#------------------------------------------------------------------------------
#$Date: 2023-11-01 04:16:27 +0100 (Wed, 01 Nov 2023) $
#$Revision: 287192 $
#$URL: svn://www.crystallography.net/cod/cif/2/02/29/2022931.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_2022931
loop_
_publ_author_name
'Kucheriv, Olesia I.'
'Golenya, Irina A.'
'Prysiazhna, Olena'
'Partsevska, Sofiia V.'
'Gural'skiy, Il'ya A.'
_publ_section_title
;
 Crystal structure and Hirshfeld surface analysis of
 bis(3-aminopyrazole-\kN 1)bis(3-aminopyrazole-\kN
 2)bis(nitrato-\kO)copper(II)
;
_journal_coeditor_code           WM5699
_journal_issue                   11
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_page_first              1100
_journal_page_last               1103
_journal_paper_doi               10.1107/S2056989023009295
_journal_volume                  79
_journal_year                    2023
_chemical_formula_iupac          '[Cu (N O3)2 (C3 H5 N3)4]'
_chemical_formula_moiety         'C12 H20 Cu N12 2+, 2(N O3 -)'
_chemical_formula_sum            'C12 H20 Cu N14 O6'
_chemical_formula_weight         519.96
_chemical_name_common
Bis(3-amino-1<i>H</i>-pyrazole-\k<i>N</i>^2^)bis(5-amino-1<i>H</i>-pyrazole-\k<i>N</i>^2^)bis(nitrato-\k<i>O</i>)copper(II)
_chemical_name_systematic
;
bis(3-aminopyrazole-\k<i>N</i>^1^)bis(3-aminoyrazole-\
\k<i>N</i>^2^)bis(nitrato-\k<i>O</i>)copper(II)
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_cell_angle_alpha                90
_cell_angle_beta                 97.6408(19)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.83222(18)
_cell_length_b                   9.9714(2)
_cell_length_c                   12.1043(2)
_cell_measurement_reflns_used    4669
_cell_measurement_temperature    200.0(2)
_cell_measurement_theta_max      75.5610
_cell_measurement_theta_min      5.0160
_cell_volume                     1056.56(4)
_computing_cell_refinement
;
CrysAlisPro (Rigaku OD, 2023)
;
_computing_data_collection
;
CrysAlisPro (Rigaku OD, 2023)
;
_computing_data_reduction
;
CrysAlisPro (Rigaku OD, 2023)
;
_computing_molecular_graphics
;
Olex2 (Dolomanov <i>et al.</i>,  2009)
;
_computing_publication_material
;
Olex2 (Dolomanov <i>et al.</i>,  2009)
;
_computing_structure_refinement
;
SHELXL (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      200.0(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.915
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0246
_diffrn_reflns_av_unetI/netI     0.0233
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6493
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.978
_diffrn_reflns_theta_min         5.770
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    2.046
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63088
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2023)
;
_exptl_crystal_colour            'clear light blue'
_exptl_crystal_density_diffrn    1.634
_exptl_crystal_description       prism
_exptl_crystal_F_000             534
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.448
_refine_diff_density_min         -0.427
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         2023
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0426
_refine_ls_R_factor_gt           0.0381
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0689P)^2^+0.4789P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1108
_refine_ls_wR_factor_ref         0.1137
_reflns_number_gt                1903
_reflns_number_total             2023
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            wm5699sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        1056.55(4)
_cod_database_code               2022931
_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   0.822
_shelx_estimated_absorpt_t_max   0.905
_shelx_hkl_file
;
   0   0  -1 21.0218 11.1387  14
   0   0  -2 31624.9 805.769  14
   0   0  -3 106.850 37.8252  14
   0   0  -4 174953. 4188.08  14
   0   0   4 173830. 4193.29  22
   0   0  -5 139.425 52.1558  14
   0   0   5 84.1819 42.3464  22
   0   0  -6 17704.7 466.799  11
   0   0   6 17871.7 654.241  22
   0   0  -6 18352.8 650.077  14
   0   0  -7-13.3324 59.8867  14
   0   0  -7 13.5412 21.0709  11
   0   0  -8 30338.2 793.997  20
   0   0  -8 32119.9 1136.33   3
   0   0  -8 32543.3 813.242  11
   0   0  -9 38.0724 25.6976  20
   0   0  -9 19.2661 29.6694  11
   0   0  -9-21.7897 73.4081   3
   0   0 -10 22229.6 1005.53   3
   0   0 -10 23303.2 646.865  11
   0   0 -11 53.5183 79.5126   3
   0   0 -11 55.9331 35.9063  11
   0   0 -12 13247.7 414.994  11
   0   0 -13 23.6070 29.9708  11
   0   0 -14 1120.32 73.9003  11
   0  -1   0 18.9908 10.3335  15
   0   1   1 100580. 2343.28  22
   0  -1  -1 98490.6 2340.39  14
   0  -1   1 100681. 2345.28  22
   0   1  -1 100250. 2341.48  14
   0   1   2 1961.22 99.7521  22
   0  -1  -2 1775.65 94.6743  14
   0   1  -2 1786.53 95.2673  14
   0  -1   2 1796.83 97.6343  22
   0  -1   3 814.518 79.2127  22
   0  -1  -3 913.790 81.0508  14
   0   1   3 910.607 83.5324  22
   0   1  -3 933.044 82.5742  14
   0   1  -4 67519.7 1707.49  14
   0  -1   4 64663.8 1706.40  22
   0  -1  -4 66446.3 1706.31  14
   0   1   4 68312.2 1713.43  22
   0   1  -5 28669.9 849.301  14
   0   1   5 28349.5 852.194  22
   0  -1  -5 26090.4 832.425  14
   0  -1  -6 35.0770 18.7592  11
   0   1  -6 10.6532 52.1490  14
   0  -1  -6 15.2480 20.7852   6
   0   1  -6 32.6199 19.5461  11
   0  -1  -7 81738.6 1951.41   6
   0   1  -7 82383.1 2218.41  14
   0  -1  -7 80895.7 1942.36  11
   0   1  -7 80439.2 1941.18  11
   0   1  -8 198.166 34.1629  20
   0  -1  -8 157.404 34.8005  11
   0  -1  -8 276.726 99.4424   3
   0  -1  -8 156.149 31.5552  20
   0   1  -8 204.995 36.4169  11
   0   1  -8 274.197 94.1618   3
   0  -1  -9 12026.5 661.139   3
   0   1  -9 12922.5 384.890  11
   0   1  -9 12437.9 673.679   3
   0   1  -9 11895.5 367.176  20
   0  -1  -9 12869.5 385.821  11
   0  -1 -10 1148.32 211.553   3
   0   1 -10 1013.67 198.212   3
   0   1 -10 1107.89 84.3827  20
   0  -1 -10 1197.25 91.9793  11
   0   1 -10 1330.68 95.6123  11
   0   1 -11 131.906 98.2557   3
   0   1 -11 64.3144 34.6101  11
   0  -1 -11-53.3465 73.3708   3
   0  -1 -12-8.96339 34.8696  11
   0   1 -12-22.1314 36.1875  11
   0   1 -13 5100.01 199.245  11
   0  -1 -13 5070.33 199.951  11
   0  -1 -14 54.6692 25.2455  11
   0   1 -14 14.1065 21.0271  11
   0  -2   0 43318.7 1062.70  15
   0  -2  -1 19973.3 496.623  14
   0   2  -1 19921.2 496.143  14
   0  -2  -2 475.401 49.5620  14
   0   2   2 481.834 50.8403  22
   0   2  -2 426.466 47.4905  14
   0  -2   2 392.287 47.5567  22
   0   2  -3 34266.7 927.772  14
   0  -2   3 35310.4 940.318  22
   0   2   3 35041.6 936.859  22
   0  -2  -3 36177.1 934.483  14
   0  -2   4 111899. 2750.64  22
   0   2  -4 111240. 2738.15  14
   0  -2  -4 112335. 2743.47  14
   0   2   4 109637. 2744.22  22
   0  -2  -5 3424.13 217.975  14
   0   2  -5 3382.74 217.135  14
   0  -2   5 3639.63 226.535  22
   0  -2  -6 25665.8 664.427   6
   0   2  -6 26158.4 848.545  14
   0  -2  -6 26176.9 650.770  11
   0   2  -6 25331.4 647.739  11
   0  -2  -6 25146.1 845.931  14
   0  -2  -6 24926.5 661.981  12
   0  -2  -7 7566.06 238.575  11
   0  -2  -7 7468.00 249.951   6
   0  -2  -7 7482.52 430.400   3
   0   2  -7 7427.67 423.443   3
   0   2  -7 7346.67 236.556  11
   0   2  -8 22221.5 597.369  11
   0  -2  -8 22255.1 611.209   6
   0  -2  -8 21825.3 893.849   3
   0   2  -8 21914.8 590.632  20
   0   2  -8 21966.0 892.528   3
   0  -2  -8 22685.8 600.990  11
   0  -2  -9 8232.44 532.871   3
   0   2  -9 9231.25 294.957  20
   0   2  -9 9217.54 302.208  11
   0   2  -9 7925.07 522.745   3
   0  -2  -9 9444.92 304.894  11
   0   2 -10 7473.90 270.222  11
   0   2 -10 7199.55 516.957   3
   0   2 -10 7529.60 261.281  20
   0  -2 -10 7593.10 272.048  11
   0  -2 -10 7508.63 528.445   3
   0   2 -11 142.605 40.4134  20
   0   2 -11 51.1832 103.634   3
   0  -2 -11 81.4525 36.6916  11
   0   2 -11 80.1845 36.4667  11
   0  -2 -11-26.0522 101.361   3
   0  -2 -12 1109.87 89.1231  11
   0   2 -12 1279.49 93.3256  11
   0   2 -13 630.416 61.0018  11
   0  -2 -13 628.783 62.7028  11
   0  -2 -14 2669.28 113.794  11
   0   2 -14 2565.96 110.641  11
   0  -3   0 91.0099 32.7756  15
   0   3  -1 51329.1 1210.55   3
   0  -3  -1 50780.2 1209.49   3
   0  -3  -2 210.679 35.0200   3
   0   3  -2 186.863 34.2336   3
   0   3  -3 31078.9 836.390  14
   0  -3  -3 30862.3 835.624  14
   0   3  -4 955.078 102.030  14
   0  -3  -4 1178.99 111.275  14
   0  -3  -5 1086.48 70.9080   7
   0  -3  -5 856.979 114.603  14
   0   3  -5 1098.33 125.927  14
   0   3  -6 4964.02 169.491  11
   0  -3  -6 5205.49 320.093   3
   0  -3  -6 5198.34 172.247  11
   0  -3  -6 5081.93 190.450   6
   0   3  -6 5211.19 320.364   3
   0  -3  -6 5133.57 189.597  12
   0  -3  -7 23366.4 635.200   6
   0   3  -7 23840.4 875.811   3
   0   3  -7 23080.7 609.512  11
   0  -3  -7 23728.9 612.207  11
   0   3  -7 22969.6 609.315  20
   0  -3  -7 23374.1 876.324   3
   0   3  -8 6811.99 232.575  11
   0   3  -8 6429.30 227.573  20
   0  -3  -8 6840.34 248.060   6
   0  -3  -8 6425.07 434.067   3
   0  -3  -8 7009.07 234.391  11
   0   3  -8 6199.15 425.372   3
   0   3  -9 29037.2 759.943  11
   0   3  -9 28965.2 755.979  20
   0  -3  -9 26274.3 1090.77   3
   0  -3  -9 28653.1 777.064   6
   0  -3  -9 28636.3 760.487  11
   0   3  -9 25787.5 1080.28   3
   0  -3 -10 1863.56 257.062   3
   0  -3 -10 1801.63 113.821  11
   0   3 -10 1906.27 110.856  20
   0   3 -10 1874.43 115.768  11
   0   3 -10 1718.14 249.276   3
   0  -3 -11 1182.79 92.1696  11
   0   3 -11 1524.14 97.1998  20
   0   3 -11 1245.98 94.8433  11
   0  -3  11 1329.41 96.3919   8
   0   3 -12 1238.81 87.8494  11
   0  -3 -12 1206.63 87.6862  11
   0  -3 -13 2313.49 114.074  11
   0   3 -13 2529.76 117.207  11
   0  -3 -14 42.2394 18.2692  16
   0  -4   0 70705.6 1774.41  15
   0  -4  -1 44674.7 1169.27  15
   0   4  -2 33101.7 816.052   3
   0  -4  -2 32586.3 814.202   3
   0   4  -3 48431.7 1238.54   3
   0  -4  -3 47891.2 1237.96   3
   0  -4  -4 3293.18 196.246   3
   0  -4  -4 3345.21 132.929  12
   0   4  -4 3323.08 197.856   3
   0  -4  -5 6084.03 213.958  12
   0   4  -5 6547.44 325.807   3
   0  -4  -5 6377.39 323.371   3
   0  -4  -6 36033.4 902.788  11
   0   4  -6 37898.9 1155.01   3
   0  -4  -6 38156.8 1158.70   3
   0  -4  -7 6451.27 211.349  11
   0   4  -7 6027.53 213.023  20
   0  -4  -7 6105.17 387.045   3
   0   4  -7 6509.03 396.809   3
   0   4  -7 6239.14 209.073  11
   0  -4  -7 6022.83 233.295   6
   0   4  -8 24878.6 643.074  20
   0  -4  -8 23937.3 666.832   6
   0  -4  -8 22807.5 927.980   3
   0  -4  -8 23232.4 632.667  11
   0   4  -8 23630.0 634.177  11
   0   4  -8 22404.2 923.619   3
   0  -4  -9 3649.17 164.103  11
   0  -4   9 4106.10 184.111   8
   0   4  -9 3311.96 331.367   3
   0  -4  -9 4230.66 190.690   6
   0   4  -9 4284.80 174.398  20
   0  -4  -9 3101.67 321.354   3
   0   4  -9 3736.66 165.413  11
   0   4 -10 5430.40 170.205  11
   0  -4  10 5641.75 186.263   8
   0  -4 -10 5278.85 168.071  11
   0   4 -11 299.006 46.7671  11
   0  -4  11 318.612 50.6318   8
   0   4 -11 270.618 43.5037  20
   0  -4 -11 201.055 41.5347  11
   0   4 -12 115.083 32.3840  11
   0  -4 -12 80.5442 29.6964  11
   0  -4 -13 50.1688 22.6121  16
   0  -4 -14 837.908 45.0657  16
   0  -5   0 40.4839 31.2174   1
   0  -5  -1 52694.2 1288.29   2
   0  -5  -1 52707.9 1400.72  15
   0  -5  -1 53214.3 1289.23   1
   0  -5  -2 16095.9 439.664   2
   0  -5  -2 16085.0 545.664  15
   0  -5  -2 16069.1 441.379  13
   0  -5  -3 41811.0 1032.48   2
   0  -5  -3 40992.5 1025.15  12
   0  -5  -3 41973.0 1040.27  13
   0  -5  -3 41812.0 1172.36  15
   0  -5   3 41239.5 1031.83   8
   0  -5   4 6213.55 220.774   8
   0  -5  -4 7025.53 230.871   7
   0  -5  -4 6534.38 232.310  13
   0  -5  -4 6590.53 223.226  12
   0  -5  -5 966.600 113.444   3
   0  -5   5 841.497 68.9197   8
   0  -5  -5 876.893 72.7006  12
   0  -5   6 38.5193 32.3709   8
   0  -5   6-3.03531 28.1091  17
   0  -5  -6 55.8436 33.7682   6
   0  -5  -6 40.8253 34.0009  12
   0   5  -6 26.5712 22.4882  20
   0  -5   7 10190.0 345.303   8
   0   5  -7 11125.4 330.837  20
   0  -5   7 10471.0 325.983  17
   0  -5   8 32.6034 35.8618   8
   0   5  -8 22.1456 26.5458  20
   0   5  -9 12556.2 367.079  20
   0  -5   9 11584.9 381.401   8
   0  -5  -9 12140.2 390.296   6
   0  -5  10 2612.89 143.303   8
   0   5 -10 2861.28 136.990  20
   0  -5  11 402.578 53.6850   8
   0   5 -11 401.445 48.3287  20
   0  -5 -12 560.160 50.9574  16
   0  -5 -13 1115.12 59.9212  16
   0  -6   0 9332.02 293.489   1
   0  -6   0 9005.53 279.313  13
   0  -6   1 31.3094 24.1700  13
   0  -6  -1 55.3748 36.0316   2
   0  -6  -1 19.2396 30.3487   1
   0  -6  -1 71.0486 43.4764  15
   0  -6  -1 6.14879 26.0736  13
   0  -6  -2 14591.2 544.058  15
   0  -6  -2 14956.5 430.395  13
   0  -6  -2 14812.2 408.562  12
   0  -6  -2 15118.4 428.883   2
   0  -6  -3 13800.7 386.914  16
   0  -6   3 13297.4 407.309   8
   0  -6  -3 14180.6 542.782  15
   0  -6  -3 14104.1 416.504  13
   0  -6  -3 13919.3 407.971   2
   0  -6  -3 14256.0 414.431   7
   0  -6  -3 14098.1 398.257  12
   0  -6   4 34483.9 896.540   8
   0  -6  -4 34138.7 870.612  16
   0  -6  -4 35204.2 892.620  12
   0  -6  -4 34496.4 909.484  13
   0  -6  -4 35024.5 903.079   7
   0  -6  -4 33945.4 1074.43  15
   0  -6  -5 39.9664 35.3413  12
   0  -6  -5 12.7786 37.3607   7
   0   6  -5 24.5053 22.8210  20
   0  -6   5-8.14265 30.3295   8
   0  -6  -5-12.9370 43.5847  15
   0  -6  -5 41.7664 24.3930  16
   0  -6  -6 42624.8 1119.00   7
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 -10   1   5 1761.41 82.9596  19
 -10  -1   4 135.606 29.7541  19
 -10   1   4 84.3343 25.8392  19
  10  -1  -3 289.927 40.7081  12
 -10  -1   3 280.190 38.0726  19
 -10   1   3 230.075 35.4086  19
  10  -1  -2 745.321 62.3027  12
 -10   1   1 7578.06 251.752   9
  10  -1  -1 7677.66 248.539  12
 -10   1   0 133.872 32.2372   9
  10  -1   0 23.8874 31.8608  12
  10   1   1 2862.53 122.008  12
  10  -1   1 3293.99 134.779  12
  10  -1   2 77.2110 26.9667  12
  10  -1   3 211.811 33.2142  12
 -10  -2   7 8.83494 13.3751  19
 -10   2   7 21.1595 14.1891  19
 -10  -2   6 1234.74 61.5507  19
 -10   2   6 1298.81 62.4186  19
 -10  -2   5 11.2254 18.3218  19
 -10   2   5 31.3659 18.7680  19
  10  -2  -4 1567.27 85.2812  12
 -10  -2   4 1604.93 78.2073  19
 -10   2   4 1672.93 78.7361  19
  10  -2  -3 16.8424 23.3861  12
 -10  -2   3 30.4402 20.2919  19
 -10   2   3 34.3622 20.0434  19
 -10   2   2 3922.63 161.196   9
  10  -2  -2 4142.88 159.614  12
 -10   2   1 63.3047 27.1085   9
  10  -2  -1 63.0532 31.1194  12
 -10   2   0 1166.81 76.5158   9
  10  -2   0 1226.10 79.2034  12
 -10   2  -1 35.8263 21.1173   9
  10  -2   1-30.7417 32.3110  12
  10  -2   2 1019.21 67.6306  12
 -10   3   6 40.6313 13.7745  19
 -10   3   5 1860.50 74.0953  19
  10  -3  -4 98.9352 27.3275  12
 -10   3   3 192.767 35.5175   9
  10  -3  -3 189.194 36.1759  12
  10  -3  -2 1397.29 82.5719  12
 -10   3   1 1759.59 95.6914   9
  10  -3  -1 2021.94 99.3013  12
 -10   3   0 8.18499 20.0980   9
  10  -3   0 54.3064 27.7846  12
 -10   3  -1 1332.86 75.2604   9
  10  -3   1 1255.88 75.1841  12
  10  -3   2 101.379 27.2299  12
  10  -4  -3-2.30352 20.0368  12
 -10   4   2 2006.36 94.5028   9
  10  -4  -2 1991.77 94.5608  12
  10  -4  -1 38.4917 22.4579  12
 -10   4   0 1556.99 79.3585   9
  10  -4   0 1441.31 77.9007  12
   0   0   0    0.00    0.00   0
TITL shS_157_IlGu_auto in P2(1)/n
REM P2(1)/n (#14 in standard setting)
CELL 1.54184   8.832218   9.971404  12.104254  90.0000  97.6408  90.0000
ZERR    2.00   0.000181   0.000201   0.000246   0.0000   0.0019   0.0000
LATT  1
SYMM -x+1/2, y+1/2,-z+1/2
SFAC C H N O Cu
UNIT 40.00 40.00 12.00 8.00 2.00
REM  CrysAlisPro recorded range (K): Min=199.8; max=200.2; aver:200.0
TEMP -73
TREF
HKLF 4
END
;
_shelx_hkl_checksum              8635
_shelx_res_file
;
TITL shS_157_IlGu_auto in P21/n #14
    shs_157_ilgu_auto.res
    created by SHELXL-2018/3 at 18:00:03 on 19-Sep-2023
REM reset to P21/n #14
CELL 1.54184 8.832218 9.971404 12.104254 90 97.6408 90
ZERR 2 0.000181 0.000201 0.000246 0 0.0019 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC C H Cu N O
UNIT 24 40 2 28 12
EQIV $1 1.5-X,-0.5+Y,1.5-Z
EQIV $2 1-X,-Y,1-Z
EQIV $3 -0.5+X,0.5-Y,0.5+Z
EQIV $4 0.5-X,0.5+Y,1.5-Z
EQIV $5 1-X,1-Y,1-Z
L.S. 10
PLAN  5
SIZE 0.05 0.1 0.1
TEMP -73.1(2)
CONF
HTAB N5 O1_$1
HTAB N5 N3_$2
HTAB N6 O3_$1
HTAB N6 O3_$3
HTAB N6 O1_$1
HTAB N2 N7_$2
HTAB N2 O1_$2
HTAB N2 O2_$2
HTAB C6 N6_$4
HTAB N3 O3
HTAB N3 O3_$5
HTAB N3 O2
MORE -1
BOND $H
fmap 2
acta
REM <olex2.extras>
REM <HklSrc "%.\\shs_157_ilgu_auto.hkl">
REM </olex2.extras>
WGHT    0.068900    0.478900
FVAR       4.82833
CU1   3    0.500000    0.000000    0.500000    10.50000    0.03619    0.02953 =
         0.03155    0.00466    0.00732    0.01035
N5    4    0.425763   -0.058095    0.727840    11.00000    0.03523    0.03244 =
         0.03209    0.00217    0.00694    0.00416
N4    4    0.392976    0.016203    0.632620    11.00000    0.03766    0.03404 =
         0.03465    0.00376    0.00684    0.00833
O3    5    0.751867    0.406546    0.588577    11.00000    0.07107    0.02932 =
         0.07061    0.00445    0.01970   -0.00275
N7    4    0.764629    0.283382    0.590027    11.00000    0.05181    0.03235 =
         0.04029    0.00134    0.00406   -0.00676
O1    5    0.890491    0.230454    0.622819    11.00000    0.04914    0.04320 =
         0.09387    0.00703    0.00440   -0.00196
C1    1    0.311114    0.240466    0.387361    11.00000    0.04232    0.03288 =
         0.03383    0.00419    0.01029    0.01172
N1    4    0.331178    0.110181    0.412429    11.00000    0.03831    0.03348 =
         0.03440    0.00372    0.00494    0.01043
O2    5    0.650586    0.210966    0.564196    11.00000    0.06660    0.04228 =
         0.09040   -0.00316   -0.03181   -0.01132
N6    4    0.353835   -0.081329    0.908645    11.00000    0.04983    0.04827 =
         0.03630    0.00179    0.01262    0.00204
N2    4    0.192445    0.051942    0.380691    11.00000    0.04688    0.03280 =
         0.05760    0.00042   -0.00531    0.00487
C4    1    0.344078   -0.017754    0.807711    11.00000    0.03444    0.03272 =
         0.03617   -0.00297    0.00805   -0.00587
C5    1    0.254743    0.087335    0.763940    11.00000    0.05539    0.04440 =
         0.05139    0.00077    0.02435    0.01562
C6    1    0.288058    0.103375    0.656969    11.00000    0.05631    0.04743 =
         0.04884    0.01058    0.01896    0.02309
C2    1    0.160219    0.263946    0.338916    11.00000    0.04817    0.03948 =
         0.04371    0.00484   -0.00008    0.01660
C3    1    0.090658    0.142326    0.336298    11.00000    0.04552    0.04620 =
         0.05793   -0.00183   -0.01206    0.00994
N3    4    0.427210    0.329044    0.401615    11.00000    0.04384    0.04669 =
         0.06801    0.01222    0.00549    0.00335
H3A   2    0.498652    0.305726    0.465249    11.00000   -1.20000
H3B   2    0.399846    0.422188    0.393271    11.00000   -1.20000
H6A   2    0.433690   -0.131527    0.927336    11.00000   -1.20000
H6B   2    0.323022   -0.033929    0.962395    11.00000   -1.20000
H2    2    0.177181   -0.028764    0.385333    11.00000   -1.20000
H5    2    0.488402   -0.116458    0.730962    11.00000   -1.20000
H3    2   -0.015838    0.116990    0.296222    11.00000   -1.20000
H6    2    0.254460    0.164938    0.608541    11.00000   -1.20000
H2A   2    0.122719    0.345628    0.306932    11.00000   -1.20000
H5A   2    0.190398    0.135208    0.797722    11.00000   -1.20000
HKLF 4
REM  shS_157_IlGu_auto in P21/n #14
REM wR2 = 0.1137, GooF = S = 1.107, Restrained GooF = 1.107 for all data
REM R1 = 0.0381 for 1903 Fo > 4sig(Fo) and 0.0426 for all 2023 data
REM 181 parameters refined using 0 restraints
END
WGHT      0.0690      0.4846
REM Highest difference peak  0.448,  deepest hole -0.427,  1-sigma level  0.074
Q1    1   0.8665  0.2176  0.5438  11.00000  0.05    0.43
Q2    1   0.6966  0.1995  0.5034  11.00000  0.05    0.39
Q3    1   0.3714  0.0946  0.4576  11.00000  0.05    0.28
Q4    1   0.2480  0.2543  0.3585  11.00000  0.05    0.26
Q5    1   0.1973  0.4985  0.2449  11.00000  0.05    0.25
;
_shelx_res_checksum              16184
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu Cu1 0.500000 0.000000 0.500000 0.03217(18) Uani d 1 . .
N N5 0.4258(2) -0.05809(18) 0.72784(15) 0.0330(4) Uani d 1 . .
N N4 0.3930(2) 0.01620(18) 0.63262(17) 0.0353(4) Uani d 1 . .
O O3 0.7519(2) 0.40655(17) 0.58858(17) 0.0561(5) Uani d 1 . .
N N7 0.7646(2) 0.28338(19) 0.59003(16) 0.0417(5) Uani d 1 . .
O O1 0.8905(2) 0.2305(2) 0.6228(2) 0.0625(5) Uani d 1 . .
C C1 0.3111(3) 0.2405(2) 0.38736(18) 0.0359(5) Uani d 1 . .
N N1 0.3312(2) 0.11018(18) 0.41243(15) 0.0354(4) Uani d 1 . .
O O2 0.6506(3) 0.2110(2) 0.5642(2) 0.0702(7) Uani d 1 . .
N N6 0.3538(3) -0.0813(2) 0.90865(17) 0.0442(5) Uani d 1 . .
N N2 0.1924(2) 0.0519(2) 0.38069(19) 0.0469(5) Uani d 1 . .
C C4 0.3441(3) -0.0178(2) 0.80771(19) 0.0341(5) Uani d 1 . .
C C5 0.2547(3) 0.0873(3) 0.7639(2) 0.0488(6) Uani d 1 . .
C C6 0.2881(3) 0.1034(3) 0.6570(2) 0.0498(6) Uani d 1 . .
C C2 0.1602(3) 0.2639(3) 0.3389(2) 0.0443(5) Uani d 1 . .
C C3 0.0907(3) 0.1423(3) 0.3363(2) 0.0516(6) Uani d 1 . .
N N3 0.4272(3) 0.3290(2) 0.4016(2) 0.0530(5) Uani d 1 . .
H H3A 0.499(4) 0.306(4) 0.465(3) 0.064 Uiso d 1 . .
H H3B 0.400(4) 0.422(4) 0.393(3) 0.064 Uiso d 1 . .
H H6A 0.434(4) -0.132(4) 0.927(3) 0.064 Uiso d 1 . .
H H6B 0.323(4) -0.034(4) 0.962(3) 0.064 Uiso d 1 . .
H H2 0.177(4) -0.029(4) 0.385(3) 0.064 Uiso d 1 . .
H H5 0.488(4) -0.116(4) 0.731(3) 0.064 Uiso d 1 . .
H H3 -0.016(4) 0.117(3) 0.296(3) 0.064 Uiso d 1 . .
H H6 0.254(4) 0.165(4) 0.609(3) 0.064 Uiso d 1 . .
H H2A 0.123(4) 0.346(4) 0.307(3) 0.064 Uiso d 1 . .
H H5A 0.190(4) 0.135(4) 0.798(3) 0.064 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
Cu1 0.0362(3) 0.0295(3) 0.0316(3) 0.01035(15) 0.00732(19) 0.00466(15)
N5 0.0352(9) 0.0324(9) 0.0321(9) 0.0042(7) 0.0069(7) 0.0022(7)
N4 0.0377(9) 0.0340(9) 0.0347(9) 0.0083(7) 0.0068(8) 0.0038(7)
O3 0.0711(12) 0.0293(8) 0.0706(12) -0.0027(8) 0.0197(10) 0.0045(8)
N7 0.0518(12) 0.0323(10) 0.0403(10) -0.0068(8) 0.0041(8) 0.0013(7)
O1 0.0491(10) 0.0432(10) 0.0939(15) -0.0020(8) 0.0044(10) 0.0070(10)
C1 0.0423(11) 0.0329(10) 0.0338(10) 0.0117(9) 0.0103(8) 0.0042(8)
N1 0.0383(9) 0.0335(9) 0.0344(9) 0.0104(7) 0.0049(7) 0.0037(7)
O2 0.0666(13) 0.0423(10) 0.0904(16) -0.0113(9) -0.0318(11) -0.0032(10)
N6 0.0498(11) 0.0483(11) 0.0363(10) 0.0020(9) 0.0126(8) 0.0018(9)
N2 0.0469(11) 0.0328(10) 0.0576(12) 0.0049(8) -0.0053(9) 0.0004(9)
C4 0.0344(11) 0.0327(10) 0.0362(11) -0.0059(8) 0.0080(9) -0.0030(8)
C5 0.0554(14) 0.0444(13) 0.0514(14) 0.0156(11) 0.0244(11) 0.0008(11)
C6 0.0563(15) 0.0474(13) 0.0488(13) 0.0231(12) 0.0190(11) 0.0106(11)
C2 0.0482(13) 0.0395(12) 0.0437(12) 0.0166(10) -0.0001(10) 0.0048(10)
C3 0.0455(14) 0.0462(14) 0.0579(15) 0.0099(11) -0.0121(12) -0.0018(11)
N3 0.0438(12) 0.0467(12) 0.0680(15) 0.0033(9) 0.0055(10) 0.0122(10)
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'
Cu Cu -1.9646 0.5888 '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
N4 Cu1 N4 . 3_656 180.0 ?
N4 Cu1 N1 . 3_656 91.01(7) ?
N4 Cu1 N1 . . 88.99(7) ?
N4 Cu1 N1 3_656 . 91.00(7) ?
N4 Cu1 N1 3_656 3_656 89.00(7) ?
N1 Cu1 N1 . 3_656 180.0 ?
N4 N5 H5 . . 120(2) ?
C4 N5 N4 . . 111.75(18) ?
C4 N5 H5 . . 128(2) ?
N5 N4 Cu1 . . 124.74(14) ?
C6 N4 Cu1 . . 130.97(17) ?
C6 N4 N5 . . 104.04(19) ?
O3 N7 O1 . . 120.1(2) ?
O3 N7 O2 . . 120.3(2) ?
O2 N7 O1 . . 119.5(2) ?
N1 C1 C2 . . 110.2(2) ?
N1 C1 N3 . . 122.1(2) ?
N3 C1 C2 . . 127.5(2) ?
C1 N1 Cu1 . . 135.03(16) ?
C1 N1 N2 . . 105.19(18) ?
N2 N1 Cu1 . . 119.06(14) ?
C4 N6 H6A . . 117(2) ?
C4 N6 H6B . . 115(2) ?
H6A N6 H6B . . 116(3) ?
N1 N2 H2 . . 123(3) ?
C3 N2 N1 . . 111.0(2) ?
C3 N2 H2 . . 126(3) ?
N5 C4 N6 . . 121.9(2) ?
N5 C4 C5 . . 106.7(2) ?
N6 C4 C5 . . 131.4(2) ?
C4 C5 H5A . . 127(2) ?
C6 C5 C4 . . 105.5(2) ?
C6 C5 H5A . . 127(2) ?
N4 C6 C5 . . 112.0(2) ?
N4 C6 H6 . . 120(2) ?
C5 C6 H6 . . 128(2) ?
C1 C2 H2A . . 125(2) ?
C3 C2 C1 . . 105.2(2) ?
C3 C2 H2A . . 129(2) ?
N2 C3 C2 . . 108.4(2) ?
N2 C3 H3 . . 123(2) ?
C2 C3 H3 . . 127.7(19) ?
C1 N3 H3A . . 111(2) ?
C1 N3 H3B . . 116(2) ?
H3A N3 H3B . . 117(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
Cu1 N4 . 1.9748(19) ?
Cu1 N4 3_656 1.9748(19) ?
Cu1 N1 . 2.0331(17) ?
Cu1 N1 3_656 2.0332(17) ?
N5 N4 . 1.368(3) ?
N5 C4 . 1.343(3) ?
N5 H5 . 0.80(4) ?
N4 C6 . 1.332(3) ?
O3 N7 . 1.233(3) ?
N7 O1 . 1.247(3) ?
N7 O2 . 1.245(3) ?
C1 N1 . 1.340(3) ?
C1 C2 . 1.403(3) ?
C1 N3 . 1.347(3) ?
N1 N2 . 1.364(3) ?
N6 C4 . 1.369(3) ?
N6 H6A . 0.87(4) ?
N6 H6B . 0.88(4) ?
N2 C3 . 1.334(3) ?
N2 H2 . 0.82(4) ?
C4 C5 . 1.375(3) ?
C5 C6 . 1.375(4) ?
C5 H5A . 0.88(3) ?
C6 H6 . 0.87(4) ?
C2 C3 . 1.358(4) ?
C2 H2A . 0.94(4) ?
C3 H3 . 1.03(3) ?
N3 H3A . 0.96(4) ?
N3 H3B . 0.96(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
N3 H3A O3 . 0.96(4) 2.71(3) 3.495(3) 139(3) yes
N3 H3A O2 . 0.96(4) 1.92(4) 2.849(3) 162(3) yes
N3 H3B O3 3_666 0.96(4) 2.20(4) 3.085(3) 153(3) yes
N6 H6A O3 2_646 0.87(4) 2.83(3) 3.480(3) 132(3) yes
N6 H6A O1 2_646 0.87(4) 2.22(4) 2.999(3) 149(3) yes
N6 H6B O3 4_566 0.88(4) 2.14(4) 3.019(3) 176(3) yes
N2 H2 N7 3_656 0.82(4) 2.60(4) 3.378(3) 159(3) yes
N2 H2 O1 3_656 0.82(4) 2.10(4) 2.908(3) 171(4) yes
N2 H2 O2 3_656 0.82(4) 2.40(4) 2.999(3) 131(3) yes
N5 H5 O1 2_646 0.80(4) 2.47(4) 3.093(3) 136(3) yes
N5 H5 N3 3_656 0.80(4) 2.82(4) 3.462(3) 139(3) yes
C6 H6 N6 2_556 0.87(4) 2.70(4) 3.438(3) 143(3) yes
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
Cu1 N4 C6 C5 . . . . -173.70(19) ?
Cu1 N1 N2 C3 . . . . 172.49(18) ?
N5 N4 C6 C5 . . . . 0.5(3) ?
N5 C4 C5 C6 . . . . 0.6(3) ?
N4 N5 C4 N6 . . . . 177.4(2) ?
N4 N5 C4 C5 . . . . -0.3(3) ?
C1 N1 N2 C3 . . . . 0.8(3) ?
C1 C2 C3 N2 . . . . 0.3(3) ?
N1 C1 C2 C3 . . . . 0.2(3) ?
N1 N2 C3 C2 . . . . -0.7(3) ?
N6 C4 C5 C6 . . . . -176.8(3) ?
C4 N5 N4 Cu1 . . . . 174.56(15) ?
C4 N5 N4 C6 . . . . -0.1(3) ?
C4 C5 C6 N4 . . . . -0.7(3) ?
C2 C1 N1 Cu1 . . . . -170.29(17) ?
C2 C1 N1 N2 . . . . -0.6(2) ?
N3 C1 N1 Cu1 . . . . 14.0(3) ?
N3 C1 N1 N2 . . . . -176.3(2) ?
N3 C1 C2 C3 . . . . 175.6(3) ?

_cod_database_fobs_code 2022931