#------------------------------------------------------------------------------
#$Date: 2023-12-07 12:52:37 +0100 (Thu, 07 Dec 2023) $
#$Revision: 288153 $
#$URL: svn://www.crystallography.net/cod/cif/2/02/29/2022911.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_2022911
loop_
_publ_author_name
'Döring, Cindy'
'Jones, Peter G.'
_publ_section_title
;
Crystal structures of five halido gold complexes involving piperidine or
pyrrolidine as ligands or (protonated) as cations.
;
_journal_coeditor_code YZ2040
_journal_issue 'Pt 11'
_journal_name_full
'Acta crystallographica. Section E, Crystallographic communications'
_journal_page_first 1017
_journal_page_last 1027
_journal_paper_doi 10.1107/S205698902300854X
_journal_volume 79
_journal_year 2023
_chemical_formula_iupac '[Au Cl3 (C5 H11 N)]'
_chemical_formula_moiety 'C5 H11 Au Cl3 N'
_chemical_formula_sum 'C5 H11 Au Cl3 N'
_chemical_formula_weight 388.46
_chemical_name_systematic
;
Trichlorido(piperidine-\kN)gold(III)
;
_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 mixed
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-2018/3
_cell_angle_alpha 90
_cell_angle_beta 93.5133(16)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 8.47646(16)
_cell_length_b 6.57436(11)
_cell_length_c 16.9961(3)
_cell_measurement_reflns_used 13188
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 30.6850
_cell_measurement_theta_min 2.3960
_cell_volume 945.37(3)
_computing_cell_refinement
;
CrysAlisPro, Version 1.171.37.35 (Agilent, 2014)
;
_computing_data_collection
;
CrysAlisPro, Version 1.171.37.35 (Agilent, 2014)
;
_computing_data_reduction
;
CrysAlisPro, Version 1.171.37.35 (Agilent, 2014)
;
_computing_molecular_graphics
;
Siemens XP (Siemens, 1994)
;
_computing_publication_material
;
SHELXL2018/3 (Sheldrick, 2015)
;
_computing_structure_refinement
;
SHELXL2018/3 (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 0.992
_diffrn_measured_fraction_theta_max 0.936
_diffrn_measurement_device_type 'Oxford Diffraction Xcalibur, Eos'
_diffrn_measurement_method '\w scan'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0374
_diffrn_reflns_av_unetI/netI 0.0225
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_k_max 9
_diffrn_reflns_limit_k_min -9
_diffrn_reflns_limit_l_max 24
_diffrn_reflns_limit_l_min -23
_diffrn_reflns_number 24604
_diffrn_reflns_theta_full 30.000
_diffrn_reflns_theta_max 31.093
_diffrn_reflns_theta_min 2.401
_diffrn_source 'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu 16.340
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.68875
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Agilent, 2014)
;
_exptl_crystal_colour yellow
_exptl_crystal_density_diffrn 2.729
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description irregular
_exptl_crystal_F_000 712
_exptl_crystal_size_max 0.17
_exptl_crystal_size_mid 0.17
_exptl_crystal_size_min 0.15
_refine_diff_density_max 0.923
_refine_diff_density_min -0.800
_refine_ls_extinction_coef 0.00109(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2018/3 (Sheldrick, 2015)
;
_refine_ls_goodness_of_fit_ref 1.132
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 96
_refine_ls_number_reflns 2853
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.132
_refine_ls_R_factor_all 0.0187
_refine_ls_R_factor_gt 0.0165
_refine_ls_shift/su_max 0.003
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0085P)^2^+0.3159P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0292
_refine_ls_wR_factor_ref 0.0296
_reflns_number_gt 2690
_reflns_number_total 2853
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file yz2040sup1.cif
_cod_data_source_block 3
_cod_depositor_comments
'Adding full bibliography for 2022910--2022914.cif.'
_cod_original_cell_volume 945.36(3)
_cod_original_sg_symbol_H-M 'P 21/c'
_cod_database_code 2022911
_cod_database_fobs_code 2022911
_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 0.168
_shelx_estimated_absorpt_t_max 0.193
_shelx_hkl_file
;
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0 0 -3-205.879 263.284 3
0 0 -3 473.862 244.430 14
0 0 3 258.886 250.238 3
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0 0 -5 748.845 318.740 2
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0 0 -5 364.294 337.512 13
0 0 5 1197.00 463.403 14
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0 0 -5 2282.05 625.506 3
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10 4 -5 25328.7 3263.35 3
10 -4 -5 23321.9 2989.62 8
-10 4 4 90822.8 6466.81 9
-10 -4 4 85213.8 6542.57 2
10 -4 -4 92609.1 5945.46 8
10 4 -4 82025.1 6507.95 15
10 4 -4 86152.3 6128.11 3
10 4 -3 12189.4 2281.04 3
-10 4 3 12014.8 2347.88 9
10 4 -3 11136.9 2093.42 1
10 4 -3 9275.38 2333.15 15
10 -4 -3 11791.2 2112.18 8
-10 -4 3 13110.2 2498.97 2
10 4 -2 415.254 1007.51 3
-10 4 2 1750.49 1194.18 9
10 -4 -2 3277.72 1454.48 16
10 4 -2 2262.42 1077.63 1
10 4 -2 311.452 1193.15 15
10 -4 -2-870.303 878.797 8
-10 -4 2 1577.00 1241.72 2
10 4 -1 9364.37 1920.18 3
-10 4 1 15877.2 2795.67 9
10 -4 -1 17299.3 2504.21 16
10 4 -1 15087.7 2889.22 15
10 4 -1 14243.0 2414.35 1
10 -4 -1 10086.1 1821.91 8
-10 -4 1 14908.4 2641.11 2
-10 4 0 83529.3 6188.44 9
10 4 0 86375.1 5840.67 1
10 -4 0 91296.8 5997.64 16
10 -4 0 84039.6 5278.02 8
-10 -4 0 88137.4 6521.12 2
10 4 0 89377.0 6681.82 15
10 4 0 85756.4 6023.86 3
10 4 1 6562.65 1716.91 3
-10 4 -1 7504.19 1886.34 10
-10 4 -1 9291.15 2148.07 9
10 -4 1 4261.64 1473.34 16
10 4 1 5695.05 1830.09 15
10 4 1 6704.95 1808.44 1
-10 -4 -1 6528.90 1718.36 2
10 4 2 117.517 1032.44 3
10 -4 2 1955.22 1313.50 16
10 4 2 1979.26 1567.78 15
10 4 2-276.158 903.515 1
-10 -4 -2 2649.45 1457.59 2
10 4 3 30578.1 3543.24 3
10 -4 3 25403.3 3295.71 16
10 4 3 29276.4 3760.44 15
10 4 3 28941.1 3407.76 1
-10 -4 -3 26081.1 3523.20 2
10 -4 4 145685. 8122.81 16
-10 -4 -4 133879. 8251.85 2
10 4 4 126714. 8146.40 15
10 -4 5 34590.1 3903.89 16
10 4 5 33272.4 4052.59 15
-10 -4 -5 33099.4 3951.88 2
10 4 6-1446.22 1310.36 15
-10 -4 -6-266.550 1052.08 2
10 4 7 6944.59 1983.85 15
-10 -4 -7 2678.48 1577.00 2
10 -5 -3 79913.8 5570.37 8
10 -5 -2 5142.46 1513.18 8
10 -5 0 3113.97 1415.79 16
10 -5 1 75310.0 5657.98 16
10 -5 2 8720.36 2080.81 16
-11 0 9 761.184 865.431 9
-11 0 8 49445.4 4717.82 2
-11 0 8 47701.0 4672.44 9
11 0 -7-99.5253 1155.89 3
-11 0 7 1116.40 1176.57 9
11 0 -7 1398.93 1476.51 15
-11 0 7 770.116 1102.11 2
11 0 -6 6014.27 1821.36 3
-11 0 6 5446.28 1790.36 9
11 0 -6 13782.7 2415.06 15
-11 0 6 10894.4 2264.85 2
11 0 -5 521.227 1252.86 3
-11 0 5 2085.20 1458.76 9
11 0 -5 412.236 1109.08 15
-11 0 5 534.349 932.881 2
-11 0 4 115333. 7435.50 9
-11 0 4 107518. 6863.70 2
11 0 -4 116787. 7451.85 15
11 0 -4 124627. 7478.53 3
11 0 -3-129.891 1099.36 3
-11 0 3-468.614 988.231 9
11 0 -3-2159.22 1211.83 15
-11 0 3 72.5505 938.709 2
11 0 -2 16235.9 2599.80 3
-11 0 2 16652.7 2678.18 9
11 0 -2 18320.3 2895.06 15
-11 0 2 18058.7 2611.19 2
11 0 -1-603.717 1026.35 3
-11 0 1 599.470 1142.00 9
11 0 -1 732.952 1092.87 15
-11 0 1-739.468 1008.78 2
-11 0 0 96857.3 6696.89 9
-11 0 0 92254.7 5988.83 2
11 0 0 105705. 6696.17 15
11 0 0 96732.4 6525.39 3
11 0 1 169.147 966.234 3
-11 0 -1 1075.91 1107.11 9
11 0 1 504.703 964.666 15
-11 0 -1 460.664 891.889 2
11 0 2 1550.99 1264.54 3
-11 0 -2-161.670 949.474 9
11 0 3 993.521 777.961 1
-11 0 -3 292.927 969.614 9
-11 0 -4 128530. 6762.90 10
-11 0 -4 128097. 7663.75 9
11 0 4 117081. 6317.23 1
-11 0 -5 534.868 894.837 10
11 0 5 391.210 712.669 1
-11 0 -5-691.615 1184.19 9
-11 0 -6 1774.80 1091.17 10
-11 0 -6 4033.40 1402.79 9
11 0 6 1584.73 1012.88 1
-11 0 -7 1426.91 1101.48 10
11 0 7 543.725 775.272 1
-11 0 -8 134069. 7250.10 10
11 0 8 127060. 6986.14 1
-11 0 -9-1289.29 1086.90 10
11 -1 -8 7535.59 2094.13 3
-11 1 8 9758.37 2179.14 9
-11 -1 8 7344.71 2002.00 9
-11 1 8 9583.31 2100.97 2
-11 1 7 56619.3 4897.60 2
-11 1 7 59906.4 5231.20 9
-11 -1 7 52285.8 4924.44 9
-11 -1 7 47558.0 4736.67 2
11 1 -7 64224.9 5691.02 15
11 -1 -7 58614.6 5188.30 3
11 -1 -6 30910.8 3753.33 3
11 1 -6 31547.1 3801.08 3
-11 1 6 41234.9 4246.26 9
-11 -1 6 29643.6 3691.63 9
11 1 -6 32271.5 3985.50 15
-11 1 6 34500.3 3780.10 2
-11 -1 6 39162.2 4180.83 2
11 -1 -5 542.784 1209.12 3
11 1 -5-510.963 1176.80 3
-11 1 5 2726.21 1382.59 9
-11 -1 5 793.591 988.837 9
11 1 -5 2411.86 1613.96 15
-11 1 5 2125.94 1315.12 2
-11 -1 5 3216.06 1272.27 2
11 -1 -4 501.726 995.692 3
11 1 -4-192.670 939.737 3
-11 1 4 3836.98 1697.81 9
-11 -1 4-442.913 1168.36 9
11 -1 -4 2511.97 1439.52 15
11 1 -4 2113.25 1469.76 15
-11 1 4 1849.46 1161.22 2
-11 -1 4 2697.35 1414.67 2
-11 1 3 101743. 6345.97 2
-11 1 3 100775. 6861.54 9
-11 -1 3 101397. 6684.89 2
11 -1 -3 109319. 6887.45 15
11 1 -3 104581. 7101.47 15
11 -1 -3 101589. 6775.16 3
11 1 -3 106065. 6901.23 3
11 -1 -2 37725.6 4128.03 3
11 1 -2 37719.8 4058.98 3
-11 1 2 38710.1 3793.12 2
-11 1 2 49847.5 4647.67 9
-11 -1 2 42237.0 4109.62 2
11 -1 -2 36320.6 3808.53 15
11 1 -2 42768.8 4286.15 15
11 -1 -1 29403.9 3538.65 3
11 1 -1 30401.7 3594.44 3
-11 1 1 32672.6 3852.19 9
11 1 -1 32078.3 3103.99 1
11 -1 -1 32703.1 3670.58 15
11 1 -1 30310.9 3734.71 15
-11 1 1 34577.3 3416.17 2
-11 -1 1 26627.0 3269.68 2
11 1 0 2627.76 1367.69 3
-11 1 0 5113.34 1807.09 9
11 1 0 5071.75 1623.98 15
11 1 0 2466.10 1016.53 1
-11 -1 0 2413.11 1229.42 2
-11 1 -1 45588.4 4452.20 9
-11 -1 -1 36282.5 4036.93 9
11 1 1 43204.3 3626.76 1
11 1 1 44818.7 4399.31 15
-11 -1 -1 37390.4 3793.76 2
11 -1 1 44085.4 4307.29 3
11 1 1 46543.3 4442.96 3
11 -1 2 22205.3 3021.76 3
11 1 2 25946.9 3344.13 3
-11 1 -2 29675.0 3602.15 9
-11 -1 -2 24874.2 3347.21 9
11 1 2 27716.6 3417.13 15
-11 -1 -2 21697.1 2898.95 2
11 1 2 26096.7 2853.30 1
11 -1 3 20064.8 2942.12 3
11 1 3 20164.2 3001.91 3
-11 1 -3 20953.4 2688.79 10
-11 1 -3 24635.0 3258.94 9
-11 -1 -3 16878.7 2685.21 9
11 1 3 13433.5 2392.10 15
11 1 3 11372.3 1929.64 1
11 1 4 5291.82 1400.68 1
-11 1 -4 3226.80 1227.42 10
-11 1 -4 6490.18 1762.12 9
-11 -1 -4 6506.47 1720.54 9
-11 1 -5 73328.2 5243.16 10
-11 1 -5 72416.1 5595.63 9
-11 -1 -5 73847.1 5703.99 9
11 1 5 72333.5 4998.97 1
-11 1 -6 51167.5 4347.23 10
11 1 6 38930.9 3680.00 1
-11 1 -7 63715.3 5007.52 10
11 1 7 65333.1 4865.78 1
11 -1 8 435.504 931.010 1
11 -2 -9 117338. 7669.40 3
11 -2 -8 19255.4 3132.76 3
11 -2 -7 10101.5 2251.18 3
11 -2 -6 12116.9 2619.47 3
-11 -2 5 117193. 7700.71 2
11 2 -5 137233. 8542.88 15
11 -2 -5 134262. 7970.80 3
11 -2 -4 3662.27 1270.44 3
11 2 -4 8203.72 1783.30 1
11 2 -4 3844.70 1950.36 15
-11 -2 4 4976.02 1698.68 2
11 -2 -3 23979.4 3194.39 3
11 2 -3 22954.8 2755.39 1
11 2 -3 23774.1 3350.74 15
-11 -2 3 24644.6 3377.49 2
11 -2 -2 1409.60 1007.11 3
11 2 -2 2059.30 1385.16 15
11 2 -2 747.424 1104.91 1
-11 -2 2 2304.27 1492.63 2
11 2 -1 106854. 6220.61 1
-11 -2 1 105623. 6935.99 2
11 2 -1 100922. 7109.96 15
11 -2 -1 91283.7 6311.15 3
11 2 -1 103445. 6832.66 3
11 -2 0 22440.5 3027.35 3
11 2 0 24128.2 3390.55 15
11 2 0 20371.6 2703.58 1
-11 -2 0 19031.6 2862.87 2
11 -2 1 22678.8 3027.62 3
11 2 1 26638.0 3607.60 15
11 2 1 25381.2 2941.19 1
-11 -2 -1 31695.1 3785.69 2
11 -2 2 3609.48 1480.85 3
-11 2 -2 4257.75 1468.79 10
11 2 2 6175.86 1841.40 15
11 2 2 5960.72 1545.02 1
-11 -2 -2 3305.71 1446.95 2
-11 2 -3 75316.2 5454.47 10
-11 -2 -3 74946.2 5622.80 2
11 2 3 70532.1 5088.62 1
11 2 3 75762.7 5861.55 15
11 -2 3 73609.0 5572.42 3
-11 2 -4 5053.07 1587.24 10
11 2 4 7023.66 1921.26 15
-11 -2 -4 8355.42 1923.37 2
11 2 4 9451.15 1979.20 1
11 2 5 33200.0 3470.46 1
11 3 -4 9812.98 1977.81 1
11 3 -3 11925.6 2180.30 1
11 3 -2 70221.3 5171.46 1
11 3 -1 1233.36 1118.44 15
11 3 -1 2631.48 1432.72 1
11 3 0 1961.63 1307.98 15
11 3 0 3016.15 1381.88 1
-11 -3 0-758.667 914.763 2
11 3 1 24589.5 3586.98 15
11 3 1 38154.6 3786.48 1
-11 -3 -1 31342.0 3801.79 2
-11 -3 -2 128998. 8006.63 2
11 3 2 129669. 8243.74 15
11 3 3 11517.7 2466.60 15
-11 -3 -3 19849.2 3098.93 2
11 3 4-235.053 1269.75 15
-11 -3 -4-441.733 898.425 2
11 3 5 10972.8 2379.81 15
-11 -3 -5 6976.93 1862.72 2
11 3 6 46634.1 4645.17 15
11 -4 -2 6506.46 1603.88 8
11 -4 0 112024. 7000.86 16
11 -4 1 15365.8 2562.20 16
12 0 -4 94123.3 6911.59 15
12 0 -3 131.455 1328.27 15
-12 0 3-335.608 849.993 2
12 0 -2 21619.3 3291.82 15
-12 0 2 20392.8 2963.06 2
12 0 -1-386.069 1258.40 15
12 -1 -4 12497.9 2624.46 15
-12 1 4 9692.59 2074.38 2
12 1 -2 20839.8 3219.33 15
12 1 -1 32639.2 4121.45 15
-12 -1 1 30386.5 3704.62 2
12 1 0 1647.04 1375.34 15
-12 -1 0 6401.61 1793.65 2
0 0 0 0.00 0.00 0
TITL Bruegge in P2(1)/c
REM P2(1)/c (#14 in standard setting)
CELL 0.71073 8.476459 6.574355 16.996055 90.0000 93.5133 90.0000
ZERR 5.00 0.000079 0.000054 0.000150 0.0000 0.0008 0.0000
LATT 1
SYMM -x, y+1/2,-z+1/2
SFAC C H N Cl Au
UNIT 25.00 55.00 5.00 15.00 5.00
TREF
HKLF 4
END
;
_shelx_hkl_checksum 26750
_shelx_res_file
;
TITL Bruegge in P2(1)/c
shelx.res
created by SHELXL-2018/3 at 10:11:50 on 17-Sep-2021
CELL 0.71073 8.476459 6.574355 16.996055 90.0000 93.5133 90.0000
ZERR 4.00 0.000160 0.000108 0.000300 0.0000 0.0016 0.0000
LATT 1
SYMM -x, y+1/2,-z+1/2
SFAC C H N Cl Au
UNIT 20.00 44.00 4.00 12.00 4.00
L.S. 8
FMAP 2
PLAN 10
SIZE 0.17 0.17 0.15
TEMP -173
ACTA 60
CONF
OMIT 1 0 0
EQIV $1 -x+1, y-1/2, -z+3/2
EQIV $2 -x+1, -y+1, -z+2
EQIV $3 x+1, y-1, z
EQIV $4 x+1, y, z
EQIV $5 -x+1, y+1/2, -z+3/2
EQIV $6 -x+1, -y+2, -z+2
HTAB N11 Cl3
HTAB N11 Cl3_$1
HTAB C12 Cl1_$2
HTAB C14 Cl1_$3
HTAB C12 Cl2_$2
HTAB C13 Cl3_$1
HTAB C15 Cl3_$4
HTAB C16 Cl3_$5
RTAB DIST Au1 Cl2_$2
RTAB DIST Au1 Cl3_$5
RTAB DIST Cl1 Cl2_$6
RTAB ANGL Au1 Cl1 Cl2_$6
RTAB DIST Cl1 Cl3_$5
RTAB ANGL Au1 Cl1 Cl3_$5
RTAB DIST Cl2 Cl1_$6
RTAB ANGL Au1 Cl2 Cl1_$6
RTAB DIST Cl2 Cl2_$2
RTAB ANGL Au1 Cl2 Cl2_$2
RTAB DIST Cl3 Cl1_$1
RTAB ANGL Au1 Cl3 Cl1_$1
RTAB DIST Cl3 Cl3_$1
RTAB ANGL Au1 Cl3 Cl3_$1
RTAB DIST Cl3 Cl3_$5
RTAB ANGL Au1 Cl3 Cl3_$5
RTAB ANGL Au1 Cl3 Au1_$1
WGHT 0.008500 0.315900
EXTI 0.001091
FVAR 3.10461
AU1 5 0.503404 0.604927 0.868019 11.00000 0.00840 0.00890 =
0.01038 0.00010 0.00037 0.00117
CL1 4 0.288096 0.810005 0.879428 11.00000 0.01489 0.01817 =
0.01681 -0.00099 0.00079 0.00777
CL2 4 0.625331 0.746856 0.977719 11.00000 0.01549 0.01650 =
0.01505 -0.00423 -0.00194 0.00080
CL3 4 0.388600 0.466654 0.755444 11.00000 0.01273 0.01595 =
0.01552 -0.00450 -0.00256 0.00156
N11 3 0.697653 0.421523 0.852138 11.00000 0.00872 0.00849 =
0.01228 -0.00021 -0.00085 0.00094
H01 2 0.659321 0.348159 0.813914 11.00000 0.02300
C12 1 0.739091 0.283710 0.920654 11.00000 0.01689 0.01332 =
0.01862 0.00644 0.00319 0.00346
AFIX 23
H12A 2 0.647301 0.196029 0.930291 11.00000 -1.20000
H12B 2 0.763017 0.366729 0.968501 11.00000 -1.20000
AFIX 0
C13 1 0.880904 0.150900 0.905544 11.00000 0.01584 0.01416 =
0.02016 0.00190 -0.00256 0.00564
AFIX 23
H13A 2 0.851842 0.054401 0.862344 11.00000 -1.20000
H13B 2 0.910481 0.070664 0.953489 11.00000 -1.20000
AFIX 0
C14 1 1.022577 0.277430 0.883389 11.00000 0.01203 0.01782 =
0.02663 -0.00231 -0.00305 0.00453
AFIX 23
H14A 2 1.059299 0.364332 0.928430 11.00000 -1.20000
H14B 2 1.110477 0.186397 0.870636 11.00000 -1.20000
AFIX 0
C15 1 0.975079 0.409628 0.812495 11.00000 0.00976 0.01772 =
0.02502 0.00113 0.00390 0.00252
AFIX 23
H15A 2 0.946403 0.321752 0.766522 11.00000 -1.20000
H15B 2 1.065906 0.495127 0.799304 11.00000 -1.20000
AFIX 0
C16 1 0.835716 0.545384 0.829011 11.00000 0.01132 0.01137 =
0.02140 0.00292 0.00526 0.00116
AFIX 23
H16A 2 0.867252 0.641410 0.872008 11.00000 -1.20000
H16B 2 0.804704 0.625874 0.781317 11.00000 -1.20000
AFIX 0
HKLF 4
REM Bruegge in P2(1)/c
REM wR2 = 0.0296, GooF = S = 1.132, Restrained GooF = 1.132 for all data
REM R1 = 0.0165 for 2690 Fo > 4sig(Fo) and 0.0187 for all 2853 data
REM 96 parameters refined using 0 restraints
END
WGHT 0.0085 0.3159
REM Highest difference peak 0.923, deepest hole -0.800, 1-sigma level 0.137
Q1 1 0.5040 0.4205 0.8728 11.00000 0.05 0.92
Q2 1 0.5348 0.6122 0.8130 11.00000 0.05 0.86
Q3 1 0.9037 0.4611 0.8278 11.00000 0.05 0.68
Q4 1 0.4849 0.6591 0.9089 11.00000 0.05 0.66
Q5 1 0.4964 0.8723 0.8581 11.00000 0.05 0.65
Q6 1 0.5104 0.5390 0.9097 11.00000 0.05 0.64
Q7 1 0.5672 0.6848 0.8494 11.00000 0.05 0.61
Q8 1 0.3334 0.9389 0.8222 11.00000 0.05 0.56
Q9 1 0.5181 -0.0042 0.8566 11.00000 0.05 0.56
Q10 1 0.1756 0.7614 0.8618 11.00000 0.05 0.49
;
_shelx_res_checksum 5744
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
Au Au1 0.50340(2) 0.60493(2) 0.86802(2) 0.00923(4) Uani d 1 . .
Cl Cl1 0.28810(7) 0.81001(9) 0.87943(4) 0.01663(12) Uani d 1 . .
Cl Cl2 0.62533(7) 0.74686(9) 0.97772(3) 0.01580(12) Uani d 1 . .
Cl Cl3 0.38860(7) 0.46665(9) 0.75544(3) 0.01487(12) Uani d 1 . .
N N11 0.6977(2) 0.4215(3) 0.85214(12) 0.0099(4) Uani d 1 . .
H H01 0.659(3) 0.348(4) 0.8139(18) 0.023(8) Uiso d 1 . .
C C12 0.7391(3) 0.2837(4) 0.92065(15) 0.0162(5) Uani d 1 . .
H H12A 0.647301 0.196029 0.930291 0.019 Uiso calc 1 . .
H H12B 0.763017 0.366729 0.968501 0.019 Uiso calc 1 . .
C C13 0.8809(3) 0.1509(4) 0.90554(16) 0.0169(5) Uani d 1 . .
H H13A 0.851842 0.054401 0.862344 0.020 Uiso calc 1 . .
H H13B 0.910481 0.070664 0.953489 0.020 Uiso calc 1 . .
C C14 1.0226(3) 0.2774(4) 0.88339(15) 0.0190(6) Uani d 1 . .
H H14A 1.059299 0.364332 0.928430 0.023 Uiso calc 1 . .
H H14B 1.110477 0.186397 0.870636 0.023 Uiso calc 1 . .
C C15 0.9751(3) 0.4096(4) 0.81249(16) 0.0174(5) Uani d 1 . .
H H15A 0.946403 0.321752 0.766522 0.021 Uiso calc 1 . .
H H15B 1.065906 0.495127 0.799304 0.021 Uiso calc 1 . .
C C16 0.8357(3) 0.5454(4) 0.82901(15) 0.0145(5) Uani d 1 . .
H H16A 0.867252 0.641410 0.872008 0.017 Uiso calc 1 . .
H H16B 0.804704 0.625874 0.781317 0.017 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 0.00840(5) 0.00890(5) 0.01038(5) 0.00117(3) 0.00037(3) 0.00010(3)
Cl1 0.0149(3) 0.0182(3) 0.0168(3) 0.0078(2) 0.0008(2) -0.0010(2)
Cl2 0.0155(3) 0.0165(3) 0.0150(3) 0.0008(2) -0.0019(2) -0.0042(2)
Cl3 0.0127(3) 0.0159(3) 0.0155(3) 0.0016(2) -0.0026(2) -0.0045(2)
N11 0.0087(10) 0.0085(10) 0.0123(10) 0.0009(8) -0.0009(8) -0.0002(7)
C12 0.0169(13) 0.0133(12) 0.0186(13) 0.0035(10) 0.0032(10) 0.0064(10)
C13 0.0158(13) 0.0142(12) 0.0202(13) 0.0056(10) -0.0026(10) 0.0019(10)
C14 0.0120(13) 0.0178(13) 0.0266(14) 0.0045(10) -0.0031(11) -0.0023(11)
C15 0.0098(12) 0.0177(13) 0.0250(14) 0.0025(10) 0.0039(10) 0.0011(10)
C16 0.0113(12) 0.0114(11) 0.0214(13) 0.0012(10) 0.0053(10) 0.0029(10)
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'
Cl Cl 0.1484 0.1585 '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'
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
N11 Au1 Cl2 . . 91.19(6) y
N11 Au1 Cl3 . . 87.73(6) y
Cl2 Au1 Cl3 . . 177.91(2) y
N11 Au1 Cl1 . . 177.36(6) y
Cl2 Au1 Cl1 . . 90.77(2) y
Cl3 Au1 Cl1 . . 90.25(2) y
C16 N11 C12 . . 112.49(19) y
C16 N11 Au1 . . 110.96(14) ?
C12 N11 Au1 . . 113.61(15) ?
N11 C12 C13 . . 111.5(2) ?
C12 C13 C14 . . 111.8(2) ?
C15 C14 C13 . . 109.4(2) ?
C14 C15 C16 . . 111.1(2) ?
N11 C16 C15 . . 110.96(19) ?
C16 N11 H01 . . 112(2) ?
C12 N11 H01 . . 108(2) ?
Au1 N11 H01 . . 99(2) ?
N11 C12 H12A . . 109.3 ?
C13 C12 H12A . . 109.3 ?
N11 C12 H12B . . 109.3 ?
C13 C12 H12B . . 109.3 ?
H12A C12 H12B . . 108.0 ?
C12 C13 H13A . . 109.3 ?
C14 C13 H13A . . 109.3 ?
C12 C13 H13B . . 109.3 ?
C14 C13 H13B . . 109.3 ?
H13A C13 H13B . . 107.9 ?
C15 C14 H14A . . 109.8 ?
C13 C14 H14A . . 109.8 ?
C15 C14 H14B . . 109.8 ?
C13 C14 H14B . . 109.8 ?
H14A C14 H14B . . 108.2 ?
C14 C15 H15A . . 109.4 ?
C16 C15 H15A . . 109.4 ?
C14 C15 H15B . . 109.4 ?
C16 C15 H15B . . 109.4 ?
H15A C15 H15B . . 108.0 ?
N11 C16 H16A . . 109.4 ?
C15 C16 H16A . . 109.4 ?
N11 C16 H16B . . 109.4 ?
C15 C16 H16B . . 109.4 ?
H16A C16 H16B . . 108.0 ?
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 N11 . 2.0718(19) y
Au1 Cl2 . 2.2757(6) y
Au1 Cl3 . 2.2817(6) y
Au1 Cl1 . 2.2868(6) y
N11 C16 . 1.498(3) ?
N11 C12 . 1.500(3) ?
C12 C13 . 1.520(3) ?
C13 C14 . 1.527(4) ?
C14 C15 . 1.520(4) ?
C15 C16 . 1.520(3) ?
N11 H01 . 0.86(3) ?
C12 H12A . 0.9900 ?
C12 H12B . 0.9900 ?
C13 H13A . 0.9900 ?
C13 H13B . 0.9900 ?
C14 H14A . 0.9900 ?
C14 H14B . 0.9900 ?
C15 H15A . 0.9900 ?
C15 H15B . 0.9900 ?
C16 H16A . 0.9900 ?
C16 H16B . 0.9900 ?
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 H01 Cl3 . 0.86(3) 2.57(3) 3.021(2) 114(2) yes
N11 H01 Cl3 2_646 0.86(3) 2.79(3) 3.558(2) 150(3) yes
C12 H12B Cl1 3_667 0.99 2.89 3.475(3) 118.6 ?
C14 H14B Cl1 1_645 0.99 2.90 3.812(3) 154.3 ?
C12 H12A Cl2 3_667 0.99 2.89 3.636(3) 132.5 ?
C13 H13A Cl3 2_646 0.99 2.83 3.661(3) 142.3 ?
C15 H15B Cl3 1_655 0.99 2.88 3.713(3) 141.7 ?
C16 H16B Cl3 2_656 0.99 2.82 3.607(2) 136.6 ?
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 . . . . -53.6(3) ?
Au1 N11 C12 C13 . . . . 179.30(16) y
N11 C12 C13 C14 . . . . 54.2(3) ?
C12 C13 C14 C15 . . . . -55.8(3) ?
C13 C14 C15 C16 . . . . 57.1(3) ?
C12 N11 C16 C15 . . . . 54.9(3) ?
Au1 N11 C16 C15 . . . . -176.54(17) y
C14 C15 C16 N11 . . . . -57.0(3) ?