#------------------------------------------------------------------------------
#$Date: 2022-06-28 04:47:49 +0300 (Tue, 28 Jun 2022) $
#$Revision: 276306 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/26/2022623.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_2022623
loop_
_publ_author_name
'Nirmal Ram, Jeyaraman Selvaraj'
'Sathya, Udhayasuriyan'
'Gomathi, Sundaramoorthy'
'Cordes, David Bradford'
_publ_section_title
;
Structure determination and Hirshfeld surface analysis of new cocrystal
and salt forms of 5-aminotetrazole with hydroxy- and nitro-substituted
carboxylic acids
;
_journal_coeditor_code ZO3022
_journal_issue 7
_journal_name_full 'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi 10.1107/S2053229622006519
_journal_volume 78
_journal_year 2022
_chemical_formula_iupac 'C H4 N5 +, C7 H3 N2 O7 -'
_chemical_formula_moiety 'C H4 N5 +, C7 H3 N2 O7 -'
_chemical_formula_sum 'C8 H7 N7 O7'
_chemical_formula_weight 313.21
_chemical_name_systematic
;
5-Aminotetrazolium 3,5-dinitrosalicylate
;
_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 dual
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_cell_angle_alpha 90
_cell_angle_beta 98.646(5)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 6.2591(3)
_cell_length_b 11.1312(5)
_cell_length_c 17.2257(9)
_cell_measurement_reflns_used 7845
_cell_measurement_temperature 173
_cell_measurement_theta_max 68.0830
_cell_measurement_theta_min 6.5320
_cell_volume 1186.50(10)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku OD, 2019)
;
_computing_data_collection
;
CrystalClear-SM Expert (Rigaku, 2015)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku OD, 2019)
;
_computing_molecular_graphics
;
Mercury (Macrae et al., 2020), PLATON (Spek, 2020) and
POVRay (Cason, 2004)
;
_computing_publication_material
;
enCIFer (Allen et al., 2004)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2018 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 173
_diffrn_detector 'hybrid photon counting detector'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device 'AFC12: Kappa 4 circle'
_diffrn_measurement_device_type 'Rigaku XtaLAB P100K'
_diffrn_measurement_method '\w and \f scans'
_diffrn_measurement_specimen_support Loop
_diffrn_radiation_monochromator 'Rigaku Osmic Confocal Optical System'
_diffrn_radiation_probe x-ray
_diffrn_radiation_type 'Cu K\a'
_diffrn_radiation_wavelength 1.54184
_diffrn_reflns_av_R_equivalents 0.0408
_diffrn_reflns_av_unetI/netI 0.0081
_diffrn_reflns_limit_h_max 7
_diffrn_reflns_limit_h_min -7
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_l_max 20
_diffrn_reflns_limit_l_min -20
_diffrn_reflns_number 4182
_diffrn_reflns_theta_full 67.684
_diffrn_reflns_theta_max 68.339
_diffrn_reflns_theta_min 4.746
_diffrn_source 'Rotating Anode'
_diffrn_standards_decay_% 0
_diffrn_standards_interval_count 0
_diffrn_standards_number 0
_exptl_absorpt_coefficient_mu 1.370
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.85966
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD, 2019)
;
_exptl_crystal_colour yellow
_exptl_crystal_density_diffrn 1.753
_exptl_crystal_description plate
_exptl_crystal_F_000 640
_exptl_crystal_size_max 0.07
_exptl_crystal_size_mid 0.03
_exptl_crystal_size_min 0.01
_refine_diff_density_max 0.458
_refine_diff_density_min -0.434
_refine_ls_extinction_coef 0.015(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2018 (Sheldrick, 2015b)
;
_refine_ls_goodness_of_fit_ref 1.042
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 221
_refine_ls_number_reflns 4182
_refine_ls_number_restraints 6
_refine_ls_restrained_S_all 1.053
_refine_ls_R_factor_all 0.0443
_refine_ls_R_factor_gt 0.0409
_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^)+(0.0876P)^2^+0.0468P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1124
_refine_ls_wR_factor_ref 0.1142
_reflns_number_gt 3644
_reflns_number_total 4182
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file zo3022sup1.cif
_cod_data_source_block II
_cod_database_code 2022623
_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_hkl_file
;
0 0 2 5733.57 29.0310 1
0 0 4 24916.3 83.9713 1
0 0 6 12988.7 79.1124 1
0 0 8 74861.4 153.515 1
0 0 10 418.389 19.9964 1
0 0 12 3114.31 69.8156 1
0 0 14 2971.24 80.0630 1
0 0 16 200.049 43.1773 1
2 0 -18 7058.67 94.2303 -2
0 0 -18 7058.67 94.2303 1
0 0 -20-4.48156 29.2973 1
0 1 1 12157.4 46.4668 1
0 -1 2 4954.28 16.2487 1
0 -1 3 7399.60 23.7674 1
0 -1 4 10160.8 39.7089 1
0 1 5 592.111 16.9036 1
0 1 6 27700.8 80.1010 1
0 1 7 11864.9 47.3282 1
0 -1 8 6331.68 33.8818 1
-1 1 9 41089.9 75.1542 -2
0 -1 9 41089.9 75.1542 1
0 1 10 13402.3 40.3732 1
0 -1 11 25197.7 66.7062 1
0 -1 -12 10320.6 46.7331 1
0 1 13 4361.51 44.3892 1
0 -1 14 1455.71 49.5124 1
0 1 15 1061.42 34.4828 1
0 1 16 2812.32 43.1285 1
0 1 17 4077.56 53.3704 1
2 1 -18 115.429 43.4720 -2
0 -1 -18 115.429 43.4720 1
0 -1 -19 20.9099 43.0157 1
-2 1 19 105.345 32.1325 -2
0 -1 19 105.345 32.1325 1
0 -1 20 234.332 21.0456 1
0 2 0 3731.55 27.9033 -2
0 -2 0 3731.55 27.9033 1
0 -2 1 38807.2 30.6245 1
0 2 2 52376.7 72.3704 1
0 -2 3 16837.2 34.7981 1
0 -2 4 968.971 13.5718 1
0 2 5 3897.90 24.1321 1
0 -2 6 5133.48 37.1348 1
0 2 7 13341.9 37.9183 1
0 2 8 955.675 13.7369 1
-1 -2 9 4086.85 29.6820 -2
0 2 9 4086.85 29.6820 1
0 2 10 1348.26 17.4152 1
0 2 11 116.145 17.1339 1
0 -2 12 3428.89 32.5732 1
0 -2 13 612.541 24.4494 1
0 2 14 111.711 24.6520 1
0 -2 15 10572.6 52.8039 1
0 -2 -16 1214.60 41.8973 1
0 -2 -17 211.714 34.2505 1
2 2 -18 778.741 45.9571 -2
0 -2 -18 778.741 45.9571 1
0 -2 -19 34.1550 43.4197 1
-2 2 19 46.6530 34.8778 -2
0 -2 19 46.6530 34.8778 1
0 -2 -20 853.276 25.5320 1
0 -3 -1 552.190 7.90291 1
0 -3 2 6083.45 16.8453 1
0 3 3 2327.94 18.8061 1
0 3 4 15738.9 38.9623 1
0 3 5 25923.1 56.8232 1
0 -3 6 7934.13 28.1532 1
0 3 7 12639.0 34.0475 1
0 3 8 6795.97 28.0220 1
1 3 -9 15787.9 55.4518 -2
0 -3 -9 15787.9 55.4518 1
0 3 10 1659.13 21.0078 1
0 -3 11 3221.30 31.8046 1
0 -3 12 19895.3 70.7007 1
0 -3 13 41137.7 101.526 1
0 3 14 25751.4 53.4208 1
0 -3 -15 49.5332 21.9210 1
0 -3 -16 3306.45 49.9306 1
0 -3 17 342.692 32.5764 1
-2 -3 17 820.718 79.2433 -2
0 3 17 820.718 79.2433 1
-2 -3 18 18.6499 30.9895 -2
0 3 18 18.6499 30.9895 1
0 -3 -19 23.3462 39.6050 1
-2 3 19 13.5871 28.7649 -2
0 -3 19 13.5871 28.7649 1
0 4 0 87323.8 186.277 -2
0 -4 0 87323.8 186.277 1
0 -4 1 18108.3 54.1671 1
0 -4 2 212.635 5.65352 1
0 4 3 234.940 7.79039 1
0 -4 4 12.2750 6.44089 1
0 4 5 11124.6 28.5445 1
0 -4 6 52.4432 9.84696 1
0 4 7 130.020 10.9783 1
0 -4 8 64.9473 11.1359 1
-1 4 9 12834.0 48.5117 -2
0 -4 9 12834.0 48.5117 1
0 4 10 1356.52 24.0196 1
0 4 11 1114.92 24.8676 1
0 -4 12 2159.95 31.6069 1
0 -4 13 3697.44 32.7036 1
0 4 14 10175.6 37.0220 1
0 -4 -15 22.8059 25.8008 1
0 -4 16 1343.79 28.2229 1
0 -4 -17 2232.68 39.3839 1
-2 -4 17 3620.22 93.4850 -2
0 4 17 3620.22 93.4850 1
2 4 -18 259.390 28.1605 -2
0 -4 -18 259.390 28.1605 1
0 -4 -19 126.504 27.4317 1
-2 4 19 332.102 31.2641 -2
0 -4 19 332.102 31.2641 1
0 -5 1 6603.01 38.7650 1
0 5 2 13285.1 32.5760 1
0 -5 3 15570.3 29.3213 1
0 -5 4 10722.2 22.9512 1
0 -5 -5 9794.28 24.8375 1
0 -5 6 16862.4 40.6653 1
0 -5 7 2343.18 16.1571 1
0 -5 -8 2488.45 19.2012 1
-1 5 9 2231.75 25.3804 -2
0 -5 9 2231.75 25.3804 1
0 -5 10 998.096 24.8631 1
0 -5 11 5293.66 41.3572 1
0 -5 12 4274.11 35.8701 1
0 5 13 6176.45 29.8179 1
0 -5 14 22.2857 18.3162 1
0 -5 15 529.435 24.1500 1
0 -5 -16 187.562 21.3236 1
0 -5 17 624.621 23.1430 1
-2 -5 17 1346.36 81.1066 -2
0 5 17 1346.36 81.1066 1
-2 5 18 76.2184 24.8002 -2
0 -5 18 76.2184 24.8002 1
0 -5 19 1004.23 41.6973 1
0 -6 0 2209.67 20.9630 -2
0 6 0 2209.67 20.9630 1
0 -6 -1 22957.9 36.8209 1
0 -6 2 2593.25 17.1360 1
0 -6 -3 7156.70 26.2728 1
0 -6 4 800.073 14.2905 1
0 -6 -5 538.710 11.9369 1
0 -6 -6 8828.12 33.4309 1
0 -6 -7 16313.9 46.2862 1
0 -6 -8 11.4632 16.5181 1
-1 6 9 3506.58 43.0318 -2
0 -6 9 3506.58 43.0318 1
0 -6 -10 14775.4 72.0201 1
0 -6 -11 17329.1 54.4747 1
0 -6 -12 10095.1 37.1395 1
0 -6 -13 3304.60 26.0384 1
0 -6 14-8.96150 21.4774 1
0 -6 15 459.215 20.1505 1
0 -6 16 877.234 19.9741 1
0 -6 -17 193.340 21.7524 1
-2 6 18 3085.87 35.6583 -2
0 -6 18 3085.87 35.6583 1
0 7 1 53.7702 10.4795 1
0 -7 -2 5108.84 23.9545 1
0 -7 -3 271.508 13.6045 1
0 -7 4 4521.83 30.1445 1
0 -7 -5 2124.01 24.2243 1
0 -7 6 1439.87 25.1333 1
0 -7 -7-1.19518 18.9376 1
0 -7 -8 210.561 21.7788 1
1 7 -9 1981.72 40.3054 -2
0 -7 -9 1981.72 40.3054 1
0 -7 10 2715.67 28.9259 1
1 7 -10 4951.70 42.6196 -2
0 -7 -10 4951.70 42.6196 1
0 -7 11 1335.40 18.6996 1
0 -7 12 4957.84 29.4041 1
0 -7 -13 4820.75 34.2436 1
0 -7 -14 1147.56 22.9506 1
0 -7 -15 455.229 19.1960 1
0 -7 16 47.0527 17.7209 1
0 -7 17 1503.47 23.2838 1
0 8 0 2584.33 32.7066 -2
0 -8 0 2584.33 32.7066 1
0 -8 -1 60.9416 14.3114 1
0 -8 2 1055.63 23.0597 1
0 -8 -3 4038.68 34.6478 1
0 -8 4 9.39448 18.9668 1
0 -8 -5 2225.60 34.9237 1
0 -8 6 7660.48 55.9239 1
0 -8 7 1610.11 34.0246 1
0 -8 -8 8435.78 31.5821 1
1 8 -8 11607.4 127.232 -2
0 -8 -8 11607.4 127.232 1
1 8 -9 1445.23 24.7555 -2
0 -8 -9 1445.23 24.7555 1
0 -8 -10 1862.98 25.4178 1
-1 8 10 6861.23 50.2861 -2
0 -8 10 6861.23 50.2861 1
0 -8 11 5691.58 29.9219 1
0 -8 -12 1975.44 24.8993 1
0 -8 13 6029.20 34.8516 1
0 -8 -14 65.9116 17.5375 1
0 -8 -15 1009.84 18.7683 1
0 -8 16 133.766 20.9380 1
0 -9 -1 10843.5 54.6170 1
0 -9 2 31088.9 89.6031 1
0 -9 -3 8151.22 49.4635 1
0 -9 4 75.0425 16.3610 1
0 -9 -5 6034.03 25.8780 1
0 -9 6 1712.25 18.0713 1
0 -9 7 2309.99 19.9594 1
0 -9 -8 1936.21 21.5294 1
-1 9 8 3116.88 63.8813 -2
0 -9 8 3116.88 63.8813 1
1 9 -9 269.968 24.3828 -2
0 -9 -9 269.968 24.3828 1
0 -9 10 301.081 25.7113 1
-1 9 10 7556.34 50.5870 -2
0 -9 10 7556.34 50.5870 1
0 -9 -11 2361.55 23.1457 1
0 -9 -12 195.884 17.6602 1
0 -9 -13 360.896 17.6437 1
0 -9 -14 776.570 16.7962 1
0 -9 -15 6.16048 23.8557 1
0 10 0 398.597 25.0509 -2
0 -10 0 398.597 25.0509 1
0 -10 1 5686.40 24.7584 1
0 10 -1 11447.9 92.9082 -2
0 -10 -1 11447.9 92.9082 1
0 -10 2 5321.09 23.5343 1
0 -10 3 3927.27 22.1382 1
0 -10 4 102.476 14.7317 1
0 -10 5 5975.36 27.7633 1
0 -10 -6 10.5502 17.5791 1
0 -10 7 7808.40 32.8337 1
0 -10 -8 1351.26 22.6989 1
1 10 -8 12876.4 88.7078 -2
0 -10 -8 12876.4 88.7078 1
-1 10 9 861.547 22.8307 -2
0 -10 9 861.547 22.8307 1
0 -10 10 63.4733 19.8761 1
1 10 -10 769.302 39.1385 -2
0 -10 -10 769.302 39.1385 1
0 -10 -11 17.1593 15.4944 1
0 -10 -12 160.042 15.5760 1
0 -10 13 1190.35 19.7459 1
0 -11 1 10031.0 37.5217 1
0 11 1 19219.1 105.523 -2
0 -11 1 19219.1 105.523 1
0 -11 2 483.575 19.5977 1
0 -11 3 5161.80 27.0918 1
0 -11 -4 1398.41 20.3359 1
0 -11 5 537.738 18.7552 1
0 -11 -6 411.593 18.0233 1
0 -11 7 734.402 17.8645 1
0 -11 8 978.166 20.3800 1
1 11 -8 1487.96 68.2058 -2
0 -11 -8 1487.96 68.2058 1
-1 11 9 1216.66 26.2966 -2
0 -11 9 1216.66 26.2966 1
0 -11 -10 550.950 25.7625 1
1 11 -10 661.718 31.3032 -2
0 -11 -10 661.718 31.3032 1
0 -11 11 4.42288 17.7940 1
0 12 0 466.762 34.3957 -2
0 -12 0 466.762 34.3957 1
0 -12 -1 1924.86 31.7122 1
0 12 1 3799.54 46.2850 -2
0 -12 1 3799.54 46.2850 1
0 -12 2 14.7439 21.5724 1
0 -12 3 95.5895 19.3820 1
0 -12 -4 232.931 19.0691 1
0 -12 -5 54.4307 17.6521 1
0 -12 6 118.486 19.0245 1
0 -12 7 3540.58 27.1062 1
0 -12 -8 975.774 31.4165 1
-1 12 8 1402.79 51.4660 -2
0 -12 8 1402.79 51.4660 1
-1 12 9 325.926 33.4065 -2
0 -12 9 325.926 33.4065 1
-1 0 20 1635.57 39.2732 1
-1 0 18 617.725 56.8637 -2
-1 0 18 617.725 56.8637 1
-1 0 16 7716.92 83.6414 1
1 0 -14 455.278 37.5502 1
-1 0 12 4353.14 36.8094 1
-1 0 10 6733.43 43.5396 1
-1 0 8 14015.5 68.8661 1
-1 0 6 6497.18 59.1220 1
-1 0 4 87855.6 117.057 1
-1 0 2 1543.45 13.2387 1
-1 0 0 90.3432 7.46255 -2
1 0 0 90.3432 7.46255 1
1 0 2 66.9570 13.7225 1
1 0 4 51656.5 156.705 1
1 0 6 13557.1 86.9513 1
1 0 8 11654.3 65.8593 1
1 0 10 1705.69 53.5435 1
1 0 12 1392.94 58.3158 1
1 0 14 51.0780 40.0454 1
1 0 16 5686.04 102.057 1
-3 0 18 850.358 38.2703 -2
1 0 18 850.358 38.2703 1
-1 1 20 111.920 21.0912 1
1 1 -19 9.56385 33.1719 -2
1 -1 -19 9.56385 33.1719 1
-1 -1 18 3718.36 62.3164 -2
-1 1 18 3718.36 62.3164 1
-1 1 17 32.6193 40.7820 1
-1 1 17 119.487 78.2109 -2
-1 -1 17 119.487 78.2109 1
-1 -1 16 1412.92 32.9323 1
-1 -1 15 622.121 28.1896 1
-1 -1 14 100.607 27.9705 1
-1 1 13 417.433 21.8396 1
1 1 -12 77.8138 15.9421 1
1 1 -11 2594.77 24.2328 1
-1 -1 10 6249.78 33.9301 1
0 1 9 44219.4 93.2563 -2
-1 -1 9 44219.4 93.2563 1
-1 1 8 39152.0 79.7656 1
-1 -1 7 80277.0 107.039 1
-1 -1 6 3018.86 25.0770 1
-1 1 5 3229.78 23.2973 1
-1 -1 4 389.785 11.9215 1
-1 1 3 12605.4 30.2920 1
-1 1 2 87111.9 54.9151 1
-1 -1 1 1437.89 8.25521 1
-1 -1 0 22286.2 29.6580 -2
1 1 0 22286.2 29.6580 1
1 1 1 11.9616 9.10431 1
1 1 2 93056.6 104.474 1
1 -1 3 7853.36 35.8969 1
1 -1 4 419.202 15.1662 1
1 1 5 8593.28 44.8975 1
1 1 6 831.082 17.2686 1
1 1 7 76539.7 106.847 1
1 -1 8 30956.4 74.1616 1
-2 1 9 30508.0 66.8689 -2
1 -1 9 30508.0 66.8689 1
1 -1 10 4682.00 31.4597 1
-1 -1 -11 1942.43 26.0221 1
1 1 12 21.0269 28.9091 1
1 1 13 866.293 42.4598 1
1 -1 14 460.962 26.2924 1
1 1 15 135.636 28.2160 1
1 1 16 307.359 38.5495 1
-1 -1 -17 165.823 28.1384 1
3 1 -18 2403.28 39.0608 -2
-1 -1 -18 2403.28 39.0608 1
3 -1 -19 47.6907 29.4057 -2
-1 1 -19 47.6907 29.4057 1
-1 2 20 433.130 18.8681 1
1 2 -19 366.462 32.9457 -2
1 -2 -19 366.462 32.9457 1
-1 -2 18 4064.85 62.5315 -2
-1 2 18 4064.85 62.5315 1
-1 -2 17 542.969 46.6118 1
-1 -2 17 922.187 84.2271 -2
-1 2 17 922.187 84.2271 1
-1 2 16 321.148 32.3227 1
1 -2 -15 3507.47 32.9381 1
-1 -2 14 8.97387 24.2064 1
1 -2 -13 66.6785 21.5494 1
-1 -2 12 247.693 19.9837 1
-1 -2 11 17.8345 14.7267 1
-1 -2 10 622.554 15.4223 1
0 2 9 4197.15 34.4186 -2
-1 -2 9 4197.15 34.4186 1
-1 -2 8 1331.10 16.5392 1
-1 2 7 362.882 12.1338 1
-1 2 6 632.697 15.9325 1
-1 -2 5 33720.5 67.6048 1
-1 2 4 5610.92 26.5862 1
-1 2 3 36611.5 58.7077 1
-1 2 2 146464. 81.8295 1
-1 -2 1 7166.37 14.6932 1
1 2 0 1744.74 12.1863 -2
-1 -2 0 1744.74 12.1863 1
1 -2 1 4029.71 17.9958 1
1 2 2 130130. 123.966 1
1 -2 3 28999.4 66.1372 1
1 2 4 7401.48 37.8424 1
1 -2 5 32413.5 83.2705 1
1 -2 6 2302.29 20.3499 1
1 -2 7 392.034 11.7780 1
1 2 8 179.774 11.2912 1
-2 -2 9 4356.84 31.0928 -2
1 2 9 4356.84 31.0928 1
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-5 1 10 1686.59 34.0318 2
-5 1 8 1930.59 33.8383 2
-5 1 7 2911.51 38.3774 2
-5 1 6 28.5874 30.8326 2
-5 1 5 62.4075 32.8319 2
-5 1 4 67.4796 34.6774 2
-5 -1 3 885.736 39.0230 2
-5 -1 2 5786.52 67.8472 2
-5 -1 1 398.575 26.6265 2
-5 -1 -1 704.640 28.3717 2
-5 -1 -2 10660.4 56.6520 2
-5 -1 -3 249.284 26.5409 2
-5 1 -4 6.20598 23.4105 2
-5 -1 -5 2503.39 27.3913 2
-5 -1 -6 203.547 19.4642 2
-5 -1 -7 3563.17 27.4177 2
-5 -1 -8 1633.99 27.4670 2
-5 1 -10 724.771 22.8051 2
-5 1 -11 95.2202 21.6229 2
-5 -1 -12 37.4249 17.5894 2
5 1 13 201.484 38.0123 2
-5 -2 17 119.187 37.6046 2
-5 2 16 7.19857 19.4442 2
-5 -2 15 311.789 22.4508 2
-5 -2 14 341.910 24.3243 2
-5 -2 13 296.192 26.1026 2
-5 -2 12 987.800 33.5246 2
-5 2 11 79.3224 29.6758 2
-5 2 10 5.30907 24.9048 2
-5 2 8 797.174 27.4692 2
-5 2 7 416.878 24.5179 2
-5 2 6 153.964 26.0883 2
-5 2 5 428.183 33.2341 2
-5 -2 4 31.8707 33.8999 2
-5 -2 3 833.718 42.3636 2
-5 -2 2 4694.90 63.3033 2
-5 -2 1 74.4910 24.6888 2
-5 -2 -1 566.062 25.7040 2
-5 2 -2 2080.22 27.3123 2
-5 2 -3 503.837 23.8873 2
-5 -2 -4 494.514 20.6503 2
-5 -2 -5 125.518 19.2168 2
-5 -2 -6 562.041 21.0702 2
-5 -2 -7 10.7278 20.2451 2
-5 -2 -8-2.61422 21.7214 2
-5 -2 -10-3.07608 20.1422 2
-5 -2 -11 72.6997 19.5282 2
5 2 12 558.132 23.0907 2
5 3 -16 449.390 31.3241 2
-5 -3 15 15.7615 20.0264 2
-5 3 14 293.545 20.7177 2
-5 -3 13 865.019 24.9398 2
-5 3 12 393.565 26.3687 2
-5 3 11 180.758 26.2137 2
-5 3 10 125.467 29.5877 2
-5 3 8 562.622 25.9711 2
-5 3 7 147.728 23.2914 2
-5 3 6 763.990 24.4465 2
-5 3 5 3676.21 31.8021 2
-5 3 4 734.853 29.7353 2
-5 -3 3 12.5541 30.0487 2
-5 -3 2 198.196 23.9602 2
-5 -3 1 345.700 25.8937 2
-5 3 -1 45.1882 19.4563 2
-5 3 -2 886.703 23.2187 2
-5 3 -3 2219.07 27.5040 2
-5 3 -4 2533.37 25.4522 2
-5 -3 -5 987.394 22.2137 2
-5 -3 -6 139.249 22.0553 2
-5 -3 -7 244.672 19.6069 2
-5 -3 -8 81.1605 20.8314 2
-5 -3 -10 33.9426 18.4025 2
-5 3 -11 187.071 20.3277 2
5 3 12 7.38400 26.8228 2
-5 -4 15 2966.15 30.7042 2
-5 -4 14 957.025 22.0742 2
-5 4 13 2602.10 30.4526 2
-5 4 12 429.466 25.1638 2
-5 4 11 445.529 26.6233 2
-5 4 10 114.603 25.9272 2
-5 4 8 789.069 24.6671 2
-5 4 7 5481.79 33.6610 2
-5 4 6 4247.40 31.2279 2
-5 4 5 1133.53 24.6994 2
-5 4 4 1251.10 24.8600 2
-5 4 3 1129.07 21.7816 2
-5 4 2 595.433 20.5336 2
-5 4 1 235.063 21.0576 2
-5 4 -1 2241.38 26.3701 2
-5 4 -2-6.75906 23.6259 2
-5 4 -3 4950.25 31.8242 2
5 4 4 1941.25 29.3031 2
-5 -4 -5 3738.47 33.4888 2
-5 -4 -6 57.1222 19.9789 2
-5 -4 -7 8.24256 19.4648 2
-5 -4 -8 42.2627 18.3220 2
-5 4 -10 584.069 22.1207 2
5 4 11 208.162 20.3568 2
5 5 -15 213.114 38.9710 2
-5 -5 14 2103.49 25.0888 2
-5 5 13 3676.94 34.9676 2
-5 5 12 550.590 27.1283 2
-5 5 11 2864.44 33.1902 2
-5 5 10 397.148 29.0518 2
-5 5 8 189.456 25.6607 2
-5 5 7 1205.56 27.4986 2
-5 5 6 10.0730 24.1541 2
-5 5 5 536.649 24.0081 2
-5 5 4 1514.82 25.0454 2
-5 -5 3 89.1162 21.4229 2
-5 5 2 942.320 24.1586 2
-5 5 1 2456.95 36.1393 2
-5 5 -1 1640.81 25.5596 2
-5 5 -2 450.672 24.0722 2
-5 -5 -3 866.963 24.4018 2
-5 -5 -4 560.560 21.7900 2
-5 5 -5 6.30420 18.1956 2
-5 5 -6 17.0096 19.5314 2
5 5 7 509.467 19.9271 2
-5 -5 -8 102.156 16.9697 2
-5 5 -10 1278.44 24.5045 2
5 6 -14-1.18316 37.4893 2
-5 6 13 2.81759 21.8476 2
-5 6 12 3223.34 33.2824 2
-5 6 11 6144.76 37.8786 2
-5 6 10 3966.17 34.8137 2
-5 6 8 393.829 23.0086 2
-5 6 7 197.662 22.9459 2
-5 6 6-0.96023 22.0289 2
-5 6 5 680.589 23.2567 2
-5 6 4 370.124 22.8412 2
-5 6 3 8.23484 22.0912 2
-5 6 2 1040.30 25.1596 2
-5 6 1 372.217 23.0762 2
-5 -6 -1 1122.62 24.4516 2
-5 -6 -2 1946.82 26.6393 2
-5 -6 -3 392.363 21.8064 2
-5 -6 -4 105.044 17.8350 2
5 6 5 319.304 18.4840 2
5 6 6 129.025 18.1384 2
-5 6 -7 191.148 17.2592 2
5 6 8 429.315 16.8874 2
-5 6 -10 1822.34 44.5890 2
5 7 -13 315.681 39.0743 2
-5 7 12 323.693 23.2996 2
-5 7 11 33.6482 23.4848 2
-5 7 10 254.104 23.8367 2
-5 7 8 25.1807 20.9998 2
-5 7 7 72.3267 20.4564 2
-5 7 6 167.504 20.8074 2
-5 7 5 335.720 22.2615 2
-5 7 4 1314.21 23.7269 2
-5 7 3 56.5477 20.4539 2
-5 7 2 4.31430 20.8201 2
-5 -7 1 547.251 20.8552 2
-5 -7 -1 388.938 21.1067 2
-5 -7 -2 664.942 19.9011 2
5 7 3 393.501 19.5981 2
5 7 4 459.626 17.8787 2
-5 7 -5 7.19198 16.0179 2
5 7 6 496.969 17.0993 2
5 7 7 53.3601 17.1281 2
-5 7 -8 837.807 25.2236 2
-5 8 11 17.2277 20.1466 2
-5 8 10 1516.14 28.0831 2
-5 8 8 1209.53 23.1365 2
-5 8 7-6.90221 17.5760 2
-5 8 6 958.405 20.5729 2
-5 8 5 69.8639 18.1948 2
-5 8 4 1100.67 22.0485 2
-5 8 3 636.644 22.0984 2
-5 8 2 115.667 19.1719 2
-5 8 1 771.978 20.2351 2
5 8 1 1393.60 23.1547 2
-5 8 -2 26.7065 17.6952 2
5 8 3 889.135 20.0948 2
5 8 4 16.5804 16.4134 2
-5 8 -5 66.9561 15.5694 2
-5 8 -6 66.8870 17.7181 2
-5 8 -7 108.457 23.1279 2
-5 9 8 17.2400 23.8069 2
-5 9 7 45.9472 25.3083 2
-5 9 6 130.455 18.0133 2
-5 9 5 234.664 17.5053 2
-5 9 4 926.389 19.8475 2
-5 9 3 4061.71 28.3118 2
-5 9 2 385.991 18.6656 2
5 9 -1 305.468 19.4044 2
5 9 1 2477.68 23.7130 2
5 9 2 1168.38 19.9027 2
5 9 3 2426.00 27.0970 2
5 9 4 1943.60 32.4357 2
-5 10 2 431.424 25.0975 2
-5 10 1 1327.40 30.6783 2
-6 0 14 856.299 27.0127 2
-6 0 12 180.104 33.9104 2
-6 0 10 2778.27 54.6779 2
-6 0 8 780.547 46.5813 2
-6 0 6 2806.08 60.4884 2
-6 0 4 88.4029 45.8497 2
-6 0 2 9939.11 86.0837 2
-6 0 -2 458.478 64.1929 2
6 0 4 173.155 38.3204 2
6 0 6 216.301 36.3594 2
6 0 8 50.7659 42.4591 2
-6 -1 14 281.278 17.1480 2
-6 1 13 25.3635 20.0382 2
-6 -1 12 91.7896 23.5434 2
-6 -1 11 192.627 25.7878 2
-6 -1 10 20.3787 26.5607 2
-6 -1 8 291.442 29.7186 2
-6 -1 7 6.22004 27.3908 2
-6 -1 6 199.704 27.8755 2
-6 -1 5 389.319 31.9556 2
-6 -1 4 9.70236 30.6584 2
-6 -1 3 1173.41 36.2916 2
-6 -1 2 1804.40 39.9956 2
-6 -1 1 2684.89 59.6645 2
-6 -1 -1 338.870 44.4946 2
6 -1 2 10.1254 32.8810 2
-6 -1 -3 68.1858 27.9290 2
6 1 4 8.91975 23.4614 2
6 1 5 4.80161 20.7326 2
6 1 6 17.8778 21.1066 2
-6 1 -7-2.85533 23.3547 2
-6 1 -8 839.790 26.1878 2
-6 -2 14 429.549 20.9240 2
-6 -2 13 17.4213 18.6991 2
-6 -2 12 40.6803 20.5266 2
-6 -2 11 153.519 23.0298 2
-6 -2 10 132.202 26.7551 2
-6 -2 8 13.8514 28.6419 2
-6 -2 7-5.14497 24.9024 2
-6 -2 6 641.647 28.7311 2
-6 -2 5-2.04358 26.6159 2
-6 -2 4 73.1576 27.0594 2
-6 -2 3 213.855 31.6927 2
-6 -2 2 801.568 35.7798 2
-6 2 1 587.580 37.3426 2
-6 2 -1 539.199 36.6941 2
-6 2 -2 313.080 30.3200 2
6 2 3 179.410 26.2570 2
-6 -2 -4 325.460 23.3851 2
6 2 5 83.3759 21.8497 2
6 2 6 36.9700 20.1969 2
6 2 7 107.260 24.1000 2
-6 2 -8 19.3672 22.9513 2
6 3 -14 3195.36 56.1498 2
-6 -3 13 3656.31 33.0640 2
-6 -3 12 1254.71 24.6432 2
-6 -3 11 490.130 23.3745 2
-6 -3 10 15.6864 23.4237 2
-6 3 8 237.410 28.3592 2
-6 3 7 427.859 24.6474 2
-6 3 6 85.9605 23.6705 2
-6 3 5 562.204 25.3332 2
-6 3 4 147.079 24.5445 2
-6 3 3 447.682 25.7243 2
-6 -3 2 80.8614 23.3289 2
-6 3 1 73.6574 30.8289 2
-6 3 -1 495.237 29.0283 2
-6 3 -2 715.044 23.9746 2
-6 -3 -3 56.1501 21.1118 2
6 3 4 38.9717 21.2725 2
6 -3 5 221.696 19.2784 2
6 3 6 294.198 19.7005 2
-6 3 -7 284.314 24.3903 2
-6 3 -8 287.675 24.7033 2
-6 -4 13 28.8539 21.6420 2
-6 -4 12-0.42142 20.3643 2
-6 4 11 3.77005 22.7508 2
-6 4 10 931.337 24.5323 2
-6 4 8-5.19266 23.2404 2
-6 4 7 166.255 22.0868 2
-6 4 6 1403.79 26.0350 2
-6 4 5 8.18580 22.2860 2
-6 4 4 29.0519 22.7811 2
-6 4 3-3.23371 23.1445 2
-6 4 2 11.9286 24.4645 2
-6 -4 1 16.9121 27.5601 2
-6 -4 -1 23.1951 22.5680 2
6 4 2 14.6492 21.9596 2
6 4 3 6.07765 21.3816 2
6 4 4 13.7112 20.5457 2
6 4 5 1.03003 17.6746 2
-6 4 -6 34.5194 20.6412 2
-6 4 -7 4.58706 20.9819 2
6 4 8 125.002 35.1584 2
-6 -5 12-8.28792 21.6111 2
-6 -5 11 34.8107 23.3835 2
-6 5 10 894.992 29.3634 2
-6 5 8 478.886 25.2845 2
-6 5 7 223.205 20.3275 2
-6 5 6 23.0029 20.1286 2
-6 5 5 1030.55 22.9053 2
-6 5 4 159.854 20.8769 2
-6 5 3 2695.72 29.7816 2
-6 5 2 1324.02 26.5170 2
-6 5 1 4.97061 23.7896 2
-6 -5 -1 474.744 22.2283 2
-6 -5 -2 153.632 20.9638 2
-6 -5 -3 592.408 21.2562 2
6 5 4 173.994 17.5422 2
6 5 5 2.55574 17.5854 2
-6 5 -6 250.791 18.9198 2
-6 5 -7 69.9916 34.3354 2
-6 6 10 1030.15 32.4463 2
-6 6 8 8.99779 21.5966 2
-6 6 7 3.76221 18.8870 2
-6 6 6 518.153 20.9220 2
-6 6 5 60.6408 18.8756 2
-6 6 4 161.813 20.2158 2
-6 6 3 82.8107 20.2869 2
6 6 -2 5.05071 18.6855 2
6 6 -1 132.865 19.9555 2
6 6 1 159.751 19.4562 2
6 6 2-0.46265 16.5268 2
6 6 3 176.370 17.6234 2
6 6 4 86.5449 16.6117 2
-6 6 -5 33.5825 19.1171 2
-6 7 8 504.352 40.8909 2
-6 7 7 238.725 27.3760 2
-6 7 6 103.572 27.3016 2
-6 7 5 32.0455 20.2119 2
-6 7 4 288.544 22.2464 2
-6 7 3 81.7427 23.8514 2
-6 7 2 120.900 24.9708 2
6 7 -1 65.3297 18.6939 2
6 7 1 41.8645 17.1679 2
6 7 2 283.983 17.8128 2
6 7 3 19.9870 15.5261 2
6 8 -2 295.609 21.8554 2
6 8 -1 501.326 22.0670 2
-7 0 10 1902.12 29.7348 2
-7 0 8 460.727 33.2791 2
-7 0 6 39.3856 33.0870 2
-7 0 4 319.012 29.6019 2
-7 0 2 430.501 47.8380 2
-7 0 -2 87.1908 23.9859 2
7 1 -10 461.078 30.1028 2
-7 -1 8 468.449 20.5579 2
-7 -1 7 301.139 21.2697 2
-7 -1 6-1.60526 22.7501 2
-7 -1 5 6.63688 19.7900 2
-7 -1 4 24.1936 23.4712 2
-7 1 3 179.321 25.8294 2
-7 1 2 1497.32 32.4914 2
7 -1 -1 105.611 24.5577 2
7 1 1 218.776 19.0954 2
-7 -1 -2 2585.88 25.1105 2
7 1 3 67.1045 19.9764 2
7 1 4-2.80754 24.4701 2
-7 -2 8 218.779 22.0524 2
-7 -2 7 29.6558 19.7283 2
-7 -2 6 22.7961 20.6121 2
-7 -2 5 45.8179 20.1236 2
-7 -2 4 18.1283 25.7239 2
-7 -2 3 50.0872 25.3464 2
-7 2 2 542.221 24.3476 2
-7 2 1 9.09170 19.2046 2
-7 -2 -1 352.374 20.6418 2
-7 -2 -2 40.2334 18.9400 2
7 2 3 142.168 17.9552 2
7 2 4 83.9232 27.6426 2
-7 -3 8 144.795 40.9167 2
-7 -3 7 121.344 40.0605 2
-7 -3 6 15.6531 41.0880 2
-7 -3 5 400.627 45.4788 2
-7 -3 4-1.51870 27.4622 2
-7 -3 3 37.0396 23.1603 2
-7 -3 2 46.4938 22.8313 2
7 3 -1 109.622 20.2133 2
7 3 1 10.9755 18.5097 2
7 3 2 24.5160 17.1716 2
-7 -3 -3 314.238 17.5392 2
-7 -4 6 862.588 44.1235 2
-7 -4 5 155.879 38.3798 2
-7 -4 4 131.077 39.7365 2
-7 4 3 342.484 21.9036 2
7 4 -2 10.9881 18.4279 2
-7 -4 1 42.5840 17.4211 2
-7 -4 -1 256.686 17.7614 2
;
_shelx_hkl_checksum 7420
_shelx_res_file
;
TITL sathya17t1_a.res in P2(1)/c
sathya17t1.res
created by SHELXL-2018/3 at 15:09:15 on 06-Oct-2020
REM Old TITL sathya17t1 in P21/c #14
REM SHELXT solution in P2(1)/c: R1 0.175, Rweak 0.010, Alpha 0.038
REM 0.000 for 0 systematic absences, Orientation as input
REM Formula found by SHELXT: C15 N2 O5
CELL 1.54184 6.2591 11.1312 17.2257 90 98.646 90
ZERR 4 0.0003 0.0005 0.0009 0 0.005 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C H N O
UNIT 32 28 28 28
EQIV $1 +X,0.5-Y,-0.5+Z
EQIV $2 +X,-1+Y,+Z
DFIX 0.98 0.01 N1 H1 N4 H4 N6 H6b N6 H6a
DFIX 0.98 0.005 O7 H7
DFIX 2 C7 H7
L.S. 4
PLAN 5
TEMP -100
CONF
HTAB O7 O2
HTAB N1 O7_$1
HTAB N4 O1
HTAB N6 O6_$2
HTAB N6 O2
FREE O2 H7
BOND $H
list 4
MORE -1
BOND $H
fmap 2
acta
REM
REM
REM
WGHT 0.087600 0.046800
EXTI 0.014977
BASF 0.47917
FVAR 5.25715
O1 4 0.209283 0.534332 0.310378 11.00000 0.10576 0.02267 =
0.02500 -0.00031 0.01315 0.00473
O2 4 0.226996 0.404354 0.409801 11.00000 0.05417 0.02061 =
0.02851 0.00087 0.00875 0.00001
O3 4 0.305927 0.578550 0.683828 11.00000 0.08536 0.03969 =
0.02619 0.00573 0.00527 0.00097
O4 4 0.206932 0.762627 0.691328 11.00000 0.08067 0.04346 =
0.02937 -0.00850 0.01839 0.00116
O5 4 0.253771 1.031405 0.473204 11.00000 0.10299 0.02332 =
0.03947 -0.00700 0.01406 -0.00160
O6 4 0.254240 0.954894 0.358844 11.00000 0.10068 0.02712 =
0.02858 0.00465 0.01450 -0.00187
O7 4 0.248865 0.479133 0.545005 11.00000 0.04701 0.02327 =
0.02480 0.00459 0.00561 -0.00097
H7 2 0.246372 0.427716 0.497508 11.00000 0.06067
N1 3 0.281714 0.186806 0.168648 11.00000 0.04188 0.02852 =
0.03345 -0.00616 0.00554 0.00066
H1 2 0.299302 0.104648 0.154830 11.00000 0.05526
N2 3 0.268173 0.268521 0.108810 11.00000 0.04909 0.03830 =
0.02931 -0.00639 0.00656 -0.00008
N3 3 0.244841 0.371312 0.138051 11.00000 0.05363 0.03684 =
0.02543 0.00007 0.00592 -0.00063
N4 3 0.242852 0.358646 0.216450 11.00000 0.05376 0.02569 =
0.02317 -0.00173 0.00702 -0.00023
H4 2 0.232080 0.427376 0.252085 11.00000 0.05337
N6 3 0.279232 0.198604 0.307606 11.00000 0.06106 0.02419 =
0.03486 0.00328 0.00863 0.00031
H6A 2 0.266789 0.115789 0.316472 11.00000 0.04739
H6B 2 0.254322 0.253620 0.347240 11.00000 0.03449
N12 3 0.252870 0.945592 0.429911 11.00000 0.05003 0.02251 =
0.03028 -0.00093 0.00513 -0.00122
N13 3 0.253773 0.676648 0.653558 11.00000 0.04733 0.03491 =
0.02307 -0.00262 0.00647 -0.00451
C5 1 0.266282 0.243531 0.235710 11.00000 0.03495 0.02451 =
0.03161 -0.00502 0.00501 -0.00192
C7 1 0.248920 0.590913 0.519414 11.00000 0.03092 0.02463 =
0.02508 0.00141 0.00458 -0.00083
C8 1 0.252171 0.691663 0.569114 11.00000 0.03455 0.03115 =
0.02239 -0.00154 0.00499 -0.00185
C9 1 0.251643 0.808020 0.540998 11.00000 0.03699 0.02709 =
0.02655 -0.00603 0.00529 -0.00124
AFIX 43
H9 2 0.252148 0.874795 0.575371 11.00000 -1.20000
AFIX 0
C10 1 0.250361 0.824231 0.461579 11.00000 0.03695 0.02181 =
0.02778 0.00013 0.00569 -0.00126
C11 1 0.242995 0.728777 0.409598 11.00000 0.03622 0.02448 =
0.02400 -0.00027 0.00607 -0.00035
AFIX 43
H11 2 0.240017 0.742847 0.355051 11.00000 -1.20000
AFIX 0
C12 1 0.240052 0.613407 0.438003 11.00000 0.03315 0.02392 =
0.02327 0.00078 0.00531 0.00021
C13 1 0.225040 0.510705 0.381500 11.00000 0.04741 0.02306 =
0.02429 0.00026 0.00642 0.00051
HKLF 5
REM sathya17t1_a.res in P2(1)/c
REM wR2 = 0.1142, GooF = S = 1.042, Restrained GooF = 1.053 for all data
REM R1 = 0.0409 for 3644 Fo > 4sig(Fo) and 0.0443 for all 4182 data
REM 221 parameters refined using 6 restraints
END
WGHT 0.0876 0.0468
REM Highest difference peak 0.458, deepest hole -0.434, 1-sigma level 0.239
Q1 1 0.4986 0.0249 0.3311 11.00000 0.05 0.46
Q2 1 0.0015 0.9614 0.4822 11.00000 0.05 0.46
Q3 1 0.5013 0.0804 0.2576 11.00000 0.05 0.46
Q4 1 0.4990 0.7533 0.5765 11.00000 0.05 0.46
Q5 1 0.4993 0.8452 0.4635 11.00000 0.05 0.46
;
_shelx_res_checksum 46676
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
O O1 0.2093(3) 0.53433(10) 0.31038(7) 0.0508(4) Uani d 1 . .
O O2 0.22700(19) 0.40435(9) 0.40980(7) 0.0342(3) Uani d 1 . .
O O3 0.3059(3) 0.57855(12) 0.68383(7) 0.0507(4) Uani d 1 . .
O O4 0.2069(2) 0.76263(12) 0.69133(7) 0.0501(4) Uani d 1 . .
O O5 0.2538(3) 1.03140(11) 0.47320(8) 0.0549(4) Uani d 1 . .
O O6 0.2542(3) 0.95489(11) 0.35884(8) 0.0516(4) Uani d 1 . .
O O7 0.24886(18) 0.47913(9) 0.54500(6) 0.0317(3) Uani d 1 . .
H H7 0.246(4) 0.4277(15) 0.4975(8) 0.061(7) Uiso d 1 . .
N N1 0.2817(2) 0.18681(13) 0.16865(9) 0.0346(3) Uani d 1 . .
H H1 0.299(3) 0.1046(13) 0.1548(14) 0.055(6) Uiso d 1 . .
N N2 0.2682(2) 0.26852(14) 0.10881(9) 0.0388(4) Uani d 1 . .
N N3 0.2448(2) 0.37131(13) 0.13805(8) 0.0386(4) Uani d 1 . .
N N4 0.2429(2) 0.35865(12) 0.21645(8) 0.0341(3) Uani d 1 . .
H H4 0.232(3) 0.4274(16) 0.2521(12) 0.053(6) Uiso d 1 . .
N N6 0.2792(3) 0.19860(13) 0.30761(9) 0.0399(4) Uani d 1 . .
H H6A 0.267(3) 0.1158(12) 0.3165(12) 0.047(6) Uiso d 1 . .
H H6B 0.254(3) 0.2536(15) 0.3472(9) 0.034(5) Uiso d 1 . .
N N12 0.2529(2) 0.94559(12) 0.42991(9) 0.0344(3) Uani d 1 . .
N N13 0.2538(2) 0.67665(12) 0.65356(8) 0.0350(4) Uani d 1 . .
C C5 0.2663(3) 0.24353(14) 0.23571(10) 0.0304(4) Uani d 1 . .
C C7 0.2489(2) 0.59091(13) 0.51941(9) 0.0268(3) Uani d 1 . .
C C8 0.2522(2) 0.69166(15) 0.56911(9) 0.0293(4) Uani d 1 . .
C C9 0.2516(2) 0.80802(14) 0.54100(9) 0.0302(4) Uani d 1 . .
H H9 0.252148 0.874795 0.575371 0.036 Uiso calc 1 . .
C C10 0.2504(2) 0.82423(13) 0.46158(9) 0.0288(4) Uani d 1 . .
C C11 0.2430(2) 0.72878(13) 0.40960(9) 0.0281(4) Uani d 1 . .
H H11 0.240017 0.742847 0.355051 0.034 Uiso calc 1 . .
C C12 0.2401(2) 0.61341(13) 0.43800(9) 0.0267(3) Uani d 1 . .
C C13 0.2250(3) 0.51070(14) 0.38150(9) 0.0315(4) Uani 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
O1 0.1058(11) 0.0227(6) 0.0250(6) 0.0047(6) 0.0131(7) -0.0003(5)
O2 0.0542(7) 0.0206(6) 0.0285(6) 0.0000(4) 0.0088(5) 0.0009(4)
O3 0.0854(10) 0.0397(7) 0.0262(7) 0.0010(6) 0.0053(6) 0.0057(5)
O4 0.0807(10) 0.0435(8) 0.0294(7) 0.0012(6) 0.0184(6) -0.0085(5)
O5 0.1030(12) 0.0233(7) 0.0395(7) -0.0016(6) 0.0141(7) -0.0070(5)
O6 0.1007(11) 0.0271(6) 0.0286(7) -0.0019(6) 0.0145(7) 0.0046(5)
O7 0.0470(7) 0.0233(6) 0.0248(6) -0.0010(4) 0.0056(5) 0.0046(4)
N1 0.0419(7) 0.0285(7) 0.0334(7) 0.0007(5) 0.0055(6) -0.0062(6)
N2 0.0491(8) 0.0383(8) 0.0293(8) -0.0001(6) 0.0066(6) -0.0064(6)
N3 0.0536(9) 0.0368(8) 0.0254(7) -0.0006(6) 0.0059(6) 0.0001(6)
N4 0.0538(8) 0.0257(7) 0.0232(7) -0.0002(6) 0.0070(6) -0.0017(5)
N6 0.0611(9) 0.0242(7) 0.0349(8) 0.0003(6) 0.0086(7) 0.0033(6)
N12 0.0500(8) 0.0225(7) 0.0303(8) -0.0012(5) 0.0051(6) -0.0009(5)
N13 0.0473(8) 0.0349(8) 0.0231(7) -0.0045(6) 0.0065(6) -0.0026(5)
C5 0.0349(8) 0.0245(7) 0.0316(9) -0.0019(6) 0.0050(6) -0.0050(6)
C7 0.0309(7) 0.0246(8) 0.0251(8) -0.0008(5) 0.0046(6) 0.0014(6)
C8 0.0346(8) 0.0312(8) 0.0224(7) -0.0018(6) 0.0050(6) -0.0015(6)
C9 0.0370(8) 0.0271(8) 0.0265(8) -0.0012(6) 0.0053(6) -0.0060(6)
C10 0.0369(8) 0.0218(8) 0.0278(8) -0.0013(5) 0.0057(6) 0.0001(6)
C11 0.0362(8) 0.0245(8) 0.0240(8) -0.0003(6) 0.0061(6) -0.0003(6)
C12 0.0332(8) 0.0239(8) 0.0233(8) 0.0002(5) 0.0053(6) 0.0008(6)
C13 0.0474(9) 0.0231(7) 0.0243(8) 0.0005(6) 0.0064(7) 0.0003(6)
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'
O O 0.0492 0.0322 '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
C7 O7 H7 . . 105.5(12) ?
N2 N1 H1 . . 116.4(15) ?
C5 N1 H1 . . 134.1(15) ?
C5 N1 N2 . . 109.50(14) ?
N3 N2 N1 . . 107.38(13) ?
N2 N3 N4 . . 108.66(14) ?
N3 N4 H4 . . 123.2(14) ?
C5 N4 N3 . . 109.36(13) ?
C5 N4 H4 . . 127.4(14) ?
H6A N6 H6B . . 119.4(18) ?
C5 N6 H6A . . 121.8(13) ?
C5 N6 H6B . . 115.8(12) ?
O5 N12 O6 . . 123.11(14) ?
O5 N12 C10 . . 119.98(14) ?
O6 N12 C10 . . 116.91(13) ?
O3 N13 C8 . . 118.92(14) ?
O4 N13 O3 . . 122.68(15) ?
O4 N13 C8 . . 118.38(14) ?
N4 C5 N1 . . 105.11(15) ?
N4 C5 N6 . . 125.92(15) ?
N6 C5 N1 . . 128.93(16) ?
O7 C7 C8 . . 123.23(14) ?
O7 C7 C12 . . 119.67(14) ?
C8 C7 C12 . . 117.09(13) ?
C7 C8 N13 . . 120.70(14) ?
C9 C8 N13 . . 117.05(14) ?
C9 C8 C7 . . 122.25(14) ?
C8 C9 H9 . . 121.0 ?
C10 C9 C8 . . 118.00(15) ?
C10 C9 H9 . . 121.0 ?
C9 C10 N12 . . 119.59(14) ?
C9 C10 C11 . . 122.37(14) ?
C11 C10 N12 . . 118.03(14) ?
C10 C11 H11 . . 120.4 ?
C12 C11 C10 . . 119.14(14) ?
C12 C11 H11 . . 120.4 ?
C7 C12 C13 . . 119.89(13) ?
C11 C12 C7 . . 121.08(14) ?
C11 C12 C13 . . 119.03(14) ?
O1 C13 O2 . . 124.49(14) ?
O1 C13 C12 . . 117.90(14) ?
O2 C13 C12 . . 117.60(13) ?
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
O1 C13 . 1.242(2) ?
O2 C13 . 1.2796(19) ?
O3 N13 . 1.2327(19) ?
O4 N13 . 1.2176(19) ?
O5 N12 . 1.2113(18) ?
O6 N12 . 1.230(2) ?
O7 H7 . 0.997(7) ?
O7 C7 . 1.3200(18) ?
N1 H1 . 0.956(13) ?
N1 N2 . 1.368(2) ?
N1 C5 . 1.333(2) ?
N2 N3 . 1.267(2) ?
N3 N4 . 1.360(2) ?
N4 H4 . 0.989(12) ?
N4 C5 . 1.326(2) ?
N6 H6A . 0.940(13) ?
N6 H6B . 0.947(12) ?
N6 C5 . 1.327(2) ?
N12 C10 . 1.458(2) ?
N13 C8 . 1.463(2) ?
C7 C8 . 1.409(2) ?
C7 C12 . 1.417(2) ?
C8 C9 . 1.383(2) ?
C9 H9 . 0.9500 ?
C9 C10 . 1.379(2) ?
C10 C11 . 1.386(2) ?
C11 H11 . 0.9500 ?
C11 C12 . 1.375(2) ?
C12 C13 . 1.495(2) ?
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
O7 H7 O2 . 0.997(7) 1.520(12) 2.4576(15) 154.6(19) yes
N1 H1 O3 4_565 0.956(13) 2.098(17) 2.967(2) 150(2) yes
N1 H1 O7 4_565 0.956(13) 2.09(2) 2.8033(17) 130.2(19) yes
N4 H4 O1 . 0.989(12) 1.578(13) 2.5668(17) 178(2) yes
N6 H6A O6 1_545 0.940(13) 1.940(14) 2.8643(19) 167.4(19) yes
N6 H6B O2 . 0.947(12) 2.015(13) 2.9367(19) 163.7(17) 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 N13 C8 C7 . . . . 17.9(2) ?
O3 N13 C8 C9 . . . . -162.77(15) ?
O4 N13 C8 C7 . . . . -163.36(16) ?
O4 N13 C8 C9 . . . . 16.0(2) ?
O5 N12 C10 C9 . . . . -0.8(3) ?
O5 N12 C10 C11 . . . . 178.14(16) ?
O6 N12 C10 C9 . . . . 179.14(15) ?
O6 N12 C10 C11 . . . . -1.9(2) ?
O7 C7 C8 N13 . . . . -0.6(2) ?
O7 C7 C8 C9 . . . . -179.84(14) ?
O7 C7 C12 C11 . . . . -179.06(14) ?
O7 C7 C12 C13 . . . . 1.6(2) ?
N1 N2 N3 N4 . . . . 0.02(19) ?
N2 N1 C5 N4 . . . . 0.20(18) ?
N2 N1 C5 N6 . . . . -177.39(16) ?
N2 N3 N4 C5 . . . . 0.1(2) ?
N3 N4 C5 N1 . . . . -0.19(18) ?
N3 N4 C5 N6 . . . . 177.50(16) ?
N12 C10 C11 C12 . . . . -179.87(14) ?
N13 C8 C9 C10 . . . . 179.93(13) ?
C5 N1 N2 N3 . . . . -0.14(19) ?
C7 C8 C9 C10 . . . . -0.8(2) ?
C7 C12 C13 O1 . . . . 177.30(15) ?
C7 C12 C13 O2 . . . . -2.0(2) ?
C8 C7 C12 C11 . . . . 2.4(2) ?
C8 C7 C12 C13 . . . . -176.95(14) ?
C8 C9 C10 N12 . . . . -179.13(14) ?
C8 C9 C10 C11 . . . . 2.0(2) ?
C9 C10 C11 C12 . . . . -1.0(2) ?
C10 C11 C12 C7 . . . . -1.3(2) ?
C10 C11 C12 C13 . . . . 178.08(14) ?
C11 C12 C13 O1 . . . . -2.1(2) ?
C11 C12 C13 O2 . . . . 178.63(15) ?
C12 C7 C8 N13 . . . . 177.89(13) ?
C12 C7 C8 C9 . . . . -1.4(2) ?
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
_twin_individual_twin_matrix_11
_twin_individual_twin_matrix_12
_twin_individual_twin_matrix_13
_twin_individual_twin_matrix_21
_twin_individual_twin_matrix_22
_twin_individual_twin_matrix_23
_twin_individual_twin_matrix_31
_twin_individual_twin_matrix_32
_twin_individual_twin_matrix_33
1 0.5208(14) 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000
2 0.4792(14) -1.0002 -0.0002 -0.1095 0.0001 -0.9999 0.0001 0.0008 0.0001 0.9999
_cod_database_fobs_code 2022623