#------------------------------------------------------------------------------
#$Date: 2023-07-12 04:08:47 +0200 (Wed, 12 Jul 2023) $
#$Revision: 285171 $
#$URL: svn://www.crystallography.net/cod/cif/2/02/28/2022815.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_2022815
loop_
_publ_author_name
'Khan, Sultana Shakila'
'Howlader, Md. Belayet Hossain'
'Sheikh, Md. Chanmiya'
'Miyatake, Ryuta'
'Zangrando, Ennio'
_publ_section_title
;
Crystal structure of
bis{S-octyl-3-[(thiophen-2-yl)methylidene]dithiocarbazato-\k2 N
3,S}nickel(II)
;
_journal_coeditor_code PK2690
_journal_issue 8
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_paper_doi 10.1107/S2056989023005935
_journal_volume 79
_journal_year 2023
_chemical_formula_iupac '[Ni (C14 H21 N2 S3)2]'
_chemical_formula_moiety 'C28 H42 N4 Ni S6'
_chemical_formula_sum 'C28 H42 N4 Ni S6'
_chemical_formula_weight 685.72
_chemical_name_systematic
Bis{S-octyl-3-[(thiophen-2-yl)methylidene]dithiocarbazato-\k^2^N^3^,S}nickel(II)
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_Hall '-P 2ybc'
_space_group_name_H-M_alt 'P 1 21/c 1'
_atom_sites_solution_hydrogens geom
_audit_creation_method SHELXL-2019/2
_cell_angle_alpha 90
_cell_angle_beta 103.675(7)
_cell_angle_gamma 90
_cell_formula_units_Z 2
_cell_length_a 15.5444(6)
_cell_length_b 5.5388(3)
_cell_length_c 20.1592(8)
_cell_measurement_reflns_used 10434
_cell_measurement_temperature 173(2)
_cell_measurement_theta_max 27.47
_cell_measurement_theta_min 2.08
_cell_volume 1686.45(14)
_computing_cell_refinement
;
RAPID-AUTO (Rigaku, 2018)
;
_computing_data_collection
;
RAPID-AUTO (Rigaku, 2018)
;
_computing_data_reduction
;
RAPID-AUTO (Rigaku, 2018)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 1999)
;
_computing_publication_material
;
WinGX (Farrugia, 2012)
;
_computing_structure_refinement
;
SHELXL2019/2 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 173(2)
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type 'Rigaku R-AXIS RAPID'
_diffrn_measurement_method \w
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71075
_diffrn_reflns_av_R_equivalents 0.0771
_diffrn_reflns_av_unetI/netI 0.0638
_diffrn_reflns_limit_h_max 20
_diffrn_reflns_limit_h_min -19
_diffrn_reflns_limit_k_max 7
_diffrn_reflns_limit_k_min -7
_diffrn_reflns_limit_l_max 25
_diffrn_reflns_limit_l_min -26
_diffrn_reflns_number 15791
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 27.465
_diffrn_reflns_theta_min 2.697
_exptl_absorpt_coefficient_mu 0.971
_exptl_absorpt_correction_T_max 0.990
_exptl_absorpt_correction_T_min 0.815
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(ABSCOR; Rigaku, 1995)
;
_exptl_crystal_colour orange
_exptl_crystal_density_diffrn 1.350
_exptl_crystal_description needle
_exptl_crystal_F_000 724
_exptl_crystal_size_max 0.080
_exptl_crystal_size_mid 0.020
_exptl_crystal_size_min 0.010
_refine_diff_density_max 0.441
_refine_diff_density_min -0.272
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 0.999
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 179
_refine_ls_number_reflns 3850
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 0.999
_refine_ls_R_factor_all 0.0832
_refine_ls_R_factor_gt 0.0446
_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^)+(0.0329P)^2^+0.0128P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0703
_refine_ls_wR_factor_ref 0.0787
_reflns_number_gt 2621
_reflns_number_total 3850
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file pk2690sup1.cif
_cod_data_source_block I
_cod_original_cell_volume 1686.44(13)
_cod_original_sg_symbol_H-M 'P 21/c'
_cod_database_code 2022815
_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 0.926
_shelx_estimated_absorpt_t_max 0.990
_shelx_hkl_file
;
0 0 3 -2.24 3.07
0 0 -3 2.02 2.85
0 0 -3 1.20 2.38
0 0 4 1099.70 16.00
0 0 -4 1119.57 13.06
0 0 -4 1113.39 12.25
0 0 5 -9.03 5.76
0 0 -5 -4.67 5.64
0 0 -5 -3.20 4.32
0 0 6 167.93 7.03
0 0 -6 175.41 8.64
0 0 7 -3.35 5.38
0 0 -7 5.51 4.41
0 0 8 270.37 8.44
0 0 -8 273.98 7.21
0 0 9 -0.17 5.25
0 0 -9 -0.09 4.51
0 0 10 451.43 10.63
0 0 -10 452.59 9.12
0 0 11 6.64 5.62
0 0 -11 -6.71 4.54
0 0 12 532.19 12.13
0 0 -12 526.13 10.75
0 0 13 4.96 6.36
0 0 -13 -2.35 8.05
0 0 14 245.70 14.16
0 0 -14 233.93 8.56
0 0 15 -1.51 7.34
0 0 -15 4.51 5.95
0 0 -15 5.13 8.57
0 0 16 868.10 18.64
0 0 -16 847.76 20.43
0 0 -16 838.13 20.49
0 0 17 1.05 12.50
0 0 -17 -15.97 7.03
0 0 -17 -3.45 9.47
0 0 18 382.52 14.16
0 0 -18 375.14 12.65
0 0 -18 383.28 21.66
0 0 19 4.47 8.98
0 0 -19 15.00 11.47
0 0 -19 8.46 10.30
0 0 20 -15.82 9.03
0 0 -20 8.13 7.74
0 0 -20 0.74 10.53
0 0 21 18.79 9.80
0 0 -21 0.98 8.37
0 0 -21 1.78 17.54
0 0 22 -11.93 14.67
0 0 -22 -4.08 13.67
0 0 -22 22.57 11.57
0 0 23 -11.30 10.37
0 0 -23 -7.40 9.54
0 0 -23 -9.22 12.33
0 0 24 105.09 12.67
0 0 -24 103.30 11.86
0 0 -24 96.02 22.35
0 0 25 12.77 15.80
0 0 -25 -5.91 14.97
0 0 -25 2.88 13.13
0 1 0 -4.71 4.52
0 -1 0 0.39 4.57
0 1 -1 3.33 7.01
0 1 1 9.94 4.63
0 -1 1 -3.01 4.44
0 -1 -1 3.55 5.04
0 1 -2 41.18 4.95
0 1 2 41.93 6.02
0 -1 2 49.99 7.87
0 -1 -2 43.41 10.28
0 1 -3 1205.42 18.04
0 1 3 1196.91 17.09
0 -1 3 1245.32 14.90
0 -1 -3 1211.45 16.88
0 1 4 702.79 14.11
0 1 -4 696.73 10.71
0 -1 4 699.01 10.66
0 -1 -4 703.09 12.24
0 -1 -4 670.60 13.44
0 1 5 159.34 8.82
0 1 -5 148.73 5.94
0 -1 5 143.56 8.77
0 -1 -5 135.20 10.73
0 -1 -5 147.95 8.21
0 1 6 29.73 7.54
0 1 -6 38.23 5.00
0 -1 6 40.68 4.83
0 -1 -6 32.79 6.00
0 -1 -6 39.27 7.37
0 1 7 19.77 7.52
0 1 -7 23.17 4.67
0 -1 -7 24.81 5.94
0 -1 -7 5.34 7.08
0 1 8 68.78 6.26
0 1 -8 60.62 5.47
0 -1 -8 63.30 10.04
0 -1 8 66.65 5.36
0 -1 -8 75.12 8.33
0 1 9 1044.01 18.97
0 1 -9 1046.79 17.37
0 -1 -9 1085.66 19.88
0 -1 9 1059.12 14.71
0 -1 -9 1049.97 18.07
0 1 10 252.24 8.49
0 1 -10 250.72 7.35
0 -1 -10 262.45 8.66
0 -1 10 247.73 7.26
0 -1 -10 271.74 10.28
0 1 11 991.09 16.33
0 1 -11 949.55 14.77
0 -1 11 994.26 17.40
0 -1 -11 972.26 16.09
0 -1 11 1007.16 15.16
0 -1 -11 1009.14 18.21
0 1 12 190.56 8.76
0 1 -12 193.96 7.28
0 -1 12 181.24 13.69
0 -1 -12 192.71 8.77
0 -1 12 205.00 10.33
0 -1 -12 182.73 10.56
0 1 13 935.95 16.83
0 1 -13 919.60 15.74
0 -1 13 962.72 18.33
0 -1 -13 946.73 20.40
0 -1 13 959.22 16.00
0 -1 -13 963.18 19.18
0 1 14 569.91 13.50
0 1 -14 539.88 12.32
0 -1 14 572.90 14.69
0 -1 -14 545.29 12.73
0 -1 -14 574.37 13.46
0 -1 -14 544.41 15.48
0 1 15 514.67 14.04
0 1 -15 554.59 12.89
0 -1 15 532.39 15.30
0 -1 -15 568.98 13.72
0 -1 -15 567.87 13.98
0 -1 -15 562.28 16.26
0 1 16 74.04 8.37
0 1 -16 63.73 7.35
0 -1 -16 74.36 8.15
0 -1 16 58.23 10.05
0 -1 -16 73.57 10.90
0 1 17 -2.24 7.64
0 1 -17 6.07 6.53
0 -1 -17 -4.15 11.24
0 -1 17 2.42 8.80
0 -1 -17 6.31 9.66
0 1 18 38.14 13.35
0 1 -18 30.11 7.63
0 -1 -18 20.79 8.55
0 -1 18 32.99 10.16
0 -1 -18 27.39 11.04
0 1 19 -7.02 8.42
0 1 -19 1.80 11.58
0 -1 -19 2.82 12.53
0 -1 19 -5.00 9.66
0 -1 -19 -1.24 16.26
0 1 20 13.46 9.40
0 1 -20 25.97 8.93
0 -1 -20 27.66 9.07
0 -1 20 27.74 10.97
0 -1 -20 28.59 11.71
0 1 21 -8.09 9.02
0 1 -21 5.39 8.42
0 -1 -21 6.09 12.96
0 -1 21 -2.66 10.18
0 -1 -21 -9.04 11.30
0 1 22 15.66 9.76
0 1 -22 12.01 11.85
0 1 -22 -7.10 8.92
0 -1 -22 13.95 9.69
0 -1 -22 5.19 12.55
0 -1 22 10.57 11.15
0 1 -23 -2.85 12.51
0 1 -23 14.52 14.30
0 -1 -23 4.31 9.78
0 -1 -23 14.55 12.29
0 -1 23 -10.41 11.28
0 1 -24 64.94 22.14
0 1 -24 84.60 16.82
0 -1 -24 79.40 12.16
0 -1 -24 89.02 14.50
0 -1 24 86.20 20.48
0 1 -25 11.03 13.16
0 1 -25 3.91 9.58
0 -1 -25 1.59 10.55
0 -1 -25 15.67 12.91
0 -1 25 12.11 11.96
0 2 0 3.51 6.89
0 -2 0 7.70 6.75
0 2 -1 8.95 10.77
0 2 1 5.03 7.32
0 -2 1 4.21 6.57
0 -2 -1 10.84 7.06
0 2 -2 641.07 12.79
0 2 2 642.27 14.13
0 -2 2 646.06 12.51
0 -2 -2 664.97 13.50
0 2 -3 321.68 9.71
0 2 3 313.64 11.20
0 -2 3 319.52 8.93
0 -2 -3 334.85 11.06
0 2 -4 549.36 11.57
0 2 4 557.40 13.41
0 -2 4 542.82 14.99
0 -2 -4 543.94 13.09
0 2 -5 843.42 18.36
0 2 5 830.55 16.52
0 -2 5 835.65 13.98
0 -2 -5 848.72 20.99
0 2 -6 138.39 7.75
0 2 6 141.17 10.11
0 -2 6 145.27 7.15
0 -2 -6 148.25 9.81
0 2 7 15.29 8.66
0 2 -7 20.21 5.98
0 -2 7 22.24 5.59
0 -2 -7 29.73 6.89
0 -2 -7 18.88 8.05
0 2 8 289.24 12.27
0 2 -8 278.69 12.15
0 -2 8 304.87 8.53
0 -2 -8 300.63 10.09
0 -2 -8 293.27 11.17
0 2 -9 8.49 5.55
0 -2 -9 7.45 6.33
0 -2 9 3.61 5.34
0 -2 -9 14.50 7.73
0 2 10 128.50 15.67
0 2 -10 125.13 10.35
0 -2 10 128.78 7.13
0 -2 -10 127.92 8.37
0 -2 -10 130.59 10.05
0 2 11 28.45 9.91
0 2 -11 20.60 6.30
0 -2 11 35.83 6.02
0 -2 -11 25.64 7.45
0 -2 -11 15.99 9.42
0 2 -12 20.69 6.24
0 -2 -12 11.23 7.39
0 -2 12 18.47 6.10
0 -2 -12 13.08 9.05
0 2 -13 89.04 7.68
0 -2 -13 92.39 8.98
0 -2 13 104.02 7.74
0 -2 -13 92.26 10.78
0 2 -14 12.44 10.52
0 -2 -14 7.48 8.05
0 -2 14 23.57 10.14
0 -2 -14 12.69 9.82
0 2 -15 115.36 12.94
0 -2 -15 143.93 15.31
0 -2 15 134.50 8.76
0 -2 -15 129.50 11.88
0 2 -16 107.37 12.93
0 -2 16 81.16 11.56
0 -2 -16 103.44 10.48
0 -2 16 82.51 8.78
0 -2 -16 116.70 12.26
0 2 -17 78.08 13.44
0 -2 17 111.43 18.51
0 -2 -17 108.89 10.76
0 -2 17 105.76 13.67
0 -2 -17 106.43 12.54
0 2 -18 136.97 15.00
0 -2 18 138.69 10.44
0 -2 -18 161.22 11.92
0 -2 -18 169.25 11.61
0 -2 18 148.84 13.65
0 -2 -18 159.81 14.60
0 2 -19 19.17 13.52
0 -2 19 27.36 11.75
0 -2 -19 21.04 9.98
0 -2 -19 19.52 10.21
0 -2 -19 41.28 12.56
0 2 -20 224.42 17.91
0 -2 20 228.33 16.19
0 -2 -20 261.25 14.02
0 -2 -20 221.52 14.16
0 -2 -20 255.01 16.78
0 2 -21 0.95 8.82
0 -2 -21 -2.98 9.65
0 -2 21 9.95 11.95
0 -2 -21 -0.18 12.46
0 2 -22 235.93 13.47
0 -2 -22 230.18 15.06
0 -2 22 251.91 17.67
0 -2 -22 268.55 17.97
0 2 -23 6.34 10.10
0 -2 -23 12.60 11.47
0 -2 23 20.38 13.18
0 -2 -23 -3.71 13.77
0 2 -24 39.60 11.28
0 -2 -24 42.24 12.26
0 -2 24 34.09 22.12
0 -2 -24 9.60 23.37
0 3 0 0.66 7.87
0 -3 0 -2.79 7.31
0 3 1 18.92 8.76
0 3 -1 25.75 8.42
0 -3 1 6.41 7.83
0 -3 -1 11.01 8.00
0 3 2 23.70 8.59
0 3 -2 21.71 8.65
0 -3 2 29.17 7.89
0 -3 -2 16.83 8.71
0 3 -3 7.22 8.06
0 3 3 8.55 8.76
0 -3 3 -3.31 7.06
0 -3 -3 11.16 8.12
0 3 -4 -9.04 11.70
0 3 4 -2.36 13.55
0 -3 4 -0.41 9.99
0 -3 -4 5.76 7.66
0 3 -5 728.37 15.14
0 3 5 734.57 17.50
0 -3 5 756.94 18.79
0 -3 -5 718.81 16.20
0 3 -6 254.98 10.31
0 3 6 234.37 12.92
0 -3 6 256.69 9.79
0 -3 -6 240.10 12.04
0 3 -7 1732.80 25.51
0 3 7 1706.97 28.98
0 -3 7 1746.01 24.87
0 -3 -7 1715.05 27.50
0 3 -8 39.52 7.89
0 3 8 35.37 17.19
0 -3 8 42.62 7.32
0 -3 -8 40.32 9.69
0 3 9 174.39 13.73
0 3 -9 182.22 10.27
0 -3 9 199.30 9.08
0 -3 -9 175.53 10.73
0 -3 -9 188.49 12.00
0 3 10 14.25 10.73
0 3 -10 14.74 11.47
0 -3 10 4.38 6.59
0 -3 -10 3.06 8.38
0 -3 -10 14.99 9.28
0 3 11 338.36 16.29
0 3 -11 315.35 12.19
0 -3 11 334.21 11.40
0 -3 -11 317.11 12.79
0 -3 -11 324.99 21.31
0 3 12 -1.25 11.47
0 3 -12 -2.32 7.79
0 -3 12 -0.33 7.04
0 -3 -12 7.55 8.71
0 -3 -12 13.00 10.34
0 3 13 57.56 13.60
0 3 -13 55.22 9.49
0 -3 13 31.19 8.29
0 -3 -13 39.29 15.15
0 -3 -13 40.69 11.92
0 3 -14 8.28 12.32
0 -3 -14 -0.86 9.22
0 -3 14 8.08 7.32
0 -3 -14 -25.75 10.48
0 3 -15 33.92 8.90
0 -3 -15 21.31 10.56
0 -3 15 27.68 8.66
0 -3 -15 30.64 12.03
0 3 -16 96.62 10.52
0 -3 -16 106.62 12.33
0 -3 16 96.82 10.02
0 -3 -16 106.39 14.13
0 3 -17 6.01 9.03
0 -3 -17 15.61 10.82
0 -3 17 11.40 8.90
0 -3 -17 26.18 12.11
0 3 -18 43.96 10.45
0 -3 -18 60.05 18.32
0 -3 18 40.59 10.04
0 -3 -18 60.35 13.90
0 3 -19 97.97 11.78
0 -3 19 138.01 15.51
0 -3 -19 84.17 13.32
0 -3 19 91.02 11.18
0 -3 -19 95.68 15.17
0 3 -20 15.76 10.75
0 -3 20 33.21 21.18
0 -3 -20 28.22 11.91
0 -3 20 20.46 10.20
0 -3 -20 31.87 13.96
0 3 -21 6.10 10.77
0 -3 21 -2.11 13.91
0 -3 -21 1.00 17.60
0 -3 21 3.83 9.52
0 -3 -21 7.50 13.36
0 3 -22 -8.51 10.39
0 -3 22 -9.01 21.14
0 -3 -22 6.83 11.59
0 -3 -22 -3.62 10.91
0 -3 -22 25.93 13.99
0 3 -23 23.41 11.53
0 -3 23 41.16 15.98
0 -3 -23 24.83 20.74
0 -3 -23 30.08 11.86
0 -3 -23 35.10 15.45
0 4 0 16.91 10.31
0 -4 0 7.27 9.80
0 4 1 148.91 12.85
0 4 -1 139.45 12.25
0 -4 1 116.83 17.08
0 -4 -1 146.90 11.94
0 4 2 172.33 13.12
0 4 -2 185.55 12.22
0 -4 2 192.95 11.62
0 -4 -2 177.89 12.34
0 4 3 11.68 11.32
0 4 -3 -3.89 15.37
0 -4 3 8.09 8.87
0 -4 -3 6.43 9.73
0 4 4 126.98 19.72
0 4 -4 102.07 11.57
0 -4 4 132.44 15.30
0 -4 -4 121.80 12.37
0 4 5 11.10 11.63
0 4 -5 6.92 14.80
0 -4 5 6.08 8.83
0 -4 -5 -2.61 10.33
0 4 -6 10.60 9.77
0 4 6 13.22 12.30
0 -4 6 30.07 9.05
0 -4 -6 16.73 11.43
0 4 -7 409.51 14.96
0 4 7 417.78 18.42
0 -4 7 420.79 14.31
0 -4 -7 416.10 24.51
0 4 -8 197.22 12.55
0 4 8 176.86 16.46
0 -4 8 191.68 11.71
0 -4 -8 177.62 14.24
0 4 -9 117.00 12.14
0 4 9 80.00 23.57
0 -4 9 86.21 10.25
0 -4 -9 86.48 13.84
0 4 10 15.97 13.66
0 4 -10 21.40 10.20
0 -4 10 10.66 9.04
0 -4 -10 5.85 10.68
0 -4 -10 46.32 18.99
0 4 11 2.16 15.00
0 4 -11 41.31 11.17
0 -4 11 30.69 15.00
0 -4 -11 35.26 11.67
0 -4 -11 36.71 13.20
0 4 12 4.32 14.55
0 4 -12 -8.38 9.83
0 -4 12 -10.76 8.94
0 -4 -12 6.84 10.84
0 -4 -12 11.75 11.74
0 4 13 26.71 15.63
0 4 -13 9.89 10.84
0 -4 13 15.69 9.76
0 -4 -13 34.88 11.70
0 -4 -13 39.58 13.40
0 4 14 39.84 25.54
0 4 -14 9.12 10.82
0 -4 14 12.05 9.78
0 -4 -14 38.52 11.87
0 -4 -14 13.40 13.50
0 4 15 55.12 18.27
0 4 -15 80.69 19.00
0 -4 15 77.94 16.56
0 -4 -15 52.98 20.67
0 -4 -15 85.56 15.67
0 4 -16 105.04 19.26
0 -4 -16 106.31 14.29
0 -4 16 85.31 11.84
0 -4 -16 90.06 24.63
0 4 -17 146.17 14.30
0 -4 -17 167.78 15.62
0 -4 17 144.63 13.25
0 -4 -17 142.74 26.31
0 4 -18 16.72 12.24
0 -4 -18 16.63 13.31
0 -4 18 30.49 16.38
0 -4 -18 31.57 22.62
0 4 -19 -2.82 11.68
0 -4 -19 5.54 19.35
0 -4 19 -2.11 10.41
0 -4 -19 -9.90 22.21
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10 0 -25 1.46 24.25
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10 0 -23 -13.96 16.17
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10 0 -20 369.07 28.69
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10 0 -17 22.00 12.36
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10 0 14 19.11 18.44
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10 -1 -24 -1.19 16.12
10 -1 -24 16.01 22.98
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10 -1 -23 12.32 16.01
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10 -1 -21 12.32 21.95
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10 -1 -20 29.69 14.64
10 -1 -20 21.70 32.13
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10 -1 -19 47.66 22.87
10 -1 -19 38.49 21.92
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10 -1 -18 44.64 13.44
10 -1 -18 11.97 19.13
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10 -1 -16 9.38 11.94
10 -1 -16 3.19 17.75
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10 -1 -15 124.25 18.26
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10 -1 -14 347.68 15.68
10 -1 -14 336.26 21.11
-10 -1 14 322.80 6.40
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10 -1 -13 282.96 20.21
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-10 -1 -1 17.33 10.61
-10 -1 -1 22.51 4.38
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-10 -1 -2 -0.17 10.61
-10 -1 -2 5.80 5.57
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-10 -1 -3 33.09 11.55
-10 -1 -3 16.59 5.28
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-10 -1 -4 -0.37 2.81
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-10 -1 -5 117.21 14.22
-10 -1 -5 99.44 3.77
10 1 6 295.55 17.61
10 1 6 305.94 6.18
10 -1 6 311.21 18.20
-10 -1 -6 320.23 25.44
-10 -1 -6 291.11 5.37
10 1 7 436.45 19.31
10 1 7 387.78 6.67
10 -1 7 383.07 20.72
-10 -1 -7 406.90 20.01
-10 -1 -7 384.05 6.61
10 1 8 17.48 14.56
10 -1 8 1.87 13.92
-10 -1 -8 13.89 15.07
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10 -1 9 390.28 31.53
-10 -1 -9 361.59 29.42
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10 -1 10 123.92 18.53
-10 -1 -10 108.77 17.26
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10 -1 11 310.57 22.21
-10 -1 -11 294.89 20.94
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10 -1 12 8.44 17.47
-10 -1 -12 20.67 17.38
10 1 13 6.96 17.81
10 -1 13 49.81 18.82
-10 -1 -13 7.74 16.73
10 1 14 38.15 18.78
10 -1 14 44.22 29.20
-10 -1 -14 22.70 18.34
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10 -1 15 11.14 19.17
-10 -1 -15 17.70 18.08
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10 -1 16 28.62 20.47
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10 -1 17 25.18 21.57
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10 -1 18 -1.74 31.82
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10 -2 -23 26.23 16.51
10 -2 -23 22.00 23.80
10 2 -22 30.39 17.59
10 -2 -22 48.93 17.20
10 -2 -22 46.34 23.14
10 2 -21 92.24 18.04
10 -2 -21 104.77 17.79
10 -2 -21 65.13 24.30
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10 -2 -20 41.46 17.09
10 -2 -20 77.28 34.41
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10 -2 -19 10.57 14.35
10 -2 -19 -27.84 30.68
-10 -2 19 9.70 13.46
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10 -2 -18 114.47 15.52
10 -2 -18 88.88 23.46
-10 -2 18 95.67 15.71
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10 -2 -17 67.95 15.12
10 -2 -17 63.53 20.55
-10 -2 17 78.29 14.61
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10 -2 -16 56.95 13.74
10 -2 -16 30.24 19.43
-10 -2 16 74.20 14.20
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10 -2 -15 38.26 12.73
10 -2 -15 19.99 18.28
-10 -2 15 27.30 6.01
-10 -2 15 13.16 13.28
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10 -2 -14 57.54 12.50
10 -2 -14 54.37 17.52
-10 -2 14 51.73 6.73
-10 -2 14 48.22 12.38
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10 -2 -13 37.89 12.10
10 -2 -13 91.59 16.87
-10 -2 13 70.66 7.42
-10 -2 13 86.80 12.44
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10 -2 -12 97.15 11.83
10 -2 -12 121.49 16.47
-10 -2 12 86.93 7.68
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10 -2 -11 78.83 11.06
10 -2 -11 65.18 5.74
10 -2 -11 85.86 15.01
-10 -2 11 84.89 11.55
-10 -2 11 56.96 11.35
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10 -2 -10 -2.64 8.71
10 -2 -10 -4.95 5.80
10 -2 -10 36.20 19.30
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10 -2 -9 310.97 8.47
10 -2 -9 349.96 16.73
-10 -2 9 345.07 11.54
-10 -2 9 348.82 14.31
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10 -2 -8 61.91 8.67
10 -2 -8 75.57 12.67
-10 -2 8 53.32 12.75
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10 -2 -7 224.42 8.05
10 -2 -7 243.76 13.99
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10 -2 -5 5.80 8.09
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10 -2 -4 29.36 6.70
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-10 -2 3 0.64 6.75
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10 -2 -2 539.03 12.25
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-10 -2 2 556.36 13.09
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10 -2 -1 140.74 10.53
10 -2 -1 138.94 10.20
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-10 -2 1 133.62 8.12
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10 -2 0 967.02 22.12
10 -2 0 984.06 18.20
-10 -2 0 1024.69 23.51
-10 -2 0 976.18 20.42
10 2 1 572.52 13.12
10 -2 1 523.63 17.30
10 -2 1 525.72 10.06
-10 -2 -1 530.03 18.43
-10 -2 -1 552.04 12.30
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10 -2 2 166.15 13.58
10 -2 2 143.98 5.46
-10 -2 -2 141.11 14.68
-10 -2 -2 144.83 7.31
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10 -2 3 8.24 17.05
10 -2 3 2.84 3.27
-10 -2 -3 12.81 11.98
-10 -2 -3 8.09 7.99
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10 -2 4 375.84 8.12
10 -2 4 379.15 6.51
-10 -2 -4 405.26 18.83
-10 -2 -4 381.71 9.70
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10 -2 5 95.81 4.04
10 -2 5 110.78 15.14
-10 -2 -5 93.57 16.03
-10 -2 -5 97.15 6.04
10 2 6 139.65 11.14
10 -2 6 138.57 16.28
-10 -2 -6 100.52 26.39
-10 -2 -6 140.00 8.96
10 2 7 -0.43 5.56
10 -2 7 7.96 13.73
-10 -2 -7 7.92 14.38
-10 -2 -7 -2.12 4.28
10 2 8 12.58 9.06
10 -2 8 -6.08 24.45
-10 -2 -8 12.96 15.82
-10 -2 -8 19.04 4.55
10 2 9 25.02 6.29
10 -2 9 20.52 17.11
-10 -2 -9 33.83 16.52
-10 -2 -9 28.35 6.95
10 2 10 14.73 15.30
10 2 10 4.53 8.99
10 -2 10 12.36 16.67
-10 -2 -10 12.19 16.37
-10 -2 -10 3.12 4.00
10 2 11 4.67 15.68
10 2 11 10.56 5.54
10 -2 11 -5.17 17.54
-10 -2 -11 -16.45 17.31
-10 -2 -11 4.54 3.75
10 2 12 39.61 18.10
10 -2 12 47.89 31.00
-10 -2 -12 34.93 18.76
10 2 13 44.55 19.43
10 -2 13 104.03 21.36
-10 -2 -13 80.28 19.63
10 -2 14 57.62 20.68
-10 -2 -14 -15.36 30.54
10 -2 15 53.51 21.51
-10 -2 -15 -5.75 19.39
10 -2 16 138.58 38.10
-10 -2 -16 108.00 22.51
10 -2 17 37.68 22.43
-10 -2 -17 17.23 31.43
10 3 -22 6.14 26.73
10 -3 -22 -2.34 27.15
10 -3 -22 29.95 35.33
-10 -3 22 13.80 26.01
10 3 -21 7.47 25.35
10 -3 -21 22.45 15.67
10 -3 -21 -13.16 32.66
-10 -3 21 -21.37 16.19
10 3 -20 32.28 23.12
10 -3 -20 -20.62 16.30
10 -3 -20 31.32 32.10
-10 -3 20 -0.27 15.53
10 3 -19 48.28 26.16
10 -3 -19 152.84 26.92
10 -3 -19 73.21 23.32
-10 -3 19 66.02 17.49
10 3 -18 10.19 22.61
10 -3 -18 -4.70 14.58
10 -3 -18 29.10 19.94
-10 -3 18 -24.93 14.15
10 3 -17 4.27 14.32
10 -3 -17 -6.99 14.69
10 -3 -17 -12.12 19.16
-10 -3 17 5.81 14.14
10 3 -16 34.88 14.83
10 -3 -16 30.88 14.31
10 -3 -16 38.85 18.96
-10 -3 16 40.59 14.23
10 3 -15 62.01 14.98
10 -3 -15 41.64 29.38
-10 -3 15 36.63 14.62
10 3 -14 40.57 14.18
10 -3 -14 12.68 27.40
-10 -3 14 2.79 21.69
10 3 -13 54.76 13.81
10 -3 -13 20.33 16.53
-10 -3 13 52.74 13.05
10 3 -12 -12.77 12.36
10 -3 -12 6.64 14.68
-10 -3 12 10.24 11.55
10 3 -11 396.62 25.53
10 -3 -11 435.79 21.05
-10 -3 11 435.17 18.02
10 3 -10 0.78 11.52
10 -3 -10 19.30 13.52
-10 -3 10 7.84 11.23
10 3 -9 336.99 16.25
10 -3 -9 378.53 18.41
-10 -3 9 360.30 22.84
10 3 -8 39.42 17.94
10 -3 -8 36.13 19.53
-10 -3 8 38.93 10.44
-10 -3 8 41.99 11.01
10 3 -7 -4.02 10.69
10 -3 -7 1.74 11.42
-10 -3 7 -4.63 10.15
-10 -3 7 -17.71 9.78
10 3 -6 4.63 9.72
10 -3 -6 -6.64 10.59
-10 -3 6 0.86 9.81
-10 -3 6 9.96 9.24
10 3 -5 119.28 11.91
10 -3 -5 131.08 12.38
-10 -3 5 129.48 12.99
-10 -3 5 115.17 11.09
10 3 -4 54.63 10.21
10 -3 -4 32.78 10.09
-10 -3 4 22.81 11.88
-10 -3 4 36.70 14.07
10 3 -3 -0.62 9.23
10 -3 -3 9.54 8.57
-10 -3 3 -2.25 17.67
-10 -3 3 1.40 8.31
10 3 -2 -11.13 13.63
10 -3 -2 6.87 11.65
-10 -3 2 5.24 11.57
-10 -3 2 -0.49 8.10
10 3 -1 20.66 9.35
10 -3 -1 9.84 7.59
-10 -3 1 30.56 12.60
-10 -3 1 24.82 8.13
10 3 0 9.80 9.02
10 -3 0 11.48 7.02
-10 -3 0 18.63 13.32
-10 -3 0 17.61 7.90
10 3 1 201.24 11.82
10 -3 1 202.23 8.96
-10 -3 -1 207.05 16.57
-10 -3 -1 207.70 15.22
10 3 2 96.29 14.90
10 -3 2 102.88 7.49
-10 -3 -2 100.58 16.27
-10 -3 -2 98.86 9.23
10 3 3 322.73 17.63
-10 3 -3 295.48 10.87
10 -3 3 306.36 18.48
-10 -3 -3 333.37 19.47
-10 -3 -3 303.09 11.50
10 -3 3 289.13 11.96
10 3 4 9.97 8.05
-10 3 -4 4.13 6.58
10 -3 4 -11.48 13.83
-10 -3 -4 33.81 14.92
-10 -3 -4 8.55 11.07
10 -3 4 5.59 5.05
10 3 5 9.18 7.86
-10 3 -5 -10.96 6.10
10 -3 5 -7.55 13.93
-10 -3 -5 -35.61 22.22
-10 -3 -5 -0.74 6.69
10 -3 5 3.07 6.59
10 3 6 34.33 9.23
10 -3 6 25.60 6.66
10 -3 6 1.16 24.25
-10 -3 -6 25.25 17.08
-10 -3 -6 38.77 7.36
10 3 7 67.72 9.87
10 -3 7 71.91 6.15
10 -3 7 37.04 17.60
-10 -3 -7 74.36 19.06
-10 -3 -7 69.33 11.87
10 3 8 -9.11 12.64
10 -3 8 1.14 3.95
10 -3 8 17.43 15.77
-10 -3 -8 -1.87 15.40
-10 -3 -8 1.61 6.45
10 3 9 64.79 14.93
10 -3 9 80.59 18.55
-10 -3 -9 92.95 19.72
-10 -3 -9 74.32 7.82
10 3 10 1.22 13.52
10 -3 10 32.52 27.61
-10 -3 -10 -8.88 27.95
-10 -3 -10 3.12 6.42
10 3 11 17.22 14.49
10 -3 11 25.76 19.22
-10 -3 -11 10.88 18.59
-10 -3 -11 2.92 10.24
10 3 12 42.05 9.97
10 -3 12 49.62 20.83
-10 -3 -12 76.09 21.26
-10 -3 -12 50.25 10.83
10 3 13 63.81 10.10
10 -3 13 74.09 23.00
-10 -3 -13 86.96 22.49
-10 -3 -13 71.25 10.81
10 -3 14 82.42 23.32
-10 -3 -14 52.43 22.29
-10 -3 -14 43.41 6.71
10 -3 15 156.40 26.74
-10 -3 -15 160.88 37.54
10 -3 16 36.73 25.16
-10 -3 -16 61.89 22.98
10 4 -20 75.52 19.41
10 -4 -20 48.05 19.96
-10 -4 20 28.53 18.68
10 4 -19 5.58 26.96
10 -4 -19 22.49 23.25
-10 -4 19 2.01 16.84
10 4 -18 9.72 27.88
10 -4 -18 49.71 22.42
-10 -4 18 64.96 17.38
10 4 -17 -15.00 24.36
10 -4 -17 28.33 20.18
-10 -4 17 -11.03 24.40
10 4 -16 42.64 16.96
10 -4 -16 -8.23 20.84
-10 -4 16 18.60 16.40
10 4 -15 48.84 18.07
10 -4 -15 66.18 32.52
-10 -4 15 80.39 17.05
10 4 -14 90.37 17.30
10 -4 -14 117.35 30.37
-10 -4 14 100.61 17.06
10 4 -13 -10.47 15.68
10 -4 -13 -0.68 18.04
-10 -4 13 -18.82 14.24
10 4 -12 137.27 16.90
10 -4 -12 115.31 19.59
-10 -4 12 87.32 24.28
10 4 -11 4.47 22.23
10 -4 -11 3.70 15.62
-10 -4 11 13.33 13.37
10 4 -10 64.59 15.45
10 -4 -10 37.88 16.43
-10 -4 10 74.51 14.48
10 4 -9 34.18 14.95
10 -4 -9 48.39 23.63
-10 -4 9 44.94 13.67
10 4 -8 35.09 21.65
10 -4 -8 54.80 14.76
-10 -4 8 4.99 12.45
10 4 -7 16.67 13.64
10 -4 -7 9.58 12.93
-10 -4 7 0.59 11.86
10 4 -6 -3.74 12.79
10 -4 -6 -4.12 18.55
-10 -4 6 -2.70 11.32
10 4 -5 101.96 14.48
10 -4 -5 90.31 13.30
-10 -4 5 94.64 15.68
-10 -4 5 92.72 12.85
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-10 4 4 1.98 12.69
10 -4 -4 18.30 16.06
-10 -4 4 0.78 16.20
-10 -4 4 -2.63 12.70
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-10 4 3 15.63 12.18
10 -4 -3 3.15 10.26
-10 -4 3 -13.30 10.56
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10 4 -2 23.30 12.41
-10 4 2 43.99 13.21
10 -4 -2 41.81 10.46
-10 -4 2 29.10 10.95
-10 -4 2 27.61 14.90
10 4 -1 80.85 13.31
-10 4 1 110.75 20.32
10 -4 -1 101.58 11.17
-10 -4 1 83.77 11.92
-10 -4 1 72.65 16.54
10 4 0 53.24 13.15
-10 4 0 75.75 12.61
10 -4 0 74.03 10.10
-10 -4 0 71.99 10.88
-10 -4 0 98.41 25.87
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-10 -4 -1 5.64 15.68
-10 -4 -1 7.97 9.81
10 -4 1 9.30 8.31
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10 4 2 57.17 12.90
-10 -4 -2 86.18 17.44
-10 -4 -2 61.62 10.52
10 -4 2 53.10 9.25
-10 4 -3 187.63 12.89
10 4 3 188.05 14.74
-10 -4 -3 186.50 20.20
-10 -4 -3 189.79 12.54
10 -4 3 176.43 10.58
-10 4 -4 224.43 19.17
10 4 4 240.20 15.26
-10 -4 -4 223.24 22.70
-10 -4 -4 238.30 13.40
10 -4 4 230.22 10.60
-10 4 -5 111.05 15.98
10 4 5 114.24 13.68
-10 -4 -5 90.98 32.39
-10 -4 -5 121.95 16.61
10 -4 5 110.76 8.48
-10 4 -6 50.63 14.36
10 4 6 56.71 19.75
-10 -4 -6 41.24 19.28
-10 -4 -6 46.77 10.28
10 -4 6 54.78 7.07
10 4 7 11.59 11.69
-10 4 -7 10.71 8.12
10 -4 7 30.10 17.63
-10 -4 -7 -21.94 18.59
-10 -4 -7 9.76 9.17
10 -4 7 5.78 5.56
10 4 8 3.18 11.35
-10 4 -8 1.08 6.76
10 -4 8 -1.11 18.35
-10 -4 -8 23.05 18.59
-10 -4 -8 6.81 8.89
10 -4 8 -0.14 4.86
10 4 9 10.34 11.99
-10 4 -9 5.53 10.00
10 -4 9 26.24 19.62
-10 -4 -9 6.16 19.85
-10 -4 -9 0.81 13.84
10 -4 9 9.28 4.57
10 4 10 6.61 12.16
10 -4 10 21.56 30.31
-10 -4 -10 24.86 31.03
-10 -4 -10 -2.41 13.81
10 4 11 21.47 12.85
10 -4 11 5.82 21.61
-10 -4 -11 32.56 21.28
-10 -4 -11 29.60 9.73
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10 -4 12 17.08 21.09
-10 -4 -12 -27.00 20.24
-10 -4 -12 -6.01 8.25
10 4 13 83.67 19.76
10 -4 13 58.32 24.24
-10 -4 -13 79.91 24.30
-10 -4 -13 44.26 9.96
10 5 -16 72.83 33.01
10 -5 -16 66.20 24.38
-10 -5 16 127.81 30.47
10 5 -15 -0.37 19.47
10 -5 -15 2.90 21.21
-10 -5 15 -26.99 17.25
10 5 -14 89.47 21.03
10 -5 -14 70.11 33.37
-10 -5 14 92.60 19.65
10 5 -13 -3.43 18.33
10 -5 -13 46.26 27.94
-10 -5 13 -5.15 16.21
10 5 -12 10.54 17.84
10 -5 -12 5.44 18.25
-10 -5 12 27.16 16.60
10 5 -11 33.19 17.70
10 -5 -11 -9.21 17.71
-10 -5 11 9.09 25.40
10 5 -10 0.94 17.25
10 -5 -10 33.61 17.92
-10 -5 10 37.97 16.40
10 5 -9 1.71 16.90
10 -5 -9 39.52 26.06
-10 -5 9 24.85 15.75
10 5 -8 60.62 17.53
10 -5 -8 48.23 17.19
-10 -5 8 49.05 15.27
10 5 -7 164.79 29.75
-10 5 7 125.71 21.89
-10 -5 7 196.49 18.17
10 -5 -7 148.14 18.19
10 5 -6 191.82 19.58
-10 5 6 209.03 22.08
-10 -5 6 226.54 18.24
10 -5 -6 201.94 28.16
10 5 -5 65.26 17.51
-10 5 5 86.81 19.23
-10 -5 5 60.70 15.53
10 -5 -5 86.84 15.68
10 5 -4 3.09 15.36
-10 5 4 -19.07 25.00
10 -5 -4 18.07 12.88
-10 -5 4 12.95 13.50
-10 -5 4 15.42 16.67
10 5 -3 9.38 14.89
-10 5 3 -19.38 16.14
10 -5 -3 20.13 12.93
-10 -5 3 -0.25 13.44
-10 -5 3 13.19 16.39
-10 5 2 -6.69 14.73
10 5 -2 -7.09 23.08
-10 -5 2 29.62 16.86
-10 -5 2 -4.67 12.71
10 -5 -2 4.86 12.04
-10 5 1 76.13 16.21
10 5 -1 76.94 16.46
-10 -5 1 24.29 20.65
-10 -5 1 61.91 14.32
10 -5 -1 81.19 12.98
-10 5 0 20.47 22.36
10 5 0 3.69 23.15
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-10 -5 0 10.59 12.76
10 -5 0 -4.15 17.14
-10 5 -1 -3.76 21.19
10 5 1 17.42 14.84
-10 -5 -1 6.17 18.47
-10 -5 -1 9.19 19.87
10 -5 1 10.64 10.94
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10 5 2 -5.16 14.35
-10 -5 -2 -2.81 19.03
-10 -5 -2 11.28 12.03
10 -5 2 9.14 10.18
-10 5 -3 -8.89 12.72
10 5 3 -2.73 14.15
-10 -5 -3 10.88 19.00
-10 -5 -3 1.29 11.86
10 -5 3 18.21 9.71
10 5 4 -2.50 14.68
-10 5 -4 9.56 12.40
-10 -5 -4 9.73 11.91
-10 -5 -4 24.52 30.17
-10 5 -5 64.79 13.67
10 5 5 63.22 24.85
-10 -5 -5 48.08 23.50
-10 -5 -5 80.17 20.43
10 -5 5 75.01 10.48
-10 5 -6 23.26 12.22
10 5 6 51.97 15.16
-10 -5 -6 54.05 21.90
-10 -5 -6 23.41 12.05
10 -5 6 29.91 9.14
-10 5 -7 19.08 16.52
10 5 7 25.26 15.40
-10 -5 -7 -0.17 33.50
-10 -5 -7 0.92 11.88
10 -5 7 13.13 7.99
-10 5 -8 8.72 14.37
10 5 8 -1.21 14.49
-10 -5 -8 -14.80 20.84
-10 -5 -8 -8.94 10.97
10 -5 8 5.12 6.69
10 5 9 32.45 15.89
-10 -5 -9 19.56 22.97
-10 -5 -9 11.87 12.16
10 5 10 34.27 15.84
10 -5 10 -10.42 23.30
-10 -5 -10 -9.84 23.67
-10 -5 -10 11.05 17.87
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10 -6 -9 9.71 18.38
-10 -6 9 7.43 27.04
10 6 -8 6.16 19.96
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10 -6 -8 9.33 27.30
10 6 -7 12.83 19.56
-10 6 7 -22.51 21.53
-10 -6 7 0.48 17.19
10 -6 -7 35.04 17.17
10 6 -6 4.61 19.66
-10 6 6 26.48 21.10
-10 -6 6 -8.14 25.53
10 -6 -6 16.63 16.86
10 6 -5 3.40 19.41
-10 6 5 -7.18 31.55
10 -6 -5 14.71 25.03
-10 -6 5 36.49 17.25
-10 6 4 99.60 22.33
10 6 -4 91.73 21.59
-10 -6 4 68.64 22.54
-10 -6 4 82.07 19.27
10 -6 -4 90.31 17.17
-10 6 3 42.10 20.07
10 6 -3 22.01 30.41
-10 -6 3 40.08 21.92
-10 -6 3 7.28 26.58
10 -6 -3 32.87 16.28
-10 6 2 20.04 18.05
10 6 -2 -9.32 18.00
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-10 -6 2 -23.37 16.02
10 -6 -2 11.50 14.34
-10 6 1 43.65 29.74
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-10 -6 1 49.25 17.45
10 -6 -1 54.02 15.91
-10 6 0 10.77 25.89
10 6 0 -30.23 17.72
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10 -6 0 -12.99 13.02
-10 6 -1 11.80 17.22
10 6 1 0.70 18.14
-10 -6 -1 1.84 21.97
-10 -6 -1 15.19 24.46
10 -6 1 3.21 13.23
-10 6 -2 79.76 18.09
10 6 2 66.83 21.05
-10 -6 -2 60.98 38.86
-10 -6 -2 66.83 17.41
10 -6 2 69.35 14.29
10 -6 3 14.93 18.31
-10 -6 -3 -0.72 14.93
11 0 -24 -2.96 16.14
11 0 -23 4.52 16.06
11 0 -22 -13.11 15.93
11 0 -21 5.42 14.88
11 0 -20 21.70 14.10
11 0 -19 9.26 13.56
11 0 -18 176.74 24.54
11 0 -17 0.27 11.44
11 0 -16 453.59 19.20
11 0 -15 14.29 11.72
11 0 -14 5.06 10.27
11 0 -13 5.81 9.88
11 0 -12 390.61 15.19
11 0 -11 1.90 8.78
11 0 -10 45.16 8.99
11 0 -9 -0.95 7.49
11 0 -8 55.57 12.06
-11 0 8 34.48 5.28
11 0 -7 1.38 4.27
11 0 -7 3.30 6.49
-11 0 7 -0.56 4.96
11 0 -6 14.54 5.05
11 0 -6 9.81 5.85
-11 0 6 28.03 9.12
11 0 -5 -0.92 8.27
11 0 -5 -4.95 5.10
-11 0 5 1.62 9.71
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11 0 -3 -1.34 10.77
11 0 -3 -6.85 4.22
-11 0 3 -2.65 7.39
11 0 -2 37.85 8.54
11 0 -2 41.34 4.53
-11 0 2 43.33 8.73
11 0 -1 4.56 8.68
11 0 -1 1.95 3.49
-11 0 1 -3.99 8.50
11 0 0 299.56 19.07
11 0 0 270.58 6.43
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-11 0 -1 -9.09 14.87
11 0 2 80.29 11.89
11 0 2 60.73 3.14
-11 0 -2 66.91 11.23
11 0 3 4.95 10.78
11 0 3 0.49 1.74
11 0 3 5.26 4.17
-11 0 -3 7.35 10.60
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11 0 5 -4.78 12.57
-11 0 -5 -5.26 12.08
11 0 6 132.86 16.10
-11 0 -6 122.14 14.90
11 0 7 -0.30 13.24
11 0 8 363.15 20.59
11 0 9 24.11 16.10
11 0 10 -24.76 17.53
11 0 11 13.60 16.80
11 0 12 82.56 20.38
11 0 13 3.59 28.83
11 0 14 12.63 18.79
11 0 15 6.38 20.37
11 0 16 0.96 19.83
11 0 17 13.98 21.10
11 1 -24 23.42 17.08
11 -1 -24 6.64 17.69
11 -1 -24 55.82 24.76
11 1 -23 2.83 16.72
11 -1 -23 12.16 16.31
11 -1 -23 31.46 23.90
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11 -1 -22 -4.74 15.25
11 -1 -22 -15.52 21.69
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11 -1 -21 98.01 17.20
11 -1 -21 60.92 23.55
11 1 -20 32.11 15.55
11 -1 -20 21.15 15.37
11 -1 -20 6.36 33.92
11 1 -19 35.63 15.25
11 -1 -19 26.78 15.28
11 -1 -19 53.00 21.23
11 1 -18 -3.79 21.45
11 -1 -18 36.53 13.72
11 -1 -18 25.87 20.06
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11 -1 -17 6.96 19.44
11 -1 -17 -28.82 18.42
11 1 -16 239.37 23.63
11 -1 -16 258.77 16.43
11 -1 -16 271.77 23.05
11 1 -15 40.55 19.26
11 -1 -15 48.06 12.87
11 -1 -15 44.79 18.47
-11 -1 15 62.05 13.24
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11 -1 -14 121.43 13.39
11 -1 -14 154.24 18.63
-11 -1 14 159.85 13.89
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11 -1 -13 17.30 10.30
11 -1 -13 36.06 15.10
-11 -1 13 13.32 6.06
-11 -1 13 17.55 10.33
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11 -1 -12 8.72 9.81
11 -1 -12 26.94 14.38
-11 -1 12 11.49 4.40
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11 -1 -11 24.01 9.16
11 -1 -11 27.69 13.63
-11 -1 11 18.92 5.08
-11 -1 11 21.23 10.11
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11 -1 -10 5.67 8.23
11 -1 -10 2.54 4.53
11 -1 -10 6.08 12.19
-11 -1 10 -2.41 5.24
-11 -1 10 17.03 8.87
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11 -1 -9 104.09 14.28
11 -1 -9 79.40 7.09
11 -1 -9 77.08 13.70
-11 -1 9 93.41 6.88
-11 -1 9 105.63 10.15
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11 -1 -8 185.26 13.95
11 -1 -8 177.28 9.20
11 -1 -8 186.00 13.96
-11 -1 8 183.39 8.62
-11 -1 8 193.46 15.38
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11 -1 -7 203.85 12.56
11 -1 -7 191.92 10.06
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-18 -3 5 26.35 11.54
18 3 -4 33.63 12.47
18 -3 -4 24.87 8.19
18 -3 -4 6.36 13.53
18 -3 -4 8.40 14.47
-18 -3 4 5.19 18.67
-18 -3 4 16.79 10.75
18 3 -3 6.24 11.87
18 -3 -3 10.23 7.04
18 -3 -3 24.01 13.92
18 -3 -3 8.72 7.78
-18 -3 3 -38.20 19.11
-18 -3 3 2.18 10.03
18 3 -2 19.35 11.77
18 -3 -2 20.94 16.59
-18 -3 2 17.60 30.95
-18 -3 2 46.64 10.69
19 0 -14 16.47 14.25
19 0 -13 1.37 12.97
19 0 -12 40.10 20.94
19 0 -11 -9.38 11.74
19 0 -10 11.07 11.56
19 0 -9 11.75 10.55
19 0 -8 75.61 16.34
19 0 -8 80.48 14.98
19 0 -7 -3.97 8.90
19 0 -7 2.08 12.40
19 0 -6 75.42 14.52
19 0 -6 58.76 13.44
19 0 -5 -7.19 7.61
19 0 -5 3.51 11.10
19 0 -4 -8.09 13.09
19 0 -4 -3.22 10.10
19 0 -4 4.15 9.69
19 0 -3 15.84 14.82
19 0 -3 0.63 9.21
19 0 -3 4.11 8.74
19 0 -2 37.75 24.96
19 0 -1 8.46 16.20
19 0 0 19.54 18.21
19 0 1 -10.36 17.92
19 0 2 -13.80 18.80
19 1 -13 83.73 16.42
19 -1 -13 80.27 14.49
19 -1 -13 83.47 20.46
19 1 -12 26.74 13.92
19 -1 -12 -8.88 12.50
19 -1 -12 4.99 17.35
19 1 -11 53.82 22.35
19 -1 -11 79.17 13.17
19 -1 -11 93.82 26.48
19 1 -10 4.08 12.65
19 -1 -10 17.55 10.80
19 -1 -10 7.70 14.49
19 1 -9 75.44 13.17
19 -1 -9 60.22 11.35
19 -1 -9 73.00 15.91
19 1 -8 18.80 17.43
19 -1 -8 25.85 14.32
19 -1 -8 11.38 9.45
19 -1 -8 15.60 13.72
19 1 -7 1.68 10.43
19 -1 -7 0.97 8.46
19 -1 -7 5.85 10.80
19 -1 -7 -5.06 12.25
-19 -1 7 20.35 12.45
19 1 -6 10.90 15.17
19 -1 -6 14.23 8.18
19 -1 -6 17.59 12.08
19 -1 -6 18.99 11.31
-19 -1 6 32.12 13.77
19 1 -5 1.09 8.33
19 -1 -5 0.50 6.91
19 -1 -5 4.34 17.76
19 -1 -5 -2.49 9.23
-19 -1 5 -1.11 13.25
19 1 -4 0.87 8.06
19 -1 -4 1.26 6.24
19 -1 -4 -7.92 12.98
19 -1 -4 14.05 13.06
-19 -1 4 22.75 14.45
19 1 -3 4.24 10.73
19 -1 -3 -0.63 14.06
-19 -1 3 -1.22 15.19
19 1 -2 27.16 7.53
19 -1 -2 28.50 16.25
-19 -1 2 30.48 17.57
19 -1 -1 51.83 25.65
-19 -1 1 -4.88 17.26
19 -1 0 -13.97 27.60
-19 -1 0 27.17 17.93
19 -1 1 -3.80 18.72
-19 -1 -1 23.80 19.08
19 2 -10 17.22 14.26
19 -2 -10 43.09 11.42
19 -2 -10 50.72 15.93
-19 -2 10 26.29 13.10
19 2 -9 17.85 12.84
19 -2 -9 25.53 15.53
19 -2 -9 3.47 8.31
19 -2 -9 -4.88 13.65
-19 -2 9 4.17 13.29
-19 -2 9 8.29 12.15
19 2 -8 31.35 12.70
19 -2 -8 18.80 9.92
19 -2 -8 9.35 10.01
19 -2 -8 34.45 19.78
-19 -2 8 10.39 14.53
-19 -2 8 17.89 11.94
19 2 -7 -2.45 12.05
19 -2 -7 7.21 8.96
19 -2 -7 9.49 10.19
19 -2 -7 14.50 11.38
-19 -2 7 3.29 14.41
-19 -2 7 -8.68 10.75
19 2 -6 45.97 12.11
19 -2 -6 18.20 8.89
19 -2 -6 23.31 12.40
19 -2 -6 30.95 11.33
-19 -2 6 14.63 16.30
-19 -2 6 50.44 11.09
19 2 -5 6.22 11.29
19 -2 -5 9.17 11.31
19 -2 -5 27.16 18.73
19 -2 -5 12.74 9.40
-19 -2 5 -16.45 16.44
-19 -2 5 1.57 9.58
19 2 -4 121.38 18.44
19 -2 -4 90.66 23.46
19 -2 -4 77.32 15.06
-19 -2 4 115.41 19.58
-19 -2 4 88.29 11.35
19 2 -3 34.88 10.29
19 -2 -3 20.02 15.05
-19 -2 3 -7.46 18.59
19 2 -2 23.54 9.24
19 -2 -2 25.86 16.38
-19 -2 2 28.73 29.38
20 0 -9 -10.78 10.77
20 0 -9 4.96 14.00
20 0 -8 39.79 11.50
20 0 -8 55.86 14.39
20 0 -7 5.55 14.29
20 0 -7 15.11 12.92
20 0 -6 5.68 7.97
20 0 -6 1.93 17.97
20 0 -5 0.92 10.89
20 0 -5 1.39 10.11
0 0 0 0.00 0.00
;
_shelx_hkl_checksum 72242
_shelx_res_file
;
TITL SH208
shelx.res
created by SHELXL-2019/2 at 20:52:57 on 14-Jun-2023
CELL 0.71075 15.54445 5.53876 20.15923 90.00000 103.67550 90.00000
ZERR 2 0.00058 0.00026 0.00076 0.00000 0.00730 0.00000
LATT 1
SYMM -X, .50+Y, .50-Z
SFAC C H N NI S
UNIT 56 84 8 2 12
L.S. 5
FMAP 2
PLAN 28
EQIV $2 x, -y+1/2, z-1/2
HTAB C2 S1_$2
EQIV $3 x, -y-1/2, z-1/2
HTAB C2 S2_$3
EQIV $1 -x+1, -y+1, -z+1
HTAB C5 S1_$1
HTAB C7 S3
EQIV $4 1-x, 1-y, 1-z
EQIV $5 x, 1+y, z
EQIV $6 1-x, 2-y, 1-z
mpla S3 C1 > c4
mpla N1 N2 Ni1 C6 S1
mpla Ni1 > S3 C1 > C14
MPLA 9 Ni1 N1 N2 C6 S1 N1_$4 N2_$4 C6_$4 S1_$4
mpla 9 NI1_$5 N1_$5 N2_$5 C6_$5 S1_$5 N1_$6 N2_$6 C6_$6 S1_$6
HTAB
BOND $H
CONF
TEMP -100.0
ACTA
SIZE 0.080 0.020 0.010
WGHT 0.032900 0.012800
FVAR 0.43160
NI1 4 0.500000 0.500000 0.500000 10.50000 0.02940 0.02126 =
0.02284 -0.00261 0.00554 -0.00160
S1 5 0.432488 0.341727 0.572395 11.00000 0.04201 0.03201 =
0.02560 -0.00524 0.00954 -0.01033
S2 5 0.300200 -0.044690 0.550729 11.00000 0.04146 0.02945 =
0.02868 0.00039 0.01048 -0.00856
S3 5 0.333207 -0.171144 0.335658 11.00000 0.04195 0.02782 =
0.02999 -0.00263 0.00615 -0.00619
N1 3 0.436770 0.268062 0.436172 11.00000 0.02989 0.02204 =
0.02695 -0.00129 0.00673 -0.00141
N2 3 0.377763 0.103358 0.454524 11.00000 0.03447 0.02246 =
0.02647 -0.00075 0.00977 -0.00495
C1 1 0.322991 -0.268935 0.253765 11.00000 0.04064 0.03300 =
0.03242 -0.01012 0.00213 -0.00415
AFIX 43
H1 2 0.290649 -0.408991 0.235505 11.00000 -1.20000
AFIX 0
C2 1 0.365792 -0.125934 0.217728 11.00000 0.03911 0.04601 =
0.02968 -0.01262 0.00761 -0.00383
AFIX 43
H2 2 0.366185 -0.152919 0.171263 11.00000 -1.20000
AFIX 0
C3 1 0.409556 0.066781 0.256682 11.00000 0.03653 0.03681 =
0.02646 -0.00510 0.00875 -0.00436
AFIX 43
H3 2 0.443110 0.184342 0.239444 11.00000 -1.20000
AFIX 0
C4 1 0.398719 0.067735 0.322964 11.00000 0.02979 0.02318 =
0.02784 -0.00252 0.00458 -0.00076
C5 1 0.441394 0.240000 0.372898 11.00000 0.03269 0.02596 =
0.02978 -0.00155 0.01089 -0.00377
AFIX 43
H5 2 0.478965 0.351305 0.357540 11.00000 -1.20000
AFIX 0
C6 1 0.372796 0.132331 0.517391 11.00000 0.02702 0.02017 =
0.02846 0.00369 0.00489 0.00084
C7 1 0.254554 -0.237723 0.478579 11.00000 0.03767 0.02608 =
0.03063 -0.00091 0.00683 -0.00448
AFIX 23
H7A 2 0.228117 -0.136545 0.438453 11.00000 -1.20000
H7B 2 0.302730 -0.334361 0.467263 11.00000 -1.20000
AFIX 0
C8 1 0.184150 -0.406953 0.493470 11.00000 0.03733 0.02906 =
0.03468 0.00186 0.00772 -0.00637
AFIX 23
H8A 2 0.210547 -0.512821 0.532553 11.00000 -1.20000
H8B 2 0.136169 -0.311795 0.505600 11.00000 -1.20000
AFIX 0
C9 1 0.146654 -0.559602 0.430569 11.00000 0.03794 0.03143 =
0.03983 -0.00265 0.00913 -0.00738
AFIX 23
H9A 2 0.123844 -0.450452 0.391478 11.00000 -1.20000
H9B 2 0.195365 -0.655482 0.419806 11.00000 -1.20000
AFIX 0
C10 1 0.072909 -0.730694 0.437571 11.00000 0.03967 0.03001 =
0.04206 -0.00197 0.01225 -0.00724
AFIX 23
H10A 2 0.025185 -0.637168 0.450618 11.00000 -1.20000
H10B 2 0.096283 -0.847621 0.474588 11.00000 -1.20000
AFIX 0
C11 1 0.034443 -0.867940 0.371953 11.00000 0.03958 0.03704 =
0.04047 -0.00371 0.00782 -0.00975
AFIX 23
H11A 2 0.011898 -0.749798 0.335090 11.00000 -1.20000
H11B 2 0.082584 -0.960448 0.359172 11.00000 -1.20000
AFIX 0
C12 1 -0.039788 -1.040752 0.376053 11.00000 0.04185 0.03553 =
0.04299 -0.00272 0.00901 -0.00888
AFIX 23
H12A 2 -0.016871 -1.163148 0.411632 11.00000 -1.20000
H12B 2 -0.087282 -0.949827 0.390228 11.00000 -1.20000
AFIX 0
C13 1 -0.078958 -1.168614 0.309295 11.00000 0.05650 0.05970 =
0.05222 -0.01139 0.00839 -0.02063
AFIX 23
H13A 2 -0.102651 -1.046174 0.273913 11.00000 -1.20000
H13B 2 -0.031228 -1.257274 0.294768 11.00000 -1.20000
AFIX 0
C14 1 -0.152142 -1.344190 0.313342 11.00000 0.06344 0.06207 =
0.07186 -0.00919 -0.00531 -0.02612
AFIX 137
H14A 2 -0.128788 -1.469718 0.347054 11.00000 -1.20000
H14B 2 -0.174872 -1.418856 0.268549 11.00000 -1.20000
H14C 2 -0.200158 -1.257687 0.327044 11.00000 -1.20000
AFIX 0
HKLF 4
REM SH208
REM wR2 = 0.0787, GooF = S = 0.999, Restrained GooF = 0.999 for all data
REM R1 = 0.0446 for 2621 Fo > 4sig(Fo) and 0.0832 for all 3850 data
REM 179 parameters refined using 0 restraints
END
WGHT 0.0329 0.0128
REM Instructions for potential hydrogen bonds
HTAB C2 S1_$2
HTAB C2 S2_$3
HTAB C5 S1_$1
HTAB C7 S3
REM Highest difference peak 0.441, deepest hole -0.272, 1-sigma level 0.067
Q1 1 0.4687 0.3825 0.5353 11.00000 0.05 0.44
Q2 1 0.4307 0.0202 0.2960 11.00000 0.05 0.30
Q3 1 0.3395 0.0747 0.5327 11.00000 0.05 0.30
Q4 1 0.2519 -0.5281 0.2873 11.00000 0.05 0.29
Q5 1 0.2687 -0.1342 0.5110 11.00000 0.05 0.29
Q6 1 0.4593 0.2473 0.4211 11.00000 0.05 0.29
Q7 1 0.5316 0.4516 0.4680 11.00000 0.05 0.28
Q8 1 0.2679 -0.0119 0.5834 11.00000 0.05 0.27
Q9 1 0.4111 0.2002 0.4419 11.00000 0.05 0.27
Q10 1 0.4599 0.3629 0.4616 11.00000 0.05 0.27
Q11 1 0.3776 -0.0294 0.3416 11.00000 0.05 0.26
Q12 1 0.3978 0.4869 0.4414 11.00000 0.05 0.26
Q13 1 0.4351 0.5279 0.5620 11.00000 0.05 0.25
Q14 1 0.3051 -0.2087 0.2779 11.00000 0.05 0.25
Q15 1 0.3506 0.0240 0.3100 11.00000 0.05 0.25
Q16 1 0.4659 0.3281 0.4770 11.00000 0.05 0.25
Q17 1 0.1084 -0.6511 0.4116 11.00000 0.05 0.24
Q18 1 0.4022 0.4216 0.5998 11.00000 0.05 0.24
Q19 1 0.0893 -1.0629 0.3782 11.00000 0.05 0.24
Q20 1 0.4210 0.1553 0.5393 11.00000 0.05 0.23
Q21 1 0.3000 -0.3497 0.2490 11.00000 0.05 0.23
Q22 1 0.3794 0.0656 0.1284 11.00000 0.05 0.23
Q23 1 0.4083 0.5437 0.6040 11.00000 0.05 0.22
Q24 1 0.4006 0.1590 0.3392 11.00000 0.05 0.22
Q25 1 0.3008 -0.2172 0.3675 11.00000 0.05 0.22
Q26 1 -0.1201 -1.4673 0.2369 11.00000 0.05 0.22
Q27 1 0.3966 0.2185 0.5523 11.00000 0.05 0.21
Q28 1 0.3101 -0.1510 0.2382 11.00000 0.05 0.21
;
_shelx_res_checksum 83466
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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 0.500000 0.500000 0.02461(12) Uani d 1 . .
S S1 0.43249(4) 0.34173(13) 0.57239(3) 0.03295(17) Uani d 1 . .
S S2 0.30020(4) -0.04469(12) 0.55073(3) 0.03283(17) Uani d 1 . .
S S3 0.33321(4) -0.17114(13) 0.33566(3) 0.03364(17) Uani d 1 . .
N N1 0.43677(12) 0.2681(4) 0.43617(10) 0.0263(5) Uani d 1 . .
N N2 0.37776(13) 0.1034(4) 0.45452(10) 0.0274(5) Uani d 1 . .
C C1 0.32299(17) -0.2689(5) 0.25377(13) 0.0364(7) Uani d 1 . .
H H1 0.290649 -0.408991 0.235505 0.044 Uiso calc 1 . .
C C2 0.36579(17) -0.1259(5) 0.21773(13) 0.0384(7) Uani d 1 . .
H H2 0.366185 -0.152919 0.171263 0.046 Uiso calc 1 . .
C C3 0.40956(16) 0.0668(5) 0.25668(12) 0.0331(6) Uani d 1 . .
H H3 0.443110 0.184342 0.239444 0.040 Uiso calc 1 . .
C C4 0.39872(15) 0.0677(4) 0.32296(12) 0.0273(6) Uani d 1 . .
C C5 0.44139(15) 0.2400(5) 0.37290(12) 0.0289(6) Uani d 1 . .
H H5 0.478965 0.351305 0.357540 0.035 Uiso calc 1 . .
C C6 0.37280(14) 0.1323(4) 0.51739(12) 0.0255(5) Uani d 1 . .
C C7 0.25455(16) -0.2377(5) 0.47858(12) 0.0317(6) Uani d 1 . .
H H7A 0.228117 -0.136545 0.438453 0.038 Uiso calc 1 . .
H H7B 0.302730 -0.334361 0.467263 0.038 Uiso calc 1 . .
C C8 0.18415(17) -0.4070(5) 0.49347(13) 0.0338(6) Uani d 1 . .
H H8A 0.210547 -0.512821 0.532553 0.041 Uiso calc 1 . .
H H8B 0.136169 -0.311795 0.505600 0.041 Uiso calc 1 . .
C C9 0.14665(17) -0.5596(5) 0.43057(13) 0.0364(7) Uani d 1 . .
H H9A 0.123844 -0.450452 0.391478 0.044 Uiso calc 1 . .
H H9B 0.195365 -0.655482 0.419806 0.044 Uiso calc 1 . .
C C10 0.07291(17) -0.7307(5) 0.43757(13) 0.0368(6) Uani d 1 . .
H H10A 0.025185 -0.637168 0.450618 0.044 Uiso calc 1 . .
H H10B 0.096283 -0.847621 0.474588 0.044 Uiso calc 1 . .
C C11 0.03444(17) -0.8679(5) 0.37195(13) 0.0393(7) Uani d 1 . .
H H11A 0.011898 -0.749798 0.335090 0.047 Uiso calc 1 . .
H H11B 0.082584 -0.960448 0.359172 0.047 Uiso calc 1 . .
C C12 -0.03979(17) -1.0408(5) 0.37605(14) 0.0403(7) Uani d 1 . .
H H12A -0.016871 -1.163148 0.411632 0.048 Uiso calc 1 . .
H H12B -0.087282 -0.949827 0.390228 0.048 Uiso calc 1 . .
C C13 -0.0790(2) -1.1686(7) 0.30929(15) 0.0569(9) Uani d 1 . .
H H13A -0.102651 -1.046174 0.273913 0.068 Uiso calc 1 . .
H H13B -0.031228 -1.257274 0.294768 0.068 Uiso calc 1 . .
C C14 -0.1521(2) -1.3442(7) 0.31334(18) 0.0693(11) Uani d 1 . .
H H14A -0.128788 -1.469718 0.347054 0.083 Uiso calc 1 . .
H H14B -0.174872 -1.418856 0.268549 0.083 Uiso calc 1 . .
H H14C -0.200158 -1.257687 0.327044 0.083 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 0.0294(2) 0.0213(3) 0.0228(2) -0.0016(2) 0.00554(18) -0.00261(19)
S1 0.0420(4) 0.0320(4) 0.0256(3) -0.0103(3) 0.0095(3) -0.0052(3)
S2 0.0415(4) 0.0294(4) 0.0287(3) -0.0086(3) 0.0105(3) 0.0004(3)
S3 0.0419(4) 0.0278(4) 0.0300(3) -0.0062(3) 0.0062(3) -0.0026(3)
N1 0.0299(11) 0.0220(12) 0.0270(11) -0.0014(9) 0.0067(9) -0.0013(9)
N2 0.0345(11) 0.0225(12) 0.0265(11) -0.0050(9) 0.0098(9) -0.0008(9)
C1 0.0406(15) 0.0330(17) 0.0324(14) -0.0041(13) 0.0021(12) -0.0101(12)
C2 0.0391(15) 0.0460(19) 0.0297(13) -0.0038(13) 0.0076(13) -0.0126(13)
C3 0.0365(14) 0.0368(17) 0.0265(12) -0.0044(12) 0.0087(12) -0.0051(11)
C4 0.0298(13) 0.0232(14) 0.0278(12) -0.0008(10) 0.0046(11) -0.0025(10)
C5 0.0327(13) 0.0260(15) 0.0298(13) -0.0038(11) 0.0109(11) -0.0015(11)
C6 0.0270(12) 0.0202(14) 0.0285(13) 0.0008(10) 0.0049(11) 0.0037(10)
C7 0.0377(14) 0.0261(15) 0.0306(13) -0.0045(11) 0.0068(12) -0.0009(11)
C8 0.0373(14) 0.0291(15) 0.0347(14) -0.0064(11) 0.0077(12) 0.0019(11)
C9 0.0379(14) 0.0314(17) 0.0398(15) -0.0074(12) 0.0091(13) -0.0027(12)
C10 0.0397(14) 0.0300(16) 0.0421(15) -0.0072(12) 0.0122(13) -0.0020(12)
C11 0.0396(15) 0.0370(18) 0.0405(15) -0.0097(13) 0.0078(13) -0.0037(13)
C12 0.0419(15) 0.0355(18) 0.0430(15) -0.0089(13) 0.0090(13) -0.0027(13)
C13 0.0565(19) 0.060(2) 0.0522(19) -0.0206(17) 0.0084(16) -0.0114(17)
C14 0.063(2) 0.062(3) 0.072(2) -0.0261(19) -0.0053(19) -0.009(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'
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'
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
N1 Ni1 N1 3_666 . 180.0 ?
N1 Ni1 S1 3_666 3_666 85.88(6) ?
N1 Ni1 S1 . 3_666 94.12(6) ?
N1 Ni1 S1 3_666 3_666 85.88(6) ?
N1 Ni1 S1 . 3_666 94.12(6) ?
S1 Ni1 S1 3_666 3_666 0.00(2) ?
N1 Ni1 S1 3_666 . 94.12(6) ?
N1 Ni1 S1 . . 85.88(6) ?
S1 Ni1 S1 3_666 . 180.0 ?
S1 Ni1 S1 3_666 . 180.0 ?
C6 S1 Ni1 . . 96.42(8) ?
C6 S2 C7 . . 100.88(12) ?
C1 S3 C4 . . 91.32(13) ?
C5 N1 N2 . . 111.8(2) ?
C5 N1 Ni1 . . 126.77(17) ?
N2 N1 Ni1 . . 121.46(14) ?
C6 N2 N1 . . 111.74(19) ?
C2 C1 S3 . . 112.9(2) ?
C2 C1 H1 . . 123.6 ?
S3 C1 H1 . . 123.6 ?
C1 C2 C3 . . 112.4(2) ?
C1 C2 H2 . . 123.8 ?
C3 C2 H2 . . 123.8 ?
C4 C3 C2 . . 112.9(2) ?
C4 C3 H3 . . 123.5 ?
C2 C3 H3 . . 123.5 ?
C3 C4 C5 . . 122.6(2) ?
C3 C4 S3 . . 110.53(18) ?
C5 C4 S3 . . 126.78(19) ?
N1 C5 C4 . . 130.1(2) ?
N1 C5 H5 . . 115.0 ?
C4 C5 H5 . . 115.0 ?
N2 C6 S1 . . 124.49(19) ?
N2 C6 S2 . . 119.99(18) ?
S1 C6 S2 . . 115.51(14) ?
C8 C7 S2 . . 111.63(17) ?
C8 C7 H7A . . 109.3 ?
S2 C7 H7A . . 109.3 ?
C8 C7 H7B . . 109.3 ?
S2 C7 H7B . . 109.3 ?
H7A C7 H7B . . 108.0 ?
C9 C8 C7 . . 109.2(2) ?
C9 C8 H8A . . 109.8 ?
C7 C8 H8A . . 109.8 ?
C9 C8 H8B . . 109.8 ?
C7 C8 H8B . . 109.8 ?
H8A C8 H8B . . 108.3 ?
C10 C9 C8 . . 114.7(2) ?
C10 C9 H9A . . 108.6 ?
C8 C9 H9A . . 108.6 ?
C10 C9 H9B . . 108.6 ?
C8 C9 H9B . . 108.6 ?
H9A C9 H9B . . 107.6 ?
C9 C10 C11 . . 112.4(2) ?
C9 C10 H10A . . 109.1 ?
C11 C10 H10A . . 109.1 ?
C9 C10 H10B . . 109.1 ?
C11 C10 H10B . . 109.1 ?
H10A C10 H10B . . 107.9 ?
C12 C11 C10 . . 114.6(2) ?
C12 C11 H11A . . 108.6 ?
C10 C11 H11A . . 108.6 ?
C12 C11 H11B . . 108.6 ?
C10 C11 H11B . . 108.6 ?
H11A C11 H11B . . 107.6 ?
C13 C12 C11 . . 113.4(2) ?
C13 C12 H12A . . 108.9 ?
C11 C12 H12A . . 108.9 ?
C13 C12 H12B . . 108.9 ?
C11 C12 H12B . . 108.9 ?
H12A C12 H12B . . 107.7 ?
C14 C13 C12 . . 113.7(3) ?
C14 C13 H13A . . 108.8 ?
C12 C13 H13A . . 108.8 ?
C14 C13 H13B . . 108.8 ?
C12 C13 H13B . . 108.8 ?
H13A C13 H13B . . 107.7 ?
C13 C14 H14A . . 109.5 ?
C13 C14 H14B . . 109.5 ?
H14A C14 H14B . . 109.5 ?
C13 C14 H14C . . 109.5 ?
H14A C14 H14C . . 109.5 ?
H14B C14 H14C . . 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 3_666 1.9168(19) ?
Ni1 N1 . 1.9168(19) ?
Ni1 S1 3_666 2.1735(7) ?
Ni1 S1 3_666 2.1735(7) ?
Ni1 S1 . 2.1735(7) ?
S1 C6 . 1.717(2) ?
S2 C6 . 1.745(2) ?
S2 C7 . 1.809(2) ?
S3 C1 . 1.709(3) ?
S3 C4 . 1.725(3) ?
N1 C5 . 1.304(3) ?
N1 N2 . 1.404(3) ?
N2 C6 . 1.298(3) ?
C1 C2 . 1.351(4) ?
C1 H1 . 0.9500 ?
C2 C3 . 1.402(4) ?
C2 H2 . 0.9500 ?
C3 C4 . 1.386(3) ?
C3 H3 . 0.9500 ?
C4 C5 . 1.431(3) ?
C5 H5 . 0.9500 ?
C7 C8 . 1.524(3) ?
C7 H7A . 0.9900 ?
C7 H7B . 0.9900 ?
C8 C9 . 1.521(3) ?
C8 H8A . 0.9900 ?
C8 H8B . 0.9900 ?
C9 C10 . 1.519(3) ?
C9 H9A . 0.9900 ?
C9 H9B . 0.9900 ?
C10 C11 . 1.520(3) ?
C10 H10A . 0.9900 ?
C10 H10B . 0.9900 ?
C11 C12 . 1.516(4) ?
C11 H11A . 0.9900 ?
C11 H11B . 0.9900 ?
C12 C13 . 1.515(4) ?
C12 H12A . 0.9900 ?
C12 H12B . 0.9900 ?
C13 C14 . 1.513(4) ?
C13 H13A . 0.9900 ?
C13 H13B . 0.9900 ?
C14 H14A . 0.9800 ?
C14 H14B . 0.9800 ?
C14 H14C . 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
_geom_hbond_publ_flag
C2 H2 S1 4_565 0.95 3.00 3.684(3) 130.5 yes
C2 H2 S2 4 0.95 2.93 3.752(3) 145.6 yes
C5 H5 S1 3_666 0.95 2.42 3.067(3) 125.0 yes
C7 H7A S3 . 0.99 2.93 3.406(3) 110.3 yes
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
C5 N1 N2 C6 . . . . -179.6(2) ?
Ni1 N1 N2 C6 . . . . 0.4(3) ?
C4 S3 C1 C2 . . . . -1.0(2) ?
S3 C1 C2 C3 . . . . 0.9(3) ?
C1 C2 C3 C4 . . . . -0.3(3) ?
C2 C3 C4 C5 . . . . 176.5(2) ?
C2 C3 C4 S3 . . . . -0.5(3) ?
C1 S3 C4 C3 . . . . 0.8(2) ?
C1 S3 C4 C5 . . . . -176.0(2) ?
N2 N1 C5 C4 . . . . -2.1(4) ?
Ni1 N1 C5 C4 . . . . 177.9(2) ?
C3 C4 C5 N1 . . . . 178.5(3) ?
S3 C4 C5 N1 . . . . -5.1(4) ?
N1 N2 C6 S1 . . . . -1.3(3) ?
N1 N2 C6 S2 . . . . 177.52(15) ?
Ni1 S1 C6 N2 . . . . 1.4(2) ?
Ni1 S1 C6 S2 . . . . -177.45(11) ?
C7 S2 C6 N2 . . . . 2.3(2) ?
C7 S2 C6 S1 . . . . -178.84(14) ?
C6 S2 C7 C8 . . . . -177.36(18) ?
S2 C7 C8 C9 . . . . 178.55(18) ?
C7 C8 C9 C10 . . . . -177.8(2) ?
C8 C9 C10 C11 . . . . 176.7(2) ?
C9 C10 C11 C12 . . . . -179.8(2) ?
C10 C11 C12 C13 . . . . 178.0(3) ?
C11 C12 C13 C14 . . . . 179.1(3) ?
_cod_database_fobs_code 2022815