# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2018
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
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# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
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data_cxy0041a
_database_code_depnum_ccdc_archive 'CCDC 1844720'
_audit_update_record
;
2018-10-10 deposited with the CCDC.
2018-10-12 downloaded from the CCDC.
;
_audit_creation_date 2018-10-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number 2016/6
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C16 H16 Au2 N10'
_chemical_formula_sum 'C16 H16 Au2 N10'
_chemical_formula_weight 742.32
_chemical_melting_point ?
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_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.
;
_space_group_crystal_system monoclinic
_space_group_IT_number 12
_space_group_name_H-M_alt 'C 1 2/m 1'
_space_group_name_Hall '-C 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'
_cell_length_a 13.0911(14)
_cell_length_b 6.4907(7)
_cell_length_c 11.9991(14)
_cell_angle_alpha 90
_cell_angle_beta 105.112(4)
_cell_angle_gamma 90
_cell_volume 984.31(19)
_cell_formula_units_Z 2
_cell_measurement_reflns_used 7242
_cell_measurement_temperature 150
_cell_measurement_theta_max 27.48
_cell_measurement_theta_min 3.22
_shelx_estimated_absorpt_T_max 0.663
_shelx_estimated_absorpt_T_min 0.081
_exptl_absorpt_coefficient_mu 14.912
_exptl_absorpt_correction_T_max 0.68
_exptl_absorpt_correction_T_min 0.37
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details SADABS
_exptl_absorpt_special_details ?
_exptl_crystal_colour yellow
_exptl_crystal_colour_primary yellow
_exptl_crystal_density_diffrn 2.505
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description plate
_exptl_crystal_F_000 680
_exptl_crystal_size_max 0.34
_exptl_crystal_size_mid 0.28
_exptl_crystal_size_min 0.03
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0710
_diffrn_reflns_av_unetI/netI 0.0313
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max 15
_diffrn_reflns_limit_h_min -15
_diffrn_reflns_limit_k_max 7
_diffrn_reflns_limit_k_min -7
_diffrn_reflns_limit_l_max 13
_diffrn_reflns_limit_l_min -13
_diffrn_reflns_number 11074
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full 24.402
_diffrn_reflns_theta_max 24.402
_diffrn_reflns_theta_min 3.224
_diffrn_ambient_temperature 150
_diffrn_detector 'Bruker PHOTO 100 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type 'CCD area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device 'three-circle diffractometer'
_diffrn_measurement_device_type 'Bruker PHOTO 100 area detector'
_diffrn_measurement_method '\w and \f scans'
_diffrn_radiation_monochromator 'mirror optics'
_diffrn_radiation_probe x-ray
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'microfocus sealed X-ray tube'
_diffrn_source_type 'Incoatec I\ms'
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 663
_reflns_number_total 894
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement ?
_computing_data_collection ?
_computing_data_reduction ?
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'XL (Sheldrick, 2008)'
_computing_structure_solution 'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max 1.250
_refine_diff_density_min -1.287
_refine_diff_density_rms 0.203
_refine_ls_extinction_coef 0.0018(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method 'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref 1.047
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 93
_refine_ls_number_reflns 894
_refine_ls_number_restraints 17
_refine_ls_R_factor_all 0.0361
_refine_ls_R_factor_gt 0.0264
_refine_ls_restrained_S_all 1.042
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0617P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0792
_refine_ls_wR_factor_ref 0.0886
_refine_special_details
;
Location of maximum Q peak
Atom Peak x y z
Q1 1.25 0.0522 0.2511 0.0964
Distances to nearest atoms (including eq.)
1.83 C1 1.96 C8 2.00 Au2 2.01 Au1
;
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H) groups, All C(H,H,H) groups
2. Restrained distances
C6-H6B = C6-H6A
0.98 with sigma of 0.02
H6A-H6B
1.58 with sigma of 0.02
N4-H6B
2 with sigma of 0.04
N4-H6A
2 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C8) \\sim Ueq, Uanis(N5) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Others
Fixed Sof: H7C(0.5) H7B(0.5) H7A(0.5)
5.a Riding coordinates:
C7(H7C,H7B,H7A)
5.b Aromatic/amide H refined with riding coordinates:
C4(H4), C3(H3)
;
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary dual
_atom_sites_solution_secondary ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Au1 Au 0.000000 0.000000 0.000000 0.0292(3) Uani 1 4 d S T P . .
N1 N 0.0668(6) 0.000000 0.2608(6) 0.0300(19) Uani 1 2 d S T P . .
N4 N 0.2044(7) 0.000000 0.1904(8) 0.028(2) Uani 1 2 d DS T P . .
N3 N 0.3423(6) 0.000000 0.3723(7) 0.0299(19) Uani 1 2 d S T P . .
N2 N 0.1611(8) 0.000000 0.4657(8) 0.033(2) Uani 1 2 d S T P . .
C7 C -0.0410(7) 0.000000 0.2724(10) 0.046(3) Uani 1 2 d S T P . .
H7C H -0.044388 0.082130 0.339918 0.055 Uiso 0.5 1 d R . . A -1
H7B H -0.062868 -0.141760 0.282277 0.055 Uiso 0.5 1 d R . . A -1
H7A H -0.088318 0.059630 0.202937 0.055 Uiso 0.5 1 d R . . A -1
C6 C 0.2700(9) 0.000000 0.1110(9) 0.041(3) Uani 1 2 d DS T P . .
C1 C 0.0961(8) 0.000000 0.1616(8) 0.029(2) Uani 1 2 d S T P . .
C5 C 0.2437(8) 0.000000 0.3094(8) 0.029(2) Uani 1 2 d S T P . .
C4 C 0.3488(9) 0.000000 0.4847(10) 0.036(3) Uani 1 2 d S T P . .
H4 H 0.417390 0.000000 0.536596 0.043 Uiso 1 2 calc RS T P . .
C2 C 0.1565(7) 0.000000 0.3553(8) 0.024(2) Uani 1 2 d S T P . .
C3 C 0.2614(8) 0.000000 0.5322(11) 0.034(3) Uani 1 2 d S T P . .
H3 H 0.273347 0.000000 0.613788 0.041 Uiso 1 2 calc RS T P . .
Au2 Au 0.000000 0.500000 0.000000 0.0272(3) Uani 1 4 d S T P . .
N5 N 0.2041(10) 0.500000 0.1843(10) 0.039(3) Uani 1 2 d S TU P . .
C8 C 0.1400(9) 0.500000 0.1275(10) 0.029(3) Uani 1 2 d S TU P . .
H6B H 0.318(3) -0.117(6) 0.128(3) 0.035 Uiso 1 1 d DR . . . .
H6A H 0.230(3) 0.000000 0.0324(15) 0.035 Uiso 1 2 d DRS T P . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Au1 0.0370(4) 0.0201(4) 0.0275(4) 0.000 0.0029(3) 0.000
N1 0.034(4) 0.023(5) 0.032(5) 0.000 0.008(4) 0.000
N4 0.032(5) 0.020(5) 0.036(6) 0.000 0.014(4) 0.000
N3 0.035(5) 0.020(4) 0.035(5) 0.000 0.010(4) 0.000
N2 0.045(6) 0.021(5) 0.034(5) 0.000 0.013(5) 0.000
C7 0.039(6) 0.053(8) 0.049(7) 0.000 0.015(5) 0.000
C6 0.057(7) 0.036(7) 0.043(7) 0.000 0.036(6) 0.000
C1 0.042(6) 0.016(5) 0.027(6) 0.000 0.005(5) 0.000
C5 0.047(6) 0.021(5) 0.022(5) 0.000 0.014(5) 0.000
C4 0.048(6) 0.017(5) 0.046(7) 0.000 0.017(6) 0.000
C2 0.031(5) 0.018(5) 0.028(6) 0.000 0.014(5) 0.000
C3 0.049(9) 0.019(7) 0.035(6) 0.000 0.011(6) 0.000
Au2 0.0316(4) 0.0218(4) 0.0297(4) 0.000 0.0105(3) 0.000
N5 0.065(7) 0.022(5) 0.036(6) 0.000 0.026(6) 0.000
C8 0.037(6) 0.018(5) 0.038(6) 0.000 0.021(5) 0.000
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Au1 C1 2.017(10) 5 ?
Au1 C1 2.017(10) . ?
Au1 Au2 3.2454(4) 1_545 ?
Au1 Au2 3.2454(4) . ?
N1 C7 1.453(11) . ?
N1 C1 1.343(11) . ?
N1 C2 1.404(11) . ?
N4 C6 1.438(12) . ?
N4 C1 1.369(14) . ?
N4 C5 1.386(13) . ?
N3 C5 1.315(11) . ?
N3 C4 1.329(13) . ?
N2 C2 1.311(12) . ?
N2 C3 1.346(14) . ?
C7 H7C 0.9803 . ?
C7 H7B 0.9801 . ?
C7 H7A 0.9797 . ?
C6 H6B 0.972(18) . ?
C6 H6B 0.972(18) 6 ?
C6 H6A 0.952(18) . ?
C5 C2 1.390(10) . ?
C4 H4 0.9500 . ?
C4 C3 1.406(13) . ?
C3 H3 0.9500 . ?
Au2 C8 2.059(12) . ?
Au2 C8 2.059(12) 5_565 ?
N5 C8 0.933(15) . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Au1 C1 180.0 5 . ?
C1 Au1 Au2 90.0 . 1_545 ?
C1 Au1 Au2 90.0 5 . ?
C1 Au1 Au2 90.0 5 1_545 ?
C1 Au1 Au2 90.0 . . ?
Au2 Au1 Au2 180.0 1_545 . ?
C1 N1 C7 126.4(9) . . ?
C1 N1 C2 110.1(8) . . ?
C2 N1 C7 123.5(8) . . ?
C1 N4 C6 126.2(9) . . ?
C1 N4 C5 109.9(8) . . ?
C5 N4 C6 123.9(9) . . ?
C5 N3 C4 112.2(8) . . ?
C2 N2 C3 112.3(9) . . ?
N1 C7 H7C 109.5 . . ?
N1 C7 H7B 109.5 . . ?
N1 C7 H7A 109.5 . . ?
H7C C7 H7B 109.5 . . ?
H7C C7 H7A 109.5 . . ?
H7B C7 H7A 109.5 . . ?
N4 C6 H6B 108(2) . . ?
N4 C6 H6B 108(2) . 6 ?
N4 C6 H6A 113(2) . . ?
H6B C6 H6B 103(7) . 6 ?
H6B C6 H6A 112(2) . . ?
H6A C6 H6B 112(2) . 6 ?
N1 C1 Au1 126.9(7) . . ?
N1 C1 N4 107.0(8) . . ?
N4 C1 Au1 126.0(7) . . ?
N4 C5 C2 106.6(8) . . ?
N3 C5 N4 129.6(8) . . ?
N3 C5 C2 123.8(8) . . ?
N3 C4 H4 117.7 . . ?
N3 C4 C3 124.6(11) . . ?
C3 C4 H4 117.7 . . ?
N2 C2 N1 128.7(8) . . ?
N2 C2 C5 125.1(9) . . ?
C5 C2 N1 106.3(8) . . ?
N2 C3 C4 122.0(12) . . ?
N2 C3 H3 119.0 . . ?
C4 C3 H3 119.0 . . ?
Au1 Au2 Au1 180.0 . 1_565 ?
C8 Au2 Au1 90.0 . . ?
C8 Au2 Au1 90.0 5_565 1_565 ?
C8 Au2 Au1 90.0 5_565 . ?
C8 Au2 Au1 90.0 . 1_565 ?
C8 Au2 C8 180.0 . 5_565 ?
N5 C8 Au2 179.0(12) . . ?
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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N4 C5 C2 N1 0.000(1) . . . . ?
N4 C5 C2 N2 180.000(2) . . . . ?
N3 C5 C2 N1 180.000(1) . . . . ?
N3 C5 C2 N2 0.000(2) . . . . ?
N3 C4 C3 N2 0.000(3) . . . . ?
C7 N1 C1 Au1 0.000(1) . . . . ?
C7 N1 C1 N4 180.000(1) . . . . ?
C7 N1 C2 N2 0.000(2) . . . . ?
C7 N1 C2 C5 180.000(1) . . . . ?
C6 N4 C1 Au1 0.000(1) . . . . ?
C6 N4 C1 N1 180.000(1) . . . . ?
C6 N4 C5 N3 0.000(1) . . . . ?
C6 N4 C5 C2 180.000(1) . . . . ?
C1 N1 C2 N2 180.000(1) . . . . ?
C1 N1 C2 C5 0.000(1) . . . . ?
C1 N4 C5 N3 180.000(1) . . . . ?
C1 N4 C5 C2 0.000(1) . . . . ?
C5 N4 C1 Au1 180.000(1) . . . . ?
C5 N4 C1 N1 0.000(1) . . . . ?
C5 N3 C4 C3 0.000(3) . . . . ?
C4 N3 C5 N4 180.000(1) . . . . ?
C4 N3 C5 C2 0.000(2) . . . . ?
C2 N1 C1 Au1 180.000(1) . . . . ?
C2 N1 C1 N4 0.000(1) . . . . ?
C2 N2 C3 C4 0.000(3) . . . . ?
C3 N2 C2 N1 180.000(2) . . . . ?
C3 N2 C2 C5 0.000(2) . . . . ?
_iucr_refine_instructions_details
;
TITL mo_cxy0041a.res in C2/m
cxy0041a.res
created by SHELXL-2016/6 at 10:02:37 on 10-Oct-2018
CELL 0.71073 13.0911 6.4907 11.9991 90 105.112 90
ZERR 2 0.0014 0.0007 0.0014 0 0.004 0
LATT 7
SYMM -X,+Y,-Z
SFAC C H Au N
UNIT 32 32 4 20
DFIX 0.98 C6 H6b C6 H6a
DANG 1.58 0.02 H6a H6b
DANG 2 N4 H6b
DANG 2 0.02 N4 H6a
ISOR 0.01 0.02 C8 N5
L.S. 5
PLAN -50
SIZE 0.34 0.28 0.03
TEMP -123.15
BOND $H
CONF
fmap 2
acta
OMIT -2 0 1
REM
REM
REM
WGHT 0.061700
EXTI 0.001834
FVAR 0.06593
AU1 3 0.000000 0.000000 0.000000 10.25000 0.03702 0.02006 =
0.02752 0.00000 0.00286 0.00000
N1 4 0.066800 0.000000 0.260812 10.50000 0.03417 0.02324 =
0.03217 0.00000 0.00808 0.00000
N4 4 0.204445 0.000000 0.190351 10.50000 0.03175 0.01996 =
0.03634 0.00000 0.01402 0.00000
N3 4 0.342274 0.000000 0.372345 10.50000 0.03451 0.02028 =
0.03545 0.00000 0.01006 0.00000
N2 4 0.161127 0.000000 0.465708 10.50000 0.04463 0.02128 =
0.03427 0.00000 0.01348 0.00000
C7 1 -0.040958 0.000000 0.272428 10.50000 0.03866 0.05281 =
0.04920 0.00000 0.01501 0.00000
PART -1
AFIX 3
H7C 2 -0.044388 0.082130 0.339918 10.50000 -1.20000
H7B 2 -0.062868 -0.141760 0.282277 10.50000 -1.20000
H7A 2 -0.088318 0.059630 0.202937 10.50000 -1.20000
AFIX 0
PART 0
C6 1 0.269952 0.000000 0.110971 10.50000 0.05670 0.03580 =
0.04330 0.00000 0.03566 0.00000
C1 1 0.096131 0.000000 0.161573 10.50000 0.04179 0.01557 =
0.02682 0.00000 0.00457 0.00000
C5 1 0.243678 0.000000 0.309360 10.50000 0.04740 0.02109 =
0.02157 0.00000 0.01399 0.00000
C4 1 0.348796 0.000000 0.484707 10.50000 0.04833 0.01724 =
0.04594 0.00000 0.01743 0.00000
AFIX 43
H4 2 0.417390 0.000000 0.536596 10.50000 -1.20000
AFIX 0
C2 1 0.156529 0.000000 0.355289 10.50000 0.03055 0.01768 =
0.02772 0.00000 0.01411 0.00000
C3 1 0.261352 0.000000 0.532218 10.50000 0.04875 0.01914 =
0.03489 0.00000 0.01075 0.00000
AFIX 43
H3 2 0.273347 0.000000 0.613788 10.50000 -1.20000
AFIX 0
AU2 3 0.000000 0.500000 0.000000 10.25000 0.03158 0.02180 =
0.02973 0.00000 0.01047 0.00000
N5 4 0.204103 0.500000 0.184348 10.50000 0.06525 0.02211 =
0.03624 0.00000 0.02643 0.00000
C8 1 0.140030 0.500000 0.127525 10.50000 0.03696 0.01797 =
0.03783 0.00000 0.02086 0.00000
H6B 2 0.317596 -0.117375 0.128434 11.00000 -1.20000
H6A 2 0.229729 0.000000 0.032422 10.50000 -1.20000
HKLF 4
REM mo_cxy0041a.res in C2/m
REM R1 = 0.0264 for 663 Fo > 4sig(Fo) and 0.0361 for all 894 data
REM 93 parameters refined using 17 restraints
END
WGHT 0.0617 0.0000
REM Highest difference peak 1.250, deepest hole -1.287, 1-sigma level 0.203
Q1 1 0.0522 0.2511 0.0964 11.00000 0.05 1.25
Q2 1 -0.0323 0.5000 -0.1421 10.50000 0.05 0.91
Q3 1 -0.1334 0.5000 -0.1632 10.50000 0.05 0.88
Q4 1 0.1451 0.0000 0.1620 10.50000 0.05 0.81
Q5 1 0.2391 0.0000 0.1640 10.50000 0.05 0.68
Q6 1 0.0360 0.0000 0.1420 10.50000 0.05 0.67
Q7 1 0.2296 0.5000 0.1688 10.50000 0.05 0.67
Q8 1 0.0457 0.0000 -0.0678 10.50000 0.05 0.54
Q9 1 0.1964 0.0000 0.4880 10.50000 0.05 0.53
Q10 1 0.0000 -0.3178 0.0000 10.50000 0.05 0.52
Q11 1 0.0817 0.2521 -0.1224 11.00000 0.05 0.52
Q12 1 -0.0532 0.0000 0.3411 10.50000 0.05 0.50
Q13 1 0.3108 0.0000 0.5179 10.50000 0.05 0.49
Q14 1 -0.0580 0.5000 0.0743 10.50000 0.05 0.49
Q15 1 0.0421 0.5000 -0.2591 10.50000 0.05 0.48
Q16 1 0.2292 0.0000 0.2408 10.50000 0.05 0.47
Q17 1 0.0000 0.1882 0.0000 10.50000 0.05 0.46
Q18 1 0.3573 0.0000 0.1863 10.50000 0.05 0.44
Q19 1 0.0690 0.0000 -0.1575 10.50000 0.05 0.43
Q20 1 0.0983 0.0000 0.3190 10.50000 0.05 0.42
Q21 1 0.2634 0.0000 0.6774 10.50000 0.05 0.42
Q22 1 0.1954 0.0000 0.3201 10.50000 0.05 0.38
Q23 1 -0.0374 0.5000 -0.2532 10.50000 0.05 0.37
Q24 1 0.4142 0.0000 0.6779 10.50000 0.05 0.37
Q25 1 -0.1478 0.0000 0.1805 10.50000 0.05 0.37
Q26 1 0.0706 0.5000 0.2459 10.50000 0.05 0.36
Q27 1 0.3938 0.0747 0.2867 11.00000 0.05 0.36
Q28 1 0.0816 0.0000 0.5379 10.50000 0.05 0.35
Q29 1 0.3989 0.0000 0.1503 10.50000 0.05 0.35
Q30 1 -0.0778 -0.3152 0.0082 11.00000 0.05 0.34
Q31 1 0.2464 0.1846 0.2227 11.00000 0.05 0.33
Q32 1 0.0754 0.0000 0.2359 10.50000 0.05 0.33
Q33 1 0.2884 0.5000 0.0767 10.50000 0.05 0.33
Q34 1 0.1602 0.0000 0.6292 10.50000 0.05 0.33
Q35 1 0.0970 0.1734 -0.0145 11.00000 0.05 0.32
Q36 1 0.0141 0.0000 0.2612 10.50000 0.05 0.31
Q37 1 0.2998 0.2175 0.2193 11.00000 0.05 0.30
Q38 1 0.1443 0.0000 0.5000 10.50000 0.05 0.28
Q39 1 0.4602 0.0000 0.3303 10.50000 0.05 0.28
Q40 1 -0.1819 -0.0655 0.2573 11.00000 0.05 0.28
Q41 1 -0.0815 0.6657 -0.1871 11.00000 0.05 0.27
Q42 1 0.2014 0.2571 0.3178 11.00000 0.05 0.27
Q43 1 -0.0391 -0.1782 0.3086 11.00000 0.05 0.26
Q44 1 0.3601 0.0000 0.3572 10.50000 0.05 0.26
Q45 1 -0.1085 -0.1053 0.2877 11.00000 0.05 0.25
Q46 1 0.2213 0.1474 0.6439 11.00000 0.05 0.25
Q47 1 0.2823 0.0000 0.0785 10.50000 0.05 0.25
Q48 1 0.1384 0.0000 0.3966 10.50000 0.05 0.24
Q49 1 0.3801 0.0306 0.4973 11.00000 0.05 0.23
Q50 1 0.3646 0.2448 0.2997 11.00000 0.05 0.21
REM The information below was added by Olex2.
REM
REM R1 = 0.0264 for 663 Fo > 4sig(Fo) and 0.0361 for all 11075 data
REM n/a parameters refined using n/a restraints
REM Highest difference peak 1.25, deepest hole -1.29
REM Mean Shift 0, Max Shift 0.000.
REM +++ Tabular Listing of Refinement Information +++
REM R1_all = 0.0361
REM R1_gt = 0.0264
REM wR_ref = 0.0886
REM GOOF = 1.047
REM Shift_max = 0.000
REM Shift_mean = 0
REM Reflections_all = 11075
REM Reflections_gt = 663
REM Parameters = n/a
REM Hole = -1.29
REM Peak = 1.25
REM Flack = n/a
;
_olex2_submission_special_instructions 'No special instructions were received'
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_cxy0495_pmn21
_database_code_depnum_ccdc_archive 'CCDC 1844721'
_audit_update_record
;
2018-10-10 deposited with the CCDC.
2018-10-12 downloaded from the CCDC.
;
_audit_creation_date 2018-10-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number 2016/6
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety '0.5(C32 H32 Au4 N20)'
_chemical_formula_sum 'C16 H16 Au2 N10'
_chemical_formula_weight 742.32
_chemical_absolute_configuration .
_chemical_melting_point ?
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_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.
;
_space_group_crystal_system orthorhombic
_space_group_IT_number 31
_space_group_name_H-M_alt 'P m n 21'
_space_group_name_Hall 'P 2ac -2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y, z'
'x+1/2, -y, z+1/2'
_cell_length_a 6.2753(7)
_cell_length_b 8.0957(10)
_cell_length_c 18.757(2)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_volume 952.93(19)
_cell_formula_units_Z 2
_cell_measurement_reflns_used 9896
_cell_measurement_temperature 100
_cell_measurement_theta_max 34.754
_cell_measurement_theta_min 2.740
_shelx_estimated_absorpt_T_max 0.861
_shelx_estimated_absorpt_T_min 0.091
_exptl_absorpt_coefficient_mu 15.403
_exptl_absorpt_correction_T_max 0.7469
_exptl_absorpt_correction_T_min 0.3806
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1602 before and 0.0901 after correction. The Ratio of minimum to maximum transmission is 0.5096. The \l/2 correction factor is Not present.'
_exptl_absorpt_special_details ?
_exptl_crystal_colour yellow
_exptl_crystal_colour_primary yellow
_exptl_crystal_density_diffrn 2.587
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description plate
_exptl_crystal_F_000 680
_exptl_crystal_size_max 0.3
_exptl_crystal_size_mid 0.06
_exptl_crystal_size_min 0.01
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0578
_diffrn_reflns_av_unetI/netI 0.0428
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max 9
_diffrn_reflns_limit_h_min -9
_diffrn_reflns_limit_k_max 11
_diffrn_reflns_limit_k_min -12
_diffrn_reflns_limit_l_max 30
_diffrn_reflns_limit_l_min -28
_diffrn_reflns_number 23319
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 34.825
_diffrn_reflns_theta_min 2.740
_diffrn_ambient_temperature 100
_diffrn_detector 'Bruker PHOTO 100 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type 'CCD area detector'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device 'three-circle diffractometer'
_diffrn_measurement_device_type 'Bruker PHOTO 100 area detector'
_diffrn_measurement_method '\w and \f scans'
_diffrn_radiation_monochromator 'mirror optics'
_diffrn_radiation_probe x-ray
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'microfocus sealed X-ray tube'
_diffrn_source_type 'Incoatec I\ms'
_reflns_Friedel_coverage 0.953
_reflns_Friedel_fraction_full 0.999
_reflns_Friedel_fraction_max 0.960
_reflns_number_gt 3496
_reflns_number_total 4134
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'SAINT V8.38A (?, 2016)'
_computing_data_collection ?
_computing_data_reduction 'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'XL (Sheldrick, 2008)'
_computing_structure_solution 'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max 2.490
_refine_diff_density_min -1.535
_refine_diff_density_rms 0.393
_refine_ls_abs_structure_details
;
Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack 0.43(2)
_refine_ls_extinction_coef 0.0048(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method 'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref 1.120
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 175
_refine_ls_number_reflns 4134
_refine_ls_number_restraints 175
_refine_ls_R_factor_all 0.0495
_refine_ls_R_factor_gt 0.0385
_refine_ls_restrained_S_all 1.104
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0470P)^2^+1.2992P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0920
_refine_ls_wR_factor_ref 0.0984
_refine_special_details
;
Refined as a 2-component inversion twin.
Location of maximum Q peak
Atom Peak x y z
Q1 2.49 0.0000 -0.4277 -0.2499
Distances to nearest atoms (including eq.)
0.71 Au2 1.41 C16 2.35 H11 2.53 N10
;
_olex2_refinement_description
;
1. Twinned data refinement
Scales: 0.57(2)
0.43(2)
2. Fixed Uiso
At 1.2 times of:
All C(H) groups
At 1.5 times of:
All C(H,H,H) groups
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
Uanis(C12) \\sim Ueq, Uanis(N4) \\sim Ueq: with sigma of 0.008 and sigma for
terminal atoms of 0.02
4. Others
Fixed Sof: H6A(0.5) H6B(0.5) H6C(0.5) H7A(0.5) H7B(0.5) H7C(0.5) H13A(0.5)
H13B(0.5) H13C(0.5) H14A(0.5) H14B(0.5) H14C(0.5)
5.a Aromatic/amide H refined with riding coordinates:
C3(H3), C4(H4), C10(H10), C11(H11)
5.b Idealised Me refined as rotating group:
C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary dual
_atom_sites_solution_secondary ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Au1 Au -0.500000 -0.48133(5) -0.24816(2) 0.01589(14) Uani 1 2 d S TU P . .
Au2 Au 0.000000 -0.51564(6) -0.25242(3) 0.0197(2) Uani 1 2 d S TU P . .
N1 N -0.500000 -0.4704(12) -0.0847(6) 0.0177(18) Uani 1 2 d S TU P . .
N2 N -0.500000 -0.2254(13) -0.1328(5) 0.0166(16) Uani 1 2 d S TU P . .
N3 N -0.500000 -0.0620(15) -0.0245(6) 0.028(2) Uani 1 2 d S TU P . .
N4 N -0.500000 -0.3832(16) 0.0404(6) 0.024(2) Uani 1 2 d S TU P . .
N5 N -0.500000 -0.7234(11) -0.3704(5) 0.0155(16) Uani 1 2 d S TU P . .
N6 N -0.500000 -0.4710(12) -0.4101(5) 0.0170(18) Uani 1 2 d S TU P . .
N7 N -0.500000 -0.5318(15) -0.5372(7) 0.023(2) Uani 1 2 d S TU P . .
N8 N -0.500000 -0.8686(15) -0.4839(5) 0.023(2) Uani 1 2 d S TU P . .
N9 N 0.000000 -0.8594(18) -0.1747(8) 0.039(3) Uani 1 2 d S TU P . .
N10 N 0.000000 -0.1631(19) -0.3221(8) 0.043(3) Uani 1 2 d S TU P . .
C1 C -0.500000 -0.3899(14) -0.1475(5) 0.0145(18) Uani 1 2 d S TU P . .
C2 C -0.500000 -0.3605(17) -0.0280(7) 0.021(2) Uani 1 2 d S TU P . .
C3 C -0.500000 -0.240(2) 0.0775(8) 0.031(3) Uani 1 2 d S TU P . .
H3 H -0.500000 -0.245876 0.128095 0.037 Uiso 1 2 calc RS T P . .
C4 C -0.500000 -0.0842(19) 0.0462(8) 0.030(3) Uani 1 2 d S TU P . .
H4 H -0.500000 0.010360 0.076198 0.036 Uiso 1 2 calc RS T P . .
C5 C -0.500000 -0.2019(17) -0.0613(7) 0.018(2) Uani 1 2 d S TU P . .
C6 C -0.500000 -0.6525(18) -0.0767(8) 0.027(3) Uani 1 2 d S TU P . .
H6A H -0.483118 -0.681177 -0.026251 0.041 Uiso 0.5 1 calc GR . . . .
H6B H -0.381771 -0.699492 -0.104143 0.041 Uiso 0.5 1 calc GR . . . .
H6C H -0.635110 -0.697204 -0.094410 0.041 Uiso 0.5 1 calc GR . . . .
C7 C -0.500000 -0.0902(17) -0.1853(8) 0.027(3) Uani 1 2 d S TU P . .
H7A H -0.397525 -0.005356 -0.170680 0.041 Uiso 0.5 1 calc GR . . . .
H7B H -0.642797 -0.041554 -0.188053 0.041 Uiso 0.5 1 calc GR . . . .
H7C H -0.459679 -0.133550 -0.232206 0.041 Uiso 0.5 1 calc GR . . . .
C8 C -0.500000 -0.5632(13) -0.3499(5) 0.0124(17) Uani 1 2 d S TU P . .
C9 C -0.500000 -0.7350(15) -0.4435(6) 0.0160(18) Uani 1 2 d S TU P . .
C10 C -0.500000 -0.8287(19) -0.5549(8) 0.027(2) Uani 1 2 d S TU P . .
H10 H -0.500000 -0.915522 -0.588941 0.032 Uiso 1 2 calc RS T P . .
C11 C -0.500000 -0.667(2) -0.5790(7) 0.026(2) Uani 1 2 d S TU P . .
H11 H -0.500000 -0.650227 -0.629106 0.031 Uiso 1 2 calc RS T P . .
C12 C -0.500000 -0.5742(15) -0.4686(7) 0.015(2) Uani 1 2 d S TU P . .
C13 C -0.500000 -0.8644(16) -0.3218(7) 0.021(2) Uani 1 2 d S TU P . .
H13A H -0.451373 -0.828642 -0.274614 0.032 Uiso 0.5 1 calc GR . . . .
H13B H -0.403958 -0.949879 -0.340108 0.032 Uiso 0.5 1 calc GR . . . .
H13C H -0.644669 -0.909128 -0.318094 0.032 Uiso 0.5 1 calc GR . . . .
C14 C -0.500000 -0.2894(16) -0.4127(7) 0.023(2) Uani 1 2 d S TU P . .
H14A H -0.408115 -0.246085 -0.374824 0.034 Uiso 0.5 1 calc GR . . . .
H14B H -0.645576 -0.248506 -0.405918 0.034 Uiso 0.5 1 calc GR . . . .
H14C H -0.446310 -0.252649 -0.459132 0.034 Uiso 0.5 1 calc GR . . . .
C15 C 0.000000 -0.7371(17) -0.2070(7) 0.024(2) Uani 1 2 d S TU P . .
C16 C 0.000000 -0.2900(19) -0.2960(7) 0.027(3) Uani 1 2 d S TU P . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Au1 0.01593(19) 0.0176(2) 0.0141(3) -0.0003(5) 0.000 0.000
Au2 0.0179(2) 0.0238(2) 0.0173(5) 0.0014(5) 0.000 0.000
N1 0.014(3) 0.027(5) 0.012(4) 0.003(3) 0.000 0.000
N2 0.010(3) 0.027(4) 0.013(3) -0.003(3) 0.000 0.000
N3 0.018(4) 0.035(5) 0.030(5) -0.014(4) 0.000 0.000
N4 0.006(3) 0.047(5) 0.018(5) 0.005(4) 0.000 0.000
N5 0.016(4) 0.022(4) 0.009(3) -0.002(3) 0.000 0.000
N6 0.013(4) 0.021(4) 0.018(4) 0.004(3) 0.000 0.000
N7 0.016(4) 0.035(5) 0.018(4) 0.002(4) 0.000 0.000
N8 0.014(4) 0.029(5) 0.028(5) -0.003(3) 0.000 0.000
N9 0.030(5) 0.035(7) 0.051(8) 0.004(6) 0.000 0.000
N10 0.053(7) 0.046(8) 0.032(6) 0.015(6) 0.000 0.000
C1 0.012(4) 0.020(4) 0.011(4) 0.002(3) 0.000 0.000
C2 0.014(4) 0.030(5) 0.020(5) -0.002(4) 0.000 0.000
C3 0.016(5) 0.056(8) 0.020(6) 0.000(6) 0.000 0.000
C4 0.012(4) 0.046(7) 0.032(6) -0.018(5) 0.000 0.000
C5 0.010(4) 0.029(5) 0.016(4) -0.005(4) 0.000 0.000
C6 0.029(6) 0.022(6) 0.030(6) 0.002(5) 0.000 0.000
C7 0.033(6) 0.023(6) 0.024(6) 0.002(5) 0.000 0.000
C8 0.011(4) 0.016(4) 0.010(4) 0.001(3) 0.000 0.000
C9 0.011(4) 0.024(5) 0.012(4) 0.002(4) 0.000 0.000
C10 0.011(4) 0.042(7) 0.028(5) -0.003(5) 0.000 0.000
C11 0.018(4) 0.046(7) 0.013(4) -0.002(5) 0.000 0.000
C12 0.009(4) 0.020(4) 0.017(4) 0.003(4) 0.000 0.000
C13 0.024(5) 0.018(5) 0.022(5) 0.003(4) 0.000 0.000
C14 0.018(5) 0.019(5) 0.032(6) 0.001(4) 0.000 0.000
C15 0.015(4) 0.031(6) 0.025(5) -0.001(4) 0.000 0.000
C16 0.008(4) 0.049(8) 0.024(6) 0.010(5) 0.000 0.000
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Au1 Au2 3.1509(4) . ?
Au1 Au2 3.1509(4) 1_455 ?
Au1 C1 2.028(10) . ?
Au1 C8 2.021(10) . ?
Au2 C15 1.985(14) . ?
Au2 C16 2.001(14) . ?
N1 C1 1.347(14) . ?
N1 C2 1.387(16) . ?
N1 C6 1.482(17) . ?
N2 C1 1.360(15) . ?
N2 C5 1.355(14) . ?
N2 C7 1.473(15) . ?
N3 C4 1.338(19) . ?
N3 C5 1.326(16) . ?
N4 C2 1.296(15) . ?
N4 C3 1.35(2) . ?
N5 C8 1.352(13) . ?
N5 C9 1.374(12) . ?
N5 C13 1.461(15) . ?
N6 C8 1.353(13) . ?
N6 C12 1.380(16) . ?
N6 C14 1.471(15) . ?
N7 C11 1.346(19) . ?
N7 C12 1.332(13) . ?
N8 C9 1.320(15) . ?
N8 C10 1.370(19) . ?
N9 C15 1.161(19) . ?
N10 C16 1.138(19) . ?
C2 C5 1.428(19) . ?
C3 H3 0.9500 . ?
C3 C4 1.39(2) . ?
C4 H4 0.9500 . ?
C6 H6A 0.98(5) 3_455 ?
C6 H6A 0.9800 . ?
C6 H6B 1.0(2) 3_455 ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C6 H6C 0.98(15) 3_455 ?
C7 H7A 0.98(11) 3_455 ?
C7 H7A 0.9800 . ?
C7 H7B 0.98(5) 3_455 ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C7 H7C 0.98(6) 3_455 ?
C9 C12 1.384(16) . ?
C10 H10 0.9500 . ?
C10 C11 1.38(2) . ?
C11 H11 0.9500 . ?
C13 H13A 0.9800 . ?
C13 H13A 0.98(6) 3_455 ?
C13 H13B 0.98(9) 3_455 ?
C13 H13B 0.9800 . ?
C13 H13C 0.98(3) 3_455 ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14A 0.98(8) 3_455 ?
C14 H14B 0.98(3) 3_455 ?
C14 H14B 0.9800 . ?
C14 H14C 0.98(6) 3_455 ?
C14 H14C 0.9800 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Au2 Au1 Au2 169.48(2) 1_455 . ?
C1 Au1 Au2 93.20(2) . 1_455 ?
C1 Au1 Au2 93.20(2) . . ?
C8 Au1 Au2 86.97(3) . . ?
C8 Au1 Au2 86.97(3) . 1_455 ?
C8 Au1 C1 177.7(4) . . ?
Au1 Au2 Au1 169.48(2) 1_655 . ?
C15 Au2 Au1 93.94(3) . . ?
C15 Au2 Au1 93.94(3) . 1_655 ?
C15 Au2 C16 178.7(5) . . ?
C16 Au2 Au1 85.98(3) . 1_655 ?
C16 Au2 Au1 85.98(3) . . ?
C1 N1 C2 111.2(10) . . ?
C1 N1 C6 124.7(10) . . ?
C2 N1 C6 124.1(11) . . ?
C1 N2 C7 126.4(10) . . ?
C5 N2 C1 109.8(10) . . ?
C5 N2 C7 123.9(11) . . ?
C5 N3 C4 113.7(13) . . ?
C2 N4 C3 112.8(12) . . ?
C8 N5 C9 110.4(9) . . ?
C8 N5 C13 124.9(9) . . ?
C9 N5 C13 124.7(10) . . ?
C8 N6 C12 109.2(9) . . ?
C8 N6 C14 125.4(10) . . ?
C12 N6 C14 125.3(10) . . ?
C12 N7 C11 110.7(12) . . ?
C9 N8 C10 111.3(12) . . ?
N1 C1 Au1 129.7(8) . . ?
N1 C1 N2 107.3(9) . . ?
N2 C1 Au1 123.1(7) . . ?
N1 C2 C5 103.9(11) . . ?
N4 C2 N1 131.9(14) . . ?
N4 C2 C5 124.1(13) . . ?
N4 C3 H3 118.0 . . ?
N4 C3 C4 124.1(13) . . ?
C4 C3 H3 118.0 . . ?
N3 C4 C3 122.7(14) . . ?
N3 C4 H4 118.6 . . ?
C3 C4 H4 118.6 . . ?
N2 C5 C2 107.9(12) . . ?
N3 C5 N2 129.5(13) . . ?
N3 C5 C2 122.6(12) . . ?
N1 C6 H6A 109.5(12) . 3_455 ?
N1 C6 H6A 109.5 . . ?
N1 C6 H6B 109.5 . . ?
N1 C6 H6B 109(4) . 3_455 ?
N1 C6 H6C 109(3) . 3_455 ?
N1 C6 H6C 109.5 . . ?
H6A C6 H6A 12.4 . 3_455 ?
H6A C6 H6B 109.5 3_455 3_455 ?
H6A C6 H6B 119.8 . 3_455 ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 98.4 . 3_455 ?
H6A C6 H6C 109.5 3_455 3_455 ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6A 119.8 . 3_455 ?
H6B C6 H6B 98.4 . 3_455 ?
H6B C6 H6C 12.4 . 3_455 ?
H6B C6 H6C 109.5 3_455 3_455 ?
H6B C6 H6C 109.5 . . ?
H6C C6 H6A 98.4 . 3_455 ?
H6C C6 H6B 12.4 . 3_455 ?
H6C C6 H6C 119.8 . 3_455 ?
N2 C7 H7A 109(2) . 3_455 ?
N2 C7 H7A 109.5 . . ?
N2 C7 H7B 109.5(11) . 3_455 ?
N2 C7 H7B 109.5 . . ?
N2 C7 H7C 109.5 . . ?
N2 C7 H7C 109.5(14) . 3_455 ?
H7A C7 H7A 82.0 . 3_455 ?
H7A C7 H7B 109.5 3_455 3_455 ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7B 29.9 . 3_455 ?
H7A C7 H7C 109.5 . . ?
H7A C7 H7C 132.2 . 3_455 ?
H7A C7 H7C 109.5 3_455 3_455 ?
H7B C7 H7A 29.9 . 3_455 ?
H7B C7 H7B 132.2 . 3_455 ?
H7B C7 H7C 109.5 . . ?
H7B C7 H7C 82.0 . 3_455 ?
H7B C7 H7C 109.5 3_455 3_455 ?
H7C C7 H7A 132.2 . 3_455 ?
H7C C7 H7B 82.0 . 3_455 ?
H7C C7 H7C 29.9 . 3_455 ?
N5 C8 Au1 125.7(7) . . ?
N5 C8 N6 107.0(8) . . ?
N6 C8 Au1 127.4(8) . . ?
N5 C9 C12 106.0(10) . . ?
N8 C9 N5 128.9(10) . . ?
N8 C9 C12 125.1(11) . . ?
N8 C10 H10 118.6 . . ?
N8 C10 C11 122.7(13) . . ?
C11 C10 H10 118.6 . . ?
N7 C11 C10 125.4(13) . . ?
N7 C11 H11 117.3 . . ?
C10 C11 H11 117.3 . . ?
N6 C12 C9 107.4(10) . . ?
N7 C12 N6 127.8(11) . . ?
N7 C12 C9 124.8(12) . . ?
N5 C13 H13A 109.5 . . ?
N5 C13 H13A 109.5(13) . 3_455 ?
N5 C13 H13B 109.5(19) . 3_455 ?
N5 C13 H13B 109.5 . . ?
N5 C13 H13C 109.5(7) . 3_455 ?
N5 C13 H13C 109.5 . . ?
H13A C13 H13A 36.3 . 3_455 ?
H13A C13 H13B 109.5 3_455 3_455 ?
H13A C13 H13B 135.8 . 3_455 ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13A C13 H13C 75.9 . 3_455 ?
H13A C13 H13C 109.5 3_455 3_455 ?
H13B C13 H13A 135.8 . 3_455 ?
H13B C13 H13B 75.9 . 3_455 ?
H13B C13 H13C 36.3 . 3_455 ?
H13B C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 3_455 3_455 ?
H13C C13 H13A 75.9 . 3_455 ?
H13C C13 H13B 36.3 . 3_455 ?
H13C C13 H13C 135.8 . 3_455 ?
N6 C14 H14A 109.5(18) . 3_455 ?
N6 C14 H14A 109.5 . . ?
N6 C14 H14B 109.5 . . ?
N6 C14 H14B 109.5(5) . 3_455 ?
N6 C14 H14C 109.5 . . ?
N6 C14 H14C 109.5(14) . 3_455 ?
H14A C14 H14A 72.1 . 3_455 ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 3_455 3_455 ?
H14A C14 H14B 40.2 . 3_455 ?
H14A C14 H14C 137.6 . 3_455 ?
H14A C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 3_455 3_455 ?
H14B C14 H14A 40.2 . 3_455 ?
H14B C14 H14B 137.6 . 3_455 ?
H14B C14 H14C 109.5 . . ?
H14B C14 H14C 72.1 . 3_455 ?
H14B C14 H14C 109.5 3_455 3_455 ?
H14C C14 H14A 137.6 . 3_455 ?
H14C C14 H14B 72.1 . 3_455 ?
H14C C14 H14C 40.2 . 3_455 ?
N9 C15 Au2 174.0(12) . . ?
N10 C16 Au2 178.7(15) . . ?
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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C2 C5 N2 0.000(2) . . . . ?
N1 C2 C5 N3 180.000(2) . . . . ?
N4 C2 C5 N2 180.000(1) . . . . ?
N4 C2 C5 N3 0.000(1) . . . . ?
N4 C3 C4 N3 0.000(1) . . . . ?
N5 C9 C12 N6 0.000(5) . . . . ?
N5 C9 C12 N7 180.000(5) . . . . ?
N8 C9 C12 N6 180.000(5) . . . . ?
N8 C9 C12 N7 0.000(8) . . . . ?
N8 C10 C11 N7 0.000(10) . . . . ?
C1 N1 C2 N4 180.000(2) . . . . ?
C1 N1 C2 C5 0.000(1) . . . . ?
C1 N2 C5 N3 180.000(1) . . . . ?
C1 N2 C5 C2 0.000(1) . . . . ?
C2 N1 C1 Au1 180.000(1) . . . . ?
C2 N1 C1 N2 0.000(1) . . . . ?
C2 N4 C3 C4 0.000(1) . . . . ?
C3 N4 C2 N1 180.000(1) . . . . ?
C3 N4 C2 C5 0.000(1) . . . . ?
C4 N3 C5 N2 180.000(1) . . . . ?
C4 N3 C5 C2 0.000(1) . . . . ?
C5 N2 C1 Au1 180.000(1) . . . . ?
C5 N2 C1 N1 0.000(2) . . . . ?
C5 N3 C4 C3 0.000(1) . . . . ?
C6 N1 C1 Au1 0.000(2) . . . . ?
C6 N1 C1 N2 180.000(2) . . . . ?
C6 N1 C2 N4 0.000(2) . . . . ?
C6 N1 C2 C5 180.000(2) . . . . ?
C7 N2 C1 Au1 0.000(2) . . . . ?
C7 N2 C1 N1 180.000(1) . . . . ?
C7 N2 C5 N3 0.000(2) . . . . ?
C7 N2 C5 C2 180.000(1) . . . . ?
C8 N5 C9 N8 180.000(5) . . . . ?
C8 N5 C9 C12 0.000(4) . . . . ?
C8 N6 C12 N7 180.000(5) . . . . ?
C8 N6 C12 C9 0.000(5) . . . . ?
C9 N5 C8 Au1 180.000(3) . . . . ?
C9 N5 C8 N6 0.000(4) . . . . ?
C9 N8 C10 C11 0.000(8) . . . . ?
C10 N8 C9 N5 180.000(6) . . . . ?
C10 N8 C9 C12 0.000(6) . . . . ?
C11 N7 C12 N6 180.000(5) . . . . ?
C11 N7 C12 C9 0.000(7) . . . . ?
C12 N6 C8 Au1 180.000(3) . . . . ?
C12 N6 C8 N5 0.000(4) . . . . ?
C12 N7 C11 C10 0.000(8) . . . . ?
C13 N5 C8 Au1 0.000(4) . . . . ?
C13 N5 C8 N6 180.000(4) . . . . ?
C13 N5 C9 N8 0.000(6) . . . . ?
C13 N5 C9 C12 180.000(5) . . . . ?
C14 N6 C8 Au1 0.000(4) . . . . ?
C14 N6 C8 N5 180.000(4) . . . . ?
C14 N6 C12 N7 0.000(7) . . . . ?
C14 N6 C12 C9 180.000(4) . . . . ?
_iucr_refine_instructions_details
;
TITL cxy0495
cxy0495_pmn21.res
created by SHELXL-2016/6 at 09:52:13 on 10-Oct-2018
CELL 0.71073 6.2753 8.0957 18.7573 90 90 90
ZERR 2 0.0007 0.001 0.0021 0 0 0
LATT -1
SYMM 0.5-X,-Y,0.5+Z
SYMM -X,+Y,+Z
SYMM 0.5+X,-Y,0.5+Z
SFAC C H Au N
UNIT 32 32 4 20
SIMU 0.01 0.02 2
ISOR 0.008 0.02 C12 N4
L.S. 10
PLAN 20
SIZE 0.3 0.06 0.01
TEMP -73.15
CONF
HTAB
BOND $H
fmap 2
acta
TWIN -1 0 0 0 -1 0 0 0 -1 2
OMIT 0 1 0
OMIT 0 0 2
REM
REM
REM
WGHT 0.047000 1.299200
EXTI 0.004758
BASF 0.42963
FVAR 0.27479
AU1 3 -0.500000 -0.481333 -0.248161 10.50000 0.01593 0.01762 =
0.01412 -0.00028 0.00000 0.00000
AU2 3 0.000000 -0.515641 -0.252415 10.50000 0.01789 0.02384 =
0.01732 0.00143 0.00000 0.00000
N1 4 -0.500000 -0.470387 -0.084669 10.50000 0.01425 0.02674 =
0.01212 0.00288 0.00000 0.00000
N2 4 -0.500000 -0.225410 -0.132839 10.50000 0.00979 0.02717 =
0.01272 -0.00341 0.00000 0.00000
N3 4 -0.500000 -0.062014 -0.024504 10.50000 0.01846 0.03524 =
0.02958 -0.01394 0.00000 0.00000
N4 4 -0.500000 -0.383181 0.040439 10.50000 0.00596 0.04663 =
0.01805 0.00487 0.00000 0.00000
N5 4 -0.500000 -0.723367 -0.370427 10.50000 0.01578 0.02201 =
0.00866 -0.00201 0.00000 0.00000
N6 4 -0.500000 -0.470992 -0.410073 10.50000 0.01256 0.02075 =
0.01758 0.00371 0.00000 0.00000
N7 4 -0.500000 -0.531844 -0.537244 10.50000 0.01550 0.03526 =
0.01804 0.00222 0.00000 0.00000
N8 4 -0.500000 -0.868602 -0.483869 10.50000 0.01401 0.02869 =
0.02758 -0.00303 0.00000 0.00000
N9 4 0.000000 -0.859414 -0.174746 10.50000 0.02989 0.03452 =
0.05127 0.00364 0.00000 0.00000
N10 4 0.000000 -0.163068 -0.322051 10.50000 0.05267 0.04555 =
0.03155 0.01475 0.00000 0.00000
C1 1 -0.500000 -0.389893 -0.147516 10.50000 0.01204 0.02035 =
0.01107 0.00217 0.00000 0.00000
C2 1 -0.500000 -0.360474 -0.027960 10.50000 0.01386 0.02987 =
0.01993 -0.00217 0.00000 0.00000
C3 1 -0.500000 -0.239812 0.077516 10.50000 0.01602 0.05616 =
0.01987 0.00026 0.00000 0.00000
AFIX 43
H3 2 -0.500000 -0.245876 0.128095 10.50000 -1.20000
AFIX 0
C4 1 -0.500000 -0.084156 0.046181 10.50000 0.01225 0.04585 =
0.03206 -0.01820 0.00000 0.00000
AFIX 43
H4 2 -0.500000 0.010360 0.076198 10.50000 -1.20000
AFIX 0
C5 1 -0.500000 -0.201883 -0.061324 10.50000 0.00963 0.02921 =
0.01596 -0.00481 0.00000 0.00000
C6 1 -0.500000 -0.652480 -0.076693 10.50000 0.02855 0.02217 =
0.03036 0.00175 0.00000 0.00000
AFIX 137
H6A 2 -0.483118 -0.681177 -0.026251 10.50000 -1.50000
H6B 2 -0.381771 -0.699492 -0.104143 10.50000 -1.50000
H6C 2 -0.635110 -0.697204 -0.094410 10.50000 -1.50000
AFIX 0
C7 1 -0.500000 -0.090156 -0.185335 10.50000 0.03347 0.02317 =
0.02438 0.00183 0.00000 0.00000
AFIX 137
H7A 2 -0.397525 -0.005356 -0.170680 10.50000 -1.50000
H7B 2 -0.642797 -0.041554 -0.188053 10.50000 -1.50000
H7C 2 -0.459679 -0.133550 -0.232206 10.50000 -1.50000
AFIX 0
C8 1 -0.500000 -0.563209 -0.349927 10.50000 0.01105 0.01614 =
0.00986 0.00110 0.00000 0.00000
C9 1 -0.500000 -0.734983 -0.443513 10.50000 0.01124 0.02422 =
0.01241 0.00177 0.00000 0.00000
C10 1 -0.500000 -0.828704 -0.554867 10.50000 0.01103 0.04246 =
0.02767 -0.00324 0.00000 0.00000
AFIX 43
H10 2 -0.500000 -0.915522 -0.588941 10.50000 -1.20000
AFIX 0
C11 1 -0.500000 -0.667067 -0.578983 10.50000 0.01831 0.04554 =
0.01319 -0.00162 0.00000 0.00000
AFIX 43
H11 2 -0.500000 -0.650227 -0.629106 10.50000 -1.20000
AFIX 0
C12 1 -0.500000 -0.574200 -0.468618 10.50000 0.00905 0.01997 =
0.01696 0.00337 0.00000 0.00000
C13 1 -0.500000 -0.864358 -0.321809 10.50000 0.02364 0.01784 =
0.02198 0.00314 0.00000 0.00000
AFIX 137
H13A 2 -0.451373 -0.828642 -0.274614 10.50000 -1.50000
H13B 2 -0.403958 -0.949879 -0.340108 10.50000 -1.50000
H13C 2 -0.644669 -0.909128 -0.318094 10.50000 -1.50000
AFIX 0
C14 1 -0.500000 -0.289408 -0.412706 10.50000 0.01776 0.01900 =
0.03173 0.00074 0.00000 0.00000
AFIX 137
H14A 2 -0.408115 -0.246085 -0.374824 10.50000 -1.50000
H14B 2 -0.645576 -0.248506 -0.405918 10.50000 -1.50000
H14C 2 -0.446310 -0.252649 -0.459132 10.50000 -1.50000
AFIX 0
C15 1 0.000000 -0.737056 -0.206985 10.50000 0.01471 0.03135 =
0.02459 -0.00075 0.00000 0.00000
C16 1 0.000000 -0.290001 -0.295984 10.50000 0.00786 0.04876 =
0.02385 0.00954 0.00000 0.00000
HKLF 4
REM cxy0495
REM R1 = 0.0385 for 3496 Fo > 4sig(Fo) and 0.0495 for all 4134 data
REM 175 parameters refined using 175 restraints
END
WGHT 0.0470 1.2992
REM Instructions for potential hydrogen bonds
EQIV $4 -x-1/2, -y, z+1/2
HTAB C4 N10_$4
EQIV $5 x-1, y+1, z
HTAB C7 N9_$5
EQIV $6 -x-1/2, -y-2, z-1/2
HTAB C10 N9_$6
REM Highest difference peak 2.490, deepest hole -1.535, 1-sigma level 0.393
Q1 1 0.0000 -0.4277 -0.2499 10.50000 0.05 2.49
Q2 1 -0.5000 -0.5392 -0.2070 10.50000 0.05 2.29
Q3 1 -0.5535 -0.5617 -0.2480 11.00000 0.05 2.24
Q4 1 -0.5000 -0.5427 -0.2885 10.50000 0.05 2.18
Q5 1 0.0000 -0.4553 -0.2118 10.50000 0.05 2.14
Q6 1 0.0000 -0.4586 -0.2915 10.50000 0.05 1.98
Q7 1 -0.5000 -0.4838 -0.2220 10.50000 0.05 1.98
Q8 1 0.0000 -0.5159 -0.2797 10.50000 0.05 1.93
Q9 1 0.0000 -0.5197 -0.3283 10.50000 0.05 1.81
Q10 1 -0.5000 -0.4772 -0.1716 10.50000 0.05 1.78
Q11 1 -0.5647 -0.4192 -0.1999 11.00000 0.05 1.70
Q12 1 -0.5000 -0.4793 -0.5016 10.50000 0.05 1.50
Q13 1 -0.5000 -0.4805 -0.3227 10.50000 0.05 1.49
Q14 1 -0.5000 -0.4204 -0.2892 10.50000 0.05 1.44
Q15 1 0.0000 -0.5190 -0.1762 10.50000 0.05 1.43
Q16 1 -0.7566 -0.5080 -0.5004 11.00000 0.05 1.41
Q17 1 0.0000 -0.5747 -0.2102 10.50000 0.05 1.37
Q18 1 -0.5000 -0.4783 0.0196 10.50000 0.05 1.34
Q19 1 0.0624 -0.5753 -0.2991 11.00000 0.05 1.30
Q20 1 -0.5000 -0.5742 -0.4973 10.50000 0.05 1.29
REM The information below was added by Olex2.
REM
REM R1 = 0.0385 for 3496 Fo > 4sig(Fo) and 0.0495 for all 24330 data
REM n/a parameters refined using n/a restraints
REM Highest difference peak 2.49, deepest hole -1.54
REM Mean Shift 0, Max Shift 0.000.
REM +++ Tabular Listing of Refinement Information +++
REM R1_all = 0.0495
REM R1_gt = 0.0385
REM wR_ref = 0.0984
REM GOOF = 1.120
REM Shift_max = 0.000
REM Shift_mean = 0
REM Reflections_all = 24330
REM Reflections_gt = 3496
REM Parameters = n/a
REM Hole = -1.54
REM Peak = 2.49
REM Flack = n/a
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.57(2)
2 0.43(2)
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_cxy0495_pmna
_database_code_depnum_ccdc_archive 'CCDC 1871225'
_audit_update_record
;
2018-10-10 deposited with the CCDC.
2018-10-12 downloaded from the CCDC.
;
_audit_creation_date 2018-09-27
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number 2016/6
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C16 H16 Au2 N10'
_chemical_formula_sum 'C16 H16 Au2 N10'
_chemical_formula_weight 742.32
_chemical_melting_point ?
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_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.
;
_space_group_crystal_system orthorhombic
_space_group_IT_number 53
_space_group_name_H-M_alt 'P m n a'
_space_group_name_Hall '-P 2ac 2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x, -y, -z'
'-x+1/2, y, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x, y, z'
'x-1/2, -y, z-1/2'
_cell_length_a 6.3484(4)
_cell_length_b 8.1538(6)
_cell_length_c 18.6895(12)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_volume 967.44(11)
_cell_formula_units_Z 2
_cell_measurement_reflns_used 6901
_cell_measurement_temperature 225
_cell_measurement_theta_max 28.232
_cell_measurement_theta_min 2.725
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 15.172
_exptl_absorpt_correction_T_max 0.0962
_exptl_absorpt_correction_T_min 0.0384
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1544 before and 0.0874 after correction. The Ratio of minimum to maximum transmission is 0.3992. The \l/2 correction factor is Not present.'
_exptl_absorpt_special_details ?
_exptl_crystal_colour yellow
_exptl_crystal_colour_primary yellow
_exptl_crystal_density_diffrn 2.548
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description plate
_exptl_crystal_F_000 680
_exptl_crystal_size_max 0.3
_exptl_crystal_size_mid 0.06
_exptl_crystal_size_min 0.01
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0590
_diffrn_reflns_av_unetI/netI 0.0264
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max 8
_diffrn_reflns_limit_h_min -8
_diffrn_reflns_limit_k_max 10
_diffrn_reflns_limit_k_min -10
_diffrn_reflns_limit_l_max 24
_diffrn_reflns_limit_l_min -24
_diffrn_reflns_number 18600
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 28.286
_diffrn_reflns_theta_min 2.179
_diffrn_ambient_temperature 225
_diffrn_detector 'Bruker PHOTO 100 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type 'CCD area detector'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device 'three-circle diffractometer'
_diffrn_measurement_device_type 'Bruker PHOTO 100 area detector'
_diffrn_measurement_method '\w and \f scans'
_diffrn_radiation_monochromator 'mirror optics'
_diffrn_radiation_probe x-ray
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'microfocus sealed X-ray tube'
_diffrn_source_type 'Incoatec I\ms'
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 1029
_reflns_number_total 1306
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'SAINT V8.38A (?, 2016)'
_computing_data_collection ?
_computing_data_reduction 'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'XL (Sheldrick, 2008)'
_computing_structure_solution 'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max 3.908
_refine_diff_density_min -2.488
_refine_diff_density_rms 0.363
_refine_ls_extinction_coef 0.0108(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method 'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref 1.268
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 90
_refine_ls_number_reflns 1306
_refine_ls_number_restraints 84
_refine_ls_R_factor_all 0.0910
_refine_ls_R_factor_gt 0.0794
_refine_ls_restrained_S_all 1.239
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0334P)^2^+46.7904P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1721
_refine_ls_wR_factor_ref 0.1776
_refine_special_details
;
Location of maximum Q peak
Atom Peak x y z
Q1 3.91 0.0000 0.0367 0.4586
Distances to nearest atoms (including eq.)
0.83 Au2 1.97 H4 3.14 N5 3.15 N3
;
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups
At 1.5 times of:
All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
3. Others
Fixed Sof: H6A(0.5) H6B(0.5) H6C(0.5) H7A(0.5) H7B(0.5) H7C(0.5)
4.a Aromatic/amide H refined with riding coordinates:
C4(H4), C5(H5)
4.b Idealised Me refined as rotating group:
C6(H6A,H6B,H6C), C7(H7A,H7B,H7C)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary dual
_atom_sites_solution_secondary ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Au1 Au 0.000000 0.000000 0.000000 0.0361(5) Uani 1 4 d S TU P . .
Au2 Au 0.500000 0.000000 0.000000 0.0437(6) Uani 1 4 d S TU P . .
N1 N 0.000000 -0.006(3) 0.1641(10) 0.039(3) Uani 1 2 d S TU P . .
N2 N 0.000000 0.252(3) 0.1201(10) 0.038(3) Uani 1 2 d S TU P . .
N3 N 0.000000 0.063(3) 0.2905(13) 0.049(4) Uani 1 2 d S TU P . .
N4 N 0.000000 0.403(3) 0.2320(13) 0.053(4) Uani 1 2 d S TU P . .
N5 N 0.500000 -0.340(4) 0.0746(17) 0.075(7) Uani 1 2 d S TU P . .
C1 C 0.000000 0.083(3) 0.1032(12) 0.036(3) Uani 1 2 d S TU P . .
C2 C 0.000000 0.110(3) 0.2190(13) 0.042(3) Uani 1 2 d S TU P . .
C3 C 0.000000 0.269(3) 0.1940(13) 0.041(3) Uani 1 2 d S TU P . .
C4 C 0.000000 0.203(4) 0.3279(15) 0.050(4) Uani 1 2 d S TU P . .
H4 H 0.000000 0.192149 0.377952 0.060 Uiso 1 2 calc RS T P . .
C5 C 0.000000 0.369(4) 0.3006(15) 0.050(4) Uani 1 2 d S TU P . .
H5 H 0.000000 0.456553 0.333448 0.061 Uiso 1 2 calc RS T P . .
C6 C 0.000000 0.372(4) 0.0676(15) 0.051(6) Uani 1 2 d S TU P . .
H6A H 0.071448 0.330825 0.025362 0.077 Uiso 0.5 1 calc GR . . A -1
H6B H 0.072606 0.468274 0.085254 0.077 Uiso 0.5 1 calc GR . . A -1
H6C H -0.144054 0.400102 0.055549 0.077 Uiso 0.5 1 calc GR . . A -1
C7 C 0.000000 -0.179(3) 0.1674(16) 0.045(5) Uani 1 2 d S TU P . .
H7A H 0.099125 -0.222580 0.132692 0.068 Uiso 0.5 1 calc GR . . B -1
H7B H -0.140087 -0.220184 0.156769 0.068 Uiso 0.5 1 calc GR . . B -1
H7C H 0.040963 -0.214386 0.215033 0.068 Uiso 0.5 1 calc GR . . B -1
C8 C 0.500000 -0.217(4) 0.0441(15) 0.052(4) Uani 1 2 d S TU P . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Au1 0.0346(7) 0.0459(8) 0.0277(7) -0.0070(5) 0.000 0.000
Au2 0.0388(8) 0.0504(9) 0.0417(8) 0.0167(6) 0.000 0.000
N1 0.031(6) 0.048(7) 0.040(6) -0.016(6) 0.000 0.000
N2 0.024(6) 0.047(7) 0.042(7) 0.001(6) 0.000 0.000
N3 0.029(6) 0.068(8) 0.051(7) -0.011(7) 0.000 0.000
N4 0.034(7) 0.069(8) 0.056(8) -0.015(7) 0.000 0.000
N5 0.071(14) 0.070(14) 0.086(15) 0.012(13) 0.000 0.000
C1 0.024(6) 0.046(8) 0.037(7) -0.002(6) 0.000 0.000
C2 0.028(6) 0.055(7) 0.045(7) -0.012(6) 0.000 0.000
C3 0.027(6) 0.052(7) 0.045(7) -0.007(6) 0.000 0.000
C4 0.030(7) 0.070(9) 0.051(8) -0.015(8) 0.000 0.000
C5 0.028(7) 0.069(9) 0.054(8) -0.020(8) 0.000 0.000
C6 0.046(12) 0.053(13) 0.056(12) 0.004(11) 0.000 0.000
C7 0.041(11) 0.026(10) 0.069(13) -0.005(10) 0.000 0.000
C8 0.046(8) 0.055(8) 0.054(8) 0.009(8) 0.000 0.000
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Au1 Au2 3.1742(2) 1_455 ?
Au1 Au2 3.1742(2) . ?
Au1 C1 2.04(2) . ?
Au1 C1 2.04(2) 5 ?
Au2 C8 1.95(3) . ?
Au2 C8 1.95(3) 5_655 ?
N1 C1 1.35(3) . ?
N1 C2 1.40(3) . ?
N1 C7 1.41(3) . ?
N2 C1 1.41(3) . ?
N2 C3 1.39(3) . ?
N2 C6 1.39(3) . ?
N3 C2 1.39(3) . ?
N3 C4 1.34(4) . ?
N4 C3 1.31(3) . ?
N4 C5 1.31(4) . ?
N5 C8 1.16(4) . ?
C2 C3 1.38(4) . ?
C4 H4 0.9400 . ?
C4 C5 1.45(4) . ?
C5 H5 0.9400 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 H6C 0.9700 . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 H7C 0.9700 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Au2 Au1 Au2 180.0 . 1_455 ?
C1 Au1 Au2 90.0 5 1_455 ?
C1 Au1 Au2 90.0 5 . ?
C1 Au1 Au2 90.0 . 1_455 ?
C1 Au1 Au2 90.0 . . ?
C1 Au1 C1 180.0 5 . ?
Au1 Au2 Au1 180.0 . 1_655 ?
C8 Au2 Au1 90.0 . . ?
C8 Au2 Au1 90.0 . 1_655 ?
C8 Au2 Au1 90.0 5_655 . ?
C8 Au2 Au1 90.0 5_655 1_655 ?
C8 Au2 C8 180.0 . 5_655 ?
C1 N1 C2 105(2) . . ?
C1 N1 C7 125(2) . . ?
C2 N1 C7 130(2) . . ?
C3 N2 C1 109(2) . . ?
C6 N2 C1 122(2) . . ?
C6 N2 C3 129(2) . . ?
C4 N3 C2 106(2) . . ?
C3 N4 C5 111(3) . . ?
N1 C1 Au1 128.1(18) . . ?
N1 C1 N2 110(2) . . ?
N2 C1 Au1 122.2(17) . . ?
N3 C2 N1 121(2) . . ?
C3 C2 N1 113(2) . . ?
C3 C2 N3 126(2) . . ?
N4 C3 N2 129(3) . . ?
N4 C3 C2 127(2) . . ?
C2 C3 N2 104(2) . . ?
N3 C4 H4 116.1 . . ?
N3 C4 C5 128(3) . . ?
C5 C4 H4 116.1 . . ?
N4 C5 C4 123(3) . . ?
N4 C5 H5 118.6 . . ?
C4 C5 H5 118.6 . . ?
N2 C6 H6A 109.5 . . ?
N2 C6 H6B 109.5 . . ?
N2 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N1 C7 H7A 109.5 . . ?
N1 C7 H7B 109.5 . . ?
N1 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N5 C8 Au2 176(3) . . ?
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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C2 C3 N2 0.000(4) . . . . ?
N1 C2 C3 N4 180.000(5) . . . . ?
N3 C2 C3 N2 180.000(4) . . . . ?
N3 C2 C3 N4 0.000(7) . . . . ?
N3 C4 C5 N4 0.000(9) . . . . ?
C1 N1 C2 N3 180.000(4) . . . . ?
C1 N1 C2 C3 0.000(4) . . . . ?
C1 N2 C3 N4 180.000(5) . . . . ?
C1 N2 C3 C2 0.000(4) . . . . ?
C2 N1 C1 Au1 180.000(3) . . . . ?
C2 N1 C1 N2 0.000(3) . . . . ?
C2 N3 C4 C5 0.000(7) . . . . ?
C3 N2 C1 Au1 180.000(4) . . . . ?
C3 N2 C1 N1 0.000(3) . . . . ?
C3 N4 C5 C4 0.000(8) . . . . ?
C4 N3 C2 N1 180.000(5) . . . . ?
C4 N3 C2 C3 0.000(6) . . . . ?
C5 N4 C3 N2 180.000(6) . . . . ?
C5 N4 C3 C2 0.000(7) . . . . ?
C6 N2 C1 Au1 0.000(3) . . . . ?
C6 N2 C1 N1 180.000(3) . . . . ?
C6 N2 C3 N4 0.000(6) . . . . ?
C6 N2 C3 C2 180.000(4) . . . . ?
C7 N1 C1 Au1 0.000(3) . . . . ?
C7 N1 C1 N2 180.000(2) . . . . ?
C7 N1 C2 N3 0.000(4) . . . . ?
C7 N1 C2 C3 180.000(4) . . . . ?
_iucr_refine_instructions_details
;
TITL cxy0495_298K
cxy0495_pmna.res
created by SHELXL-2016/6 at 12:28:41 on 27-Sep-2018
CELL 0.71073 6.3484 8.1538 18.6895 90 90 90
ZERR 2 0.0004 0.0006 0.0012 0 0 0
LATT 1
SYMM 0.5-X,-Y,0.5+Z
SYMM +X,-Y,-Z
SYMM 0.5-X,+Y,0.5-Z
SFAC C H Au N
UNIT 32 32 4 20
SIMU 0.01 0.02 2
L.S. 20
PLAN -20
TEMP -23.15
BOND $H
CONF
fmap 2
acta
OMIT 0 1 0
REM
REM
REM
WGHT 0.033400 46.790401
EXTI 0.010753
FVAR 0.39540
AU1 3 0.000000 0.000000 0.000000 10.25000 0.03459 0.04590 =
0.02771 -0.00703 0.00000 0.00000
AU2 3 0.500000 0.000000 0.000000 10.25000 0.03883 0.05039 =
0.04173 0.01675 0.00000 0.00000
N1 4 0.000000 -0.006180 0.164132 10.50000 0.03065 0.04759 =
0.03957 -0.01558 0.00000 0.00000
N2 4 0.000000 0.251639 0.120078 10.50000 0.02401 0.04687 =
0.04207 0.00051 0.00000 0.00000
N3 4 0.000000 0.063154 0.290451 10.50000 0.02926 0.06751 =
0.05074 -0.01056 0.00000 0.00000
N4 4 0.000000 0.403142 0.231950 10.50000 0.03379 0.06940 =
0.05611 -0.01526 0.00000 0.00000
N5 4 0.500000 -0.340413 0.074637 10.50000 0.07057 0.06977 =
0.08576 0.01186 0.00000 0.00000
C1 1 0.000000 0.082976 0.103247 10.50000 0.02420 0.04612 =
0.03704 -0.00197 0.00000 0.00000
C2 1 0.000000 0.110054 0.218958 10.50000 0.02771 0.05460 =
0.04453 -0.01177 0.00000 0.00000
C3 1 0.000000 0.268698 0.193983 10.50000 0.02669 0.05184 =
0.04548 -0.00725 0.00000 0.00000
C4 1 0.000000 0.203090 0.327883 10.50000 0.03037 0.06963 =
0.05094 -0.01469 0.00000 0.00000
AFIX 43
H4 2 0.000000 0.192149 0.377952 10.50000 -1.20000
AFIX 0
C5 1 0.000000 0.369241 0.300605 10.50000 0.02833 0.06936 =
0.05361 -0.02031 0.00000 0.00000
AFIX 43
H5 2 0.000000 0.456553 0.333448 10.50000 -1.20000
AFIX 0
C6 1 0.000000 0.371711 0.067629 10.50000 0.04581 0.05252 =
0.05577 0.00448 0.00000 0.00000
PART -1
AFIX 137
H6A 2 0.071448 0.330825 0.025362 10.50000 -1.50000
H6B 2 0.072606 0.468274 0.085254 10.50000 -1.50000
H6C 2 -0.144054 0.400102 0.055549 10.50000 -1.50000
AFIX 0
PART 0
C7 1 0.000000 -0.179433 0.167414 10.50000 0.04061 0.02586 =
0.06912 -0.00485 0.00000 0.00000
PART -1
AFIX 137
H7A 2 0.099125 -0.222580 0.132692 10.50000 -1.50000
H7B 2 -0.140087 -0.220184 0.156769 10.50000 -1.50000
H7C 2 0.040963 -0.214386 0.215033 10.50000 -1.50000
AFIX 0
PART 0
C8 1 0.500000 -0.216795 0.044117 10.50000 0.04595 0.05519 =
0.05397 0.00884 0.00000 0.00000
HKLF 4
REM cxy0495_298K
REM R1 = 0.0794 for 1029 Fo > 4sig(Fo) and 0.0910 for all 1306 data
REM 90 parameters refined using 84 restraints
END
WGHT 0.0334 46.8039
REM Highest difference peak 3.908, deepest hole -2.488, 1-sigma level 0.363
Q1 1 0.0000 0.0367 0.4586 10.50000 0.05 3.91
Q2 1 0.0000 -0.0387 0.0419 10.50000 0.05 3.81
Q3 1 0.0000 -0.0967 0.4889 10.50000 0.05 2.30
Q4 1 0.0000 -0.2641 0.3358 10.50000 0.05 1.56
Q5 1 0.0000 0.0967 0.0118 10.50000 0.05 1.55
Q6 1 0.0000 0.1694 0.2912 10.50000 0.05 1.35
Q7 1 0.0000 0.0811 0.1550 10.50000 0.05 1.19
Q8 1 0.0000 -0.1224 0.3099 10.50000 0.05 1.18
Q9 1 0.0000 0.0194 0.0820 10.50000 0.05 1.11
Q10 1 0.0000 0.4092 0.3688 10.50000 0.05 1.09
Q11 1 0.0000 -0.0514 0.3777 10.50000 0.05 1.02
Q12 1 0.0959 0.0883 0.0534 11.00000 0.05 0.96
Q13 1 0.0000 0.0437 0.3269 10.50000 0.05 0.93
Q14 1 0.0000 -0.3075 0.0146 10.50000 0.05 0.90
Q15 1 0.0000 -0.1559 0.0591 10.50000 0.05 0.89
Q16 1 0.0000 -0.3682 0.1785 10.50000 0.05 0.85
Q17 1 0.0000 0.6280 0.2270 10.50000 0.05 0.83
Q18 1 0.0000 -0.1810 0.1298 10.50000 0.05 0.81
Q19 1 0.1217 0.0000 0.0000 10.50000 0.05 0.81
Q20 1 0.0000 0.4430 0.2874 10.50000 0.05 0.79
REM The information below was added by Olex2.
REM
REM R1 = 0.0794 for 1029 Fo > 4sig(Fo) and 0.0910 for all 19790 data
REM n/a parameters refined using n/a restraints
REM Highest difference peak 3.91, deepest hole -2.49
REM Mean Shift 0, Max Shift 0.000.
REM +++ Tabular Listing of Refinement Information +++
REM R1_all = 0.0910
REM R1_gt = 0.0794
REM wR_ref = 0.1776
REM GOOF = 1.268
REM Shift_max = 0.000
REM Shift_mean = 0
REM Reflections_all = 19790
REM Reflections_gt = 1029
REM Parameters = n/a
REM Hole = -2.49
REM Peak = 3.91
REM Flack = n/a
;
_olex2_submission_special_instructions 'No special instructions were received'
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_cxy0495_pmn21_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1871224'
_audit_update_record
;
2018-10-10 deposited with the CCDC.
2018-10-12 downloaded from the CCDC.
;
_audit_creation_date 2018-10-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number 2016/6
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety '0.5(C32 H32 Au4 N20)'
_chemical_formula_sum 'C16 H16 Au2 N10'
_chemical_formula_weight 742.32
_chemical_absolute_configuration .
_chemical_melting_point ?
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_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.
;
_space_group_crystal_system orthorhombic
_space_group_IT_number 31
_space_group_name_H-M_alt 'P m n 21'
_space_group_name_Hall 'P 2ac -2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y, z'
'x+1/2, -y, z+1/2'
_cell_length_a 6.3306(4)
_cell_length_b 8.1410(5)
_cell_length_c 18.7077(11)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_volume 964.15(10)
_cell_formula_units_Z 2
_cell_measurement_reflns_used 8899
_cell_measurement_temperature 200
_cell_measurement_theta_max 28.320
_cell_measurement_theta_min 2.728
_shelx_estimated_absorpt_T_max 0.863
_shelx_estimated_absorpt_T_min 0.092
_exptl_absorpt_coefficient_mu 15.224
_exptl_absorpt_correction_T_max 0.7457
_exptl_absorpt_correction_T_min 0.3840
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1605 before and 0.0908 after correction. The Ratio of minimum to maximum transmission is 0.5150. The \l/2 correction factor is Not present.'
_exptl_absorpt_special_details ?
_exptl_crystal_colour yellow
_exptl_crystal_colour_primary yellow
_exptl_crystal_density_diffrn 2.557
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description plate
_exptl_crystal_F_000 680
_exptl_crystal_size_max 0.3
_exptl_crystal_size_mid 0.06
_exptl_crystal_size_min 0.01
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0543
_diffrn_reflns_av_unetI/netI 0.0351
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max 8
_diffrn_reflns_limit_h_min -8
_diffrn_reflns_limit_k_max 10
_diffrn_reflns_limit_k_min -10
_diffrn_reflns_limit_l_max 24
_diffrn_reflns_limit_l_min -24
_diffrn_reflns_number 18339
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 28.326
_diffrn_reflns_theta_min 2.177
_diffrn_ambient_temperature 200
_diffrn_detector 'Bruker PHOTO 100 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type 'CCD area detector'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device 'three-circle diffractometer'
_diffrn_measurement_device_type 'Bruker PHOTO 100 area detector'
_diffrn_measurement_method '\w and \f scans'
_diffrn_radiation_monochromator 'mirror optics'
_diffrn_radiation_probe x-ray
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'microfocus sealed X-ray tube'
_diffrn_source_type 'Incoatec I\ms'
_reflns_Friedel_coverage 0.944
_reflns_Friedel_fraction_full 0.998
_reflns_Friedel_fraction_max 0.998
_reflns_number_gt 2154
_reflns_number_total 2603
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'SAINT V8.38A (?, 2016)'
_computing_data_collection ?
_computing_data_reduction 'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'XL (Sheldrick, 2008)'
_computing_structure_solution 'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max 2.279
_refine_diff_density_min -2.263
_refine_diff_density_rms 0.589
_refine_ls_abs_structure_details
;
Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack 0.41(3)
_refine_ls_extinction_coef 0.0132(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method 'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref 1.222
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 175
_refine_ls_number_reflns 2603
_refine_ls_number_restraints 169
_refine_ls_R_factor_all 0.0566
_refine_ls_R_factor_gt 0.0440
_refine_ls_restrained_S_all 1.205
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0757P)^2^+0.1187P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1158
_refine_ls_wR_factor_ref 0.1336
_refine_special_details
;
Refined as a 2-component inversion twin.
Location of maximum Q peak
Atom Peak x y z
Q1 2.28 0.0000 -0.4365 -0.2507
Distances to nearest atoms (including eq.)
0.60 Au2 1.47 C16 2.48 H11 2.54 C15
;
_olex2_refinement_description
;
1. Twinned data refinement
Scales: 0.59(3)
0.41(3)
2. Fixed Uiso
At 1.2 times of:
All C(H) groups
At 1.5 times of:
All C(H,H,H) groups
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
4. Others
Fixed Sof: H6A(0.5) H6B(0.5) H6C(0.5) H7A(0.5) H7B(0.5) H7C(0.5) H13A(0.5)
H13B(0.5) H13C(0.5) H14A(0.5) H14B(0.5) H14C(0.5)
5.a Aromatic/amide H refined with riding coordinates:
C3(H3), C4(H4), C10(H10), C11(H11)
5.b Idealised Me refined as rotating group:
C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary dual
_atom_sites_solution_secondary ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Au1 Au -0.500000 -0.48763(8) -0.24828(2) 0.0254(3) Uani 1 2 d S TU P . .
Au2 Au 0.000000 -0.50976(8) -0.25080(7) 0.0315(4) Uani 1 2 d S TU P . .
N1 N -0.500000 -0.481(2) -0.0840(10) 0.031(3) Uani 1 2 d S TU P . .
N2 N -0.500000 -0.235(2) -0.1315(9) 0.031(3) Uani 1 2 d S TU P . .
N3 N -0.500000 -0.075(2) -0.0220(10) 0.047(4) Uani 1 2 d S TU P . .
N4 N -0.500000 -0.404(2) 0.0417(10) 0.040(3) Uani 1 2 d S TU P . .
N5 N -0.500000 -0.7321(16) -0.3691(8) 0.028(3) Uani 1 2 d S TU P . .
N6 N -0.500000 -0.483(2) -0.4110(8) 0.031(3) Uani 1 2 d S TU P . .
N7 N -0.500000 -0.548(2) -0.5381(10) 0.035(3) Uani 1 2 d S TU P . .
N8 N -0.500000 -0.878(2) -0.4807(9) 0.043(4) Uani 1 2 d S TU P . .
N9 N 0.000000 -0.852(3) -0.1735(14) 0.065(6) Uani 1 2 d S TU P . .
N10 N 0.000000 -0.167(3) -0.3228(14) 0.074(6) Uani 1 2 d S TU P . .
C1 C -0.500000 -0.396(2) -0.1462(9) 0.028(3) Uani 1 2 d S TU P . .
C2 C -0.500000 -0.372(3) -0.0292(11) 0.036(3) Uani 1 2 d S TU P . .
C3 C -0.500000 -0.256(4) 0.0790(15) 0.052(5) Uani 1 2 d S TU P . .
H3 H -0.500000 -0.261856 0.129687 0.062 Uiso 1 2 calc RS T P . .
C4 C -0.500000 -0.102(3) 0.0488(12) 0.052(4) Uani 1 2 d S TU P . .
H4 H -0.500000 -0.009157 0.079703 0.062 Uiso 1 2 calc RS T P . .
C5 C -0.500000 -0.208(3) -0.0600(12) 0.038(3) Uani 1 2 d S TU P . .
C6 C -0.500000 -0.662(3) -0.0781(15) 0.049(5) Uani 1 2 d S TU P . .
H6A H -0.518482 -0.693197 -0.027937 0.073 Uiso 0.5 1 calc GR . . . .
H6B H -0.365380 -0.704911 -0.095817 0.073 Uiso 0.5 1 calc GR . . . .
H6C H -0.616138 -0.706775 -0.106619 0.073 Uiso 0.5 1 calc GR . . . .
C7 C -0.500000 -0.102(3) -0.1823(12) 0.042(5) Uani 1 2 d S TU P . .
H7A H -0.555541 -0.140835 -0.228188 0.063 Uiso 0.5 1 calc GR . . . .
H7B H -0.355343 -0.061726 -0.188905 0.063 Uiso 0.5 1 calc GR . . . .
H7C H -0.589116 -0.012422 -0.164422 0.063 Uiso 0.5 1 calc GR . . . .
C8 C -0.500000 -0.571(2) -0.3496(8) 0.025(3) Uani 1 2 d S TU P . .
C9 C -0.500000 -0.749(3) -0.4429(9) 0.030(3) Uani 1 2 d S TU P . .
C10 C -0.500000 -0.848(3) -0.5536(12) 0.048(4) Uani 1 2 d S TU P . .
H10 H -0.500000 -0.936140 -0.586587 0.057 Uiso 1 2 calc RS T P . .
C11 C -0.500000 -0.690(3) -0.5773(12) 0.041(4) Uani 1 2 d S TU P . .
H11 H -0.500000 -0.676733 -0.627784 0.049 Uiso 1 2 calc RS T P . .
C12 C -0.500000 -0.587(2) -0.4666(11) 0.028(3) Uani 1 2 d S TU P . .
C13 C -0.500000 -0.868(3) -0.3192(13) 0.038(4) Uani 1 2 d S TU P . .
H13A H -0.433156 -0.834068 -0.274359 0.056 Uiso 0.5 1 calc GR . . . .
H13B H -0.421061 -0.960504 -0.339733 0.056 Uiso 0.5 1 calc GR . . . .
H13C H -0.645783 -0.902531 -0.309758 0.056 Uiso 0.5 1 calc GR . . . .
C14 C -0.500000 -0.297(3) -0.4145(14) 0.044(5) Uani 1 2 d S TU P . .
H14A H -0.428982 -0.252994 -0.372134 0.067 Uiso 0.5 1 calc GR . . . .
H14B H -0.645933 -0.257337 -0.416002 0.067 Uiso 0.5 1 calc GR . . . .
H14C H -0.425085 -0.261454 -0.457589 0.067 Uiso 0.5 1 calc GR . . . .
C15 C 0.000000 -0.730(3) -0.2049(10) 0.041(4) Uani 1 2 d S TU P . .
C16 C 0.000000 -0.286(3) -0.2942(13) 0.043(4) Uani 1 2 d S TU P . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Au1 0.0257(4) 0.0300(4) 0.0204(4) 0.0008(12) 0.000 0.000
Au2 0.0288(4) 0.0371(5) 0.0285(8) 0.0023(11) 0.000 0.000
N1 0.028(6) 0.043(7) 0.023(6) -0.003(6) 0.000 0.000
N2 0.020(5) 0.046(7) 0.028(6) -0.010(6) 0.000 0.000
N3 0.030(6) 0.063(8) 0.049(8) -0.023(6) 0.000 0.000
N4 0.006(5) 0.086(9) 0.028(7) -0.003(7) 0.000 0.000
N5 0.027(5) 0.048(7) 0.010(5) 0.002(5) 0.000 0.000
N6 0.022(6) 0.044(7) 0.028(7) 0.002(6) 0.000 0.000
N7 0.018(6) 0.064(8) 0.024(6) 0.006(7) 0.000 0.000
N8 0.027(6) 0.074(9) 0.030(8) -0.014(6) 0.000 0.000
N9 0.073(11) 0.060(13) 0.062(13) 0.015(11) 0.000 0.000
N10 0.096(13) 0.069(15) 0.056(11) 0.025(12) 0.000 0.000
C1 0.018(6) 0.042(7) 0.024(7) 0.003(7) 0.000 0.000
C2 0.022(6) 0.057(8) 0.028(6) -0.006(6) 0.000 0.000
C3 0.019(6) 0.090(11) 0.046(10) -0.011(9) 0.000 0.000
C4 0.023(6) 0.079(10) 0.053(9) -0.025(9) 0.000 0.000
C5 0.025(6) 0.055(8) 0.033(7) -0.017(7) 0.000 0.000
C6 0.042(9) 0.056(13) 0.050(12) 0.005(10) 0.000 0.000
C7 0.062(10) 0.046(12) 0.019(8) -0.004(8) 0.000 0.000
C8 0.017(6) 0.043(8) 0.015(6) -0.005(5) 0.000 0.000
C9 0.021(5) 0.056(8) 0.013(6) -0.003(6) 0.000 0.000
C10 0.025(7) 0.087(10) 0.032(8) -0.016(8) 0.000 0.000
C11 0.023(6) 0.079(11) 0.020(8) -0.005(7) 0.000 0.000
C12 0.005(5) 0.052(8) 0.025(6) 0.004(6) 0.000 0.000
C13 0.047(9) 0.039(11) 0.027(9) -0.001(8) 0.000 0.000
C14 0.043(9) 0.039(11) 0.051(12) -0.008(10) 0.000 0.000
C15 0.036(7) 0.049(9) 0.037(8) -0.002(7) 0.000 0.000
C16 0.037(7) 0.052(10) 0.042(8) 0.012(7) 0.000 0.000
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Au1 Au2 3.1708(2) . ?
Au1 Au2 3.1708(2) 1_455 ?
Au1 C1 2.050(18) . ?
Au1 C8 2.014(16) . ?
Au2 C15 1.99(2) . ?
Au2 C16 1.99(2) . ?
N1 C1 1.35(2) . ?
N1 C2 1.35(2) . ?
N1 C6 1.48(3) . ?
N2 C1 1.34(2) . ?
N2 C5 1.36(2) . ?
N2 C7 1.44(3) . ?
N3 C4 1.34(3) . ?
N3 C5 1.29(2) . ?
N4 C2 1.35(2) . ?
N4 C3 1.39(3) . ?
N5 C8 1.36(2) . ?
N5 C9 1.387(17) . ?
N5 C13 1.45(2) . ?
N6 C8 1.353(19) . ?
N6 C12 1.34(2) . ?
N6 C14 1.51(2) . ?
N7 C11 1.37(3) . ?
N7 C12 1.376(19) . ?
N8 C9 1.27(2) . ?
N8 C10 1.39(3) . ?
N9 C15 1.15(3) . ?
N10 C16 1.11(3) . ?
C2 C5 1.45(3) . ?
C3 H3 0.9500 . ?
C3 C4 1.38(3) . ?
C4 H4 0.9500 . ?
C6 H6A 0.98(7) 3_455 ?
C6 H6A 0.9800 . ?
C6 H6B 1.0(2) 3_455 ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C6 H6C 1.0(3) 3_455 ?
C7 H7A 0.98(8) 3_455 ?
C7 H7A 0.9800 . ?
C7 H7B 0.98(3) 3_455 ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C7 H7C 0.98(10) 3_455 ?
C9 C12 1.39(3) . ?
C10 H10 0.9500 . ?
C10 C11 1.36(4) . ?
C11 H11 0.9500 . ?
C13 H13A 0.9800 . ?
C13 H13A 0.98(8) 3_455 ?
C13 H13B 0.98(10) 3_455 ?
C13 H13B 0.9800 . ?
C13 H13C 0.980(10) 3_455 ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14A 0.98(10) 3_455 ?
C14 H14B 0.980(3) 3_455 ?
C14 H14B 0.9800 . ?
C14 H14C 0.98(10) 3_455 ?
C14 H14C 0.9800 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Au2 Au1 Au2 173.27(4) 1_455 . ?
C1 Au1 Au2 91.97(3) . 1_455 ?
C1 Au1 Au2 91.97(3) . . ?
C8 Au1 Au2 88.10(4) . . ?
C8 Au1 Au2 88.10(4) . 1_455 ?
C8 Au1 C1 178.5(7) . . ?
Au1 Au2 Au1 173.27(4) 1_655 . ?
C15 Au2 Au1 92.57(3) . 1_655 ?
C15 Au2 Au1 92.57(3) . . ?
C15 Au2 C16 178.4(10) . . ?
C16 Au2 Au1 87.37(3) . 1_655 ?
C16 Au2 Au1 87.37(3) . . ?
C1 N1 C2 108.7(15) . . ?
C1 N1 C6 124.9(18) . . ?
C2 N1 C6 126.4(18) . . ?
C1 N2 C5 111.1(17) . . ?
C1 N2 C7 127.0(16) . . ?
C5 N2 C7 121.9(18) . . ?
C5 N3 C4 114(2) . . ?
C2 N4 C3 108.9(19) . . ?
C8 N5 C9 111.3(13) . . ?
C8 N5 C13 124.4(15) . . ?
C9 N5 C13 124.4(16) . . ?
C8 N6 C14 124.4(17) . . ?
C12 N6 C8 109.0(15) . . ?
C12 N6 C14 126.7(17) . . ?
C11 N7 C12 109(2) . . ?
C9 N8 C10 114(2) . . ?
N1 C1 Au1 128.2(13) . . ?
N2 C1 Au1 123.1(12) . . ?
N2 C1 N1 108.8(15) . . ?
N1 C2 N4 128(2) . . ?
N1 C2 C5 107.4(16) . . ?
N4 C2 C5 124.4(18) . . ?
N4 C3 H3 117.1 . . ?
C4 C3 N4 126(2) . . ?
C4 C3 H3 117.1 . . ?
N3 C4 C3 123(2) . . ?
N3 C4 H4 118.3 . . ?
C3 C4 H4 118.3 . . ?
N2 C5 C2 104.0(18) . . ?
N3 C5 N2 133(2) . . ?
N3 C5 C2 123.4(19) . . ?
N1 C6 H6A 109.5(19) . 3_455 ?
N1 C6 H6A 109.5 . . ?
N1 C6 H6B 109(4) . 3_455 ?
N1 C6 H6B 109.5 . . ?
N1 C6 H6C 109(6) . 3_455 ?
N1 C6 H6C 109.5 . . ?
H6A C6 H6A 13.7 . 3_455 ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6B 97.2 . 3_455 ?
H6A C6 H6B 109.5 3_455 3_455 ?
H6A C6 H6C 109.5 . . ?
H6A C6 H6C 120.8 . 3_455 ?
H6A C6 H6C 109.5 3_455 3_455 ?
H6B C6 H6A 97.2 . 3_455 ?
H6B C6 H6B 120.8 . 3_455 ?
H6B C6 H6C 13.7 . 3_455 ?
H6B C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 3_455 3_455 ?
H6C C6 H6A 120.8 . 3_455 ?
H6C C6 H6B 13.7 . 3_455 ?
H6C C6 H6C 97.2 . 3_455 ?
N2 C7 H7A 109.5(19) . 3_455 ?
N2 C7 H7A 109.5 . . ?
N2 C7 H7B 109.5(6) . 3_455 ?
N2 C7 H7B 109.5 . . ?
N2 C7 H7C 109.5 . . ?
N2 C7 H7C 109(2) . 3_455 ?
H7A C7 H7A 42.1 . 3_455 ?
H7A C7 H7B 109.5 3_455 3_455 ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7B 70.3 . 3_455 ?
H7A C7 H7C 109.5 . . ?
H7A C7 H7C 138.3 . 3_455 ?
H7A C7 H7C 109.5 3_455 3_455 ?
H7B C7 H7A 70.3 . 3_455 ?
H7B C7 H7B 138.3 . 3_455 ?
H7B C7 H7C 109.5 . . ?
H7B C7 H7C 42.1 . 3_455 ?
H7B C7 H7C 109.5 3_455 3_455 ?
H7C C7 H7A 138.3 . 3_455 ?
H7C C7 H7B 42.1 . 3_455 ?
H7C C7 H7C 70.3 . 3_455 ?
N5 C8 Au1 125.3(10) . . ?
N6 C8 Au1 128.4(13) . . ?
N6 C8 N5 106.3(12) . . ?
N5 C9 C12 102.9(15) . . ?
N8 C9 N5 129.7(17) . . ?
N8 C9 C12 127.5(17) . . ?
N8 C10 H10 120.3 . . ?
C11 C10 N8 119(2) . . ?
C11 C10 H10 120.3 . . ?
N7 C11 H11 115.8 . . ?
C10 C11 N7 128(2) . . ?
C10 C11 H11 115.8 . . ?
N6 C12 N7 127.5(19) . . ?
N6 C12 C9 110.5(16) . . ?
N7 C12 C9 121.9(18) . . ?
N5 C13 H13A 109(2) . 3_455 ?
N5 C13 H13A 109.5 . . ?
N5 C13 H13B 109.5 . . ?
N5 C13 H13B 109(2) . 3_455 ?
N5 C13 H13C 109.5 . . ?
N5 C13 H13C 109.5(2) . 3_455 ?
H13A C13 H13A 51.2 . 3_455 ?
H13A C13 H13B 109.5 3_455 3_455 ?
H13A C13 H13B 140.7 . 3_455 ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13A C13 H13C 61.3 . 3_455 ?
H13A C13 H13C 109.5 3_455 3_455 ?
H13B C13 H13A 140.7 . 3_455 ?
H13B C13 H13B 61.3 . 3_455 ?
H13B C13 H13C 51.2 . 3_455 ?
H13B C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 3_455 3_455 ?
H13C C13 H13A 61.3 . 3_455 ?
H13C C13 H13B 51.2 . 3_455 ?
H13C C13 H13C 140.7 . 3_455 ?
N6 C14 H14A 109(2) . 3_455 ?
N6 C14 H14A 109.5 . . ?
N6 C14 H14B 109.5 . . ?
N6 C14 H14B 109.47(7) . 3_455 ?
N6 C14 H14C 109.5 . . ?
N6 C14 H14C 109(2) . 3_455 ?
H14A C14 H14A 54.6 . 3_455 ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 3_455 3_455 ?
H14A C14 H14B 57.9 . 3_455 ?
H14A C14 H14C 141.0 . 3_455 ?
H14A C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 3_455 3_455 ?
H14B C14 H14A 57.9 . 3_455 ?
H14B C14 H14B 141.0 . 3_455 ?
H14B C14 H14C 109.5 . . ?
H14B C14 H14C 54.6 . 3_455 ?
H14B C14 H14C 109.5 3_455 3_455 ?
H14C C14 H14A 141.0 . 3_455 ?
H14C C14 H14B 54.6 . 3_455 ?
H14C C14 H14C 57.9 . 3_455 ?
N9 C15 Au2 174.9(19) . . ?
N10 C16 Au2 175(3) . . ?
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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C2 C5 N2 0.000(3) . . . . ?
N1 C2 C5 N3 180.000(3) . . . . ?
N4 C2 C5 N2 180.000(2) . . . . ?
N4 C2 C5 N3 0.000(2) . . . . ?
N4 C3 C4 N3 0.000(2) . . . . ?
N5 C9 C12 N6 0.000(7) . . . . ?
N5 C9 C12 N7 180.000(8) . . . . ?
N8 C9 C12 N6 180.000(9) . . . . ?
N8 C9 C12 N7 0.000(12) . . . . ?
N8 C10 C11 N7 0.000(17) . . . . ?
C1 N1 C2 N4 180.000(3) . . . . ?
C1 N1 C2 C5 0.000(2) . . . . ?
C1 N2 C5 N3 180.000(3) . . . . ?
C1 N2 C5 C2 0.000(3) . . . . ?
C2 N1 C1 Au1 180.000(1) . . . . ?
C2 N1 C1 N2 0.000(3) . . . . ?
C2 N4 C3 C4 0.000(2) . . . . ?
C3 N4 C2 N1 180.000(2) . . . . ?
C3 N4 C2 C5 0.000(2) . . . . ?
C4 N3 C5 N2 180.000(2) . . . . ?
C4 N3 C5 C2 0.000(2) . . . . ?
C5 N2 C1 Au1 180.000(1) . . . . ?
C5 N2 C1 N1 0.000(3) . . . . ?
C5 N3 C4 C3 0.000(2) . . . . ?
C6 N1 C1 Au1 0.000(3) . . . . ?
C6 N1 C1 N2 180.000(3) . . . . ?
C6 N1 C2 N4 0.000(3) . . . . ?
C6 N1 C2 C5 180.000(2) . . . . ?
C7 N2 C1 Au1 0.000(3) . . . . ?
C7 N2 C1 N1 180.000(3) . . . . ?
C7 N2 C5 N3 0.000(3) . . . . ?
C7 N2 C5 C2 180.000(2) . . . . ?
C8 N5 C9 N8 180.000(8) . . . . ?
C8 N5 C9 C12 0.000(7) . . . . ?
C8 N6 C12 N7 180.000(7) . . . . ?
C8 N6 C12 C9 0.000(7) . . . . ?
C9 N5 C8 Au1 180.000(5) . . . . ?
C9 N5 C8 N6 0.000(6) . . . . ?
C9 N8 C10 C11 0.000(14) . . . . ?
C10 N8 C9 N5 180.000(8) . . . . ?
C10 N8 C9 C12 0.000(11) . . . . ?
C11 N7 C12 N6 180.000(8) . . . . ?
C11 N7 C12 C9 0.000(10) . . . . ?
C12 N6 C8 Au1 180.000(5) . . . . ?
C12 N6 C8 N5 0.000(6) . . . . ?
C12 N7 C11 C10 0.000(14) . . . . ?
C13 N5 C8 Au1 0.000(6) . . . . ?
C13 N5 C8 N6 180.000(5) . . . . ?
C13 N5 C9 N8 0.000(10) . . . . ?
C13 N5 C9 C12 180.000(7) . . . . ?
C14 N6 C8 Au1 0.000(7) . . . . ?
C14 N6 C8 N5 180.000(6) . . . . ?
C14 N6 C12 N7 0.000(10) . . . . ?
C14 N6 C12 C9 180.000(7) . . . . ?
_iucr_refine_instructions_details
;
TITL cxy0495
cxy0495_pmn21.res
created by SHELXL-2016/6 at 10:10:35 on 10-Oct-2018
CELL 0.71073 6.3306 8.141 18.7077 90 90 90
ZERR 2 0.0004 0.0005 0.0011 0 0 0
LATT -1
SYMM 0.5-X,-Y,0.5+Z
SYMM -X,+Y,+Z
SYMM 0.5+X,-Y,0.5+Z
SFAC C H Au N
UNIT 32 32 4 20
SIMU 0.01 0.02 2
L.S. 10
PLAN 20
SIZE 0.3 0.06 0.01
TEMP -73.15
CONF
HTAB
BOND $H
fmap 2
acta
TWIN -1 0 0 0 -1 0 0 0 -1 2
REM
REM
REM
WGHT 0.075700 0.118700
EXTI 0.013176
BASF 0.41000
FVAR 0.36600
AU1 3 -0.500000 -0.487625 -0.248280 10.50000 0.02566 0.03002 =
0.02041 0.00083 0.00000 0.00000
AU2 3 0.000000 -0.509757 -0.250797 10.50000 0.02883 0.03710 =
0.02852 0.00234 0.00000 0.00000
N1 4 -0.500000 -0.480689 -0.084011 10.50000 0.02804 0.04275 =
0.02286 -0.00294 0.00000 0.00000
N2 4 -0.500000 -0.235144 -0.131492 10.50000 0.02014 0.04650 =
0.02785 -0.00988 0.00000 0.00000
N3 4 -0.500000 -0.075309 -0.021953 10.50000 0.03015 0.06331 =
0.04880 -0.02283 0.00000 0.00000
N4 4 -0.500000 -0.404320 0.041747 10.50000 0.00631 0.08604 =
0.02776 -0.00262 0.00000 0.00000
N5 4 -0.500000 -0.732060 -0.369105 10.50000 0.02654 0.04822 =
0.01016 0.00162 0.00000 0.00000
N6 4 -0.500000 -0.483267 -0.411005 10.50000 0.02205 0.04386 =
0.02777 0.00169 0.00000 0.00000
N7 4 -0.500000 -0.548152 -0.538123 10.50000 0.01751 0.06388 =
0.02423 0.00576 0.00000 0.00000
N8 4 -0.500000 -0.877944 -0.480693 10.50000 0.02653 0.07367 =
0.02980 -0.01436 0.00000 0.00000
N9 4 0.000000 -0.851538 -0.173462 10.50000 0.07325 0.05990 =
0.06205 0.01453 0.00000 0.00000
N10 4 0.000000 -0.166976 -0.322827 10.50000 0.09645 0.06903 =
0.05595 0.02510 0.00000 0.00000
C1 1 -0.500000 -0.396353 -0.146154 10.50000 0.01848 0.04193 =
0.02362 0.00270 0.00000 0.00000
C2 1 -0.500000 -0.372289 -0.029238 10.50000 0.02240 0.05718 =
0.02816 -0.00565 0.00000 0.00000
C3 1 -0.500000 -0.255994 0.078969 10.50000 0.01946 0.08974 =
0.04578 -0.01128 0.00000 0.00000
AFIX 43
H3 2 -0.500000 -0.261856 0.129687 10.50000 -1.20000
AFIX 0
C4 1 -0.500000 -0.101724 0.048782 10.50000 0.02325 0.07917 =
0.05274 -0.02532 0.00000 0.00000
AFIX 43
H4 2 -0.500000 -0.009157 0.079703 10.50000 -1.20000
AFIX 0
C5 1 -0.500000 -0.208139 -0.059994 10.50000 0.02484 0.05548 =
0.03278 -0.01689 0.00000 0.00000
C6 1 -0.500000 -0.661615 -0.078098 10.50000 0.04160 0.05581 =
0.04954 0.00504 0.00000 0.00000
AFIX 137
H6A 2 -0.518482 -0.693197 -0.027937 10.50000 -1.50000
H6B 2 -0.365380 -0.704911 -0.095817 10.50000 -1.50000
H6C 2 -0.616138 -0.706775 -0.106619 10.50000 -1.50000
AFIX 0
C7 1 -0.500000 -0.101838 -0.182330 10.50000 0.06184 0.04559 =
0.01945 -0.00442 0.00000 0.00000
AFIX 137
H7A 2 -0.555541 -0.140835 -0.228188 10.50000 -1.50000
H7B 2 -0.355343 -0.061726 -0.188905 10.50000 -1.50000
H7C 2 -0.589116 -0.012422 -0.164422 10.50000 -1.50000
AFIX 0
C8 1 -0.500000 -0.571092 -0.349599 10.50000 0.01696 0.04292 =
0.01465 -0.00462 0.00000 0.00000
C9 1 -0.500000 -0.748977 -0.442901 10.50000 0.02122 0.05611 =
0.01278 -0.00294 0.00000 0.00000
C10 1 -0.500000 -0.847503 -0.553558 10.50000 0.02508 0.08653 =
0.03174 -0.01585 0.00000 0.00000
AFIX 43
H10 2 -0.500000 -0.936140 -0.586587 10.50000 -1.20000
AFIX 0
C11 1 -0.500000 -0.690184 -0.577342 10.50000 0.02309 0.07886 =
0.02037 -0.00467 0.00000 0.00000
AFIX 43
H11 2 -0.500000 -0.676733 -0.627784 10.50000 -1.20000
AFIX 0
C12 1 -0.500000 -0.587131 -0.466572 10.50000 0.00533 0.05197 =
0.02525 0.00354 0.00000 0.00000
C13 1 -0.500000 -0.868334 -0.319194 10.50000 0.04716 0.03916 =
0.02656 -0.00063 0.00000 0.00000
AFIX 137
H13A 2 -0.433156 -0.834068 -0.274359 10.50000 -1.50000
H13B 2 -0.421061 -0.960504 -0.339733 10.50000 -1.50000
H13C 2 -0.645783 -0.902531 -0.309758 10.50000 -1.50000
AFIX 0
C14 1 -0.500000 -0.297351 -0.414490 10.50000 0.04297 0.03873 =
0.05131 -0.00839 0.00000 0.00000
AFIX 137
H14A 2 -0.428982 -0.252994 -0.372134 10.50000 -1.50000
H14B 2 -0.645933 -0.257337 -0.416002 10.50000 -1.50000
H14C 2 -0.425085 -0.261454 -0.457589 10.50000 -1.50000
AFIX 0
C15 1 0.000000 -0.729785 -0.204924 10.50000 0.03580 0.04944 =
0.03722 -0.00246 0.00000 0.00000
C16 1 0.000000 -0.286090 -0.294177 10.50000 0.03664 0.05155 =
0.04225 0.01245 0.00000 0.00000
HKLF 4
REM cxy0495
REM R1 = 0.0440 for 2154 Fo > 4sig(Fo) and 0.0566 for all 2603 data
REM 175 parameters refined using 169 restraints
END
WGHT 0.0757 0.1187
REM Instructions for potential hydrogen bonds
EQIV $4 -x-1/2, -y, z+1/2
HTAB C4 N10_$4
EQIV $5 -x-1/2, -y-2, z-1/2
HTAB C10 N9_$5
REM Highest difference peak 2.279, deepest hole -2.263, 1-sigma level 0.589
Q1 1 0.0000 -0.4365 -0.2507 10.50000 0.05 2.28
Q2 1 -0.5000 -0.5724 -0.2470 10.50000 0.05 1.88
Q3 1 -0.2502 -0.9988 -0.3751 11.00000 0.05 1.79
Q4 1 -0.7456 0.0039 -0.1220 11.00000 0.05 1.78
Q5 1 -0.7504 -1.0120 -0.5714 11.00000 0.05 1.65
Q6 1 -0.7562 -0.0019 0.0738 11.00000 0.05 1.60
Q7 1 -0.5000 -0.9934 -0.4415 10.50000 0.05 1.40
Q8 1 -0.5000 -0.9815 -0.3884 10.50000 0.05 1.38
Q9 1 -0.5000 -0.0015 -0.0541 10.50000 0.05 1.37
Q10 1 -0.5000 0.0111 0.1083 10.50000 0.05 1.35
Q11 1 -0.5000 -0.9866 -0.6082 10.50000 0.05 1.32
Q12 1 -0.5000 -0.9804 -0.5533 10.50000 0.05 1.31
Q13 1 -0.5000 0.0190 -0.1060 10.50000 0.05 1.27
Q14 1 -0.5000 0.0307 0.0570 10.50000 0.05 1.22
Q15 1 -0.7587 -0.1122 -0.2466 11.00000 0.05 1.18
Q16 1 -0.2187 -0.0108 -0.2348 11.00000 0.05 1.12
Q17 1 -0.5000 -0.0577 -0.1156 10.50000 0.05 1.10
Q18 1 -0.2684 -0.8720 -0.2508 11.00000 0.05 1.08
Q19 1 -0.7401 -1.0085 -0.2651 11.00000 0.05 1.07
Q20 1 -0.5000 -0.1065 -0.4215 10.50000 0.05 1.02
REM The information below was added by Olex2.
REM
REM R1 = 0.0440 for 2154 Fo > 4sig(Fo) and 0.0566 for all 19246 data
REM n/a parameters refined using n/a restraints
REM Highest difference peak 2.28, deepest hole -2.26
REM Mean Shift 0, Max Shift 0.000.
REM +++ Tabular Listing of Refinement Information +++
REM R1_all = 0.0566
REM R1_gt = 0.0440
REM wR_ref = 0.1336
REM GOOF = 1.222
REM Shift_max = 0.000
REM Shift_mean = 0
REM Reflections_all = 19246
REM Reflections_gt = 2154
REM Parameters = n/a
REM Hole = -2.26
REM Peak = 2.28
REM Flack = n/a
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.59(3)
2 0.41(3)
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_cxy0495_pmn21_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 1871223'
_audit_update_record
;
2018-10-10 deposited with the CCDC.
2018-10-12 downloaded from the CCDC.
;
_audit_creation_date 2018-10-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number 2016/6
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety '0.5(C32 H32 Au4 N20)'
_chemical_formula_sum 'C16 H16 Au2 N10'
_chemical_formula_weight 742.32
_chemical_absolute_configuration .
_chemical_melting_point ?
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_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.
;
_space_group_crystal_system orthorhombic
_space_group_IT_number 31
_space_group_name_H-M_alt 'P m n 21'
_space_group_name_Hall 'P 2ac -2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y, z'
'x+1/2, -y, z+1/2'
_cell_length_a 6.2961(6)
_cell_length_b 8.1146(8)
_cell_length_c 18.7357(17)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_volume 957.21(16)
_cell_formula_units_Z 2
_cell_measurement_reflns_used 9978
_cell_measurement_temperature 150
_cell_measurement_theta_max 28.282
_cell_measurement_theta_min 2.736
_shelx_estimated_absorpt_T_max 0.862
_shelx_estimated_absorpt_T_min 0.091
_exptl_absorpt_coefficient_mu 15.334
_exptl_absorpt_correction_T_max 0.7457
_exptl_absorpt_correction_T_min 0.3813
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1605 before and 0.0892 after correction. The Ratio of minimum to maximum transmission is 0.5113. The \l/2 correction factor is Not present.'
_exptl_absorpt_special_details ?
_exptl_crystal_colour yellow
_exptl_crystal_colour_primary yellow
_exptl_crystal_density_diffrn 2.576
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description plate
_exptl_crystal_F_000 680
_exptl_crystal_size_max 0.3
_exptl_crystal_size_mid 0.06
_exptl_crystal_size_min 0.01
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0519
_diffrn_reflns_av_unetI/netI 0.0344
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max 8
_diffrn_reflns_limit_h_min -8
_diffrn_reflns_limit_k_max 10
_diffrn_reflns_limit_k_min -10
_diffrn_reflns_limit_l_max 24
_diffrn_reflns_limit_l_min -25
_diffrn_reflns_number 17919
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 28.328
_diffrn_reflns_theta_min 2.174
_diffrn_ambient_temperature 150
_diffrn_detector 'Bruker PHOTO 100 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type 'CCD area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device 'three-circle diffractometer'
_diffrn_measurement_device_type 'Bruker PHOTO 100 area detector'
_diffrn_measurement_method '\w and \f scans'
_diffrn_radiation_monochromator 'mirror optics'
_diffrn_radiation_probe x-ray
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'microfocus sealed X-ray tube'
_diffrn_source_type 'Incoatec I\ms'
_reflns_Friedel_coverage 0.944
_reflns_Friedel_fraction_full 1.000
_reflns_Friedel_fraction_max 0.999
_reflns_number_gt 2296
_reflns_number_total 2582
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'SAINT V8.38A (?, 2016)'
_computing_data_collection ?
_computing_data_reduction 'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'XL (Sheldrick, 2008)'
_computing_structure_solution 'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max 3.517
_refine_diff_density_min -1.836
_refine_diff_density_rms 0.732
_refine_ls_abs_structure_details
;
Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack 0.41(3)
_refine_ls_extinction_coef 0.0119(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method 'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref 1.256
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 175
_refine_ls_number_reflns 2582
_refine_ls_number_restraints 181
_refine_ls_R_factor_all 0.0493
_refine_ls_R_factor_gt 0.0416
_refine_ls_restrained_S_all 1.232
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0704P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1081
_refine_ls_wR_factor_ref 0.1208
_refine_special_details
;
Refined as a 2-component inversion twin.
Location of maximum Q peak
Atom Peak x y z
Q1 3.53 0.0000 -0.4328 -0.2493
Distances to nearest atoms (including eq.)
0.66 Au2 1.42 C16 2.40 H11 2.55 C15
;
_olex2_refinement_description
;
1. Twinned data refinement
Scales: 0.59(3)
0.41(3)
2. Fixed Uiso
At 1.2 times of:
All C(H) groups
At 1.5 times of:
All C(H,H,H) groups
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
Uanis(C12) \\sim Ueq, Uanis(N4) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Others
Fixed Sof: H6A(0.5) H6B(0.5) H6C(0.5) H7A(0.5) H7B(0.5) H7C(0.5) H13A(0.5)
H13B(0.5) H13C(0.5) H14A(0.5) H14B(0.5) H14C(0.5)
5.a Aromatic/amide H refined with riding coordinates:
C3(H3), C4(H4), C10(H10), C11(H11)
5.b Idealised Me refined as rotating group:
C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary dual
_atom_sites_solution_secondary ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Au1 Au -0.500000 -0.48342(8) -0.24828(2) 0.0186(3) Uani 1 2 d S TU P . .
Au2 Au 0.000000 -0.51373(8) -0.25188(5) 0.0234(4) Uani 1 2 d S TU P . .
N1 N -0.500000 -0.4721(17) -0.0838(9) 0.021(3) Uani 1 2 d S TU P . .
N2 N -0.500000 -0.2283(18) -0.1316(8) 0.021(2) Uani 1 2 d S TU P . .
N3 N -0.500000 -0.067(2) -0.0231(8) 0.034(4) Uani 1 2 d S TU P . .
N4 N -0.500000 -0.390(2) 0.0417(9) 0.031(3) Uani 1 2 d S TU P . .
N5 N -0.500000 -0.7267(16) -0.3691(7) 0.020(2) Uani 1 2 d S TU P . .
N6 N -0.500000 -0.4755(18) -0.4104(8) 0.025(3) Uani 1 2 d S TU P . .
N7 N -0.500000 -0.539(2) -0.5375(9) 0.026(3) Uani 1 2 d S TU P . .
N8 N -0.500000 -0.872(2) -0.4833(8) 0.031(3) Uani 1 2 d S TU P . .
N9 N 0.000000 -0.857(3) -0.1744(12) 0.050(5) Uani 1 2 d S TU P . .
N10 N 0.000000 -0.167(3) -0.3228(13) 0.059(6) Uani 1 2 d S TU P . .
C1 C -0.500000 -0.391(2) -0.1468(8) 0.020(3) Uani 1 2 d S TU P . .
C2 C -0.500000 -0.365(2) -0.0284(10) 0.027(3) Uani 1 2 d S TU P . .
C3 C -0.500000 -0.245(3) 0.0781(12) 0.036(4) Uani 1 2 d S TU P . .
H3 H -0.500000 -0.250793 0.128707 0.043 Uiso 1 2 calc RS T P . .
C4 C -0.500000 -0.091(3) 0.0474(11) 0.037(4) Uani 1 2 d S TU P . .
H4 H -0.500000 0.002141 0.077814 0.045 Uiso 1 2 calc RS T P . .
C5 C -0.500000 -0.203(2) -0.0601(11) 0.024(3) Uani 1 2 d S TU P . .
C6 C -0.500000 -0.655(3) -0.0761(11) 0.032(4) Uani 1 2 d S TU P . .
H6A H -0.483550 -0.683677 -0.025632 0.048 Uiso 0.5 1 calc GR . . . .
H6B H -0.381937 -0.701293 -0.103553 0.048 Uiso 0.5 1 calc GR . . . .
H6C H -0.634513 -0.699139 -0.094024 0.048 Uiso 0.5 1 calc GR . . . .
C7 C -0.500000 -0.095(3) -0.1846(11) 0.034(4) Uani 1 2 d S TU P . .
H7A H -0.409071 -0.005122 -0.167968 0.051 Uiso 0.5 1 calc GR . . . .
H7B H -0.645217 -0.054531 -0.191217 0.051 Uiso 0.5 1 calc GR . . . .
H7C H -0.445712 -0.137289 -0.230158 0.051 Uiso 0.5 1 calc GR . . . .
C8 C -0.500000 -0.566(2) -0.3506(8) 0.017(3) Uani 1 2 d S TU P . .
C9 C -0.500000 -0.740(2) -0.4434(9) 0.022(3) Uani 1 2 d S TU P . .
C10 C -0.500000 -0.836(3) -0.5539(10) 0.031(3) Uani 1 2 d S TU P . .
H10 H -0.500000 -0.922551 -0.587891 0.037 Uiso 1 2 calc RS T P . .
C11 C -0.500000 -0.676(3) -0.5774(10) 0.028(4) Uani 1 2 d S TU P . .
H11 H -0.500000 -0.659926 -0.627629 0.034 Uiso 1 2 calc RS T P . .
C12 C -0.500000 -0.579(2) -0.4676(10) 0.020(3) Uani 1 2 d S TU P . .
C13 C -0.500000 -0.864(3) -0.3207(12) 0.027(4) Uani 1 2 d S TU P . .
H13A H -0.443953 -0.828777 -0.274308 0.041 Uiso 0.5 1 calc GR . . . .
H13B H -0.410569 -0.952219 -0.339972 0.041 Uiso 0.5 1 calc GR . . . .
H13C H -0.645479 -0.904662 -0.314674 0.041 Uiso 0.5 1 calc GR . . . .
C14 C -0.500000 -0.292(3) -0.4145(12) 0.033(4) Uani 1 2 d S TU P . .
H14A H -0.422587 -0.247177 -0.373554 0.050 Uiso 0.5 1 calc GR . . . .
H14B H -0.646675 -0.251995 -0.413814 0.050 Uiso 0.5 1 calc GR . . . .
H14C H -0.430738 -0.257380 -0.458812 0.050 Uiso 0.5 1 calc GR . . . .
C15 C 0.000000 -0.731(2) -0.2060(9) 0.031(3) Uani 1 2 d S TU P . .
C16 C 0.000000 -0.291(2) -0.2941(11) 0.033(4) Uani 1 2 d S TU P . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Au1 0.0187(3) 0.0216(4) 0.0156(5) 0.0005(10) 0.000 0.000
Au2 0.0213(4) 0.0287(4) 0.0202(8) 0.0018(10) 0.000 0.000
N1 0.018(5) 0.028(6) 0.016(6) 0.000(5) 0.000 0.000
N2 0.014(5) 0.031(6) 0.016(5) -0.002(5) 0.000 0.000
N3 0.021(6) 0.045(8) 0.036(8) -0.018(5) 0.000 0.000
N4 0.006(4) 0.062(8) 0.025(6) 0.003(6) 0.000 0.000
N5 0.018(5) 0.034(6) 0.008(5) 0.001(5) 0.000 0.000
N6 0.015(5) 0.032(7) 0.028(7) 0.005(5) 0.000 0.000
N7 0.015(6) 0.049(8) 0.014(6) 0.010(6) 0.000 0.000
N8 0.021(5) 0.046(8) 0.027(8) -0.007(5) 0.000 0.000
N9 0.052(9) 0.048(12) 0.050(11) 0.012(9) 0.000 0.000
N10 0.070(11) 0.062(14) 0.046(10) 0.020(11) 0.000 0.000
C1 0.015(5) 0.028(7) 0.015(6) 0.002(6) 0.000 0.000
C2 0.017(6) 0.042(7) 0.022(6) -0.001(6) 0.000 0.000
C3 0.017(6) 0.065(10) 0.027(8) -0.005(8) 0.000 0.000
C4 0.018(6) 0.056(9) 0.037(9) -0.019(7) 0.000 0.000
C5 0.013(5) 0.038(7) 0.021(6) -0.010(6) 0.000 0.000
C6 0.035(8) 0.036(10) 0.025(8) 0.008(8) 0.000 0.000
C7 0.050(9) 0.034(10) 0.019(8) -0.003(7) 0.000 0.000
C8 0.014(5) 0.027(7) 0.011(6) 0.003(5) 0.000 0.000
C9 0.014(5) 0.039(7) 0.011(6) -0.004(6) 0.000 0.000
C10 0.015(6) 0.057(9) 0.020(7) -0.005(7) 0.000 0.000
C11 0.016(6) 0.058(10) 0.010(7) -0.001(6) 0.000 0.000
C12 0.008(5) 0.033(6) 0.019(6) 0.003(6) 0.000 0.000
C13 0.030(7) 0.024(10) 0.027(8) 0.002(7) 0.000 0.000
C14 0.032(8) 0.030(10) 0.037(10) 0.000(8) 0.000 0.000
C15 0.024(6) 0.044(9) 0.024(7) 0.000(6) 0.000 0.000
C16 0.021(6) 0.045(9) 0.033(8) 0.010(7) 0.000 0.000
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Au1 Au2 3.1584(3) 1_455 ?
Au1 Au2 3.1584(3) . ?
Au1 C1 2.043(16) . ?
Au1 C8 2.032(15) . ?
Au2 C15 1.96(2) . ?
Au2 C16 1.971(19) . ?
N1 C1 1.35(2) . ?
N1 C2 1.36(2) . ?
N1 C6 1.49(3) . ?
N2 C1 1.35(2) . ?
N2 C5 1.356(18) . ?
N2 C7 1.47(2) . ?
N3 C4 1.34(3) . ?
N3 C5 1.30(2) . ?
N4 C2 1.328(19) . ?
N4 C3 1.36(3) . ?
N5 C8 1.348(19) . ?
N5 C9 1.396(16) . ?
N5 C13 1.44(2) . ?
N6 C8 1.339(18) . ?
N6 C12 1.36(2) . ?
N6 C14 1.49(2) . ?
N7 C11 1.33(3) . ?
N7 C12 1.349(17) . ?
N8 C9 1.31(2) . ?
N8 C10 1.36(2) . ?
N9 C15 1.18(3) . ?
N10 C16 1.14(3) . ?
C2 C5 1.44(3) . ?
C3 H3 0.9500 . ?
C3 C4 1.37(3) . ?
C4 H4 0.9500 . ?
C6 H6A 0.98(6) 3_455 ?
C6 H6A 0.9800 . ?
C6 H6B 1.0(2) 3_455 ?
C6 H6B 0.9800 . ?
C6 H6C 0.98(19) 3_455 ?
C6 H6C 0.9800 . ?
C7 H7A 0.98(10) 3_455 ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7B 0.98(3) 3_455 ?
C7 H7C 0.9800 . ?
C7 H7C 0.98(7) 3_455 ?
C9 C12 1.38(2) . ?
C10 H10 0.9500 . ?
C10 C11 1.37(3) . ?
C11 H11 0.9500 . ?
C13 H13A 0.98(7) 3_455 ?
C13 H13A 0.9800 . ?
C13 H13B 0.98(10) 3_455 ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C13 H13C 0.98(3) 3_455 ?
C14 H14A 0.9800 . ?
C14 H14A 0.98(9) 3_455 ?
C14 H14B 0.9800 . ?
C14 H14B 0.980(6) 3_455 ?
C14 H14C 0.98(8) 3_455 ?
C14 H14C 0.9800 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Au2 Au1 Au2 170.74(4) . 1_455 ?
C1 Au1 Au2 92.77(3) . 1_455 ?
C1 Au1 Au2 92.77(3) . . ?
C8 Au1 Au2 87.37(4) . . ?
C8 Au1 Au2 87.37(4) . 1_455 ?
C8 Au1 C1 177.8(6) . . ?
Au1 Au2 Au1 170.74(4) 1_655 . ?
C15 Au2 Au1 93.47(3) . 1_655 ?
C15 Au2 Au1 93.47(3) . . ?
C15 Au2 C16 177.6(8) . . ?
C16 Au2 Au1 86.40(4) . . ?
C16 Au2 Au1 86.40(4) . 1_655 ?
C1 N1 C2 110.9(13) . . ?
C1 N1 C6 124.7(15) . . ?
C2 N1 C6 124.4(15) . . ?
C1 N2 C5 111.0(15) . . ?
C1 N2 C7 125.2(14) . . ?
C5 N2 C7 123.8(16) . . ?
C5 N3 C4 113.6(18) . . ?
C2 N4 C3 111.3(17) . . ?
C8 N5 C9 109.3(12) . . ?
C8 N5 C13 126.0(14) . . ?
C9 N5 C13 124.8(15) . . ?
C8 N6 C12 108.7(14) . . ?
C8 N6 C14 126.3(16) . . ?
C12 N6 C14 125.0(16) . . ?
C11 N7 C12 110.3(18) . . ?
C9 N8 C10 112.1(17) . . ?
N1 C1 Au1 129.4(12) . . ?
N1 C1 N2 106.9(14) . . ?
N2 C1 Au1 123.7(10) . . ?
N1 C2 C5 105.7(15) . . ?
N4 C2 N1 131.1(19) . . ?
N4 C2 C5 123.2(17) . . ?
N4 C3 H3 117.5 . . ?
N4 C3 C4 125.1(19) . . ?
C4 C3 H3 117.5 . . ?
N3 C4 C3 123.3(19) . . ?
N3 C4 H4 118.4 . . ?
C3 C4 H4 118.4 . . ?
N2 C5 C2 105.5(17) . . ?
N3 C5 N2 131.0(19) . . ?
N3 C5 C2 123.5(17) . . ?
N1 C6 H6A 109.5 . . ?
N1 C6 H6A 109.5(16) . 3_455 ?
N1 C6 H6B 109(5) . 3_455 ?
N1 C6 H6B 109.5 . . ?
N1 C6 H6C 109(4) . 3_455 ?
N1 C6 H6C 109.5 . . ?
H6A C6 H6A 12.1 . 3_455 ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 3_455 3_455 ?
H6A C6 H6B 119.6 . 3_455 ?
H6A C6 H6C 98.7 . 3_455 ?
H6A C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 3_455 3_455 ?
H6B C6 H6A 119.6 . 3_455 ?
H6B C6 H6B 98.7 . 3_455 ?
H6B C6 H6C 12.1 . 3_455 ?
H6B C6 H6C 109.5 3_455 3_455 ?
H6B C6 H6C 109.5 . . ?
H6C C6 H6A 98.7 . 3_455 ?
H6C C6 H6B 12.1 . 3_455 ?
H6C C6 H6C 119.6 . 3_455 ?
N2 C7 H7A 109.5 . . ?
N2 C7 H7A 109(2) . 3_455 ?
N2 C7 H7B 109.5(6) . 3_455 ?
N2 C7 H7B 109.5 . . ?
N2 C7 H7C 109.5 . . ?
N2 C7 H7C 109.5(18) . 3_455 ?
H7A C7 H7A 71.5 . 3_455 ?
H7A C7 H7B 40.8 . 3_455 ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 3_455 3_455 ?
H7A C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 3_455 3_455 ?
H7A C7 H7C 137.8 . 3_455 ?
H7B C7 H7A 40.8 . 3_455 ?
H7B C7 H7B 137.8 . 3_455 ?
H7B C7 H7C 71.5 . 3_455 ?
H7B C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 3_455 3_455 ?
H7C C7 H7A 137.8 . 3_455 ?
H7C C7 H7B 71.5 . 3_455 ?
H7C C7 H7C 40.8 . 3_455 ?
N5 C8 Au1 124.2(10) . . ?
N6 C8 Au1 127.4(12) . . ?
N6 C8 N5 108.5(12) . . ?
N8 C9 N5 129.2(15) . . ?
N8 C9 C12 126.1(16) . . ?
C12 C9 N5 104.7(14) . . ?
N8 C10 H10 119.3 . . ?
N8 C10 C11 121.4(19) . . ?
C11 C10 H10 119.3 . . ?
N7 C11 C10 127.3(18) . . ?
N7 C11 H11 116.3 . . ?
C10 C11 H11 116.3 . . ?
N6 C12 C9 108.9(15) . . ?
N7 C12 N6 128.3(17) . . ?
N7 C12 C9 122.8(17) . . ?
N5 C13 H13A 109.5 . . ?
N5 C13 H13A 109.5(18) . 3_455 ?
N5 C13 H13B 109.5 . . ?
N5 C13 H13B 109(2) . 3_455 ?
N5 C13 H13C 109.5 . . ?
N5 C13 H13C 109.5(6) . 3_455 ?
H13A C13 H13A 42.2 . 3_455 ?
H13A C13 H13B 138.3 . 3_455 ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 3_455 3_455 ?
H13A C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 3_455 3_455 ?
H13A C13 H13C 70.1 . 3_455 ?
H13B C13 H13A 138.3 . 3_455 ?
H13B C13 H13B 70.1 . 3_455 ?
H13B C13 H13C 109.5 . . ?
H13B C13 H13C 42.2 . 3_455 ?
H13B C13 H13C 109.5 3_455 3_455 ?
H13C C13 H13A 70.1 . 3_455 ?
H13C C13 H13B 42.2 . 3_455 ?
H13C C13 H13C 138.3 . 3_455 ?
N6 C14 H14A 109.5 . . ?
N6 C14 H14A 109(2) . 3_455 ?
N6 C14 H14B 109.5 . . ?
N6 C14 H14B 109.47(14) . 3_455 ?
N6 C14 H14C 109.5 . . ?
N6 C14 H14C 109(2) . 3_455 ?
H14A C14 H14A 59.6 . 3_455 ?
H14A C14 H14B 109.5 3_455 3_455 ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14B 52.8 . 3_455 ?
H14A C14 H14C 140.9 . 3_455 ?
H14A C14 H14C 109.5 3_455 3_455 ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14A 52.8 . 3_455 ?
H14B C14 H14B 140.9 . 3_455 ?
H14B C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 3_455 3_455 ?
H14B C14 H14C 59.6 . 3_455 ?
H14C C14 H14A 140.9 . 3_455 ?
H14C C14 H14B 59.6 . 3_455 ?
H14C C14 H14C 52.8 . 3_455 ?
N9 C15 Au2 176.0(17) . . ?
N10 C16 Au2 176(2) . . ?
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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C2 C5 N2 0.000(3) . . . . ?
N1 C2 C5 N3 180.000(2) . . . . ?
N4 C2 C5 N2 180.000(2) . . . . ?
N4 C2 C5 N3 0.000(2) . . . . ?
N4 C3 C4 N3 0.000(2) . . . . ?
N5 C9 C12 N6 0.000(6) . . . . ?
N5 C9 C12 N7 180.000(7) . . . . ?
N8 C9 C12 N6 180.000(7) . . . . ?
N8 C9 C12 N7 0.000(11) . . . . ?
N8 C10 C11 N7 0.000(15) . . . . ?
C1 N1 C2 N4 180.000(3) . . . . ?
C1 N1 C2 C5 0.000(2) . . . . ?
C1 N2 C5 N3 180.000(2) . . . . ?
C1 N2 C5 C2 0.000(3) . . . . ?
C2 N1 C1 Au1 180.000(1) . . . . ?
C2 N1 C1 N2 0.000(2) . . . . ?
C2 N4 C3 C4 0.000(1) . . . . ?
C3 N4 C2 N1 180.000(2) . . . . ?
C3 N4 C2 C5 0.000(2) . . . . ?
C4 N3 C5 N2 180.000(1) . . . . ?
C4 N3 C5 C2 0.000(1) . . . . ?
C5 N2 C1 Au1 180.000(1) . . . . ?
C5 N2 C1 N1 0.000(2) . . . . ?
C5 N3 C4 C3 0.000(1) . . . . ?
C6 N1 C1 Au1 0.000(3) . . . . ?
C6 N1 C1 N2 180.000(2) . . . . ?
C6 N1 C2 N4 0.000(3) . . . . ?
C6 N1 C2 C5 180.000(2) . . . . ?
C7 N2 C1 Au1 0.000(3) . . . . ?
C7 N2 C1 N1 180.000(2) . . . . ?
C7 N2 C5 N3 0.000(3) . . . . ?
C7 N2 C5 C2 180.000(2) . . . . ?
C8 N5 C9 N8 180.000(7) . . . . ?
C8 N5 C9 C12 0.000(6) . . . . ?
C8 N6 C12 N7 180.000(8) . . . . ?
C8 N6 C12 C9 0.000(7) . . . . ?
C9 N5 C8 Au1 180.000(4) . . . . ?
C9 N5 C8 N6 0.000(6) . . . . ?
C9 N8 C10 C11 0.000(13) . . . . ?
C10 N8 C9 N5 180.000(8) . . . . ?
C10 N8 C9 C12 0.000(8) . . . . ?
C11 N7 C12 N6 180.000(8) . . . . ?
C11 N7 C12 C9 0.000(9) . . . . ?
C12 N6 C8 Au1 180.000(5) . . . . ?
C12 N6 C8 N5 0.000(5) . . . . ?
C12 N7 C11 C10 0.000(13) . . . . ?
C13 N5 C8 Au1 0.000(6) . . . . ?
C13 N5 C8 N6 180.000(5) . . . . ?
C13 N5 C9 N8 0.000(9) . . . . ?
C13 N5 C9 C12 180.000(7) . . . . ?
C14 N6 C8 Au1 0.000(6) . . . . ?
C14 N6 C8 N5 180.000(5) . . . . ?
C14 N6 C12 N7 0.000(10) . . . . ?
C14 N6 C12 C9 180.000(6) . . . . ?
_iucr_refine_instructions_details
;
TITL cxy0495
cxy0495_pmn21.res
created by SHELXL-2016/6 at 14:04:47 on 10-Oct-2018
CELL 0.71073 6.2961 8.1146 18.7357 90 90 90
ZERR 2 0.0006 0.0008 0.0017 0 0 0
LATT -1
SYMM 0.5-X,-Y,0.5+Z
SYMM -X,+Y,+Z
SYMM 0.5+X,-Y,0.5+Z
SFAC C H Au N
UNIT 32 32 4 20
SIMU 0.01 0.02 2
ISOR 0.01 0.02 C12 N4
L.S. 10
PLAN 20
SIZE 0.3 0.06 0.01
TEMP -73.15
CONF
HTAB
BOND $H
fmap 2
acta
TWIN -1 0 0 0 -1 0 0 0 -1 2
REM
REM
REM
WGHT 0.070400
EXTI 0.011886
BASF 0.41297
FVAR 0.28038
AU1 3 -0.500000 -0.483415 -0.248280 10.50000 0.01865 0.02159 =
0.01557 0.00047 0.00000 0.00000
AU2 3 0.000000 -0.513730 -0.251880 10.50000 0.02128 0.02873 =
0.02016 0.00178 0.00000 0.00000
N1 4 -0.500000 -0.472084 -0.083843 10.50000 0.01847 0.02776 =
0.01613 -0.00032 0.00000 0.00000
N2 4 -0.500000 -0.228317 -0.131598 10.50000 0.01427 0.03112 =
0.01641 -0.00181 0.00000 0.00000
N3 4 -0.500000 -0.067080 -0.023125 10.50000 0.02115 0.04474 =
0.03634 -0.01798 0.00000 0.00000
N4 4 -0.500000 -0.389736 0.041661 10.50000 0.00642 0.06243 =
0.02533 0.00333 0.00000 0.00000
N5 4 -0.500000 -0.726696 -0.369080 10.50000 0.01766 0.03390 =
0.00840 0.00101 0.00000 0.00000
N6 4 -0.500000 -0.475504 -0.410381 10.50000 0.01521 0.03166 =
0.02803 0.00458 0.00000 0.00000
N7 4 -0.500000 -0.539268 -0.537533 10.50000 0.01513 0.04949 =
0.01418 0.01000 0.00000 0.00000
N8 4 -0.500000 -0.872444 -0.483311 10.50000 0.02060 0.04639 =
0.02689 -0.00672 0.00000 0.00000
N9 4 0.000000 -0.856552 -0.174401 10.50000 0.05226 0.04762 =
0.05040 0.01162 0.00000 0.00000
N10 4 0.000000 -0.167441 -0.322752 10.50000 0.06996 0.06241 =
0.04557 0.01952 0.00000 0.00000
C1 1 -0.500000 -0.391241 -0.146826 10.50000 0.01534 0.02839 =
0.01528 0.00237 0.00000 0.00000
C2 1 -0.500000 -0.364509 -0.028362 10.50000 0.01726 0.04171 =
0.02192 -0.00087 0.00000 0.00000
C3 1 -0.500000 -0.245236 0.078059 10.50000 0.01686 0.06463 =
0.02655 -0.00496 0.00000 0.00000
AFIX 43
H3 2 -0.500000 -0.250793 0.128707 10.50000 -1.20000
AFIX 0
C4 1 -0.500000 -0.091488 0.047374 10.50000 0.01829 0.05601 =
0.03735 -0.01875 0.00000 0.00000
AFIX 43
H4 2 -0.500000 0.002141 0.077814 10.50000 -1.20000
AFIX 0
C5 1 -0.500000 -0.202745 -0.060059 10.50000 0.01316 0.03803 =
0.02059 -0.01003 0.00000 0.00000
C6 1 -0.500000 -0.654638 -0.076102 10.50000 0.03522 0.03628 =
0.02506 0.00834 0.00000 0.00000
AFIX 137
H6A 2 -0.483550 -0.683677 -0.025632 10.50000 -1.50000
H6B 2 -0.381937 -0.701293 -0.103553 10.50000 -1.50000
H6C 2 -0.634513 -0.699139 -0.094024 10.50000 -1.50000
AFIX 0
C7 1 -0.500000 -0.095267 -0.184640 10.50000 0.05000 0.03380 =
0.01850 -0.00339 0.00000 0.00000
AFIX 137
H7A 2 -0.409071 -0.005122 -0.167968 10.50000 -1.50000
H7B 2 -0.645217 -0.054531 -0.191217 10.50000 -1.50000
H7C 2 -0.445712 -0.137289 -0.230158 10.50000 -1.50000
AFIX 0
C8 1 -0.500000 -0.566150 -0.350633 10.50000 0.01435 0.02719 =
0.01085 0.00284 0.00000 0.00000
C9 1 -0.500000 -0.739898 -0.443387 10.50000 0.01443 0.03881 =
0.01130 -0.00430 0.00000 0.00000
C10 1 -0.500000 -0.835587 -0.553944 10.50000 0.01455 0.05716 =
0.02040 -0.00477 0.00000 0.00000
AFIX 43
H10 2 -0.500000 -0.922551 -0.587891 10.50000 -1.20000
AFIX 0
C11 1 -0.500000 -0.675552 -0.577377 10.50000 0.01604 0.05826 =
0.01013 -0.00085 0.00000 0.00000
AFIX 43
H11 2 -0.500000 -0.659926 -0.627629 10.50000 -1.20000
AFIX 0
C12 1 -0.500000 -0.578626 -0.467574 10.50000 0.00755 0.03272 =
0.01925 0.00270 0.00000 0.00000
C13 1 -0.500000 -0.864002 -0.320660 10.50000 0.03043 0.02447 =
0.02742 0.00189 0.00000 0.00000
AFIX 137
H13A 2 -0.443953 -0.828777 -0.274308 10.50000 -1.50000
H13B 2 -0.410569 -0.952219 -0.339972 10.50000 -1.50000
H13C 2 -0.645479 -0.904662 -0.314674 10.50000 -1.50000
AFIX 0
C14 1 -0.500000 -0.292387 -0.414491 10.50000 0.03171 0.03040 =
0.03737 0.00018 0.00000 0.00000
AFIX 137
H14A 2 -0.422587 -0.247177 -0.373554 10.50000 -1.50000
H14B 2 -0.646675 -0.251995 -0.413814 10.50000 -1.50000
H14C 2 -0.430738 -0.257380 -0.458812 10.50000 -1.50000
AFIX 0
C15 1 0.000000 -0.730545 -0.205960 10.50000 0.02445 0.04408 =
0.02447 -0.00038 0.00000 0.00000
C16 1 0.000000 -0.291281 -0.294088 10.50000 0.02089 0.04492 =
0.03346 0.01012 0.00000 0.00000
HKLF 4
REM cxy0495
REM R1 = 0.0416 for 2296 Fo > 4sig(Fo) and 0.0493 for all 2582 data
REM 175 parameters refined using 181 restraints
END
WGHT 0.0704 0.0000
REM Instructions for potential hydrogen bonds
EQIV $4 -x-1/2, -y, z+1/2
HTAB C4 N10_$4
EQIV $5 -x-1/2, -y-2, z-1/2
HTAB C10 N9_$5
REM Highest difference peak 3.517, deepest hole -1.836, 1-sigma level 0.732
Q1 1 0.0000 -0.4328 -0.2493 10.50000 0.05 3.52
Q2 1 -0.5000 -0.5673 -0.2496 10.50000 0.05 2.81
Q3 1 -0.5000 -0.9970 -0.4392 10.50000 0.05 2.02
Q4 1 -0.7737 0.0033 0.0486 11.00000 0.05 1.89
Q5 1 -0.5000 -0.0024 -0.0524 10.50000 0.05 1.87
Q6 1 -0.7420 -0.0106 -0.0483 11.00000 0.05 1.85
Q7 1 -0.5000 0.0032 0.0487 10.50000 0.05 1.85
Q8 1 -0.5000 -0.0263 0.0336 10.50000 0.05 1.81
Q9 1 -0.5000 -1.0037 -0.5573 10.50000 0.05 1.80
Q10 1 -0.7206 -0.0133 0.0015 11.00000 0.05 1.80
Q11 1 -0.5000 -1.0217 -0.5284 10.50000 0.05 1.78
Q12 1 -0.5000 -1.0329 -0.4720 10.50000 0.05 1.76
Q13 1 -0.7518 -0.9079 -0.0685 11.00000 0.05 1.40
Q14 1 -0.5000 -0.8784 -0.5009 10.50000 0.05 1.26
Q15 1 -0.7449 0.0014 -0.2494 11.00000 0.05 1.21
Q16 1 -0.2365 -0.2331 -0.3495 11.00000 0.05 1.07
Q17 1 -0.7817 -0.1163 -0.3793 11.00000 0.05 1.05
Q18 1 -0.7886 -0.2166 -0.4032 11.00000 0.05 1.04
Q19 1 -0.5000 -0.1646 -0.4417 10.50000 0.05 1.03
Q20 1 -0.7097 -0.8029 -0.0938 11.00000 0.05 1.02
REM The information below was added by Olex2.
REM
REM R1 = 0.0416 for 2296 Fo > 4sig(Fo) and 0.0493 for all 18805 data
REM n/a parameters refined using n/a restraints
REM Highest difference peak 3.52, deepest hole -1.84
REM Mean Shift 0, Max Shift 0.000.
REM +++ Tabular Listing of Refinement Information +++
REM R1_all = 0.0493
REM R1_gt = 0.0416
REM wR_ref = 0.1208
REM GOOF = 1.256
REM Shift_max = 0.000
REM Shift_mean = 0
REM Reflections_all = 18805
REM Reflections_gt = 2296
REM Parameters = n/a
REM Hole = -1.84
REM Peak = 3.52
REM Flack = n/a
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.59(3)
2 0.41(3)
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_cxy0495_pmna_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1844722'
_audit_update_record
;
2018-10-10 deposited with the CCDC.
2018-10-12 downloaded from the CCDC.
;
_audit_creation_date 2018-09-27
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number 2016/6
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C16 H16 Au2 N10'
_chemical_formula_sum 'C16 H16 Au2 N10'
_chemical_formula_weight 742.32
_chemical_melting_point ?
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_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.
;
_space_group_crystal_system orthorhombic
_space_group_IT_number 53
_space_group_name_H-M_alt 'P m n a'
_space_group_name_Hall '-P 2ac 2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x, -y, -z'
'-x+1/2, y, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x, y, z'
'x-1/2, -y, z-1/2'
_cell_length_a 6.3929(4)
_cell_length_b 8.1734(6)
_cell_length_c 18.6898(12)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_volume 976.57(11)
_cell_formula_units_Z 2
_cell_measurement_reflns_used 5798
_cell_measurement_temperature 298
_cell_measurement_theta_max 28.276
_cell_measurement_theta_min 2.720
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 15.030
_exptl_absorpt_correction_T_max 0.7457
_exptl_absorpt_correction_T_min 0.3901
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1602 before and 0.0919 after correction. The Ratio of minimum to maximum transmission is 0.5231. The \l/2 correction factor is Not present.'
_exptl_absorpt_special_details ?
_exptl_crystal_colour yellow
_exptl_crystal_colour_primary yellow
_exptl_crystal_density_diffrn 2.524
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description plate
_exptl_crystal_F_000 680
_exptl_crystal_size_max 0.3
_exptl_crystal_size_mid 0.06
_exptl_crystal_size_min 0.01
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0653
_diffrn_reflns_av_unetI/netI 0.0298
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max 8
_diffrn_reflns_limit_h_min -8
_diffrn_reflns_limit_k_max 10
_diffrn_reflns_limit_k_min -10
_diffrn_reflns_limit_l_max 24
_diffrn_reflns_limit_l_min -24
_diffrn_reflns_number 18575
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 28.333
_diffrn_reflns_theta_min 2.179
_diffrn_ambient_temperature 298
_diffrn_detector 'Bruker PHOTO 100 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type 'CCD area detector'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device 'three-circle diffractometer'
_diffrn_measurement_device_type 'Bruker PHOTO 100 area detector'
_diffrn_measurement_method '\w and \f scans'
_diffrn_radiation_monochromator 'mirror optics'
_diffrn_radiation_probe x-ray
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'microfocus sealed X-ray tube'
_diffrn_source_type 'Incoatec I\ms'
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 905
_reflns_number_total 1321
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'SAINT V8.38A (?, 2016)'
_computing_data_collection ?
_computing_data_reduction 'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'XL (Sheldrick, 2008)'
_computing_structure_solution 'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max 2.263
_refine_diff_density_min -1.331
_refine_diff_density_rms 0.416
_refine_ls_extinction_coef 0.0113(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method 'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref 1.165
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 90
_refine_ls_number_reflns 1321
_refine_ls_number_restraints 84
_refine_ls_R_factor_all 0.0921
_refine_ls_R_factor_gt 0.0699
_refine_ls_restrained_S_all 1.148
_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^)+(0.0965P)^2^+12.5000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1933
_refine_ls_wR_factor_ref 0.2161
_refine_special_details
;
Location of maximum Q peak
Atom Peak x y z
Q1 2.26 0.1048 0.0000 0.0000
Distances to nearest atoms (including eq.)
0.67 Au1 2.53 Au2 2.86 H6A 3.07 H7A
;
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups
At 1.5 times of:
All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
3. Others
Fixed Sof: H6A(0.5) H6B(0.5) H6C(0.5) H7A(0.5) H7B(0.5) H7C(0.5)
4.a Aromatic/amide H refined with riding coordinates:
C4(H4), C5(H5)
4.b Idealised Me refined as rotating group:
C6(H6A,H6B,H6C), C7(H7A,H7B,H7C)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary dual
_atom_sites_solution_secondary ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Au1 Au 0.000000 0.000000 0.000000 0.0393(5) Uani 1 4 d S TU P . .
Au2 Au 0.500000 0.000000 0.000000 0.0481(5) Uani 1 4 d S TU P . .
N1 N 0.000000 0.0060(16) 0.1637(7) 0.040(3) Uani 1 2 d S TU P . .
N2 N 0.000000 0.2479(17) 0.1190(6) 0.037(2) Uani 1 2 d S TU P . .
N3 N 0.000000 0.069(2) 0.2892(7) 0.044(3) Uani 1 2 d S TU P . .
N4 N 0.000000 0.398(2) 0.2301(8) 0.052(3) Uani 1 2 d S TU P . .
N5 N 0.500000 -0.342(3) 0.0742(11) 0.094(6) Uani 1 2 d S TU P . .
C1 C 0.000000 0.0876(19) 0.1012(7) 0.031(3) Uani 1 2 d S TU P . .
C2 C 0.000000 0.112(2) 0.2202(8) 0.038(3) Uani 1 2 d S TU P . .
C3 C 0.000000 0.265(2) 0.1922(8) 0.039(3) Uani 1 2 d S TU P . .
C4 C 0.000000 0.201(3) 0.3285(10) 0.052(3) Uani 1 2 d S TU P . .
H4 H 0.000000 0.186600 0.377859 0.063 Uiso 1 2 calc RS T P . .
C5 C 0.000000 0.365(2) 0.3024(9) 0.053(3) Uani 1 2 d S TU P . .
H5 H 0.000000 0.450847 0.334911 0.063 Uiso 1 2 calc RS T P . .
C6 C 0.000000 0.379(2) 0.0683(9) 0.055(4) Uani 1 2 d S TU P . .
H6A H 0.066050 0.343908 0.024828 0.083 Uiso 0.5 1 calc GR . . A -1
H6B H 0.075425 0.470725 0.087674 0.083 Uiso 0.5 1 calc GR . . A -1
H6C H -0.141475 0.411519 0.058333 0.083 Uiso 0.5 1 calc GR . . A -1
C7 C 0.000000 -0.171(2) 0.1685(10) 0.050(4) Uani 1 2 d S TU P . .
H7A H 0.098086 -0.215057 0.134715 0.076 Uiso 0.5 1 calc GR . . B -1
H7B H -0.137461 -0.211773 0.157999 0.076 Uiso 0.5 1 calc GR . . B -1
H7C H 0.039375 -0.203590 0.216000 0.076 Uiso 0.5 1 calc GR . . B -1
C8 C 0.500000 -0.215(3) 0.0462(10) 0.059(4) Uani 1 2 d S TU P . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Au1 0.0391(6) 0.0479(7) 0.0308(6) -0.0004(4) 0.000 0.000
Au2 0.0450(7) 0.0556(7) 0.0437(7) 0.0059(4) 0.000 0.000
N1 0.033(5) 0.052(6) 0.034(5) 0.002(5) 0.000 0.000
N2 0.028(4) 0.052(5) 0.031(5) -0.002(5) 0.000 0.000
N3 0.023(5) 0.074(7) 0.035(5) 0.006(5) 0.000 0.000
N4 0.039(6) 0.070(7) 0.047(5) -0.016(6) 0.000 0.000
N5 0.096(12) 0.091(12) 0.095(12) 0.027(11) 0.000 0.000
C1 0.019(5) 0.045(6) 0.027(5) 0.002(5) 0.000 0.000
C2 0.025(5) 0.056(6) 0.032(5) 0.008(5) 0.000 0.000
C3 0.030(5) 0.055(6) 0.033(5) -0.001(5) 0.000 0.000
C4 0.032(5) 0.081(8) 0.043(6) -0.009(6) 0.000 0.000
C5 0.033(6) 0.079(8) 0.047(6) -0.026(6) 0.000 0.000
C6 0.072(11) 0.061(10) 0.033(7) 0.002(8) 0.000 0.000
C7 0.052(9) 0.042(9) 0.057(9) 0.001(8) 0.000 0.000
C8 0.057(7) 0.066(8) 0.055(7) 0.019(7) 0.000 0.000
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Au1 Au2 3.1964(2) 1_455 ?
Au1 Au2 3.1964(2) . ?
Au1 C1 2.022(13) 5 ?
Au1 C1 2.022(13) . ?
Au2 C8 1.959(19) . ?
Au2 C8 1.959(19) 5_655 ?
N1 C1 1.346(18) . ?
N1 C2 1.366(19) . ?
N1 C7 1.45(2) . ?
N2 C1 1.352(19) . ?
N2 C3 1.376(18) . ?
N2 C6 1.43(2) . ?
N3 C2 1.34(2) . ?
N3 C4 1.31(2) . ?
N4 C3 1.30(2) . ?
N4 C5 1.38(2) . ?
N5 C8 1.16(3) . ?
C2 C3 1.36(2) . ?
C4 H4 0.9300 . ?
C4 C5 1.43(3) . ?
C5 H5 0.9300 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Au2 Au1 Au2 180.0 . 1_455 ?
C1 Au1 Au2 90.0 5 1_455 ?
C1 Au1 Au2 90.0 . . ?
C1 Au1 Au2 90.0 . 1_455 ?
C1 Au1 Au2 90.0 5 . ?
C1 Au1 C1 180.0 . 5 ?
Au1 Au2 Au1 180.0 . 1_655 ?
C8 Au2 Au1 90.0 . . ?
C8 Au2 Au1 90.0 . 1_655 ?
C8 Au2 Au1 90.0 5_655 . ?
C8 Au2 Au1 90.0 5_655 1_655 ?
C8 Au2 C8 180.0 . 5_655 ?
C1 N1 C2 110.8(12) . . ?
C1 N1 C7 123.2(14) . . ?
C2 N1 C7 125.9(13) . . ?
C1 N2 C3 110.2(13) . . ?
C1 N2 C6 124.3(13) . . ?
C3 N2 C6 125.5(15) . . ?
C4 N3 C2 108.8(16) . . ?
C3 N4 C5 111.6(16) . . ?
N1 C1 Au1 129.6(11) . . ?
N1 C1 N2 105.4(12) . . ?
N2 C1 Au1 125.0(10) . . ?
N3 C2 N1 125.1(14) . . ?
N3 C2 C3 128.1(16) . . ?
C3 C2 N1 106.8(13) . . ?
N4 C3 N2 129.1(16) . . ?
N4 C3 C2 124.3(15) . . ?
C2 C3 N2 106.7(14) . . ?
N3 C4 H4 117.1 . . ?
N3 C4 C5 125.8(16) . . ?
C5 C4 H4 117.1 . . ?
N4 C5 C4 121.5(16) . . ?
N4 C5 H5 119.2 . . ?
C4 C5 H5 119.2 . . ?
N2 C6 H6A 109.5 . . ?
N2 C6 H6B 109.5 . . ?
N2 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N1 C7 H7A 109.5 . . ?
N1 C7 H7B 109.5 . . ?
N1 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N5 C8 Au2 179(2) . . ?
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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C2 C3 N2 0.000(2) . . . . ?
N1 C2 C3 N4 180.000(3) . . . . ?
N3 C2 C3 N2 180.000(2) . . . . ?
N3 C2 C3 N4 0.000(4) . . . . ?
N3 C4 C5 N4 0.000(6) . . . . ?
C1 N1 C2 N3 180.000(2) . . . . ?
C1 N1 C2 C3 0.000(2) . . . . ?
C1 N2 C3 N4 180.000(3) . . . . ?
C1 N2 C3 C2 0.000(3) . . . . ?
C2 N1 C1 Au1 180.000(2) . . . . ?
C2 N1 C1 N2 0.000(2) . . . . ?
C2 N3 C4 C5 0.000(5) . . . . ?
C3 N2 C1 Au1 180.000(2) . . . . ?
C3 N2 C1 N1 0.000(2) . . . . ?
C3 N4 C5 C4 0.000(5) . . . . ?
C4 N3 C2 N1 180.000(3) . . . . ?
C4 N3 C2 C3 0.000(4) . . . . ?
C5 N4 C3 N2 180.000(3) . . . . ?
C5 N4 C3 C2 0.000(4) . . . . ?
C6 N2 C1 Au1 0.000(2) . . . . ?
C6 N2 C1 N1 180.000(2) . . . . ?
C6 N2 C3 N4 0.000(4) . . . . ?
C6 N2 C3 C2 180.000(2) . . . . ?
C7 N1 C1 Au1 0.000(2) . . . . ?
C7 N1 C1 N2 180.000(1) . . . . ?
C7 N1 C2 N3 0.000(3) . . . . ?
C7 N1 C2 C3 180.000(3) . . . . ?
_iucr_refine_instructions_details
;
TITL cxy0495_298K
cxy0495_pmna.res
created by SHELXL-2016/6 at 10:59:12 on 27-Sep-2018
CELL 0.71073 6.3929 8.1734 18.6898 90 90 90
ZERR 2 0.0004 0.0006 0.0012 0 0 0
LATT 1
SYMM 0.5-X,-Y,0.5+Z
SYMM +X,-Y,-Z
SYMM 0.5-X,+Y,0.5-Z
SFAC C H Au N
UNIT 32 32 4 20
SIMU 0.01 0.02 2
L.S. 5
PLAN -20
TEMP 23
BOND $H
CONF
fmap 2
acta
OMIT 0 1 0
REM
REM
REM
WGHT 0.096500 12.500000
EXTI 0.011338
FVAR 0.33456
AU1 3 0.000000 0.000000 0.000000 10.25000 0.03908 0.04794 =
0.03083 -0.00036 0.00000 0.00000
AU2 3 0.500000 0.000000 0.000000 10.25000 0.04499 0.05557 =
0.04375 0.00594 0.00000 0.00000
N1 4 0.000000 0.005951 0.163741 10.50000 0.03327 0.05214 =
0.03427 0.00191 0.00000 0.00000
N2 4 0.000000 0.247907 0.119005 10.50000 0.02758 0.05226 =
0.03115 -0.00210 0.00000 0.00000
N3 4 0.000000 0.068518 0.289183 10.50000 0.02337 0.07402 =
0.03479 0.00596 0.00000 0.00000
N4 4 0.000000 0.398379 0.230138 10.50000 0.03930 0.07023 =
0.04651 -0.01631 0.00000 0.00000
N5 4 0.500000 -0.341641 0.074232 10.50000 0.09603 0.09114 =
0.09477 0.02701 0.00000 0.00000
C1 1 0.000000 0.087583 0.101179 10.50000 0.01937 0.04492 =
0.02724 0.00201 0.00000 0.00000
C2 1 0.000000 0.112113 0.220170 10.50000 0.02478 0.05635 =
0.03152 0.00776 0.00000 0.00000
C3 1 0.000000 0.265375 0.192213 10.50000 0.03001 0.05468 =
0.03265 -0.00126 0.00000 0.00000
C4 1 0.000000 0.200697 0.328483 10.50000 0.03246 0.08111 =
0.04323 -0.00898 0.00000 0.00000
AFIX 43
H4 2 0.000000 0.186600 0.377859 10.50000 -1.20000
AFIX 0
C5 1 0.000000 0.364680 0.302414 10.50000 0.03269 0.07900 =
0.04670 -0.02574 0.00000 0.00000
AFIX 43
H5 2 0.000000 0.450847 0.334911 10.50000 -1.20000
AFIX 0
C6 1 0.000000 0.379362 0.068274 10.50000 0.07206 0.06125 =
0.03305 0.00171 0.00000 0.00000
PART -1
AFIX 137
H6A 2 0.066050 0.343908 0.024828 10.50000 -1.50000
H6B 2 0.075425 0.470725 0.087674 10.50000 -1.50000
H6C 2 -0.141475 0.411519 0.058333 10.50000 -1.50000
AFIX 0
PART 0
C7 1 0.000000 -0.171063 0.168517 10.50000 0.05214 0.04170 =
0.05722 0.00142 0.00000 0.00000
PART -1
AFIX 137
H7A 2 0.098086 -0.215057 0.134715 10.50000 -1.50000
H7B 2 -0.137461 -0.211773 0.157999 10.50000 -1.50000
H7C 2 0.039375 -0.203590 0.216000 10.50000 -1.50000
AFIX 0
PART 0
C8 1 0.500000 -0.215083 0.046240 10.50000 0.05685 0.06557 =
0.05543 0.01872 0.00000 0.00000
HKLF 4
REM cxy0495_298K
REM R1 = 0.0699 for 905 Fo > 4sig(Fo) and 0.0921 for all 1321 data
REM 90 parameters refined using 84 restraints
END
WGHT 0.0768 9.2111
REM Highest difference peak 2.263, deepest hole -1.331, 1-sigma level 0.416
Q1 1 0.1048 0.0000 0.0000 10.50000 0.05 2.26
Q2 1 0.5000 -0.0184 -0.0396 10.50000 0.05 1.85
Q3 1 0.0000 -0.0430 0.0374 10.50000 0.05 1.83
Q4 1 0.4075 0.0000 0.0000 10.50000 0.05 1.63
Q5 1 0.0000 0.0335 0.0283 10.50000 0.05 1.55
Q6 1 0.0000 0.2884 0.3232 10.50000 0.05 1.12
Q7 1 0.5000 0.0796 -0.0077 10.50000 0.05 1.09
Q8 1 0.0000 -0.2691 0.3204 10.50000 0.05 1.08
Q9 1 0.0000 0.1608 0.2959 10.50000 0.05 1.08
Q10 1 0.1943 0.5000 0.5000 10.50000 0.05 1.04
Q11 1 0.0000 -0.1829 0.2040 10.50000 0.05 0.85
Q12 1 0.0000 -0.2377 0.1549 10.50000 0.05 0.83
Q13 1 0.0000 0.2660 0.1634 10.50000 0.05 0.83
Q14 1 0.0000 -0.1424 0.2581 10.50000 0.05 0.78
Q15 1 0.0000 -0.1907 0.2511 10.50000 0.05 0.78
Q16 1 0.0373 -0.1498 0.2948 11.00000 0.05 0.77
Q17 1 0.1942 -0.2276 0.2209 11.00000 0.05 0.76
Q18 1 0.2285 0.0005 0.0855 11.00000 0.05 0.74
Q19 1 0.1939 -0.3023 0.1560 11.00000 0.05 0.74
Q20 1 0.1941 0.2275 0.2191 11.00000 0.05 0.74
REM The information below was added by Olex2.
REM
REM R1 = 0.0699 for 905 Fo > 4sig(Fo) and 0.0921 for all 19771 data
REM n/a parameters refined using n/a restraints
REM Highest difference peak 2.26, deepest hole -1.33
REM Mean Shift 0, Max Shift 0.001.
REM +++ Tabular Listing of Refinement Information +++
REM R1_all = 0.0921
REM R1_gt = 0.0699
REM wR_ref = 0.2161
REM GOOF = 1.165
REM Shift_max = 0.001
REM Shift_mean = 0
REM Reflections_all = 19771
REM Reflections_gt = 905
REM Parameters = n/a
REM Hole = -1.33
REM Peak = 2.26
REM Flack = n/a
;
_olex2_submission_special_instructions 'No special instructions were received'
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_cxy0495_pmna_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 1871226'
_audit_update_record
;
2018-10-10 deposited with the CCDC.
2018-10-12 downloaded from the CCDC.
;
_audit_creation_date 2018-09-27
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number 2016/6
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C16 H16 Au2 N10'
_chemical_formula_sum 'C16 H16 Au2 N10'
_chemical_formula_weight 742.32
_chemical_melting_point ?
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_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.
;
_space_group_crystal_system orthorhombic
_space_group_IT_number 53
_space_group_name_H-M_alt 'P m n a'
_space_group_name_Hall '-P 2ac 2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x, -y, -z'
'-x+1/2, y, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x, y, z'
'x-1/2, -y, z-1/2'
_cell_length_a 6.3632(4)
_cell_length_b 8.1603(6)
_cell_length_c 18.6843(12)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_volume 970.19(11)
_cell_formula_units_Z 2
_cell_measurement_reflns_used 6156
_cell_measurement_temperature 250
_cell_measurement_theta_max 28.293
_cell_measurement_theta_min 2.724
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 15.129
_exptl_absorpt_correction_T_max 0.7457
_exptl_absorpt_correction_T_min 0.3891
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1594 before and 0.0909 after correction. The Ratio of minimum to maximum transmission is 0.5218. The \l/2 correction factor is Not present.'
_exptl_absorpt_special_details ?
_exptl_crystal_colour yellow
_exptl_crystal_colour_primary yellow
_exptl_crystal_density_diffrn 2.541
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description plate
_exptl_crystal_F_000 680
_exptl_crystal_size_max 0.3
_exptl_crystal_size_mid 0.06
_exptl_crystal_size_min 0.01
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0611
_diffrn_reflns_av_unetI/netI 0.0280
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max 8
_diffrn_reflns_limit_h_min -8
_diffrn_reflns_limit_k_max 10
_diffrn_reflns_limit_k_min -10
_diffrn_reflns_limit_l_max 24
_diffrn_reflns_limit_l_min -24
_diffrn_reflns_number 18401
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 28.311
_diffrn_reflns_theta_min 2.180
_diffrn_ambient_temperature 250
_diffrn_detector 'Bruker PHOTO 100 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type 'CCD area detector'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device 'three-circle diffractometer'
_diffrn_measurement_device_type 'Bruker PHOTO 100 area detector'
_diffrn_measurement_method '\w and \f scans'
_diffrn_radiation_monochromator 'mirror optics'
_diffrn_radiation_probe x-ray
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'microfocus sealed X-ray tube'
_diffrn_source_type 'Incoatec I\ms'
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 957
_reflns_number_total 1312
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'SAINT V8.38A (?, 2016)'
_computing_data_collection ?
_computing_data_reduction 'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'XL (Sheldrick, 2008)'
_computing_structure_solution 'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max 2.064
_refine_diff_density_min -1.585
_refine_diff_density_rms 0.406
_refine_ls_extinction_coef 0.0148(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method 'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref 1.276
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 90
_refine_ls_number_reflns 1312
_refine_ls_number_restraints 84
_refine_ls_R_factor_all 0.0886
_refine_ls_R_factor_gt 0.0718
_refine_ls_restrained_S_all 1.251
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0746P)^2^+17.9723P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1881
_refine_ls_wR_factor_ref 0.2015
_refine_special_details
;
Location of maximum Q peak
Atom Peak x y z
Q1 2.06 0.0000 -0.0423 0.0414
Distances to nearest atoms (including eq.)
0.85 Au1 1.51 C1 2.36 H7A 2.75 H7B
;
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups
At 1.5 times of:
All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
3. Others
Fixed Sof: H6A(0.5) H6B(0.5) H6C(0.5) H7A(0.5) H7B(0.5) H7C(0.5)
4.a Aromatic/amide H refined with riding coordinates:
C4(H4), C5(H5)
4.b Idealised Me refined as rotating group:
C6(H6A,H6B,H6C), C7(H7A,H7B,H7C)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary dual
_atom_sites_solution_secondary ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Au1 Au 0.000000 0.000000 0.000000 0.0339(5) Uani 1 4 d S TU P . .
Au2 Au 0.500000 0.000000 0.000000 0.0416(5) Uani 1 4 d S TU P . .
N1 N 0.000000 -0.0001(18) 0.1643(8) 0.035(3) Uani 1 2 d S TU P . .
N2 N 0.000000 0.2483(19) 0.1196(7) 0.032(2) Uani 1 2 d S TU P . .
N3 N 0.000000 0.067(2) 0.2897(8) 0.040(3) Uani 1 2 d S TU P . .
N4 N 0.000000 0.397(2) 0.2312(9) 0.048(3) Uani 1 2 d S TU P . .
N5 N 0.500000 -0.342(3) 0.0735(12) 0.078(6) Uani 1 2 d S TU P . .
C1 C 0.000000 0.083(2) 0.1011(7) 0.028(3) Uani 1 2 d S TU P . .
C2 C 0.000000 0.111(2) 0.2202(9) 0.037(3) Uani 1 2 d S TU P . .
C3 C 0.000000 0.264(2) 0.1924(8) 0.035(3) Uani 1 2 d S TU P . .
C4 C 0.000000 0.202(3) 0.3288(10) 0.045(3) Uani 1 2 d S TU P . .
H4 H 0.000000 0.189062 0.378728 0.054 Uiso 1 2 calc RS T P . .
C5 C 0.000000 0.366(3) 0.3024(10) 0.046(3) Uani 1 2 d S TU P . .
H5 H 0.000000 0.454021 0.334910 0.055 Uiso 1 2 calc RS T P . .
C6 C 0.000000 0.377(3) 0.0677(10) 0.050(5) Uani 1 2 d S TU P . .
H6A H 0.066929 0.339088 0.024146 0.074 Uiso 0.5 1 calc GR . . A -1
H6B H 0.076682 0.470521 0.086444 0.074 Uiso 0.5 1 calc GR . . A -1
H6C H -0.143611 0.409268 0.057410 0.074 Uiso 0.5 1 calc GR . . A -1
C7 C 0.000000 -0.1771(19) 0.1688(11) 0.039(4) Uani 1 2 d S TU P . .
H7A H 0.100374 -0.221291 0.134847 0.058 Uiso 0.5 1 calc GR . . B -1
H7B H -0.139269 -0.218236 0.157752 0.058 Uiso 0.5 1 calc GR . . B -1
H7C H 0.038895 -0.210354 0.216859 0.058 Uiso 0.5 1 calc GR . . B -1
C8 C 0.500000 -0.216(3) 0.0450(11) 0.053(4) Uani 1 2 d S TU P . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Au1 0.0328(6) 0.0422(7) 0.0267(6) -0.0022(4) 0.000 0.000
Au2 0.0377(7) 0.0480(8) 0.0389(7) 0.0089(4) 0.000 0.000
N1 0.028(5) 0.046(6) 0.031(5) 0.002(5) 0.000 0.000
N2 0.022(5) 0.046(6) 0.028(5) 0.001(5) 0.000 0.000
N3 0.019(5) 0.068(7) 0.034(6) 0.002(6) 0.000 0.000
N4 0.031(6) 0.068(7) 0.044(6) -0.015(6) 0.000 0.000
N5 0.079(12) 0.072(12) 0.083(12) 0.024(11) 0.000 0.000
C1 0.019(5) 0.042(6) 0.024(5) 0.006(5) 0.000 0.000
C2 0.023(5) 0.053(6) 0.034(5) 0.004(5) 0.000 0.000
C3 0.024(5) 0.050(6) 0.031(5) -0.002(5) 0.000 0.000
C4 0.026(6) 0.069(8) 0.039(6) -0.007(6) 0.000 0.000
C5 0.026(6) 0.070(8) 0.042(6) -0.022(7) 0.000 0.000
C6 0.058(11) 0.057(11) 0.034(8) 0.003(8) 0.000 0.000
C7 0.040(9) 0.016(7) 0.060(10) 0.010(7) 0.000 0.000
C8 0.047(7) 0.058(8) 0.054(7) 0.014(7) 0.000 0.000
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Au1 Au2 3.1816(2) 1_455 ?
Au1 Au2 3.1816(2) . ?
Au1 C1 2.006(15) . ?
Au1 C1 2.006(15) 5 ?
Au2 C8 1.95(2) 5_655 ?
Au2 C8 1.95(2) . ?
N1 C1 1.36(2) . ?
N1 C2 1.38(2) . ?
N1 C7 1.45(2) . ?
N2 C1 1.39(2) . ?
N2 C3 1.37(2) . ?
N2 C6 1.43(2) . ?
N3 C2 1.35(2) . ?
N3 C4 1.32(3) . ?
N4 C3 1.30(2) . ?
N4 C5 1.35(2) . ?
N5 C8 1.16(3) . ?
C2 C3 1.35(3) . ?
C4 H4 0.9400 . ?
C4 C5 1.42(3) . ?
C5 H5 0.9400 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 H6C 0.9700 . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 H7C 0.9700 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Au2 Au1 Au2 180.0 . 1_455 ?
C1 Au1 Au2 90.0 . 1_455 ?
C1 Au1 Au2 90.0 5 . ?
C1 Au1 Au2 90.0 5 1_455 ?
C1 Au1 Au2 90.0 . . ?
C1 Au1 C1 180.0 5 . ?
Au1 Au2 Au1 180.0 . 1_655 ?
C8 Au2 Au1 90.0 5_655 . ?
C8 Au2 Au1 90.0 . 1_655 ?
C8 Au2 Au1 90.0 . . ?
C8 Au2 Au1 90.0 5_655 1_655 ?
C8 Au2 C8 180.0 5_655 . ?
C1 N1 C2 109.2(14) . . ?
C1 N1 C7 123.1(15) . . ?
C2 N1 C7 127.7(15) . . ?
C1 N2 C6 123.0(14) . . ?
C3 N2 C1 109.9(14) . . ?
C3 N2 C6 127.2(17) . . ?
C4 N3 C2 108.2(17) . . ?
C3 N4 C5 113.2(18) . . ?
N1 C1 Au1 130.5(13) . . ?
N1 C1 N2 105.5(13) . . ?
N2 C1 Au1 124.0(11) . . ?
N3 C2 N1 123.6(17) . . ?
N3 C2 C3 127.9(18) . . ?
C3 C2 N1 108.4(15) . . ?
N4 C3 N2 129.4(18) . . ?
N4 C3 C2 123.6(17) . . ?
C2 C3 N2 107.1(16) . . ?
N3 C4 H4 116.9 . . ?
N3 C4 C5 126.3(18) . . ?
C5 C4 H4 116.9 . . ?
N4 C5 C4 120.9(18) . . ?
N4 C5 H5 119.6 . . ?
C4 C5 H5 119.6 . . ?
N2 C6 H6A 109.5 . . ?
N2 C6 H6B 109.5 . . ?
N2 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N1 C7 H7A 109.5 . . ?
N1 C7 H7B 109.5 . . ?
N1 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N5 C8 Au2 178(2) . . ?
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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C2 C3 N2 0.000(3) . . . . ?
N1 C2 C3 N4 180.000(4) . . . . ?
N3 C2 C3 N2 180.000(3) . . . . ?
N3 C2 C3 N4 0.000(5) . . . . ?
N3 C4 C5 N4 0.000(6) . . . . ?
C1 N1 C2 N3 180.000(3) . . . . ?
C1 N1 C2 C3 0.000(3) . . . . ?
C1 N2 C3 N4 180.000(4) . . . . ?
C1 N2 C3 C2 0.000(3) . . . . ?
C2 N1 C1 Au1 180.000(2) . . . . ?
C2 N1 C1 N2 0.000(2) . . . . ?
C2 N3 C4 C5 0.000(5) . . . . ?
C3 N2 C1 Au1 180.000(2) . . . . ?
C3 N2 C1 N1 0.000(2) . . . . ?
C3 N4 C5 C4 0.000(6) . . . . ?
C4 N3 C2 N1 180.000(4) . . . . ?
C4 N3 C2 C3 0.000(4) . . . . ?
C5 N4 C3 N2 180.000(4) . . . . ?
C5 N4 C3 C2 0.000(4) . . . . ?
C6 N2 C1 Au1 0.000(2) . . . . ?
C6 N2 C1 N1 180.000(2) . . . . ?
C6 N2 C3 N4 0.000(4) . . . . ?
C6 N2 C3 C2 180.000(3) . . . . ?
C7 N1 C1 Au1 0.000(2) . . . . ?
C7 N1 C1 N2 180.000(1) . . . . ?
C7 N1 C2 N3 0.000(3) . . . . ?
C7 N1 C2 C3 180.000(3) . . . . ?
_iucr_refine_instructions_details
;
TITL cxy0495_298K
cxy0495_pmna.res
created by SHELXL-2016/6 at 11:06:50 on 27-Sep-2018
CELL 0.71073 6.3632 8.1603 18.6843 90 90 90
ZERR 2 0.0004 0.0006 0.0012 0 0 0
LATT 1
SYMM 0.5-X,-Y,0.5+Z
SYMM +X,-Y,-Z
SYMM 0.5-X,+Y,0.5-Z
SFAC C H Au N
UNIT 32 32 4 20
SIMU 0.01 0.02 2
L.S. 20
PLAN -20
TEMP -23.15
BOND $H
CONF
fmap 2
acta
OMIT 0 1 0
REM
REM
REM
WGHT 0.074600 17.972300
EXTI 0.014787
FVAR 0.35879
AU1 3 0.000000 0.000000 0.000000 10.25000 0.03284 0.04223 =
0.02673 -0.00220 0.00000 0.00000
AU2 3 0.500000 0.000000 0.000000 10.25000 0.03769 0.04804 =
0.03892 0.00895 0.00000 0.00000
N1 4 0.000000 -0.000089 0.164311 10.50000 0.02804 0.04550 =
0.03085 0.00250 0.00000 0.00000
N2 4 0.000000 0.248276 0.119590 10.50000 0.02227 0.04605 =
0.02761 0.00063 0.00000 0.00000
N3 4 0.000000 0.067416 0.289709 10.50000 0.01934 0.06778 =
0.03393 0.00231 0.00000 0.00000
N4 4 0.000000 0.396797 0.231180 10.50000 0.03143 0.06779 =
0.04356 -0.01534 0.00000 0.00000
N5 4 0.500000 -0.341600 0.073529 10.50000 0.07910 0.07249 =
0.08332 0.02444 0.00000 0.00000
C1 1 0.000000 0.082848 0.101102 10.50000 0.01906 0.04153 =
0.02369 0.00606 0.00000 0.00000
C2 1 0.000000 0.111135 0.220192 10.50000 0.02347 0.05343 =
0.03364 0.00398 0.00000 0.00000
C3 1 0.000000 0.264310 0.192361 10.50000 0.02404 0.04981 =
0.03073 -0.00175 0.00000 0.00000
C4 1 0.000000 0.202396 0.328757 10.50000 0.02585 0.06861 =
0.03931 -0.00735 0.00000 0.00000
AFIX 43
H4 2 0.000000 0.189062 0.378728 10.50000 -1.20000
AFIX 0
C5 1 0.000000 0.366067 0.302422 10.50000 0.02588 0.06961 =
0.04224 -0.02189 0.00000 0.00000
AFIX 43
H5 2 0.000000 0.454021 0.334910 10.50000 -1.20000
AFIX 0
C6 1 0.000000 0.377153 0.067726 10.50000 0.05752 0.05663 =
0.03446 0.00254 0.00000 0.00000
PART -1
AFIX 137
H6A 2 0.066929 0.339088 0.024146 10.50000 -1.50000
H6B 2 0.076682 0.470521 0.086444 10.50000 -1.50000
H6C 2 -0.143611 0.409268 0.057410 10.50000 -1.50000
AFIX 0
PART 0
C7 1 0.000000 -0.177071 0.168813 10.50000 0.04046 0.01625 =
0.05967 0.01021 0.00000 0.00000
PART -1
AFIX 137
H7A 2 0.100374 -0.221291 0.134847 10.50000 -1.50000
H7B 2 -0.139269 -0.218236 0.157752 10.50000 -1.50000
H7C 2 0.038895 -0.210354 0.216859 10.50000 -1.50000
AFIX 0
PART 0
C8 1 0.500000 -0.215742 0.044999 10.50000 0.04672 0.05762 =
0.05435 0.01393 0.00000 0.00000
HKLF 4
REM cxy0495_298K
REM R1 = 0.0718 for 957 Fo > 4sig(Fo) and 0.0886 for all 1312 data
REM 90 parameters refined using 84 restraints
END
WGHT 0.0746 17.9888
REM Highest difference peak 2.064, deepest hole -1.585, 1-sigma level 0.406
Q1 1 0.0000 -0.0423 0.0414 10.50000 0.05 2.06
Q2 1 0.5000 -0.0348 -0.0396 10.50000 0.05 1.80
Q3 1 0.5000 0.0786 -0.0093 10.50000 0.05 1.68
Q4 1 0.1006 0.0000 0.0000 10.50000 0.05 1.58
Q5 1 0.5000 -0.2594 0.1705 10.50000 0.05 1.45
Q6 1 0.0000 0.0739 0.0097 10.50000 0.05 1.40
Q7 1 0.3064 0.5000 0.0000 10.50000 0.05 1.16
Q8 1 0.1951 0.5000 0.0000 10.50000 0.05 1.14
Q9 1 0.4167 -0.0089 -0.0160 11.00000 0.05 1.09
Q10 1 0.0000 0.4464 0.2795 10.50000 0.05 1.07
Q11 1 0.0000 0.2601 0.1701 10.50000 0.05 1.06
Q12 1 0.0000 0.1565 0.2957 10.50000 0.05 0.99
Q13 1 0.0000 0.4649 0.2063 10.50000 0.05 0.97
Q14 1 0.0000 0.0207 0.1290 10.50000 0.05 0.92
Q15 1 0.2701 0.1430 -0.0728 11.00000 0.05 0.91
Q16 1 0.0000 -0.3606 0.1832 10.50000 0.05 0.87
Q17 1 0.5000 -0.2247 0.1270 10.50000 0.05 0.86
Q18 1 0.0000 -0.1360 0.2570 10.50000 0.05 0.86
Q19 1 0.0000 -0.1016 0.1604 10.50000 0.05 0.83
Q20 1 0.0000 0.5394 0.2181 10.50000 0.05 0.83
REM The information below was added by Olex2.
REM
REM R1 = 0.0718 for 957 Fo > 4sig(Fo) and 0.0886 for all 19592 data
REM n/a parameters refined using n/a restraints
REM Highest difference peak 2.06, deepest hole -1.59
REM Mean Shift 0, Max Shift 0.000.
REM +++ Tabular Listing of Refinement Information +++
REM R1_all = 0.0886
REM R1_gt = 0.0718
REM wR_ref = 0.2015
REM GOOF = 1.276
REM Shift_max = 0.000
REM Shift_mean = 0
REM Reflections_all = 19592
REM Reflections_gt = 957
REM Parameters = n/a
REM Hole = -1.59
REM Peak = 2.06
REM Flack = n/a
;
_olex2_submission_special_instructions 'No special instructions were received'