#------------------------------------------------------------------------------
#$Date: 2025-03-28 04:20:15 +0100 (Fri, 28 Mar 2025) $
#$Revision: 298641 $
#$URL: svn://www.crystallography.net/cod/cif/2/02/34/2023458.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_2023458
loop_
_publ_author_name
'Lerch, Timothy G.'
'Albert, Daniel R.'
'Gau, Michael'
'Rajaseelan, Edward'
_publ_section_title
;
Syntheses and crystal structures of 4-benzyl-1-ethyl-1,2,4-triazolium
bromide and its corresponding NHC complexes of rhodium and iridium
;
_journal_coeditor_code HB8128
_journal_issue 4
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_page_first 350
_journal_page_last 357
_journal_paper_doi 10.1107/S2056989025002671
_journal_volume 81
_journal_year 2025
_chemical_formula_iupac 'C11 H14 N3 +, Br -'
_chemical_formula_moiety 'C11 H14 N3 +, Br -'
_chemical_formula_sum 'C11 H14 Br N3'
_chemical_formula_weight 268.16
_chemical_name_systematic
;
4-Benzyl-1-ethyl-1,2,4-triazolium bromide
;
_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
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_cell_angle_alpha 90
_cell_angle_beta 100.400(4)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 19.6908(10)
_cell_length_b 4.7431(2)
_cell_length_c 12.6482(5)
_cell_measurement_reflns_used 7642
_cell_measurement_temperature 100
_cell_measurement_theta_max 28.1790
_cell_measurement_theta_min 2.0890
_cell_volume 1161.88(9)
_computing_cell_refinement
;
CrysAlisPro 1.171.43.142a (Rigaku OD, 2024)
;
_computing_data_collection
;
CrysAlisPro 1.171.43.142a (Rigaku OD, 2024)
;
_computing_data_reduction
;
CrysAlisPro 1.171.43.142a (Rigaku OD, 2024)
;
_computing_molecular_graphics
;
Olex2 1.3 (Dolomanov et al., 2009)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2018/3 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2018/2 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 100.15
_diffrn_detector_area_resol_mean 10.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device '\k-geometry diffractometer'
_diffrn_measurement_device_type 'Rigaku XtaLAB Synergy-S'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0710
_diffrn_reflns_av_unetI/netI 0.0435
_diffrn_reflns_limit_h_max 26
_diffrn_reflns_limit_h_min -26
_diffrn_reflns_limit_k_max 6
_diffrn_reflns_limit_k_min -5
_diffrn_reflns_limit_l_max 16
_diffrn_reflns_limit_l_min -16
_diffrn_reflns_number 22182
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 28.282
_diffrn_reflns_theta_min 2.103
_exptl_absorpt_coefficient_mu 3.510
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.64082
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(SCALE3 ABSPACK; Rigaku OD, 2024)
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.533
_exptl_crystal_description plate
_exptl_crystal_F_000 544
_exptl_crystal_size_max 0.38
_exptl_crystal_size_mid 0.19
_exptl_crystal_size_min 0.02
_refine_diff_density_max 1.396
_refine_diff_density_min -0.576
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.053
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 137
_refine_ls_number_reflns 2883
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.053
_refine_ls_R_factor_all 0.0535
_refine_ls_R_factor_gt 0.0383
_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^)+(0.0242P)^2^+1.9068P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0697
_refine_ls_wR_factor_ref 0.0738
_reflns_number_gt 2356
_reflns_number_total 2883
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file hb8128.cif
_cod_data_source_block 2
_cod_database_code 2023458
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_hkl_file
;
0 0 2 159.78 9.29
0 0 2 171.27 10.78
0 0 -2 165.40 11.01
0 0 -2 205.18 10.86
0 0 2 170.23 10.58
0 0 3 2.18 4.42
0 0 -3 -3.96 6.71
0 0 3 5.68 6.04
0 0 -4 3702.55 175.20
0 0 4 3848.17 175.24
0 0 -4 3970.79 178.18
0 0 4 4070.33 177.37
0 0 5 -3.17 9.00
0 0 -5 0.98 7.31
0 0 5 5.27 6.72
0 0 -5 6.57 9.92
0 0 6 3399.17 154.11
0 0 -6 3235.90 154.45
0 0 -6 3489.54 158.72
0 0 6 3323.58 157.00
0 0 -6 3415.69 157.27
0 0 -7 -3.92 13.76
0 0 7 1.78 8.80
0 0 -7 -4.83 9.52
0 0 -7 5.56 13.53
0 0 7 -1.11 12.23
0 0 -8 431.32 27.55
0 0 -8 485.44 34.40
0 0 8 497.76 27.56
0 0 8 410.24 30.93
0 0 -8 490.07 32.60
0 0 8 441.78 31.43
0 0 -9 -10.16 18.34
0 0 9 -10.56 16.09
0 0 -9 -15.01 19.60
0 0 9 9.51 12.27
0 0 -9 -22.36 13.25
0 0 9 1.43 16.91
0 0 10 924.00 54.49
0 0 -10 946.26 58.43
0 0 -10 923.98 54.79
0 0 -10 872.13 56.02
0 0 10 932.29 48.45
0 0 10 803.31 53.61
0 0 -11 -9.03 26.10
0 0 11 8.71 16.31
0 0 11 7.54 20.73
0 0 -11 -8.20 27.26
0 0 11 -15.80 22.35
0 0 -11 12.60 23.89
0 0 -12 298.70 37.13
0 0 12 238.92 33.36
0 0 12 320.68 34.92
0 0 -12 322.61 35.45
0 0 13 45.31 26.12
0 0 13 24.74 26.73
0 0 -13 63.81 29.97
0 0 14 435.60 44.45
0 0 14 398.82 42.64
0 0 -14 467.41 44.82
0 0 15 2.62 32.18
0 0 15 16.62 32.62
0 0 16 1012.33 73.81
0 0 16 1117.51 74.03
0 -1 0 -2.10 4.51
0 -1 0 1.62 4.24
0 -1 0 0.72 3.54
0 1 1 74.55 8.49
0 -1 -1 75.91 8.76
0 -1 1 84.08 5.65
0 -1 -1 72.35 7.99
0 -1 -1 88.33 8.49
0 -1 -1 81.58 5.78
0 -1 1 69.98 6.90
0 -1 -2 3827.91 171.00
0 1 -2 3752.51 169.53
0 -1 2 3790.64 169.21
0 -1 -2 3708.67 171.78
0 -1 -2 3714.39 170.39
0 1 2 3654.49 171.95
0 -1 -2 3774.04 171.94
0 1 -3 8734.03 380.98
0 -1 -3 7744.35 383.65
0 1 3 8870.15 384.38
0 1 -3 6944.87 382.54
0 -1 3 8922.08 381.87
0 -1 -3 8562.18 384.39
0 1 3 8700.67 384.74
0 -1 3 8878.59 380.73
0 1 -3 8151.99 383.30
0 -1 -3 8636.42 383.28
0 1 -3 8476.96 382.03
0 -1 4 21.20 6.25
0 1 4 31.11 10.04
0 -1 4 17.09 6.14
0 1 -4 17.37 7.52
0 -1 -4 16.97 9.76
0 1 -4 20.64 6.50
0 1 4 25.40 8.98
0 1 -4 27.63 10.03
0 -1 -4 20.66 8.48
0 1 -5 564.84 30.64
0 -1 5 499.17 27.90
0 -1 5 489.15 26.83
0 1 -5 518.40 27.80
0 -1 -5 507.79 30.93
0 1 5 464.94 30.54
0 -1 -5 517.90 29.88
0 1 -5 576.73 31.20
0 -1 -5 511.52 30.12
0 1 -5 474.17 24.07
0 1 5 595.60 30.41
0 -1 -6 272.74 21.12
0 1 6 339.75 21.85
0 1 -6 254.98 14.85
0 1 -6 273.70 22.10
0 1 -6 309.63 20.02
0 -1 -6 318.84 24.07
0 1 6 294.36 23.30
0 -1 6 284.22 18.90
0 -1 -6 281.62 22.50
0 1 -6 333.18 23.48
0 -1 6 251.27 19.60
0 -1 -7 1488.69 75.02
0 1 7 1610.15 75.58
0 1 -7 1393.25 69.16
0 1 -7 1636.11 78.13
0 1 -7 1514.77 74.25
0 -1 7 1462.93 73.07
0 1 7 1487.52 77.44
0 -1 -7 1565.24 77.00
0 1 -7 1543.09 77.47
0 -1 7 1596.71 75.39
0 1 -8 607.79 34.05
0 -1 -8 648.93 40.41
0 1 8 759.17 41.54
0 1 -8 778.32 45.09
0 1 -8 749.76 40.90
0 -1 8 721.57 39.45
0 1 8 748.62 44.06
0 1 -8 698.48 43.75
0 -1 -8 724.34 43.48
0 -1 8 736.87 42.01
0 -1 -9 1178.22 67.11
0 1 9 1327.81 67.91
0 1 -9 1311.13 72.25
0 1 -9 1286.96 67.88
0 1 9 1374.46 71.71
0 -1 9 1281.40 66.77
0 -1 -9 1260.48 70.25
0 1 -9 1305.02 70.98
0 -1 9 1231.45 68.50
0 -1 10 3.14 18.59
0 1 -10 30.37 22.77
0 1 10 -7.46 21.70
0 -1 10 13.81 17.54
0 1 -10 15.17 19.79
0 -1 -10 -7.39 23.10
0 -1 -10 5.42 22.04
0 1 -10 -15.07 23.75
0 1 10 6.39 18.30
0 -1 11 36.87 21.42
0 1 -11 51.25 24.81
0 -1 11 82.50 21.30
0 1 11 95.36 27.24
0 -1 -11 73.07 25.51
0 1 -11 44.72 23.01
0 1 11 56.42 23.91
0 -1 -11 59.91 23.97
0 1 -11 45.58 25.18
0 1 11 36.13 20.95
0 -1 12 83.55 26.22
0 1 12 83.19 28.38
0 -1 12 74.54 24.16
0 1 -12 68.68 29.76
0 -1 -12 47.47 31.39
0 -1 -12 108.23 30.72
0 1 -12 77.99 25.91
0 1 12 84.89 23.89
0 1 -12 92.53 31.02
0 -1 -12 100.05 28.73
0 1 12 77.27 26.65
0 -1 -13 801.75 58.07
0 1 -13 774.14 53.38
0 1 -13 709.10 58.63
0 -1 -13 787.40 59.85
0 1 13 835.27 57.45
0 1 13 805.76 57.37
0 -1 13 746.08 51.58
0 -1 13 734.35 54.46
0 1 13 808.01 50.99
0 1 14 268.93 32.97
0 1 14 308.40 40.63
0 -1 14 246.63 34.42
0 1 14 243.74 38.14
0 1 -14 332.37 39.12
0 -1 -14 312.01 44.25
0 1 -14 330.05 44.20
0 -1 14 323.15 38.22
0 -1 -15 100.84 40.22
0 1 -15 136.68 39.81
0 1 -15 207.90 39.53
0 1 15 126.82 39.23
0 -1 15 136.25 33.43
0 -1 15 110.18 37.31
0 1 15 161.44 38.05
0 -1 16 39.06 35.76
0 1 16 17.77 38.63
0 1 16 58.96 39.26
0 1 -16 46.53 39.52
0 -1 -16 26.91 42.60
0 2 0 444.12 25.11
0 -2 0 457.97 24.13
0 -2 0 412.01 23.11
0 2 0 407.54 23.28
0 -2 0 444.14 23.45
0 2 0 432.16 26.42
0 -2 -1 3899.91 166.83
0 2 1 3589.25 167.17
0 -2 -1 3537.81 169.97
0 2 -1 3581.67 170.63
0 2 -1 3858.65 169.98
0 2 1 3736.59 170.77
0 -2 -1 3887.36 169.86
0 2 -1 3593.69 167.41
0 2 1 3301.23 169.84
0 2 -1 3705.24 167.21
0 -2 1 3533.77 169.57
0 2 -1 3892.24 167.70
0 2 -2 127.06 9.72
0 -2 -2 119.05 9.59
0 -2 -2 123.95 7.87
0 2 -2 147.51 8.88
0 2 -2 149.44 13.19
0 2 2 158.05 13.46
0 -2 -2 116.36 14.14
0 -2 -2 124.66 14.21
0 2 -2 131.89 8.85
0 2 -2 141.85 12.55
0 2 2 115.39 13.55
0 2 -2 124.28 12.16
0 2 -3 85.86 11.93
0 -2 3 101.12 8.37
0 -2 -3 108.49 14.06
0 -2 -3 87.45 14.13
0 2 -3 73.40 8.41
0 2 -3 83.13 10.32
0 -2 -3 93.42 10.51
0 2 -3 101.26 9.19
0 2 3 94.66 14.38
0 -2 -3 84.31 14.97
0 2 -3 86.38 10.50
0 2 3 103.53 14.04
0 -2 -4 81.06 11.17
0 -2 4 83.76 8.02
0 2 -4 78.02 13.19
0 -2 -4 72.28 13.91
0 2 -4 85.69 10.37
0 -2 -4 52.48 14.11
0 2 -4 48.34 8.62
0 2 -4 79.05 11.68
0 -2 -4 81.39 15.59
0 2 -4 75.38 9.20
0 2 4 77.40 15.35
0 2 -5 4486.97 206.19
0 -2 -5 4627.20 207.88
0 2 -5 4660.06 209.02
0 -2 5 4576.10 203.85
0 -2 -5 4588.10 209.45
0 2 -5 4053.56 202.34
0 2 5 4829.90 210.15
0 -2 -5 4760.70 206.98
0 2 -5 4710.89 207.45
0 2 -6 1216.59 55.48
0 -2 -6 1063.41 56.18
0 -2 6 1141.86 52.04
0 2 -6 1135.47 57.93
0 -2 -6 1161.01 58.47
0 2 6 1192.77 58.21
0 -2 -6 1121.69 55.11
0 2 -6 1207.59 56.45
0 -2 -7 58.37 17.82
0 2 7 81.26 18.76
0 2 -7 82.21 16.31
0 -2 7 56.61 13.04
0 -2 -7 57.03 19.47
0 2 -7 80.57 12.61
0 -2 7 76.40 9.97
0 2 -7 61.41 17.33
0 -2 -7 85.68 16.45
0 -2 -8 25.30 18.98
0 2 8 4.62 17.94
0 2 -8 31.95 18.41
0 -2 -8 16.56 17.28
0 2 -8 24.04 19.15
0 -2 -8 40.99 21.51
0 2 -8 24.99 13.08
0 -2 8 14.57 10.56
0 2 8 14.48 20.89
0 -2 8 33.00 15.18
0 -2 -9 199.29 25.04
0 2 -9 195.80 26.29
0 2 -9 228.26 20.92
0 2 9 136.50 25.19
0 2 -9 225.15 26.83
0 2 9 161.35 27.11
0 -2 9 173.35 17.53
0 -2 -9 265.42 30.70
0 -2 9 198.34 22.30
0 2 -10 667.86 40.10
0 -2 -10 725.84 49.44
0 -2 10 642.26 41.91
0 2 10 639.19 47.50
0 -2 10 592.16 36.91
0 2 -10 705.73 47.26
0 2 -10 611.60 45.71
0 -2 -10 601.85 44.01
0 2 10 672.36 45.73
0 2 -11 1370.23 70.23
0 2 -11 1373.05 78.11
0 2 -11 1300.67 76.77
0 -2 -11 1288.68 75.27
0 -2 11 1274.54 67.33
0 2 11 1397.22 78.78
0 2 11 1296.23 74.89
0 -2 11 1265.27 72.36
0 -2 12 51.83 24.88
0 2 12 122.11 30.10
0 2 -12 85.76 29.87
0 -2 -12 50.10 30.55
0 -2 -12 71.13 27.89
0 2 -12 122.26 25.18
0 2 12 181.70 32.41
0 -2 12 76.08 20.43
0 2 -12 97.68 30.78
0 2 12 55.73 29.56
0 -2 13 34.14 27.10
0 -2 13 -10.91 22.32
0 2 13 10.46 32.12
0 2 13 -7.85 31.51
0 2 13 19.42 30.07
0 -2 -13 19.32 35.15
0 2 -13 83.79 34.82
0 -2 14 107.10 32.50
0 2 14 157.20 38.76
0 2 14 216.73 38.69
0 2 14 161.49 35.16
0 -2 -14 209.50 41.29
0 2 -14 246.63 41.49
0 -2 15 379.41 45.19
0 2 15 417.84 49.96
0 2 -15 460.55 52.55
0 -2 -15 433.01 53.43
0 2 15 473.43 45.65
0 2 15 481.23 51.37
0 -3 0 -3.70 10.61
0 3 0 -23.66 15.09
0 -3 0 3.89 12.00
0 3 0 -1.12 14.47
0 -3 0 2.94 9.24
0 3 0 -3.34 9.88
0 3 -1 28.07 8.17
0 -3 1 15.70 10.23
0 -3 -1 13.09 9.67
0 3 1 30.49 14.24
0 3 -1 24.09 13.49
0 -3 -1 40.96 12.99
0 3 -1 23.51 6.02
0 -3 -1 29.43 5.87
0 3 1 17.18 11.90
0 3 -1 28.17 8.32
0 -3 -1 44.10 13.12
0 3 1 26.78 15.10
0 3 -1 34.43 14.49
0 3 -2 3098.62 146.79
0 -3 -2 3155.27 146.44
0 3 -2 3240.62 146.52
0 -3 -2 3173.27 145.86
0 3 2 3224.98 147.06
0 3 -2 3025.39 141.46
0 3 2 3049.93 146.91
0 3 -2 3078.31 141.72
0 3 -3 8.45 12.71
0 -3 -3 -12.80 15.31
0 3 -3 -9.06 13.12
0 -3 -3 -4.56 15.05
0 3 -3 -1.18 7.12
0 3 -3 -6.88 7.51
0 -3 -3 -0.44 7.89
0 3 -3 -3.14 7.02
0 3 3 15.88 15.18
0 3 -3 -0.63 9.86
0 3 -4 865.85 46.10
0 -3 -4 977.60 47.88
0 3 -4 989.99 47.85
0 -3 -4 988.11 54.23
0 -3 -4 946.05 45.49
0 3 -4 941.32 46.38
0 -3 -4 827.41 53.00
0 3 -4 968.03 52.91
0 3 4 898.12 53.44
0 3 -4 982.37 50.33
0 3 -4 1025.63 52.58
0 3 4 1028.54 56.89
0 3 -4 958.71 49.53
0 3 -5 150.81 16.49
0 -3 -5 135.20 15.89
0 3 5 151.98 23.06
0 3 -5 115.48 14.51
0 3 -5 140.04 13.73
0 -3 -5 145.13 22.69
0 -3 -5 98.75 22.19
0 3 -5 145.75 20.02
0 3 5 151.73 22.61
0 -3 6 151.29 14.81
0 3 -6 126.97 17.71
0 -3 -6 143.68 18.18
0 3 6 85.33 22.00
0 3 -6 123.70 13.98
0 3 -6 153.55 16.43
0 -3 -6 115.69 23.63
0 -3 -6 144.54 24.27
0 3 -6 167.53 21.33
0 3 6 167.25 24.25
0 -3 7 102.98 14.87
0 3 -7 90.12 18.78
0 -3 -7 115.27 19.22
0 3 7 110.12 24.90
0 3 -7 92.48 10.68
0 3 -7 130.56 18.14
0 -3 -7 103.98 24.70
0 -3 -7 83.14 23.99
0 3 7 143.49 26.39
0 3 -7 125.74 22.13
0 -3 -8 2541.55 122.72
0 3 -8 2459.11 122.82
0 -3 -8 2435.62 126.59
0 3 -8 2496.23 121.54
0 -3 -8 2490.93 125.24
0 3 8 2572.36 128.24
0 -3 8 2438.46 118.18
0 3 -8 2471.47 125.82
0 3 8 2595.75 127.47
0 -3 9 -16.71 17.93
0 3 -9 -6.41 21.75
0 -3 -9 41.23 21.61
0 3 9 28.39 25.20
0 3 -9 23.49 19.56
0 -3 -9 14.64 26.63
0 -3 -9 1.80 25.79
0 3 -9 34.50 24.38
0 3 9 -15.83 28.92
0 3 -10 -14.40 24.65
0 -3 -10 28.69 24.08
0 3 10 52.53 29.17
0 3 -10 -1.69 23.30
0 -3 -10 -2.02 24.91
0 -3 -10 42.98 29.86
0 -3 -10 34.03 31.20
0 -3 10 21.72 19.33
0 3 -10 -2.24 26.15
0 -3 -11 40.72 25.27
0 -3 -11 51.06 33.82
0 -3 -11 13.52 29.41
0 3 -11 30.64 27.45
0 3 -11 1.98 26.91
0 3 11 -41.61 30.41
0 -3 11 26.08 21.75
0 -3 -12 570.71 52.53
0 3 -12 687.26 51.22
0 3 12 650.36 52.12
0 3 -12 620.47 50.84
0 -3 12 595.39 44.66
0 3 13 -29.24 38.45
0 3 13 -26.06 33.93
0 3 13 28.11 34.80
0 3 -13 21.26 30.95
0 -3 -13 56.14 34.83
0 3 14 520.71 54.51
0 3 14 486.61 53.75
0 3 14 474.99 50.56
0 3 -14 500.23 50.86
0 -3 -14 511.70 52.33
0 4 0 1008.18 56.55
0 4 0 899.62 49.06
0 4 0 924.08 56.26
0 4 1 442.77 34.48
0 -4 -1 446.94 31.18
0 4 1 442.81 30.26
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-10 1 -2 832.65 44.19
10 -1 2 891.16 48.07
10 1 2 804.52 46.66
-10 -1 -2 855.84 45.96
10 -1 2 809.68 44.08
-10 -1 -2 864.52 47.87
-10 -1 -3 30.34 15.05
-10 1 -3 1.08 13.27
10 -1 3 30.19 14.04
-10 -1 -3 9.34 16.03
-10 -1 -3 29.00 16.71
-10 1 -3 26.45 13.23
10 -1 3 53.80 17.04
10 1 3 23.46 14.90
-10 -1 -3 48.27 13.29
-10 1 -4 90.19 18.37
-10 -1 -4 134.76 20.99
-10 1 -4 78.84 17.95
10 -1 4 107.08 17.78
-10 -1 -4 99.58 17.83
-10 -1 -4 124.46 17.13
10 1 4 138.22 20.24
10 -1 4 134.23 21.18
-10 1 -5 1574.35 85.75
-10 -1 -5 1706.78 87.06
10 -1 5 1609.47 86.40
-10 -1 -5 1712.53 84.99
-10 -1 -5 1800.07 88.65
-10 1 -5 1752.87 86.46
-10 1 -6 619.20 41.36
-10 -1 -6 607.91 38.59
-10 -1 -6 585.83 40.73
-10 1 -6 592.08 40.38
-10 -1 -6 593.93 40.47
10 -1 6 561.01 40.27
-10 1 -6 624.74 40.05
-10 1 -7 452.72 38.08
-10 -1 -7 588.54 36.82
-10 -1 -7 509.60 37.80
-10 1 -7 422.34 34.78
-10 1 -7 486.86 37.97
-10 -1 -7 517.52 38.26
10 -1 7 462.31 37.69
-10 1 -7 483.20 37.01
-10 1 -8 19.78 21.45
-10 -1 -8 18.55 22.71
-10 1 -8 49.69 22.96
10 -1 8 33.38 22.86
-10 1 -8 11.53 20.13
-10 -1 -8 30.02 22.43
-10 1 -8 -19.66 24.24
-10 -1 -8 9.29 19.65
-10 1 -9 287.95 32.73
-10 -1 -9 283.31 32.72
-10 -1 -9 350.48 37.55
-10 1 -9 220.66 31.62
10 -1 9 232.96 33.59
-10 -1 -9 257.38 31.97
-10 1 -9 232.81 28.72
-10 1 -9 292.19 34.76
-10 -1 -9 285.00 31.08
-10 1 -10 161.34 31.76
-10 -1 -10 141.41 29.24
-10 1 -10 77.91 24.91
10 -1 10 116.33 31.16
-10 -1 -10 90.15 33.08
-10 1 -10 107.30 28.76
-10 1 -10 134.46 31.20
-10 -1 -10 111.44 27.11
-10 1 -11 571.28 48.75
-10 -1 -11 500.07 46.75
-10 1 -11 559.68 43.91
10 -1 11 700.58 53.68
-10 1 -11 716.60 52.99
-10 -1 -11 603.14 47.44
-10 1 -12 -1.63 27.10
-10 1 -12 38.01 35.46
-10 -1 -12 24.40 32.18
10 -1 12 -37.68 36.03
-10 1 -13 21.91 38.65
-10 -1 -13 -50.51 34.53
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-10 -2 15 11.92 35.25
10 -2 -15 13.30 35.63
10 2 -15 5.65 37.96
-10 2 15 53.33 43.02
10 2 -14 132.95 37.05
10 -2 -14 91.95 35.40
-10 2 14 124.12 41.04
-10 2 14 88.88 34.05
-10 2 14 80.48 33.24
-10 -2 14 48.57 32.76
10 2 -13 942.10 62.75
10 -2 -13 804.26 61.78
-10 2 13 912.89 68.05
-10 -2 13 843.06 57.81
-10 2 13 830.13 60.45
-10 2 13 927.47 62.09
-10 -2 13 860.69 58.75
10 2 -12 10.68 26.78
10 -2 -12 28.94 29.37
10 2 -12 2.20 27.60
10 -2 -12 17.06 27.11
10 -2 -12 46.69 29.60
-10 2 12 24.97 26.43
-10 -2 12 77.88 25.24
-10 2 12 12.99 28.70
-10 2 12 19.73 34.40
-10 -2 12 1.66 25.30
10 2 -11 118.69 27.70
10 -2 -11 114.81 30.44
10 -2 -11 92.08 28.53
10 2 -11 136.80 28.75
-10 -2 11 139.94 26.11
-10 2 11 49.97 34.38
-10 2 11 97.04 26.25
-10 -2 11 95.42 25.79
-10 2 11 61.22 28.84
10 -2 -10 15.64 24.83
10 2 -10 -5.53 22.96
-10 -2 10 8.25 24.94
10 -2 -10 5.35 22.98
-10 2 10 -4.89 28.75
-10 -2 10 -9.78 20.50
-10 2 10 -31.19 22.36
-10 -2 10 10.93 21.05
10 2 -10 -7.29 21.41
-10 2 10 -17.90 26.06
-10 2 9 673.48 50.78
10 -2 -9 789.26 46.95
-10 -2 9 695.42 42.90
10 -2 -9 704.13 45.67
10 2 -9 730.24 46.21
-10 -2 9 822.99 48.54
-10 2 9 767.24 46.93
-10 -2 9 737.12 44.21
10 2 -9 691.88 45.13
-10 2 9 808.44 49.74
-10 -2 8 -13.10 20.94
10 2 -8 50.52 25.24
10 -2 -8 66.59 21.62
10 2 -8 25.99 20.56
10 2 -8 45.53 19.41
10 -2 -8 31.54 18.81
-10 -2 8 33.08 20.70
-10 -2 8 36.71 17.11
-10 2 8 16.75 24.98
-10 -2 8 55.75 18.30
10 2 -8 12.08 18.64
-10 2 8 77.40 20.75
-10 -2 8 28.58 13.62
-10 -2 7 1467.07 70.44
10 -2 -7 1536.72 75.64
-10 -2 7 1447.88 76.97
10 2 -7 1538.80 78.98
-10 2 7 1456.42 76.46
10 2 -7 1412.92 76.65
10 -2 -7 1487.86 75.73
-10 2 7 1389.44 75.79
-10 -2 7 1431.27 78.04
-10 -2 7 1378.22 74.34
10 2 -7 1333.29 74.94
10 2 -7 1374.11 75.23
-10 -2 6 307.87 22.22
10 -2 -6 327.85 25.68
10 2 -6 259.24 25.66
10 -2 -6 278.36 24.45
-10 -2 6 261.73 25.98
-10 2 6 289.84 25.44
10 2 -6 319.34 29.49
-10 -2 6 269.37 26.09
-10 -2 6 255.08 24.50
-10 2 6 298.20 24.87
10 2 -6 288.13 25.68
10 2 -6 274.00 25.54
10 2 -5 16.26 14.81
10 -2 -5 12.74 15.11
10 2 -5 26.13 15.26
10 -2 -5 5.16 13.77
-10 -2 5 -1.23 15.06
-10 2 5 36.96 14.82
-10 -2 5 27.00 13.55
10 2 -5 2.85 18.59
-10 -2 5 22.53 15.58
10 2 -5 3.66 15.26
-10 2 5 14.18 13.58
-10 -2 5 16.70 13.43
10 2 -4 436.05 30.32
10 -2 -4 446.88 27.46
-10 -2 4 432.48 29.42
-10 2 4 431.01 27.44
10 2 -4 494.71 31.89
10 -2 -4 373.54 20.13
10 -2 -4 467.47 27.89
10 2 -4 465.79 30.07
-10 2 4 323.13 20.74
-10 2 4 418.56 26.83
-10 -2 4 488.32 31.10
-10 -2 4 377.96 26.47
10 2 -4 430.31 27.54
10 -2 -4 416.97 28.02
10 2 -3 1182.80 59.20
10 -2 -3 1129.80 60.34
10 2 -3 1146.69 63.04
10 -2 -3 1221.48 59.81
-10 2 3 1151.93 59.09
-10 -2 3 1189.15 61.93
10 2 -3 1232.39 63.98
10 -2 -3 1122.31 58.95
10 2 -3 1026.32 61.31
-10 2 3 1197.54 58.70
-10 2 3 1162.83 61.66
-10 -2 3 1164.02 59.33
10 -2 -2 923.09 52.64
-10 -2 2 1041.35 55.44
10 2 -2 1010.41 57.49
-10 2 2 1032.77 52.18
10 2 -2 1156.87 58.45
-10 -2 2 1061.03 57.63
10 -2 -2 1014.89 51.50
-10 2 2 1062.46 55.43
10 -2 -2 1009.70 54.11
10 2 -2 977.12 52.37
-10 -2 2 984.08 53.21
10 2 -2 974.54 56.02
-10 2 2 1015.51 50.98
-10 2 1 509.32 29.15
10 -2 -1 555.70 29.91
10 -2 -1 531.13 33.75
-10 2 1 512.46 34.13
10 2 -1 567.53 32.27
10 -2 -1 526.14 32.26
10 2 -1 530.08 34.79
-10 -2 1 492.92 34.53
-10 2 1 538.58 31.55
10 2 -1 539.95 37.47
-10 -2 1 538.09 37.17
-10 -2 1 544.37 33.63
-10 -2 1 569.14 33.72
-10 -2 1 582.23 33.00
-10 -2 0 134.28 18.04
10 2 0 145.48 21.43
-10 -2 0 147.05 21.90
10 -2 0 122.79 11.93
10 -2 0 66.70 14.14
10 2 0 104.82 17.81
-10 2 0 99.48 14.44
-10 -2 0 177.27 20.24
-10 -2 0 103.57 15.41
-10 2 0 145.33 17.76
10 2 0 100.91 15.08
10 -2 0 101.41 17.25
-10 -2 0 79.69 17.21
10 2 1 273.84 26.04
10 -2 1 361.56 24.51
-10 -2 -1 290.53 25.98
10 2 1 360.64 31.63
-10 2 -1 349.18 19.36
-10 -2 -1 388.52 30.39
-10 -2 -1 399.95 29.13
-10 2 -1 350.98 24.26
-10 -2 -1 353.59 27.19
10 -2 1 336.09 20.40
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10 -2 1 360.75 27.36
10 2 1 271.50 23.73
-10 -2 -1 373.51 24.79
10 -2 2 572.62 35.32
10 2 2 653.94 38.73
-10 2 -2 595.97 35.91
-10 -2 -2 592.42 39.11
-10 -2 -2 617.46 38.38
-10 2 -2 570.05 31.70
-10 -2 -2 663.26 42.33
10 2 2 561.87 41.15
-10 -2 -2 635.11 39.06
10 2 2 626.74 36.47
-10 -2 -2 610.18 35.20
-10 2 -2 584.43 37.03
10 -2 2 636.96 38.75
10 -2 2 535.06 30.96
10 -2 3 1373.30 73.07
10 2 3 1451.39 76.30
-10 -2 -3 1489.28 77.20
-10 2 -3 1385.49 73.44
-10 -2 -3 1475.99 76.56
-10 -2 -3 1476.38 78.57
10 2 3 1398.38 79.35
10 -2 3 1494.94 76.35
10 2 3 1532.89 74.28
-10 2 -3 1464.58 74.92
-10 -2 -3 1336.44 72.22
-10 -2 -3 1700.39 77.81
10 -2 3 1397.39 68.87
-10 -2 -4 449.35 33.04
-10 -2 -4 466.51 33.91
-10 -2 -4 323.81 33.82
-10 2 -4 420.56 30.32
-10 -2 -4 407.58 27.71
10 -2 4 343.86 22.62
-10 2 -4 329.08 27.55
-10 -2 -4 362.87 30.16
10 -2 4 384.26 28.83
10 2 4 372.10 30.99
10 -2 5 35.44 17.15
-10 2 -5 10.85 17.21
-10 -2 -5 -2.77 17.94
10 2 5 46.22 20.41
-10 -2 -5 11.07 25.03
-10 -2 -5 23.71 15.53
-10 2 -5 14.49 18.30
-10 2 -5 31.32 17.58
-10 -2 -5 80.47 22.99
10 2 6 16.99 21.04
10 -2 6 34.01 18.15
-10 -2 -6 18.66 23.35
-10 2 -6 10.87 17.47
-10 -2 -6 25.54 19.93
-10 2 -6 14.78 18.92
-10 -2 -6 32.11 17.77
-10 2 -6 28.58 21.13
-10 -2 -6 35.74 28.47
-10 2 -7 1006.14 58.11
-10 -2 -7 1111.74 65.28
-10 -2 -7 1126.20 67.87
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10 -2 7 1002.39 61.52
10 2 7 1008.38 63.52
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-10 -2 -7 1113.07 58.73
-10 -2 -7 921.65 61.79
10 -2 8 117.45 27.57
10 2 8 109.34 27.91
-10 -2 -8 152.44 31.90
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10 2 8 114.55 27.91
-10 -2 -8 143.80 28.78
-10 -2 -8 157.47 27.72
-10 2 -8 132.61 27.48
-10 -2 -8 123.37 36.16
-10 -2 -8 143.05 24.81
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-10 -2 -9 753.84 46.07
10 2 9 643.96 48.98
-10 -2 -9 669.03 49.24
-10 2 -9 575.10 42.54
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-10 -2 -9 648.24 48.59
10 -2 9 590.00 48.61
10 2 9 648.59 50.81
-10 2 -9 573.00 43.67
-10 2 -10 48.14 28.27
-10 2 -10 20.98 23.91
10 2 10 32.89 31.52
10 -2 10 -7.24 30.96
-10 2 -10 16.72 25.41
10 2 10 21.76 30.15
-10 2 -10 -4.45 30.16
-10 -2 -10 -25.87 25.65
-10 2 -11 71.45 26.44
10 2 11 87.11 36.32
-10 2 -11 159.21 36.22
-10 -2 -11 108.61 29.37
10 2 11 63.02 32.92
-10 2 -11 91.46 29.36
10 2 12 58.81 39.55
10 2 12 84.59 36.44
-10 2 -12 72.80 37.33
-10 -2 -12 66.80 31.12
10 2 13 256.01 49.56
10 2 13 426.40 49.48
-10 2 -13 355.18 49.70
-10 -2 -13 320.66 42.40
10 3 -14 15.08 36.14
10 -3 -14 64.94 36.11
-10 3 14 170.76 48.98
-10 -3 14 113.63 37.65
-10 3 14 60.75 37.35
-10 3 14 114.45 41.61
10 3 -13 25.56 32.26
10 -3 -13 31.33 31.63
10 3 -13 -2.75 43.04
-10 3 13 79.80 44.76
-10 3 13 18.12 33.10
-10 -3 13 4.17 31.48
-10 3 13 5.41 36.26
10 3 -12 68.79 30.88
10 -3 -12 89.05 31.11
10 -3 -12 71.65 31.96
-10 3 12 69.32 35.57
-10 3 12 138.28 34.69
-10 -3 12 58.51 29.61
10 3 -12 90.17 43.73
10 3 -11 53.87 27.05
10 -3 -11 20.38 26.80
10 -3 -11 73.33 28.27
10 3 -11 55.62 27.25
10 -3 -11 43.74 27.81
10 3 -11 7.25 39.20
-10 3 11 31.58 29.05
-10 -3 11 21.90 27.35
-10 3 11 13.09 31.49
-10 -3 10 853.76 53.02
-10 3 10 820.17 54.43
10 3 -10 747.78 51.81
10 -3 -10 696.40 51.88
10 3 -10 708.97 52.02
10 -3 -10 758.88 52.26
10 3 -10 809.71 60.05
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10 -3 -10 820.26 52.07
10 3 -9 25.33 23.22
-10 3 9 3.82 24.03
-10 -3 9 55.02 23.17
10 -3 -9 30.96 22.96
10 -3 -9 -13.18 23.14
10 3 -9 71.78 25.50
10 -3 -9 4.67 21.81
10 3 -9 11.96 21.86
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-10 3 9 19.12 29.65
-10 3 9 43.34 31.37
-10 -3 9 -7.75 17.83
-10 -3 8 146.39 26.97
10 -3 -8 111.14 22.43
-10 3 8 206.18 33.55
-10 -3 8 108.62 18.71
10 3 -8 125.46 24.67
10 -3 -8 109.28 24.00
10 -3 -8 100.07 22.31
10 3 -8 96.06 24.29
-10 -3 8 132.27 26.23
-10 3 8 148.75 32.12
-10 3 8 160.17 26.04
-10 -3 8 109.92 24.30
10 3 -8 111.63 23.40
-10 -3 7 20.58 22.57
10 -3 -7 10.39 18.58
10 3 -7 4.07 19.40
10 -3 -7 3.67 19.16
10 3 -7 1.52 19.66
10 -3 -7 12.31 18.02
-10 -3 7 7.86 19.58
-10 -3 7 25.07 15.43
-10 3 7 -18.35 20.37
10 3 -7 27.45 19.04
-10 3 7 2.20 26.49
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10 -3 -6 1225.76 63.99
10 3 -6 1211.09 66.75
10 -3 -6 1173.55 62.98
-10 -3 6 1119.71 65.23
10 -3 -6 1254.58 58.99
-10 3 6 1252.17 64.95
-10 -3 6 1135.61 68.51
10 3 -6 1155.46 64.79
10 3 -6 1192.44 64.06
-10 3 6 1150.48 70.43
-10 -3 5 10.01 14.32
10 -3 -5 12.29 17.26
10 3 -5 5.19 16.11
10 -3 -5 9.55 14.51
10 3 -5 5.98 18.83
-10 -3 5 1.31 17.22
-10 -3 5 8.68 18.52
-10 3 5 29.47 21.74
-10 3 5 8.96 15.68
10 3 -5 17.00 17.01
-10 -3 5 37.64 18.75
-10 -3 4 1496.87 73.36
10 3 -4 1408.40 70.15
10 -3 -4 1406.68 72.07
10 3 -4 1265.96 74.78
10 -3 -4 1373.39 69.74
-10 -3 4 1395.68 73.19
-10 3 4 1425.30 70.63
-10 -3 4 1317.25 69.13
-10 -3 4 1447.23 76.44
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10 3 -4 1305.15 72.99
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-10 -3 3 -5.00 17.60
-10 3 3 44.83 20.41
-10 -3 3 59.27 20.57
10 -3 -3 6.34 16.63
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10 3 -3 13.27 13.65
10 3 -3 6.34 18.80
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10 -3 -3 43.71 13.42
-10 3 3 7.27 13.23
-10 -3 3 1.78 14.71
10 3 -3 10.23 16.68
-10 3 3 17.69 12.15
10 3 -2 425.75 31.16
-10 3 2 376.78 23.28
-10 -3 2 348.38 27.57
10 -3 -2 357.46 28.40
10 3 -2 342.94 25.43
10 -3 -2 361.71 25.22
10 3 -2 425.65 31.24
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-10 3 2 348.10 24.20
-10 -3 2 487.13 36.35
-10 3 2 342.65 29.08
-10 3 2 439.82 32.30
-10 -3 2 396.74 31.47
-10 -3 1 33.24 19.96
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10 3 -1 43.68 18.65
10 3 -1 44.78 17.06
10 -3 -1 66.29 13.24
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10 -3 -1 77.96 17.66
10 3 -1 46.13 13.89
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10 -3 0 2032.64 96.01
10 3 0 1756.48 91.98
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10 3 0 1799.10 95.94
10 -3 0 1907.09 91.55
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-10 -3 0 2089.33 100.95
10 3 0 1895.89 97.65
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-10 -3 -1 120.87 23.42
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10 3 2 150.91 18.55
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10 3 3 210.20 25.25
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-10 3 -3 224.04 23.39
-10 -3 -3 177.54 19.39
-10 -3 -3 210.71 31.94
-10 -3 -3 214.29 27.96
-10 -3 -4 440.89 37.37
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-10 -3 -4 491.58 40.21
-10 -3 -4 583.05 43.78
10 -3 4 457.12 32.89
10 3 4 528.09 37.60
-10 -3 -4 526.34 31.45
-10 3 -4 502.46 35.96
-10 -3 -4 484.97 39.27
-10 -3 -5 38.59 29.54
10 -3 5 -4.04 18.38
10 3 5 30.22 21.35
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-10 -3 -5 10.15 16.46
10 3 5 20.82 26.00
-10 -3 -5 44.53 24.88
-10 3 -5 67.65 22.11
-10 3 -5 42.73 17.52
-10 -3 -5 46.15 24.47
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10 -3 6 652.22 41.43
-10 -3 -6 770.85 44.61
10 3 6 774.85 46.10
10 3 6 685.04 46.68
-10 -3 -6 772.73 48.72
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-10 3 -6 587.45 36.50
-10 -3 -6 859.28 50.07
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-10 3 -7 38.61 21.86
-10 -3 -7 -6.86 24.02
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10 3 7 -17.54 27.27
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-10 3 -8 24.52 24.41
-10 -3 -8 -9.27 26.48
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10 -3 8 -23.54 26.50
10 3 8 -9.40 27.61
-10 3 -8 17.61 27.74
-10 -3 -8 6.77 21.63
10 3 8 -20.60 31.16
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-10 3 -9 55.04 30.86
-10 -3 -9 52.00 25.07
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10 3 9 38.53 32.75
10 3 9 -7.75 30.29
-10 3 -10 407.72 42.44
10 3 10 484.45 48.80
-10 -3 -10 434.81 39.69
-10 3 -10 470.11 46.29
10 3 11 9.19 33.94
-10 3 -11 29.49 34.95
10 3 12 250.99 47.29
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25 0 -4 65.88 37.46
-25 0 3 48.95 38.01
25 0 -3 -5.15 35.25
-25 0 2 387.45 49.34
25 0 -2 467.17 48.81
-25 0 1 2.66 35.20
25 0 -1 48.58 34.86
-25 0 0 90.77 36.37
25 0 0 104.08 38.61
-25 0 -1 10.30 35.23
25 0 1 32.23 35.97
-25 0 -2 -15.68 37.04
25 0 2 -8.40 37.17
-25 -1 7 30.35 37.52
-25 1 7 13.86 32.53
25 1 -7 62.02 42.76
25 -1 -7 46.06 41.76
25 1 -6 -57.62 43.24
25 -1 -6 22.22 40.03
-25 -1 6 11.93 36.38
-25 1 6 32.53 32.14
25 1 -6 10.59 43.45
25 1 -5 190.28 45.92
25 -1 -5 183.66 42.73
25 1 -5 221.87 44.09
25 1 -4 52.12 40.46
25 -1 -4 73.81 37.69
25 1 -4 108.49 39.08
25 1 -3 9.71 39.47
25 -1 -3 117.21 37.58
25 1 -3 13.31 35.51
-25 -1 2 57.21 36.91
25 1 -2 76.76 39.22
25 -1 -2 93.55 36.27
25 1 -2 95.32 38.00
-25 -1 1 2.61 35.01
25 -1 -1 12.34 33.98
25 1 -1 2.66 37.52
-25 1 0 24.50 40.38
-25 -1 0 -10.17 35.54
25 -1 0 20.21 35.24
25 1 0 54.16 37.04
-25 -1 -1 378.69 48.08
25 -1 1 433.55 48.69
-26 0 4 319.76 50.74
26 0 -4 296.08 47.96
-26 0 3 -62.89 42.80
26 0 -3 10.80 37.29
-26 0 2 48.90 40.58
26 0 -2 -24.12 38.35
-26 0 1 -13.96 38.96
26 0 -1 -42.86 39.40
0 0 0 0.00 0.00
TITL 99726 in P2(1)/c
REM P2(1)/c (#14 in standard setting)
CELL 0.71073 19.690846 4.743103 12.648231 90.0000 100.4001 90.0000
ZERR 4.00 0.000976 0.000181 0.000502 0.0000 0.0044 0.0000
LATT 1
SYMM -x, y+1/2,-z+1/2
SFAC C H N Cl Br
UNIT 44.00 56.00 12.00 8.00 4.00
REM CrysAlisPro recorded range (K): Min=100.0; max=100.0; aver:100.0
TEMP -173
TREF
HKLF 4
END
_computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)'
;
_shelx_hkl_checksum 70941
_shelx_res_file
;
TITL 99726.res in P2(1)/c
99726.res
created by SHELXL-2018/3 at 14:25:59 on 29-Jan-2025
REM Old TITL 99726 in P2(1)/c
REM SHELXT solution in P2(1)/c: R1 0.093, Rweak 0.005, Alpha 0.049
REM 0.370 for 304 systematic absences, Orientation as input
REM Formula found by SHELXT: C12 N2 Br
CELL 0.71073 19.6908 4.7431 12.6482 90 100.4 90
ZERR 4 0.001 0.0002 0.0005 0 0.004 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C H Br N
UNIT 44 56 4 12
EQIV $1 +X,-1+Y,+Z
EQIV $2 +X,2.5-Y,-0.5+Z
L.S. 4 0 0
PLAN 2
TEMP -173
CONF
HTAB C1 Br1_$1
HTAB C2 Br1_$2
list 4
WPDB -2
fmap 2 53
acta
MORE -1
BOND $H
REM
REM
REM
WGHT 0.024200 1.906800
FVAR 0.57989
BR1 3 0.275929 1.082234 0.655526 11.00000 0.02611 0.01224 =
0.01118 -0.00042 0.00559 -0.00239
N1 4 0.371565 0.609700 0.482705 11.00000 0.01983 0.01252 =
0.00908 0.00151 0.00358 -0.00068
N2 4 0.393682 0.791327 0.410808 11.00000 0.02291 0.02079 =
0.01309 0.00424 0.00516 -0.00315
N3 4 0.279867 0.797778 0.395258 11.00000 0.01944 0.01013 =
0.01074 -0.00021 0.00355 0.00026
C1 1 0.304033 0.617112 0.474448 11.00000 0.01978 0.00978 =
0.01136 -0.00125 0.00405 0.00084
AFIX 43
H1 2 0.277417 0.513698 0.516732 11.00000 -1.20000
AFIX 0
C2 1 0.336298 0.897990 0.358533 11.00000 0.02552 0.01612 =
0.01060 0.00184 0.00366 -0.00395
AFIX 43
H2 2 0.334033 1.030051 0.301532 11.00000 -1.20000
AFIX 0
C3 1 0.421770 0.462331 0.563674 11.00000 0.01927 0.01595 =
0.01781 0.00630 0.00316 0.00311
AFIX 23
H3A 2 0.455642 0.362518 0.528078 11.00000 -1.20000
H3B 2 0.397652 0.320393 0.600822 11.00000 -1.20000
AFIX 0
C4 1 0.459229 0.670279 0.645236 11.00000 0.02468 0.02646 =
0.01615 0.00292 0.00098 0.00263
AFIX 137
H4A 2 0.482324 0.812772 0.608167 11.00000 -1.50000
H4B 2 0.493647 0.569756 0.697392 11.00000 -1.50000
H4C 2 0.425887 0.762499 0.682781 11.00000 -1.50000
AFIX 0
C5 1 0.207752 0.895063 0.359305 11.00000 0.01806 0.01595 =
0.01549 0.00202 -0.00127 0.00101
AFIX 23
H5A 2 0.201490 0.950344 0.282680 11.00000 -1.20000
H5B 2 0.199664 1.064231 0.401177 11.00000 -1.20000
AFIX 0
C6 1 0.155105 0.674111 0.372350 11.00000 0.01689 0.01352 =
0.01303 0.00057 0.00279 0.00582
C7 1 0.139415 0.619362 0.474096 11.00000 0.02113 0.01889 =
0.01491 -0.00146 0.00378 0.00320
AFIX 43
H7 2 0.163016 0.718389 0.535103 11.00000 -1.20000
AFIX 0
C8 1 0.089418 0.420582 0.486187 11.00000 0.02367 0.02837 =
0.01679 0.00439 0.00703 0.00257
AFIX 43
H8 2 0.079519 0.382201 0.555547 11.00000 -1.20000
AFIX 0
C9 1 0.054068 0.278613 0.397461 11.00000 0.01777 0.01664 =
0.02822 0.00258 0.00544 0.00051
AFIX 43
H9 2 0.019573 0.144551 0.405767 11.00000 -1.20000
AFIX 0
C10 1 0.069101 0.332444 0.296409 11.00000 0.01794 0.01830 =
0.02116 -0.00393 0.00090 0.00204
AFIX 43
H10 2 0.044887 0.234676 0.235544 11.00000 -1.20000
AFIX 0
C11 1 0.119359 0.528493 0.283765 11.00000 0.01928 0.01874 =
0.01546 0.00157 0.00462 0.00333
AFIX 43
H11 2 0.129458 0.563655 0.214295 11.00000 -1.20000
AFIX 0
HKLF 4
REM 99726.res in P2(1)/c
REM wR2 = 0.0738, GooF = S = 1.053, Restrained GooF = 1.053 for all data
REM R1 = 0.0383 for 2356 Fo > 4sig(Fo) and 0.0535 for all 2883 data
REM 137 parameters refined using 0 restraints
END
WGHT 0.0242 1.9068
REM Highest difference peak 1.396, deepest hole -0.576, 1-sigma level 0.100
Q1 1 0.3216 1.0839 0.6667 11.00000 0.05 1.40
Q2 1 0.2270 1.0845 0.6415 11.00000 0.05 1.17
;
_shelx_res_checksum 69927
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
Br Br1 0.27593(2) 1.08223(5) 0.65553(2) 0.01623(9) Uani d 1 . .
N N1 0.37156(11) 0.6097(5) 0.48270(16) 0.0137(4) Uani d 1 . .
N N2 0.39368(12) 0.7913(5) 0.41081(18) 0.0187(5) Uani d 1 . .
N N3 0.27987(11) 0.7978(4) 0.39526(17) 0.0133(5) Uani d 1 . .
C C1 0.30403(14) 0.6171(5) 0.4744(2) 0.0135(5) Uani d 1 . .
H H1 0.277417 0.513698 0.516732 0.016 Uiso calc 1 . .
C C2 0.33630(14) 0.8980(6) 0.3585(2) 0.0174(6) Uani d 1 . .
H H2 0.334033 1.030051 0.301532 0.021 Uiso calc 1 . .
C C3 0.42177(14) 0.4623(6) 0.5637(2) 0.0177(6) Uani d 1 . .
H H3A 0.455642 0.362518 0.528078 0.021 Uiso calc 1 . .
H H3B 0.397652 0.320393 0.600822 0.021 Uiso calc 1 . .
C C4 0.45923(16) 0.6703(6) 0.6452(2) 0.0228(6) Uani d 1 . .
H H4A 0.482324 0.812772 0.608167 0.034 Uiso calc 1 . .
H H4B 0.493647 0.569756 0.697392 0.034 Uiso calc 1 . .
H H4C 0.425887 0.762499 0.682781 0.034 Uiso calc 1 . .
C C5 0.20775(14) 0.8951(6) 0.3593(2) 0.0170(6) Uani d 1 . .
H H5A 0.201490 0.950344 0.282680 0.020 Uiso calc 1 . .
H H5B 0.199664 1.064231 0.401177 0.020 Uiso calc 1 . .
C C6 0.15510(14) 0.6741(5) 0.3724(2) 0.0145(5) Uani d 1 . .
C C7 0.13942(14) 0.6194(6) 0.4741(2) 0.0182(6) Uani d 1 . .
H H7 0.163016 0.718389 0.535103 0.022 Uiso calc 1 . .
C C8 0.08942(15) 0.4206(7) 0.4862(2) 0.0225(6) Uani d 1 . .
H H8 0.079519 0.382201 0.555547 0.027 Uiso calc 1 . .
C C9 0.05407(14) 0.2786(6) 0.3975(2) 0.0207(6) Uani d 1 . .
H H9 0.019573 0.144551 0.405767 0.025 Uiso calc 1 . .
C C10 0.06910(14) 0.3324(6) 0.2964(2) 0.0195(6) Uani d 1 . .
H H10 0.044887 0.234676 0.235544 0.023 Uiso calc 1 . .
C C11 0.11936(14) 0.5285(6) 0.2838(2) 0.0176(6) Uani d 1 . .
H H11 0.129458 0.563655 0.214295 0.021 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
Br1 0.02611(15) 0.01224(13) 0.01118(12) -0.00239(12) 0.00559(9) -0.00042(11)
N1 0.0198(12) 0.0125(11) 0.0091(10) -0.0007(9) 0.0036(9) 0.0015(9)
N2 0.0229(13) 0.0208(12) 0.0131(11) -0.0032(10) 0.0052(10) 0.0042(10)
N3 0.0194(12) 0.0101(11) 0.0107(11) 0.0003(9) 0.0036(9) -0.0002(9)
C1 0.0198(13) 0.0098(12) 0.0114(12) 0.0008(11) 0.0041(10) -0.0013(10)
C2 0.0255(15) 0.0161(13) 0.0106(12) -0.0040(12) 0.0037(11) 0.0018(11)
C3 0.0193(14) 0.0159(14) 0.0178(13) 0.0031(11) 0.0032(11) 0.0063(11)
C4 0.0247(16) 0.0265(16) 0.0161(14) 0.0026(12) 0.0010(12) 0.0029(12)
C5 0.0181(14) 0.0160(13) 0.0155(13) 0.0010(11) -0.0013(10) 0.0020(11)
C6 0.0169(14) 0.0135(13) 0.0130(13) 0.0058(10) 0.0028(11) 0.0006(10)
C7 0.0211(14) 0.0189(14) 0.0149(13) 0.0032(12) 0.0038(11) -0.0015(11)
C8 0.0237(15) 0.0284(16) 0.0168(13) 0.0026(14) 0.0070(11) 0.0044(13)
C9 0.0178(14) 0.0166(14) 0.0282(16) 0.0005(12) 0.0054(12) 0.0026(12)
C10 0.0179(14) 0.0183(14) 0.0212(14) 0.0020(11) 0.0009(12) -0.0039(11)
C11 0.0193(14) 0.0187(14) 0.0155(13) 0.0033(11) 0.0046(11) 0.0016(11)
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'
Br Br -0.2901 2.4595 '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'
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
N2 N1 C3 . . 120.3(2) ?
C1 N1 N2 . . 111.5(2) ?
C1 N1 C3 . . 127.8(2) ?
C2 N2 N1 . . 103.2(2) ?
C1 N3 C2 . . 106.0(2) ?
C1 N3 C5 . . 128.3(2) ?
C2 N3 C5 . . 125.5(2) ?
N1 C1 N3 . . 107.1(2) y
N1 C1 H1 . . 126.4 ?
N3 C1 H1 . . 126.4 ?
N2 C2 N3 . . 112.1(2) ?
N2 C2 H2 . . 123.9 ?
N3 C2 H2 . . 123.9 ?
N1 C3 H3A . . 109.6 ?
N1 C3 H3B . . 109.6 ?
N1 C3 C4 . . 110.4(2) ?
H3A C3 H3B . . 108.1 ?
C4 C3 H3A . . 109.6 ?
C4 C3 H3B . . 109.6 ?
C3 C4 H4A . . 109.5 ?
C3 C4 H4B . . 109.5 ?
C3 C4 H4C . . 109.5 ?
H4A C4 H4B . . 109.5 ?
H4A C4 H4C . . 109.5 ?
H4B C4 H4C . . 109.5 ?
N3 C5 H5A . . 109.0 ?
N3 C5 H5B . . 109.0 ?
N3 C5 C6 . . 113.0(2) ?
H5A C5 H5B . . 107.8 ?
C6 C5 H5A . . 109.0 ?
C6 C5 H5B . . 109.0 ?
C7 C6 C5 . . 120.0(2) ?
C11 C6 C5 . . 121.0(2) ?
C11 C6 C7 . . 118.9(3) ?
C6 C7 H7 . . 119.9 ?
C8 C7 C6 . . 120.3(3) ?
C8 C7 H7 . . 119.9 ?
C7 C8 H8 . . 119.9 ?
C9 C8 C7 . . 120.2(3) ?
C9 C8 H8 . . 119.9 ?
C8 C9 H9 . . 120.1 ?
C8 C9 C10 . . 119.9(3) ?
C10 C9 H9 . . 120.1 ?
C9 C10 H10 . . 119.8 ?
C9 C10 C11 . . 120.3(3) ?
C11 C10 H10 . . 119.8 ?
C6 C11 H11 . . 119.8 ?
C10 C11 C6 . . 120.4(3) ?
C10 C11 H11 . . 119.8 ?
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
N1 N2 . 1.379(3) ?
N1 C1 . 1.315(3) y
N1 C3 . 1.466(3) ?
N2 C2 . 1.304(4) ?
N3 C1 . 1.339(3) y
N3 C2 . 1.365(3) ?
N3 C5 . 1.484(3) ?
C1 H1 . 0.9500 ?
C2 H2 . 0.9500 ?
C3 H3A . 0.9900 ?
C3 H3B . 0.9900 ?
C3 C4 . 1.519(4) ?
C4 H4A . 0.9800 ?
C4 H4B . 0.9800 ?
C4 H4C . 0.9800 ?
C5 H5A . 0.9900 ?
C5 H5B . 0.9900 ?
C5 C6 . 1.504(4) ?
C6 C7 . 1.401(4) ?
C6 C11 . 1.394(4) ?
C7 H7 . 0.9500 ?
C7 C8 . 1.391(4) ?
C8 H8 . 0.9500 ?
C8 C9 . 1.384(4) ?
C9 H9 . 0.9500 ?
C9 C10 . 1.387(4) ?
C10 H10 . 0.9500 ?
C10 C11 . 1.388(4) ?
C11 H11 . 0.9500 ?
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
C1 H1 Br1 1_545 0.95 2.70 3.528(3) 146 yes
C2 H2 Br1 4_585 0.95 2.71 3.603(3) 157 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
N1 N2 C2 N3 . . . . 1.3(3) ?
N2 N1 C1 N3 . . . . 1.6(3) ?
N2 N1 C3 C4 . . . . 67.8(3) ?
N3 C5 C6 C7 . . . . 77.2(3) ?
N3 C5 C6 C11 . . . . -105.3(3) ?
C1 N1 N2 C2 . . . . -1.8(3) ?
C1 N1 C3 C4 . . . . -104.3(3) ?
C1 N3 C2 N2 . . . . -0.4(3) ?
C1 N3 C5 C6 . . . . -32.3(4) ?
C2 N3 C1 N1 . . . . -0.7(3) ?
C2 N3 C5 C6 . . . . 153.9(2) ?
C3 N1 N2 C2 . . . . -175.0(2) ?
C3 N1 C1 N3 . . . . 174.2(2) ?
C5 N3 C1 N1 . . . . -175.4(2) ?
C5 N3 C2 N2 . . . . 174.5(2) ?
C5 C6 C7 C8 . . . . 178.3(3) ?
C5 C6 C11 C10 . . . . -177.6(2) ?
C6 C7 C8 C9 . . . . -1.0(4) ?
C7 C6 C11 C10 . . . . 0.0(4) ?
C7 C8 C9 C10 . . . . 0.7(4) ?
C8 C9 C10 C11 . . . . -0.1(4) ?
C9 C10 C11 C6 . . . . -0.2(4) ?
C11 C6 C7 C8 . . . . 0.6(4) ?