307.87 54.09
7 -2 0 3367.06 54.49
7 -2 0 3275.67 53.79
7 -2 0 3307.07 56.09
-7 -2 0 3304.67 54.49
-7 2 0 3229.38 54.79
-7 2 0 3315.67 52.99
-7 2 0 3286.27 53.49
7 2 0 3361.26 53.89
7 2 0 3370.16 54.19
-8 -2 0 563.34 11.90
-8 -2 0 551.34 12.30
8 -2 0 559.04 11.60
8 -2 0 535.15 12.20
8 2 0 546.35 11.60
8 2 0 561.94 12.00
-8 2 0 556.74 10.80
-8 2 0 549.25 11.30
-8 2 0 572.74 12.70
9 -2 0 1275.87 23.80
9 -2 0 1268.07 23.00
-9 -2 0 1270.77 23.70
-9 -2 0 1245.78 23.00
-9 2 0 1224.48 23.90
-9 2 0 1261.87 21.90
9 2 0 1253.27 22.90
-9 2 0 1249.88 22.50
9 2 0 1250.27 23.30
-10 -2 0 353.66 9.50
10 -2 0 351.36 10.10
-10 -2 0 377.76 10.30
10 -2 0 338.27 9.30
10 2 0 330.97 9.00
-10 2 0 363.46 8.40
-10 2 0 352.86 9.00
10 2 0 339.27 9.50
-10 2 0 342.77 10.30
11 -2 0 473.25 11.50
11 -2 0 461.95 12.20
-11 -2 0 452.85 11.60
-11 -2 0 436.26 12.10
-11 2 0 448.56 12.50
-11 2 0 444.86 10.30
-11 2 0 467.45 11.10
11 2 0 445.46 11.60
11 2 0 459.65 11.30
-12 -2 0 154.98 7.00
-12 -2 0 164.08 7.80
12 -2 0 160.58 7.00
12 -2 0 149.69 7.60
-12 2 0 152.98 6.00
12 2 0 149.49 7.10
-12 2 0 157.08 6.60
12 2 0 153.28 6.70
-12 2 0 174.28 8.40
13 -2 0 893.01 20.40
-13 -2 0 920.31 20.10
-13 -2 0 928.21 19.30
13 -2 0 917.81 19.50
-13 2 0 917.01 18.60
-13 2 0 913.81 17.90
13 2 0 884.71 19.50
13 2 0 865.31 19.00
-13 2 0 854.41 20.30
-14 -2 0 236.58 13.40
14 -2 0 243.88 9.20
-14 -2 0 240.38 9.20
14 -2 0 264.47 10.40
-14 -2 0 268.47 10.30
14 2 0 248.88 8.90
14 2 0 265.57 9.60
-14 2 0 259.67 8.10
-14 2 0 251.17 10.40
-14 2 0 254.27 8.70
15 -2 0 275.07 10.10
-15 -2 0 242.28 14.80
-15 -2 0 271.97 10.10
-15 -2 0 273.87 10.80
15 -2 0 282.27 11.20
15 2 0 291.97 9.90
-15 2 0 270.07 11.40
15 2 0 302.17 10.30
-15 2 0 274.07 9.20
-15 2 0 275.87 8.60
0 -3 0 -0.30 2.00
1 -3 0 626.64 13.20
-1 -3 0 635.44 13.80
-1 3 0 643.54 13.60
2 -3 0 98.89 4.60
-2 3 0 93.89 5.20
3 -3 0 228.28 4.60
-3 -3 0 243.08 5.20
3 -3 0 248.08 6.70
3 -3 0 236.28 4.90
-3 -3 0 235.78 5.30
-3 3 0 243.58 7.40
4 -3 0 2375.86 39.80
4 -3 0 2344.07 38.00
-4 -3 0 2404.76 38.60
4 -3 0 2399.16 38.30
-4 -3 0 2327.17 38.60
-4 3 0 2400.76 40.60
5 -3 0 537.55 10.60
5 -3 0 541.15 11.60
5 -3 0 529.75 10.10
-5 -3 0 545.35 10.70
-5 -3 0 534.45 10.80
-5 3 0 551.84 12.20
6 -3 0 1483.75 26.40
-6 -3 0 1457.15 25.30
6 -3 0 1454.15 25.00
-6 -3 0 1498.35 25.10
6 3 0 1299.47 23.90
6 3 0 1446.96 24.10
-6 3 0 1471.85 26.40
7 -3 0 82.89 4.50
-7 -3 0 76.39 4.60
7 -3 0 101.49 5.70
-7 -3 0 74.39 4.20
7 -3 0 83.19 3.90
-7 3 0 85.79 3.00
-7 3 0 83.19 2.80
7 3 0 83.59 3.60
-7 3 0 91.09 5.10
7 3 0 73.89 3.60
-8 -3 0 3.60 2.20
8 -3 0 3.60 2.90
8 -3 0 1.90 1.90
-8 -3 0 6.20 2.50
8 -3 0 2.00 2.20
-8 3 0 3.40 2.50
-8 3 0 1.20 1.40
-8 3 0 2.80 1.60
8 3 0 2.00 1.70
8 3 0 4.60 1.90
-9 -3 0 1699.03 29.90
9 -3 0 1676.03 30.30
-9 -3 0 1677.03 30.40
9 -3 0 1697.83 29.50
-9 3 0 1676.63 28.20
-9 3 0 1661.33 27.80
9 3 0 1697.73 29.30
-9 3 0 1662.63 31.00
9 3 0 1650.73 29.00
10 -3 0 135.49 6.50
-10 -3 0 138.29 6.20
-10 -3 0 125.59 6.60
10 -3 0 129.39 5.80
10 3 0 124.39 5.30
-10 3 0 135.79 6.80
10 3 0 139.59 5.80
-10 3 0 130.39 4.90
-10 3 0 136.69 4.50
11 -3 0 -2.50 2.70
-11 -3 0 3.70 2.80
-11 -3 0 -0.90 3.00
11 -3 0 -1.20 2.40
-11 3 0 -0.40 2.10
11 3 0 0.90 2.30
11 3 0 -1.30 2.10
-11 3 0 -3.90 1.70
-11 3 0 3.40 3.00
12 -3 0 39.70 4.20
-12 -3 0 47.50 4.80
12 -3 0 49.50 5.00
-12 -3 0 38.50 4.10
12 3 0 41.00 3.80
-12 3 0 45.50 5.70
12 3 0 45.70 4.20
-12 3 0 49.60 3.70
-12 3 0 43.90 4.10
13 -3 0 266.47 9.30
13 -3 0 255.97 10.10
-13 -3 0 278.67 10.30
-13 -3 0 270.47 9.50
-13 3 0 272.67 7.40
13 3 0 277.67 8.80
-13 3 0 271.97 8.00
13 3 0 291.17 9.10
-13 3 0 265.57 10.20
14 -3 0 77.39 6.30
-14 -3 0 95.29 7.30
14 -3 0 77.49 7.20
-14 -3 0 86.69 6.70
14 3 0 91.19 5.50
-14 3 0 76.99 6.70
14 3 0 97.09 6.10
-14 3 0 86.69 4.80
-14 3 0 77.59 5.10
0 -4 0 8174.78 131.39
-1 -4 0 1747.63 32.10
1 -4 0 1709.23 31.30
-2 -4 0 550.94 13.80
2 -4 0 553.34 12.70
-2 4 0 580.44 13.50
3 -4 0 508.45 11.70
-3 -4 0 512.75 9.50
-3 -4 0 505.45 9.50
-3 4 0 518.05 12.70
-4 -4 0 162.18 4.70
4 -4 0 172.28 6.00
4 -4 0 162.68 4.00
4 -4 0 155.98 4.30
-4 -4 0 165.68 4.60
-4 4 0 153.38 6.80
5 -4 0 623.64 11.90
5 -4 0 621.94 11.40
5 -4 0 637.24 13.50
-5 -4 0 611.34 12.30
-5 -4 0 632.94 12.20
-5 4 0 635.24 14.50
6 -4 0 49.00 3.60
-6 -4 0 53.19 3.70
6 -4 0 46.50 3.20
-6 -4 0 50.49 3.90
6 -4 0 51.99 4.50
-6 4 0 47.80 5.10
7 -4 0 116.69 5.10
-7 -4 0 110.79 5.20
-7 -4 0 126.09 5.20
7 -4 0 114.99 6.50
-7 4 0 118.29 6.50
8 -4 0 199.08 6.10
8 -4 0 189.68 6.70
-8 -4 0 190.28 6.60
8 -4 0 203.58 8.30
-8 -4 0 191.28 7.00
-8 4 0 187.38 8.00
9 -4 0 -2.50 3.00
9 -4 0 -0.40 2.20
-9 -4 0 -1.60 2.40
-9 -4 0 -3.30 2.60
9 -4 0 -1.10 2.50
9 4 0 1.60 1.60
9 4 0 3.00 1.60
-9 4 0 2.90 2.60
10 -4 0 388.66 10.90
10 -4 0 416.96 13.00
10 -4 0 393.46 10.20
-10 -4 0 403.86 10.70
-10 -4 0 403.36 11.20
10 4 0 394.26 8.80
10 4 0 394.26 8.90
-10 4 0 404.46 12.10
11 -4 0 27.30 3.90
-11 -4 0 18.00 3.40
-11 -4 0 23.50 4.00
11 -4 0 28.10 3.60
-11 4 0 22.50 3.90
11 4 0 28.00 2.70
11 4 0 31.60 2.90
-12 -4 0 15.40 3.80
12 -4 0 7.30 3.00
-12 -4 0 10.50 3.30
12 -4 0 8.90 3.50
12 4 0 7.90 2.30
-12 4 0 11.80 3.50
12 4 0 7.40 2.30
-13 -4 0 330.07 10.70
13 -4 0 321.57 10.30
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15 -2 -8 163.88 8.60
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14 -2 -8 -0.90 2.80
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9 -2 -8 235.38 9.70
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9 -2 -8 229.28 7.90
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6 -2 -8 4917.71 78.89
6 -2 -8 4930.71 79.99
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5 -2 -8 354.26 8.70
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4 -2 -8 4297.27 70.09
4 -2 -8 4372.26 71.19
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3 -2 -8 1505.65 25.40
3 -2 -8 1422.76 26.40
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2 -2 -8 9075.49 141.49
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1 -2 -8 1546.65 28.50
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1 -2 -8 1553.64 26.40
1 -2 -8 1559.94 27.00
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1 -2 8 4445.76 70.89
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5 -2 8 27.50 2.80
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8 -1 -9 48.70 4.30
8 -1 -9 49.10 3.70
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8 -1 -9 51.29 5.80
-8 -1 9 50.29 4.50
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8 1 -9 52.79 3.50
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7 -1 -9 23.10 2.90
-7 -1 9 19.40 2.40
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-7 -1 9 13.10 2.60
7 -1 -9 19.60 3.30
7 -1 -9 19.30 2.40
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7 1 -9 19.00 2.10
7 1 -9 24.20 2.70
-6 -1 9 745.03 15.00
6 -1 -9 754.42 16.40
-6 -1 9 792.32 16.30
6 -1 -9 738.63 14.10
6 -1 -9 747.63 15.10
-6 -1 9 748.93 14.00
6 1 -9 750.62 14.40
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-5 -1 9 364.26 7.90
5 -1 -9 354.26 8.00
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5 -1 -9 362.66 8.90
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5 -1 -9 373.36 9.70
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5 1 -9 373.86 7.60
5 1 -9 367.86 8.20
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4 -1 -9 744.73 13.70
-4 -1 9 739.53 14.20
4 -1 -9 720.53 14.50
-4 -1 9 732.43 13.50
4 -1 -9 766.82 15.10
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4 1 -9 751.82 13.70
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4 1 -9 760.52 13.20
3 -1 -9 306.97 8.10
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3 -1 -9 317.87 7.80
-3 -1 9 321.97 7.20
3 -1 -9 308.37 7.10
3 1 -9 310.87 6.90
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3 1 -9 303.07 6.40
-2 -1 9 70.49 3.20
2 -1 -9 67.99 4.40
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2 -1 -9 66.39 4.00
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2 -1 -9 68.09 3.70
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2 1 -9 60.29 2.80
2 1 -9 67.89 3.20
2 1 -9 64.69 3.90
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1 -1 -9 11.80 2.10
1 -1 -9 13.60 2.70
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1 -1 -9 11.10 2.10
1 1 -9 12.60 1.60
1 1 -9 16.30 1.80
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1 1 -9 18.10 2.00
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0 -1 -9 474.35 10.80
0 -1 -9 458.05 10.00
0 -1 9 459.05 9.20
0 -1 9 464.75 9.70
0 -1 -9 464.35 9.60
0 1 9 461.55 10.90
0 1 -9 468.85 8.70
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-1 -1 -9 9.10 2.80
-1 -1 -9 8.90 2.10
-1 -1 -9 8.60 2.10
1 -1 9 11.00 1.90
-1 1 -9 9.90 1.70
1 1 9 11.00 2.30
-1 1 -9 9.60 1.70
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2 -1 9 0.40 1.80
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-2 -1 -9 0.80 1.90
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-3 -1 -9 96.09 4.50
3 -1 9 87.29 4.30
-3 -1 -9 89.59 5.40
-3 -1 -9 87.29 4.50
3 -1 9 88.19 4.20
-3 1 -9 91.89 3.80
3 1 9 92.99 4.50
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3 1 9 87.79 4.60
-4 -1 -9 32.50 3.00
-4 -1 -9 36.00 3.70
4 -1 9 35.00 3.50
4 -1 9 27.20 2.90
-4 1 -9 27.80 2.90
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4 1 9 27.90 2.90
-4 1 -9 32.80 3.10
-5 -1 -9 58.89 4.30
5 -1 9 49.80 4.10
5 -1 9 50.09 4.00
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-5 1 -9 51.29 3.60
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5 1 9 49.40 4.30
6 -1 9 230.08 7.30
-6 -1 -9 222.58 7.40
-6 -1 -9 215.58 7.10
6 -1 9 226.08 7.20
-6 1 -9 215.08 6.50
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-6 1 -9 224.88 6.40
-7 -1 -9 127.39 5.90
-7 -1 -9 124.19 6.10
7 -1 9 125.49 5.80
7 -1 9 122.99 6.00
-7 1 -9 122.69 5.10
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-8 -1 -9 311.17 9.40
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-8 -1 -9 312.27 9.20
8 -1 9 307.67 9.50
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-8 1 -9 315.37 8.40
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-9 -1 -9 -1.90 2.80
-9 -1 -9 -1.40 2.50
9 -1 9 1.80 2.80
9 -1 9 1.90 2.90
-9 1 -9 -2.20 2.20
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-10 -1 -9 14.70 3.60
-10 -1 -9 13.50 3.20
10 -1 9 18.80 3.60
10 -1 9 7.90 3.10
10 1 9 20.70 3.70
-10 1 -9 14.50 3.30
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-10 1 -9 18.90 3.10
11 -1 9 270.47 10.00
-11 -1 -9 269.27 9.80
11 -1 9 267.97 9.80
-11 -1 -9 261.07 9.20
-11 1 -9 278.17 11.20
-11 1 -9 269.07 8.50
11 1 9 275.87 9.80
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-11 1 -9 257.27 8.70
-12 -1 -9 5.70 3.30
12 -1 9 0.60 3.20
-12 -1 -9 3.70 3.20
12 -1 9 6.40 3.50
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12 1 9 5.10 3.10
-12 1 -9 -1.80 3.00
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-12 1 -9 6.00 2.80
13 -1 9 13.30 3.90
-13 -1 -9 0.60 3.30
13 -1 9 0.50 3.20
-13 -1 -9 9.00 3.60
-13 1 -9 7.50 3.10
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-16 -2 9 6.20 3.60
16 -2 -9 3.00 3.60
16 -2 -9 1.70 3.30
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16 2 -9 3.40 2.80
16 2 -9 2.50 2.40
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15 -2 -9 58.19 5.70
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15 -2 -9 53.19 5.00
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15 2 -9 69.69 5.10
14 -2 -9 3.30 2.80
14 -2 -9 5.90 3.40
-14 -2 9 1.60 3.20
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14 2 -9 2.90 2.40
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14 2 -9 5.10 2.70
-13 -2 9 18.10 4.00
-13 -2 9 19.10 3.40
-13 -2 9 7.30 4.60
13 -2 -9 25.60 4.10
13 -2 -9 16.40 3.20
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13 2 -9 22.40 3.00
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12 -2 -9 91.79 6.50
12 -2 -9 90.29 5.60
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12 2 -9 92.59 5.50
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12 2 -9 93.79 4.90
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-11 -2 9 188.68 10.10
11 -2 -9 190.58 6.90
-11 -2 9 192.68 7.00
11 -2 -9 198.78 10.80
11 -2 -9 187.78 7.90
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11 2 -9 180.58 6.80
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10 -2 -9 3.40 2.70
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10 -2 -9 4.00 3.60
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10 2 -9 4.00 2.20
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9 -2 -9 108.39 7.30
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9 -2 -9 106.09 5.90
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9 -2 -9 105.39 5.00
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8 -2 -9 5.70 3.50
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8 -2 -9 -3.30 2.10
8 -2 -9 -1.10 1.90
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7 -2 -9 350.96 10.30
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7 -2 -9 332.07 8.20
7 -2 -9 341.47 9.10
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6 -2 -9 65.99 4.50
6 -2 -9 71.19 5.20
6 -2 -9 70.19 3.90
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6 2 -9 70.49 3.30
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6 2 -9 67.39 2.90
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5 -2 -9 65.89 4.40
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5 -2 -9 60.09 3.80
5 -2 -9 81.69 5.20
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5 2 -9 73.89 2.60
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4 -2 -9 6.20 2.10
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3 -2 -9 2.90 2.10
3 -2 -9 3.00 2.50
3 -2 -9 3.30 1.90
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2 -2 -9 2371.56 39.80
2 -2 -9 2348.67 41.00
2 -2 -9 2361.56 39.00
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1 -2 -9 672.73 12.80
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1 -2 -9 664.83 13.40
1 -2 -9 669.53 14.70
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0 -2 -9 203.98 6.30
0 -2 -9 203.08 5.90
0 -2 -9 200.68 7.50
0 -2 9 214.98 5.10
0 -2 9 215.98 5.50
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1 -2 9 55.09 3.10
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1 -2 9 50.69 3.20
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1 2 9 46.10 3.50
2 -2 9 332.97 7.40
-2 -2 -9 335.37 8.50
2 -2 9 328.87 7.70
-2 -2 -9 349.57 8.30
-2 -2 -9 336.57 10.10
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2 2 9 335.37 8.00
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3 -2 9 42.10 3.30
3 -2 9 48.00 3.40
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4 -2 9 2.00 1.90
-4 -2 -9 1.90 2.70
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5 -2 9 9.30 2.40
5 -2 9 13.90 2.60
-5 -2 -9 10.80 2.70
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6 -2 9 15.40 2.80
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6 -2 9 15.70 2.90
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8 -2 9 48.40 5.00
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9 -2 9 150.88 7.00
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10 -2 9 0.60 2.80
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12 -2 9 21.00 4.00
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15 -3 -9 8.00 3.20
15 -3 -9 12.10 3.80
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14 -3 -9 18.30 3.70
14 -3 -9 27.40 4.40
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13 -3 -9 35.40 5.80
13 -3 -9 24.40 4.20
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13 -3 -9 20.20 3.50
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12 -3 -9 33.90 3.80
12 -3 -9 33.90 5.70
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12 -3 -9 44.00 4.80
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11 -3 -9 122.29 10.00
11 -3 -9 134.49 7.20
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10 -3 -9 60.09 7.30
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9 -3 -9 2.70 2.20
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8 -3 -9 8.00 2.70
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7 -3 -9 25.10 3.20
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6 -3 -9 22.10 2.90
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6 -3 -9 21.00 2.50
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5 -3 -9 71.59 3.90
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5 -3 -9 73.49 4.60
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4 -3 -9 90.09 4.70
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3 -3 -9 45.90 5.00
3 -3 -9 55.49 3.60
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2 -3 -9 558.94 12.00
2 -3 -9 541.75 13.70
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2 -3 -9 566.34 11.30
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1 -3 -9 6.70 2.90
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1 -3 -9 6.40 2.20
1 -3 -9 5.50 2.00
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2 -3 9 4.30 1.60
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3 -3 9 5.90 1.90
3 -3 9 7.90 1.90
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0 -2 -11 81.09 5.60
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1 -2 11 21.20 2.40
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2 -2 11 9.40 2.20
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11 -3 -11 125.89 7.20
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9 -3 -11 653.93 15.50
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4 -2 -25 6.60 3.00
4 -2 -25 1.90 3.20
4 -2 -25 -6.40 4.00
-4 -2 25 0.90 3.60
-4 -2 25 0.60 3.10
-4 2 25 4.60 3.40
-4 2 25 2.70 3.80
-4 2 25 6.90 3.80
4 2 -25 0.10 1.60
-3 -2 25 -1.40 3.00
3 -2 -25 0.10 2.80
-3 -2 25 7.10 3.90
3 -2 -25 2.20 4.40
3 -2 -25 -2.40 3.00
-3 2 25 7.60 3.70
3 2 -25 1.80 1.60
3 2 -25 0.90 1.70
-3 2 25 1.60 3.40
-2 -2 25 8.80 3.70
2 -2 -25 9.00 3.20
-2 -2 25 4.60 3.30
2 -2 -25 -2.40 3.60
2 -2 -25 4.40 3.50
2 2 -25 4.50 1.80
2 2 -25 3.50 1.60
-2 2 25 11.80 3.90
-2 2 25 12.30 3.90
-7 0 26 35.30 5.00
-6 0 26 307.77 11.90
6 0 -26 393.66 15.70
-6 0 26 350.66 11.50
-6 0 26 344.67 12.50
6 0 -26 332.87 9.60
6 0 -26 319.37 10.50
-5 0 26 306.47 10.80
5 0 -26 302.87 9.00
-5 0 26 273.97 11.00
-5 0 26 301.17 11.70
5 0 -26 352.66 14.80
5 0 -26 294.07 9.90
4 0 -26 59.69 4.90
-4 0 26 75.69 6.60
-4 0 26 53.79 6.10
-4 0 26 68.99 7.20
4 0 -26 55.79 5.30
-3 0 26 43.50 5.00
-3 0 26 38.10 5.30
3 0 -26 41.10 3.90
3 0 -26 53.69 4.90
-6 -1 26 11.50 3.50
-6 1 26 16.80 4.20
-5 -1 26 42.70 5.50
-5 -1 26 44.70 4.90
5 -1 -26 45.90 5.00
5 -1 -26 72.69 9.50
5 -1 -26 56.69 5.50
-5 -1 26 39.60 5.40
5 1 -26 45.20 4.70
-5 1 26 51.19 6.80
5 1 -26 51.99 4.30
-5 1 26 68.29 7.00
-5 1 26 59.29 5.40
4 -1 -26 39.50 5.90
-4 -1 26 35.20 4.10
-4 1 26 31.60 5.00
0 0 0 0.00 0.00
_computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)'
;
_shelx_hkl_checksum 27767
_shelx_res_file
;
TITL PA60_a.res in P2(1)/c
PA60_A.res
created by SHELXL-2019/1 at 23:50:14 on 24-Mar-2023
CELL 0.71073 13.3305 6.8212 20.9547 90.000 106.681 90.000
ZERR 4.00 0.0005 0.0003 0.0008 0.000 0.001 0.000
LATT 1
SYMM - X, 1/2 + Y, 1/2 - Z
SFAC C H N O S NA
UNIT 40 76 16 36 4 4
SIZE 0.100 0.210 0.270
TEMP -123.00
MERG 2
FMAP 2
PLAN 0
L.S. 24
BOND $H
LIST 4
CONF
ACTA
EQIV $3 x, y+1, z
HTAB O5 S1_$3
HTAB O5 O4_$3
EQIV $4 -x, y+1/2, -z+1/2
HTAB O5 O6_$4
HTAB O6 O5
HTAB O6 O3
EQIV $5 x, y-1, z
HTAB O7 O5_$5
EQIV $6 x-1, y, z
HTAB O7 N4_$6
EQIV $2 -x, -y+1, -z+1
HTAB O8 O3_$2
EQIV $1 -x, -y, -z+1
HTAB O8 O2_$1
HTAB O9 O6
EQIV $7 x+1, y, z
HTAB N4 O8_$7
WGHT 0.039700 0.837700
FVAR 0.78038
NA1 6 0.016328 0.248851 0.502255 11.00000 0.02258 0.01846 =
0.02458 0.00084 0.01122 0.00087
S1 5 0.240442 0.247655 0.435226 11.00000 0.01257 0.01943 =
0.02187 0.00011 0.00653 -0.00042
O1 4 0.645428 0.035480 0.266602 11.00000 0.02678 0.04987 =
0.02086 -0.00169 0.01105 0.00967
O2 4 0.168426 0.184778 0.471276 11.00000 0.01931 0.04277 =
0.03535 0.00606 0.01398 -0.00458
O3 4 0.217724 0.442901 0.406480 11.00000 0.02192 0.02367 =
0.02670 0.00426 0.00275 0.00239
O4 4 0.249434 0.103531 0.385471 11.00000 0.01631 0.03258 =
0.03614 -0.01513 0.00338 -0.00056
O5 4 0.050483 0.956380 0.314891 11.00000 0.02289 0.03346 =
0.01920 0.00119 0.00253 -0.00519
AFIX 3
H5A 2 0.111073 1.003570 0.332701 11.00000 -1.50000
H5B 2 0.026423 0.994300 0.274741 11.00000 -1.50000
AFIX 0
O6 4 0.025117 0.559766 0.317949 11.00000 0.02862 0.02755 =
0.02293 0.00094 0.00071 0.00141
AFIX 3
H6A 2 0.036537 0.682516 0.319429 11.00000 -1.50000
H6B 2 0.083707 0.512606 0.340269 11.00000 -1.50000
AFIX 0
O7 4 -0.054152 0.002747 0.417562 11.00000 0.01718 0.02557 =
0.02177 0.00146 0.00632 0.00302
AFIX 3
H7A 2 -0.029422 -0.003553 0.384492 11.00000 -1.50000
H7B 2 -0.116822 0.035287 0.397482 11.00000 -1.50000
AFIX 0
O8 4 -0.156766 0.248144 0.518097 11.00000 0.02870 0.02371 =
0.03158 -0.00005 0.01467 0.00120
AFIX 3
H8A 2 -0.183026 0.329914 0.539397 11.00000 -1.50000
H8B 2 -0.170926 0.135404 0.530527 11.00000 -1.50000
AFIX 0
O9 4 -0.073347 0.489828 0.418478 11.00000 0.03521 0.02400 =
0.03049 0.00056 0.01261 -0.00429
AFIX 3
H9A 2 -0.044937 0.508569 0.387489 11.00000 -1.50000
H9B 2 -0.120247 0.402548 0.405278 11.00000 -1.50000
AFIX 0
N1 3 0.456953 0.192226 0.411793 11.00000 0.01394 0.02015 =
0.01827 -0.00093 0.00518 -0.00103
AFIX 3
H1N 2 0.394133 0.153936 0.384683 11.00000 -1.20000
AFIX 0
N2 3 0.546485 0.179688 0.397134 11.00000 0.01700 0.01726 =
0.02263 0.00341 0.00849 0.00199
N3 3 0.376525 0.027049 0.249944 11.00000 0.03384 0.05532 =
0.03077 -0.00773 0.00593 -0.00530
N4 3 0.739364 0.143908 0.370310 11.00000 0.02153 0.05806 =
0.02136 0.00057 0.00875 0.00787
AFIX 3
H4N 2 0.728594 0.183478 0.410070 11.00000 -1.20000
AFIX 0
C1 1 0.458898 0.237868 0.477515 11.00000 0.01752 0.01249 =
0.01800 0.00132 0.00528 -0.00116
C2 1 0.554358 0.257969 0.526817 11.00000 0.01721 0.01907 =
0.02334 0.00108 0.00380 -0.00147
AFIX 43
H2 2 0.618229 0.240330 0.515954 11.00000 -1.20000
AFIX 0
C3 1 0.556033 0.303504 0.591410 11.00000 0.02586 0.02145 =
0.02106 0.00087 -0.00048 -0.00393
AFIX 43
H3 2 0.621321 0.316534 0.624649 11.00000 -1.20000
AFIX 0
C4 1 0.463816 0.330423 0.608376 11.00000 0.03723 0.02240 =
0.01652 -0.00093 0.00762 -0.00182
AFIX 43
H4 2 0.465840 0.363154 0.652795 11.00000 -1.20000
AFIX 0
C5 1 0.368620 0.309150 0.559940 11.00000 0.02696 0.01954 =
0.02296 0.00082 0.01250 0.00030
AFIX 43
H5 2 0.305188 0.326402 0.571371 11.00000 -1.20000
AFIX 0
C6 1 0.365310 0.262709 0.494700 11.00000 0.01689 0.01414 =
0.01940 0.00135 0.00589 -0.00035
C7 1 0.548463 0.122210 0.338552 11.00000 0.02084 0.02196 =
0.02021 0.00279 0.00786 0.00303
C8 1 0.653353 0.104367 0.327864 11.00000 0.02365 0.03336 =
0.02200 0.00530 0.01106 0.00826
C9 1 0.455149 0.067595 0.287284 11.00000 0.02754 0.02986 =
0.02144 -0.00084 0.01182 0.00185
C10 1 0.744034 0.002278 0.252224 11.00000 0.03170 0.08260 =
0.02732 -0.00139 0.01547 0.01885
AFIX 137
H10C 2 0.730573 -0.048535 0.206797 11.00000 -1.50000
H10D 2 0.785594 -0.093168 0.283906 11.00000 -1.50000
H10E 2 0.782662 0.126071 0.256239 11.00000 -1.50000
AFIX 0
HKLF 4
REM PA60_a.res in P2(1)/c
REM wR2 = 0.0808, GooF = S = 1.066, Restrained GooF = 1.066 for all data
REM R1 = 0.0280 for 3389 Fo > 4sig(Fo) and 0.0321 for all 3748 data
REM 227 parameters refined using 0 restraints
END
WGHT 0.0397 0.8377
REM Highest difference peak 0.346, deepest hole -0.362, 1-sigma level 0.041
Q1 1 0.1651 0.2862 0.4917 11.00000 0.05 0.35
Q2 1 0.3108 0.2533 0.4699 11.00000 0.05 0.34
Q3 1 0.5976 0.1104 0.3288 11.00000 0.05 0.31
Q4 1 0.2404 0.0775 0.4168 11.00000 0.05 0.30
Q5 1 0.4111 0.2418 0.4875 11.00000 0.05 0.28
Q6 1 0.5062 0.2513 0.4981 11.00000 0.05 0.27
Q7 1 0.5490 0.2956 0.5569 11.00000 0.05 0.23
Q8 1 -0.1510 0.4867 0.3862 11.00000 0.05 0.23
Q9 1 0.3965 0.1016 0.2925 11.00000 0.05 0.22
Q10 1 0.4188 0.3546 0.5800 11.00000 0.05 0.21
Q11 1 0.5033 0.0929 0.3129 11.00000 0.05 0.20
Q12 1 0.3728 0.2774 0.5279 11.00000 0.05 0.20
Q13 1 0.2280 0.3683 0.4186 11.00000 0.05 0.20
Q14 1 0.5121 0.2751 0.6010 11.00000 0.05 0.20
Q15 1 0.5069 0.3547 0.5906 11.00000 0.05 0.20
Q16 1 0.2049 0.2133 0.4567 11.00000 0.05 0.20
Q17 1 0.4585 0.2150 0.4505 11.00000 0.05 0.19
Q18 1 0.1736 0.4379 0.3938 11.00000 0.05 0.18
Q19 1 0.4208 0.2717 0.5860 11.00000 0.05 0.18
Q20 1 0.5060 0.1932 0.4005 11.00000 0.05 0.17
;
_shelx_res_checksum 7338
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
Na Na1 0.01633(4) 0.24885(7) 0.50226(3) 0.02094(13) Uani d 1 . .
S S1 0.24044(2) 0.24765(4) 0.43523(2) 0.01763(9) Uani d 1 . .
O O1 0.64543(8) 0.03548(17) 0.26660(5) 0.0316(2) Uani d 1 . .
O O2 0.16843(7) 0.18478(17) 0.47128(5) 0.0312(2) Uani d 1 . .
O O3 0.21772(7) 0.44290(14) 0.40648(5) 0.0250(2) Uani d 1 . .
O O4 0.24943(7) 0.10353(15) 0.38547(5) 0.0292(2) Uani d 1 . .
O O5 0.05048(7) 0.95638(15) 0.31489(4) 0.0259(2) Uani d 1 . .
H H5A 0.111073 1.003570 0.332701 0.039 Uiso d 1 . .
H H5B 0.026423 0.994300 0.274741 0.039 Uiso d 1 . .
O O6 0.02512(8) 0.55977(15) 0.31795(5) 0.0278(2) Uani d 1 . .
H H6A 0.036537 0.682516 0.319429 0.042 Uiso d 1 . .
H H6B 0.083707 0.512606 0.340269 0.042 Uiso d 1 . .
O O7 -0.05415(7) 0.00275(14) 0.41756(4) 0.0214(2) Uani d 1 . .
H H7A -0.029422 -0.003553 0.384492 0.032 Uiso d 1 . .
H H7B -0.116822 0.035287 0.397482 0.032 Uiso d 1 . .
O O8 -0.15677(8) 0.24814(14) 0.51810(5) 0.0267(2) Uani d 1 . .
H H8A -0.183026 0.329914 0.539397 0.040 Uiso d 1 . .
H H8B -0.170926 0.135404 0.530527 0.040 Uiso d 1 . .
O O9 -0.07335(8) 0.48983(15) 0.41848(5) 0.0292(2) Uani d 1 . .
H H9A -0.044937 0.508569 0.387489 0.044 Uiso d 1 . .
H H9B -0.120247 0.402548 0.405278 0.044 Uiso d 1 . .
N N1 0.45695(8) 0.19223(16) 0.41179(5) 0.0173(2) Uani d 1 . .
H H1N 0.394133 0.153936 0.384683 0.021 Uiso d 1 . .
N N2 0.54648(8) 0.17969(16) 0.39713(5) 0.0184(2) Uani d 1 . .
N N3 0.37653(11) 0.0270(2) 0.24994(7) 0.0407(3) Uani d 1 . .
N N4 0.73936(9) 0.1439(2) 0.37031(6) 0.0331(3) Uani d 1 . .
H H4N 0.728594 0.183478 0.410070 0.040 Uiso d 1 . .
C C1 0.45890(9) 0.23787(17) 0.47751(6) 0.0160(2) Uani d 1 . .
C C2 0.55436(10) 0.25797(18) 0.52682(7) 0.0203(3) Uani d 1 . .
H H2 0.618229 0.240330 0.515954 0.024 Uiso calc 1 . .
C C3 0.55603(11) 0.3035(2) 0.59141(6) 0.0243(3) Uani d 1 . .
H H3 0.621321 0.316534 0.624649 0.029 Uiso calc 1 . .
C C4 0.46382(11) 0.3304(2) 0.60838(6) 0.0254(3) Uani d 1 . .
H H4 0.465840 0.363154 0.652795 0.030 Uiso calc 1 . .
C C5 0.36862(10) 0.30915(19) 0.55994(6) 0.0220(3) Uani d 1 . .
H H5 0.305188 0.326402 0.571371 0.026 Uiso calc 1 . .
C C6 0.36531(9) 0.26271(17) 0.49470(6) 0.0167(2) Uani d 1 . .
C C7 0.54846(10) 0.12221(19) 0.33855(6) 0.0206(3) Uani d 1 . .
C C8 0.65335(10) 0.1044(2) 0.32786(6) 0.0254(3) Uani d 1 . .
C C9 0.45515(11) 0.0676(2) 0.28728(6) 0.0253(3) Uani d 1 . .
C C10 0.74403(13) 0.0023(3) 0.25222(8) 0.0457(5) Uani d 1 . .
H H10C 0.730573 -0.048535 0.206797 0.069 Uiso calc 1 . .
H H10D 0.785594 -0.093168 0.283906 0.069 Uiso calc 1 . .
H H10E 0.782662 0.126071 0.256239 0.069 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
Na1 0.0226(3) 0.0185(3) 0.0246(3) 0.00087(19) 0.0112(2) 0.00084(19)
S1 0.01257(15) 0.01943(17) 0.02187(16) -0.00042(10) 0.00653(12) 0.00011(11)
O1 0.0268(5) 0.0499(7) 0.0209(5) 0.0097(5) 0.0111(4) -0.0017(4)
O2 0.0193(5) 0.0428(6) 0.0354(5) -0.0046(4) 0.0140(4) 0.0061(5)
O3 0.0219(4) 0.0237(5) 0.0267(5) 0.0024(4) 0.0027(4) 0.0043(4)
O4 0.0163(4) 0.0326(5) 0.0361(5) -0.0006(4) 0.0034(4) -0.0151(4)
O5 0.0229(4) 0.0335(5) 0.0192(4) -0.0052(4) 0.0025(4) 0.0012(4)
O6 0.0286(5) 0.0276(5) 0.0229(5) 0.0014(4) 0.0007(4) 0.0009(4)
O7 0.0172(4) 0.0256(5) 0.0218(4) 0.0030(3) 0.0063(3) 0.0015(4)
O8 0.0287(5) 0.0237(5) 0.0316(5) 0.0012(4) 0.0147(4) -0.0001(4)
O9 0.0352(5) 0.0240(5) 0.0305(5) -0.0043(4) 0.0126(4) 0.0006(4)
N1 0.0139(5) 0.0202(5) 0.0183(5) -0.0010(4) 0.0052(4) -0.0009(4)
N2 0.0170(5) 0.0173(5) 0.0226(5) 0.0020(4) 0.0085(4) 0.0034(4)
N3 0.0338(7) 0.0553(9) 0.0308(7) -0.0053(6) 0.0059(6) -0.0077(6)
N4 0.0215(6) 0.0581(9) 0.0214(5) 0.0079(6) 0.0088(5) 0.0006(6)
C1 0.0175(6) 0.0125(5) 0.0180(6) -0.0012(4) 0.0053(5) 0.0013(4)
C2 0.0172(6) 0.0191(6) 0.0233(6) -0.0015(4) 0.0038(5) 0.0011(5)
C3 0.0259(6) 0.0215(6) 0.0211(6) -0.0039(5) -0.0005(5) 0.0009(5)
C4 0.0372(7) 0.0224(7) 0.0165(6) -0.0018(6) 0.0076(5) -0.0009(5)
C5 0.0270(6) 0.0195(6) 0.0230(6) 0.0003(5) 0.0125(5) 0.0008(5)
C6 0.0169(6) 0.0141(6) 0.0194(6) -0.0003(4) 0.0059(5) 0.0014(4)
C7 0.0208(6) 0.0220(6) 0.0202(6) 0.0030(5) 0.0079(5) 0.0028(5)
C8 0.0237(6) 0.0334(7) 0.0220(6) 0.0083(5) 0.0111(5) 0.0053(5)
C9 0.0275(7) 0.0299(7) 0.0214(6) 0.0019(6) 0.0118(5) -0.0008(5)
C10 0.0317(8) 0.0826(14) 0.0273(7) 0.0189(8) 0.0155(6) -0.0014(8)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O2 Na1 O7 . 3_556 92.10(4) ?
O2 Na1 O9 . 3_566 101.69(4) ?
O7 Na1 O9 3_556 3_566 94.98(4) ?
O2 Na1 O8 . . 166.44(4) ?
O7 Na1 O8 3_556 . 85.30(3) ?
O9 Na1 O8 3_566 . 91.80(4) ?
O2 Na1 O7 . . 81.51(4) ?
O7 Na1 O7 3_556 . 88.64(3) ?
O9 Na1 O7 3_566 . 175.04(4) ?
O8 Na1 O7 . . 85.12(3) ?
O2 Na1 O9 . . 102.11(4) ?
O7 Na1 O9 3_556 . 163.96(4) ?
O9 Na1 O9 3_566 . 89.43(4) ?
O8 Na1 O9 . . 79.14(4) ?
O7 Na1 O9 . . 86.18(4) ?
O2 Na1 Na1 . 3_556 85.44(3) ?
O7 Na1 Na1 3_556 3_556 45.20(3) ?
O9 Na1 Na1 3_566 3_556 140.07(4) ?
O8 Na1 Na1 . 3_556 83.29(3) ?
O7 Na1 Na1 . 3_556 43.45(2) ?
O9 Na1 Na1 . 3_556 127.86(4) ?
O2 Na1 Na1 . 3_566 106.87(4) ?
O7 Na1 Na1 3_556 3_566 137.99(4) ?
O9 Na1 Na1 3_566 3_566 45.24(3) ?
O8 Na1 Na1 . 3_566 83.58(3) ?
O7 Na1 Na1 . 3_566 130.32(3) ?
O9 Na1 Na1 . 3_566 44.19(3) ?
Na1 Na1 Na1 3_556 3_566 166.02(3) ?
O2 Na1 H9B . . 109.6 ?
O7 Na1 H9B 3_556 . 146.3 ?
O9 Na1 H9B 3_566 . 105.0 ?
O8 Na1 H9B . . 67.5 ?
O7 Na1 H9B . . 70.2 ?
O9 Na1 H9B . . 19.5 ?
Na1 Na1 H9B 3_556 . 109.4 ?
Na1 Na1 H9B 3_566 . 60.7 ?
O2 S1 O3 . . 113.36(6) ?
O2 S1 O4 . . 112.05(6) ?
O3 S1 O4 . . 111.68(6) ?
O2 S1 C6 . . 106.26(6) ?
O3 S1 C6 . . 106.22(5) ?
O4 S1 C6 . . 106.71(5) ?
C8 O1 C10 . . 115.26(11) ?
S1 O2 Na1 . . 147.89(7) ?
H5A O5 H5B . . 111.1 ?
H6A O6 H6B . . 103.1 ?
Na1 O7 Na1 3_556 . 91.36(3) ?
Na1 O7 H7A 3_556 . 119.5 ?
Na1 O7 H7A . . 118.2 ?
Na1 O7 H7B 3_556 . 121.5 ?
Na1 O7 H7B . . 107.5 ?
H7A O7 H7B . . 99.5 ?
Na1 O8 H8A . . 128.5 ?
Na1 O8 H8B . . 110.3 ?
H8A O8 H8B . . 105.8 ?
Na1 O9 Na1 3_566 . 90.57(4) ?
Na1 O9 H9A 3_566 . 107.1 ?
Na1 O9 H9A . . 114.5 ?
Na1 O9 H9B 3_566 . 143.2 ?
Na1 O9 H9B . . 85.7 ?
H9A O9 H9B . . 107.7 ?
N2 N1 C1 . . 118.67(10) ?
N2 N1 H1N . . 124.9 ?
C1 N1 H1N . . 115.6 ?
C7 N2 N1 . . 120.42(11) ?
C8 N4 H4N . . 110.6 ?
C2 C1 C6 . . 119.09(11) ?
C2 C1 N1 . . 120.22(11) ?
C6 C1 N1 . . 120.68(11) ?
C3 C2 C1 . . 120.10(12) ?
C3 C2 H2 . . 120.0 ?
C1 C2 H2 . . 120.0 ?
C2 C3 C4 . . 120.96(12) ?
C2 C3 H3 . . 119.5 ?
C4 C3 H3 . . 119.5 ?
C3 C4 C5 . . 119.41(12) ?
C3 C4 H4 . . 120.3 ?
C5 C4 H4 . . 120.3 ?
C4 C5 C6 . . 120.48(12) ?
C4 C5 H5 . . 119.8 ?
C6 C5 H5 . . 119.8 ?
C5 C6 C1 . . 119.95(11) ?
C5 C6 S1 . . 117.54(10) ?
C1 C6 S1 . . 122.45(9) ?
N2 C7 C9 . . 122.47(11) ?
N2 C7 C8 . . 116.37(11) ?
C9 C7 C8 . . 121.07(11) ?
N4 C8 O1 . . 123.70(12) ?
N4 C8 C7 . . 125.53(12) ?
O1 C8 C7 . . 110.75(11) ?
N3 C9 C7 . . 174.65(14) ?
O1 C10 H10C . . 109.5 ?
O1 C10 H10D . . 109.5 ?
H10C C10 H10D . . 109.5 ?
O1 C10 H10E . . 109.5 ?
H10C C10 H10E . . 109.5 ?
H10D C10 H10E . . 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
Na1 O2 . 2.3407(11) ?
Na1 O7 3_556 2.3530(10) ?
Na1 O9 3_566 2.4061(11) ?
Na1 O8 . 2.4237(11) ?
Na1 O7 . 2.4276(10) ?
Na1 O9 . 2.4511(11) ?
Na1 Na1 3_556 3.4206(10) ?
Na1 Na1 3_566 3.4517(10) ?
Na1 H9B . 2.5336 ?
S1 O2 . 1.4466(9) ?
S1 O3 . 1.4572(10) ?
S1 O4 . 1.4627(10) ?
S1 C6 . 1.7730(13) ?
O1 C8 . 1.3424(16) ?
O1 C10 . 1.4482(17) ?
O5 H5A . 0.8498 ?
O5 H5B . 0.8501 ?
O6 H6A . 0.8500 ?
O6 H6B . 0.8500 ?
O7 H7A . 0.8496 ?
O7 H7B . 0.8500 ?
O8 H8A . 0.8500 ?
O8 H8B . 0.8503 ?
O9 H9A . 0.8501 ?
O9 H9B . 0.8500 ?
N1 N2 . 1.3178(14) ?
N1 C1 . 1.4049(15) ?
N1 H1N . 0.9050 ?
N2 C7 . 1.2961(16) ?
N3 C9 . 1.1474(19) ?
N4 C8 . 1.2621(18) ?
N4 H4N . 0.9254 ?
C1 C2 . 1.3967(17) ?
C1 C6 . 1.4045(17) ?
C2 C3 . 1.3826(19) ?
C2 H2 . 0.9500 ?
C3 C4 . 1.386(2) ?
C3 H3 . 0.9500 ?
C4 C5 . 1.3864(19) ?
C4 H4 . 0.9500 ?
C5 C6 . 1.3916(18) ?
C5 H5 . 0.9500 ?
C7 C9 . 1.4398(18) ?
C7 C8 . 1.4832(17) ?
C10 H10C . 0.9800 ?
C10 H10D . 0.9800 ?
C10 H10E . 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
O5 H5A O4 1_565 0.85 1.98 2.8243(13) 172.5 yes
O5 H5B O6 2 0.85 1.92 2.7660(13) 175.5 yes
O6 H6A O5 . 0.85 1.88 2.7295(15) 174.2 yes
O6 H6B O3 . 0.85 1.98 2.8169(13) 168.0 yes
O7 H7A O5 1_545 0.85 2.06 2.8978(13) 170.6 yes
O7 H7B N4 1_455 0.85 1.98 2.8141(14) 166.6 yes
O8 H8A O3 3_566 0.85 2.05 2.8874(14) 168.2 yes
O8 H8B O2 3_556 0.85 2.18 2.9689(15) 153.2 yes
O9 H9A O6 . 0.85 1.97 2.8241(14) 177.6 yes
N4 H4N O8 1_655 0.93 2.38 3.0905(16) 133.4 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
O3 S1 O2 Na1 . . . . 5.69(15) ?
O4 S1 O2 Na1 . . . . -121.84(12) ?
C6 S1 O2 Na1 . . . . 121.98(12) ?
C1 N1 N2 C7 . . . . 174.30(11) ?
N2 N1 C1 C2 . . . . -3.68(17) ?
N2 N1 C1 C6 . . . . 176.71(11) ?
C6 C1 C2 C3 . . . . -0.59(18) ?
N1 C1 C2 C3 . . . . 179.80(11) ?
C1 C2 C3 C4 . . . . -0.2(2) ?
C2 C3 C4 C5 . . . . 0.7(2) ?
C3 C4 C5 C6 . . . . -0.5(2) ?
C4 C5 C6 C1 . . . . -0.26(19) ?
C4 C5 C6 S1 . . . . -177.60(10) ?
C2 C1 C6 C5 . . . . 0.81(17) ?
N1 C1 C6 C5 . . . . -179.58(11) ?
C2 C1 C6 S1 . . . . 178.00(9) ?
N1 C1 C6 S1 . . . . -2.39(16) ?
O2 S1 C6 C5 . . . . -30.12(12) ?
O3 S1 C6 C5 . . . . 90.88(10) ?
O4 S1 C6 C5 . . . . -149.84(10) ?
O2 S1 C6 C1 . . . . 152.62(10) ?
O3 S1 C6 C1 . . . . -86.38(11) ?
O4 S1 C6 C1 . . . . 32.90(12) ?
N1 N2 C7 C9 . . . . -0.71(19) ?
N1 N2 C7 C8 . . . . -177.34(11) ?
C10 O1 C8 N4 . . . . 1.9(2) ?
C10 O1 C8 C7 . . . . -176.78(13) ?
N2 C7 C8 N4 . . . . -1.5(2) ?
C9 C7 C8 N4 . . . . -178.15(15) ?
N2 C7 C8 O1 . . . . 177.19(12) ?
C9 C7 C8 O1 . . . . 0.51(18) ?