#------------------------------------------------------------------------------
#$Date: 2024-11-01 03:56:04 +0100 (Fri, 01 Nov 2024) $
#$Revision: 295715 $
#$URL: svn://www.crystallography.net/cod/cif/2/02/33/2023301.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_2023301
loop_
_publ_author_name
'Znovjyak, Kateryna'
'Shova, Sergiu'
'Panov, Dmitriy M.'
'Kariaka, Nataliia S.'
'Fritsky, Igor O.'
'Malinkin, Sergey O.'
'Seredyuk, Maksym'
_publ_section_title
;
Crystal structure of
bis{5-(4-chlorophenyl)-3-[6-(1H-pyrazol-1-yl)pyridin-2-yl]-1H-1,2,4-triazol-1-ido}nickel(II)
methanol disolvate
;
_journal_coeditor_code TX2090
_journal_issue 11
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_page_first 1235
_journal_page_last 1239
_journal_paper_doi 10.1107/S2056989024010338
_journal_volume 80
_journal_year 2024
_chemical_formula_iupac '[Ni (C16 H10 Cl1 N6 )2], 2C H4 O'
_chemical_formula_moiety 'C32 H20 Cl2 N12 Ni, 2(C H4 O)'
_chemical_formula_sum 'C34 H28 Cl2 N12 Ni O2'
_chemical_formula_weight 766.29
_chemical_name_systematic
'Bis{5-(4-chlorophenyl)-3-[6-(1H-pyrazol-1-yl)pyridin-2-yl]-1H-1,2,4-triazol-1-ido}nickel(II) methanol disolvate'
_space_group_crystal_system orthorhombic
_space_group_IT_number 60
_space_group_name_Hall '-P 2n 2ab'
_space_group_name_H-M_alt 'P b c n'
_atom_sites_solution_hydrogens mixed
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 12.8146(4)
_cell_length_b 10.1523(4)
_cell_length_c 27.5618(10)
_cell_measurement_reflns_used 3630
_cell_measurement_temperature 200.00(10)
_cell_measurement_theta_max 26.8520
_cell_measurement_theta_min 2.1640
_cell_volume 3585.7(2)
_computing_cell_refinement
;
CrysAlisPro 1.171.43.124a (Rigaku OD, 2024)
;
_computing_data_collection
;
CrysAlisPro 1.171.43.124a (Rigaku OD, 2024)
;
_computing_data_reduction
;
CrysAlisPro 1.171.43.124a (Rigaku OD, 2024)
;
_computing_molecular_graphics
;
Olex2 1.3 (Dolomanov et al., 2009)
;
_computing_publication_material
;
Olex2 1.3 (Dolomanov et al., 2009)
;
_computing_structure_refinement
;
SHELXL2018/3 (Sheldrick, 2015)
;
_diffrn_ambient_temperature 200.00(10)
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean 16.1593
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'Xcalibur, Eos'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_probe x-ray
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0395
_diffrn_reflns_av_unetI/netI 0.0460
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_h_min -15
_diffrn_reflns_limit_k_max 12
_diffrn_reflns_limit_k_min -8
_diffrn_reflns_limit_l_max 32
_diffrn_reflns_limit_l_min -28
_diffrn_reflns_number 11432
_diffrn_reflns_theta_full 25.024
_diffrn_reflns_theta_max 25.024
_diffrn_reflns_theta_min 2.170
_diffrn_source 'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu 0.740
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.98240
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2024)
;
_exptl_crystal_colour 'clear light colourless'
_exptl_crystal_density_diffrn 1.419
_exptl_crystal_description plate
_exptl_crystal_F_000 1576
_exptl_crystal_size_max 0.3
_exptl_crystal_size_mid 0.2
_exptl_crystal_size_min 0.03
_refine_diff_density_max 0.378
_refine_diff_density_min -0.426
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.053
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 236
_refine_ls_number_reflns 3169
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.053
_refine_ls_R_factor_all 0.0607
_refine_ls_R_factor_gt 0.0417
_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^)+(0.0279P)^2^+2.4046P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0802
_refine_ls_wR_factor_ref 0.0870
_reflns_number_gt 2460
_reflns_number_total 3169
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file tx2090.cif
_cod_data_source_block I
_cod_database_code 2023301
_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 0.808
_shelx_estimated_absorpt_t_max 0.978
_shelx_hkl_file
;
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-15 -1 10 1367.40 651.903 2
-15 1 10 1528.93 637.239 2
-15 -1 -10 223.180 465.347 2
-15 1 -10 591.575 449.258 2
-15 -1 11 5822.95 995.318 2
-15 1 11 8253.52 1166.94 2
-15 -1 -11 7802.40 1133.28 2
-15 1 -11 5805.37 1011.74 2
-15 -2 0 673.057 496.350 2
-15 2 0 45.1559 398.758 2
-15 -2 -1 908.657 444.293 2
-15 2 -1 577.231 397.687 2
-15 -2 1 691.572 482.480 2
-15 2 1 1710.02 667.691 2
-15 -2 -2-394.335 485.059 2
-15 2 -2 505.997 483.510 2
-15 -2 2 322.973 454.929 2
-15 2 2-203.648 378.887 2
-15 -2 -3 985.004 587.707 2
-15 2 -3 15.0168 408.823 2
-15 -2 3-142.200 363.945 2
-15 2 3 801.113 483.161 2
-15 -2 -4-13.0651 427.307 2
-15 2 -4 92.7419 372.623 2
-15 -2 4 29.9179 399.146 2
-15 2 4 636.689 448.071 2
-15 -2 -5-180.280 384.370 2
-15 2 -5 470.553 442.767 2
-15 -2 5 8.67381 393.990 2
-15 2 5 201.353 356.372 2
-15 -2 6 1125.90 594.953 2
-15 2 6 943.972 524.016 2
-15 -2 -6 1482.05 598.030 2
-15 2 -6 716.509 490.271 2
-15 -2 7 497.140 481.247 2
-15 2 7 342.536 456.750 2
-15 -2 -7-367.006 381.951 2
-15 2 -7 892.303 508.164 2
-15 -2 8-16.9335 403.149 2
-15 2 8 113.142 436.093 2
-15 -2 -8 204.490 447.898 2
-15 2 -8 651.675 441.900 2
-15 -2 9-132.430 382.956 2
-15 2 9 342.317 397.779 2
-15 -2 -9-579.101 457.606 2
-15 2 -9 96.3674 358.071 2
-15 -2 10 1301.89 596.913 2
-15 2 10-96.4149 389.267 2
-15 -2 -10 432.552 428.944 2
-15 2 -10 808.551 397.262 2
-15 -2 11 655.601 564.613 2
-15 2 -11-10.1811 397.260 2
-15 -3 0 3351.54 761.969 2
-15 3 0 4395.60 843.183 2
-15 -3 -1-167.994 374.002 2
-15 3 -1 201.475 428.942 2
-15 -3 1 371.237 438.131 2
-15 3 1 277.869 450.385 2
-15 -3 -2 5431.68 901.739 2
-15 3 -2 6519.85 986.924 2
-15 -3 2 3759.97 812.468 2
-15 3 2 5357.39 949.489 2
-15 -3 -3 1011.26 546.539 2
-15 3 -3 969.800 536.465 2
-15 -3 3-361.347 410.427 2
-15 3 3 616.506 430.722 2
-15 -3 -4 1770.96 622.457 2
-15 3 -4 2085.60 649.258 2
-15 -3 4 3024.47 732.222 2
-15 3 4 1566.32 585.673 2
-15 -3 -5-314.659 353.776 2
-15 3 -5 327.338 387.389 2
-15 -3 5 658.344 474.170 2
-15 3 5-92.2774 415.640 2
-15 -3 6 4313.39 862.093 2
-15 3 6 3599.52 822.178 2
-15 -3 -6 3956.61 845.111 2
-15 3 -6 2185.97 672.222 2
-15 -3 7 636.669 527.178 2
-15 3 7-133.076 386.797 2
-15 -3 -7 379.723 408.965 2
-15 3 -7 669.307 510.937 2
-15 -3 8 2442.33 615.981 2
-15 3 8 2671.45 763.316 2
-15 3 -8 3028.80 758.401 2
-15 -3 -8 3042.88 748.189 2
-15 -3 9-98.4237 355.813 2
-15 3 9 301.270 406.611 2
-15 -3 -9 486.796 591.475 2
-15 -3 10 6677.49 1044.06 2
-15 3 10 5233.49 922.658 2
-15 -3 -10 7570.95 1133.56 2
-15 3 -10 7476.97 1111.86 2
-15 -3 11 3775.99 897.938 2
-15 -3 -11 2222.54 725.698 2
-15 -4 0-305.443 478.678 2
-15 4 0 709.852 420.456 2
-15 -4 -1 736.728 429.533 2
-15 4 -1-76.2101 437.712 2
-15 -4 1 559.062 497.342 2
-15 4 1 461.086 406.683 2
-15 -4 -2 742.937 529.708 2
-15 4 -2 419.017 409.152 2
-15 -4 2 304.052 398.520 2
-15 4 2 390.517 414.472 2
-15 -4 -3-175.311 404.358 2
-15 4 -3-171.437 343.829 2
-15 -4 3 1439.99 620.283 2
-15 4 3 1661.70 617.320 2
-15 -4 -4 372.225 367.782 2
-15 4 -4 266.865 420.038 2
-15 -4 4 1338.99 607.775 2
-15 4 4 330.006 429.098 2
-15 -4 5 1178.76 580.996 2
-15 4 5 136.461 332.301 2
-15 -4 -5-32.3424 357.231 2
-15 4 -5 678.315 513.450 2
-15 -4 6 12.1516 391.921 2
-15 4 6 605.775 420.264 2
-15 -4 -6-52.5336 385.724 2
-15 4 -6 367.344 415.029 2
-15 -4 7 143.802 409.612 2
-15 4 7 560.059 458.380 2
-15 4 -7 34.5814 396.697 2
-15 -4 -7 135.203 413.004 2
-15 -4 8-412.679 469.431 2
-15 4 8 31.7014 403.149 2
-15 -4 -8-11.0944 400.819 2
-15 4 -8 766.059 439.220 2
-15 -4 9 670.860 470.723 2
-15 4 9 141.646 450.797 2
-15 -4 -9 911.525 477.310 2
-15 4 -9 245.936 480.161 2
-15 -4 10 319.248 356.072 2
-15 -4 -10 506.053 428.650 2
-15 -5 0 1494.03 641.036 2
-15 5 0-388.291 413.021 2
-15 -5 -1 25.7410 407.901 2
-15 5 -1 931.448 427.438 2
-15 -5 1-426.382 465.972 2
-15 5 1-100.246 376.342 2
-15 -5 -2 528.195 440.891 2
-15 5 -2 508.774 379.576 2
-15 -5 2-30.9316 353.825 2
-15 5 2 792.801 528.058 2
-15 -5 -3 432.962 404.798 2
-15 5 -3 1415.41 570.986 2
-15 -5 3 708.331 447.053 2
-15 5 3 1014.96 493.160 2
-15 -5 4 2025.51 648.104 2
-15 5 4 976.891 470.210 2
-15 -5 -4 3393.63 819.875 2
-15 5 -4 2136.41 637.992 2
-15 -5 5 955.083 472.584 2
-15 5 5 1130.31 547.232 2
-15 -5 -5 1893.98 635.338 2
-15 5 -5 2727.80 700.125 2
-15 -5 -6 4050.03 818.976 2
-15 5 -6 4549.64 891.396 2
-15 -5 6 3801.41 829.259 2
-15 5 6 2564.57 683.760 2
-15 -5 -7 13.1007 416.161 2
-15 5 -7 616.128 481.894 2
-15 -5 7 920.657 551.188 2
-15 5 7 492.222 494.552 2
-15 -5 8 5428.94 964.445 2
-15 5 8 6730.17 1074.66 2
-15 5 -8 5299.09 972.152 2
-15 -5 -8 3539.29 791.030 2
-15 -5 9 659.667 594.443 2
-15 -5 -9 80.1926 440.932 2
-15 -6 0-306.263 412.403 2
-15 6 0 667.388 523.578 2
-15 -6 -1 56.3525 360.588 2
-15 6 -1-493.906 319.265 2
-15 -6 1-491.859 483.155 2
-15 6 1-680.683 520.356 2
-15 -6 -2 1043.04 582.443 2
-15 6 -2 1221.61 556.063 2
-15 -6 2-405.249 450.200 2
-15 6 2 809.391 519.061 2
-15 -6 3 1210.46 549.888 2
-15 6 3 564.255 372.734 2
-15 -6 -3-336.897 457.203 2
-15 6 -3 1169.75 468.049 2
-15 -6 4-111.458 451.426 2
-15 6 4-474.172 387.247 2
-15 -6 -4-504.000 564.017 2
-15 6 -4-204.974 389.689 2
-15 -6 5 1086.28 580.113 2
-15 6 5 1113.55 642.935 2
-15 -6 -5 396.580 379.042 2
-15 6 -5 810.728 493.411 2
-15 -6 -6 68.1478 407.427 2
-15 6 -6-37.0963 353.019 2
-15 -6 6 5.08519 407.049 2
-15 6 6 1265.19 566.720 2
-15 -6 -7 376.941 409.157 2
-15 -6 7 672.659 556.945 2
-15 7 0-182.697 466.225 2
-15 7 -1 742.709 365.805 2
-15 7 1 2129.81 660.244 2
-15 7 2 710.036 453.620 2
-15 7 -2 169.759 365.477 2
-15 7 3 1342.35 553.478 2
-15 7 -3-13.2510 347.236 2
-16 0 -1 442.372 503.760 2
0 0 0 0.00 0.00 0
TITL shI_6445_MaSe_auto in Pbcn
REM Pbcn (#60, found as Pcan in ba-c setting)
CELL 0.71073 12.814593 10.152283 27.561779 90.0000 90.0000 90.0000
ZERR 5.00 0.000406 0.000397 0.001000 0.0000 0.0000 0.0000
LATT 1
SYMM -x+1/2,-y+1/2, z+1/2
SYMM -x, y,-z+1/2
SYMM x+1/2,-y+1/2,-z
SFAC C H N O Cl Ni
UNIT 150.00 150.00 30.00 10.00 5.00 5.00
REM CrysAlisPro recorded range (K): Min=200.0; max=200.0; aver:200.0
TEMP -73
TREF
HKLF 4
END
;
_shelx_hkl_checksum 51352
_shelx_res_file
;
TITL shi_6445_mase_auto_a.res in Pbcn
shi_6445_mase_auto.res
created by SHELXL-2018/3 at 12:50:41 on 28-Sep-2024
REM Old TITL shI_6445_MaSe_auto in Pbcn
REM SHELXT solution in Pbcn: R1 0.158, Rweak 0.252, Alpha 0.034
REM 0.713 for 441 systematic absences, Orientation as input
REM Formula found by SHELXT: C38 N10 Cl2 Ni
CELL 0.71073 12.814593 10.152283 27.561779 90 90 90
ZERR 4 0.000406 0.000397 0.001 0 0 0
LATT 1
SYMM 0.5-X,0.5-Y,0.5+Z
SYMM -X,+Y,0.5-Z
SYMM 0.5+X,0.5-Y,-Z
SFAC C H Cl N Ni O
UNIT 136 112 8 48 4 8
L.S. 44
PLAN 2
SIZE 0.03 0.2 0.3
TEMP -73
CONF
fmap 2
acta
MORE -1
BOND $H
SHEL 999 0.84
OMIT 0 0 2
OMIT 0 2 5
OMIT 0 2 6
REM
REM
REM
WGHT 0.027900 2.404600
FVAR 2.56117
NI1 5 0.500000 0.691214 0.750000 10.50000 0.01413 0.02642 =
0.02197 0.00000 -0.00045 0.00000
CL1 3 0.655253 0.024899 0.487654 11.00000 0.10827 0.06726 =
0.04408 -0.02988 0.00192 0.00391
N4 4 0.562682 0.552844 0.701904 11.00000 0.01920 0.02771 =
0.02259 -0.00234 -0.00030 -0.00170
N3 4 0.655337 0.699415 0.765627 11.00000 0.01723 0.02468 =
0.02194 0.00035 -0.00126 -0.00134
N6 4 0.705840 0.443864 0.677577 11.00000 0.02145 0.03088 =
0.02573 -0.00734 -0.00022 0.00074
O1 6 0.352555 0.558041 0.618388 11.00000 0.03241 0.07151 =
0.05690 0.02417 -0.00827 -0.00441
N1 4 0.511843 0.836629 0.806705 11.00000 0.01717 0.03182 =
0.02731 0.00006 -0.00120 0.00250
N2 4 0.613742 0.859840 0.820145 11.00000 0.01898 0.02811 =
0.02730 -0.00661 -0.00163 0.00094
N5 4 0.532719 0.470172 0.665530 11.00000 0.02335 0.02881 =
0.02614 -0.00382 -0.00162 -0.00311
C9 1 0.665903 0.534778 0.707333 11.00000 0.01819 0.02607 =
0.02313 -0.00071 0.00000 -0.00052
C11 1 0.625728 0.311496 0.611938 11.00000 0.03315 0.02614 =
0.02640 -0.00070 0.00322 -0.00587
C10 1 0.620498 0.407240 0.651851 11.00000 0.02480 0.02492 =
0.02227 -0.00110 0.00005 -0.00228
C4 1 0.692288 0.785254 0.797214 11.00000 0.02112 0.02361 =
0.02295 -0.00342 -0.00018 -0.00065
C8 1 0.721062 0.619144 0.741595 11.00000 0.02041 0.02522 =
0.02388 -0.00133 0.00317 0.00142
C1 1 0.455961 0.911419 0.836344 11.00000 0.02176 0.03443 =
0.02708 0.00047 0.00200 0.00814
AFIX 43
H1 2 0.381914 0.915928 0.836126 11.00000 -1.20000
AFIX 0
C5 1 0.797697 0.800786 0.806887 11.00000 0.02217 0.03550 =
0.03469 -0.01181 -0.00324 -0.00317
AFIX 43
H5 2 0.822378 0.864474 0.829382 11.00000 -1.20000
AFIX 0
C12 1 0.710039 0.226466 0.608842 11.00000 0.04127 0.03923 =
0.03571 -0.01035 -0.00528 0.00352
AFIX 43
H12 2 0.762240 0.228747 0.633302 11.00000 -1.20000
AFIX 0
C15 1 0.559818 0.218966 0.537480 11.00000 0.05771 0.03989 =
0.02496 0.00268 -0.00793 -0.00986
AFIX 43
H15 2 0.508238 0.216511 0.512739 11.00000 -1.20000
AFIX 0
C16 1 0.549957 0.306507 0.575816 11.00000 0.04125 0.03255 =
0.02989 -0.00072 -0.00243 -0.00386
AFIX 43
H16 2 0.491181 0.363367 0.577433 11.00000 -1.20000
AFIX 0
C14 1 0.644041 0.135978 0.535308 11.00000 0.06384 0.03434 =
0.02482 -0.00681 0.00649 -0.00421
C3 1 0.619660 0.948030 0.856793 11.00000 0.03067 0.03663 =
0.03506 -0.01226 -0.00342 -0.00008
AFIX 43
H3 2 0.681449 0.979665 0.871858 11.00000 -1.20000
AFIX 0
C7 1 0.827687 0.626187 0.749383 11.00000 0.01813 0.03826 =
0.03849 -0.01114 -0.00152 0.00340
AFIX 43
H7 2 0.874286 0.569090 0.732760 11.00000 -1.20000
AFIX 0
C2 1 0.519715 0.982739 0.867926 11.00000 0.03332 0.04255 =
0.03599 -0.01282 0.00233 0.00969
AFIX 43
H2 2 0.497898 1.043138 0.892220 11.00000 -1.20000
AFIX 0
C13 1 0.719711 0.138171 0.570772 11.00000 0.05226 0.04371 =
0.04321 -0.01108 0.00364 0.01057
AFIX 43
H13 2 0.777684 0.080013 0.569161 11.00000 -1.20000
AFIX 0
C6 1 0.864569 0.718977 0.782146 11.00000 0.01384 0.04843 =
0.04343 -0.00894 -0.00257 -0.00127
AFIX 43
H6 2 0.937557 0.726096 0.787585 11.00000 -1.20000
AFIX 0
C17 1 0.380966 0.635486 0.578657 11.00000 0.08196 0.05695 =
0.06089 0.01655 -0.01478 -0.01362
AFIX 137
H17A 2 0.401889 0.578408 0.551683 11.00000 -1.50000
H17B 2 0.439474 0.692602 0.587693 11.00000 -1.50000
H17C 2 0.321473 0.689799 0.568711 11.00000 -1.50000
AFIX 0
H1A 2 0.407435 0.528769 0.631493 11.00000 0.06240
HKLF 4
REM shi_6445_mase_auto_a.res in Pbcn
REM wR2 = 0.0870, GooF = S = 1.053, Restrained GooF = 1.053 for all data
REM R1 = 0.0417 for 2460 Fo > 4sig(Fo) and 0.0607 for all 3169 data
REM 236 parameters refined using 0 restraints
END
WGHT 0.0277 2.4185
REM Highest difference peak 0.378, deepest hole -0.426, 1-sigma level 0.053
Q1 1 0.7225 0.0837 0.4816 11.00000 0.05 0.38
Q2 1 0.5428 0.5945 0.7507 11.00000 0.05 0.24
;
_shelx_res_checksum 51370
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-x, y, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'x, -y, z-1/2'
'-x-1/2, y-1/2, z'
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 0.69121(4) 0.750000 0.02084(14) Uani d 1 . .
Cl Cl1 0.65525(9) 0.02490(10) 0.48765(3) 0.0732(3) Uani d 1 . .
N N4 0.56268(15) 0.5528(2) 0.70190(7) 0.0232(5) Uani d 1 . .
N N3 0.65534(14) 0.6994(2) 0.76563(7) 0.0213(5) Uani d 1 . .
N N6 0.70584(15) 0.4439(2) 0.67758(7) 0.0260(5) Uani d 1 . .
O O1 0.35256(17) 0.5580(2) 0.61839(9) 0.0536(7) Uani d 1 . .
N N1 0.51184(15) 0.8366(2) 0.80671(8) 0.0254(5) Uani d 1 . .
N N2 0.61374(15) 0.8598(2) 0.82014(8) 0.0248(5) Uani d 1 . .
N N5 0.53272(16) 0.4702(2) 0.66553(8) 0.0261(5) Uani d 1 . .
C C9 0.66590(18) 0.5348(2) 0.70733(9) 0.0225(6) Uani d 1 . .
C C11 0.6257(2) 0.3115(3) 0.61194(9) 0.0286(6) Uani d 1 . .
C C10 0.62050(19) 0.4072(2) 0.65185(9) 0.0240(6) Uani d 1 . .
C C4 0.69229(18) 0.7853(2) 0.79721(9) 0.0226(6) Uani d 1 . .
C C8 0.72106(18) 0.6191(2) 0.74160(9) 0.0232(6) Uani d 1 . .
C C1 0.4560(2) 0.9114(3) 0.83634(9) 0.0278(6) Uani d 1 . .
H H1 0.381914 0.915928 0.836126 0.033 Uiso calc 1 . .
C C5 0.79770(19) 0.8008(3) 0.80689(10) 0.0308(7) Uani d 1 . .
H H5 0.822378 0.864474 0.829382 0.037 Uiso calc 1 . .
C C12 0.7100(2) 0.2265(3) 0.60884(10) 0.0387(7) Uani d 1 . .
H H12 0.762240 0.228747 0.633302 0.046 Uiso calc 1 . .
C C15 0.5598(3) 0.2190(3) 0.53748(10) 0.0409(8) Uani d 1 . .
H H15 0.508238 0.216511 0.512739 0.049 Uiso calc 1 . .
C C16 0.5500(2) 0.3065(3) 0.57582(10) 0.0346(7) Uani d 1 . .
H H16 0.491181 0.363367 0.577433 0.041 Uiso calc 1 . .
C C14 0.6440(3) 0.1360(3) 0.53531(10) 0.0410(8) Uani d 1 . .
C C3 0.6197(2) 0.9480(3) 0.85679(10) 0.0341(7) Uani d 1 . .
H H3 0.681449 0.979665 0.871858 0.041 Uiso calc 1 . .
C C7 0.82769(19) 0.6262(3) 0.74938(10) 0.0316(7) Uani d 1 . .
H H7 0.874286 0.569090 0.732760 0.038 Uiso calc 1 . .
C C2 0.5197(2) 0.9827(3) 0.86793(11) 0.0373(7) Uani d 1 . .
H H2 0.497898 1.043138 0.892220 0.045 Uiso calc 1 . .
C C13 0.7197(3) 0.1382(3) 0.57077(11) 0.0464(8) Uani d 1 . .
H H13 0.777684 0.080013 0.569161 0.056 Uiso calc 1 . .
C C6 0.8646(2) 0.7190(3) 0.78215(10) 0.0352(7) Uani d 1 . .
H H6 0.937557 0.726096 0.787585 0.042 Uiso calc 1 . .
C C17 0.3810(3) 0.6355(4) 0.57866(13) 0.0666(11) Uani d 1 . .
H H17A 0.401889 0.578408 0.551683 0.100 Uiso calc 1 . .
H H17B 0.439474 0.692602 0.587693 0.100 Uiso calc 1 . .
H H17C 0.321473 0.689799 0.568711 0.100 Uiso calc 1 . .
H H1A 0.407(3) 0.529(3) 0.6315(12) 0.062(11) 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
Ni1 0.0141(2) 0.0264(3) 0.0220(3) 0.000 -0.00045(19) 0.000
Cl1 0.1083(8) 0.0673(7) 0.0441(6) 0.0039(6) 0.0019(5) -0.0299(5)
N4 0.0192(11) 0.0277(12) 0.0226(12) -0.0017(9) -0.0003(9) -0.0023(10)
N3 0.0172(10) 0.0247(12) 0.0219(12) -0.0013(9) -0.0013(8) 0.0004(10)
N6 0.0214(11) 0.0309(13) 0.0257(12) 0.0007(9) -0.0002(9) -0.0073(10)
O1 0.0324(13) 0.0715(17) 0.0569(16) -0.0044(12) -0.0083(11) 0.0242(13)
N1 0.0172(11) 0.0318(13) 0.0273(12) 0.0025(9) -0.0012(9) 0.0001(10)
N2 0.0190(11) 0.0281(12) 0.0273(12) 0.0009(9) -0.0016(9) -0.0066(11)
N5 0.0234(12) 0.0288(13) 0.0261(13) -0.0031(9) -0.0016(9) -0.0038(11)
C9 0.0182(13) 0.0261(15) 0.0231(14) -0.0005(10) 0.0000(11) -0.0007(12)
C11 0.0332(15) 0.0261(15) 0.0264(15) -0.0059(12) 0.0032(12) -0.0007(13)
C10 0.0248(14) 0.0249(14) 0.0223(14) -0.0023(11) 0.0000(11) -0.0011(12)
C4 0.0211(13) 0.0236(14) 0.0230(14) -0.0006(11) -0.0002(11) -0.0034(12)
C8 0.0204(13) 0.0252(14) 0.0239(14) 0.0014(11) 0.0032(11) -0.0013(12)
C1 0.0218(13) 0.0344(16) 0.0271(16) 0.0081(12) 0.0020(12) 0.0005(13)
C5 0.0222(14) 0.0355(16) 0.0347(16) -0.0032(12) -0.0032(12) -0.0118(14)
C12 0.0413(18) 0.0392(18) 0.0357(17) 0.0035(14) -0.0053(14) -0.0104(15)
C15 0.058(2) 0.0399(19) 0.0250(16) -0.0099(16) -0.0079(14) 0.0027(15)
C16 0.0413(17) 0.0325(17) 0.0299(16) -0.0039(14) -0.0024(13) -0.0007(14)
C14 0.064(2) 0.0343(18) 0.0248(16) -0.0042(16) 0.0065(15) -0.0068(14)
C3 0.0307(15) 0.0366(17) 0.0351(17) -0.0001(13) -0.0034(13) -0.0123(15)
C7 0.0181(13) 0.0383(16) 0.0385(17) 0.0034(11) -0.0015(12) -0.0111(15)
C2 0.0333(17) 0.0425(18) 0.0360(17) 0.0097(13) 0.0023(13) -0.0128(15)
C13 0.052(2) 0.0437(19) 0.0432(19) 0.0106(16) 0.0036(16) -0.0111(16)
C6 0.0138(13) 0.0484(19) 0.0434(18) -0.0013(12) -0.0026(12) -0.0089(16)
C17 0.082(3) 0.057(2) 0.061(3) -0.014(2) -0.015(2) 0.017(2)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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 Ni1 N4 . 3_656 95.63(11) ?
N4 Ni1 N1 3_656 . 91.57(8) ?
N4 Ni1 N1 . 3_656 91.58(8) ?
N4 Ni1 N1 . . 153.19(7) ?
N4 Ni1 N1 3_656 3_656 153.19(7) ?
N3 Ni1 N4 . . 77.66(8) ?
N3 Ni1 N4 3_656 3_656 77.66(8) ?
N3 Ni1 N4 3_656 . 105.57(8) ?
N3 Ni1 N4 . 3_656 105.58(8) ?
N3 Ni1 N3 . 3_656 175.32(12) ?
N3 Ni1 N1 . . 75.52(8) ?
N3 Ni1 N1 3_656 . 101.19(8) ?
N3 Ni1 N1 . 3_656 101.19(8) ?
N3 Ni1 N1 3_656 3_656 75.52(8) ?
N1 Ni1 N1 3_656 . 93.53(11) ?
N5 N4 Ni1 . . 140.50(15) ?
C9 N4 Ni1 . . 113.52(16) ?
C9 N4 N5 . . 105.97(19) ?
C4 N3 Ni1 . . 121.12(16) ?
C4 N3 C8 . . 120.0(2) ?
C8 N3 Ni1 . . 118.84(16) ?
C9 N6 C10 . . 101.6(2) ?
C17 O1 H1A . . 108(2) ?
N2 N1 Ni1 . . 112.27(14) ?
C1 N1 Ni1 . . 143.26(18) ?
C1 N1 N2 . . 104.4(2) ?
N1 N2 C4 . . 117.7(2) ?
C3 N2 N1 . . 111.6(2) ?
C3 N2 C4 . . 130.6(2) ?
C10 N5 N4 . . 105.23(19) ?
N4 C9 C8 . . 118.0(2) ?
N6 C9 N4 . . 113.8(2) ?
N6 C9 C8 . . 128.1(2) ?
C12 C11 C10 . . 119.6(2) ?
C12 C11 C16 . . 118.5(3) ?
C16 C11 C10 . . 121.9(2) ?
N6 C10 C11 . . 122.4(2) ?
N5 C10 N6 . . 113.4(2) ?
N5 C10 C11 . . 124.1(2) ?
N3 C4 N2 . . 113.2(2) ?
N3 C4 C5 . . 123.5(2) ?
C5 C4 N2 . . 123.3(2) ?
N3 C8 C9 . . 111.8(2) ?
N3 C8 C7 . . 120.6(2) ?
C7 C8 C9 . . 127.5(2) ?
N1 C1 H1 . . 124.3 ?
N1 C1 C2 . . 111.4(2) ?
C2 C1 H1 . . 124.3 ?
C4 C5 H5 . . 121.8 ?
C6 C5 C4 . . 116.3(2) ?
C6 C5 H5 . . 121.8 ?
C11 C12 H12 . . 119.4 ?
C11 C12 C13 . . 121.3(3) ?
C13 C12 H12 . . 119.4 ?
C16 C15 H15 . . 120.0 ?
C14 C15 H15 . . 120.0 ?
C14 C15 C16 . . 119.9(3) ?
C11 C16 H16 . . 119.8 ?
C15 C16 C11 . . 120.3(3) ?
C15 C16 H16 . . 119.8 ?
C15 C14 Cl1 . . 119.8(2) ?
C15 C14 C13 . . 120.9(3) ?
C13 C14 Cl1 . . 119.3(3) ?
N2 C3 H3 . . 126.7 ?
N2 C3 C2 . . 106.7(2) ?
C2 C3 H3 . . 126.7 ?
C8 C7 H7 . . 120.9 ?
C8 C7 C6 . . 118.2(2) ?
C6 C7 H7 . . 120.9 ?
C1 C2 H2 . . 127.0 ?
C3 C2 C1 . . 106.0(2) ?
C3 C2 H2 . . 127.0 ?
C12 C13 H13 . . 120.5 ?
C14 C13 C12 . . 119.0(3) ?
C14 C13 H13 . . 120.5 ?
C5 C6 C7 . . 121.4(2) ?
C5 C6 H6 . . 119.3 ?
C7 C6 H6 . . 119.3 ?
O1 C17 H17A . . 109.5 ?
O1 C17 H17B . . 109.5 ?
O1 C17 H17C . . 109.5 ?
H17A C17 H17B . . 109.5 ?
H17A C17 H17C . . 109.5 ?
H17B C17 H17C . . 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 N4 3_656 2.092(2) ?
Ni1 N4 . 2.092(2) ?
Ni1 N3 . 2.0383(19) ?
Ni1 N3 3_656 2.0384(19) ?
Ni1 N1 . 2.155(2) ?
Ni1 N1 3_656 2.155(2) ?
Cl1 C14 . 1.737(3) ?
N4 N5 . 1.363(3) ?
N4 C9 . 1.344(3) ?
N3 C4 . 1.320(3) ?
N3 C8 . 1.346(3) ?
N6 C9 . 1.337(3) ?
N6 C10 . 1.355(3) ?
O1 C17 . 1.396(4) ?
O1 H1A . 0.84(3) ?
N1 N2 . 1.378(3) ?
N1 C1 . 1.325(3) ?
N2 C4 . 1.409(3) ?
N2 C3 . 1.352(3) ?
N5 C10 . 1.347(3) ?
C9 C8 . 1.458(3) ?
C11 C10 . 1.470(4) ?
C11 C12 . 1.386(4) ?
C11 C16 . 1.392(4) ?
C4 C5 . 1.386(3) ?
C8 C7 . 1.385(3) ?
C1 H1 . 0.9500 ?
C1 C2 . 1.396(4) ?
C5 H5 . 0.9500 ?
C5 C6 . 1.374(4) ?
C12 H12 . 0.9500 ?
C12 C13 . 1.386(4) ?
C15 H15 . 0.9500 ?
C15 C16 . 1.386(4) ?
C15 C14 . 1.371(4) ?
C16 H16 . 0.9500 ?
C14 C13 . 1.377(4) ?
C3 H3 . 0.9500 ?
C3 C2 . 1.363(4) ?
C7 H7 . 0.9500 ?
C7 C6 . 1.388(4) ?
C2 H2 . 0.9500 ?
C13 H13 . 0.9500 ?
C6 H6 . 0.9500 ?
C17 H17A . 0.9800 ?
C17 H17B . 0.9800 ?
C17 H17C . 0.9800 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
C2 H2 C14 3_666 0.95 2.86 3.73(4) 153
C2 H2 C15 3_666 0.95 2.74 3.686(4) 178
C2 H2 C16 3_666 0.95 2.88 3.743(4) 151
C3 H3 O1 6_667 0.95 2.35 3.259(4) 160
C5 H5 O1 6_667 0.95 2.47 3.399(4) 167
C1 H1 N6 6_567 0.95 2.31 3.245(6) 170
C7 H7 C1 6_567 0.95 2.70 3.611(4) 161
O1 H1A N5 . 0.84 1.96 2.795(6) 176
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 N4 N5 C10 . . . . -178.80(19) ?
Ni1 N4 C9 N6 . . . . 178.29(16) ?
Ni1 N4 C9 C8 . . . . -5.4(3) ?
Ni1 N3 C4 N2 . . . . 4.2(3) ?
Ni1 N3 C4 C5 . . . . -175.7(2) ?
Ni1 N3 C8 C9 . . . . -0.9(3) ?
Ni1 N3 C8 C7 . . . . 176.8(2) ?
Ni1 N1 N2 C4 . . . . -2.1(3) ?
Ni1 N1 N2 C3 . . . . -178.00(17) ?
Ni1 N1 C1 C2 . . . . 176.5(2) ?
Cl1 C14 C13 C12 . . . . -179.6(2) ?
N4 N5 C10 N6 . . . . 0.4(3) ?
N4 N5 C10 C11 . . . . -177.5(2) ?
N4 C9 C8 N3 . . . . 4.2(3) ?
N4 C9 C8 C7 . . . . -173.3(3) ?
N3 C4 C5 C6 . . . . -1.2(4) ?
N3 C8 C7 C6 . . . . -0.7(4) ?
N6 C9 C8 N3 . . . . 180.0(2) ?
N6 C9 C8 C7 . . . . 2.5(4) ?
N1 N2 C4 N3 . . . . -1.1(3) ?
N1 N2 C4 C5 . . . . 178.9(2) ?
N1 N2 C3 C2 . . . . 0.5(3) ?
N1 C1 C2 C3 . . . . -0.4(3) ?
N2 N1 C1 C2 . . . . 0.7(3) ?
N2 C4 C5 C6 . . . . 178.9(2) ?
N2 C3 C2 C1 . . . . 0.0(3) ?
N5 N4 C9 N6 . . . . -1.2(3) ?
N5 N4 C9 C8 . . . . 175.2(2) ?
C9 N4 N5 C10 . . . . 0.4(3) ?
C9 N6 C10 N5 . . . . -1.1(3) ?
C9 N6 C10 C11 . . . . 176.9(2) ?
C9 C8 C7 C6 . . . . 176.6(3) ?
C11 C12 C13 C14 . . . . 0.4(5) ?
C10 N6 C9 N4 . . . . 1.4(3) ?
C10 N6 C9 C8 . . . . -174.6(3) ?
C10 C11 C12 C13 . . . . -177.6(3) ?
C10 C11 C16 C15 . . . . 177.0(2) ?
C4 N3 C8 C9 . . . . -178.1(2) ?
C4 N3 C8 C7 . . . . -0.5(4) ?
C4 N2 C3 C2 . . . . -174.7(3) ?
C4 C5 C6 C7 . . . . 0.0(4) ?
C8 N3 C4 N2 . . . . -178.6(2) ?
C8 N3 C4 C5 . . . . 1.5(4) ?
C8 C7 C6 C5 . . . . 0.9(4) ?
C1 N1 N2 C4 . . . . 175.2(2) ?
C1 N1 N2 C3 . . . . -0.7(3) ?
C12 C11 C10 N6 . . . . 19.7(4) ?
C12 C11 C10 N5 . . . . -162.5(3) ?
C12 C11 C16 C15 . . . . -0.6(4) ?
C15 C14 C13 C12 . . . . -0.4(5) ?
C16 C11 C10 N6 . . . . -157.9(3) ?
C16 C11 C10 N5 . . . . 19.9(4) ?
C16 C11 C12 C13 . . . . 0.1(4) ?
C16 C15 C14 Cl1 . . . . 179.1(2) ?
C16 C15 C14 C13 . . . . -0.1(5) ?
C14 C15 C16 C11 . . . . 0.6(4) ?
C3 N2 C4 N3 . . . . 173.9(2) ?
C3 N2 C4 C5 . . . . -6.2(4) ?