#------------------------------------------------------------------------------
#$Date: 2022-10-07 02:53:21 +0100 (Fri, 07 Oct 2022) $
#$Revision: 278482 $
#$URL: svn://www.crystallography.net/cod/cif/2/24/41/2244195.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_2244195
loop_
_publ_author_name
'N\"ather, Christian'
'Jess, Inke'
'Krebs, Christoph'
_publ_section_title
;
 Synthesis, crystal structure and properties of
 <i>catena</i>-poly[[[bis(3-methylpyridine-\k<i>N</i>)nickel(II)]-di-\m-1,3-thiocyanato]
 acetonitrile monosolvate]
;
_journal_coeditor_code           JY2022
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2056989022009598
_journal_volume                  78
_journal_year                    2022
_chemical_formula_iupac          '[Ni (N C S)2 (C6 H7 N1)2], C2 H3 N'
_chemical_formula_moiety         'C14 H14 N4 Ni S2, C2 H3 N'
_chemical_formula_sum            'C16 H17 N5 Ni S2'
_chemical_formula_weight         402.17
_chemical_name_systematic
'<i>catena</i>-Poly[[[bis(3-methylpyridine-\k<i>N</i>)nickel(II)]-di-\m-1,3-thiocyanato] acetonitrile monosolvate]'
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2020.11.27 svn.r5f609507 for Rigaku Oxford Diffraction, GUI svn.r6214)
;
_cell_angle_alpha                90
_cell_angle_beta                 117.043(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.2934(9)
_cell_length_b                   11.7472(4)
_cell_length_c                   9.7341(5)
_cell_measurement_reflns_used    9752
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      77.2380
_cell_measurement_theta_min      4.5780
_cell_volume                     1863.11(18)
_computing_cell_refinement
;
CrysAlisPro (Rigaku OD, 2021)
;
_computing_data_collection
;
CrysAlisPro (Rigaku OD, 2021)
;
_computing_data_reduction
;
CrysAlisPro (Rigaku OD, 2021)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg & Putz, 1999)
;
_computing_publication_material
;
Publcif (Westrip, 2010)
;
_computing_structure_refinement
;
<i>SHELXL2016/6</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT2014/5</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      99.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.987
_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     1.54178
_diffrn_reflns_av_R_equivalents  0.0153
_diffrn_reflns_av_unetI/netI     0.0063
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            11840
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         77.664
_diffrn_reflns_theta_min         4.640
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.653
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70518
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2021)
;
_exptl_crystal_colour            'light green'
_exptl_crystal_density_diffrn    1.434
_exptl_crystal_description       plate
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.271
_refine_diff_density_min         -0.366
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     125
_refine_ls_number_reflns         1966
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0242
_refine_ls_R_factor_gt           0.0240
_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^)+(0.0356P)^2^+1.9913P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0657
_refine_ls_wR_factor_ref         0.0658
_reflns_number_gt                1955
_reflns_number_total             1966
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jy2022sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        1863.11(17)
_cod_database_code               2244195
_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   1 107.874 17.0615   1
   0   0  -1 88.7789 15.4427  37
   0   0   1 11.9484 11.6877  38
   0   0  -1 16.6868 12.4568  41
   0   0  -2 1342.25 49.9736  37
   0   0  -2 1307.89 42.7769  41
   0   0  -3 2.94562 27.9585  41
   0   0  -3 27.5389 32.3913  37
   0   0   3 24.0244 27.9093  38
   0   0   4 126834. 632.892   9
   0   0  -4 123246. 589.342  41
   0   0   4 121452. 663.289   1
   0   0   4 119413. 585.357  38
   0   0  -4 123823. 648.859  37
   0   0   5 5.89285 48.5732   1
   0   0   5-0.50338 22.8726   3
   0   0  -5 23.8409 33.0360  41
   0   0   5 44.4288 38.4660   8
   0   0   5 87.1485 48.4624   7
   0   0   5 49.1464 33.8270   9
   0   0  -5 13.4310 42.7012  37
   0   0  -5 6.61779 45.3938  40
   0   0   5 10.1020 32.9332  38
   0   0   6 128660. 794.964   9
   0   0   6 126020. 887.651   7
   0   0  -6 126975. 851.283  40
   0   0   6 127202. 867.521   1
   0   0   7 125.727 34.0803  30
   0   0   7 96.0669 48.6042   9
   0   0   7 89.6272 69.9024   7
   0   0  -7 61.4091 62.6850  40
   0   0   7 191.784 73.9010   1
   0   0   7 89.7901 42.5836   3
   0   0   7 68.0649 38.0044  15
   0   0   7 117.399 31.5591  14
   0   0  -7 70.9238 59.8991  37
   0   0   8 96949.7 431.184  14
   0   0   8 100633. 449.661  30
   0   0   8 101330. 490.154   3
   0   0   8 99846.6 476.691   4
   0   0   8 97833.3 440.993  15
   0   0   9 86.8020 45.1467   4
   0   0   9 67.5377 40.4698   3
   0   0  10 3927.36 71.2217   4
   0   2   0 10468.7 86.8079   8
   0  -2   0 9579.94 84.9413  38
   0   2   0 9205.71 87.7641  40
   0   2   0 10067.6 70.4451  36
   0  -2   0 9753.10 99.6397  35
   0   2   1 271146. 780.620  36
   0  -2  -1 262061. 790.346  35
   0   2   1 259667. 756.754   1
   0  -2   1 265218. 757.316   1
   0   2   1 271317. 849.888   9
   0   2   1 272330. 819.482   6
   0   2  -1 268344. 825.189  39
   0  -2   1 269344. 846.846  38
   0   2   2 106148. 448.005   1
   0  -2   2 108786. 449.004   1
   0   2   2 104540. 448.944   7
   0  -2   2 106039. 474.832   7
   0   2   2 104722. 463.967   9
   0   2   2 105121. 466.646   6
   0  -2  -2 107878. 457.424  41
   0   2  -2 106596. 456.372  39
   0   2  -2 107343. 468.895  37
   0   2   3 70432.0 413.544   7
   0  -2   3 68382.3 425.339   7
   0   2   3 70230.6 405.694   9
   0  -2   3 69315.4 402.479   1
   0   2   3 68267.2 405.536   1
   0   2  -3 67283.6 409.588  37
   0  -2   3 66542.0 435.511  38
   0   2  -3 68574.2 396.277  39
   0   2   3 65511.8 239.826  38
   0  -2  -3 70648.7 392.528  41
   0  -2  -4 7418.40 136.948  41
   0  -2   4 8007.33 168.136   7
   0   2   4 8002.89 150.161   9
   0   2   4 7808.04 158.846   7
   0   2   4 7846.18 158.773   1
   0  -2   4 8436.60 160.042   1
   0  -2   4 7747.35 137.524  35
   0   2  -4 7649.73 142.868  39
   0  -2   4 6931.71 156.368  38
   0   2  -4 7557.87 151.917  37
   0  -2  -4 7306.05 156.273  37
   0  -2  -5 102976. 616.618  41
   0   2   5 106039. 695.371   8
   0  -2   5 105380. 732.395   7
   0   2   5 108746. 667.286   9
   0   2   5 107438. 708.399   7
   0  -2   5 106126. 684.334   1
   0  -2   5 103833. 410.257   3
   0   2   5 105775. 690.175   1
   0   2   5 103936. 413.904   3
   0  -2   5 100533. 563.174  35
   0   2  -5 104394. 678.795  37
   0  -2  -5 107171. 701.836  37
   0   2  -5 105314. 634.644  39
   0  -2   5 101949. 693.685  38
   0   2   6 31389.4 410.931   1
   0  -2   6 30895.6 215.136   3
   0   2   6 31880.6 223.736   3
   0  -2   6 31435.8 408.761   1
   0   2   6 31617.1 382.017   9
   0   2   6 31474.1 420.816   7
   0   2   6 30986.9 398.319   8
   0  -2   6 30559.9 432.865   7
   0  -2  -6 30452.4 405.955  40
   0  -2   6 29458.7 394.419  38
   0  -2  -6 30733.5 405.305  37
   0   2  -6 30756.4 400.922  37
   0   2  -6 30406.3 358.860  39
   0  -2   7 23659.4 186.852  43
   0  -2  -7 23116.8 392.930  40
   0   2  -7 23774.1 194.029  19
   0  -2  -7 23858.3 387.858  37
   0   2  -7 23750.1 387.209  37
   0   2   7 23504.3 195.032  30
   0  -2   7 23775.5 186.301  30
   0   2   7 23331.5 193.971  14
   0   2   7 23083.3 180.106  24
   0  -2   7 22818.9 202.361   3
   0   2   7 23619.8 395.589   1
   0   2   7 23178.4 208.167   3
   0  -2   7 22882.2 387.391   1
   0   2   7 23477.0 201.984  15
   0  -2   7 23748.2 360.491   9
   0   2   7 23153.8 359.683   9
   0   2   7 22778.6 394.074   7
   0  -2   8 24541.5 194.623  30
   0  -2   8 24984.3 210.315   4
   0   2   8 25694.5 214.303   4
   0   2   8 25071.5 208.953  15
   0  -2   8 24487.4 215.370   3
   0   2   8 25540.5 220.504   3
   0  -2   8 23922.2 187.245  43
   0  -2   9 28300.9 212.604   4
   0   2   9 28654.8 212.354   4
   0   2   9 27513.9 198.651  15
   0  -2   9 26221.4 185.317  30
   0  -2   9 27035.1 219.071   3
   0   2   9 27411.8 219.388   3
   0   2  10 9167.42 97.0736   4
   0   2  10 9083.80 103.165  32
   0   4   0 45207.8 273.011   8
   0  -4   0 47081.3 323.288  35
   0   4   0 44839.6 224.970  36
   0   4   0 47323.9 300.128  40
   0  -4   0 46645.8 279.098  38
   0   4   1 34998.2 257.933   6
   0   4  -1 33971.6 208.189  36
   0  -4  -1 33296.8 256.276  35
   0   4   1 31744.8 198.628  36
   0   4  -1 33877.5 260.965  37
   0  -4   1 33264.9 282.740  35
   0   4  -1 32920.4 178.578   8
   0   4   1 34073.2 265.522   8
   0   4   1 32417.8 128.754   1
   0  -4   1 33971.8 139.409   1
   0   4  -1 33318.4 247.216  40
   0  -4   1 33930.8 267.087  38
   0   4  -1 34356.7 269.657  39
   0   4   2 76174.9 441.080   6
   0  -4  -2 73842.2 384.263  35
   0  -4   2 75483.2 473.807  35
   0   4   2 74671.1 465.881   8
   0   4   2 73386.8 367.824   7
   0  -4  -2 76382.5 453.926  41
   0   4  -2 76585.5 430.903  40
   0   4   2 72916.7 340.411   1
   0  -4   2 75401.0 346.854   1
   0  -4   2 74961.1 472.242  38
   0   4  -2 76916.6 447.810  39
   0   4   3 37863.4 344.616   6
   0   4  -3 36759.6 320.885  39
   0  -4   3 36618.7 362.049  38
   0   4   3 36027.6 357.548   8
   0   4   3 36936.6 293.743   7
   0   4   3 37550.0 346.307   9
   0  -4   3 35868.0 277.798   1
   0   4   3 35622.9 277.100   1
   0   4  -3 36439.5 318.404  40
   0  -4  -3 37130.4 332.437  41
   0  -4   3 36200.0 344.428  35
   0  -4  -3 36007.1 245.707  35
   0  -4   4 139227. 768.353  35
   0   4   4 133615. 488.539  11
   0   4   4 137088. 770.635   9
   0   4   4 137308. 717.305   7
   0  -4  -4 138098. 746.326  41
   0   4  -4 137153. 748.895  40
   0  -4   4 132714. 818.277  38
   0   4  -4 135455. 733.601  39
   0  -4   4 139791. 706.026   1
   0   4   4 139532. 711.629   1
   0   4   5 36607.1 383.296   1
   0  -4   5 35278.0 373.206   1
   0   4   5 35626.7 210.519   3
   0  -4   5 35778.6 206.795   3
   0   4  -5 35374.6 398.758  40
   0  -4  -5 35113.0 378.635  41
   0   4   5 35322.8 405.400   9
   0   4   5 35858.6 389.267   7
   0   4   5 35932.0 435.762   8
   0  -4  -5 36348.9 431.782  37
   0  -4   5 34183.5 431.006  38
   0   4  -5 34328.7 377.663  39
   0   4  -5 35366.5 404.365  37
   0  -4   5 36466.8 392.671  35
   0   4  -6 57264.5 572.129  37
   0   4   6 57612.2 546.755   1
   0   4   6 57594.9 301.196   3
   0  -4   6 57606.6 540.915   1
   0  -4   6 56663.8 296.526   3
   0  -4   6 56251.9 295.269  30
   0   4   6 55472.5 300.306  24
   0   4   6 57267.2 603.275   8
   0   4   6 55777.4 560.322   9
   0   4   6 57146.4 554.135   7
   0   4  -6 57581.1 322.034  19
   0   4  -6 56820.6 565.892  40
   0  -4   6 56311.4 319.537  42
   0  -4  -6 56771.3 598.118  37
   0   4  -6 56334.5 525.048  39
   0  -4   6 54739.2 608.005  38
   0  -4  -7 70314.1 729.079  40
   0  -4   7 66421.6 359.134  42
   0   4  -7 65291.9 649.118  40
   0  -4   7 67648.8 359.426  43
   0   4  -7 66942.3 360.011  19
   0  -4  -7 67782.1 690.817  37
   0  -4   7 63139.4 675.892  38
   0   4  -7 66008.2 654.648  37
   0  -4   7 66083.8 333.764  30
   0   4   7 68496.8 341.815   4
   0  -4   7 66539.8 336.506   4
   0   4   7 64840.7 345.602  24
   0   4   7 64371.6 673.792   8
   0   4   7 68191.7 369.455  15
   0  -4   7 65248.5 346.641   3
   0  -4   7 65901.3 621.232   1
   0   4   7 65883.1 349.786   3
   0   4   7 67118.0 629.212   1
   0  -4   8 3851.77 75.4768  30
   0   4   8 4170.29 94.1411  32
   0   4   8 3959.13 83.0955  33
   0   4   8 3806.17 78.7961  24
   0  -4   8 3986.09 79.7023   4
   0   4   8 4157.93 81.2995   4
   0   4   8 3750.47 88.5479  15
   0   4   8 3873.93 83.1624   3
   0  -4   8 3928.43 81.3517   3
   0  -4   8 3992.06 80.2921  43
   0   4   9 1376.85 55.2812  15
   0  -4   9 1339.19 42.0202  30
   0   4   9 1396.17 60.0490  32
   0  -4   9 1263.49 46.1199   4
   0   4   9 1320.48 46.9593   4
   0   4  10 11253.1 92.0088  15
   0   4  10 12116.8 106.826  32
   0  -6   0 131458. 708.634  35
   0  -6   0 130373. 618.017  38
   0   6  -1 194906. 865.587  40
   0  -6   1 193156. 884.512  38
   0   6   1 196417. 875.126   8
   0  -6  -1 195668. 887.954  35
   0  -6   1 196606. 950.090  35
   0   6   1 195319. 845.968   6
   0   6   2 34357.1 336.668   6
   0   6  -2 32805.1 322.498  40
   0   6  -2 33059.1 354.510  39
   0  -6   2 32676.4 353.790  38
   0   6   2 32614.6 188.404  11
   0   6   2 32695.8 187.971  13
   0   6   2 34753.6 357.957   8
   0   6  -2 32093.4 261.509  36
   0  -6  -2 31752.6 299.775  35
   0  -6  -2 31211.2 336.663  41
   0   6   3 5199.36 148.151   6
   0   6   3 4614.99 75.3419  13
   0   6   3 4723.86 75.2471  11
   0   6  -3 4561.39 62.5569  12
   0   6   3 5144.37 159.716   8
   0   6  -3 4306.27 134.902  37
   0  -6   3 4646.68 151.485  35
   0  -6  -3 4469.10 136.395  41
   0  -6   3 4552.80 150.131  38
   0   6  -3 4482.69 127.340  40
   0   6  -3 4626.14 138.968  39
   0   6  -4 105.526 21.2282  12
   0   6   4 62.6161 31.3838  11
   0   6  -4 241.716 54.3168  39
   0   6  -4 129.889 50.4257  40
   0  -6   4 106.362 57.3520  38
   0   6   4 135.383 59.8323   8
   0  -6   4 89.1424 53.9311  35
   0   6  -4 53.9146 49.9018  37
   0  -6  -4 96.9354 47.1867  41
   0  -6   5 36793.1 450.190  35
   0   6   5 37733.2 258.192  32
   0   6  -5 36561.7 432.431  40
   0   6   5 38315.5 493.349   8
   0   6   5 36983.8 250.889  24
   0  -6  -5 38417.2 503.912  37
   0   6  -5 35891.8 434.167  39
   0   6   5 36820.4 246.133  15
   0   6   6 2015.78 71.3808  15
   0   6   6 1933.69 72.7938  32
   0  -6   6 1931.42 58.4223  30
   0   6   6 1951.39 67.8345  24
   0   6   6 2055.67 135.138   8
   0   6  -6 2033.09 73.9858  19
   0   6   6 1922.34 61.9844  21
   0   6  -6 1881.84 113.008  40
   0   6  -6 1868.38 110.921  39
   0  -6  -6 2045.39 135.682  37
   0  -6   6 1804.59 131.179  38
   0  -6   7 96501.0 421.476  30
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   8   4   4 56861.1 641.649   7
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   8   4   6 14894.2 136.901   3
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   8   4   7 484.791 36.2097  15
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   8   6  -1 23567.5 343.687   6
   8  -6  -1 24726.9 323.450  38
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   8   6   1 183910. 644.053  13
   8  -6   1 189801. 1110.29  38
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   8   6   1 186968. 1127.93   6
   8   6   1 190504. 679.752  10
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   8   6   2 7755.89 111.527  10
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   8   6   3 22314.1 184.652  15
   8   6   3 21390.6 187.718  10
   8   6   3 21314.5 364.119   7
   8  -6   3 21857.4 394.183  38
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  18   6  -5 9871.82 120.816  10
 -18  -6   5 10415.6 117.036  28
 -18   6   5 9829.99 108.541  27
 -18  -6   4 3812.74 75.5175  26
 -18   6   4 3898.72 72.9662  25
  18   6  -4 3867.57 80.3180  10
 -18  -6   4 3903.96 74.9622  28
 -18   6   4 3785.97 68.1858  27
 -18  -6   3 5904.59 87.8855  26
 -18   6   3 6035.50 86.4962  25
  18   6  -3 5967.35 95.2027  10
 -18  -6   3 5884.82 87.6030  28
 -18  -6   2 2465.90 56.8398  26
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  18   6  -2 2402.07 62.2886  10
 -18  -6   2 2446.09 56.4728  28
 -18  -6   1 14380.9 116.036  26
 -18   6   1 14400.4 115.284  25
 -18  -6   0 835.806 31.0621  17
 -18  -6   0 860.332 29.5674  28
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  18   8  -7 17123.7 102.774  18
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  18   8  -6 3044.85 54.5611  18
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 -18  -8   5 3420.56 49.7385  28
 -18  -8   5 3174.41 49.9696  26
 -18  -8   4 8536.93 79.5805  28
 -18  -8   4 8043.24 77.6992  26
  18   8  -3 3999.32 60.9516  18
 -18  -8   3 4027.72 54.8582  28
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  18   8  -2 19800.1 117.528  18
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 -18  -8   1 112.071 13.3201  28
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 -19   1  10 11362.7 91.7912  23
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 -19   1   8 46773.7 243.756  23
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 -19  -1   8 48609.3 277.818  28
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 -19  -1   7 762.044 46.8170  27
 -19   1   7 758.573 52.5550  27
 -19  -1   7 748.319 47.4962  26
 -19   1   7 806.221 43.7133  28
 -19  -1   7 765.788 49.8070  28
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 -19  -1   7 660.849 46.4457  25
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 -19   1   6 56133.7 323.953  27
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 -19  -1   6 54489.7 306.238  28
 -19  -1   6 53840.3 298.914  25
 -19   1   6 55713.1 324.314  25
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 -19   1   5 1820.77 67.8220  27
 -19   1   5 1694.20 51.7025  28
 -19   1   5 1638.63 66.1764   5
 -19  -1   5 1624.52 64.9493   5
 -19  -1   5 1705.99 58.9554  26
 -19  -1   5 1758.87 60.3405  25
 -19   1   5 1761.32 67.9045  25
 -19  -1   4 10245.8 121.302  28
 -19   1   4 10526.3 134.073  27
 -19  -1   4 10460.4 128.990  27
 -19  -1   4 10684.1 134.098   5
 -19   1   4 10472.6 134.155   5
 -19  -1   4 10165.9 120.401  26
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 -19   1   4 10674.1 135.099  25
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  19   1  -3 9005.18 116.512  10
 -19  -1   2 664.649 37.8470  26
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 -19  -1   2 729.207 40.7404  17
 -19  -1   2 663.032 45.0968   5
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  19   1  -2 697.339 42.3603  10
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 -19   1   1 11179.7 118.052   5
  19   1  -1 11470.7 120.846  10
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 -19  -1   0 32294.6 182.977   5
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  19  -1   0 31028.3 190.596   3
  19   1   0 30230.0 184.990   3
 -19  -1   0 30212.2 152.468  25
 -19  -1  -1 5646.39 61.5428   5
 -19   1  -1 5744.60 62.6013   5
 -19  -3  10 16570.4 111.458  23
 -19  -3  10 16884.7 108.159  22
 -19  -3   9 9909.18 96.6610  22
 -19   3   9 9128.75 106.046  27
 -19  -3   8 2780.69 59.0382  22
 -19   3   8 2809.65 71.0314  27
 -19  -3   8 2763.92 67.5820  28
 -19  -3   7 14458.2 149.974  26
 -19   3   7 14919.7 153.038  27
  19   3  -6 144.360 31.3705  10
 -19  -3   6 124.465 38.0528  28
 -19  -3   6 128.788 39.8689  26
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 -19  -3   5 1162.99 42.6750  27
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 -19  -3   5 1191.92 52.5247   5
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 -19  -3   4 16545.3 139.562  27
 -19   3   4 16916.3 163.125  27
  19   3  -4 16644.1 158.711  10
 -19  -3   4 16776.4 155.342   5
 -19   3   4 17263.9 158.718   5
 -19  -3   4 17073.0 160.366  26
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 -19  -3   3 81069.6 366.914   5
 -19   3   3 81057.4 370.754   5
 -19  -3   3 79681.0 345.889  27
 -19  -3   3 79534.6 367.345  28
 -19   3   3 80393.3 380.707  27
 -19  -3   3 80322.4 375.224  17
  19   3  -3 80359.5 387.105  10
 -19  -3   3 81537.2 373.656  26
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 -19  -3   2 6053.33 85.0850   5
 -19   3   2 6263.31 88.2929   5
 -19  -3   2 6194.53 86.4125  28
 -19  -3   2 5928.08 89.5066  17
  19   3  -2 6088.83 95.5967  10
 -19  -3   2 5985.78 86.9014  26
 -19  -3   1 598.113 33.3083   5
 -19   3   1 632.222 34.5548   5
 -19  -3   1 596.520 32.3845  28
 -19  -3   1 577.319 36.1949  17
 -19  -3   1 627.364 34.7311  26
  19   3  -1 655.265 38.5690  10
 -19  -3   0 1744.87 39.0662  26
 -19  -3   0 1650.79 41.8736  17
 -19  -3   0 1704.35 38.0007   5
 -19   3   0 1742.80 39.0116   5
 -19  -3  -1 763.585 22.9334  17
 -19  -5   9 3851.05 52.6602  23
 -19  -5   8 181.829 28.1733  28
 -19  -5   8 180.071 25.2979  22
 -19  -5   8 187.153 29.5951  23
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  19   5  -7 45388.0 225.468  18
  19   5  -7 44637.7 232.901  10
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  19   5  -6 5967.35 85.6023  18
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  19   5  -5 558.009 39.7719  10
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 -19   5   4 24036.1 171.643  27
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  19   5  -3 5638.57 87.9262  10
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  19   5  -2 19857.9 157.853  10
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  19   5  -1 24898.0 162.464  10
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 -19  -5   0 173.926 17.7214  26
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  19   7  -7 59063.3 220.758  18
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  19   7  -6 2873.74 52.4257  18
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  19   7  -4 2643.90 54.5094  18
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 -21  -5   6 23545.8 136.011  28
  21   5  -5 8853.32 76.0224  18
 -21   5   5 8860.27 78.1385  27
 -21   5   4 1292.34 34.2601  25
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 -21  -5   3 2432.84 38.5392  26
 -21   5   3 2457.80 39.3618  25
 -21  -5   3 2497.59 37.1804  28
 -22   0   7 32.2905 21.1422  27
 -22   0   6 18617.3 123.024  25
 -22   0   6 19283.6 128.570  27
 -22   0   5-2.24134 22.6280  25
 -22   0   5 27.9076 23.4050  27
 -22   0   4 676.783 27.8388  25
 -22   0   4 707.411 33.3681   5
 -22   0   4 736.570 31.7216  27
 -22   0   3 6.57553 14.1758  25
 -22   0   3-2.75770 18.7585   5
 -22   0   3 16.5912 18.9503  27
 -22   0   2 39224.3 160.521   5
 -22   0   2 38891.8 154.954  27
 -22   2   8 1769.21 35.8877  27
 -22   2   7 27015.8 152.208  27
 -22  -2   7 26787.7 140.735  28
 -22   2   6 35956.5 185.166  25
 -22   2   6 36370.2 187.970  27
 -22   2   5 10768.2 94.6840  25
 -22   2   5 11060.0 96.1991  27
 -22   2   4-1.92599 22.1039  25
 -22  -2   4 15.8050 14.0469  27
 -22   2   4 52.5589 22.8374  27
 -22   2   3 10.2655 17.9294  25
 -22   4   7 2229.28 35.2597  27
 -22   4   6 23700.2 123.800  27
 -22  -4   6 25053.1 123.368  28
 -22   4   5 14739.5 93.7369  27
 -22  -4   5 14634.2 91.9027  26
 -22  -4   5 14586.2 89.6810  28
 -23   1   5 1247.81 26.8640  27
   0   0   0    0.00    0.00   0
TITL 3Pic16a in C2/c
REM C2/c (#15 with fixed user cell (not necessary: std = user cell)!)
CELL 1.54184  18.293367  11.747190   9.734090  90.0000 117.0425  90.0000
ZERR    4.00   0.000895   0.000433   0.000483   0.0000   0.0063   0.0000
LATT  7
SYMM -x, y,-z+1/2
SFAC C H N S Ni
UNIT 56.00 72.00 16.00 8.00 4.00
REM  CrysAlisPro recorded range (K): Min=99.9; max=100.1; aver:100.0
TEMP -173
TREF
HKLF 4
END
;
_shelx_hkl_checksum              23417
_shelx_res_file
;
TITL 3pic16ac2c_a.res in C2/c
    3pic16a.res
    created by SHELXL-2016/6 at 09:11:13 on 29-Sep-2022
REM Old TITL 3pic16ac2c in C2/c
REM SHELXT solution in C2/c
REM R1 0.078, Rweak 0.004, Alpha 0.024, Orientation as input
REM Formula found by SHELXT: C17 N6 S2 Ni
CELL 1.54178 18.293367 11.74719 9.73409 90 117.0425 90
ZERR 4 0.000895 0.000433 0.000483 0 0.0063 0
LATT 7
SYMM -X,+Y,0.5-Z
SFAC C H N Ni S
UNIT 64 68 20 4 8
L.S. 10
PLAN  5
TEMP -173
CONF
BOND $H
MORE -1
fmap 2
acta
REM <olex2.extras>
REM <HklSrc "%.\\3pic16A.hkl">
REM </olex2.extras>
WGHT    0.035600    1.991300
FVAR       4.40406
NI1   4    0.500000    0.119497    0.250000    10.50000    0.01446    0.01706 =
         0.01370    0.00000    0.00635    0.00000
N1    3    0.549648    0.112778    0.101484    11.00000    0.01756    0.02006 =
         0.01774   -0.00045    0.00795   -0.00159
C1    1    0.572309    0.082512    0.014057    11.00000    0.01344    0.01644 =
         0.01628    0.00105    0.00392   -0.00172
S1    5    0.603444    0.037982   -0.110913    11.00000    0.01886    0.02257 =
         0.02138   -0.00468    0.01220   -0.00378
N11   3    0.585399    0.240764    0.385954    11.00000    0.01721    0.01922 =
         0.01841   -0.00208    0.00844   -0.00100
C11   1    0.624536    0.228280    0.539936    11.00000    0.01897    0.02367 =
         0.01886   -0.00267    0.00874   -0.00296
AFIX  43
H11   2    0.607248    0.168907    0.584775    11.00000   -1.20000
AFIX   0
C12   1    0.689006    0.297583    0.637287    11.00000    0.01993    0.02882 =
         0.02447   -0.00684    0.01011   -0.00491
C13   1    0.712697    0.384287    0.569743    11.00000    0.02747    0.03050 =
         0.03242   -0.01050    0.01482   -0.01236
AFIX  43
H13   2    0.756660    0.433386    0.631780    11.00000   -1.20000
AFIX   0
C14   1    0.672069    0.399130    0.411481    11.00000    0.03585    0.02682 =
         0.03475   -0.00184    0.02026   -0.01008
AFIX  43
H14   2    0.687354    0.458893    0.363972    11.00000   -1.20000
AFIX   0
C15   1    0.608763    0.325573    0.323263    11.00000    0.02714    0.02231 =
         0.02449   -0.00055    0.01348   -0.00219
AFIX  43
H15   2    0.581066    0.335802    0.214608    11.00000   -1.20000
AFIX   0
C16   1    0.731698    0.274722    0.807944    11.00000    0.02836    0.04541 =
         0.02194   -0.00984    0.00698   -0.01406
AFIX 137
H16A  2    0.696992    0.226009    0.835783    11.00000   -1.50000
H16B  2    0.741856    0.346916    0.864123    11.00000   -1.50000
H16C  2    0.784063    0.236346    0.835127    11.00000   -1.50000
AFIX   0
PART -1
N21   3    0.495817    0.534349    0.037953    10.50000    0.07115    0.04566 =
         0.04306    0.00912    0.02797   -0.00224
C21   1    0.498953    0.588204    0.136865    10.50000    0.04396    0.02987 =
         0.03812    0.00911    0.02060    0.00306
C22   1    0.498056    0.655716    0.237982    10.50000    0.08007    0.03976 =
         0.07480    0.01726    0.05004   -0.00433
AFIX 137
H22A  2    0.511446    0.613590    0.333381    10.50000   -1.50000
H22B  2    0.443345    0.689575    0.200183    10.50000   -1.50000
H22C  2    0.538683    0.716083    0.258413    10.50000   -1.50000
AFIX   0
HKLF 4
REM  3pic16ac2c_a.res in C2/c
REM R1 =  0.0240 for    1955 Fo > 4sig(Fo)  and  0.0242 for all    1966 data
REM    125 parameters refined using      0 restraints
END
WGHT      0.0356      1.9913
REM Highest difference peak  0.271,  deepest hole -0.366,  1-sigma level  0.048
Q1    1   0.7244  0.1885  0.8365  11.00000  0.05    0.27
Q2    1   0.5317  0.0800  0.1815  11.00000  0.05    0.25
Q3    1   0.6818  0.4045  0.4956  11.00000  0.05    0.23
Q4    1   0.7051  0.3144  0.8572  11.00000  0.05    0.23
Q5    1   0.7093  0.3258  0.5947  11.00000  0.05    0.22
;
_shelx_res_checksum              38962
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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
Ni Ni1 0.500000 0.11950(2) 0.250000 0.01509(10) Uani d 1 . .
N N1 0.54965(7) 0.11278(9) 0.10148(12) 0.0185(2) Uani d 1 . .
C C1 0.57231(7) 0.08251(10) 0.01406(14) 0.0165(2) Uani d 1 . .
S S1 0.60344(2) 0.03798(3) -0.11091(4) 0.01977(10) Uani d 1 . .
N N11 0.58540(6) 0.24076(9) 0.38595(12) 0.0181(2) Uani d 1 . .
C C11 0.62454(8) 0.22828(11) 0.53994(15) 0.0204(3) Uani d 1 . .
H H11 0.607248 0.168907 0.584775 0.025 Uiso calc 1 . .
C C12 0.68901(8) 0.29758(12) 0.63729(16) 0.0244(3) Uani d 1 . .
C C13 0.71270(9) 0.38429(13) 0.56974(18) 0.0297(3) Uani d 1 . .
H H13 0.756660 0.433386 0.631780 0.036 Uiso calc 1 . .
C C14 0.67207(10) 0.39913(13) 0.41148(19) 0.0309(3) Uani d 1 . .
H H14 0.687354 0.458893 0.363972 0.037 Uiso calc 1 . .
C C15 0.60876(9) 0.32557(12) 0.32326(16) 0.0240(3) Uani d 1 . .
H H15 0.581066 0.335802 0.214608 0.029 Uiso calc 1 . .
C C16 0.73170(9) 0.27472(15) 0.80794(17) 0.0336(3) Uani d 1 . .
H H16A 0.696992 0.226009 0.835783 0.050 Uiso calc 1 . .
H H16B 0.741856 0.346916 0.864123 0.050 Uiso calc 1 . .
H H16C 0.784063 0.236346 0.835127 0.050 Uiso calc 1 . .
N N21 0.4958(3) 0.5343(3) 0.0380(4) 0.0525(8) Uani d 0.5 A -1
C C21 0.4990(2) 0.5882(3) 0.1369(4) 0.0366(7) Uani d 0.5 A -1
C C22 0.4981(19) 0.6557(4) 0.238(3) 0.059(3) Uani d 0.5 A -1
H H22A 0.511446 0.613590 0.333381 0.089 Uiso calc 0.5 A -1
H H22B 0.443345 0.689575 0.200183 0.089 Uiso calc 0.5 A -1
H H22C 0.538683 0.716083 0.258413 0.089 Uiso calc 0.5 A -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 0.01446(16) 0.01706(17) 0.01370(16) 0.000 0.00635(12) 0.000
N1 0.0176(5) 0.0201(5) 0.0177(5) -0.0016(4) 0.0080(4) -0.0005(4)
C1 0.0134(5) 0.0164(6) 0.0163(6) -0.0017(4) 0.0039(4) 0.0010(4)
S1 0.01886(16) 0.02257(18) 0.02138(17) -0.00378(11) 0.01220(13) -0.00468(11)
N11 0.0172(5) 0.0192(5) 0.0184(5) -0.0010(4) 0.0084(4) -0.0021(4)
C11 0.0190(6) 0.0237(6) 0.0189(6) -0.0030(5) 0.0087(5) -0.0027(5)
C12 0.0199(6) 0.0288(7) 0.0245(6) -0.0049(5) 0.0101(5) -0.0068(5)
C13 0.0275(7) 0.0305(8) 0.0324(8) -0.0124(6) 0.0148(6) -0.0105(6)
C14 0.0358(8) 0.0268(7) 0.0348(8) -0.0101(6) 0.0203(7) -0.0018(6)
C15 0.0271(6) 0.0223(6) 0.0245(6) -0.0022(5) 0.0135(5) -0.0006(5)
C16 0.0284(7) 0.0454(9) 0.0219(7) -0.0141(7) 0.0070(6) -0.0098(6)
N21 0.071(2) 0.0457(19) 0.0431(19) -0.0022(17) 0.0280(17) 0.0091(14)
C21 0.0440(19) 0.0299(16) 0.0381(18) 0.0031(14) 0.0206(15) 0.0091(15)
C22 0.080(3) 0.0398(18) 0.075(7) -0.004(6) 0.050(4) 0.017(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'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N1 Ni1 N1 . 2_655 175.54(6) y
N1 Ni1 S1 . 6_556 83.43(3) y
N1 Ni1 S1 2_655 6_556 93.32(3) ?
N1 Ni1 S1 . 5_655 93.32(3) y
N1 Ni1 S1 2_655 5_655 83.43(3) ?
N1 Ni1 N11 . . 91.71(4) y
N1 Ni1 N11 . 2_655 91.34(4) y
N1 Ni1 N11 2_655 . 91.34(4) ?
N1 Ni1 N11 2_655 2_655 91.71(4) ?
S1 Ni1 S1 5_655 6_556 87.022(18) y
N11 Ni1 S1 2_655 6_556 173.74(3) ?
N11 Ni1 S1 . 5_655 173.74(3) y
N11 Ni1 S1 2_655 5_655 89.87(3) ?
N11 Ni1 S1 . 6_556 89.87(3) y
N11 Ni1 N11 . 2_655 93.73(6) y
C1 N1 Ni1 . . 163.89(10) ?
N1 C1 S1 . . 179.13(12) ?
C1 S1 Ni1 . 5_655 101.56(4) ?
C11 N11 Ni1 . . 119.96(9) ?
C15 N11 Ni1 . . 121.53(9) ?
C15 N11 C11 . . 118.17(11) ?
N11 C11 H11 . . 118.2 ?
N11 C11 C12 . . 123.56(12) ?
C12 C11 H11 . . 118.2 ?
C11 C12 C16 . . 120.10(13) ?
C13 C12 C11 . . 117.29(13) ?
C13 C12 C16 . . 122.58(13) ?
C12 C13 H13 . . 120.1 ?
C14 C13 C12 . . 119.72(13) ?
C14 C13 H13 . . 120.1 ?
C13 C14 H14 . . 120.5 ?
C13 C14 C15 . . 119.06(13) ?
C15 C14 H14 . . 120.5 ?
N11 C15 C14 . . 122.18(13) ?
N11 C15 H15 . . 118.9 ?
C14 C15 H15 . . 118.9 ?
C12 C16 H16A . . 109.5 ?
C12 C16 H16B . . 109.5 ?
C12 C16 H16C . . 109.5 ?
H16A C16 H16B . . 109.5 ?
H16A C16 H16C . . 109.5 ?
H16B C16 H16C . . 109.5 ?
N21 C21 C22 . . 174.4(12) ?
C21 C22 H22A . . 109.5 ?
C21 C22 H22B . . 109.5 ?
C21 C22 H22C . . 109.5 ?
H22A C22 H22B . . 109.5 ?
H22A C22 H22C . . 109.5 ?
H22B C22 H22C . . 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 . 2.0285(11) y
Ni1 N1 2_655 2.0286(11) y
Ni1 S1 5_655 2.5508(4) ?
Ni1 S1 6_556 2.5508(4) y
Ni1 N11 2_655 2.0836(11) ?
Ni1 N11 . 2.0836(11) y
N1 C1 . 1.1590(17) ?
C1 S1 . 1.6456(13) ?
N11 C11 . 1.3435(16) ?
N11 C15 . 1.3360(17) ?
C11 H11 . 0.9500 ?
C11 C12 . 1.3912(18) ?
C12 C13 . 1.384(2) ?
C12 C16 . 1.504(2) ?
C13 H13 . 0.9500 ?
C13 C14 . 1.384(2) ?
C14 H14 . 0.9500 ?
C14 C15 . 1.386(2) ?
C15 H15 . 0.9500 ?
C16 H16A . 0.9800 ?
C16 H16B . 0.9800 ?
C16 H16C . 0.9800 ?
N21 C21 . 1.132(5) ?
C21 C22 . 1.270(19) ?
C22 H22A . 0.9800 ?
C22 H22B . 0.9800 ?
C22 H22C . 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
Ni1 N11 C11 C12 . . . . 172.20(10) ?
Ni1 N11 C15 C14 . . . . -172.51(11) ?
N11 C11 C12 C13 . . . . 0.6(2) ?
N11 C11 C12 C16 . . . . -177.52(13) ?
C11 N11 C15 C14 . . . . 0.8(2) ?
C11 C12 C13 C14 . . . . 0.4(2) ?
C12 C13 C14 C15 . . . . -0.8(2) ?
C13 C14 C15 N11 . . . . 0.2(2) ?
C15 N11 C11 C12 . . . . -1.20(19) ?
C16 C12 C13 C14 . . . . 178.47(15) ?

_cod_database_fobs_code 2244195