#------------------------------------------------------------------------------
#$Date: 2024-08-07 01:06:04 +0300 (Wed, 07 Aug 2024) $
#$Revision: 293998 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/31/2023171.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_2023171
loop_
_publ_author_name
'Döring, Cindy'
'Jones, Peter G.'
_publ_section_title
;
Crystal structures of four gold(I) complexes [AuL
2]+[AuX 2]- and a
by-product
(L·LH+)[AuBr2]-
(L = substituted pyridine, X = Cl or Br).
;
_journal_coeditor_code YZ2055
_journal_issue 'Pt 7'
_journal_name_full
'Acta crystallographica. Section E, Crystallographic communications'
_journal_page_first 729
_journal_page_last 737
_journal_paper_doi 10.1107/S2056989024005437
_journal_volume 80
_journal_year 2024
_chemical_formula_iupac '(C5 H5 Br N) [Au Br2], C5 H4 Br N'
_chemical_formula_moiety 'C5 H5 Br N +, Au Br2 -, C5 H4 Br N'
_chemical_formula_sum 'C10 H9 Au Br4 N2'
_chemical_formula_weight 673.80
_chemical_name_systematic
;
2-Bromopyridinium dibromidoaurate(I)--2-bromopyridine (1/1)
;
_space_group_crystal_system triclinic
_space_group_IT_number 2
_space_group_name_Hall '-P 1'
_space_group_name_H-M_alt 'P -1'
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-2019/3
_cell_angle_alpha 87.202(4)
_cell_angle_beta 74.635(4)
_cell_angle_gamma 81.406(4)
_cell_formula_units_Z 2
_cell_length_a 7.9931(4)
_cell_length_b 8.4672(3)
_cell_length_c 11.3923(5)
_cell_measurement_reflns_used 14102
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 30.6010
_cell_measurement_theta_min 2.4330
_cell_volume 735.08(6)
_computing_cell_refinement
;
CrysAlisPro, Version 1.171.36.28 (Rigaku OD, 2014)
;
_computing_data_collection
;
CrysAlisPro, Version 1.171.36.28 (Rigaku OD, 2014)
;
_computing_data_reduction
;
CrysAlisPro, Version 1.171.36.28 (Rigaku OD, 2014)
;
_computing_molecular_graphics
;
Bruker XP, Version 5.1 (Bruker, 1998)
;
_computing_publication_material
;
SHELXL2019/3 (Sheldrick, 2015)
;
_computing_structure_refinement
;
SHELXL2019/3 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature 100(2)
_diffrn_detector_area_resol_mean 16.1419
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.936
_diffrn_measurement_device_type 'Oxford Diffrection Xcalibur, Eos'
_diffrn_measurement_method '\w scan'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0439
_diffrn_reflns_av_unetI/netI 0.0259
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_k_max 12
_diffrn_reflns_limit_k_min -11
_diffrn_reflns_limit_l_max 16
_diffrn_reflns_limit_l_min -16
_diffrn_reflns_number 42320
_diffrn_reflns_theta_full 30.000
_diffrn_reflns_theta_max 30.907
_diffrn_reflns_theta_min 2.433
_diffrn_source 'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu 20.857
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.24142
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2014)
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 3.044
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 604
_exptl_crystal_size_max 0.15
_exptl_crystal_size_mid 0.10
_exptl_crystal_size_min 0.04
_refine_diff_density_max 1.153
_refine_diff_density_min -1.493
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.072
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 158
_refine_ls_number_reflns 4361
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.072
_refine_ls_R_factor_all 0.0285
_refine_ls_R_factor_gt 0.0228
_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^)+(0.0232P)^2^+0.2423P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0460
_refine_ls_wR_factor_ref 0.0480
_reflns_number_gt 3917
_reflns_number_total 4361
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file yz2055.cif
_cod_data_source_block 5
_cod_depositor_comments
'Adding full bibliography for 2023167--2023171.cif.'
_cod_original_cell_volume 735.09(6)
_cod_database_code 2023171
_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 0.146
_shelx_estimated_absorpt_t_max 0.489
_shelx_hkl_file
;
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-10 -2 -7 7605.70 1597.36 6
-10 -2 -7 5392.40 1374.77 16
10 2 7 5862.44 761.706 15
10 2 7 6616.96 855.217 24
10 2 8 5897.98 851.074 23
10 2 8 6110.03 811.378 4
10 2 8 6526.51 892.180 22
10 2 8 6302.76 881.960 21
-10 -2 -8 9332.16 1688.70 6
-10 -2 -8 5566.70 1466.64 16
10 2 8 5502.74 782.667 15
10 2 8 5344.83 798.288 24
10 2 9 619.087 345.740 4
10 2 9-446.548 349.049 23
10 2 9 143.639 359.166 22
10 2 9 164.914 241.421 21
-10 -2 -9-110.747 530.905 6
-10 -2 -9 12.7637 764.482 16
10 2 9-109.699 264.735 15
10 2 9 627.776 399.963 24
-10 -2 -10 14805.3 1928.63 6
10 2 10 11271.7 1247.33 15
10 2 10 13070.0 1218.89 4
-10 -2 -11 12461.2 1737.23 6
-10 -3 3-631.326 618.708 6
-10 -3 3 142.439 502.848 8
10 3 -2 606.830 367.484 23
10 3 -2 1072.83 428.610 22
10 3 -2 948.478 469.028 21
-10 -3 2 1082.51 571.616 6
10 3 -2 801.660 562.672 2
-10 -3 2 1929.43 651.466 8
-10 -3 2 647.766 352.725 25
10 3 -1 23201.4 1639.42 22
10 3 -1 23355.4 1640.68 21
-10 -3 1 27195.2 2917.77 6
10 3 -1 23993.9 2032.92 2
-10 -3 1 25804.2 2150.00 17
-10 -3 1 21919.5 2182.36 8
-10 -3 1 24085.3 1709.67 25
10 3 -1 23515.5 1811.99 13
10 3 -1 24277.1 1669.78 23
10 3 0 3890.02 668.687 23
10 3 0 1447.95 460.948 22
10 3 0 2558.94 547.668 21
-10 -3 0 3726.84 1274.56 6
-10 -3 0 4558.82 940.227 17
-10 -3 0 2507.22 773.893 8
10 3 0 2570.46 699.131 2
-10 -3 0 3516.55 647.470 25
10 3 0 2405.66 575.612 13
10 3 1 2026.38 514.926 23
10 3 1 1908.65 488.873 22
10 3 1 1395.70 428.396 21
-10 -3 -1 2387.61 1134.39 6
10 3 1 1448.71 362.892 9
-10 -3 -1 2193.60 672.510 17
10 3 1 2634.57 631.886 2
-10 -3 -1 2250.15 544.289 25
10 3 1 2838.12 675.120 13
10 3 2 11334.9 1082.12 22
10 3 2 11247.1 1078.90 21
-10 -3 -2 13640.8 2417.36 6
10 3 2 13620.9 1167.21 9
-10 -3 -2 12558.2 1426.93 17
-10 -3 -2 9975.82 1030.95 25
10 3 2 12797.3 1240.78 13
10 3 2 10662.0 1004.66 1
10 3 2 10860.5 1061.86 23
10 3 3 5152.18 726.840 23
10 3 3 5760.10 770.702 22
10 3 3 6582.01 825.931 21
-10 -3 -3 5449.43 1624.29 6
-10 -3 -3 6520.19 1057.71 17
-10 -3 -3 4411.48 907.552 16
10 3 3 5902.00 747.456 1
-10 -3 -3 5138.06 757.495 25
10 3 3 6499.77 906.140 13
10 3 4 816.126 337.875 23
10 3 4 796.593 378.141 22
10 3 4 1150.34 379.577 21
-10 -3 -4 1679.67 1114.85 6
10 3 4 483.723 233.460 1
-10 -3 -4 1746.03 636.864 17
-10 -3 -4-295.867 556.292 16
-10 -3 -4 516.853 255.874 25
10 3 4 1023.66 418.558 13
10 3 5 3562.37 620.398 23
10 3 5 4557.25 682.934 1
10 3 5 4627.90 700.373 4
10 3 5 3811.98 653.833 22
10 3 5 4514.07 704.324 21
-10 -3 -5 4650.49 1411.65 6
-10 -3 -5 4048.14 813.792 17
-10 -3 -5 4079.46 1067.18 16
10 3 5 3780.52 710.973 13
10 3 6-8.58389 247.589 23
10 3 6 154.236 236.790 4
10 3 6-150.866 310.628 22
10 3 6 50.5535 302.388 21
-10 -3 -6-136.492 710.083 6
-10 -3 -6 326.623 384.289 17
-10 -3 -6-89.5207 619.881 16
10 3 6 616.926 356.897 1
10 3 6-347.637 363.459 24
10 3 7 6022.24 816.632 23
10 3 7 6778.94 823.653 4
10 3 7 7218.29 890.239 22
10 3 7 6033.88 817.512 21
-10 -3 -7 7228.15 1595.95 6
-10 -3 -7 7305.02 1073.90 17
10 3 7 6923.39 879.010 1
-10 -3 -7 4626.08 1254.12 16
10 3 7 6506.88 853.082 24
10 3 8 4849.98 757.714 23
10 3 8 3994.29 640.203 4
10 3 8 4985.02 770.273 22
10 3 8 4435.96 716.165 21
-10 -3 -8 6171.09 1444.96 6
10 3 8 3650.47 642.341 1
-10 -3 -8 6351.66 1466.86 16
10 3 8 4102.28 670.024 15
10 3 8 3300.62 624.916 24
10 3 9 12329.2 1226.03 22
10 3 9 13478.1 1299.73 21
-10 -3 -9 15382.4 2067.53 6
10 3 9 13728.5 1336.10 1
10 3 9 12792.2 1240.28 15
10 3 9 14165.3 1309.93 24
10 3 9 13654.3 1276.29 23
10 3 10 9262.77 1164.67 1
-10 -3 -10 9402.80 1565.66 6
10 3 10 9805.08 1154.00 15
10 3 11 6831.01 1073.59 1
-10 -3 -11 4385.93 1080.77 6
-10 -4 3 1202.55 634.683 8
10 4 -2 3911.18 675.073 23
10 4 -2 3370.87 648.106 22
10 4 -2 4275.05 755.846 21
-10 -4 2 4208.70 1126.00 6
10 4 -2 3701.13 928.153 2
-10 -4 2 3018.44 967.570 8
-10 -4 2 3318.38 702.848 25
10 4 -1 5669.27 804.630 23
10 4 -1 6060.80 834.500 22
10 4 -1 5922.27 820.436 21
-10 -4 1 2288.37 944.918 6
-10 -4 1 4162.69 940.742 17
10 4 -1 6199.48 1055.23 2
-10 -4 1 6094.32 847.050 25
10 4 0 21150.4 1508.64 22
10 4 0 21554.5 1531.32 1
10 4 0 19630.2 1463.69 21
-10 -4 0 22584.4 2781.81 6
10 4 0 22673.5 1883.22 2
-10 -4 0 23228.3 2070.98 17
-10 -4 0 19673.7 1484.57 25
10 4 0 22185.2 1706.86 13
10 4 0 20836.6 1502.03 23
10 4 1 8628.71 954.315 23
10 4 1 6840.38 848.110 22
10 4 1 8059.50 910.597 21
-10 -4 -1 5555.86 1538.01 6
-10 -4 -1 6393.24 1087.94 17
10 4 1 7963.57 1051.40 2
-10 -4 -1 7353.81 888.006 25
10 4 1 7592.72 883.330 1
10 4 1 7541.27 972.302 13
10 4 2 11954.0 1089.18 22
10 4 2 12781.0 1122.90 21
-10 -4 -2 14357.9 2492.67 6
-10 -4 -2 14407.3 1577.17 17
-10 -4 -2 13628.5 1178.98 25
10 4 2 12788.5 1243.65 13
10 4 2 12299.7 1121.11 23
10 4 2 13236.0 1163.38 1
10 4 3 456.381 333.860 23
10 4 3 242.116 260.470 22
10 4 3 907.335 393.860 21
-10 -4 -3 1613.86 1053.11 6
-10 -4 -3 860.163 521.578 17
-10 -4 -3 435.729 405.563 16
-10 -4 -3-42.9634 296.629 25
10 4 3 591.810 259.435 1
10 4 3 594.087 347.270 13
10 4 4 3353.46 604.493 23
10 4 4 3671.29 607.037 22
10 4 4 3732.28 611.446 21
-10 -4 -4 4564.78 1665.90 6
10 4 4 4445.34 703.725 1
-10 -4 -4 3862.21 807.709 17
-10 -4 -4 2577.29 733.795 16
10 4 4 3551.53 645.034 13
10 4 5 463.839 283.214 23
10 4 5 4.10525 269.493 4
10 4 5 240.198 257.635 22
10 4 5 646.085 315.237 1
10 4 5 357.807 295.062 21
-10 -4 -5 324.733 630.120 6
-10 -4 -5 270.479 394.804 17
-10 -4 -5-799.193 664.206 16
10 4 5 480.120 311.869 24
10 4 5 338.393 318.153 13
10 4 6 546.554 358.489 23
10 4 6 388.707 200.650 4
10 4 6 391.313 269.944 22
10 4 6 880.860 376.711 21
-10 -4 -6 1549.72 945.657 6
-10 -4 -6 1306.27 515.732 17
-10 -4 -6 1701.55 861.204 16
10 4 6 822.794 352.248 24
10 4 6 1133.68 445.353 1
10 4 7 70.4660 320.354 23
10 4 7 404.651 331.220 22
10 4 7 188.183 238.365 21
-10 -4 -7-44.4807 706.191 6
-10 -4 -7-770.878 734.826 16
10 4 7-219.042 299.262 1
10 4 7 316.785 367.508 24
10 4 8 13211.4 1242.09 22
10 4 8 13511.4 1246.92 21
-10 -4 -8 14699.7 2151.50 6
10 4 8 11712.3 1209.08 1
-10 -4 -8 11471.0 1894.87 16
10 4 8 12927.9 1227.62 24
10 4 8 13108.3 1220.47 23
10 4 9 4729.11 772.708 23
10 4 9 6276.43 903.502 22
10 4 9 6415.60 896.670 21
-10 -4 -9 4688.11 1169.77 6
10 4 9 5953.81 894.451 1
10 4 9 6872.92 907.876 24
10 4 10 2471.49 623.787 23
10 4 10 2109.37 581.864 22
10 4 10 2236.31 578.649 21
-10 -4 -10 2164.13 874.257 6
10 4 10 2629.33 655.320 1
10 4 10 1351.11 494.744 15
10 4 10 1882.92 547.574 24
10 5 -2 577.632 318.403 23
10 5 -2 46.3681 276.507 22
10 5 -2 160.526 306.792 21
-10 -5 2 74.8602 304.218 25
10 5 -1 9720.55 1018.70 23
10 5 -1 7466.51 911.700 22
10 5 -1 8610.72 968.766 21
10 5 -1 7997.68 1205.55 2
-10 -5 1 8636.25 995.427 25
10 5 0 18780.7 1405.33 22
10 5 0 20861.1 1574.52 1
10 5 0 20809.1 1478.58 21
-10 -5 0 20600.2 2690.60 6
10 5 0 20158.3 1791.23 2
-10 -5 0 21448.6 2094.14 17
-10 -5 0 19699.0 1468.20 25
10 5 0 20470.9 1641.31 13
10 5 0 20275.3 1454.41 23
10 5 1-210.543 293.157 23
10 5 1-91.6954 239.871 1
10 5 1-132.352 242.286 22
10 5 1 799.410 398.555 21
-10 -5 -1-780.741 854.975 6
-10 -5 -1 93.0594 393.293 17
-10 -5 -1-214.168 300.756 25
10 5 1-129.393 272.493 13
10 5 2 1117.59 380.565 23
10 5 2 1447.12 449.837 22
10 5 2 1148.58 358.505 21
-10 -5 -2 1770.46 1057.60 6
10 5 2 577.501 296.368 1
-10 -5 -2 232.109 449.594 17
-10 -5 -2 1277.32 402.410 25
10 5 2 1738.85 545.760 13
10 5 3 7326.38 841.149 23
10 5 3 6610.99 811.772 22
10 5 3 8422.74 900.646 21
-10 -5 -3 5334.73 1695.23 6
-10 -5 -3 7839.89 1205.02 17
-10 -5 -3 9009.09 1214.40 16
-10 -5 -3 7329.74 847.694 25
10 5 3 8085.34 949.000 1
10 5 3 8538.07 988.824 13
10 5 4 4004.61 649.030 23
10 5 4 4008.09 629.016 22
10 5 4 4216.05 636.095 21
-10 -5 -4 1530.80 961.323 6
-10 -5 -4 5223.08 1003.13 17
10 5 4 2755.36 603.434 1
-10 -5 -4 2544.86 755.932 16
10 5 4 3729.30 663.578 13
10 5 5 2658.24 568.148 23
10 5 5 1661.39 442.003 22
10 5 5 1700.81 449.132 21
-10 -5 -5 844.944 738.518 6
10 5 5 2036.11 484.484 1
-10 -5 -5 2355.22 681.193 16
10 5 5 2451.13 548.909 24
10 5 5 3127.85 636.749 13
10 5 6 758.556 307.344 23
10 5 6 1264.71 447.181 1
10 5 6 608.410 292.185 22
10 5 6 431.910 270.921 21
-10 -5 -6 131.453 772.391 6
-10 -5 -6 1760.57 758.722 16
10 5 6 1121.97 435.728 24
10 5 7 13222.2 1192.73 22
10 5 7 12439.6 1167.31 21
-10 -5 -7 12418.2 2142.74 6
-10 -5 -7 12603.3 1841.96 16
10 5 7 12541.8 1247.41 1
10 5 7 10563.2 1084.12 24
10 5 7 13937.8 1226.82 23
10 5 8-411.366 358.026 23
10 5 8 566.511 384.437 22
10 5 8 884.344 416.970 21
10 5 8-163.878 301.370 1
10 5 8 162.540 297.310 24
10 5 9 3293.14 671.677 23
10 5 9 2534.70 617.373 22
10 5 9 3022.99 616.475 21
10 5 9 2508.81 602.398 1
10 5 9 3725.72 673.628 24
10 5 10 14330.8 1360.90 22
10 5 10 11968.3 1261.05 21
10 5 10 15923.9 1430.68 24
10 5 10 13979.5 1354.33 23
10 6 -1 13508.8 1615.62 2
10 6 1 3463.21 673.297 1
-10 -6 -1 3312.07 915.414 17
10 6 1 2922.61 624.249 13
-10 -6 -2 17161.7 1950.92 17
10 6 2 18140.6 1466.61 13
10 6 2 17621.6 1468.23 1
-10 -6 -3 1301.89 631.419 17
-10 -6 -3 962.574 463.360 16
10 6 3 418.034 325.738 13
10 6 3 702.556 381.089 1
10 6 4 251.662 294.420 1
-10 -6 -4-325.700 551.015 16
10 6 4 711.279 356.275 13
10 6 5 1474.82 515.014 1
-10 -6 -5 1449.47 725.331 16
10 6 5 845.550 325.941 13
10 6 6-4.07234 319.356 1
-10 -6 -6 95.9417 458.322 16
-10 -7 -1 2906.06 982.145 17
10 7 2 1772.36 502.613 13
-10 -7 -3 3923.93 815.128 16
10 7 3 4509.56 730.978 13
-10 -7 -4 2796.85 745.185 16
-11 1 -2 14491.8 1906.56 5
11 -1 4 5307.24 776.242 15
11 -1 5 10265.3 1105.28 15
11 -1 6 2254.69 557.721 15
-11 0 -2 2261.04 922.587 5
-11 0 -3 21534.7 2341.88 5
-11 0 -4 6332.79 1284.03 5
-11 0 -4 5856.29 1506.73 16
11 0 6 1380.52 483.106 15
11 0 7 3666.40 700.932 15
-11 -1 0 847.010 527.424 11
11 1 0 1760.14 497.821 9
11 1 1 1338.87 496.801 9
11 1 2 6507.34 922.328 9
-11 -1 -3 18101.4 2242.34 5
11 1 3 21119.9 1664.12 9
11 1 4 404.036 336.299 9
-11 -1 -4-462.093 761.341 16
-11 -1 -5 959.717 713.862 16
-11 -1 -6 4738.54 1470.46 16
11 1 7 2825.76 564.286 15
11 1 8 3194.90 637.999 15
11 2 1 2840.82 607.474 9
11 2 2 11216.2 1153.97 9
11 2 3 4934.67 824.261 9
11 2 4 11010.7 1143.98 4
-11 -2 -4 9883.82 1328.05 17
-11 -2 -4 9909.96 1543.16 16
-11 -2 -5 12951.7 1488.46 17
-11 -2 -5 10866.4 1823.52 16
11 2 5 12938.9 1246.58 4
11 2 6 605.179 319.500 4
-11 -2 -6 389.737 366.297 17
-11 -2 -6-294.250 606.653 16
11 2 7 1089.98 466.971 4
11 2 8 3167.81 619.832 4
11 2 9 1756.17 562.145 15
11 3 2 433.023 354.271 9
11 3 3 31186.8 1965.11 9
11 3 4 535.114 363.118 23
11 3 4 150.166 277.014 22
11 3 4 862.294 440.660 21
-11 -3 -4-181.987 494.074 16
11 3 5 369.742 349.822 4
-11 -3 -5 799.872 487.907 17
-11 -3 -5 1333.48 703.367 16
11 3 6 4259.15 708.739 4
-11 -3 -6 4171.46 910.414 17
-11 -3 -6 3844.11 1146.75 16
11 3 7 3087.76 624.620 4
-11 -3 -7 3505.13 851.734 17
11 4 3 1336.70 473.655 23
11 4 3 604.117 356.084 22
11 4 3 984.903 376.690 21
-11 -4 -3 1897.12 504.059 25
11 4 4 5775.29 836.864 23
11 4 4 4263.11 711.414 22
11 4 4 3377.89 630.855 21
-11 -4 -4 4267.33 941.247 17
-11 -4 -4 3783.66 920.025 16
11 4 5 11490.9 1168.77 22
11 4 5 10221.1 1098.78 21
-11 -4 -5 13462.1 1597.06 17
-11 -4 -5 10397.7 1602.71 16
11 4 5 12294.9 1153.17 4
11 4 5 10533.3 1122.40 24
11 4 5 12356.1 1205.15 23
11 4 6 4780.08 788.847 23
11 4 6 4732.94 763.581 22
11 4 6 4462.29 748.850 21
11 4 6 2834.11 608.700 24
11 5 3 19157.5 1543.62 1
11 5 4 6872.87 875.485 23
11 5 4 5581.11 808.263 22
11 5 4 6542.88 882.720 21
11 5 4 5192.39 810.056 1
-11 -5 -4 5744.02 1101.20 17
-11 -5 -4 4587.90 972.477 16
11 5 5 4834.13 767.196 23
11 5 5 3872.47 684.565 22
11 5 5 4878.12 833.858 1
11 5 5 4061.82 691.732 21
11 5 5 4019.03 701.044 24
11 5 6 1026.80 434.079 23
11 5 6 38.4550 333.135 22
11 5 6 469.993 280.603 21
11 5 6 544.333 310.853 24
0 0 0 0.00 0.00 0
TITL Fuessen in P-1
REM P-1 (#2 in standard setting)
CELL 0.71073 7.993130 8.467240 11.392261 87.2023 74.6349 81.4063
ZERR 5.00 0.000199 0.000164 0.000246 0.0017 0.0020 0.0019
LATT 1
SFAC C H N Br Au
UNIT 25.00 20.00 5.00 10.00 5.00
TREF
HKLF 4
END
;
_shelx_hkl_checksum 46657
_shelx_res_file
;
TITL Fuessen in P-1
shelx.res
created by SHELXL-2019/3 at 11:21:45 on 26-Mar-2024
CELL 0.71073 7.99313 8.46724 11.392261 87.2023 74.6349 81.4063
ZERR 2 0.0004 0.00033 0.0005 0.0035 0.004 0.004
LATT 1
SFAC C H Au Br N
UNIT 20 18 2 8 4
EQIV $1 1+X,1+Y,+Z
EQIV $2 1-X,1-Y,1-Z
EQIV $3 -1+X,+Y,+Z
EQIV $4 +X,1+Y,+Z
EQIV $5 1+X,+Y,+Z
EQIV $6 +X,-1+Y,+Z
L.S. 6
FMAP 2
PLAN 10
SIZE 0.15 0.1 0.04
TEMP -173
ACTA 60
BOND $H
CONF
HTAB N11 N21
HTAB C16 Br1
HTAB C13 Br2_$1
HTAB C26 Br2_$2
HTAB C26 Br3
HTAB C16 Br4
RTAB DIST Au1 Br4
RTAB DIST Br1 Br4
RTAB ANGL Au1 Br1 Br4
RTAB DIST Br2 Br3_$2
RTAB ANGL Au1 Br2 Br3_$2
RTAB DIST Br2 Br4_$3
RTAB ANGL Au1 Br2 Br4_$3
RTAB DIST Br3 Br2_$2
RTAB ANGL C12 Br3 Br2_$2
RTAB DIST Br3 Br4_$2
RTAB ANGL C12 Br3 Br4_$2
RTAB DIST Br3 Br4_$4
RTAB ANGL C12 Br3 Br4_$4
RTAB DIST Br4 Au1
RTAB ANGL C22 Br4 Au1
RTAB DIST Br4 Br1
RTAB ANGL C22 Br4 Br1
RTAB DIST Br4 Br2_$5
RTAB ANGL C22 Br4 Br2_$5
RTAB DIST Br4 Br3_$2
RTAB ANGL C22 Br4 Br3_$2
RTAB DIST Br4 Br3_$6
RTAB ANGL C22 Br4 Br3_$6
WGHT 0.023200 0.242300
FVAR 1.98803
AU1 3 0.406132 0.198003 0.142370 11.00000 0.01907 0.01413 =
0.01280 0.00052 -0.00677 -0.00329
BR1 4 0.707826 0.202531 0.044406 11.00000 0.02015 0.02330 =
0.01494 -0.00038 -0.00459 -0.00386
BR2 4 0.102878 0.199773 0.241269 11.00000 0.01936 0.02198 =
0.01792 -0.00229 -0.00596 -0.00588
BR3 4 0.875214 0.807052 0.458160 11.00000 0.01851 0.01701 =
0.01330 -0.00125 -0.00431 -0.00387
BR4 4 0.619103 0.207055 0.379518 11.00000 0.01940 0.01518 =
0.01382 -0.00023 -0.00620 -0.00519
N11 5 0.799274 0.599281 0.307977 11.00000 0.01836 0.01329 =
0.01271 0.00300 -0.00488 -0.00127
H11 2 0.776584 0.536991 0.371970 11.00000 0.02273
C12 1 0.848632 0.743932 0.310386 11.00000 0.01301 0.01398 =
0.01322 -0.00046 -0.00347 -0.00033
C13 1 0.879622 0.838086 0.206640 11.00000 0.01749 0.01553 =
0.01620 -0.00012 -0.00143 -0.00631
AFIX 43
H13 2 0.915444 0.939910 0.207838 11.00000 -1.20000
AFIX 0
C14 1 0.857394 0.780975 0.101041 11.00000 0.01769 0.01786 =
0.01500 0.00626 -0.00428 -0.00389
AFIX 43
H14 2 0.874796 0.845044 0.029191 11.00000 -1.20000
AFIX 0
C15 1 0.809843 0.630662 0.099707 11.00000 0.02368 0.01847 =
0.01313 -0.00199 -0.00499 -0.00153
AFIX 43
H15 2 0.797788 0.589640 0.026693 11.00000 -1.20000
AFIX 0
C16 1 0.780409 0.541873 0.204838 11.00000 0.02614 0.01463 =
0.01861 0.00070 -0.00906 -0.00320
AFIX 43
H16 2 0.746428 0.439010 0.205056 11.00000 -1.20000
AFIX 0
N21 5 0.705046 0.413700 0.525954 11.00000 0.01928 0.01026 =
0.01212 0.00105 -0.00472 -0.00143
C22 1 0.650672 0.272603 0.528791 11.00000 0.01355 0.01337 =
0.01303 -0.00322 -0.00366 -0.00032
C23 1 0.615267 0.173425 0.629459 11.00000 0.01832 0.01262 =
0.01761 -0.00014 -0.00315 -0.00383
AFIX 43
H23 2 0.578118 0.072941 0.624963 11.00000 -1.20000
AFIX 0
C24 1 0.635960 0.225984 0.737058 11.00000 0.02236 0.01545 =
0.01291 0.00127 -0.00081 -0.00230
AFIX 43
H24 2 0.613599 0.161686 0.808677 11.00000 -1.20000
AFIX 0
C25 1 0.690015 0.374423 0.738998 11.00000 0.02407 0.01735 =
0.01352 -0.00075 -0.00615 -0.00038
AFIX 43
H25 2 0.702604 0.414288 0.812244 11.00000 -1.20000
AFIX 0
C26 1 0.725086 0.462859 0.631946 11.00000 0.02393 0.01079 =
0.01643 -0.00139 -0.00693 -0.00069
AFIX 43
H26 2 0.765117 0.562785 0.633051 11.00000 -1.20000
AFIX 0
HKLF 4
REM Fuessen in P-1
REM wR2 = 0.0480, GooF = S = 1.072, Restrained GooF = 1.072 for all data
REM R1 = 0.0228 for 3917 Fo > 4sig(Fo) and 0.0285 for all 4361 data
REM 158 parameters refined using 0 restraints
END
WGHT 0.0232 0.2423
REM Highest difference peak 1.153, deepest hole -1.493, 1-sigma level 0.181
Q1 1 0.4216 0.2023 0.0780 11.00000 0.05 1.15
Q2 1 0.4955 0.1374 0.1388 11.00000 0.05 1.02
Q3 1 0.4043 0.3041 0.1427 11.00000 0.05 0.96
Q4 1 0.3929 0.1987 0.2075 11.00000 0.05 0.92
Q5 1 0.4206 0.0955 0.1426 11.00000 0.05 0.77
Q6 1 0.3947 0.2569 0.0573 11.00000 0.05 0.76
Q7 1 0.7795 0.8805 0.4631 11.00000 0.05 0.76
Q8 1 0.5315 0.0963 0.2563 11.00000 0.05 0.75
Q9 1 0.3095 0.2728 0.1430 11.00000 0.05 0.74
Q10 1 0.9984 0.8285 0.4613 11.00000 0.05 0.73
;
_shelx_res_checksum 29663
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Au Au1 0.40613(2) 0.19800(2) 0.14237(2) 0.01475(4) Uani d 1 . .
Br Br1 0.70783(4) 0.20253(4) 0.04441(3) 0.01937(7) Uani d 1 . .
Br Br2 0.10288(4) 0.19977(4) 0.24127(3) 0.01916(7) Uani d 1 . .
Br Br3 0.87521(4) 0.80705(4) 0.45816(3) 0.01607(7) Uani d 1 . .
Br Br4 0.61910(4) 0.20705(4) 0.37952(3) 0.01548(7) Uani d 1 . .
N N11 0.7993(3) 0.5993(3) 0.3080(2) 0.0148(5) Uani d 1 . .
H H11 0.777(5) 0.537(5) 0.372(4) 0.023(10) Uiso d 1 . .
C C12 0.8486(4) 0.7439(4) 0.3104(3) 0.0136(6) Uani d 1 . .
C C13 0.8796(4) 0.8381(4) 0.2066(3) 0.0166(6) Uani d 1 . .
H H13 0.915444 0.939910 0.207838 0.020 Uiso calc 1 . .
C C14 0.8574(4) 0.7810(4) 0.1010(3) 0.0169(6) Uani d 1 . .
H H14 0.874796 0.845044 0.029191 0.020 Uiso calc 1 . .
C C15 0.8098(4) 0.6307(4) 0.0997(3) 0.0185(7) Uani d 1 . .
H H15 0.797788 0.589640 0.026693 0.022 Uiso calc 1 . .
C C16 0.7804(4) 0.5419(4) 0.2048(3) 0.0192(7) Uani d 1 . .
H H16 0.746428 0.439010 0.205056 0.023 Uiso calc 1 . .
N N21 0.7050(3) 0.4137(3) 0.5260(2) 0.0139(5) Uani d 1 . .
C C22 0.6507(4) 0.2726(4) 0.5288(3) 0.0133(6) Uani d 1 . .
C C23 0.6153(4) 0.1734(4) 0.6295(3) 0.0163(6) Uani d 1 . .
H H23 0.578118 0.072941 0.624963 0.020 Uiso calc 1 . .
C C24 0.6360(4) 0.2260(4) 0.7371(3) 0.0177(6) Uani d 1 . .
H H24 0.613599 0.161686 0.808677 0.021 Uiso calc 1 . .
C C25 0.6900(4) 0.3744(4) 0.7390(3) 0.0183(6) Uani d 1 . .
H H25 0.702604 0.414288 0.812244 0.022 Uiso calc 1 . .
C C26 0.7251(4) 0.4629(4) 0.6319(3) 0.0169(6) Uani d 1 . .
H H26 0.765117 0.562785 0.633051 0.020 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
Au1 0.01907(6) 0.01413(7) 0.01280(6) -0.00329(4) -0.00677(4) 0.00052(4)
Br1 0.02015(15) 0.02330(17) 0.01494(15) -0.00386(12) -0.00459(12) -0.00038(12)
Br2 0.01936(15) 0.02198(17) 0.01792(16) -0.00588(12) -0.00596(12) -0.00229(12)
Br3 0.01851(14) 0.01701(16) 0.01330(14) -0.00387(11) -0.00431(11) -0.00125(11)
Br4 0.01940(14) 0.01518(15) 0.01382(15) -0.00519(11) -0.00620(11) -0.00023(11)
N11 0.0184(12) 0.0133(13) 0.0127(13) -0.0013(10) -0.0049(10) 0.0030(10)
C12 0.0130(13) 0.0140(15) 0.0132(14) -0.0003(11) -0.0035(11) -0.0005(11)
C13 0.0175(14) 0.0155(16) 0.0162(15) -0.0063(12) -0.0014(12) -0.0001(12)
C14 0.0177(14) 0.0179(16) 0.0150(15) -0.0039(12) -0.0043(12) 0.0063(12)
C15 0.0237(16) 0.0185(16) 0.0131(15) -0.0015(13) -0.0050(12) -0.0020(12)
C16 0.0261(16) 0.0146(16) 0.0186(16) -0.0032(13) -0.0091(13) 0.0007(12)
N21 0.0193(12) 0.0103(12) 0.0121(12) -0.0014(10) -0.0047(10) 0.0011(9)
C22 0.0135(13) 0.0134(15) 0.0130(14) -0.0003(11) -0.0037(11) -0.0032(11)
C23 0.0183(14) 0.0126(15) 0.0176(16) -0.0038(12) -0.0031(12) -0.0001(12)
C24 0.0224(15) 0.0154(16) 0.0129(15) -0.0023(12) -0.0008(12) 0.0013(12)
C25 0.0241(16) 0.0173(16) 0.0135(15) -0.0004(13) -0.0061(12) -0.0007(12)
C26 0.0239(15) 0.0108(15) 0.0164(16) -0.0007(12) -0.0069(12) -0.0014(12)
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'
Au Au -2.0133 8.8022 '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
Br1 Au1 Br2 . . 178.713(12) y
C12 N11 C16 . . 121.2(3) y
C12 N11 H11 . . 123(3) ?
C16 N11 H11 . . 116(3) ?
N11 C12 C13 . . 120.5(3) ?
N11 C12 Br3 . . 116.9(2) ?
C13 C12 Br3 . . 122.6(2) ?
C12 C13 C14 . . 118.5(3) ?
C12 C13 H13 . . 120.7 ?
C14 C13 H13 . . 120.7 ?
C13 C14 C15 . . 120.1(3) ?
C13 C14 H14 . . 119.9 ?
C15 C14 H14 . . 119.9 ?
C16 C15 C14 . . 119.2(3) ?
C16 C15 H15 . . 120.4 ?
C14 C15 H15 . . 120.4 ?
N11 C16 C15 . . 120.4(3) ?
N11 C16 H16 . . 119.8 ?
C15 C16 H16 . . 119.8 ?
C22 N21 C26 . . 116.2(3) y
N21 C22 C23 . . 125.6(3) ?
N21 C22 Br4 . . 115.6(2) ?
C23 C22 Br4 . . 118.8(2) ?
C22 C23 C24 . . 117.4(3) ?
C22 C23 H23 . . 121.3 ?
C24 C23 H23 . . 121.3 ?
C23 C24 C25 . . 119.1(3) ?
C23 C24 H24 . . 120.5 ?
C25 C24 H24 . . 120.5 ?
C26 C25 C24 . . 118.6(3) ?
C26 C25 H25 . . 120.7 ?
C24 C25 H25 . . 120.7 ?
N21 C26 C25 . . 123.1(3) ?
N21 C26 H26 . . 118.4 ?
C25 C26 H26 . . 118.4 ?
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
Au1 Br1 . 2.3790(4) y
Au1 Br2 . 2.3851(4) y
Br3 C12 . 1.864(3) ?
Br4 C22 . 1.904(3) ?
N11 C12 . 1.345(4) y
N11 C16 . 1.346(4) y
N11 H11 . 0.87(4) ?
C12 C13 . 1.380(4) ?
C13 C14 . 1.381(5) ?
C13 H13 . 0.9500 ?
C14 C15 . 1.383(5) ?
C14 H14 . 0.9500 ?
C15 C16 . 1.368(5) ?
C15 H15 . 0.9500 ?
C16 H16 . 0.9500 ?
N21 C22 . 1.327(4) y
N21 C26 . 1.352(4) y
C22 C23 . 1.380(4) ?
C23 C24 . 1.382(5) ?
C23 H23 . 0.9500 ?
C24 C25 . 1.392(5) ?
C24 H24 . 0.9500 ?
C25 C26 . 1.385(5) ?
C25 H25 . 0.9500 ?
C26 H26 . 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
N11 H11 N21 . 0.87(4) 1.99(4) 2.861(4) 174(4) yes
C16 H16 Br1 . 0.95 2.88 3.675(3) 141.9 yes
C13 H13 Br2 1_665 0.95 2.93 3.853(3) 163.4 yes
C26 H26 Br2 2_666 0.95 2.99 3.843(3) 150.6 yes
C26 H26 Br3 . 0.95 2.87 3.616(3) 136.3 yes
C16 H16 Br4 . 0.95 2.83 3.584(3) 137.4 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
C16 N11 C12 C13 . . . . 0.6(4) ?
C16 N11 C12 Br3 . . . . -178.5(2) ?
N11 C12 C13 C14 . . . . 0.5(4) ?
Br3 C12 C13 C14 . . . . 179.6(2) ?
C12 C13 C14 C15 . . . . -1.8(5) ?
C13 C14 C15 C16 . . . . 1.9(5) ?
C12 N11 C16 C15 . . . . -0.6(5) ?
C14 C15 C16 N11 . . . . -0.7(5) ?
C26 N21 C22 C23 . . . . -0.6(4) ?
C26 N21 C22 Br4 . . . . 178.9(2) ?
N21 C22 C23 C24 . . . . 0.9(5) ?
Br4 C22 C23 C24 . . . . -178.7(2) ?
C22 C23 C24 C25 . . . . 0.3(4) ?
C23 C24 C25 C26 . . . . -1.5(5) ?
C22 N21 C26 C25 . . . . -0.7(4) ?
C24 C25 C26 N21 . . . . 1.7(5) ?