##############################################################################
# #
# This CIF contains the data in a paper accepted for publication in #
# Acta Crystallographica Section E. It conforms to the requirements of #
# Notes for Authors for Acta Crystallographica Section E, and has been #
# peer reviewed under the auspices of the IUCr Commission on Journals. #
# #
# Full details of the Crystallographic Information File format #
# are given in the paper "The Crystallographic Information File (CIF): #
# a New Standard Archive File for Crystallography" by S. R. Hall, F. H. #
# Allen and I. D. Brown [Acta Cryst. (1991), A47, 655-685]. #
# #
# The current version of the core CIF dictionary is obtainable from #
# ftp://ftp.iucr.org/pub/cif_core.dic. #
# #
# Software is freely available for graphical display of the structure(s) #
# in this CIF. For information consult the CIF software page #
# http://www.iucr.org/resources/cif/software. #
# #
# This file may be used for bona fide research purposes within the #
# scientific community so long as proper attribution is given to the journal #
# article from which it was obtained. #
# #
##############################################################################
data_1
_audit_creation_method 'SHELXL-2019/3'
_chemical_name_systematic
;
Trichlorido(4-methylpiperidine)gold(III)
;
_chemical_name_common ?
_chemical_formula_moiety 'C6 H13 Au Cl3 N'
_chemical_formula_sum 'C6 H13 Au Cl3 N'
_chemical_formula_iupac '[Au Cl3 (C6 H13 N)]'
_chemical_formula_weight 402.49
_chemical_melting_point ?
_space_group_crystal_system orthorhombic
_space_group_name_H-M_alt 'P b c a'
_space_group_name_Hall '-P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'
_cell_length_a 12.5716(6)
_cell_length_b 8.3940(3)
_cell_length_c 20.3319(7)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_volume 2145.53(14)
_cell_formula_units_Z 8
_cell_measurement_reflns_used 7041
_cell_measurement_theta_min 2.5820
_cell_measurement_theta_max 30.3250
_cell_measurement_temperature 100(2)
_exptl_crystal_description needle
_exptl_crystal_colour yellow
_exptl_crystal_size_max 0.22
_exptl_crystal_size_mid 0.03
_exptl_crystal_size_min 0.01
_exptl_crystal_density_diffrn 2.492
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1488
_exptl_absorpt_coefficient_mu 14.404
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2015)
;
_exptl_absorpt_correction_T_min 0.70240
_exptl_absorpt_correction_T_max 1.00000
_diffrn_ambient_temperature 100(2)
_diffrn_source 'Enhance (Mo) X-ray Source'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_measurement_device_type 'Oxford Diffraction Xcalibur, Eos'
_diffrn_measurement_method '\w scan'
_diffrn_detector_area_resol_mean 16.1419
_diffrn_reflns_number 53277
_diffrn_reflns_av_R_equivalents 0.0795
_diffrn_reflns_av_unetI/netI 0.0287
_diffrn_reflns_theta_min 2.577
_diffrn_reflns_theta_max 29.127
_diffrn_reflns_theta_full 29.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_limit_h_min -17
_diffrn_reflns_limit_h_max 17
_diffrn_reflns_limit_k_min -11
_diffrn_reflns_limit_k_max 11
_diffrn_reflns_limit_l_min -27
_diffrn_reflns_limit_l_max 27
_refine_special_details ?
_reflns_number_total 2887
_reflns_number_gt 2134
_reflns_threshold_expression 'I > 2\s(I)'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_R_factor_all 0.0426
_refine_ls_R_factor_gt 0.0242
_refine_ls_wR_factor_gt 0.0383
_refine_ls_wR_factor_ref 0.0419
_refine_ls_goodness_of_fit_ref 1.046
_refine_ls_restrained_S_all 1.046
_refine_ls_number_reflns 2887
_refine_ls_number_parameters 105
_refine_ls_number_restraints 0
_refine_ls_hydrogen_treatment mixed
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0105P)^2^+2.0478P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_diff_density_max 0.863
_refine_diff_density_min -0.859
_refine_ls_extinction_method none
_refine_ls_extinction_coef .
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'
'Au' 'Au' -2.0133 8.8022
'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'
_computing_data_collection
;
CrysAlisPro, Version 1.171.36.28 (Rigaku OD, 2015)
;
_computing_cell_refinement
;
CrysAlisPro, Version 1.171.36.28 (Rigaku OD, 2015)
;
_computing_data_reduction
;
CrysAlisPro, Version 1.171.36.28 (Rigaku OD, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL2019/3 (Sheldrick, 2015)
;
_computing_molecular_graphics
;
XP, Version 5.1 (Bruker, 1998)
;
_computing_publication_material
;
SHELXL2019/3 (Sheldrick, 2015)
;
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 0.24309(2) 0.30864(2) 0.12540(2) 0.01126(5) Uani d 1 . .
Cl Cl1 0.06218(8) 0.27039(12) 0.11903(6) 0.0183(2) Uani d 1 . .
Cl Cl2 0.23963(8) 0.47300(12) 0.03594(5) 0.0152(2) Uani d 1 . .
Cl Cl3 0.25068(9) 0.13911(12) 0.21305(5) 0.0163(2) Uani d 1 . .
N N11 0.4051(3) 0.3526(4) 0.12740(19) 0.0140(7) Uani d 1 . .
H H01 0.413(3) 0.459(5) 0.116(2) 0.016(12) Uiso d 1 . .
C C12 0.4627(4) 0.2518(5) 0.0768(2) 0.0164(10) Uani d 1 . .
H H12A 0.461894 0.138753 0.090652 0.020 Uiso calc 1 . .
H H12B 0.426095 0.260030 0.033863 0.020 Uiso calc 1 . .
C C13 0.5764(3) 0.3084(5) 0.0700(2) 0.0172(9) Uani d 1 . .
H H13A 0.576749 0.418818 0.052940 0.021 Uiso calc 1 . .
H H13B 0.613978 0.240127 0.037781 0.021 Uiso calc 1 . .
C C14 0.6356(3) 0.3033(5) 0.1356(2) 0.0171(9) Uani d 1 . .
H H14 0.637276 0.190175 0.150987 0.020 Uiso calc 1 . .
C C15 0.5748(4) 0.4004(5) 0.1862(2) 0.0167(9) Uani d 1 . .
H H15A 0.610893 0.391913 0.229285 0.020 Uiso calc 1 . .
H H15B 0.575131 0.513867 0.172913 0.020 Uiso calc 1 . .
C C16 0.4608(3) 0.3441(5) 0.1930(2) 0.0183(10) Uani d 1 . .
H H16A 0.459812 0.233002 0.209420 0.022 Uiso calc 1 . .
H H16B 0.422949 0.411771 0.225335 0.022 Uiso calc 1 . .
C C17 0.7505(3) 0.3604(5) 0.1278(2) 0.0226(9) Uani d 1 . .
H H17A 0.750776 0.472073 0.113702 0.034 Uiso calc 1 . .
H H17B 0.786546 0.295036 0.094620 0.034 Uiso calc 1 . .
H H17C 0.787735 0.350621 0.169907 0.034 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 0.01234(7) 0.00980(8) 0.01163(7) 0.00022(6) 0.00052(7) -0.00063(6)
Cl1 0.0153(5) 0.0172(5) 0.0225(6) -0.0036(4) 0.0014(5) 0.0009(5)
Cl2 0.0187(5) 0.0130(5) 0.0139(5) -0.0011(4) -0.0021(4) 0.0019(4)
Cl3 0.0227(5) 0.0127(5) 0.0135(4) -0.0006(4) 0.0019(5) 0.0015(4)
N11 0.0121(16) 0.0110(17) 0.0189(18) 0.0001(13) -0.0004(16) 0.0011(16)
C12 0.014(2) 0.021(3) 0.015(2) 0.0004(17) 0.0039(19) -0.0070(17)
C13 0.013(2) 0.023(3) 0.016(2) 0.001(2) 0.0022(17) -0.0025(19)
C14 0.013(2) 0.020(2) 0.019(2) -0.0010(18) -0.0001(17) 0.0024(19)
C15 0.018(2) 0.019(2) 0.013(2) 0.0014(18) -0.0065(18) -0.0034(17)
C16 0.018(2) 0.025(3) 0.012(2) -0.0002(19) -0.0024(17) -0.0042(18)
C17 0.019(2) 0.026(2) 0.022(2) -0.0043(18) -0.004(2) 0.007(2)
_geom_special_details ?
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 . 2.070(3) y
Au1 Cl3 . 2.2826(10) y
Au1 Cl2 . 2.2832(10) y
Au1 Cl1 . 2.3006(10) y
N11 C16 . 1.509(5) ?
N11 C12 . 1.516(5) ?
N11 H01 . 0.93(4) ?
C12 C13 . 1.512(6) ?
C12 H12A . 0.9900 ?
C12 H12B . 0.9900 ?
C13 C14 . 1.528(6) ?
C13 H13A . 0.9900 ?
C13 H13B . 0.9900 ?
C14 C15 . 1.518(6) ?
C14 C17 . 1.531(6) ?
C14 H14 . 1.0000 ?
C15 C16 . 1.515(6) ?
C15 H15A . 0.9900 ?
C15 H15B . 0.9900 ?
C16 H16A . 0.9900 ?
C16 H16B . 0.9900 ?
C17 H17A . 0.9800 ?
C17 H17B . 0.9800 ?
C17 H17C . 0.9800 ?
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 Cl3 . . 93.13(11) y
N11 Au1 Cl2 . . 85.80(11) y
Cl3 Au1 Cl2 . . 178.07(4) y
N11 Au1 Cl1 . . 176.94(11) y
Cl3 Au1 Cl1 . . 89.90(4) y
Cl2 Au1 Cl1 . . 91.18(4) y
C16 N11 C12 . . 110.6(3) y
C16 N11 Au1 . . 117.8(3) y
C12 N11 Au1 . . 111.0(3) y
C16 N11 H01 . . 103(3) ?
C12 N11 H01 . . 108(3) ?
Au1 N11 H01 . . 106(3) ?
C13 C12 N11 . . 109.8(3) ?
C13 C12 H12A . . 109.7 ?
N11 C12 H12A . . 109.7 ?
C13 C12 H12B . . 109.7 ?
N11 C12 H12B . . 109.7 ?
H12A C12 H12B . . 108.2 ?
C12 C13 C14 . . 111.8(3) ?
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 C13 . . 109.4(3) ?
C15 C14 C17 . . 112.2(4) ?
C13 C14 C17 . . 111.1(3) ?
C15 C14 H14 . . 108.0 ?
C13 C14 H14 . . 108.0 ?
C17 C14 H14 . . 108.0 ?
C16 C15 C14 . . 111.8(3) ?
C16 C15 H15A . . 109.3 ?
C14 C15 H15A . . 109.3 ?
C16 C15 H15B . . 109.3 ?
C14 C15 H15B . . 109.3 ?
H15A C15 H15B . . 107.9 ?
N11 C16 C15 . . 110.0(3) ?
N11 C16 H16A . . 109.7 ?
C15 C16 H16A . . 109.7 ?
N11 C16 H16B . . 109.7 ?
C15 C16 H16B . . 109.7 ?
H16A C16 H16B . . 108.2 ?
C14 C17 H17A . . 109.5 ?
C14 C17 H17B . . 109.5 ?
H17A C17 H17B . . 109.5 ?
C14 C17 H17C . . 109.5 ?
H17A C17 H17C . . 109.5 ?
H17B C17 H17C . . 109.5 ?
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
Cl3 Au1 N11 C16 . . . . -30.0(3) y
Cl2 Au1 N11 C16 . . . . 151.6(3) y
Cl3 Au1 N11 C12 . . . . 98.8(3) y
Cl2 Au1 N11 C12 . . . . -79.6(3) y
C16 N11 C12 C13 . . . . -58.4(4) ?
Au1 N11 C12 C13 . . . . 169.1(3) y
N11 C12 C13 C14 . . . . 57.4(5) ?
C12 C13 C14 C15 . . . . -55.8(5) ?
C12 C13 C14 C17 . . . . 179.8(4) y
C13 C14 C15 C16 . . . . 55.7(5) ?
C17 C14 C15 C16 . . . . 179.4(4) y
C12 N11 C16 C15 . . . . 58.4(4) ?
Au1 N11 C16 C15 . . . . -172.6(3) y
C14 C15 C16 N11 . . . . -57.7(5) ?
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 Cl1 8_665 0.93(4) 2.64(4) 3.535(4) 163(4) yes
C15 H15B Cl1 8_665 0.99 2.97 3.804(4) 142.7 yes
C13 H13B Cl2 4 0.99 2.82 3.798(4) 170.6 yes
C15 H15A Cl3 3_655 0.99 2.95 3.610(4) 124.9 yes
C15 H15A Cl3 6_656 0.99 2.99 3.728(4) 131.8 yes
C16 H16B Cl3 8_665 0.99 2.91 3.656(5) 132.8 yes
_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 0.144
_shelx_estimated_absorpt_T_max 0.869
_shelx_hkl_file
;
0 0 -3-4.91706 42.7484 10
0 0 -3 7.15724 41.1850 1
0 0 3 64.7624 44.8845 10
0 0 3-28.6558 27.3013 9
0 0 3-23.4565 32.3839 13
0 0 -3-13.0116 23.0819 9
0 0 3 35.8069 28.2579 12
0 0 3-4.78724 25.8791 17
0 0 -3 22.1446 40.6984 12
0 0 3 29.4066 47.8765 1
0 0 3 49.4335 26.2606 5
0 0 -3-9.77367 26.4633 13
0 0 -3 14.4594 28.1643 17
0 0 4 81844.1 782.866 9
0 0 -4 85423.1 961.110 12
0 0 4 87125.4 876.381 17
0 0 4 80278.4 959.938 10
0 0 -4 84299.3 895.406 13
0 0 4 85342.6 791.988 5
0 0 -4 85893.4 1024.70 1
0 0 4 84578.8 877.189 13
0 0 -4 83775.0 777.182 9
0 0 4 80107.7 941.323 12
0 0 4 84327.2 932.054 11
0 0 -4 86740.0 870.250 17
0 0 4 82262.5 987.845 1
0 0 -5 60.3653 68.6721 10
0 0 -5 41.2466 74.0148 1
0 0 5 82.8855 62.0644 13
0 0 -5-12.5507 35.3517 9
0 0 5-25.5742 44.0927 12
0 0 -5 1.29600 58.1321 12
0 0 5-22.7892 38.5444 9
0 0 -5-81.9766 55.8678 17
0 0 5-23.4975 46.0022 11
0 0 5-23.8286 60.0902 1
0 0 5-22.4394 39.2938 5
0 0 5 7.97199 32.4658 17
0 0 5 69.3440 63.2371 10
0 0 6 138.146 68.0002 5
0 0 6 101.204 53.7003 12
0 0 6 73.1956 43.6145 9
0 0 6 202.044 97.1799 1
0 0 6 81.3399 57.6951 13
0 0 6 63.1374 57.5869 11
0 0 -6 58.2247 42.8469 9
0 0 6 90.1194 50.2997 17
0 0 -6 115.706 87.8280 10
0 0 -6 306.941 86.5596 12
0 0 -6-2.57709 71.1613 1
0 0 6 26.1780 48.9898 10
0 0 -6 108.031 51.9175 17
0 0 7-24.5983 43.3953 10
0 0 7-87.7082 60.4424 5
0 0 -7-31.4741 79.0288 10
0 0 -7-49.4677 53.0930 9
0 0 7-16.6667 53.6175 13
0 0 7 54.3554 54.1182 17
0 0 7 93.5805 58.2533 9
0 0 7 84.9010 81.2662 11
0 0 -7 71.3546 55.9218 17
0 0 -7-25.9085 74.4682 12
0 0 -8 49387.9 942.813 17
0 0 8 47409.6 992.063 11
0 0 -8 47141.9 1031.81 12
0 0 8 46496.2 832.115 9
0 0 -8 45300.4 1087.18 10
0 0 -8 47165.8 832.842 9
0 0 8 46187.1 836.237 5
0 0 8 46547.6 944.706 13
0 0 9 82.2617 75.5868 13
0 0 -9-32.0987 101.798 10
0 0 -9 55.3607 57.6135 9
0 0 -9 5.63476 91.7206 12
0 0 9 31.8525 65.1195 5
0 0 9 63.6896 55.9364 9
0 0 9 57.1643 78.0892 11
0 0 -9-40.8931 59.9182 17
0 0 -10 119.060 65.4169 17
0 0 -10 238.996 122.679 12
0 0 -10 99.6601 54.6024 9
0 0 10 176.019 88.5540 13
0 0 -10 170.012 113.933 15
0 0 10 248.140 112.095 11
0 0 10 170.542 77.2095 5
0 0 -10 133.242 93.7070 10
0 0 -11 146.496 120.168 15
0 0 11 47.1430 62.3911 5
0 0 -11 59.2622 49.1204 9
0 0 11-5.03295 77.8668 11
0 0 -11-149.021 129.674 10
0 0 11-41.2581 70.7209 13
0 0 -11-82.2271 89.4790 12
0 0 12 72657.2 1536.95 11
0 0 -12 70187.6 1461.36 15
0 0 12 69169.9 1428.13 13
0 0 -12 67194.4 1666.04 10
0 0 -12 73324.7 1276.65 9
0 0 12 68916.3 1277.35 5
0 0 -12 69204.5 1557.05 12
0 0 -13 281.148 188.687 10
0 0 13 120.086 85.1534 5
0 0 -13 63.8065 77.3146 9
0 0 -13 50.4017 89.8930 15
0 0 -13 291.640 163.770 12
0 0 13 365.647 147.753 13
0 0 13 203.899 132.322 11
0 0 14 47.1858 106.422 11
0 0 14 161.954 120.877 2
0 0 -14 98.0979 101.422 15
0 0 -14 74.7938 77.6095 9
0 0 14 44.5369 72.5292 13
0 0 -14-4.42145 119.133 10
0 0 14-8.39602 70.4798 5
0 0 -14-61.6453 115.835 12
0 0 -15 133.469 164.276 10
0 0 15-41.2188 94.8887 11
0 0 15-23.4561 72.5311 13
0 0 -15 97.1352 72.1471 9
0 0 -15-5.01219 107.213 12
0 0 15 101.760 113.784 2
0 0 15-123.534 80.0175 5
0 0 -15-18.2454 93.1721 15
0 0 16 22282.3 1012.12 11
0 0 -16 23127.7 953.666 15
0 0 -16 22372.7 1045.15 12
0 0 -16 21779.0 815.367 9
0 0 16 22140.9 860.301 5
0 0 -16 21804.7 1127.10 10
0 0 16 22247.7 960.726 13
0 0 16 22167.3 913.462 2
0 0 17 277.390 162.649 11
0 0 -17 224.389 142.275 12
0 0 17 278.569 160.418 13
0 0 17 30.5078 85.7620 5
0 0 -17 88.5854 68.3144 9
0 0 -17 109.546 153.889 10
0 0 -17 261.663 134.117 15
0 0 17 164.824 116.529 2
0 0 18 237.839 125.934 2
0 0 18 210.300 114.937 13
0 0 18 45.7421 102.861 11
0 0 -18 350.874 263.674 10
0 0 -18 154.843 93.7537 15
0 0 -18-91.4066 114.707 12
0 0 18 214.377 105.466 5
0 0 -18 168.616 88.8942 9
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-9 -10 -1 507.693 246.802 3
-9 -10 1 320.532 149.543 3
-9 10 -1 404.291 216.890 6
-9 10 1 656.575 254.496 6
-9 10 -1 431.852 201.050 12
-9 10 1 367.592 207.855 12
9 -10 2 4445.00 653.841 2
-9 -10 -2 3246.52 564.166 3
-9 -10 2 2776.81 519.808 3
-9 10 -2 5270.81 730.236 6
-9 10 2 3960.01 633.510 6
-9 10 -2 3360.80 585.036 12
-9 10 2 3965.85 630.845 12
9 -10 3 1614.41 406.208 2
-9 -10 -3 1797.89 409.962 3
-9 -10 3 1533.86 391.478 3
-9 10 3 1874.58 441.582 6
-9 10 3 1511.58 398.715 12
-9 -10 -4 47.6953 149.081 3
-9 -10 4 97.3113 157.841 3
-9 10 4-134.870 159.398 6
-9 10 4-34.0695 107.081 12
-9 -10 -5 928.933 304.545 3
-9 -10 5 634.249 265.421 3
-9 10 5 634.118 286.824 6
-9 10 5 1146.36 342.968 12
9 -10 -6 5302.25 714.903 9
-9 10 6 6253.61 780.942 6
-9 10 6 7103.52 857.769 5
-9 10 7 1042.51 388.179 5
10 -10 1 1254.48 385.020 2
0 -11 0-33.6879 172.169 8
0 11 0 34.5041 124.741 10
0 -11 1 50.7954 154.127 8
0 -11 -1-144.446 140.965 8
0 11 1 97.7657 181.098 10
0 11 -1-48.6817 144.152 10
0 11 2-21.4574 94.0396 5
0 -11 2-177.574 150.113 8
0 -11 -2 5.89000 106.532 8
0 11 2-106.476 139.868 10
0 11 -2 17.0011 115.225 10
0 11 3-49.9111 118.800 5
0 -11 3 45.4954 202.274 8
0 -11 -3 70.7691 213.100 8
0 11 3-150.430 173.421 10
0 -11 3 33.9632 150.171 2
0 11 -3 60.2615 181.977 10
0 -11 4 143.719 121.638 2
0 11 4-148.413 156.098 5
0 -11 4 509.025 265.088 8
0 -11 -4 137.472 174.274 8
0 11 4-48.9541 139.289 10
0 11 -4-181.521 196.935 10
0 11 5 112.209 122.768 5
0 -11 5-56.4081 140.661 2
0 -11 5 242.530 226.068 8
0 -11 -5-154.419 165.996 8
0 11 -5 238.525 181.744 10
0 11 6 393.126 243.933 5
0 -11 6 275.729 187.577 8
0 -11 -6 453.507 270.529 8
0 11 -6 7.23040 189.516 10
0 11 7 84.5455 114.017 5
0 -11 7-78.6248 171.694 8
0 -11 -7-164.875 143.555 8
0 11 -7 208.200 217.273 10
0 11 8-128.549 156.781 5
0 -11 -8-15.7598 144.481 8
0 11 9-69.2925 113.992 5
0 11 11-206.645 154.002 13
0 11 12-104.833 157.069 13
-1 -11 0 89.1196 187.187 8
1 -11 0-333.045 233.164 8
1 11 0 175.846 134.638 10
-1 11 0 10.2232 161.672 10
1 11 1 164.791 134.319 5
1 11 -1 347.873 195.093 1
-1 -11 1 124.871 219.218 8
-1 -11 -1-342.733 192.485 8
1 -11 1-35.5637 189.107 8
1 -11 -1-168.774 212.302 8
1 11 1 102.621 174.161 10
1 -11 1-26.9826 150.557 2
1 11 -1 469.883 275.437 10
-1 11 1-49.3581 132.033 10
-1 11 -1 15.8430 117.065 10
1 -11 2-79.9566 179.802 2
1 11 2 439.743 225.098 5
-1 -11 2-125.784 193.600 8
-1 -11 -2 131.779 190.861 8
1 -11 2 580.524 245.865 8
1 -11 -2 116.048 196.741 8
1 11 -2 90.7530 125.357 1
1 11 2-142.330 168.826 10
1 11 -2 337.643 225.643 10
-1 11 2-29.7690 137.957 10
-1 11 -2-197.692 184.335 10
-1 11 2-32.5053 82.8754 5
1 -11 3-188.969 134.899 2
1 11 3-199.394 188.148 5
1 11 -3-55.3195 138.621 1
-1 -11 3-248.519 207.001 8
-1 -11 -3 13.4064 145.975 8
1 -11 3-4.31544 135.214 8
1 -11 -3-19.4592 170.107 8
1 11 3-103.686 151.514 10
-1 11 3-221.631 160.318 10
1 11 -3 30.0214 157.119 10
-1 11 -3-82.2858 118.060 10
-1 11 3 178.184 141.468 5
1 11 4-195.484 154.935 5
1 -11 4 254.650 210.967 2
-1 -11 4 279.854 172.534 8
-1 -11 -4 215.334 173.642 8
1 -11 4 43.7452 103.994 8
1 -11 -4 222.027 209.187 8
1 11 -4-254.723 205.234 1
-1 11 4 254.161 185.775 10
1 11 -4 134.597 212.853 10
-1 11 -4-33.0811 110.365 10
-1 11 4-158.168 132.948 5
1 11 5 150.618 173.638 5
1 -11 5-5.61715 129.669 2
-1 -11 5-11.2725 157.505 8
-1 -11 -5 157.600 182.556 8
1 -11 5-56.2543 134.299 8
1 -11 -5 249.655 190.176 8
-1 11 5-110.074 146.509 10
-1 -11 5 0.55742 174.064 2
1 11 -5-150.322 172.642 10
-1 11 -5 137.434 222.756 10
-1 11 5-142.097 173.728 5
1 11 6-271.216 223.390 5
-1 -11 6 170.412 165.104 8
-1 -11 -6-127.719 156.320 8
1 -11 6-114.891 172.094 8
1 -11 -6 249.201 204.709 8
1 11 -6 137.939 188.953 10
-1 11 -6-98.6434 164.782 10
-1 11 6-219.124 188.239 5
1 11 7 206.931 172.725 5
-1 -11 7 67.3085 155.293 8
-1 -11 -7-67.5017 149.702 8
1 -11 7 98.8497 132.478 8
1 -11 -7-172.966 181.268 8
-1 11 -7-175.633 194.346 10
-1 11 7-221.624 190.338 5
1 11 8-136.131 151.555 5
-1 -11 8-155.893 210.693 8
-1 11 8 123.421 139.286 5
-1 11 9-30.5007 147.389 5
1 11 10-119.041 112.011 13
1 11 11-59.4512 94.8895 13
-2 -11 0 125.963 149.118 8
2 -11 0 324.734 195.187 8
2 11 0 255.038 151.077 10
2 11 0 494.392 221.505 1
2 -11 0 500.495 251.922 2
-2 11 0 297.858 194.357 10
2 -11 1 910.945 364.928 2
2 11 -1 131.460 148.703 1
-2 -11 1 82.3630 147.973 8
-2 -11 -1 661.754 297.846 8
2 -11 1 9.83891 139.789 8
2 -11 -1 40.4811 177.161 8
2 11 1 200.986 170.796 1
2 11 1-103.852 136.208 10
2 11 -1 277.277 195.863 10
-2 11 1-106.480 138.527 10
-2 11 -1 216.452 168.140 10
2 -11 2-61.1660 152.109 2
2 11 2-216.172 192.261 1
-2 -11 2 49.0027 182.761 8
-2 -11 -2-81.3514 178.474 8
2 -11 2 243.321 198.614 8
2 -11 -2-137.462 152.211 8
2 11 -2 162.502 144.312 1
2 11 -2 109.890 202.665 10
-2 11 2 68.3669 111.542 10
-2 11 -2 67.9035 132.197 10
2 -11 3 209.509 199.405 2
2 11 -3 82.3210 123.932 1
-2 -11 3 104.529 203.635 8
-2 -11 -3-211.368 185.669 8
2 -11 3-145.563 130.687 8
2 -11 -3-207.344 211.493 8
2 11 -3 78.2032 129.596 10
-2 11 3-22.5725 110.181 10
-2 11 -3-7.62321 127.319 10
-2 11 3-300.993 199.270 5
2 -11 4 159.994 206.150 2
-2 -11 4 235.711 222.902 8
-2 -11 -4-34.6341 120.398 8
2 -11 4-86.5721 130.611 8
2 -11 -4 34.6277 190.635 8
2 11 -4 29.5906 134.878 10
-2 11 -4-9.88425 106.558 10
-2 11 4-121.835 122.883 5
2 11 -4 224.015 148.050 1
-2 -11 5-90.3794 123.186 8
-2 -11 -5 65.0251 164.494 8
2 11 -5 69.6317 162.388 1
2 11 -5 91.2995 148.129 10
-2 11 -5 119.304 204.668 10
-2 11 5 338.771 199.024 5
2 11 6 15.5549 157.454 5
-2 -11 6 158.765 231.662 8
-2 -11 -6-42.3301 153.986 8
-2 11 -6-276.596 226.543 10
-2 11 6-88.6458 136.207 5
2 11 7-137.203 156.558 5
-2 11 7 34.9434 153.732 5
2 11 8-448.465 228.475 5
-2 11 8 469.552 231.464 5
2 11 9-18.6203 141.006 13
-2 11 9-42.4252 175.896 5
2 11 10 195.609 144.248 13
2 11 11 85.7368 143.080 13
3 -11 0 107.699 147.645 2
-3 -11 0 52.5484 126.662 8
-3 11 0 330.501 197.494 10
3 -11 1 7.61927 180.701 2
3 11 -1-127.611 193.778 1
-3 -11 1 134.119 180.114 8
-3 -11 -1-129.201 156.318 8
3 11 1-86.7885 191.511 1
3 11 -1 220.723 196.425 10
3 -11 -1 245.120 199.272 2
-3 11 1-63.9264 109.324 10
-3 11 -1 359.755 224.310 10
3 -11 2 286.208 178.455 2
3 11 2-93.3284 158.102 1
-3 -11 2-262.845 227.517 8
-3 -11 -2 69.5536 146.826 8
3 11 -2 148.452 180.586 1
3 11 -2-63.4889 119.809 10
-3 11 -2-27.9679 121.258 10
3 -11 3-91.0611 152.244 2
3 11 3-28.4863 167.108 1
-3 -11 3 196.688 174.859 8
-3 -11 -3 4.93193 192.499 8
3 11 -3 53.5151 141.162 1
3 11 -3 216.804 200.524 10
-3 11 -3-18.1743 127.914 10
3 -11 4 35.1797 151.890 2
3 11 -4-35.1369 154.347 1
3 11 -4-48.2208 215.884 10
-3 11 -4 279.235 185.151 10
-3 11 4-275.045 177.272 5
3 11 4-280.776 209.840 1
3 11 -5-112.352 173.717 1
3 11 5-166.657 183.701 1
-3 11 -5 346.703 199.159 10
-3 11 5 163.663 162.681 5
3 11 -6-125.507 215.906 1
-3 11 -6-20.8676 132.945 10
-3 11 6 3.56807 140.122 5
-3 11 -7-23.8285 149.453 10
-3 11 7-17.4303 119.791 5
3 11 8 10.2675 104.699 13
-3 11 8 129.078 157.314 5
3 11 9 200.295 186.087 13
3 11 10-56.7727 123.529 13
4 -11 0-61.8492 157.424 2
4 11 0-329.996 229.525 1
4 -11 -1 262.184 178.210 2
4 11 -1-141.331 152.716 1
4 -11 1 134.102 117.324 2
4 11 1 98.9233 159.651 1
-4 11 -1 227.579 178.177 10
4 -11 2-95.4574 114.946 2
4 11 -2 51.6234 130.030 1
4 11 2-232.915 206.604 1
4 -11 -2-95.3811 174.996 2
-4 11 -2-212.204 198.557 10
4 -11 3 400.236 237.680 2
4 11 3 169.302 140.197 1
4 11 -3 176.808 185.972 1
-4 11 -3-160.223 196.387 10
4 11 -4 70.1333 158.615 1
-4 11 -4 159.130 152.602 10
4 11 4-270.371 204.380 1
4 11 5 211.668 143.867 1
4 11 -5 203.652 173.000 1
-4 11 5 283.082 125.474 5
-4 11 -5 86.2723 143.717 10
4 11 6-11.6722 121.432 1
4 11 -6 22.5596 122.466 1
-4 11 6-244.171 190.808 5
-4 11 -6 63.4752 122.002 10
4 11 7 367.949 227.170 1
-4 11 7 136.837 102.252 5
-4 11 -7 118.330 198.377 10
-4 11 8 145.665 156.511 5
5 -11 0 97.0556 110.615 2
5 11 0 335.641 214.616 1
5 -11 -1 122.164 126.321 2
5 -11 1 350.785 197.370 2
5 11 1-117.604 179.456 1
5 11 -1 218.894 195.574 1
5 -11 -2 340.328 200.566 2
5 11 -2 533.123 279.011 1
5 11 2 594.675 274.343 1
5 11 3-62.8483 150.713 1
5 11 -3 64.2830 121.569 1
-5 11 -3 61.1969 127.859 6
5 -11 -3 504.287 271.660 2
-5 11 -3 247.423 227.213 10
-5 11 -4-140.932 165.303 6
5 11 -4 334.764 231.854 1
5 11 4-187.367 184.501 1
-5 11 -4-184.733 190.872 10
5 -11 -5 388.319 202.055 9
-5 11 -5 57.0051 146.206 6
5 11 5 28.7374 155.791 1
-5 11 5 199.220 187.656 5
-5 11 -5 254.311 191.155 10
5 -11 -6 68.6545 84.8624 9
5 11 6-386.718 206.844 1
-5 11 6-141.410 200.246 5
-5 11 -6 213.974 206.124 10
5 -11 -7-156.822 190.929 9
5 11 7 19.6484 173.723 1
-5 11 7-228.249 236.461 5
-5 11 -7 90.7957 140.498 10
5 11 8 40.2147 117.576 1
5 11 9 158.937 170.772 1
6 -11 0 425.716 232.207 2
6 -11 -1 251.672 192.998 2
6 -11 -2-124.204 176.746 2
-6 11 -2 193.795 191.532 6
6 -11 -3-79.9802 137.030 2
-6 11 -3 330.247 199.173 6
-6 11 -4-70.5528 161.561 6
6 -11 -4 73.0843 158.628 2
-6 11 -5-42.3567 172.594 6
6 -11 -6 207.925 180.344 9
-6 11 -6-191.149 176.840 6
-6 11 6-214.397 202.216 5
-6 11 -6-220.864 216.452 10
-6 11 7-292.351 240.923 5
-6 11 -7 19.9638 111.754 10
-7 11 0-32.8347 132.947 6
-7 11 -1-273.709 200.490 6
7 -11 -2 133.196 145.247 2
-7 11 -2 614.392 275.036 6
-7 11 -2 274.572 210.957 12
7 -11 -3-283.133 218.795 2
-7 11 -3 142.457 165.456 6
-7 11 -3 271.508 200.218 12
-7 11 -4 397.099 202.781 12
0 12 4 208.147 155.757 10
-1 12 1 3086.97 551.499 10
-1 12 2 479.843 252.050 10
-2 12 0 1718.34 420.851 10
0 0 0 0.00 0.00 0
TITL Oxford in Pbca
REM Pbca (#61, found as Pcab in ba-c setting)
CELL 0.71073 12.571619 8.393956 20.331872 90.0000 90.0000 90.0000
ZERR 11.00 0.000275 0.000143 0.000355 0.0000 0.0000 0.0000
LATT 1
SYMM -x+1/2,-y, z+1/2
SYMM -x, y+1/2,-z+1/2
SYMM x+1/2,-y+1/2,-z
SFAC C H N Au
UNIT 99.00 143.00 11.00 11.00
TREF
HKLF 4
END
;
_shelx_hkl_checksum 46886
_shelx_res_file
;
TITL Oxford in Pbca
shelx.res
created by SHELXL-2019/3 at 09:26:26 on 08-Mar-2024
REM Pbca (#61, found as Pcab in ba-c setting)
CELL 0.71073 12.571619 8.393956 20.331872 90.0000 90.0000 90.0000
ZERR 8.00 0.000550 0.000290 0.000710 0.0000 0.0000 0.0000
LATT 1
SYMM -x+1/2,-y, z+1/2
SYMM -x, y+1/2,-z+1/2
SYMM x+1/2,-y+1/2,-z
SFAC C H N Au Cl
UNIT 48.00 104.00 8.00 8.00 24.00
L.S. 8
FMAP 2
PLAN 10
SIZE 0.22 0.03 0.01
TEMP -173
SHEL 999 0.73
ACTA 58
BOND $H
CONF 2.4
EQIV $1 -x+1/2, y+1/2, z
EQIV $2 x+1/2, -y+1/2, -z
EQIV $3 -x+1, y+1/2, -z+1/2
EQIV $4 x+1/2, y, -z+1/2
EQIV $5 -x+1/2, y-1/2, z
HTAB N11 Cl1_$1
HTAB C15 Cl1_$1
HTAB C13 Cl2_$2
HTAB C15 Cl3_$3
HTAB C15 Cl3_$4
HTAB C16 Cl3_$1
RTAB DIST Au1 Au1_$1
RTAB DIST Au1 Au1_$5
RTAB DIST Au1 Cl2_$5
RTAB DIST Au1 Cl3_$1
RTAB DIST Cl1 Cl2_$5
RTAB ANGL Au1 Cl1 Cl2_$5
RTAB DIST Cl2 Au1_$1
RTAB ANGL Au1 Cl2 Au1_$1
RTAB DIST Cl2 CL3_$1
RTAB ANGL Au1 Cl2 Cl3_$1
RTAB DIST Cl3 Au1_$5
RTAB ANGL Au1 Cl3 Au1_$5
RTAB DIST Cl3 Cl2_$5
RTAB ANGL Au1 Cl3 Cl2_$5
WGHT 0.010500 2.047800
FVAR 0.40722
AU1 4 0.243095 0.308640 0.125397 11.00000 0.01234 0.00980 =
0.01163 -0.00063 0.00052 0.00022
CL1 5 0.062179 0.270390 0.119033 11.00000 0.01532 0.01715 =
0.02250 0.00092 0.00141 -0.00357
CL2 5 0.239628 0.472999 0.035943 11.00000 0.01872 0.01297 =
0.01386 0.00194 -0.00213 -0.00106
CL3 5 0.250680 0.139109 0.213051 11.00000 0.02268 0.01268 =
0.01347 0.00153 0.00192 -0.00062
N11 3 0.405055 0.352579 0.127401 11.00000 0.01212 0.01097 =
0.01890 0.00109 -0.00038 0.00010
H01 2 0.413442 0.458700 0.115568 11.00000 0.01625
C12 1 0.462744 0.251834 0.076827 11.00000 0.01374 0.02099 =
0.01458 -0.00705 0.00385 0.00038
AFIX 23
H12A 2 0.461894 0.138753 0.090652 11.00000 -1.20000
H12B 2 0.426095 0.260030 0.033863 11.00000 -1.20000
AFIX 0
C13 1 0.576423 0.308357 0.070003 11.00000 0.01276 0.02268 =
0.01614 -0.00252 0.00216 0.00127
AFIX 23
H13A 2 0.576749 0.418818 0.052940 11.00000 -1.20000
H13B 2 0.613978 0.240127 0.037781 11.00000 -1.20000
AFIX 0
C14 1 0.635550 0.303325 0.135633 11.00000 0.01279 0.01980 =
0.01862 0.00240 -0.00015 -0.00103
AFIX 13
H14 2 0.637276 0.190175 0.150987 11.00000 -1.20000
AFIX 0
C15 1 0.574753 0.400379 0.186166 11.00000 0.01791 0.01910 =
0.01314 -0.00338 -0.00652 0.00138
AFIX 23
H15A 2 0.610893 0.391913 0.229285 11.00000 -1.20000
H15B 2 0.575131 0.513867 0.172913 11.00000 -1.20000
AFIX 0
C16 1 0.460775 0.344066 0.193046 11.00000 0.01838 0.02480 =
0.01186 -0.00419 -0.00241 -0.00019
AFIX 23
H16A 2 0.459812 0.233002 0.209420 11.00000 -1.20000
H16B 2 0.422949 0.411771 0.225335 11.00000 -1.20000
AFIX 0
C17 1 0.750490 0.360397 0.127757 11.00000 0.01927 0.02633 =
0.02232 0.00662 -0.00367 -0.00433
AFIX 137
H17A 2 0.750776 0.472073 0.113702 11.00000 -1.50000
H17B 2 0.786546 0.295036 0.094620 11.00000 -1.50000
H17C 2 0.787735 0.350621 0.169907 11.00000 -1.50000
AFIX 0
HKLF 4
REM Oxford in Pbca
REM wR2 = 0.0419, GooF = S = 1.046, Restrained GooF = 1.046 for all data
REM R1 = 0.0242 for 2134 Fo > 4sig(Fo) and 0.0426 for all 2887 data
REM 105 parameters refined using 0 restraints
END
WGHT 0.0105 2.0478
REM Highest difference peak 0.863, deepest hole -0.859, 1-sigma level 0.165
Q1 1 0.2405 0.1771 0.1271 11.00000 0.05 0.86
Q2 1 0.2435 0.4579 0.1258 11.00000 0.05 0.84
Q3 1 0.0200 0.3105 0.1124 11.00000 0.05 0.79
Q4 1 0.0542 0.2222 0.1312 11.00000 0.05 0.73
Q5 1 0.1058 0.2897 0.1121 11.00000 0.05 0.72
Q6 1 0.1626 0.3632 0.1267 11.00000 0.05 0.70
Q7 1 0.5218 0.3028 0.0772 11.00000 0.05 0.69
Q8 1 0.0765 0.2879 0.1393 11.00000 0.05 0.66
Q9 1 0.1612 0.4816 0.0716 11.00000 0.05 0.60
Q10 1 0.7007 0.6042 0.1656 11.00000 0.05 0.56
;
_shelx_res_checksum 34170
data_2a
_audit_creation_method 'SHELXL-2019/3'
_chemical_name_systematic
;
Tribromido(4-methylpiperidine)gold(III)
;
_chemical_name_common ?
_chemical_formula_moiety 'C6 H13 Au Br3 N'
_chemical_formula_sum 'C6 H13 Au Br3 N'
_chemical_formula_iupac '[Au Br3 (C6 H13 N)]'
_chemical_formula_weight 535.87
_chemical_melting_point ?
_space_group_crystal_system orthorhombic
_space_group_name_H-M_alt 'P n m a'
_space_group_name_Hall '-P 2ac 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'
_cell_length_a 9.9871(5)
_cell_length_b 7.1505(4)
_cell_length_c 15.7160(8)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_volume 1122.32(10)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 4663
_cell_measurement_theta_min 3.1160
_cell_measurement_theta_max 30.2880
_cell_measurement_temperature 100(2)
_exptl_crystal_description needle
_exptl_crystal_colour orange
_exptl_crystal_size_max 0.27
_exptl_crystal_size_mid 0.06
_exptl_crystal_size_min 0.03
_exptl_crystal_density_diffrn 3.171
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 960
_exptl_absorpt_coefficient_mu 23.735
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2015)
;
_exptl_absorpt_correction_T_min 0.23996
_exptl_absorpt_correction_T_max 1.00000
_diffrn_ambient_temperature 100(2)
_diffrn_source 'fine-focus sealed X-ray tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_measurement_device_type 'Oxford Diffraction Xcalibur, Eos'
_diffrn_measurement_method '\w scan'
_diffrn_detector_area_resol_mean 16.1419
_diffrn_reflns_number 28605
_diffrn_reflns_av_R_equivalents 0.0701
_diffrn_reflns_av_unetI/netI 0.0332
_diffrn_reflns_theta_min 2.416
_diffrn_reflns_theta_max 31.093
_diffrn_reflns_theta_full 30.000
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_limit_h_min -14
_diffrn_reflns_limit_h_max 14
_diffrn_reflns_limit_k_min -10
_diffrn_reflns_limit_k_max 10
_diffrn_reflns_limit_l_min -22
_diffrn_reflns_limit_l_max 22
_refine_special_details ?
_reflns_number_total 1864
_reflns_number_gt 1581
_reflns_threshold_expression 'I > 2\s(I)'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_R_factor_all 0.0422
_refine_ls_R_factor_gt 0.0295
_refine_ls_wR_factor_gt 0.0472
_refine_ls_wR_factor_ref 0.0504
_refine_ls_goodness_of_fit_ref 1.110
_refine_ls_restrained_S_all 1.110
_refine_ls_number_reflns 1864
_refine_ls_number_parameters 65
_refine_ls_number_restraints 0
_refine_ls_hydrogen_treatment mixed
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0121P)^2^+3.4353P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_diff_density_max 1.564
_refine_diff_density_min -1.185
_refine_ls_extinction_method
;
SHELXL2019/3 (Sheldrick, 2015)
;
_refine_ls_extinction_coef 0.00051(4)
_refine_ls_extinction_expression
'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^'
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'
'Br' 'Br' -0.2901 2.4595
'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'
_computing_data_collection
;
CrysAlisPro, Version 1.171.38.43 (Rigaku OD, 2015)
;
_computing_cell_refinement
;
CrysAlisPro, Version 1.171.38.43 (Rigaku OD, 2015)
;
_computing_data_reduction
;
CrysAlisPro, Version 1.171.38.43 (Rigaku OD, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL2019/3 (Sheldrick, 2015)
;
_computing_molecular_graphics
;
XP, Version 5.1 (Bruker, 1998)
;
_computing_publication_material
;
SHELXL2019/3 (Sheldrick, 2015)
;
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 0.09315(2) 0.750000 0.04663(2) 0.01176(7) Uani d 1 . .
Br Br1 -0.07000(6) 0.750000 0.15933(4) 0.01882(14) Uani d 1 . .
Br Br2 -0.08081(6) 0.750000 -0.06122(4) 0.01351(13) Uani d 1 . .
Br Br3 0.26712(6) 0.750000 0.15298(4) 0.02039(15) Uani d 1 . .
N N11 0.2339(5) 0.750000 -0.0523(3) 0.0161(11) Uani d 1 . .
H H01 0.184(7) 0.750000 -0.099(4) 0.013(17) Uiso d 1 . .
C C12 0.3183(4) 0.9225(6) -0.0547(3) 0.0182(9) Uani d 1 . .
H H12A 0.373767 0.928684 -0.002574 0.022 Uiso calc 1 . .
H H12B 0.259617 1.034089 -0.055751 0.022 Uiso calc 1 . .
C C13 0.4087(4) 0.9241(6) -0.1324(3) 0.0193(9) Uani d 1 . .
H H13A 0.465879 1.037237 -0.131098 0.023 Uiso calc 1 . .
H H13B 0.353144 0.929562 -0.184542 0.023 Uiso calc 1 . .
C C14 0.4975(6) 0.750000 -0.1354(4) 0.0152(12) Uani d 1 . .
H H14 0.554971 0.750002 -0.083321 0.018 Uiso calc 1 . .
C C15 0.5896(7) 0.750000 -0.2129(4) 0.0253(16) Uani d 1 . .
H H15A 0.534829 0.750000 -0.264018 0.038 Uiso d 1 . .
H H15B 0.647617 0.860443 -0.211145 0.038 Uiso d 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 0.01034(11) 0.01467(12) 0.01027(12) 0.000 0.00112(9) 0.000
Br1 0.0180(3) 0.0253(3) 0.0132(3) 0.000 0.0057(2) 0.000
Br2 0.0113(3) 0.0163(3) 0.0129(3) 0.000 -0.0005(2) 0.000
Br3 0.0172(3) 0.0304(4) 0.0135(3) 0.000 -0.0042(2) 0.000
N11 0.011(2) 0.027(3) 0.010(3) 0.000 0.000(2) 0.000
C12 0.018(2) 0.016(2) 0.021(2) 0.0031(17) 0.0090(18) 0.0020(19)
C13 0.016(2) 0.022(2) 0.020(2) -0.0009(19) 0.0067(19) 0.005(2)
C14 0.013(3) 0.016(3) 0.017(3) 0.000 0.007(2) 0.000
C15 0.017(3) 0.033(4) 0.026(4) 0.000 0.009(3) 0.000
_geom_special_details ?
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 . 2.096(5) y
Au1 Br1 . 2.4066(7) y
Au1 Br3 . 2.4110(7) y
Au1 Br2 . 2.4273(6) y
N11 C12 7_575 1.494(5) ?
N11 C12 . 1.494(5) ?
N11 H01 . 0.89(6) ?
C12 C13 . 1.520(6) ?
C12 H12A . 0.9900 ?
C12 H12B . 0.9900 ?
C13 C14 . 1.529(5) ?
C13 H13A . 0.9900 ?
C13 H13B . 0.9900 ?
C14 C15 . 1.526(8) ?
C14 H14 . 1.0000 ?
C15 H15A . 0.9713 ?
C15 H15B . 0.9800 ?
C15 H15B 7_575 0.9800 ?
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 Br1 . . 179.50(15) y
N11 Au1 Br3 . . 91.78(15) y
Br1 Au1 Br3 . . 88.72(2) y
N11 Au1 Br2 . . 87.82(15) y
Br1 Au1 Br2 . . 91.68(2) y
Br3 Au1 Br2 . . 179.60(2) y
C12 N11 C12 7_575 . 111.2(5) y
C12 N11 Au1 7_575 . 113.4(3) y
C12 N11 Au1 . . 113.4(3) ?
C12 N11 H01 7_575 . 107(2) ?
C12 N11 H01 . . 107(2) ?
Au1 N11 H01 . . 104(4) ?
N11 C12 C13 . . 111.2(4) ?
N11 C12 H12A . . 109.4 ?
C13 C12 H12A . . 109.4 ?
N11 C12 H12B . . 109.4 ?
C13 C12 H12B . . 109.4 ?
H12A C12 H12B . . 108.0 ?
C12 C13 C14 . . 111.3(4) ?
C12 C13 H13A . . 109.4 ?
C14 C13 H13A . . 109.4 ?
C12 C13 H13B . . 109.4 ?
C14 C13 H13B . . 109.4 ?
H13A C13 H13B . . 108.0 ?
C15 C14 C13 . 7_575 111.9(3) ?
C15 C14 C13 . . 111.9(3) ?
C13 C14 C13 7_575 . 109.0(5) ?
C15 C14 H14 . . 107.9 ?
C13 C14 H14 7_575 . 107.9 ?
C13 C14 H14 . . 107.9 ?
C14 C15 H15A . . 108.7 ?
C14 C15 H15B . . 109.5 ?
H15A C15 H15B . . 110.9 ?
C14 C15 H15B . 7_575 109.48(19) ?
H15A C15 H15B . 7_575 110.9 ?
H15B C15 H15B . 7_575 107.4 ?
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
Br3 Au1 N11 C12 . . . 7_575 64.1(3) ?
Br2 Au1 N11 C12 . . . 7_575 -115.9(3) ?
Br3 Au1 N11 C12 . . . . -64.1(3) y
Br2 Au1 N11 C12 . . . . 115.9(3) y
C12 N11 C12 C13 7_575 . . . 56.4(6) ?
Au1 N11 C12 C13 . . . . -174.4(3) y
N11 C12 C13 C14 . . . . -56.8(5) ?
C12 C13 C14 C15 . . . . -179.7(4) y
C12 C13 C14 C13 . . . 7_575 55.9(6) ?
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 Br2 . 0.89(6) 2.71(6) 3.146(5) 111(5) yes
C12 H12B Br1 5_575 0.99 2.94 3.786(5) 144.6 yes
C12 H12B Br2 5_575 0.99 2.99 3.798(4) 139.3 yes
C15 H15A Br2 6_655 0.97 2.98 3.936(7) 168.5 yes
C12 H12A Br3 . 0.99 2.96 3.526(4) 117.6 yes
C13 H13A Br3 5_675 0.99 3.09 4.002(4) 153.8 yes
C15 H15B Br3 5_675 0.98 3.05 3.965(3) 155.3 yes
_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 0.060
_shelx_estimated_absorpt_T_max 0.536
_shelx_hkl_file
;
0 0 -2 117904. 3582.34 3
0 0 2 119532. 3323.00 1
0 0 -2 121824. 3184.69 4
0 0 2 126668. 3034.57 13
0 0 2 121124. 3025.34 12
0 0 -3 16.6177 177.353 1
0 0 -3-36.7456 188.495 3
0 0 3 24.4726 86.6680 12
0 0 -3 293.651 152.272 4
0 0 -3 208.302 122.016 13
0 0 3-128.513 153.410 1
0 0 3 221.636 112.493 4
0 0 3 258.635 209.751 3
0 0 -3-104.456 98.6705 12
0 0 4 13089.1 1172.13 3
0 0 -4 13815.3 789.302 12
0 0 -4 14018.5 1318.77 3
0 0 4 14560.5 984.214 4
0 0 -4 13044.8 942.989 4
0 0 4 13477.2 851.190 12
0 0 -4 12622.5 800.218 13
0 0 -4 14044.3 1094.07 1
0 0 4 13441.8 1057.08 1
0 0 -4 14292.7 651.638 9
0 0 -5 330.583 300.851 1
0 0 5 342.506 340.933 3
0 0 5 761.529 356.763 1
0 0 -5 267.515 199.760 13
0 0 -5 389.286 201.379 4
0 0 -5 1482.42 528.173 3
0 0 5 24.9025 135.249 12
0 0 -5 235.801 169.437 12
0 0 5 905.204 306.239 4
0 0 -5 277.757 126.557 9
0 0 -6 8587.43 763.040 12
0 0 -6 8160.52 783.034 13
0 0 -6 8149.86 539.953 9
0 0 -6 9296.20 1127.97 1
0 0 6 8740.77 1151.98 3
0 0 -6 8125.77 954.866 4
0 0 -6 10496.2 1426.31 3
0 0 -7-37.8122 348.429 1
0 0 -7-213.295 221.022 4
0 0 -7 53.9668 85.6616 9
0 0 7 219.463 474.965 3
0 0 -7 154.063 202.068 12
0 0 -8 120857. 5102.07 1
0 0 8 120067. 5196.00 3
0 0 -8 115715. 3852.57 12
0 0 -8 116743. 4569.70 4
0 0 -8 117600. 3185.65 9
0 0 -9 343.887 151.148 9
0 0 9 420.403 344.140 3
0 0 -9 402.891 282.993 12
0 0 -9 80.6303 290.510 4
0 0 -9-270.392 447.416 1
0 0 10 338637. 11097.5 3
0 0 -10 333652. 11007.2 1
0 0 -10 338066. 9116.76 12
0 0 -10 347533. 7997.16 9
0 0 -11 538.209 173.816 9
0 0 11 797.775 648.871 3
0 0 -11 465.882 327.114 12
0 0 -11 227.766 561.040 1
0 0 -12 24014.2 1716.57 12
0 0 -12 20274.8 2427.71 1
0 0 -12 21377.3 971.003 9
0 0 12 22037.8 2423.02 3
0 0 13 240.155 650.483 3
0 0 -13 131.430 95.5288 9
0 0 -13 1041.35 778.897 1
0 0 13 301.627 343.299 2
0 0 14 278.461 418.508 3
0 0 -14 749.936 808.758 1
0 0 14-305.247 352.036 2
0 0 15 140.222 371.870 2
0 0 -15-89.0356 619.352 5
0 0 16 2257.51 731.793 2
0 0 -16 3486.83 1408.56 5
0 0 17-177.380 353.568 2
0 0 17 453.547 442.460 8
0 0 18 35661.1 3783.94 8
0 0 18 30208.9 2846.01 2
0 0 -18 32069.1 3934.74 5
0 0 19 1389.34 916.096 8
0 0 19 730.889 642.480 2
0 0 -19 688.994 1030.61 5
0 0 -20 55412.3 5437.22 5
0 0 20 46138.8 3797.06 2
0 0 20 51393.0 4879.61 8
0 0 21 1132.33 609.297 8
0 0 -21 730.762 573.293 5
0 0 21-377.921 428.381 2
-1 0 -1 182187. 4222.66 4
1 0 1 184915. 4212.74 11
1 0 -1 163017. 4773.54 3
1 0 1 185085. 4259.44 13
-1 0 1 176943. 4178.10 1
1 0 -1 175667. 4241.13 10
-1 0 -1 176752. 4366.65 2
1 0 -1 176308. 4710.62 11
-1 0 -2 33569.8 1257.31 4
1 0 -2 35120.9 1336.97 1
-1 0 2 34218.1 1298.66 1
1 0 -2 33253.7 1340.87 8
-1 0 2 35960.7 1958.62 3
-1 0 -2 33342.4 1193.04 13
1 0 -2 34674.3 1137.29 10
1 0 2 33205.8 1170.56 13
-1 0 -2 34197.1 1115.07 11
1 0 -2 35040.1 1896.62 3
-1 0 2 34707.7 1299.59 8
1 0 2 35037.1 1449.10 1
1 0 2 34439.3 1292.22 2
-1 0 2 33489.9 1120.66 10
-1 0 -2 32691.4 1234.93 5
1 0 -2 34944.9 1552.30 11
1 0 2 34138.5 1260.41 4
-1 0 -2 33954.0 1289.60 2
-1 0 3 41371.5 2309.30 3
1 0 3 41635.2 1819.11 1
-1 0 -3 39109.3 1632.91 3
1 0 -3 42200.0 2382.03 3
1 0 3 37745.7 1384.91 13
-1 0 3 38289.2 1627.25 1
-1 0 -3 36058.8 1131.17 6
-1 0 3 38443.9 1626.82 8
-1 0 -3 38076.3 1548.16 4
-1 0 -3 39518.1 1522.85 2
1 0 -3 41352.5 1366.97 10
-1 0 -3 38006.3 1396.04 13
1 0 3 38669.1 1514.11 2
1 0 -3 39041.4 1775.41 11
1 0 -3 38607.4 1681.87 1
1 0 3 40342.8 1564.09 4
-1 0 -4 18853.6 1274.95 3
1 0 4 18695.2 1111.96 4
-1 0 -4 16123.3 1204.82 1
1 0 -4 16389.9 1156.12 12
-1 0 -4 17511.1 1112.17 4
1 0 -4 17410.3 1237.70 1
-1 0 -4 17720.6 956.943 13
1 0 4 18617.7 970.445 13
-1 0 4 20643.9 1756.66 3
1 0 -4 19129.5 1735.02 3
1 0 4 19341.1 845.459 12
-1 0 -4 17220.6 767.248 6
-1 0 4 18407.3 1186.40 4
-1 0 4 17232.8 1172.71 1
1 0 4 17566.0 1286.43 1
1 0 4 19345.6 1080.25 2
1 0 5 935.690 242.726 13
-1 0 5 1445.20 397.178 1
1 0 -5 1168.09 383.465 12
-1 0 -5 702.233 188.561 13
1 0 5 1289.28 326.876 3
-1 0 -5 957.252 278.902 1
1 0 -5 1774.12 477.076 1
1 0 5 1077.65 378.049 1
1 0 5 1189.01 298.297 2
1 0 -5 1295.12 527.776 3
1 0 5 893.287 191.944 12
-1 0 -5 1421.80 400.895 4
-1 0 -5 1156.44 327.558 3
-1 0 5 2152.98 684.067 3
-1 0 5 1123.21 362.889 4
1 0 5 1309.04 354.640 4
1 0 -6 24965.6 1545.79 12
1 0 6 25217.6 1252.03 12
-1 0 -6 27598.9 2013.35 1
1 0 6 24610.3 1668.11 3
-1 0 6 26099.1 2235.93 3
-1 0 -6 25915.7 1645.06 4
-1 0 -6 25507.1 2000.77 3
-1 0 -6 23991.4 1350.92 13
1 0 6 25313.0 1375.89 13
1 0 6 25287.9 1468.70 2
1 0 -6 26096.9 1867.69 1
1 0 7 27511.7 938.779 7
1 0 -7 28205.4 1727.16 12
1 0 7 31255.9 1659.31 13
1 0 7 29211.6 1966.84 3
1 0 7 29652.7 1708.72 2
-1 0 -7 30384.2 1920.79 4
1 0 7 29106.4 1488.21 12
-1 0 -7 31001.9 2209.17 1
1 0 -7 31886.2 2213.55 1
-1 0 7 31504.2 2596.89 3
-1 0 -8 24853.2 2110.37 1
-1 0 -8 24430.0 1492.84 9
1 0 8 23946.8 1650.41 2
1 0 -8 29020.7 2284.75 1
-1 0 -8 24121.1 1842.14 4
1 0 8 25950.8 1525.70 12
1 0 8 28177.6 2057.57 3
1 0 -8 23545.0 1654.67 12
-1 0 8 29646.8 2594.46 3
1 0 8 27413.8 1645.78 13
1 0 9 167328. 6175.78 3
1 0 -9 158848. 5368.24 12
1 0 9 165545. 5261.03 13
-1 0 -9 156622. 6369.48 1
-1 0 -9 152528. 4850.48 9
-1 0 9 167835. 7135.12 3
1 0 9 167215. 5171.51 12
-1 0 -9 164298. 5907.73 4
1 0 -9 160567. 6471.55 1
1 0 9 163947. 5436.00 2
1 0 10 83.4471 243.446 2
1 0 -10 354.711 307.999 12
-1 0 -10 220.979 387.591 4
-1 0 -10 138.771 166.046 9
-1 0 -10-65.1291 510.840 1
-1 0 10-554.899 498.107 3
1 0 -10-257.344 522.732 1
-1 0 -11 49934.6 3543.57 1
-1 0 -11 46213.4 2104.00 9
-1 0 -11 41089.8 2923.89 4
1 0 11 45591.3 2688.52 2
1 0 -11 48335.8 3570.04 1
1 0 -11 47526.0 2656.21 12
-1 0 11 48909.4 3805.13 3
1 0 -12 16947.8 1593.57 12
1 0 12 17354.5 1679.44 2
-1 0 -12 16835.4 1927.89 4
-1 0 12 16628.6 2259.33 3
1 0 -12 16637.9 2199.59 1
-1 0 -12 17216.3 1193.63 9
1 0 -13 4413.47 830.494 12
1 0 13 4433.88 895.228 2
-1 0 13 5134.02 1277.43 3
-1 0 -13 4847.19 1369.80 5
-1 0 -13 4372.12 577.271 9
-1 0 -13 3441.76 939.015 4
1 0 -13 4761.91 1252.64 1
-1 0 14 6621.13 1427.02 8
1 0 -14 3400.14 1073.39 1
-1 0 -14 4693.45 566.653 9
1 0 -14 5600.00 969.054 12
-1 0 -14 3368.31 1181.25 5
1 0 14 4961.81 975.732 2
-1 0 14 4226.72 1388.37 3
-1 0 15 3414.99 1119.86 8
1 0 -15 5651.13 1002.31 12
-1 0 -15 5981.72 1570.37 5
1 0 -15 3929.34 1243.43 1
1 0 15 4764.89 998.072 2
-1 0 15 2576.98 995.691 3
-1 0 -16 7533.58 1773.17 5
-1 0 16 4967.38 1381.81 3
-1 0 16 3755.30 1173.65 8
1 0 -16 5392.64 1424.45 1
1 0 -16 4918.45 1674.89 5
1 0 16 4287.74 1006.26 2
-1 0 17 7381.75 1312.50 2
1 0 17 6903.50 1342.88 2
-1 0 17 7655.87 1639.78 8
1 0 -17 13024.5 2703.27 5
-1 0 -17 8502.99 1991.33 5
-1 0 -18 11659.0 2349.97 5
1 0 -18 17588.7 3155.44 5
-1 0 18 12465.3 2159.94 8
-1 0 18 9965.66 1619.94 2
1 0 18 10570.9 1681.90 2
-1 0 19 33663.9 3779.51 8
1 0 -19 33368.1 4368.04 5
1 0 19 33607.9 3918.91 8
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-4 9 5 6383.04 1514.82 9
-4 9 5 9326.34 2164.77 8
4 9 6-643.889 745.116 13
4 -9 6-1269.11 944.906 1
4 9 -6 77.2175 404.329 6
4 9 7 3797.40 1264.05 13
4 9 -7 4652.78 1267.23 6
4 9 -8 629.305 702.266 6
-5 -9 0 469.552 667.890 11
-5 9 0-50.6129 728.533 9
-5 9 0-604.273 1008.42 8
-5 -9 1 2268.44 1216.22 11
-5 -9 -1-518.135 525.196 11
5 9 -1 1282.04 856.517 6
5 -9 1 71.5953 768.088 1
-5 9 1-470.975 581.655 9
-5 9 1-381.582 786.315 8
-5 -9 2 3084.73 1077.09 11
-5 -9 -2 5121.34 1514.70 11
5 9 -2 5211.86 1422.25 6
-5 9 2 6841.09 1720.35 9
-5 -9 3 111.439 460.754 11
-5 -9 -3 1723.01 976.328 11
5 9 -3 44.5818 502.353 6
-5 9 3 1087.31 828.755 9
-5 -9 -3 1134.23 754.502 4
5 9 4 3289.80 1135.92 13
5 9 -4 3642.53 1254.90 6
-5 9 4 5391.53 1461.71 9
-5 -9 -4 3883.09 1188.61 4
5 9 5 641.771 787.153 13
-5 9 5 2702.48 1189.51 9
-5 -9 -5 1707.19 921.817 4
5 9 6 8191.58 1736.72 13
-5 9 6 7070.81 1604.57 9
-5 -9 -6 12454.2 2146.06 4
-5 -9 -7-217.100 475.231 4
-5 -9 -8 9592.83 1893.04 4
-6 -9 0 6848.60 1666.51 11
-6 -9 0 4863.47 1417.75 4
-6 -9 1 2040.39 1017.70 11
-6 -9 1 4127.42 1249.39 4
-6 -9 -1 2367.75 1004.11 4
-6 -9 2 1101.32 920.382 11
-6 9 -2-184.024 496.699 10
-6 -9 -2 285.700 589.154 4
-6 -9 3 2008.22 909.176 11
-6 9 -3 4139.03 1587.00 10
-6 -9 -3 2122.30 887.111 4
6 9 4 149.884 443.995 13
-6 -9 -4 627.492 671.778 4
6 9 5-40.2443 655.208 13
-6 -9 -5-392.564 558.672 4
-7 -9 0-124.756 675.188 4
-7 -9 1 6446.47 1633.26 4
-7 -9 -1 7775.41 1847.70 4
-7 -9 2 943.685 746.060 4
-7 -9 3 1367.47 946.067 4
0 -10 0 48459.5 4644.53 3
0 -10 1-1005.31 873.382 3
0 -10 -1-490.608 665.662 3
0 -10 2 9874.25 2087.56 3
0 -10 -3 462.551 476.218 11
0 -10 3-816.026 502.182 3
0 -10 -4 705.615 632.537 11
0 -10 4-192.236 529.435 3
1 -10 0-590.656 665.336 3
1 -10 0-77.7677 491.562 1
1 -10 -1 13213.8 2318.47 1
-1 -10 1 17631.7 2820.37 3
1 -10 1 16520.2 2634.61 3
1 -10 -1 14302.1 2483.49 3
1 -10 1 14650.5 2476.47 1
-1 10 1 15596.9 2588.28 8
-1 -10 -2 2480.94 1107.25 11
1 -10 -2 1851.98 875.408 1
-1 -10 2 2164.97 1091.43 3
-1 10 2 4266.66 1335.52 8
1 -10 -3 2512.24 1150.82 1
-1 -10 -3 3398.28 1096.85 11
-1 -10 3 3776.94 1321.19 3
-1 10 3 2127.62 1023.37 8
1 -10 -4 5560.00 1604.91 1
1 -10 -4 3406.93 1179.98 11
-1 -10 4 3093.48 1204.64 3
-1 10 4 5071.15 1643.42 8
2 -10 0 4522.97 1498.30 1
-2 10 0 2637.47 1234.17 8
2 -10 1-58.2588 615.677 1
-2 -10 -1 197.146 519.279 11
2 -10 -1 1880.12 1013.52 1
-2 10 1 1451.17 791.485 8
2 -10 2 3881.74 1427.27 1
-2 -10 -2 1609.95 812.327 11
2 -10 3 9171.64 2129.97 1
2 -10 4-394.640 716.351 1
-3 -10 -1 1151.78 698.736 11
0 0 0 0.00 0.00 0
TITL Turin in Pnma
REM Pnma (#62, found as Pmnb in ba-c setting)
CELL 0.71073 9.987060 7.150530 15.716025 90.0000 90.0000 90.0000
ZERR 3.00 0.000240 0.000186 0.000403 0.0000 0.0000 0.0000
LATT 1
SYMM -x+1/2,-y, z+1/2
SYMM -x, y+1/2,-z
SYMM x+1/2,-y+1/2,-z+1/2
SFAC C H N Br Au
UNIT 36.00 84.00 6.00 21.00 3.00
TREF
HKLF 4
END
;
_shelx_hkl_checksum 52790
_shelx_res_file
;
TITL Turin in Pnma
shelx.res
created by SHELXL-2019/3 at 10:01:59 on 08-Mar-2024
CELL 0.71073 9.987060 7.150530 15.716025 90.0000 90.0000 90.0000
ZERR 4.00 0.000500 0.000400 0.000800 0.0000 0.0000 0.0000
LATT 1
SYMM -x+1/2,-y, z+1/2
SYMM -x, y+1/2,-z
SYMM x+1/2,-y+1/2,-z+1/2
SFAC C H N Br Au
UNIT 24.00 52.00 4.00 12.00 4.00
MERG 2
FMAP 2
PLAN 10
L.S. 8
SIZE 0.27 0.06 0.03
TEMP -173
ACTA 60
CONF 2.45
BOND $H
EQIV $1 -x, -y+2, -z
EQIV $2 -x, -y+1, -z
EQIV $3 x+1/2, y, -z-1/2
EQIV $4 -x+1, -y+2, -z
EQIV $5 x-1/2, y, -z+1/2
EQIV $6 x+1/2, y, -z+1/2
HTAB N11 Br2
HTAB C12 Br1_$1
HTAB C12 Br2_$1
HTAB C15 Br2_$3
HTAB C12 Br3
HTAB C13 Br3_$4
HTAB C15 Br3_$4
RTAB DIST Br1 Br3_$5
RTAB ANGL Au1 Br1 Br3_$5
RTAB DIST Br2 Au1_$1
RTAB DIST Br2 Au1_$2
RTAB ANGL Au1 Br2 Au1_$1
RTAB ANGL Au1 Br2 Au1_$2
RTAB DIST Br3 Br1_$6
RTAB ANGL Au1 Br3 Br1_$6
WGHT 0.012100 3.435300
EXTI 0.000514
FVAR 1.31257
AU1 5 0.093152 0.750000 0.046627 10.50000 0.01034 0.01467 =
0.01027 0.00000 0.00112 0.00000
BR1 4 -0.069995 0.750000 0.159326 10.50000 0.01795 0.02533 =
0.01318 0.00000 0.00567 0.00000
BR2 4 -0.080815 0.750000 -0.061223 10.50000 0.01135 0.01625 =
0.01294 0.00000 -0.00046 0.00000
BR3 4 0.267124 0.750000 0.152984 10.50000 0.01719 0.03044 =
0.01353 0.00000 -0.00423 0.00000
N11 3 0.233861 0.750000 -0.052305 10.50000 0.01138 0.02699 =
0.00990 0.00000 0.00011 0.00000
H01 2 0.183691 0.750000 -0.099462 10.50000 0.01283
C12 1 0.318263 0.922492 -0.054691 11.00000 0.01826 0.01558 =
0.02074 0.00198 0.00897 0.00313
AFIX 23
H12A 2 0.373767 0.928684 -0.002574 11.00000 -1.20000
H12B 2 0.259617 1.034089 -0.055751 11.00000 -1.20000
AFIX 0
C13 1 0.408744 0.924135 -0.132449 11.00000 0.01594 0.02195 =
0.01987 0.00534 0.00675 -0.00089
AFIX 23
H13A 2 0.465879 1.037237 -0.131098 11.00000 -1.20000
H13B 2 0.353144 0.929562 -0.184542 11.00000 -1.20000
AFIX 0
C14 1 0.497496 0.750000 -0.135424 10.50000 0.01306 0.01553 =
0.01702 0.00000 0.00659 0.00000
AFIX 13
H14 2 0.554971 0.750002 -0.083321 10.50000 -1.20000
AFIX 0
C15 1 0.589581 0.750000 -0.212936 10.50000 0.01729 0.03276 =
0.02581 0.00000 0.00867 0.00000
AFIX 3
H15A 2 0.534829 0.750000 -0.264018 10.50000 -1.50000
H15B 2 0.647617 0.860443 -0.211145 11.00000 -1.50000
AFIX 0
HKLF 4
REM Turin in Pnma
REM wR2 = 0.0504, GooF = S = 1.110, Restrained GooF = 1.110 for all data
REM R1 = 0.0295 for 1581 Fo > 4sig(Fo) and 0.0422 for all 1864 data
REM 65 parameters refined using 0 restraints
END
WGHT 0.0121 3.4353
REM Highest difference peak 1.564, deepest hole -1.185, 1-sigma level 0.252
Q1 1 0.0916 0.8672 0.0521 11.00000 0.05 1.56
Q2 1 0.5177 1.2500 -0.0782 10.50000 0.05 1.48
Q3 1 0.1233 0.7500 -0.1277 10.50000 0.05 1.20
Q4 1 0.0657 0.7500 0.0064 10.50000 0.05 1.08
Q5 1 0.3342 0.7500 0.1239 10.50000 0.05 1.07
Q6 1 0.3605 0.7500 0.2106 10.50000 0.05 1.07
Q7 1 0.4559 1.2500 -0.1158 10.50000 0.05 1.02
Q8 1 0.3244 1.2500 -0.1677 10.50000 0.05 0.99
Q9 1 -0.1440 0.7500 -0.0770 10.50000 0.05 0.97
Q10 1 0.1465 0.7500 0.2109 10.50000 0.05 0.96
;
_shelx_res_checksum 30500
data_2b
_audit_creation_method 'SHELXL-2019/3'
_chemical_name_systematic
;
Tribromido(4-methylpiperidine)gold(III)
;
_chemical_name_common ?
_chemical_formula_moiety 'C6 H13 Au Br3 N'
_chemical_formula_sum 'C6 H13 Au Br3 N'
_chemical_formula_iupac '[Au Br3 (C6 H13 N)]'
_chemical_formula_weight 535.87
_chemical_melting_point ?
_space_group_crystal_system orthorhombic
_space_group_name_H-M_alt 'P b c a'
_space_group_name_Hall '-P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'
_cell_length_a 12.6471(5)
_cell_length_b 8.7247(3)
_cell_length_c 21.0262(7)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_volume 2320.07(15)
_cell_formula_units_Z 8
_cell_measurement_reflns_used 5682
_cell_measurement_theta_min 3.2160
_cell_measurement_theta_max 29.6930
_cell_measurement_temperature 100(2)
_exptl_crystal_description needle
_exptl_crystal_colour red
_exptl_crystal_size_max 0.14
_exptl_crystal_size_mid 0.04
_exptl_crystal_size_min 0.03
_exptl_crystal_density_diffrn 3.068
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1920
_exptl_absorpt_coefficient_mu 22.964
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2015)
;
_exptl_absorpt_correction_T_min 0.38001
_exptl_absorpt_correction_T_max 1.00000
_diffrn_ambient_temperature 100(2)
_diffrn_source 'Enhance (Mo) X-ray Source'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_measurement_device_type 'Oxford Diffraction Xcalibur, Eos'
_diffrn_measurement_method '\w scan'
_diffrn_detector_area_resol_mean 16.1419
_diffrn_reflns_number 38297
_diffrn_reflns_av_R_equivalents 0.0735
_diffrn_reflns_av_unetI/netI 0.0378
_diffrn_reflns_theta_min 2.519
_diffrn_reflns_theta_max 30.033
_diffrn_reflns_theta_full 30.000
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_limit_h_min -17
_diffrn_reflns_limit_h_max 17
_diffrn_reflns_limit_k_min -11
_diffrn_reflns_limit_k_max 12
_diffrn_reflns_limit_l_min -29
_diffrn_reflns_limit_l_max 29
_refine_special_details ?
_reflns_number_total 3371
_reflns_number_gt 2495
_reflns_threshold_expression 'I > 2\s(I)'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_R_factor_all 0.0520
_refine_ls_R_factor_gt 0.0294
_refine_ls_wR_factor_gt 0.0388
_refine_ls_wR_factor_ref 0.0429
_refine_ls_goodness_of_fit_ref 1.035
_refine_ls_restrained_S_all 1.035
_refine_ls_number_reflns 3371
_refine_ls_number_parameters 105
_refine_ls_number_restraints 0
_refine_ls_hydrogen_treatment mixed
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0081P)^2^+2.1449P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_diff_density_max 0.987
_refine_diff_density_min -0.994
_refine_ls_extinction_method none
_refine_ls_extinction_coef .
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'
'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'
_computing_data_collection
;
CrysAlisPro, Version 1.171.37.35 (Rigaku OD, 2015)
;
_computing_cell_refinement
;
CrysAlisPro, Version 1.171.37.35 (Rigaku OD, 2015)
;
_computing_data_reduction
;
CrysAlisPro, Version 1.171.37.35 (Rigaku OD, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL2019/3 (Sheldrick, 2015)
;
_computing_molecular_graphics
;
XP, Version 5.1 (Bruker, 1998)
;
_computing_publication_material
;
SHELXL2019/3 (Sheldrick, 2015)
;
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 0.24373(2) 0.30618(2) 0.12636(2) 0.01070(5) Uani d 1 . .
Br Br1 0.05410(4) 0.27328(5) 0.12037(2) 0.01833(11) Uani d 1 . .
Br Br2 0.24027(4) 0.47282(5) 0.03411(2) 0.01409(10) Uani d 1 . .
Br Br3 0.24951(4) 0.13133(5) 0.21592(2) 0.01560(10) Uani d 1 . .
N N11 0.4069(3) 0.3465(4) 0.12801(19) 0.0115(8) Uani d 1 . .
H H01 0.416(4) 0.454(5) 0.116(2) 0.019(14) Uiso d 1 . .
C C12 0.4638(4) 0.2527(5) 0.0784(2) 0.0169(11) Uani d 1 . .
H H12A 0.426683 0.261747 0.037140 0.020 Uiso calc 1 . .
H H12B 0.463810 0.143443 0.091066 0.020 Uiso calc 1 . .
C C13 0.5769(4) 0.3088(6) 0.0714(2) 0.0201(11) Uani d 1 . .
H H13A 0.576259 0.415630 0.055540 0.024 Uiso calc 1 . .
H H13B 0.613889 0.244725 0.039599 0.024 Uiso calc 1 . .
C C14 0.6373(4) 0.3028(5) 0.1341(2) 0.0162(10) Uani d 1 . .
H H14 0.640778 0.193362 0.148091 0.019 Uiso calc 1 . .
C C15 0.5762(4) 0.3927(5) 0.1845(2) 0.0154(11) Uani d 1 . .
H H15A 0.612751 0.382498 0.225900 0.018 Uiso calc 1 . .
H H15B 0.575849 0.502588 0.172813 0.018 Uiso calc 1 . .
C C16 0.4628(4) 0.3372(5) 0.1914(2) 0.0180(11) Uani d 1 . .
H H16A 0.462434 0.229940 0.206773 0.022 Uiso calc 1 . .
H H16B 0.425261 0.401276 0.222985 0.022 Uiso calc 1 . .
C C17 0.7504(4) 0.3616(6) 0.1266(2) 0.0253(11) Uani d 1 . .
H H17A 0.748980 0.471144 0.116451 0.038 Uiso calc 1 . .
H H17B 0.785491 0.305515 0.092217 0.038 Uiso calc 1 . .
H H17C 0.789141 0.345693 0.166448 0.038 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 0.01025(9) 0.00994(8) 0.01190(8) 0.00053(7) 0.00084(8) -0.00021(7)
Br1 0.0108(2) 0.0184(2) 0.0259(3) -0.00129(18) 0.0015(2) 0.0018(2)
Br2 0.0151(2) 0.0137(2) 0.0135(2) -0.0008(2) -0.0013(2) 0.00201(17)
Br3 0.0207(3) 0.0128(2) 0.0133(2) 0.0001(2) 0.0017(2) 0.00118(17)
N11 0.011(2) 0.0125(19) 0.011(2) -0.0006(15) -0.0018(17) 0.0001(16)
C12 0.016(3) 0.021(3) 0.013(2) 0.001(2) 0.003(2) -0.0075(19)
C13 0.015(3) 0.025(3) 0.021(3) 0.002(2) 0.000(2) -0.001(2)
C14 0.011(2) 0.018(2) 0.020(3) -0.002(2) -0.002(2) 0.002(2)
C15 0.013(3) 0.016(2) 0.017(3) 0.003(2) -0.008(2) -0.002(2)
C16 0.016(3) 0.021(3) 0.017(3) 0.001(2) -0.002(2) -0.003(2)
C17 0.018(3) 0.034(3) 0.024(3) -0.006(2) -0.003(3) 0.007(2)
_geom_special_details ?
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 . 2.094(4) y
Au1 Br1 . 2.4187(5) y
Au1 Br2 . 2.4244(5) y
Au1 Br3 . 2.4246(5) y
N11 C12 . 1.508(6) ?
N11 C16 . 1.511(6) ?
N11 H01 . 0.97(4) ?
C12 C13 . 1.518(7) ?
C12 H12A . 0.9900 ?
C12 H12B . 0.9900 ?
C13 C14 . 1.524(7) ?
C13 H13A . 0.9900 ?
C13 H13B . 0.9900 ?
C14 C15 . 1.527(6) ?
C14 C17 . 1.527(6) ?
C14 H14 . 1.0000 ?
C15 C16 . 1.520(7) ?
C15 H15A . 0.9900 ?
C15 H15B . 0.9900 ?
C16 H16A . 0.9900 ?
C16 H16B . 0.9900 ?
C17 H17A . 0.9800 ?
C17 H17B . 0.9800 ?
C17 H17C . 0.9800 ?
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 Br1 . . 176.50(11) y
N11 Au1 Br2 . . 86.00(11) y
Br1 Au1 Br2 . . 90.665(18) y
N11 Au1 Br3 . . 93.62(11) y
Br1 Au1 Br3 . . 89.751(18) y
Br2 Au1 Br3 . . 177.736(17) y
C12 N11 C16 . . 110.9(4) y
C12 N11 Au1 . . 111.6(3) y
C16 N11 Au1 . . 117.8(3) y
C12 N11 H01 . . 107(3) ?
C16 N11 H01 . . 102(3) ?
Au1 N11 H01 . . 106(3) ?
N11 C12 C13 . . 110.0(4) ?
N11 C12 H12A . . 109.7 ?
C13 C12 H12A . . 109.7 ?
N11 C12 H12B . . 109.7 ?
C13 C12 H12B . . 109.7 ?
H12A C12 H12B . . 108.2 ?
C12 C13 C14 . . 112.2(4) ?
C12 C13 H13A . . 109.2 ?
C14 C13 H13A . . 109.2 ?
C12 C13 H13B . . 109.2 ?
C14 C13 H13B . . 109.2 ?
H13A C13 H13B . . 107.9 ?
C13 C14 C15 . . 109.2(4) ?
C13 C14 C17 . . 111.6(4) ?
C15 C14 C17 . . 111.9(4) ?
C13 C14 H14 . . 108.0 ?
C15 C14 H14 . . 108.0 ?
C17 C14 H14 . . 108.0 ?
C16 C15 C14 . . 112.3(4) ?
C16 C15 H15A . . 109.1 ?
C14 C15 H15A . . 109.1 ?
C16 C15 H15B . . 109.1 ?
C14 C15 H15B . . 109.1 ?
H15A C15 H15B . . 107.9 ?
N11 C16 C15 . . 109.9(4) ?
N11 C16 H16A . . 109.7 ?
C15 C16 H16A . . 109.7 ?
N11 C16 H16B . . 109.7 ?
C15 C16 H16B . . 109.7 ?
H16A C16 H16B . . 108.2 ?
C14 C17 H17A . . 109.5 ?
C14 C17 H17B . . 109.5 ?
H17A C17 H17B . . 109.5 ?
C14 C17 H17C . . 109.5 ?
H17A C17 H17C . . 109.5 ?
H17B C17 H17C . . 109.5 ?
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
Br2 Au1 N11 C12 . . . . -78.0(3) y
Br3 Au1 N11 C12 . . . . 99.8(3) y
Br2 Au1 N11 C16 . . . . 152.0(3) y
Br3 Au1 N11 C16 . . . . -30.2(3) y
C16 N11 C12 C13 . . . . -58.4(5) ?
Au1 N11 C12 C13 . . . . 168.1(3) y
N11 C12 C13 C14 . . . . 57.4(5) ?
C12 C13 C14 C15 . . . . -55.0(5) ?
C12 C13 C14 C17 . . . . -179.2(4) y
C13 C14 C15 C16 . . . . 54.8(5) ?
C17 C14 C15 C16 . . . . 178.9(4) y
C12 N11 C16 C15 . . . . 58.0(5) ?
Au1 N11 C16 C15 . . . . -171.6(3) y
C14 C15 C16 N11 . . . . -56.8(5) ?
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 Br1 8_665 0.97(4) 2.81(4) 3.759(4) 164(4) yes
C12 H12A Br2 . 0.99 2.99 3.542(5) 116.2 yes
C13 H13B Br2 4 0.99 2.93 3.903(5) 169.4 yes
C16 H16B Br3 8_665 0.99 2.99 3.750(5) 134.5 yes
_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 0.141
_shelx_estimated_absorpt_T_max 0.546
_shelx_hkl_file
;
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-7 11 6 602.049 347.802 5
7 11 -6 479.292 334.211 7
7 11 6 941.958 522.466 3
-7 -11 -6 267.260 300.114 6
-7 11 7-500.445 319.043 5
7 11 -7-542.464 396.349 7
-7 -11 -7-346.968 280.734 6
7 11 -8 455.169 304.475 7
-7 -11 -8-153.520 327.235 6
7 11 -9-2.65854 290.535 7
-8 11 2 307.696 341.547 5
8 11 -2-280.663 308.143 7
8 11 2 215.106 347.063 3
-8 11 3 1082.59 522.546 5
8 11 -3 773.367 406.812 7
8 11 3-227.477 383.686 3
-8 11 4 314.912 393.209 5
8 11 -4 896.157 416.689 7
8 11 4 534.144 492.964 3
-8 11 5 803.349 429.883 5
-8 11 6-344.186 401.471 5
-8 11 7 650.301 410.098 5
9 11 2 709.960 367.421 3
-1 12 -9 2756.61 668.887 5
2 12 0 8923.44 1165.51 8
2 12 -1 10174.1 1259.50 8
2 12 -2-381.093 389.382 8
-2 12 -7 1666.29 559.256 5
-2 12 -8 1313.61 518.201 5
3 12 0 868.005 448.148 8
3 12 -1 13745.0 1457.90 8
3 12 1 14161.7 1479.74 8
3 12 -2 4225.02 841.730 8
3 12 2 5873.41 996.436 8
3 12 -3 5255.11 923.169 8
3 12 -4-35.1075 312.950 8
-3 12 -5 2594.06 630.062 5
-3 12 -6 690.866 487.523 5
-3 12 -7 3409.17 711.341 5
4 12 0 7778.73 1090.71 8
4 12 -1 6281.44 986.216 8
4 12 1 5108.08 905.397 8
4 12 -2-11.2130 305.694 8
4 12 2 76.2646 312.489 8
-4 12 -3 3175.56 715.413 5
4 12 -3 3584.87 793.780 8
-4 12 -4-9.57532 303.993 5
4 12 -4-73.9374 331.583 8
-4 12 -5 1552.70 537.835 5
4 12 -5 607.728 365.351 8
5 12 0-178.826 255.652 8
5 12 -1 4595.16 866.033 8
-5 12 -1 4280.67 786.080 5
5 12 1 4251.45 831.947 8
5 12 -2 3225.60 670.458 8
-5 12 -2 2534.23 616.494 5
-5 12 -3 502.462 351.383 5
5 12 -3 1705.51 539.857 8
5 12 3 1243.85 502.104 8
5 12 -4 1204.85 576.607 8
5 12 -5-246.163 285.139 8
-6 12 0 8027.85 1125.43 5
0 0 0 0.00 0.00 0
TITL Rennes in Pbca
REM Pbca (#61, found as Pcab in ba-c setting)
CELL 0.71073 12.647128 8.724666 21.026178 90.0000 90.0000 90.0000
ZERR 12.00 0.000243 0.000152 0.000359 0.0000 0.0000 0.0000
LATT 1
SYMM -x+1/2,-y, z+1/2
SYMM -x, y+1/2,-z+1/2
SYMM x+1/2,-y+1/2,-z
SFAC C H N Br Au
UNIT 72.00 156.00 12.00 36.00 12.00
TREF
HKLF 4
END
;
_shelx_hkl_checksum 86606
_shelx_res_file
;
TITL Rennes in Pbca
shelx.res
created by SHELXL-2019/3 at 10:11:57 on 08-Mar-2024
CELL 0.71073 12.647128 8.724666 21.026178 90.0000 90.0000 90.0000
ZERR 8.00 0.000510 0.000340 0.000720 0.0000 0.0000 0.0000
LATT 1
SYMM -x+1/2,-y, z+1/2
SYMM -x, y+1/2,-z+1/2
SYMM x+1/2,-y+1/2,-z
SFAC C H N Au Br
UNIT 48.00 104.00 8.00 8.00 24.00
L.S. 8
FMAP 2
PLAN 10
SIZE 0.14 0.04 0.03
TEMP -173
SHEL 999 0.71
ACTA 60
BOND $H
CONF 2.45
EQIV $1 -x+1/2, y+1/2, z
EQIV $2 x+1/2, -y+1/2, -z
EQIV $3 -x+1/2, y-1/2, z
HTAB N11 Br1_$1
HTAB C12 Br2
HTAB C13 Br2_$2
HTAB C16 Br3_$1
RTAB DIST Au1 Au1_$1
RTAB DIST Au1 Au1_$3
RTAB ANGL Au1_$1 Au1 Au1_$3
RTAB DIST Au1 Br2_$3
RTAB DIST Au1 Br3_$1
RTAB DIST Br2 Au1_$1
RTAB ANGL Au1 Br2 Au1_$1
RTAB DIST Br3 Au1_$3
RTAB ANGL Au1 Br3 Au1_$3
WGHT 0.008100 2.144900
FVAR 0.49599
AU1 4 0.243730 0.306176 0.126360 11.00000 0.01025 0.00994 =
0.01190 -0.00021 0.00084 0.00053
BR1 5 0.054096 0.273276 0.120371 11.00000 0.01077 0.01837 =
0.02586 0.00177 0.00153 -0.00129
BR2 5 0.240266 0.472815 0.034112 11.00000 0.01507 0.01368 =
0.01351 0.00201 -0.00133 -0.00084
BR3 5 0.249508 0.131327 0.215921 11.00000 0.02069 0.01276 =
0.01335 0.00118 0.00168 0.00009
N11 3 0.406903 0.346503 0.128012 11.00000 0.01098 0.01251 =
0.01108 0.00007 -0.00185 -0.00065
H01 2 0.416296 0.453787 0.116399 11.00000 0.01930
C12 1 0.463827 0.252743 0.078417 11.00000 0.01628 0.02091 =
0.01344 -0.00751 0.00258 0.00090
AFIX 23
H12A 2 0.426683 0.261747 0.037140 11.00000 -1.20000
H12B 2 0.463810 0.143443 0.091066 11.00000 -1.20000
AFIX 0
C13 1 0.576882 0.308829 0.071441 11.00000 0.01462 0.02492 =
0.02068 -0.00110 0.00021 0.00245
AFIX 23
H13A 2 0.576259 0.415630 0.055540 11.00000 -1.20000
H13B 2 0.613889 0.244725 0.039599 11.00000 -1.20000
AFIX 0
C14 1 0.637265 0.302808 0.134126 11.00000 0.01112 0.01778 =
0.01982 0.00172 -0.00231 -0.00235
AFIX 13
H14 2 0.640778 0.193362 0.148091 11.00000 -1.20000
AFIX 0
C15 1 0.576202 0.392655 0.184477 11.00000 0.01273 0.01596 =
0.01739 -0.00210 -0.00784 0.00286
AFIX 23
H15A 2 0.612751 0.382498 0.225900 11.00000 -1.20000
H15B 2 0.575849 0.502588 0.172813 11.00000 -1.20000
AFIX 0
C16 1 0.462830 0.337175 0.191381 11.00000 0.01561 0.02108 =
0.01722 -0.00270 -0.00234 0.00080
AFIX 23
H16A 2 0.462434 0.229940 0.206773 11.00000 -1.20000
H16B 2 0.425261 0.401276 0.222985 11.00000 -1.20000
AFIX 0
C17 1 0.750352 0.361554 0.126640 11.00000 0.01776 0.03403 =
0.02410 0.00663 -0.00322 -0.00605
AFIX 137
H17A 2 0.748980 0.471144 0.116451 11.00000 -1.50000
H17B 2 0.785491 0.305515 0.092217 11.00000 -1.50000
H17C 2 0.789141 0.345693 0.166448 11.00000 -1.50000
AFIX 0
HKLF 4
REM Rennes in Pbca
REM wR2 = 0.0429, GooF = S = 1.035, Restrained GooF = 1.035 for all data
REM R1 = 0.0294 for 2495 Fo > 4sig(Fo) and 0.0520 for all 3371 data
REM 105 parameters refined using 0 restraints
END
WGHT 0.0081 2.1436
REM Highest difference peak 0.987, deepest hole -0.994, 1-sigma level 0.227
Q1 1 0.1990 0.4752 0.0684 11.00000 0.05 0.99
Q2 1 0.1084 0.1755 0.1210 11.00000 0.05 0.90
Q3 1 0.4019 0.4749 0.2308 11.00000 0.05 0.89
Q4 1 0.3585 0.4798 0.1202 11.00000 0.05 0.88
Q5 1 0.2572 0.2524 0.1875 11.00000 0.05 0.83
Q6 1 0.7807 0.2343 0.0716 11.00000 0.05 0.82
Q7 1 0.6213 0.3597 0.1902 11.00000 0.05 0.79
Q8 1 0.3236 0.3787 0.1491 11.00000 0.05 0.79
Q9 1 0.2814 0.2949 0.1821 11.00000 0.05 0.79
Q10 1 0.5560 0.1102 0.1743 11.00000 0.05 0.78
;
_shelx_res_checksum 57991
data_global
_journal_date_recd_electronic 2024-03-25
_journal_date_accepted 2024-03-29
_journal_name_full 'Acta Crystallographica, Section E'
_journal_year 2024
_journal_volume 80
_journal_issue 5
_journal_page_first 0
_journal_page_last 0
_journal_paper_category GM
_journal_paper_doi 10.1107/S2056989024002822
_journal_coeditor_code PK2705
_publ_contact_author_name
;
Peter G. Jones
;
_publ_contact_author_address
;
Institut f\"ur Anorganische und Analytische Chemie
Technische Universit\"at Braunschweig
Hagenring 30
D-38106 Braunschweig
Germany
;
_publ_contact_author_email 'p.jones@tu-braunschweig.de'
_publ_contact_author_fax ?
_publ_contact_author_phone ?
_publ_section_title
;
Crystal structures of trichlorido(4-methylpiperidine)gold(III) and two
polymorphs of tribromido(4-methylpiperidine)gold(III)
;
_publ_section_title_footnote
;
Gold complexes with amine ligands, Part 15. Part 14: D\"oring & Jones
(2023b).
;
loop_
_publ_author_name
_publ_author_address
'D\"oring, Cindy'
;
Institut f\"ur Anorganische und Analytische Chemie
Technische Universit\"at Braunschweig
Hagenring 30
D-38106 Braunschweig
Germany
;
'Jones, Peter G.'
;
Institut f\"ur Anorganische und Analytische Chemie
Technische Universit\"at Braunschweig
Hagenring 30
D-38106 Braunschweig
Germany
;
_publ_section_synopsis
;
All three structures involve chains of molecules linked by Au...halogen
contacts; these are accompanied by hydrogen bonds or halogen...halogen
contacts.
;