#------------------------------------------------------------------------------
#$Date: 2023-12-01 04:10:55 +0100 (Fri, 01 Dec 2023) $
#$Revision: 287920 $
#$URL: svn://www.crystallography.net/cod/cif/2/02/29/2022953.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_2022953
loop_
_publ_author_name
'Al Isawi, Wisam A.'
'Zeller, Matthias'
'Mezei, Gellert'
_publ_section_title
;
An octanuclear nickel(II) pyrazolate cluster with a cubic Ni8 core and
its methyl- and n-octyl-functionalized derivatives
;
_journal_coeditor_code XI2028
_journal_issue 12
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_page_first 1199
_journal_page_last 1206
_journal_paper_doi 10.1107/S2056989023010101
_journal_volume 79
_journal_year 2023
_chemical_formula_iupac
'(C16 H36 N) (C4 H12 N) [Ni8 (C3 H3 N2)12 (O H)6]'
_chemical_formula_moiety
'C16 H36 N +, C4 H12 N +, C36 H42 N24 Ni8 O6 2-'
_chemical_formula_sum 'C56 H90 N26 Ni8 O6'
_chemical_formula_weight 1693.21
_chemical_name_systematic
;
Tetrabutylazanium tetramethylazanium
hexa-\m~4~-hydroxido-dodeca-\m~2~-pyrazolato-hexahedro-octanickel
;
_space_group_crystal_system tetragonal
_space_group_IT_number 139
_space_group_name_Hall '-I 4 2'
_space_group_name_H-M_alt 'I 4/m m m'
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary dual
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-2018/3
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 2
_cell_length_a 16.6921(4)
_cell_length_b 16.6921(4)
_cell_length_c 12.4112(4)
_cell_measurement_reflns_used 8487
_cell_measurement_temperature 150(2)
_cell_measurement_theta_max 79.4875
_cell_measurement_theta_min 6.9223
_cell_volume 3458.09(16)
_computing_cell_refinement
;
SAINT V8.40B (Bruker, 2020)
;
_computing_data_collection
;
APEX4 v2021.10-RC6 (Bruker, 2021)
;
_computing_data_reduction
;
SAINT V8.40B (Bruker, 2020)
;
_computing_structure_refinement
;
SHELXL2018/3 (Sheldrick, 2015b),
ShelXle Rev1275(H\"ubschle et al., 2011)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 150(2)
_diffrn_detector_area_resol_mean 7.4074
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type
;
Bruker AXS D8 Quest diffractometer with PhotonIII_C14 charge-integrating and
photon counting pixel array detector
;
_diffrn_measurement_method 'omega and phi scans'
_diffrn_radiation_monochromator 'laterally graded multilayer (Goebel) mirror'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54178
_diffrn_reflns_av_R_equivalents 0.0515
_diffrn_reflns_av_unetI/netI 0.0287
_diffrn_reflns_limit_h_max 21
_diffrn_reflns_limit_h_min -21
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_k_min -19
_diffrn_reflns_limit_l_max 15
_diffrn_reflns_limit_l_min -15
_diffrn_reflns_number 10921
_diffrn_reflns_theta_full 67.679
_diffrn_reflns_theta_max 79.620
_diffrn_reflns_theta_min 6.921
_diffrn_source 'I-mu-S microsource X-ray tube'
_diffrn_source_current '1.0 mA'
_diffrn_source_voltage '50 kV'
_exptl_absorpt_coefficient_mu 2.863
_exptl_absorpt_correction_T_max 0.7543
_exptl_absorpt_correction_T_min 0.5966
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause et al., 2015)
;
_exptl_crystal_colour blue
_exptl_crystal_density_diffrn 1.626
_exptl_crystal_description block
_exptl_crystal_F_000 1760
_exptl_crystal_size_max 0.250
_exptl_crystal_size_mid 0.230
_exptl_crystal_size_min 0.190
_refine_diff_density_max 0.556
_refine_diff_density_min -0.403
_refine_ls_extinction_coef 0.00094(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2018/3 (Sheldrick, 2015b)
;
_refine_ls_goodness_of_fit_ref 1.122
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 109
_refine_ls_number_reflns 1094
_refine_ls_number_restraints 4
_refine_ls_restrained_S_all 1.120
_refine_ls_R_factor_all 0.0446
_refine_ls_R_factor_gt 0.0435
_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^)+(0.0406P)^2^+14.3393P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1125
_refine_ls_wR_factor_ref 0.1133
_reflns_number_gt 1052
_reflns_number_total 1094
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file xi2028sup1.cif
_cod_data_source_block 1
_cod_original_cell_volume 3458.09(18)
_cod_database_code 2022953
_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 0.535
_shelx_estimated_absorpt_t_max 0.612
_shelx_hkl_file
;
2 -2 0 32.8138 3.52201 1
2 -2 0 36.0313 2.85719 5
2 2 0 33.9473 4.40964 1
-2 2 0 34.4553 3.53967 1
-2 -2 0 35.0691 4.40115 1
-1 3 0 1296.43 85.1903 1
3 1 0 1408.80 86.4067 1
1 3 0 1332.19 86.2316 1
3 -1 0 1285.22 85.2247 1
1 -3 0 1282.50 85.1417 1
3 1 0 1305.71 86.0534 1
-1 -3 0 1259.81 85.9013 1
-3 1 0 1350.91 85.3240 1
3 -3 0 35.8107 4.29782 1
3 3 0 39.1891 5.81280 1
-3 -3 0 36.0115 3.35578 3
3 -3 0 34.4877 3.26577 5
-3 3 0 39.7839 4.58064 1
0 -4 0 51.8764 4.00396 3
0 4 0 56.4800 4.03835 3
0 -4 0 49.0754 5.88470 1
-4 0 0 49.7726 6.14848 1
0 4 0 52.2325 6.13404 1
4 -2 0 2188.40 148.308 1
-4 2 0 2458.22 148.570 1
4 2 0 2419.18 150.550 1
-2 4 0 2324.76 148.284 1
4 2 0 2171.63 149.715 1
2 4 0 2321.46 150.317 1
-2 -4 0 2273.26 149.847 1
2 -4 0 2259.23 148.205 1
4 4 0 2317.17 124.841 1
4 -4 0 1554.90 115.934 1
4 4 0 1691.60 119.379 1
-4 4 0 1738.57 116.222 1
-4 -4 0 1677.18 114.530 3
-1 -5 0 965.147 66.9621 1
1 5 0 986.350 67.4086 1
5 1 0 986.604 67.1530 1
1 -5 0 987.806 63.6063 5
1 5 0 983.388 63.2473 3
-1 5 0 957.306 63.4878 3
1 -5 0 959.959 66.0082 1
-1 5 0 994.753 66.3366 1
5 1 0 1012.34 67.5415 1
5 -1 0 983.998 66.3588 1
-1 -5 0 1008.16 63.2947 3
-5 1 0 1018.00 66.5575 1
5 -3 0 17.0356 2.36510 5
-3 -5 0 17.8676 2.26190 3
3 -5 0 17.2813 2.27738 5
5 3 0 25.7313 7.52939 1
3 -5 0 21.7826 4.23135 1
5 -3 0 19.6092 4.34162 1
-5 3 0 16.8726 4.41197 1
-3 5 0 17.9920 4.07073 1
-3 5 0 15.7737 2.68185 3
5 3 0 18.8089 6.98400 1
3 5 0 9.73522 3.68622 1
5 5 0 3714.45 253.783 1
-5 5 0 4175.83 250.354 1
5 -5 0 3716.15 249.954 1
5 5 0 3954.46 255.168 1
0 -6 0 2723.36 180.840 1
6 0 0 2951.10 181.844 1
0 6 0 2795.88 181.547 1
0 6 0 2664.41 176.906 3
6 -2 0 256.562 20.5144 1
2 6 0 247.721 22.1893 1
-2 6 0 259.470 20.2469 1
6 -2 0 246.621 17.5979 5
6 2 0 260.458 22.6213 1
2 -6 0 236.560 19.8880 1
6 2 0 243.044 21.8226 1
-2 6 0 245.262 17.6010 3
-2 -6 0 261.051 17.0656 3
-6 2 0 244.193 20.4061 1
-2 -6 0 278.229 22.3311 1
2 -6 0 234.759 17.2850 5
6 4 0 1214.49 83.3783 1
-4 6 0 1112.05 76.6034 3
4 -6 0 1092.79 75.6029 5
6 4 0 1170.07 82.3273 1
-4 -6 0 1198.71 75.7642 3
4 6 0 1144.21 82.8276 1
4 6 0 1147.70 82.2328 1
6 -4 0 1179.94 78.6972 1
6 -4 0 1127.69 75.8644 5
4 -6 0 1187.30 78.2262 1
-4 6 0 1197.04 78.2240 1
-6 4 0 1247.40 78.8243 1
-6 6 0 7847.52 462.976 1
6 -6 0 6846.78 460.894 1
6 6 0 6970.91 467.074 1
6 6 0 7213.86 468.656 1
1 -7 0 1220.59 87.4741 1
-1 7 0 1250.59 83.6414 3
-1 7 0 1409.34 89.0245 1
1 7 0 1298.17 89.7340 1
7 1 0 1324.03 90.0202 1
1 7 0 1275.70 83.3199 3
7 -1 0 1347.78 88.8033 1
7 1 0 1280.89 89.3699 1
-3 -7 0 550.551 35.4655 3
7 3 0 486.496 41.7750 1
-7 3 0 566.173 40.0530 1
7 -3 0 520.333 36.1772 5
3 -7 0 541.205 35.8957 5
3 7 0 545.508 43.2837 1
-3 7 0 496.593 36.3354 3
7 -3 0 547.390 40.1391 1
3 -7 0 538.853 39.0416 1
-3 7 0 575.973 39.5809 1
-5 -7 0 2098.92 143.004 3
5 -7 0 2136.11 145.580 1
-5 7 0 2305.06 146.119 1
7 5 0 2162.42 155.026 1
5 7 0 2115.80 152.711 1
5 7 0 2605.79 157.127 1
7 -5 0 2127.30 143.343 5
7 5 0 2250.98 153.392 1
5 -7 0 2098.15 143.083 5
-7 -5 0 2096.47 143.769 3
7 -5 0 2375.54 147.973 1
-7 5 0 2389.47 150.256 1
-7 -7 0 3302.32 211.545 3
7 -7 0 3143.18 210.995 5
-7 -7 0 3218.87 214.587 4
7 7 0 3321.14 225.687 1
-7 7 0 3476.48 216.333 1
0 -8 0 299.590 25.9134 1
8 0 0 276.917 25.8574 1
0 8 0 311.207 26.6452 1
0 8 0 261.021 19.5057 3
8 0 0 299.690 26.6799 1
2 -8 0 27.6870 8.10305 1
-2 8 0 24.9521 3.86389 3
-2 8 0 28.9411 8.42092 1
8 -2 0 27.0376 7.54141 1
8 -2 0 33.7793 8.53929 1
8 2 0 36.7797 10.5543 1
2 8 0 23.0234 7.91176 1
8 2 0 31.3713 9.63669 1
8 4 0 678.947 52.2653 1
8 4 0 551.882 47.8920 1
8 -4 0 520.411 41.8820 1
-4 -8 0 530.028 36.6105 3
4 8 0 647.977 51.6526 1
-8 -4 0 519.225 38.2581 3
-4 8 0 572.370 41.5977 1
4 -8 0 533.106 37.2630 5
8 -4 0 541.279 37.7320 5
4 -8 0 492.016 40.2039 1
4 8 0 543.481 48.0054 1
-6 -8 0 120.003 10.0884 2
8 6 0 105.290 26.1273 1
8 6 0 145.146 30.7908 1
8 -6 0 163.644 11.5164 5
6 8 0 104.781 26.1909 1
8 -6 0 118.451 15.4633 1
-8 -6 0 126.500 13.3120 4
-8 -6 0 121.006 11.2599 3
6 -8 0 52.1445 16.0437 1
6 -8 0 122.915 10.4566 5
-6 -8 0 120.408 12.9770 4
-6 -8 0 125.187 10.4467 3
-8 -8 0 254.050 19.4455 2
-8 -8 0 294.739 23.8788 4
8 -8 0 257.643 20.4463 6
8 -8 0 238.907 17.5610 2
8 -8 0 269.500 20.2115 5
-8 -8 0 257.041 20.6174 3
-1 9 0 224.064 15.7159 3
1 9 0 217.000 24.2971 1
1 -9 0 193.663 22.1605 1
9 -1 0 218.675 16.5737 5
-1 9 0 238.603 23.0654 1
-1 -9 0 210.691 23.7392 1
9 -1 0 218.487 23.4343 1
9 1 0 221.596 24.6944 1
3 -9 0 286.050 26.5271 1
9 3 0 268.772 31.6937 1
-3 9 0 269.655 21.9150 3
9 -3 0 324.824 22.2585 5
9 -3 0 289.809 28.2916 1
-3 9 0 318.343 34.1733 1
3 9 0 366.639 39.0043 1
9 -5 0 1093.93 65.1981 5
-5 9 0 953.339 77.1366 1
-5 -9 0 1051.66 67.8636 4
5 -9 0 1010.45 64.1712 5
9 -5 0 943.404 69.2078 1
9 -5 0 1014.86 65.1977 6
-9 -5 0 1007.76 65.7838 3
5 -9 0 659.775 67.8920 1
-9 -7 0 255.999 22.3421 4
-9 -7 0 219.520 18.0059 2
7 -9 0 233.312 18.8890 6
7 -9 0 217.382 16.1317 2
-7 -9 0 237.746 18.0519 2
-9 -7 0 245.865 19.9539 3
7 -9 0 240.132 18.5698 5
-7 -9 0 228.642 18.3781 3
9 -7 0 263.619 19.3271 5
-7 -9 0 262.860 22.1265 4
9 -7 0 243.248 19.2895 6
-9 -9 0 630.088 45.3610 4
9 -9 0 547.200 40.9099 5
9 -9 0 569.968 41.3592 6
10 0 0 1010.49 66.0388 5
0 -10 0 971.194 64.5519 2
2 -10 0 695.622 49.6567 2
10 -2 0 840.865 51.6706 5
-10 -2 0 739.011 54.0246 4
-4 -10 0 441.004 31.4224 2
4 -10 0 428.046 30.3022 2
-10 -4 0 452.946 33.9032 3
-4 -10 0 481.855 34.8745 4
10 -4 0 503.109 33.1080 5
-10 -4 0 463.370 35.7400 4
10 -4 0 441.382 32.7092 6
-10 -6 0 2265.49 147.956 4
-6 -10 0 2097.37 142.679 2
10 -6 0 2212.31 144.316 6
10 -6 0 2256.25 144.271 5
6 -10 0 2162.52 143.848 6
-10 -6 0 2124.74 143.111 2
-10 -6 0 2244.30 145.380 3
-6 -10 0 2342.80 147.304 4
-8 -10 0 29.2157 6.52944 4
10 -8 0 40.3734 6.16880 6
8 -10 0 28.5923 5.15777 6
-10 -8 0 33.9750 8.17652 3
10 -8 0 38.8301 6.11027 5
-8 -10 0 29.1788 4.51577 2
-10 -8 0 31.2786 6.96745 4
10 -10 0 734.702 52.2042 6
-10 -10 0 740.473 51.0322 2
-10 -10 0 772.140 56.1139 4
10 -10 0 747.947 52.0725 5
-11 1 0 1962.18 128.619 4
1 -11 0 1872.02 123.468 2
-1 -11 0 1911.11 123.811 2
-11 -1 0 1934.12 128.631 4
11 -1 0 1935.19 125.521 5
-3 -11 0 20.9378 3.40246 2
-11 -3 0 20.7096 5.40835 4
11 -3 0 24.2234 4.43524 6
-11 -3 0 18.5672 5.35571 3
-3 -11 0 21.6178 5.30945 4
3 -11 0 24.3121 3.00738 2
-11 -5 0 2652.71 168.133 4
-5 -11 0 2693.37 166.578 4
5 -11 0 2373.89 160.638 2
-5 -11 0 2403.57 162.286 2
-11 -5 0 2293.49 165.122 3
11 -5 0 2790.41 164.606 5
-11 -5 0 2424.23 162.937 2
11 -5 0 2552.79 164.118 6
11 -7 0 480.746 34.3066 6
-7 -11 0 431.864 32.4853 2
-7 -11 0 486.495 36.8299 4
-11 -7 0 460.517 37.6001 4
11 -7 0 466.475 34.3743 5
-11 -9 0 275.390 21.3041 2
9 -11 0 272.043 21.9208 6
-11 -9 0 304.702 26.3046 4
-9 -11 0 299.121 25.5692 4
11 -9 0 263.856 22.5657 5
-9 -11 0 276.784 21.1836 2
11 -9 0 281.669 22.5363 6
9 -11 0 255.067 23.3793 5
-11 -11 0 1365.73 80.5996 2
11 -11 0 969.339 77.1728 6
-11 -11 0 1011.44 81.1917 4
0 -12 0 3276.04 219.671 2
12 0 0 3452.08 222.023 5
-12 0 0 3597.08 225.596 4
-2 -12 0 841.308 55.9228 2
-12 -2 0 822.711 60.3118 3
-12 2 0 866.507 60.8091 4
-12 -2 0 842.794 61.1194 4
12 2 0 857.986 57.9267 5
2 -12 0 816.645 55.1799 2
12 -2 0 825.430 57.6593 6
12 -2 0 866.168 58.0449 5
12 -4 0 267.453 20.4944 5
4 -12 0 243.721 16.8636 2
-12 -4 0 274.216 24.4719 4
-4 -12 0 242.324 18.2655 2
-12 -4 0 208.343 21.6959 3
-12 -4 0 229.224 18.8299 2
-4 -12 0 225.499 20.2553 4
12 -4 0 248.209 20.2721 6
6 -12 0 688.526 48.8485 2
-6 -12 0 762.324 54.2893 4
-12 -6 0 616.851 53.9712 3
12 -6 0 803.858 52.7648 6
-12 -6 0 804.513 56.7642 4
-6 -12 0 750.123 50.6911 2
-12 -6 0 749.645 51.4710 2
12 -6 0 807.184 53.0103 5
-12 -8 0 7.12283 2.88957 2
-12 -8 0 6.58686 4.14326 4
-8 -12 0 7.25981 4.05615 4
-8 -12 0 4.88303 2.33855 2
12 -8 0 3.97334 2.39777 6
12 -8 0 2.10417 3.63215 5
-10 -12 0 497.873 40.1405 4
12 -10 0 558.236 37.7218 6
-12 -10 0 489.400 41.5103 4
-12 -10 0 476.933 36.0555 2
-10 -12 0 531.999 37.1307 2
-12 -12 0 273.014 21.4258 2
-12 -12 0 300.674 25.1779 4
-13 -1 0 546.393 47.4085 3
1 -13 0 587.220 40.3139 2
13 -1 0 625.213 43.3888 5
-1 -13 0 595.991 40.7273 2
-13 1 0 547.507 51.9852 4
13 -1 0 598.593 42.8742 6
-13 -1 0 610.030 46.6742 4
13 1 0 707.519 43.9175 5
13 -3 0 9.79514 4.11383 5
13 -3 0 11.1450 3.41693 6
3 -13 0 9.99874 2.18668 2
-3 -13 0 11.0421 2.76857 2
13 3 0 12.5796 4.36458 5
-13 -3 0 8.55614 4.33764 4
5 -13 0 542.333 36.4893 2
-13 -5 0 552.425 39.5086 2
-5 -13 0 439.515 39.9173 4
13 -5 0 630.193 41.7824 5
13 -5 0 613.724 41.1844 6
-5 -13 0 577.950 38.9275 2
-13 -5 0 597.889 44.9839 4
13 -7 0 255.055 36.2221 5
13 -7 0 504.039 33.9244 6
-13 -7 0 469.461 32.2480 2
-13 -7 0 500.682 37.9369 4
-7 -13 0 484.986 31.8749 2
-7 -13 0 411.802 33.9566 4
13 9 0 121.809 11.2793 6
-9 -13 0 122.681 13.6587 4
-13 -9 0 131.373 15.2397 4
-9 -13 0 124.811 11.1459 2
-13 -9 0 122.547 11.3284 2
13 -9 0 119.399 12.1661 6
-11 -13 0 76.3632 10.3725 4
-13 -11 0 95.7051 9.07506 2
-13 -11 0 99.9441 12.2060 4
-11 -13 0 100.206 9.15246 2
-13 -13 0 1.23291 2.01767 4
-13 -13 0 3.19311 2.26277 2
14 0 0 0.27361 2.96820 5
-14 0 0 1.25018 2.65964 4
14 2 0 5.72590 2.56336 6
-14 -2 0 6.54176 3.99710 4
-14 2 0 5.87973 3.71334 4
14 -2 0 11.0323 4.26049 5
-2 -14 0 7.29224 2.39725 2
14 2 0 5.34960 3.48305 5
14 -2 0 6.52928 2.62964 6
2 -14 0 9.22254 2.17230 2
-4 -14 0 41.5685 5.33481 2
14 -4 0 52.3687 11.6057 5
14 -4 0 39.4149 6.35344 6
-14 -4 0 41.1080 8.35577 4
4 -14 0 37.1117 3.60156 2
-14 4 0 39.7005 7.70509 4
-14 -6 0 116.994 14.7508 4
-6 -14 0 122.414 10.6090 2
-14 -6 0 99.0050 10.8571 2
14 -6 0 116.011 11.9001 6
-14 6 0 111.830 14.1975 4
14 -6 0 114.183 12.8737 5
14 6 0 119.111 12.4659 5
14 8 0 75.8093 10.0325 5
14 -8 0 33.5032 10.5794 5
-8 -14 0 75.5966 7.76301 2
14 -8 0 79.5702 9.08777 6
14 8 0 79.7020 8.24846 6
-14 -8 0 75.7197 8.12056 2
-14 -8 0 76.6436 11.1737 4
-10 -14 0 51.9467 6.06488 2
-14 -10 0 52.4884 6.27679 2
14 -10 0 52.1386 6.91394 6
-10 -14 0 46.6520 6.94314 4
-14 -10 0 51.1014 8.63196 4
-14 -12 0 23.2691 5.07387 4
-12 -14 0 19.1161 3.91772 4
-12 -14 0 37.3278 6.04479 2
-14 -12 0 30.8811 4.21777 2
-14 -14 0 21.1308 3.13987 2
-1 -15 0 462.694 34.4160 2
1 -15 0 502.148 34.0903 2
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2 5 -13 186.699 13.7125 2
2 -5 13 167.707 14.0626 2
5 2 13 173.331 18.6597 4
-5 -2 -13 169.080 13.6541 2
-2 5 -13 186.362 14.0016 2
5 -2 13 159.828 16.6013 4
-2 -5 13 217.756 19.2042 4
5 2 -13 179.888 12.5292 2
2 5 13 200.244 17.1689 4
-5 2 13 168.305 16.2526 4
4 -5 13 250.951 17.0720 2
-4 -5 -13 222.660 15.8244 2
-5 4 -13 250.107 17.4085 2
5 4 13 214.906 19.8758 4
-5 -4 13 227.614 19.7119 4
4 -5 13 233.909 21.1921 4
4 5 -13 222.179 16.2669 2
-4 5 -13 223.998 17.3001 2
-5 -4 -13 233.713 16.3658 2
5 4 -13 232.491 16.0269 2
5 -4 13 237.674 21.4121 4
-4 -5 13 223.790 19.6584 4
4 5 13 235.857 20.1755 4
5 -4 13 230.157 16.8335 2
-6 1 -13 390.885 34.8965 2
1 -6 13 471.321 35.8279 2
-1 6 13 558.603 38.0207 4
1 6 -13 643.905 38.4709 2
-6 1 13 526.178 38.8042 4
1 6 13 633.696 38.3607 4
-1 6 -13 455.611 37.4011 2
-1 -6 13 345.066 39.0595 4
-6 -3 13 9.67189 3.14082 4
6 3 13 9.46260 3.58201 4
3 6 -13 11.6391 2.39548 2
3 -6 13 10.3067 3.47945 4
-6 3 -13 12.1711 2.74601 2
3 -6 13 11.8590 2.72755 2
-3 6 -13 8.70269 2.47677 2
6 3 -13 9.00772 1.35765 2
-6 -3 -13 11.6574 2.45232 2
6 -3 13 7.12822 3.30670 4
3 6 13 11.2525 3.75058 4
-3 -6 13 10.3245 3.62235 4
5 -6 13 424.649 32.8702 4
5 6 -13 486.272 30.1171 2
6 5 13 378.722 33.2186 4
-6 -5 13 408.741 33.0649 4
5 -6 13 475.399 30.6818 2
-5 -6 -13 447.310 29.7028 2
-6 5 -13 487.951 30.9607 2
-5 6 -13 466.362 30.8574 2
6 -5 13 505.158 33.8844 4
-6 -5 -13 473.958 30.0726 2
6 -5 13 478.261 30.8419 2
6 5 -13 457.922 29.6777 2
5 6 13 374.084 33.0775 4
-5 -6 13 470.516 33.8134 4
0 -7 13 221.903 14.9636 2
-7 0 -13 227.538 15.2876 2
0 7 -13 232.279 15.1748 2
7 0 13 233.810 18.5351 4
0 7 13 180.049 16.4004 4
0 -7 13 191.138 17.5389 4
-7 0 13 139.402 17.1250 4
7 2 13 187.033 15.9172 4
2 7 -13 185.793 12.3379 2
-7 -2 13 138.605 13.9218 4
2 -7 13 149.240 12.9628 2
-7 2 -13 184.441 12.6649 2
2 -7 13 164.217 14.8933 4
-2 -7 13 142.092 14.5150 4
7 -2 13 138.428 14.4104 4
-2 7 -13 177.856 12.5410 2
-7 -2 -13 171.933 12.3039 2
2 7 13 135.422 14.5762 4
7 4 13 103.182 11.3576 4
4 7 -13 132.985 8.91255 2
-7 -4 13 110.568 11.0293 4
-7 4 -13 123.125 9.27627 2
4 -7 13 120.295 11.0898 4
4 -7 13 108.714 9.38921 2
4 7 13 103.450 10.9978 4
-4 7 -13 121.973 9.21836 2
7 -4 13 79.4578 10.0215 4
-7 -4 -13 116.881 8.71767 2
-4 -7 13 100.592 10.9361 4
7 6 13 164.410 13.8766 4
6 -7 13 155.931 11.4619 2
6 7 -13 153.946 10.4509 2
-7 -6 13 99.5005 11.9835 4
-7 6 -13 141.302 10.9977 2
7 -6 13 139.877 10.9257 2
7 6 -13 161.632 10.2786 2
-6 -7 13 128.943 12.7461 4
-6 7 -13 139.814 10.9710 2
-7 -6 -13 157.582 10.7623 2
6 7 13 163.044 13.7437 4
1 -8 13 19.2195 2.92755 2
-8 -1 13 17.2472 3.50124 4
8 1 13 15.8355 3.85823 4
-8 1 -13 18.2766 2.97680 2
1 -8 13 16.6785 3.83486 4
1 8 -13 20.4978 2.93701 2
-8 -1 -13 19.3245 2.89906 2
8 -1 13 16.3126 3.92734 4
-1 -8 13 21.9830 3.87331 2
-1 -8 13 18.1452 4.01090 4
-1 8 -13 21.0268 3.00727 2
8 3 13 2.76995 2.23868 4
3 8 -13 1.33423 1.02644 2
-8 3 -13 3.68642 1.62025 2
3 -8 13 1.36802 1.49040 2
3 -8 13 6.06796 2.33712 4
8 -3 13 1.54651 1.60803 4
-3 8 -13 4.47678 1.78900 2
3 8 13 1.26992 1.79189 4
-8 -3 -13 1.58662 1.24164 2
-3 -8 13 2.52178 1.96477 4
5 8 -13 23.4370 2.62012 2
-8 -5 13 20.1174 4.76134 4
5 -8 13 19.8831 3.33281 4
8 5 13 21.3436 4.18963 4
-8 5 -13 22.6746 2.97867 2
5 -8 13 21.4960 2.67452 2
5 8 13 26.6921 4.35209 4
-5 8 -13 24.6806 3.03871 2
-8 -5 -13 27.6006 2.83422 2
8 -5 13 12.2794 3.63593 4
-5 -8 13 14.2746 3.43945 4
8 7 13 5.95564 2.19657 4
7 8 -13 5.75545 1.01692 2
-8 7 -13 5.72609 1.49042 2
7 -8 13 5.86334 1.33703 2
-8 -7 13 2.52528 1.51482 4
-7 -8 13 4.48414 1.95490 4
7 8 13 4.76115 2.07484 4
-7 8 -13 5.41263 1.45175 2
-9 0 -13 61.3157 5.42018 2
0 -9 13 53.8964 5.09324 2
0 9 -13 68.7779 5.62357 2
0 -9 13 56.9556 6.69670 4
9 0 13 47.7902 6.67875 4
9 2 13 6.47814 2.54361 4
-9 2 -13 9.86328 2.02650 2
2 -9 13 7.48269 1.95893 2
-9 -2 13 6.25510 2.76356 4
2 -9 13 5.55500 2.16489 4
2 9 -13 7.53040 1.82652 2
-2 9 -13 9.80401 1.99872 2
9 -2 13 7.00464 2.46020 4
-9 -2 -13 7.11624 1.92371 2
-2 -9 13 3.78274 2.12173 4
4 -9 13 4.08367 1.64138 4
9 4 13 5.98422 2.32477 4
4 -9 13 7.33731 1.64096 2
4 9 -13 7.17287 1.58235 2
-9 4 -13 8.70530 2.41068 2
-9 -4 13 5.80040 2.18303 4
9 -4 13 4.20994 1.73381 4
-4 -9 13 2.78539 1.67511 4
-9 -4 -13 8.07132 1.61875 2
-4 9 -13 5.75428 1.76750 2
-9 -6 13 32.2041 4.03296 4
-9 6 -13 32.5642 3.31695 2
6 -9 13 39.9494 3.27539 2
6 9 -13 38.4865 2.90489 2
9 6 13 20.6463 3.91061 4
-9 -6 -13 39.6231 2.91082 2
-6 -9 13 20.7299 3.75208 4
-6 9 -13 38.0878 3.45811 2
6 9 13 20.5599 3.73323 4
-9 -8 13 27.4568 3.53677 4
9 8 13 28.2771 3.61006 4
-8 -9 13 22.2872 3.06081 4
-10 1 -13 147.690 9.83389 2
1 10 -13 144.451 9.67319 2
1 -10 13 90.0146 9.94007 4
1 -10 13 138.261 9.63282 2
-1 10 -13 170.672 10.4740 2
-1 -10 13 94.6720 10.6128 4
10 -1 13 112.440 10.7998 4
3 -10 13 20.2219 2.23259 2
10 3 13 10.5823 3.11551 4
-10 3 -13 18.9907 2.36201 2
10 -3 13 8.06947 2.26359 4
-3 10 -13 17.8769 2.28655 2
-3 -10 13 12.4707 3.11790 4
-10 -3 -13 10.7735 2.06219 2
5 10 -13 177.855 10.5426 2
-10 5 -13 149.816 10.8223 2
5 -10 13 160.867 10.7084 2
-5 10 -13 132.685 10.7694 2
-10 -5 -13 145.176 10.0860 2
-5 -10 13 117.350 11.4631 4
11 0 13 316.860 26.2988 4
0 11 -13 380.726 25.7721 2
-11 0 -13 468.504 26.0483 2
11 2 13 9.92049 2.24006 4
-11 2 -13 17.0460 2.20245 2
2 -11 13 20.1135 2.34470 2
2 11 -13 15.2387 2.01178 2
-11 -2 -13 19.3697 2.22822 2
-2 -11 13 12.7168 2.29986 4
-2 11 -13 14.2274 2.07571 2
-11 4 -13 136.922 9.91127 2
4 -11 13 133.216 10.0630 2
4 11 -13 135.709 9.09507 2
-11 -4 -13 128.399 9.13631 2
-4 -11 13 116.468 10.0054 4
1 12 -13 166.744 13.1242 2
-12 1 -13 205.873 14.0553 2
-12 -1 -13 189.795 12.7799 2
0 0 14 6.51509 2.79763 4
0 0 -14 7.64246 1.52240 2
1 -1 14 -0.5087 1.29920 4
-1 1 14 1.69840 1.96895 4
1 1 14 0.34433 1.53846 4
-1 1 -14 0.49943 0.90359 2
-1 -1 -14 0.63803 0.82419 2
1 1 -14 0.32105 0.74556 2
-1 -1 14 1.25670 1.78474 4
0 -2 14 62.1332 8.04510 4
0 2 14 59.2472 7.65668 4
-2 0 -14 57.5564 5.11232 2
-2 0 14 47.4563 6.97305 4
2 0 14 63.4319 8.14149 4
0 2 -14 59.1679 5.17028 2
2 2 -14 12.1469 1.77216 2
-2 2 -14 11.9032 2.19086 2
2 2 14 10.8036 3.24388 4
-2 -2 14 13.7226 3.72922 4
-2 2 14 11.8571 3.31871 4
-2 -2 -14 12.0807 1.71960 2
2 -2 14 13.4187 3.72168 4
1 -3 14 0.49064 1.66278 4
3 1 14 0.67400 1.72492 4
-3 -1 14 0.65925 1.37575 4
-3 1 -14 0.76330 1.02099 2
1 3 -14 0.73745 0.93836 2
-1 3 14 0.66622 2.10497 4
-3 -1 -14 0.83393 0.97587 2
-3 1 14 2.63228 2.05549 4
-1 3 -14 0.82766 1.04720 2
1 3 14 1.41973 1.71534 4
-1 -3 14 0.82260 1.72715 4
3 -1 14 0.38039 1.58815 4
-3 3 -14 22.6356 2.93262 2
3 -3 14 18.5543 4.11497 4
3 3 14 22.6668 4.37872 4
-3 -3 -14 16.8538 2.10312 2
-3 -3 14 22.1845 4.39076 4
3 3 -14 21.9649 2.18539 2
-3 3 14 14.0630 4.08768 4
0 -4 14 88.7249 9.16703 4
0 4 -14 78.8571 6.15562 2
-4 0 -14 79.3346 6.14438 2
4 0 14 62.0922 8.11553 4
-4 0 14 56.8706 8.50931 4
0 4 14 53.5910 8.20437 4
-2 4 14 0.83461 1.96907 4
-4 2 -14 1.39845 1.13092 2
4 2 14 0.88233 1.67695 4
-4 -2 14 0.38733 1.31553 4
2 -4 14 0.80452 1.58008 4
2 4 -14 0.70192 0.83532 2
2 4 14 1.68002 1.84041 4
-2 -4 14 0.36195 1.42878 4
-4 -2 -14 1.99589 1.00492 2
-4 2 14 1.20809 2.00109 4
-2 4 -14 4.73596 1.77100 2
4 -2 14 1.34208 1.83935 4
4 -4 14 14.1278 3.32749 4
-4 4 -14 18.7092 2.57453 2
4 4 -14 19.3267 1.95863 2
4 4 14 9.27439 3.07210 4
-4 -4 14 19.9525 3.94207 4
1 -5 14 68.7597 8.49508 4
1 5 -14 96.3616 6.81979 2
-1 5 14 80.0394 10.1964 4
-5 1 -14 94.2558 6.97492 2
5 1 14 98.9984 9.66029 4
-5 -1 14 83.1026 8.81190 4
1 5 14 49.0444 7.51345 4
-5 -1 -14 92.7987 6.72979 2
5 -1 14 76.4904 8.86104 4
-1 5 -14 95.2955 7.02382 2
-5 1 14 77.0663 8.39601 4
-1 -5 14 77.3044 8.81121 4
5 3 14 8.13763 2.84934 4
3 5 -14 7.23872 1.27877 2
-5 -3 14 8.23193 3.13244 4
3 -5 14 6.35314 2.41514 4
-5 3 -14 9.91753 2.00952 2
-5 -3 -14 8.42801 1.88822 2
3 5 14 9.18720 3.35423 4
-3 -5 14 6.52338 2.45814 4
5 -3 14 7.43896 2.66682 4
-3 5 -14 9.81199 1.93388 2
5 -5 14 39.0031 5.29782 4
-5 -5 14 42.8488 5.84024 4
5 5 14 61.7403 6.61817 4
-6 0 -14 71.5900 5.78898 2
0 -6 14 58.0086 7.24004 4
-6 0 14 60.9337 7.93763 4
0 6 -14 68.8140 5.69963 2
6 0 14 72.8420 7.89786 4
-6 -2 14 12.2079 2.95406 4
-6 2 -14 24.8524 2.86437 2
2 6 -14 21.7743 2.36853 2
6 2 14 19.0208 3.83727 4
2 -6 14 27.0774 4.20124 4
-6 -2 -14 22.6253 2.44006 2
-2 -6 14 16.4991 3.62112 4
-2 6 -14 24.6904 2.88767 2
6 -2 14 12.1153 3.19964 4
2 6 14 21.1605 3.61879 4
4 6 -14 60.8679 4.00862 2
6 4 14 48.5048 6.44243 4
-6 -4 14 52.6724 5.96353 4
4 -6 14 31.3602 5.38444 4
-6 4 -14 59.9377 4.73349 2
-4 6 -14 64.5046 4.79684 2
6 -4 14 40.5025 5.55558 4
4 6 14 29.9261 5.05554 4
-4 -6 14 55.8625 6.97816 4
-6 -4 -14 50.0091 3.79616 2
-6 6 -14 49.7122 4.17055 2
-6 -6 14 36.4027 4.71346 4
1 -7 14 46.7253 5.46795 4
1 7 -14 56.0692 4.36009 2
7 1 14 37.7931 5.46180 4
-7 1 -14 48.2409 4.20262 2
7 -1 14 33.9416 5.10571 4
-1 7 -14 51.1023 4.24280 2
-1 -7 14 26.0993 4.74257 4
-7 -1 -14 48.6958 4.04140 2
3 -7 14 0.74920 1.11373 4
-7 -3 14 2.31448 1.60817 4
7 3 14 1.13739 1.24147 4
3 7 -14 2.48810 1.05137 2
-7 3 -14 1.69313 1.19699 2
-3 -7 14 0.35199 1.16695 4
7 -3 14 0.82016 1.35444 4
-3 7 -14 0.87966 0.81723 2
3 7 14 2.44952 2.42195 4
-7 -3 -14 2.34270 0.83115 2
-7 5 -14 26.3648 2.56844 2
5 -7 14 13.8239 2.55298 4
-7 -5 14 23.7445 3.71064 4
7 5 14 22.5347 3.36497 4
5 7 14 18.3587 3.68321 4
-5 7 -14 30.2073 2.83948 2
-5 -7 14 12.7665 2.80122 4
7 -5 14 27.9514 3.64950 4
0 8 -14 31.7843 3.38703 2
-8 0 -14 24.7983 2.90793 2
8 2 14 2.05818 1.32143 4
2 -8 14 2.73818 1.29598 4
2 8 -14 5.34701 1.24705 2
-8 2 -14 4.50325 1.22419 2
-2 -8 14 1.92453 1.35767 4
8 -2 14 4.22171 1.73709 4
-8 -2 -14 4.43203 1.12988 2
-2 8 -14 2.32466 0.88119 2
4 8 -14 0.32487 0.61925 2
8 4 14 -0.0337 0.83879 4
-8 4 -14 0.72233 0.68283 2
-4 8 -14 0.23460 0.70709 2
-4 -8 14 0.05901 0.80980 4
9 1 14 3.11207 1.42699 4
-9 1 -14 4.40423 1.26392 2
1 -9 14 1.71598 1.25024 4
1 9 -14 3.92363 1.09816 2
-1 -9 14 3.11447 1.33991 4
-1 9 -14 4.44079 1.14771 2
9 -1 14 2.48157 1.14472 4
-9 -1 -14 3.49438 0.97971 2
-9 3 -14 0.76647 0.74634 2
9 3 14 0.36742 0.79634 4
3 9 -14 0.61137 0.67980 2
-3 9 -14 0.62562 0.64544 2
-3 -9 14 0.62678 0.85825 4
1 0 15 2.15493 1.55910 4
0 -1 15 1.33991 1.45136 4
0 1 15 1.76051 1.48888 4
-1 0 15 2.87366 1.85215 4
-1 2 15 18.0261 3.48508 4
-2 -1 15 19.4333 3.22952 4
1 -2 15 15.7340 3.65561 4
2 1 15 9.27832 2.62571 4
-1 -2 15 15.3312 3.09831 4
-1 2 -15 18.5480 1.91700 2
1 2 15 10.2877 2.66755 4
2 -1 15 17.5150 3.66322 4
-2 1 15 17.2621 3.34890 4
3 0 15 6.26934 2.29033 4
0 -3 15 4.93535 2.07963 4
-3 0 15 8.22857 3.01351 4
3 2 15 5.65340 2.11096 4
-3 2 -15 5.18732 1.03046 2
2 -3 15 2.09007 1.46888 4
-3 -2 15 4.39240 1.73343 4
-2 -3 15 4.17529 1.74275 4
3 -2 15 4.23166 1.93059 4
2 3 15 4.87515 2.13628 4
-2 3 -15 5.29413 1.06705 2
1 -4 15 33.8019 4.24535 4
4 1 15 27.6259 4.01815 4
-4 1 -15 27.4753 2.30359 2
4 -1 15 16.0369 3.33036 4
-1 4 -15 34.6408 2.53230 2
4 3 15 2.28385 1.46809 4
-4 -3 15 2.24948 1.34836 4
3 -4 15 0.73920 1.01916 4
-4 3 -15 1.98180 0.76520 2
3 4 15 0.33993 1.22950 4
4 -3 15 1.29007 1.17231 4
-3 -4 15 2.19775 1.31150 4
-3 4 -15 2.17953 0.73490 2
5 0 15 79.9934 7.61994 4
0 -5 15 81.5500 7.54572 4
5 2 15 22.7862 3.34760 4
5 -2 15 23.2901 3.27540 4
-2 -5 15 21.2323 3.18605 4
-5 4 -15 1.63529 0.72730 2
4 -5 15 0.45108 1.26271 4
5 -4 15 0.23922 0.84243 4
-4 5 -15 2.11452 0.82656 2
-4 -5 15 1.58886 0.96467 4
1 -6 15 42.1824 4.60069 4
6 1 15 28.4602 3.86683 4
6 -1 15 28.1663 3.55811 4
-3 -6 15 24.2938 3.03634 4
0 0 0 0.00 0.00 0
_exptl_absorpt_process_details
)
SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
J. Appl. Cryst. 48 (2015) 3-10
)
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_max 0.7543
_exptl_absorpt_correction_T_min 0.5966
_exptl_special_details
)
The following wavelength and cell were deduced by SADABS from the
direction cosines etc. They are given here for emergency use only:
CELL 1.54184 16.694 16.686 12.410 90.019 89.992 89.956
)
;
_shelx_hkl_checksum 55723
_shelx_res_file
;
TITL Mezei_6_0m in I4/mmm
Mezei_6_0m.res
created by SHELXL-2018/3 at 16:39:22 on 08-Mar-2022
CELL 1.54178 16.69210 16.69210 12.41120 90.0000 90.0000 90.0000
ZERR 2.00 0.00035 0.00035 0.00040 0.0000 0.0000 0.0000
LATT 2
SYMM -X, -Y, Z
SYMM -Y, X, Z
SYMM Y, -X, Z
SYMM -X, Y, -Z
SYMM X, -Y, -Z
SYMM Y, X, -Z
SYMM -Y, -X, -Z
SFAC C H N O NI
UNIT 112 180 52 12 16
LIST 4 ! automatically inserted. Change 6 to 4 for CHECKCIF!!
TEMP -123.150
SIZE 0.25 0.23 0.19
L.S. 24
BOND $H
ACTA
CONF
HTAB
FMAP 2
PLAN 20
DFIX 1.53 C6 C7
DFIX 1.55 C7 C8
DFIX 0.84 O1 H1 O2 H2
REM EQIV $1 1-x, 1-y, +z
REM EQIV $2 +x, 1-y, 1-z
REM EQIV $3 1-x, +y, 1-z
REM BIND N4 C9_$1
REM BIND N4 C9_$2
REM BIND N4 C9_$3
WGHT 0.040600 14.339300
EXTI 0.000937
FVAR 0.28844 1.07625
NI1 5 0.410657 0.410657 0.120522 10.50000 0.02369 0.02369 =
0.01638 0.00026 0.00026 -0.00530
O1 4 0.500000 0.379776 0.000000 10.25000 0.03004 0.01518 =
0.01738 0.00000 0.00000 0.00000
H1 2 0.500000 0.329762 0.000000 10.25000 -1.50000
O2 4 0.500000 0.500000 0.162010 10.12500 0.01885 0.01885 =
0.01672 0.00000 0.00000 0.00000
H2 2 0.500000 0.500000 0.229668 10.12500 -1.50000
N1 3 0.332866 0.332866 0.054084 10.50000 0.04271 0.04271 =
0.02043 -0.00035 -0.00035 -0.02180
N2 3 0.459681 0.332718 0.226979 11.00000 0.03722 0.02680 =
0.02569 0.00671 0.00089 -0.00351
C1 1 0.278795 0.278795 0.087520 10.50000 0.08740 0.08740 =
0.02564 0.00085 0.00085 -0.06761
AFIX 43
H1A 2 0.266967 0.266967 0.160683 10.50000 -1.20000
AFIX 0
C2 1 0.243097 0.243097 0.000000 10.25000 0.12581 0.12581 =
0.02998 0.00000 0.00000 -0.10665
AFIX 43
H2A 2 0.202853 0.202853 0.000000 10.25000 -1.20000
AFIX 0
C3 1 0.434942 0.279465 0.300281 11.00000 0.05423 0.05662 =
0.05127 0.03069 0.00718 -0.00836
AFIX 43
H3 2 0.380575 0.267830 0.316641 11.00000 -1.20000
AFIX 0
C4 1 0.500000 0.244228 0.348214 10.50000 0.07572 0.08517 =
0.07561 0.05889 0.00000 0.00000
AFIX 43
H4 2 0.500001 0.204215 0.402647 10.50000 -1.20000
AFIX 0
N3 3 0.500000 0.000000 0.250000 10.06250 0.03197 0.03197 =
0.02895 0.00000 0.00000 0.00000
PART -1
C5 1 0.478341 0.072082 0.182617 10.25000 0.04200 0.03529 =
0.03145 0.00058 -0.00508 -0.00061
AFIX 23
H5A 2 0.468859 0.117955 0.231542 10.25000 -1.20000
H5B 2 0.427289 0.060735 0.144993 10.25000 -1.20000
AFIX 0
C6 1 0.540261 0.097031 0.098986 10.25000 0.05633 0.03412 =
0.05550 0.00567 -0.00252 -0.00704
AFIX 23
H6A 2 0.552850 0.050796 0.051982 10.25000 -1.20000
H6B 2 0.590225 0.113460 0.135851 10.25000 -1.20000
AFIX 0
C7 1 0.509344 0.166521 0.029993 10.25000 0.07610 0.03429 =
0.04362 0.01056 0.01814 -0.00024
AFIX 23
H7A 2 0.554558 0.188280 -0.012533 10.25000 -1.20000
H7B 2 0.490304 0.209624 0.078433 10.25000 -1.20000
AFIX 0
C8 1 0.440601 0.144031 -0.048292 10.25000 0.14128 0.05384 =
0.07985 0.03099 -0.02111 -0.00360
AFIX 137
H8A 2 0.428498 0.189868 -0.094870 10.25000 -1.50000
H8B 2 0.392763 0.129637 -0.006811 10.25000 -1.50000
H8C 2 0.457069 0.098365 -0.092701 10.25000 -1.50000
AFIX 0
PART 0
N4 3 0.500000 0.500000 0.500000 10.06250 0.08979 0.08979 =
0.08060 0.00000 0.00000 0.00000
PART -1
C9 1 0.468603 0.565954 0.439362 10.25000 0.12624 0.08007 =
0.17529 0.04950 -0.00506 -0.00399
AFIX 137
H9A 2 0.482964 0.616355 0.474958 10.25000 -1.50000
H9B 2 0.410149 0.561458 0.435149 10.25000 -1.50000
H9C 2 0.491223 0.565160 0.366504 10.25000 -1.50000
PART 0
AFIX 0
HKLF 4
REM Mezei_6_0m in I4/mmm
REM wR2 = 0.1133, GooF = S = 1.122, Restrained GooF = 1.120 for all data
REM R1 = 0.0435 for 1052 Fo > 4sig(Fo) and 0.0446 for all 1094 data
REM 109 parameters refined using 4 restraints
END
WGHT 0.0406 14.3397
REM Instructions for potential hydrogen bonds
EQIV $1 -x+1, -y+1, z
HTAB C9 N2_$1
EQIV $9 x, -y+1, z
HTAB C9 N2_$9
REM Highest difference peak 0.556, deepest hole -0.403, 1-sigma level 0.075
Q1 1 0.5000 0.5000 0.0000 10.06250 0.05 0.56
Q2 1 0.5000 0.5000 0.0484 10.12500 0.05 0.42
Q3 1 0.5000 0.5000 0.2688 10.12500 0.05 0.39
Q4 1 0.3383 0.3383 0.0000 10.25000 0.05 0.33
Q5 1 0.4210 0.3486 0.1808 11.00000 0.05 0.29
Q6 1 0.5301 0.2412 0.3008 11.00000 0.05 0.27
Q7 1 0.4123 0.5877 0.2965 10.50000 0.05 0.27
Q8 1 0.5000 0.5000 0.1918 10.12500 0.05 0.27
Q9 1 0.5304 0.4112 0.0569 11.00000 0.05 0.26
Q10 1 0.4298 0.4688 0.0778 11.00000 0.05 0.26
Q11 1 0.5000 0.2262 0.3033 10.50000 0.05 0.26
Q12 1 0.3556 0.3556 0.1079 10.50000 0.05 0.25
Q13 1 0.5000 0.0000 0.1806 10.25000 0.05 0.25
Q14 1 0.4710 0.4710 0.1378 10.50000 0.05 0.25
Q15 1 0.3934 0.4671 0.1748 11.00000 0.05 0.24
Q16 1 0.5000 0.1869 0.5000 10.25000 0.05 0.24
Q17 1 0.5000 0.3401 0.2356 10.50000 0.05 0.24
Q18 1 0.4565 0.3844 0.0387 11.00000 0.05 0.23
Q19 1 0.3815 0.2944 0.3247 11.00000 0.05 0.23
Q20 1 0.5000 0.2716 0.3670 10.50000 0.05 0.23
;
_shelx_res_checksum 82379
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'-x, y, -z'
'x, -y, -z'
'y, x, -z'
'-y, -x, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'y+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'y, -x, -z'
'-y, x, -z'
'x, -y, z'
'-x, y, z'
'-y, -x, z'
'y, x, z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, x+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
Ni Ni1 0.41066(2) 0.41066(2) 0.12052(4) 0.0213(3) Uani d 1 . .
O O1 0.500000 0.3798(2) 0.000000 0.0209(7) Uani d 1 . .
H H1 0.500000 0.3298(12) 0.000000 0.031 Uiso d 1 . .
O O2 0.500000 0.500000 0.1620(4) 0.0181(9) Uani d 1 . .
H H2 0.500000 0.500000 0.2297(17) 0.027 Uiso d 1 . .
N N1 0.33287(13) 0.33287(13) 0.0541(2) 0.0353(8) Uani d 1 . .
N N2 0.45968(14) 0.33272(13) 0.22698(17) 0.0299(5) Uani d 1 . .
C C1 0.27880(19) 0.27880(19) 0.0875(4) 0.0668(19) Uani d 1 . .
H H1A 0.266967 0.266967 0.160683 0.080 Uiso calc 1 . .
C C2 0.2431(3) 0.2431(3) 0.000000 0.094(4) Uani d 1 . .
H H2A 0.202853 0.202853 0.000000 0.113 Uiso calc 1 . .
C C3 0.4349(2) 0.2795(2) 0.3003(3) 0.0540(9) Uani d 1 . .
H H3 0.380575 0.267830 0.316641 0.065 Uiso calc 1 . .
C C4 0.500000 0.2442(4) 0.3482(5) 0.079(2) Uani d 1 . .
H H4 0.500001 0.204215 0.402647 0.095 Uiso calc 1 . .
N N3 0.500000 0.000000 0.250000 0.031(3) Uani d 0.5 . .
C C5 0.4783(6) 0.0721(7) 0.1826(9) 0.036(3) Uani d 0.25 A -1
H H5A 0.468859 0.117955 0.231542 0.043 Uiso calc 0.25 A -1
H H5B 0.427289 0.060735 0.144993 0.043 Uiso calc 0.25 A -1
C C6 0.5403(9) 0.0970(8) 0.0990(12) 0.049(3) Uani d 0.25 A -1
H H6A 0.552850 0.050796 0.051982 0.058 Uiso calc 0.25 A -1
H H6B 0.590225 0.113460 0.135851 0.058 Uiso calc 0.25 A -1
C C7 0.509(2) 0.1665(8) 0.0300(11) 0.051(6) Uani d 0.25 A -1
H H7A 0.554558 0.188280 -0.012533 0.062 Uiso calc 0.25 A -1
H H7B 0.490304 0.209624 0.078433 0.062 Uiso calc 0.25 A -1
C C8 0.4406(15) 0.1440(12) -0.0483(16) 0.092(7) Uani d 0.25 A -1
H H8A 0.428498 0.189868 -0.094870 0.137 Uiso calc 0.25 A -1
H H8B 0.392763 0.129637 -0.006811 0.137 Uiso calc 0.25 A -1
H H8C 0.457069 0.098365 -0.092701 0.137 Uiso calc 0.25 A -1
N N4 0.500000 0.500000 0.500000 0.087(5) Uani d 1 . .
C C9 0.4686(14) 0.5660(12) 0.4394(18) 0.127(13) Uani d 0.25 B -1
H H9A 0.482964 0.616355 0.474958 0.191 Uiso calc 0.25 B -1
H H9B 0.410149 0.561458 0.435149 0.191 Uiso calc 0.25 B -1
H H9C 0.491223 0.565160 0.366504 0.191 Uiso calc 0.25 B -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
Ni1 0.0237(3) 0.0237(3) 0.0164(4) -0.0053(2) 0.00026(15) 0.00026(15)
O1 0.0300(18) 0.0152(15) 0.0174(15) 0.000 0.000 0.000
O2 0.0188(13) 0.0188(13) 0.017(2) 0.000 0.000 0.000
N1 0.0427(12) 0.0427(12) 0.0204(16) -0.0218(16) -0.0004(9) -0.0004(9)
N2 0.0372(12) 0.0268(11) 0.0257(11) -0.0035(9) 0.0009(9) 0.0067(9)
C1 0.087(3) 0.087(3) 0.026(2) -0.068(4) 0.0009(13) 0.0009(13)
C2 0.126(7) 0.126(7) 0.030(3) -0.107(7) 0.000 0.000
C3 0.054(2) 0.057(2) 0.0513(19) -0.0084(17) 0.0072(17) 0.0307(17)
C4 0.076(4) 0.085(5) 0.076(4) 0.000 0.000 0.059(4)
N3 0.032(4) 0.032(4) 0.029(6) 0.000 0.000 0.000
C5 0.042(8) 0.035(5) 0.031(5) -0.001(4) -0.005(4) 0.001(4)
C6 0.056(8) 0.034(7) 0.055(8) -0.007(6) -0.003(7) 0.006(6)
C7 0.076(18) 0.034(5) 0.044(7) 0.000(11) 0.018(15) 0.011(4)
C8 0.14(2) 0.054(12) 0.080(13) -0.004(13) -0.021(15) 0.031(11)
N4 0.090(8) 0.090(8) 0.081(12) 0.000 0.000 0.000
C9 0.13(3) 0.080(14) 0.18(2) -0.004(14) -0.005(16) 0.050(16)
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'
Ni Ni -3.0029 0.5091 '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
N1 Ni1 N2 . . 96.51(9) ?
N1 Ni1 N2 . 24 96.51(9) ?
N2 Ni1 N2 . 24 95.35(13) ?
N1 Ni1 O2 . . 169.54(15) ?
N2 Ni1 O2 . . 90.51(10) ?
N2 Ni1 O2 24 . 90.51(10) ?
N1 Ni1 O1 . 19_565 90.44(9) ?
N2 Ni1 O1 . 19_565 169.90(11) ?
N2 Ni1 O1 24 19_565 91.11(8) ?
O2 Ni1 O1 . 19_565 81.65(11) ?
N1 Ni1 O1 . . 90.44(9) ?
N2 Ni1 O1 . . 91.11(8) ?
N2 Ni1 O1 24 . 169.90(11) ?
O2 Ni1 O1 . . 81.65(11) ?
O1 Ni1 O1 19_565 . 81.48(13) ?
N1 Ni1 Ni1 . 3_655 130.17(3) ?
N2 Ni1 Ni1 . 3_655 66.19(6) ?
N2 Ni1 Ni1 24 3_655 129.93(6) ?
O2 Ni1 Ni1 . 3_655 46.61(3) ?
O1 Ni1 Ni1 19_565 3_655 103.71(9) ?
O1 Ni1 Ni1 . 3_655 46.69(2) ?
N1 Ni1 Ni1 . 4_565 130.17(3) ?
N2 Ni1 Ni1 . 4_565 129.93(6) ?
N2 Ni1 Ni1 24 4_565 66.19(6) ?
O2 Ni1 Ni1 . 4_565 46.61(3) ?
O1 Ni1 Ni1 19_565 4_565 46.69(2) ?
O1 Ni1 Ni1 . 4_565 103.71(9) ?
Ni1 Ni1 Ni1 3_655 4_565 90.0 ?
N1 Ni1 Ni1 . 18 65.82(9) ?
N2 Ni1 Ni1 . 18 130.68(6) ?
N2 Ni1 Ni1 24 18 130.69(6) ?
O2 Ni1 Ni1 . 18 103.72(12) ?
O1 Ni1 Ni1 19_565 18 46.53(2) ?
O1 Ni1 Ni1 . 18 46.53(2) ?
Ni1 Ni1 Ni1 3_655 18 90.0 ?
Ni1 Ni1 Ni1 4_565 18 90.0 ?
Ni1 O1 Ni1 3_655 18 152.57(17) ?
Ni1 O1 Ni1 3_655 20_655 86.94(5) ?
Ni1 O1 Ni1 18 20_655 86.61(5) ?
Ni1 O1 Ni1 3_655 . 86.61(5) ?
Ni1 O1 Ni1 18 . 86.94(5) ?
Ni1 O1 Ni1 20_655 . 152.57(17) ?
Ni1 O1 H1 3_655 . 103.72(9) ?
Ni1 O1 H1 18 . 103.72(8) ?
Ni1 O1 H1 20_655 . 103.72(9) ?
Ni1 O1 H1 . . 103.71(8) ?
Ni1 O2 Ni1 2_665 4_565 86.77(5) ?
Ni1 O2 Ni1 2_665 3_655 86.77(5) ?
Ni1 O2 Ni1 4_565 3_655 152.6(2) ?
Ni1 O2 Ni1 2_665 . 152.6(2) ?
Ni1 O2 Ni1 4_565 . 86.78(5) ?
Ni1 O2 Ni1 3_655 . 86.78(5) ?
Ni1 O2 H2 2_665 . 103.72(12) ?
Ni1 O2 H2 4_565 . 103.72(12) ?
Ni1 O2 H2 3_655 . 103.72(12) ?
Ni1 O2 H2 . . 103.72(12) ?
C1 N1 N1 . 18 108.0(2) ?
C1 N1 Ni1 . . 137.8(3) ?
N1 N1 Ni1 18 . 114.18(9) ?
C3 N2 N2 . 22_655 108.0(2) ?
C3 N2 Ni1 . . 138.2(2) ?
N2 N2 Ni1 22_655 . 113.81(6) ?
N1 C1 C2 . . 109.8(4) ?
N1 C1 H1A . . 125.1 ?
C2 C1 H1A . . 125.1 ?
C1 C2 C1 18 . 104.4(6) ?
C1 C2 H2A 18 . 127.8 ?
C1 C2 H2A . . 127.8 ?
N2 C3 C4 . . 109.6(3) ?
N2 C3 H3 . . 125.2 ?
C4 C3 H3 . . 125.2 ?
C3 C4 C3 22_655 . 104.8(5) ?
C3 C4 H4 22_655 . 127.6 ?
C3 C4 H4 . . 127.6 ?
N3 C5 C6 . . 115.7(9) ?
N3 C5 H5A . . 108.4 ?
C6 C5 H5A . . 108.4 ?
N3 C5 H5B . . 108.4 ?
C6 C5 H5B . . 108.4 ?
H5A C5 H5B . . 107.4 ?
C5 C6 C7 . . 111.1(15) ?
C5 C6 H6A . . 109.4 ?
C7 C6 H6A . . 109.4 ?
C5 C6 H6B . . 109.4 ?
C7 C6 H6B . . 109.4 ?
H6A C6 H6B . . 108.0 ?
C6 C7 C8 . . 114.6(15) ?
C6 C7 H7A . . 108.6 ?
C8 C7 H7A . . 108.6 ?
C6 C7 H7B . . 108.6 ?
C8 C7 H7B . . 108.6 ?
H7A C7 H7B . . 107.6 ?
C7 C8 H8A . . 109.5 ?
C7 C8 H8B . . 109.5 ?
H8A C8 H8B . . 109.5 ?
C7 C8 H8C . . 109.5 ?
H8A C8 H8C . . 109.5 ?
H8B C8 H8C . . 109.5 ?
N4 C9 H9A . . 109.5 ?
N4 C9 H9B . . 109.5 ?
H9A C9 H9B . . 109.5 ?
N4 C9 H9C . . 109.5 ?
H9A C9 H9C . . 109.5 ?
H9B C9 H9C . . 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
Ni1 N1 . 2.013(3) ?
Ni1 N2 . 2.027(2) ?
Ni1 N2 24 2.027(2) ?
Ni1 O2 . 2.1710(12) ?
Ni1 O1 19_565 2.1742(9) ?
Ni1 O1 . 2.1742(9) ?
Ni1 Ni1 3_655 2.9826(8) ?
Ni1 Ni1 4_565 2.9826(8) ?
Ni1 Ni1 18 2.9916(11) ?
O1 H1 . 0.83(2) ?
O2 H2 . 0.84(2) ?
N1 C1 . 1.342(5) ?
N1 N1 18 1.343(6) ?
N2 C3 . 1.337(4) ?
N2 N2 22_655 1.346(5) ?
C1 C2 . 1.375(6) ?
C1 H1A . 0.9500 ?
C2 H2A . 0.9500 ?
C3 C4 . 1.371(5) ?
C3 H3 . 0.9500 ?
C4 H4 . 0.9500 ?
N3 C5 . 1.509(11) ?
C5 C6 . 1.523(18) ?
C5 H5A . 0.9900 ?
C5 H5B . 0.9900 ?
C6 C7 . 1.531(15) ?
C6 H6A . 0.9900 ?
C6 H6B . 0.9900 ?
C7 C8 . 1.55(2) ?
C7 H7A . 0.9900 ?
C7 H7B . 0.9900 ?
C8 H8A . 0.9800 ?
C8 H8B . 0.9800 ?
C8 H8C . 0.9800 ?
N4 C9 . 1.433(19) ?
C9 H9A . 0.9800 ?
C9 H9B . 0.9800 ?
C9 H9C . 0.9800 ?
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
N1 N1 C1 C2 18 . . . 0.000000 ?
Ni1 N1 C1 C2 . . . . 180.000000 ?
N1 C1 C2 C1 . . . 18 0.0000(10) ?
N2 N2 C3 C4 22_655 . . . -0.2(5) ?
Ni1 N2 C3 C4 . . . . -179.9(4) ?
N2 C3 C4 C3 . . . 22_655 0.3(8) ?
N3 C5 C6 C7 . . . . 175.7(11) ?
C5 C6 C7 C8 . . . . -70(2) ?
_cod_database_fobs_code 2022953