#------------------------------------------------------------------------------
#$Date: 2025-01-04 03:37:25 +0100 (Sat, 04 Jan 2025) $
#$Revision: 297060 $
#$URL: svn://www.crystallography.net/cod/cif/2/02/33/2023342.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_2023342
loop_
_publ_author_name
'Tsymbal, Liudmyla V.'
'Andriichuk, Irina L.'
'Bahrin, Lucian G.'
'Lampeka, Yaroslaw D.'
_publ_section_title
;
Syntheses and structures of two coordination polymers formed by
Ni(cyclam)2+ cations and sulfate anions
;
_journal_coeditor_code HB8118
_journal_issue 2
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_paper_doi 10.1107/S2056989024012337
_journal_volume 81
_journal_year 2025
_chemical_formula_iupac '[Ni (S O4) (C10 H24 N4)]'
_chemical_formula_moiety 'C10 H24 N4 Ni O4 S'
_chemical_formula_sum 'C10 H24 N4 Ni O4 S'
_chemical_formula_weight 355.10
_chemical_name_systematic
catena-Poly[[(1,4,8,11-tetraazacyclotetradecane-\k^4^N^1^,N^4^,N^8^,N^11^)nickel(II)]-\m~2~-sulfato-\k^2^O^3^:O^4^]
_space_group_crystal_system triclinic
_space_group_IT_number 2
_space_group_name_Hall '-P 1'
_space_group_name_H-M_alt 'P -1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary dual
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_cell_angle_alpha 108.308(7)
_cell_angle_beta 102.767(7)
_cell_angle_gamma 99.145(6)
_cell_formula_units_Z 2
_cell_length_a 7.9935(6)
_cell_length_b 8.3181(6)
_cell_length_c 12.1998(9)
_cell_measurement_reflns_used 2779
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 27.8810
_cell_measurement_theta_min 2.6220
_cell_volume 727.87(11)
_computing_cell_refinement
;
CrysAlisPro (Rigaku OD, 2022)
;
_computing_data_collection
;
CrysAlisPro (Rigaku OD, 2022)
;
_computing_data_reduction
;
CrysAlisPro (Rigaku OD, 2022)
;
_computing_molecular_graphics
;
Mercury (Macrae et al., 2020)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2018/3 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2018/2 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 293(2)
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean 16.1593
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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 0.0363
_diffrn_reflns_av_unetI/netI 0.0554
_diffrn_reflns_limit_h_max 9
_diffrn_reflns_limit_h_min -9
_diffrn_reflns_limit_k_max 10
_diffrn_reflns_limit_k_min -10
_diffrn_reflns_limit_l_max 15
_diffrn_reflns_limit_l_min -15
_diffrn_reflns_number 7381
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 26.371
_diffrn_reflns_theta_min 1.837
_diffrn_source 'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu 1.495
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.98609
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2022)
;
_exptl_crystal_colour 'clear light violet'
_exptl_crystal_density_diffrn 1.620
_exptl_crystal_description prism
_exptl_crystal_F_000 376
_exptl_crystal_size_max 0.10
_exptl_crystal_size_mid 0.05
_exptl_crystal_size_min 0.04
_refine_diff_density_max 0.407
_refine_diff_density_min -0.414
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.019
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 184
_refine_ls_number_reflns 2965
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.019
_refine_ls_R_factor_all 0.0530
_refine_ls_R_factor_gt 0.0379
_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^)+(0.0285P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0716
_refine_ls_wR_factor_ref 0.0795
_reflns_number_gt 2356
_reflns_number_total 2965
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file hb8118.cif
_cod_data_source_block I
_cod_original_cell_volume 727.88(10)
_cod_database_code 2023342
_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 0.865
_shelx_estimated_absorpt_t_max 0.943
_shelx_hkl_file
;
0 0 -1 6.83 1.13
0 0 1 3.01 0.72
0 0 -1 3.83 0.81
0 0 2 1461.76 21.92
0 0 -2 1522.71 21.35
0 0 -2 1546.48 22.27
0 0 -3 6.49 2.20
0 0 3 2.76 1.28
0 0 -3 3.09 1.32
0 0 -4 324.62 13.98
0 0 -4 271.65 13.57
0 0 4 329.92 14.59
0 0 5 45.67 6.08
0 0 -5 48.54 6.11
0 0 -5 41.47 6.02
0 0 -6 266.29 16.46
0 0 7 3.68 3.30
0 0 -7 4.37 3.40
0 0 7 -0.39 1.28
0 0 8 431.26 24.55
0 0 -8 419.52 24.34
0 0 8 377.36 21.97
0 0 -9 2.92 2.69
0 0 9 1.07 2.26
0 0 9 -0.58 1.72
0 0 10 18.89 5.70
0 0 10 15.42 6.05
0 0 11 46.13 9.90
0 0 -11 44.14 9.75
0 0 11 41.78 9.00
0 0 12 207.76 21.18
0 0 12 235.69 23.70
0 0 -12 237.00 23.46
0 0 -13 30.62 8.99
0 0 13 29.83 8.61
0 0 13 48.98 11.58
0 0 14 7.83 5.46
0 1 -14 0.95 2.64
0 -1 14 9.92 5.88
0 -1 14 7.07 4.84
0 -1 13 2.49 2.79
0 -1 13 1.99 3.05
0 1 -13 2.20 4.03
0 1 -12 222.41 22.08
0 -1 12 199.92 21.37
0 -1 12 174.40 18.59
0 -1 11 10.07 4.80
0 -1 11 1.16 2.36
0 1 -11 3.24 3.53
0 1 -10 36.62 7.87
0 1 -9 -2.43 2.18
0 1 -8 311.86 20.10
0 1 -7 2.37 2.03
0 -1 6 132.89 4.40
0 1 -6 122.16 10.76
0 -1 6 130.37 10.27
0 -1 6 129.63 4.58
0 -1 5 116.82 8.92
0 -1 5 120.06 4.59
0 1 -5 121.55 9.57
0 -1 5 106.33 9.01
0 -1 5 121.63 4.92
0 -1 4 1454.23 17.63
0 -1 4 1420.11 27.15
0 -1 4 1468.58 29.31
0 1 -4 1439.00 16.62
0 1 -4 1428.70 29.05
0 -1 4 1448.76 16.75
0 1 -3 25.13 3.49
0 -1 3 29.42 3.60
0 -1 3 22.16 2.92
0 -1 3 24.54 2.20
0 1 -3 26.57 2.37
0 1 -2 858.07 13.12
0 1 -2 856.15 15.54
0 -1 2 892.08 15.81
0 -1 2 886.71 13.27
0 1 -1 122.55 4.90
0 -1 1 126.17 5.01
0 -1 1 131.61 4.84
0 -1 0 5589.59 33.32
0 -1 0 5342.79 34.44
0 1 0 5158.99 30.22
0 -1 0 5177.93 30.08
0 1 0 5436.61 33.01
0 -1 -1 86.41 4.17
0 -1 -1 87.31 5.47
0 1 1 86.51 4.15
0 1 1 82.85 5.10
0 1 1 81.65 5.27
0 -1 -1 87.65 5.26
0 -1 -2 633.40 17.22
0 -1 -2 613.39 11.01
0 1 2 564.54 16.46
0 1 2 590.91 16.32
0 -1 -2 596.92 16.40
0 -1 -2 598.22 11.11
0 1 2 590.47 10.88
0 -1 -3 22.85 3.98
0 1 3 34.11 2.60
0 1 3 29.57 4.32
0 1 3 38.57 5.10
0 -1 -3 38.17 4.96
0 -1 -3 31.22 2.43
0 -1 -3 36.65 2.71
0 -1 -4 488.12 9.36
0 -1 -4 468.31 19.17
0 1 4 487.14 9.29
0 1 4 482.68 18.97
0 1 4 460.62 19.20
0 -1 -4 490.07 9.34
0 -1 -5 18.80 1.63
0 1 5 23.35 4.73
0 -1 -5 20.36 4.63
0 1 5 31.28 5.71
0 -1 -5 18.37 1.60
0 1 6 532.00 24.05
0 1 6 598.27 26.46
0 -1 -6 580.86 25.63
0 1 7 113.55 12.49
0 1 7 116.48 12.19
0 -1 -7 108.69 12.00
0 -1 -8 571.62 29.80
0 1 8 587.69 29.14
0 1 8 506.89 28.17
0 1 9 8.23 4.08
0 -1 -9 -1.59 1.87
0 1 9 2.74 4.73
0 1 10 17.54 6.59
0 1 10 2.50 2.99
0 -1 -10 12.53 5.52
0 -1 -11 28.26 8.28
0 1 11 13.29 5.13
0 1 11 26.96 7.29
0 1 12 267.65 26.08
0 -1 -12 267.40 26.21
0 1 12 222.83 22.90
0 -1 -13 18.34 6.92
0 1 13 19.91 7.59
0 1 13 4.39 4.09
0 -2 15 13.94 6.29
0 2 -14 40.21 10.57
0 -2 14 28.00 8.12
0 -2 14 20.58 6.96
0 2 -13 12.92 5.69
0 -2 13 2.11 2.36
0 2 -12 382.56 28.47
0 2 -11 2.78 3.18
0 2 -10 143.73 15.32
0 -2 9 94.91 10.87
0 2 -9 85.12 11.06
0 -2 9 79.82 4.61
0 -2 9 78.87 4.71
0 -2 8 526.05 23.48
0 -2 8 512.78 13.15
0 -2 8 502.23 13.74
0 2 -8 532.00 25.63
0 -2 7 25.68 4.80
0 -2 7 23.23 3.16
0 2 -7 27.24 5.54
0 -2 7 26.77 3.18
0 2 -6 50.35 6.77
0 -2 6 53.19 6.83
0 -2 6 51.54 4.54
0 -2 6 60.63 6.92
0 -2 6 56.88 4.95
0 2 -6 66.71 5.14
0 -2 5 433.63 13.24
0 -2 5 415.02 13.41
0 2 -5 428.98 17.71
0 2 -5 428.63 13.03
0 -2 5 446.19 17.90
0 2 -4 641.69 16.17
0 -2 4 637.04 16.03
0 -2 4 639.41 19.15
0 2 -4 645.10 19.40
0 -2 3 185.90 8.61
0 -2 3 172.86 8.77
0 2 -3 168.59 8.28
0 2 -3 165.08 8.61
0 2 -2 171.92 8.67
0 2 -2 173.89 8.50
0 -2 2 167.36 8.22
0 -2 2 161.19 7.72
0 2 -1 26.56 3.32
0 2 -1 27.88 3.43
0 -2 1 27.23 3.41
0 -2 1 27.38 3.37
0 2 -1 46.02 4.09
0 -2 1 25.47 2.95
0 -2 0 880.38 19.82
0 2 0 816.86 18.26
0 -2 0 863.80 17.44
0 -2 0 844.23 18.41
0 2 0 833.89 17.32
0 2 1 2.46 1.44
0 -2 -1 1.04 1.33
0 -2 -1 0.78 0.61
0 -2 -1 0.72 1.56
0 -2 -1 4.18 1.61
0 2 1 0.87 1.19
0 2 2 463.26 13.86
0 -2 -2 463.82 13.70
0 2 2 455.43 17.87
0 -2 -2 467.58 14.18
0 -2 -2 478.99 16.11
0 -2 -2 454.23 17.04
0 2 2 457.25 16.99
0 -2 -2 455.42 17.67
0 2 3 348.00 17.11
0 2 3 383.87 12.45
0 -2 -3 392.87 12.89
0 -2 -3 393.21 17.97
0 2 3 360.14 16.86
0 -2 -3 393.01 12.56
0 -2 -3 396.10 17.59
0 -2 -4 1822.45 27.43
0 2 4 1680.82 39.85
0 -2 -4 1764.86 26.57
0 -2 -4 1805.41 40.69
0 2 4 1772.12 26.31
0 2 4 1740.45 41.48
0 -2 -5 87.80 9.94
0 2 5 111.99 11.06
0 2 5 109.62 11.40
0 -2 -5 112.34 6.47
0 -2 -5 106.38 6.42
0 2 5 119.32 6.72
0 -2 -6 216.19 8.57
0 -2 -6 202.26 8.26
0 -2 -6 202.87 16.17
0 2 6 163.44 14.52
0 2 6 197.62 16.17
0 2 7 59.91 9.58
0 2 7 63.97 9.68
0 -2 -7 52.33 3.89
0 -2 -7 70.06 4.20
0 -2 -7 65.95 10.02
0 -2 -8 394.65 26.12
0 2 8 370.76 24.66
0 2 8 399.41 26.36
0 2 9 27.97 7.38
0 -2 -9 42.73 9.10
0 2 9 44.73 9.40
0 -2 -10 16.24 6.16
0 2 10 26.70 8.06
0 2 10 26.27 6.93
0 2 11 4.73 3.64
0 2 11 16.10 6.94
0 -2 -11 11.45 6.27
0 -2 -12 140.59 19.43
0 2 12 128.75 17.97
0 2 12 128.86 18.88
0 3 -15 -6.80 4.68
0 -3 15 2.21 5.70
0 3 -14 23.62 7.64
0 3 -13 105.82 15.46
0 3 -12 409.53 28.94
0 -3 11 25.45 6.49
0 3 -11 19.34 6.04
0 -3 10 66.24 9.50
0 3 -10 84.20 11.57
0 3 -9 31.35 6.92
0 -3 9 34.26 4.58
0 -3 9 28.57 5.93
0 -3 9 29.34 4.04
0 -3 8 566.58 19.09
0 3 -8 576.45 26.37
0 -3 8 645.71 19.60
0 3 -8 593.20 18.96
0 -3 8 575.14 24.10
0 3 -7 23.26 3.83
0 -3 7 27.94 4.23
0 -3 7 29.28 5.10
0 3 -7 18.69 4.53
0 -3 7 21.89 3.93
0 3 -6 228.15 14.11
0 -3 6 211.04 11.86
0 -3 6 210.40 11.43
0 -3 6 204.77 13.40
0 3 -6 195.12 10.93
0 3 -5 756.11 21.56
0 3 -5 729.63 23.44
0 -3 5 780.69 21.96
0 -3 5 733.26 22.22
0 -3 5 772.79 23.73
0 -3 4 865.49 23.30
0 3 -4 862.71 23.22
0 -3 4 897.64 23.36
0 3 -4 851.12 23.31
0 -3 3 96.48 7.21
0 3 -3 82.75 7.25
0 3 -3 97.42 7.64
0 -3 3 93.80 7.67
0 3 -3 83.72 7.47
0 -3 2 519.96 17.81
0 -3 2 505.08 17.82
0 3 -2 477.67 17.33
0 3 -2 531.21 18.12
0 3 -2 497.14 16.29
0 3 -1 7.82 2.20
0 3 -1 7.96 2.22
0 -3 1 8.61 2.49
0 -3 1 6.31 2.01
0 -3 1 9.46 2.42
0 3 -1 7.56 2.57
0 3 0 1936.52 32.37
0 -3 0 2012.76 35.03
0 -3 0 1943.60 34.45
0 3 0 1903.64 34.15
0 -3 0 1991.37 32.40
0 -3 0 1868.96 36.13
0 -3 -1 64.57 6.22
0 -3 -1 62.14 6.21
0 -3 -1 59.52 6.94
0 3 1 61.08 6.24
0 3 1 60.44 6.19
0 -3 -1 57.86 6.52
0 -3 -2 506.36 20.56
0 -3 -2 535.10 18.64
0 -3 -2 505.22 21.58
0 3 2 478.63 17.24
0 -3 -2 517.17 17.88
0 -3 -2 529.36 19.23
0 -3 -3 76.81 7.09
0 -3 -3 68.46 6.56
0 3 3 63.64 6.32
0 3 3 65.05 8.04
0 -3 -3 71.62 7.77
0 3 4 877.95 31.37
0 -3 -4 888.31 23.89
0 -3 -4 895.16 23.48
0 3 4 834.99 32.13
0 3 4 867.92 23.09
0 3 5 148.53 14.45
0 -3 -5 152.03 9.69
0 -3 -5 129.48 8.84
0 -3 -5 152.36 13.84
0 3 5 135.59 9.05
0 3 5 123.90 12.76
0 -3 -6 6.00 2.02
0 -3 -6 5.18 3.03
0 -3 -6 9.87 2.47
0 3 6 2.54 2.56
0 3 6 8.23 3.57
0 -3 -7 5.53 1.82
0 -3 -7 2.50 1.35
0 3 7 13.98 5.55
0 -3 -7 3.51 2.21
0 3 7 9.11 3.63
0 3 8 289.90 23.24
0 3 8 248.14 22.42
0 -3 -8 265.57 22.38
0 3 9 5.55 2.23
0 -3 -9 16.14 6.08
0 3 9 19.10 6.87
0 3 10 64.52 12.29
0 3 10 64.33 12.79
0 -3 -10 72.14 13.18
0 3 11 40.77 10.74
0 3 11 20.19 7.17
0 -3 -11 26.30 8.00
0 -4 16 43.27 10.59
0 4 -15 36.28 10.27
0 4 -14 -0.67 2.48
0 4 -13 59.50 11.67
0 -4 12 221.00 19.17
0 4 -12 243.41 22.17
0 4 -11 77.88 13.26
0 -4 11 75.39 10.74
0 -4 10 57.37 8.75
0 4 -10 56.51 9.72
0 -4 9 34.79 6.55
0 -4 9 32.24 5.19
0 4 -9 23.08 4.41
0 4 -9 27.28 6.25
0 4 -8 610.33 27.50
0 4 -8 619.07 22.85
0 -4 8 639.38 23.09
0 4 -7 90.93 10.04
0 4 -7 106.23 9.49
0 -4 7 112.07 9.73
0 4 -6 232.34 14.18
0 4 -6 225.55 14.67
0 -4 6 236.76 14.12
0 4 -5 316.15 16.31
0 -4 5 351.04 17.12
0 -4 5 325.88 16.28
0 4 -4 716.38 24.06
0 4 -4 645.37 23.24
0 -4 4 728.74 23.27
0 -4 4 733.48 24.61
0 4 -4 726.32 25.50
0 4 -3 -0.53 1.19
0 -4 3 0.95 1.09
0 4 -3 -0.81 1.78
0 -4 3 3.85 1.78
0 4 -3 1.34 1.79
0 -4 2 561.12 21.87
0 4 -2 604.64 22.54
0 -4 2 619.16 22.60
0 -4 2 602.41 20.40
0 4 -2 620.17 22.70
0 4 -2 587.02 20.45
0 4 -1 8.45 2.59
0 -4 1 9.35 2.73
0 -4 1 7.85 2.94
0 -4 1 7.64 2.72
0 4 -1 11.94 3.13
0 -4 0 779.80 25.34
0 4 0 742.12 24.96
0 4 0 728.09 23.28
0 -4 0 792.81 26.51
0 -4 0 757.11 26.50
0 -4 0 746.12 23.00
0 -4 -1 3.16 1.96
0 4 1 8.15 2.77
0 -4 -1 5.44 2.24
0 -4 -1 -0.96 2.23
0 4 1 0.67 1.72
0 4 2 72.97 7.84
0 4 3 2.01 1.97
0 4 4 608.36 22.58
0 -4 -5 189.85 12.84
0 4 5 174.93 12.08
0 -4 -5 211.18 17.49
0 -4 -6 49.12 6.41
0 4 6 44.53 8.83
0 4 6 45.49 9.19
0 -4 -6 48.16 8.84
0 -4 -7 122.17 15.23
0 4 7 109.47 15.05
0 4 7 91.56 13.32
0 -4 -8 146.78 17.70
0 4 8 137.36 18.08
0 4 8 136.37 17.02
0 4 9 24.19 7.53
0 4 9 15.26 6.88
0 -4 -9 17.58 6.54
0 4 10 20.92 8.18
0 -4 -10 30.94 8.77
0 4 10 35.23 9.56
0 5 -15 -0.51 3.07
0 5 -14 8.31 5.28
0 -5 14 1.86 1.91
0 -5 13 10.70 4.64
0 5 -13 13.61 5.67
0 5 -12 256.06 22.78
0 -5 12 284.47 21.67
0 -5 11 10.77 3.99
0 5 -11 10.73 4.72
0 5 -10 51.99 7.54
0 5 -10 47.74 8.88
0 -5 10 56.63 8.71
0 5 -9 55.40 9.05
0 5 -9 65.58 8.49
0 5 -8 208.23 14.98
0 5 -8 186.07 15.43
0 5 -7 282.74 17.40
0 5 -6 116.31 11.55
0 5 -6 116.74 11.19
0 5 -5 73.66 8.84
0 5 -5 73.24 8.68
0 -5 4 945.62 29.08
0 5 -4 885.64 30.84
0 5 -4 926.17 29.87
0 5 -3 7.95 2.77
0 5 -3 6.68 3.28
0 5 -2 406.51 21.00
0 -5 2 414.04 21.04
0 5 -2 396.15 18.96
0 -5 1 3.32 2.75
0 5 -1 1.94 1.61
0 5 -1 3.57 2.33
0 5 0 532.25 22.68
0 -5 0 527.82 25.02
0 5 0 507.43 23.37
0 -5 -1 3.01 2.61
0 5 1 3.68 2.08
0 5 1 7.33 2.73
0 5 2 254.79 16.57
0 -5 -2 226.29 17.73
0 5 3 61.50 8.29
0 5 4 597.33 25.49
0 5 5 56.75 8.00
0 -5 -5 70.34 11.02
0 -5 -6 56.28 10.47
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-8 0 1 24.80 7.90
-8 0 0 185.91 20.37
-8 0 -1 23.00 8.02
-8 0 -2 30.29 9.98
-8 0 -3 1.95 3.00
-8 0 -4 142.68 18.07
8 0 5 8.07 5.15
-8 0 -5 -0.76 1.96
-8 0 -6 5.86 4.35
-8 -1 12 54.03 12.59
8 1 -12 69.16 12.08
-8 -1 11 8.33 4.80
8 1 -11 7.42 3.85
-8 -1 11 9.28 5.47
-8 -1 10 29.92 8.43
8 1 -10 17.08 6.51
-8 -1 9 0.66 2.04
8 1 -9 0.93 2.40
-8 -1 8 159.52 19.35
-8 -1 7 2.17 3.81
-8 -1 6 78.70 13.49
-8 -1 5 3.89 3.22
-8 -1 4 326.75 27.30
-8 -1 3 5.25 3.87
-8 -1 2 31.78 8.78
-8 -1 1 10.01 5.83
-8 -1 0 213.35 22.33
-8 -1 -1 13.80 6.17
-8 -1 -2 47.36 10.87
8 1 2 37.98 9.07
8 1 3 39.26 9.53
-8 -1 -3 37.79 10.11
-8 -1 -4 153.65 18.72
8 1 4 120.19 16.08
8 2 -13 6.74 4.04
8 2 -12 44.62 10.01
-8 -2 12 43.69 10.79
-8 -2 11 6.10 4.32
8 2 -11 2.50 2.68
-8 -2 10 16.21 6.81
8 2 -10 8.20 4.36
-8 -2 9 0.19 2.24
8 2 -9 3.12 2.74
-8 -2 8 77.62 13.49
8 2 -8 82.29 13.75
-8 -2 7 -4.90 3.97
8 2 -7 0.62 3.10
-8 -2 6 56.76 11.85
8 2 -6 71.89 12.30
-8 -2 5 -2.39 2.74
8 2 -5 0.81 2.67
-8 -2 4 321.54 27.75
8 2 -4 266.92 24.24
-8 -2 3 0.81 1.52
8 2 -3 2.99 3.02
-8 -2 2 53.05 11.52
8 2 -2 33.15 8.32
-8 -2 1 8.14 4.86
8 2 -1 8.19 4.33
-8 -2 0 192.65 21.62
8 2 0 158.30 18.94
-8 -2 -1 5.32 4.03
8 2 1 -0.81 2.74
-8 -2 -2 51.38 11.25
8 2 2 53.54 11.23
8 2 3 47.58 10.16
-8 -2 -3 49.41 11.43
8 3 -13 3.21 2.56
-8 -3 12 122.48 18.03
8 3 -12 123.62 16.98
-8 -3 11 -2.45 2.12
8 3 -11 -1.79 3.28
-8 -3 10 16.85 6.76
8 3 -10 15.75 6.93
-8 -3 9 2.50 4.19
8 3 -9 1.14 3.54
8 3 -8 48.13 11.24
8 3 -7 4.11 3.95
8 3 -6 18.90 6.78
8 3 -5 -1.85 3.02
8 3 -4 207.55 21.97
8 3 -3 6.15 4.62
8 3 -2 41.63 10.05
-8 -3 1 2.08 2.60
8 3 -1 1.45 2.70
-8 -3 0 123.14 18.07
8 3 0 112.23 16.21
-8 -3 0 134.95 16.58
-8 -3 -1 0.41 3.44
8 3 1 9.44 5.56
-8 -3 -2 17.61 6.97
8 3 2 32.89 9.03
8 3 3 32.85 8.78
-8 -3 -3 33.87 9.19
-8 -4 12 113.55 18.10
8 4 -12 115.24 16.99
8 4 -11 -5.11 5.31
8 4 -10 -1.78 2.30
8 4 -9 -1.92 2.67
8 4 -8 44.59 11.08
8 4 -7 3.12 1.96
8 4 -6 9.04 5.29
8 4 -5 9.42 6.80
8 4 -4 76.28 13.85
8 4 -3 3.73 3.55
8 4 -2 22.61 8.03
8 4 -1 26.08 8.35
8 4 0 41.11 10.24
-8 -4 0 55.74 11.56
-8 -4 -1 -3.37 3.30
8 4 1 2.20 3.15
-8 -4 -1 3.45 1.98
-9 7 0 7.99 5.47
-9 7 -1 38.42 10.29
-9 7 -2 0.58 3.23
-9 6 1 135.13 18.38
-9 6 1 120.83 18.51
-9 6 0 39.45 9.82
-9 6 0 15.34 6.70
-9 6 -1 19.95 7.36
-9 6 -2 1.82 2.81
-9 6 -3 117.52 16.82
-9 6 -4 11.31 5.86
-9 6 -5 -0.02 1.99
-9 5 7 1.26 2.08
-9 5 6 7.05 4.60
-9 5 5 87.57 15.62
-9 5 4 -6.64 5.41
-9 5 3 90.24 15.80
-9 5 2 -0.11 2.33
-9 5 1 135.91 17.27
-9 5 1 124.06 18.18
-9 5 0 22.06 6.96
-9 5 0 19.60 7.26
-9 5 -1 0.01 2.03
-9 5 -1 7.23 5.00
-9 5 -2 2.81 3.21
-9 5 -2 9.71 5.17
-9 5 -3 108.56 15.04
-9 5 -3 129.56 18.78
-9 5 -4 11.19 5.28
-9 5 -4 18.79 7.86
-9 5 -5 17.13 7.54
-9 4 9 24.25 8.42
-9 4 8 -2.23 3.82
-9 4 7 9.92 4.74
-9 4 6 8.68 4.38
-9 4 5 75.19 14.17
-9 4 4 -4.98 4.98
-9 4 3 24.91 8.64
-9 4 2 2.89 2.96
-9 4 1 101.61 16.19
-9 4 0 6.28 3.98
-9 4 0 21.51 8.15
-9 4 -1 21.74 6.71
-9 4 -1 11.09 5.37
-9 4 -2 -0.59 1.43
-9 4 -2 -3.62 3.85
-9 4 -3 297.01 27.76
-9 4 -4 10.40 5.95
-9 4 -5 50.69 11.65
-9 4 -6 -2.98 3.07
-9 3 10 0.17 2.04
-9 3 9 32.24 9.27
-9 3 9 17.41 6.74
-9 3 8 6.32 4.13
-9 3 8 12.58 5.55
-9 3 7 8.27 4.48
-9 3 6 5.11 4.61
-9 3 5 105.08 16.31
-9 3 4 -1.49 3.60
-9 3 3 34.29 9.25
-9 3 2 6.73 6.13
-9 3 1 201.55 22.61
-9 3 0 -1.64 3.53
-9 3 -1 50.20 11.49
-9 3 -2 12.29 7.14
-9 3 -3 208.46 23.28
-9 3 -4 7.26 5.12
-9 3 -5 18.45 6.77
-9 2 10 4.93 3.49
-9 2 10 3.34 3.13
-9 2 9 33.25 9.40
-9 2 9 47.14 10.41
-9 2 8 6.78 4.55
-9 2 8 9.04 4.11
-9 2 7 10.66 3.87
-9 2 7 17.73 6.68
-9 2 6 -1.31 2.42
-9 2 6 0.69 3.16
-9 2 5 153.98 16.06
-9 2 5 172.26 20.62
-9 2 4 0.28 3.09
-9 2 3 36.65 9.86
-9 2 2 1.23 3.51
-9 2 1 120.08 17.48
-9 2 0 4.11 2.85
-9 2 -1 10.75 5.86
-9 2 -2 34.52 9.48
-9 2 -3 63.23 13.10
-9 2 -4 0.83 2.48
-9 2 -5 5.75 3.88
-9 1 11 11.12 5.35
-9 1 11 16.28 6.65
-9 1 10 9.80 4.95
-9 1 10 12.03 5.68
-9 1 9 38.41 9.76
-9 1 9 37.49 10.05
-9 1 8 0.52 2.64
-9 1 8 3.24 3.69
-9 1 7 39.33 9.98
-9 1 6 4.39 4.47
-9 1 5 219.24 23.60
-9 1 4 -0.57 3.51
-9 1 3 5.49 5.25
-9 1 2 3.08 4.24
-9 1 1 104.58 16.64
-9 1 0 13.80 6.19
-9 1 -1 14.34 6.05
-9 1 -2 8.01 4.87
-9 1 -3 103.16 16.37
-9 1 -4 1.78 3.00
9 0 -12 6.02 4.16
-9 0 11 2.33 4.65
9 0 -11 -1.05 3.72
-9 0 11 0.49 2.20
-9 0 10 8.50 4.60
-9 0 10 16.93 6.86
-9 0 9 39.65 10.17
-9 0 8 -1.25 2.48
-9 0 7 38.00 10.28
-9 0 6 10.28 5.88
-9 0 5 226.94 24.31
-9 0 4 9.46 5.39
-9 0 3 35.41 9.72
-9 0 2 -0.57 2.51
-9 0 1 138.65 19.16
-9 0 0 -0.63 2.00
-9 0 -1 64.97 13.27
-9 0 -2 3.09 4.18
-9 0 -3 86.13 15.27
9 0 4 10.77 5.69
-9 0 -4 3.42 1.89
9 1 -12 2.46 4.17
9 1 -11 14.21 6.67
-9 -1 11 1.65 2.80
9 1 -10 6.52 5.79
-9 -1 10 8.00 5.91
-9 -1 9 58.40 12.46
9 1 -9 39.16 10.23
-9 -1 8 -2.56 3.08
9 1 -8 1.70 2.07
-9 -1 7 13.93 6.50
-9 -1 6 5.72 4.49
-9 -1 5 120.85 18.21
-9 -1 4 -3.40 3.41
-9 -1 3 9.68 4.96
-9 -1 2 7.32 5.73
-9 -1 1 135.44 19.11
-9 -1 0 1.10 3.66
9 1 0 0.79 2.42
-9 -1 -1 47.78 11.72
9 1 1 47.03 10.92
9 1 2 7.20 4.15
-9 -1 -2 16.35 7.45
9 1 3 88.05 14.86
-9 -1 -3 75.95 14.48
9 2 -11 -0.09 3.69
-9 -2 11 3.93 3.15
-9 -2 10 2.16 4.07
9 2 -10 7.82 4.48
-9 -2 9 62.59 13.25
9 2 -9 76.52 13.77
-9 -2 8 -10.56 5.58
9 2 -8 -2.20 2.52
-9 -2 7 -3.08 4.17
9 2 -7 -4.08 3.33
-9 -2 6 8.42 5.25
9 2 -6 11.25 6.32
-9 -2 5 71.84 13.98
9 2 -5 62.38 12.78
-9 -2 4 1.41 2.98
9 2 -4 4.52 4.05
-9 -2 3 9.19 5.87
9 2 -3 15.16 6.71
-9 -2 2 -0.37 2.27
9 2 -2 3.92 4.51
-9 -2 1 103.98 17.22
9 2 -1 110.74 16.84
-9 -2 0 3.64 3.00
9 2 0 10.14 4.50
-9 -2 -1 15.36 7.10
9 2 1 9.39 4.48
9 3 -6 7.07 5.80
9 3 -5 86.47 15.31
9 3 -4 3.73 4.29
-10 6 0 36.89 9.60
-10 6 -1 -1.98 4.24
-10 2 4 6.98 5.08
-10 2 3 8.42 4.40
-10 1 9 -1.40 2.68
-10 1 8 -2.96 3.84
0 0 0 0.00 0.00
TITL I in P-1
REM P-1 (#2 in standard setting)
CELL 0.71073 7.993493 8.318147 12.199764 108.3080 102.7668 99.1447
ZERR 1.00 0.000620 0.000563 0.000945 0.0065 0.0066 0.0060
LATT 1
SFAC C H N O Cl Ni
UNIT 30.00 30.00 2.00 12.00 2.00 1.00
TREF
HKLF 4
END
_computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)'
;
_shelx_hkl_checksum 27157
_shelx_res_file
;
TITL I_b.res in P-1
I.res
created by SHELXL-2018/3 at 15:46:03 on 12-Feb-2024
REM Old TITL I_a.res in P1
REM SHELXT solution in P-1: R1 0.404, Rweak 0.057, Alpha 0.199
REM 0.000 for 0 systematic absences, Orientation as input
REM Formula found by SHELXT: N12 Ni Cl3
CELL 0.71073 7.993493 8.318147 12.199764 108.308 102.7668 99.1447
ZERR 2 0.00062 0.000563 0.000945 0.0065 0.0066 0.006
LATT 1
SFAC C H N Ni O S
UNIT 20 48 8 2 8 2
EQIV $1 -X,1-Y,1-Z
EQIV $2 1-X,1-Y,2-Z
EQIV $3 1-X,2-Y,2-Z
EQIV $4 1-X,1-Y,1-Z
L.S. 10
PLAN 3
SIZE 0.04 0.05 0.1
CONF
HTAB C3 O1_$1
HTAB N4 S1
HTAB N4 O3
HTAB N3 O4
HTAB N3 S1
HTAB C6 O2_$2
HTAB C6 O4_$3
HTAB N1 S1
HTAB N1 O3
HTAB C1 O1_$1
HTAB N2 O4
HTAB N2 S1
HTAB C8 O2_$2
HTAB C5 O3_$4
htab
LIST 4
MORE -1
BOND $H
fmap 2
acta
SHEL 999 0.8
OMIT -5 -7 4
OMIT -2 -3 2
OMIT -1 -6 1
REM
REM
REM
WGHT 0.028500
FVAR 0.55571
NI1 4 0.000000 0.500000 0.500000 10.50000 0.01608 0.02533 =
0.01394 0.00907 0.00150 0.00519
NI2 4 0.500000 0.500000 1.000000 10.50000 0.01767 0.01963 =
0.01461 0.00763 0.00097 0.00435
S1 6 0.254154 0.524461 0.756382 11.00000 0.01908 0.03168 =
0.01660 0.01381 -0.00223 0.00204
O2 5 0.285382 0.423436 0.835416 11.00000 0.02726 0.02583 =
0.01802 0.01294 -0.00440 0.00371
O3 5 0.408749 0.560602 0.715354 11.00000 0.02031 0.13600 =
0.04438 0.06188 0.00235 0.00381
O1 5 0.098666 0.424487 0.651521 11.00000 0.02508 0.02959 =
0.01651 0.01038 -0.00440 0.00227
O4 5 0.218571 0.690187 0.824444 11.00000 0.08163 0.02760 =
0.02855 0.00457 -0.01562 0.01972
N4 3 0.688488 0.554471 0.915720 11.00000 0.02143 0.02822 =
0.01935 0.01110 0.00062 0.00507
AFIX 13
H4 2 0.625381 0.552117 0.836403 11.00000 -1.20000
AFIX 0
N1 3 0.243061 0.518879 0.466531 11.00000 0.02209 0.03864 =
0.01806 0.01377 0.00362 0.00804
AFIX 13
H1 2 0.326732 0.513375 0.536522 11.00000 -1.20000
AFIX 0
N2 3 0.054906 0.761445 0.607653 11.00000 0.02761 0.02723 =
0.01674 0.01063 0.00068 0.00777
AFIX 13
H2 2 0.126128 0.775590 0.688102 11.00000 -1.20000
AFIX 0
N3 3 0.469578 0.751823 1.057882 11.00000 0.02332 0.02026 =
0.01975 0.00650 -0.00204 0.00519
AFIX 13
H3 2 0.389541 0.764987 0.989536 11.00000 -1.20000
AFIX 0
C4 1 -0.117783 0.794773 0.618084 11.00000 0.04039 0.04007 =
0.03428 0.01035 0.01093 0.02249
AFIX 23
H4A 2 -0.181748 0.808385 0.545437 11.00000 -1.20000
H4B 2 -0.100321 0.901524 0.685933 11.00000 -1.20000
AFIX 0
C5 1 0.222244 0.357533 0.363829 11.00000 0.02792 0.05031 =
0.03170 0.01513 0.01646 0.01787
AFIX 23
H5A 2 0.337616 0.339375 0.358732 11.00000 -1.20000
H5B 2 0.160841 0.367627 0.289181 11.00000 -1.20000
AFIX 0
C10 1 0.375421 0.760824 1.149710 11.00000 0.03697 0.03063 =
0.02459 0.00394 0.00762 0.01504
AFIX 23
H10A 2 0.325008 0.861514 1.163556 11.00000 -1.20000
H10B 2 0.456846 0.772294 1.225193 11.00000 -1.20000
AFIX 0
C7 1 0.727960 0.875225 1.001783 11.00000 0.03399 0.02765 =
0.03906 0.01788 -0.00112 -0.00315
AFIX 23
H7A 2 0.816441 0.983602 1.025167 11.00000 -1.20000
H7B 2 0.642961 0.860916 0.926965 11.00000 -1.20000
AFIX 0
C6 1 0.633070 0.891571 1.098011 11.00000 0.03553 0.01905 =
0.03402 0.00855 -0.00062 0.00244
AFIX 23
H6A 2 0.711889 0.887524 1.169491 11.00000 -1.20000
H6B 2 0.603806 1.004011 1.119676 11.00000 -1.20000
AFIX 0
C3 1 0.154877 0.882907 0.566026 11.00000 0.04321 0.02348 =
0.02484 0.00889 0.00032 0.00082
AFIX 23
H3A 2 0.176117 1.001434 0.622139 11.00000 -1.20000
H3B 2 0.084841 0.875543 0.487966 11.00000 -1.20000
AFIX 0
C2 1 0.330610 0.842787 0.555745 11.00000 0.03329 0.04094 =
0.03344 0.02127 0.00164 -0.01009
AFIX 23
H2A 2 0.390275 0.829608 0.629642 11.00000 -1.20000
H2B 2 0.403653 0.942128 0.549018 11.00000 -1.20000
AFIX 0
C9 1 0.769929 0.405288 0.895498 11.00000 0.02663 0.03961 =
0.02506 0.01044 0.00771 0.01344
AFIX 23
H9A 2 0.852602 0.415529 0.970157 11.00000 -1.20000
H9B 2 0.834192 0.403040 0.836469 11.00000 -1.20000
AFIX 0
C8 1 0.818502 0.724706 0.978238 11.00000 0.02405 0.03649 =
0.03022 0.01603 0.00206 -0.00226
AFIX 23
H8A 2 0.896344 0.739395 0.929486 11.00000 -1.20000
H8B 2 0.890260 0.727149 1.054362 11.00000 -1.20000
AFIX 0
C1 1 0.317956 0.679810 0.449765 11.00000 0.02399 0.05774 =
0.03126 0.02466 0.00890 0.00456
AFIX 23
H1A 2 0.244293 0.684103 0.376506 11.00000 -1.20000
H1B 2 0.435079 0.677907 0.440370 11.00000 -1.20000
AFIX 0
HKLF 4
REM I_b.res in P-1
REM wR2 = 0.0795, GooF = S = 1.019, Restrained GooF = 1.019 for all data
REM R1 = 0.0379 for 2356 Fo > 4sig(Fo) and 0.0530 for all 2965 data
REM 184 parameters refined using 0 restraints
END
WGHT 0.0288 0.0000
REM Instructions for potential hydrogen bonds
HTAB N4 S1
HTAB N4 O3
HTAB N1 S1
HTAB N1 O3
HTAB N2 S1
HTAB N2 O4
HTAB N3 S1
HTAB N3 O4
HTAB C5 O3_$4
HTAB C6 O2_$2
HTAB C6 O4_$3
HTAB C3 O1_$1
HTAB C8 O2_$2
HTAB C1 O1_$1
REM Highest difference peak 0.407, deepest hole -0.414, 1-sigma level 0.073
Q1 1 0.3753 0.4339 0.6874 11.00000 0.05 0.41
Q2 1 0.1624 0.5966 0.8197 11.00000 0.05 0.40
Q3 1 0.3069 0.6835 0.7941 11.00000 0.05 0.37
;
_shelx_res_checksum 76265
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -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 0.000000 0.500000 0.500000 0.01844(14) Uani d 1 . .
Ni Ni2 0.500000 0.500000 1.000000 0.01761(14) Uani d 1 . .
S S1 0.25415(9) 0.52446(9) 0.75638(5) 0.02297(18) Uani d 1 . .
O O2 0.2854(2) 0.4234(2) 0.83542(14) 0.0247(4) Uani d 1 . .
O O3 0.4087(3) 0.5606(4) 0.71535(19) 0.0627(8) Uani d 1 . .
O O1 0.0987(2) 0.4245(2) 0.65152(14) 0.0255(5) Uani d 1 . .
O O4 0.2186(3) 0.6902(3) 0.82444(17) 0.0520(7) Uani d 1 . .
N N4 0.6885(3) 0.5545(3) 0.91572(18) 0.0234(5) Uani d 1 . .
H H4 0.625381 0.552117 0.836403 0.028 Uiso calc 1 . .
N N1 0.2431(3) 0.5189(3) 0.46653(18) 0.0257(5) Uani d 1 . .
H H1 0.326732 0.513375 0.536522 0.031 Uiso calc 1 . .
N N2 0.0549(3) 0.7614(3) 0.60765(18) 0.0241(5) Uani d 1 . .
H H2 0.126128 0.775590 0.688102 0.029 Uiso calc 1 . .
N N3 0.4696(3) 0.7518(3) 1.05788(18) 0.0227(5) Uani d 1 . .
H H3 0.389541 0.764987 0.989536 0.027 Uiso calc 1 . .
C C4 -0.1178(4) 0.7948(4) 0.6181(3) 0.0375(8) Uani d 1 . .
H H4A -0.181748 0.808385 0.545437 0.045 Uiso calc 1 . .
H H4B -0.100321 0.901524 0.685933 0.045 Uiso calc 1 . .
C C5 0.2222(4) 0.3575(4) 0.3638(2) 0.0342(8) Uani d 1 . .
H H5A 0.337616 0.339375 0.358732 0.041 Uiso calc 1 . .
H H5B 0.160841 0.367627 0.289181 0.041 Uiso calc 1 . .
C C10 0.3754(4) 0.7608(4) 1.1497(2) 0.0316(7) Uani d 1 . .
H H10A 0.325008 0.861514 1.163556 0.038 Uiso calc 1 . .
H H10B 0.456846 0.772294 1.225193 0.038 Uiso calc 1 . .
C C7 0.7280(4) 0.8752(4) 1.0018(3) 0.0354(8) Uani d 1 . .
H H7A 0.816441 0.983602 1.025167 0.043 Uiso calc 1 . .
H H7B 0.642961 0.860916 0.926965 0.043 Uiso calc 1 . .
C C6 0.6331(4) 0.8916(3) 1.0980(3) 0.0322(7) Uani d 1 . .
H H6A 0.711889 0.887524 1.169491 0.039 Uiso calc 1 . .
H H6B 0.603806 1.004011 1.119676 0.039 Uiso calc 1 . .
C C3 0.1549(4) 0.8829(4) 0.5660(2) 0.0330(7) Uani d 1 . .
H H3A 0.176117 1.001434 0.622139 0.040 Uiso calc 1 . .
H H3B 0.084841 0.875543 0.487966 0.040 Uiso calc 1 . .
C C2 0.3306(4) 0.8428(4) 0.5557(3) 0.0377(8) Uani d 1 . .
H H2A 0.390275 0.829608 0.629642 0.045 Uiso calc 1 . .
H H2B 0.403653 0.942128 0.549018 0.045 Uiso calc 1 . .
C C9 0.7699(4) 0.4053(4) 0.8955(2) 0.0301(7) Uani d 1 . .
H H9A 0.852602 0.415529 0.970157 0.036 Uiso calc 1 . .
H H9B 0.834192 0.403040 0.836469 0.036 Uiso calc 1 . .
C C8 0.8185(4) 0.7247(4) 0.9782(2) 0.0314(7) Uani d 1 . .
H H8A 0.896344 0.739395 0.929486 0.038 Uiso calc 1 . .
H H8B 0.890260 0.727149 1.054362 0.038 Uiso calc 1 . .
C C1 0.3180(4) 0.6798(4) 0.4498(3) 0.0360(8) Uani d 1 . .
H H1A 0.244293 0.684103 0.376506 0.043 Uiso calc 1 . .
H H1B 0.435079 0.677907 0.440370 0.043 Uiso calc 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 0.0161(3) 0.0253(3) 0.0139(2) 0.0052(2) 0.00150(19) 0.0091(2)
Ni2 0.0177(3) 0.0196(3) 0.0146(2) 0.0044(2) 0.00097(19) 0.0076(2)
S1 0.0191(4) 0.0317(4) 0.0166(3) 0.0020(3) -0.0022(3) 0.0138(3)
O2 0.0273(11) 0.0258(10) 0.0180(9) 0.0037(9) -0.0044(8) 0.0129(8)
O3 0.0203(12) 0.136(2) 0.0444(14) 0.0038(13) 0.0024(10) 0.0619(15)
O1 0.0251(11) 0.0296(11) 0.0165(9) 0.0023(9) -0.0044(8) 0.0104(8)
O4 0.0816(18) 0.0276(12) 0.0285(12) 0.0197(12) -0.0156(12) 0.0046(10)
N4 0.0214(13) 0.0282(13) 0.0193(11) 0.0051(10) 0.0006(10) 0.0111(10)
N1 0.0221(13) 0.0386(14) 0.0181(12) 0.0080(11) 0.0036(10) 0.0138(11)
N2 0.0276(14) 0.0272(13) 0.0167(11) 0.0078(11) 0.0007(10) 0.0106(10)
N3 0.0233(13) 0.0203(12) 0.0197(11) 0.0052(10) -0.0020(10) 0.0065(10)
C4 0.040(2) 0.0401(19) 0.0343(17) 0.0225(16) 0.0109(15) 0.0104(15)
C5 0.0279(18) 0.050(2) 0.0317(17) 0.0179(16) 0.0165(14) 0.0151(15)
C10 0.0370(19) 0.0306(17) 0.0246(15) 0.0150(14) 0.0076(13) 0.0039(13)
C7 0.0340(19) 0.0276(16) 0.0391(18) -0.0032(13) -0.0011(14) 0.0179(14)
C6 0.0355(19) 0.0190(15) 0.0340(17) 0.0024(13) -0.0006(14) 0.0085(13)
C3 0.043(2) 0.0235(16) 0.0248(16) 0.0008(14) 0.0003(14) 0.0089(13)
C2 0.0333(19) 0.0409(19) 0.0334(17) -0.0101(15) 0.0016(14) 0.0213(15)
C9 0.0266(17) 0.0396(18) 0.0251(15) 0.0134(14) 0.0077(13) 0.0104(14)
C8 0.0240(17) 0.0365(18) 0.0302(16) -0.0023(13) 0.0021(13) 0.0160(14)
C1 0.0240(17) 0.058(2) 0.0313(16) 0.0046(15) 0.0089(13) 0.0247(16)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
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'
S S 0.1246 0.1234 '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
O1 Ni1 O1 2_566 . 180.0 ?
N1 Ni1 O1 . . 90.53(7) ?
N1 Ni1 O1 2_566 . 89.47(7) ?
N1 Ni1 O1 2_566 2_566 90.53(7) ?
N1 Ni1 O1 . 2_566 89.47(7) ?
N1 Ni1 N1 2_566 . 180.0 ?
N1 Ni1 N2 . . 94.49(9) ?
N1 Ni1 N2 . 2_566 85.51(9) ?
N1 Ni1 N2 2_566 . 85.51(9) ?
N1 Ni1 N2 2_566 2_566 94.49(9) ?
N2 Ni1 O1 2_566 . 87.02(7) ?
N2 Ni1 O1 . . 92.98(7) ?
N2 Ni1 O1 2_566 2_566 92.98(7) ?
N2 Ni1 O1 . 2_566 87.02(7) ?
N2 Ni1 N2 . 2_566 180.00(7) ?
O2 Ni2 O2 . 2_667 180.0 ?
N4 Ni2 O2 2_667 2_667 92.22(7) ?
N4 Ni2 O2 . 2_667 87.78(7) ?
N4 Ni2 O2 2_667 . 87.78(7) ?
N4 Ni2 O2 . . 92.22(7) ?
N4 Ni2 N4 . 2_667 180.0 ?
N3 Ni2 O2 2_667 . 87.88(7) ?
N3 Ni2 O2 . 2_667 87.87(7) ?
N3 Ni2 O2 2_667 2_667 92.12(7) ?
N3 Ni2 O2 . . 92.13(7) ?
N3 Ni2 N4 2_667 . 85.41(9) ?
N3 Ni2 N4 . . 94.59(9) ?
N3 Ni2 N4 . 2_667 85.41(9) ?
N3 Ni2 N4 2_667 2_667 94.58(9) ?
N3 Ni2 N3 . 2_667 180.00(11) ?
O2 S1 O1 . . 109.61(11) ?
O2 S1 O4 . . 108.92(11) ?
O3 S1 O2 . . 109.99(12) ?
O3 S1 O1 . . 109.64(12) ?
O3 S1 O4 . . 109.85(16) ?
O1 S1 O4 . . 108.81(11) ?
S1 O2 Ni2 . . 126.36(11) ?
S1 O1 Ni1 . . 126.17(11) ?
Ni2 N4 H4 . . 107.4 ?
C9 N4 Ni2 . . 104.98(17) ?
C9 N4 H4 . . 107.4 ?
C9 N4 C8 . . 113.3(2) ?
C8 N4 Ni2 . . 116.05(17) ?
C8 N4 H4 . . 107.4 ?
Ni1 N1 H1 . . 106.9 ?
C5 N1 Ni1 . . 105.39(17) ?
C5 N1 H1 . . 106.9 ?
C1 N1 Ni1 . . 116.45(17) ?
C1 N1 H1 . . 106.9 ?
C1 N1 C5 . . 113.8(2) ?
Ni1 N2 H2 . . 107.5 ?
C4 N2 Ni1 . . 105.35(17) ?
C4 N2 H2 . . 107.5 ?
C3 N2 Ni1 . . 114.87(16) ?
C3 N2 H2 . . 107.5 ?
C3 N2 C4 . . 113.8(2) ?
Ni2 N3 H3 . . 107.1 ?
C10 N3 Ni2 . . 105.45(16) ?
C10 N3 H3 . . 107.1 ?
C10 N3 C6 . . 114.1(2) ?
C6 N3 Ni2 . . 115.61(16) ?
C6 N3 H3 . . 107.1 ?
N2 C4 H4A . . 110.0 ?
N2 C4 H4B . . 110.0 ?
N2 C4 C5 . 2_566 108.6(2) ?
H4A C4 H4B . . 108.3 ?
C5 C4 H4A 2_566 . 110.0 ?
C5 C4 H4B 2_566 . 110.0 ?
N1 C5 C4 . 2_566 108.9(2) ?
N1 C5 H5A . . 109.9 ?
N1 C5 H5B . . 109.9 ?
C4 C5 H5A 2_566 . 109.9 ?
C4 C5 H5B 2_566 . 109.9 ?
H5A C5 H5B . . 108.3 ?
N3 C10 H10A . . 110.1 ?
N3 C10 H10B . . 110.1 ?
N3 C10 C9 . 2_667 108.2(2) ?
H10A C10 H10B . . 108.4 ?
C9 C10 H10A 2_667 . 110.1 ?
C9 C10 H10B 2_667 . 110.1 ?
H7A C7 H7B . . 107.5 ?
C6 C7 H7A . . 108.5 ?
C6 C7 H7B . . 108.5 ?
C6 C7 C8 . . 115.2(2) ?
C8 C7 H7A . . 108.5 ?
C8 C7 H7B . . 108.5 ?
N3 C6 C7 . . 112.4(2) ?
N3 C6 H6A . . 109.1 ?
N3 C6 H6B . . 109.1 ?
C7 C6 H6A . . 109.1 ?
C7 C6 H6B . . 109.1 ?
H6A C6 H6B . . 107.8 ?
N2 C3 H3A . . 109.2 ?
N2 C3 H3B . . 109.2 ?
N2 C3 C2 . . 111.9(2) ?
H3A C3 H3B . . 107.9 ?
C2 C3 H3A . . 109.2 ?
C2 C3 H3B . . 109.2 ?
C3 C2 H2A . . 108.5 ?
C3 C2 H2B . . 108.5 ?
C3 C2 C1 . . 115.1(2) ?
H2A C2 H2B . . 107.5 ?
C1 C2 H2A . . 108.5 ?
C1 C2 H2B . . 108.5 ?
N4 C9 C10 . 2_667 108.4(2) ?
N4 C9 H9A . . 110.0 ?
N4 C9 H9B . . 110.0 ?
C10 C9 H9A 2_667 . 110.0 ?
C10 C9 H9B 2_667 . 110.0 ?
H9A C9 H9B . . 108.4 ?
N4 C8 C7 . . 111.5(2) ?
N4 C8 H8A . . 109.3 ?
N4 C8 H8B . . 109.3 ?
C7 C8 H8A . . 109.3 ?
C7 C8 H8B . . 109.3 ?
H8A C8 H8B . . 108.0 ?
N1 C1 C2 . . 112.0(2) ?
N1 C1 H1A . . 109.2 ?
N1 C1 H1B . . 109.2 ?
C2 C1 H1A . . 109.2 ?
C2 C1 H1B . . 109.2 ?
H1A C1 H1B . . 107.9 ?
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 O1 2_566 2.1625(16) ?
Ni1 O1 . 2.1625(16) ?
Ni1 N1 . 2.064(2) ?
Ni1 N1 2_566 2.064(2) ?
Ni1 N2 . 2.072(2) ?
Ni1 N2 2_566 2.072(2) ?
Ni2 O2 2_667 2.1696(16) ?
Ni2 O2 . 2.1696(16) ?
Ni2 N4 2_667 2.072(2) ?
Ni2 N4 . 2.072(2) ?
Ni2 N3 2_667 2.063(2) ?
Ni2 N3 . 2.063(2) ?
S1 O2 . 1.4722(17) ?
S1 O3 . 1.455(2) ?
S1 O1 . 1.4742(17) ?
S1 O4 . 1.477(2) ?
N4 H4 . 0.9800 ?
N4 C9 . 1.470(3) ?
N4 C8 . 1.473(3) ?
N1 H1 . 0.9800 ?
N1 C5 . 1.476(3) ?
N1 C1 . 1.471(4) ?
N2 H2 . 0.9800 ?
N2 C4 . 1.475(3) ?
N2 C3 . 1.470(3) ?
N3 H3 . 0.9800 ?
N3 C10 . 1.471(3) ?
N3 C6 . 1.475(4) ?
C4 H4A . 0.9700 ?
C4 H4B . 0.9700 ?
C4 C5 2_566 1.507(4) ?
C5 H5A . 0.9700 ?
C5 H5B . 0.9700 ?
C10 H10A . 0.9700 ?
C10 H10B . 0.9700 ?
C10 C9 2_667 1.514(4) ?
C7 H7A . 0.9700 ?
C7 H7B . 0.9700 ?
C7 C6 . 1.516(4) ?
C7 C8 . 1.526(4) ?
C6 H6A . 0.9700 ?
C6 H6B . 0.9700 ?
C3 H3A . 0.9700 ?
C3 H3B . 0.9700 ?
C3 C2 . 1.517(4) ?
C2 H2A . 0.9700 ?
C2 H2B . 0.9700 ?
C2 C1 . 1.522(4) ?
C9 H9A . 0.9700 ?
C9 H9B . 0.9700 ?
C8 H8A . 0.9700 ?
C8 H8B . 0.9700 ?
C1 H1A . 0.9700 ?
C1 H1B . 0.9700 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
N1 H1 O3 . 0.98 2.02 2.916(3) 150.6 yes
N2 H2 O4 . 0.98 2.05 2.960(3) 154.4 yes
N3 H3 O4 . 0.98 2.01 2.938(3) 157.2 yes
N4 H4 O3 . 0.98 2.04 2.946(3) 152.9 yes
C5 H5A O3 2_666 0.97 2.52 3.336(4) 141.4 yes
C6 H6B O4 2_677 0.97 2.51 3.245(3) 132.8 yes
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
Ni1 N1 C5 C4 . . . 2_566 -41.9(2) ?
Ni1 N1 C1 C2 . . . . 54.9(3) ?
Ni1 N2 C4 C5 . . . 2_566 41.8(2) ?
Ni1 N2 C3 C2 . . . . -58.0(2) ?
Ni2 N4 C9 C10 . . . 2_667 43.1(2) ?
Ni2 N4 C8 C7 . . . . -56.2(3) ?
Ni2 N3 C10 C9 . . . 2_667 -42.5(2) ?
Ni2 N3 C6 C7 . . . . 56.2(3) ?
O2 S1 O1 Ni1 . . . . -175.93(11) ?
O3 S1 O2 Ni2 . . . . 57.29(17) ?
O3 S1 O1 Ni1 . . . . -55.11(17) ?
O1 S1 O2 Ni2 . . . . 177.90(11) ?
O4 S1 O2 Ni2 . . . . -63.16(16) ?
O4 S1 O1 Ni1 . . . . 65.05(16) ?
N2 C3 C2 C1 . . . . 73.0(3) ?
C4 N2 C3 C2 . . . . -179.6(2) ?
C5 N1 C1 C2 . . . . 177.9(2) ?
C10 N3 C6 C7 . . . . 178.8(2) ?
C6 N3 C10 C9 . . . 2_667 -170.5(2) ?
C6 C7 C8 N4 . . . . 71.5(3) ?
C3 N2 C4 C5 . . . 2_566 168.5(2) ?
C3 C2 C1 N1 . . . . -70.7(3) ?
C9 N4 C8 C7 . . . . -177.7(2) ?
C8 N4 C9 C10 . . . 2_667 170.7(2) ?
C8 C7 C6 N3 . . . . -71.8(3) ?
C1 N1 C5 C4 . . . 2_566 -170.7(2) ?