#------------------------------------------------------------------------------
#$Date: 2016-03-26 13:02:54 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180220 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/06/7110601.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_7110601
loop_
_publ_author_name
'Jones, Peter G.'
'Friedrichs, Steffi'
_publ_section_title
;
 Deprotonated ethylenethiourea as a ligand in an unusual tetrameric
 gold(I) complex†
;
_journal_issue                   15
_journal_name_full               'Chemical Communications'
_journal_page_first              1365
_journal_paper_doi               10.1039/a904137k
_journal_year                    1999
_chemical_formula_sum            'C12 H20 Au4 N8 S4'
_chemical_formula_weight         1192.47
_chemical_name_systematic
;

 ?

;
_space_group_IT_number           45
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'I 2 -2c'
_symmetry_space_group_name_H-M   'I b a 2'
_atom_sites_solution_hydrogens   riding
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.1973(9)
_cell_length_b                   10.3143(6)
_cell_length_c                   13.2818(7)
_cell_measurement_reflns_used    4174
_cell_measurement_temperature    143(2)
_cell_measurement_theta_max      28
_cell_measurement_theta_min      2
_cell_volume                     2218.9(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Siemens XP'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      143(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD'
_diffrn_measurement_method       ω-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0555
_diffrn_reflns_av_sigmaI/netI    0.0437
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11368
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.34
_exptl_absorpt_coefficient_mu    26.758
_exptl_absorpt_correction_T_max  0.962
_exptl_absorpt_correction_T_min  0.453
_exptl_absorpt_correction_type   'multiple scans (SADABS)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.570
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2112
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         2.260
_refine_diff_density_min         -2.200
_refine_diff_density_rms         0.282
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.46(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     119
_refine_ls_number_reflns         2759
_refine_ls_number_restraints     154
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0463
_refine_ls_R_factor_gt           0.0323
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0402P)²+10.6284P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0753
_refine_ls_wR_factor_ref         0.0807
_reflns_number_gt                2208
_reflns_number_total             2759
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            904137ksup1.cif
_cod_data_source_block           nichda
_cod_database_code               7110601
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'x+1, -y+1, z+1/2'
'-x+1, y+1, z+1/2'
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Au1 Au 0.38047(2) 0.64015(3) 0.31366(16) 0.02618(11) Uani 1 1 d .
S1 S 0.2862(2) 0.4787(3) 0.3388(2) 0.0372(9) Uiso 1 1 d D
C11 C 0.3339(8) 0.3654(12) 0.2121(9) 0.031(3) Uani 1 1 d DU
N11 N 0.2911(8) 0.2555(12) 0.1834(10) 0.044(3) Uani 1 1 d DU
H11 H 0.2379 0.2448 0.1940 0.052 Uiso 1 1 calc R
C12 C 0.3342(14) 0.175(2) 0.1423(16) 0.049(5) Uani 1 1 d DU
H12A H 0.3063 0.1413 0.0814 0.059 Uiso 1 1 calc R
H12B H 0.3451 0.1017 0.1884 0.059 Uiso 1 1 calc R
C13 C 0.4192(10) 0.2452(14) 0.1122(14) 0.047(4) Uani 1 1 d DU
H13A H 0.4680 0.1915 0.1284 0.057 Uiso 1 1 calc R
H13B H 0.4206 0.2707 0.0404 0.057 Uiso 1 1 calc R
N12 N 0.4111(7) 0.3603(12) 0.1811(9) 0.029(3) Uani 1 1 d DU
Au2 Au 0.5000 0.5000 0.18340(4) 0.0200(3) Uani 1 2 d S
S2 S 0.4555(2) 0.8272(3) 0.2886(3) 0.0378(9) Uiso 1 1 d D
C21 C 0.5399(9) 0.7819(12) 0.4088(10) 0.034(3) Uani 1 1 d DU
N21 N 0.5958(8) 0.8776(11) 0.4330(10) 0.042(3) Uani 1 1 d DU
H21 H 0.5907 0.9589 0.4141 0.050 Uiso 1 1 calc R
C22 C 0.6525(14) 0.8379(17) 0.4828(15) 0.041(4) Uani 1 1 d DU
H22A H 0.6572 0.8886 0.5458 0.049 Uiso 1 1 calc R
H22B H 0.7048 0.8466 0.4450 0.049 Uiso 1 1 calc R
C23 C 0.6355(9) 0.6895(13) 0.5082(11) 0.034(3) Uani 1 1 d DU
H23A H 0.6819 0.6333 0.4871 0.040 Uiso 1 1 calc R
H23B H 0.6242 0.6762 0.5807 0.040 Uiso 1 1 calc R
N22 N 0.5597(8) 0.6668(11) 0.4449(10) 0.034(3) Uani 1 1 d DU
Au3 Au 0.5000 0.5000 0.44426(3) 0.0202(3) Uani 1 2 d S
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
S1 Au1 S2 169.78(13) . .
S1 Au1 Au2 99.57(9) . .
S2 Au1 Au2 88.84(9) . .
S1 Au1 Au3 89.74(9) . .
S2 Au1 Au3 98.51(9) . .
Au2 Au1 Au3 71.281(13) . .
C11 S1 Au1 92.3(4) . .
N12 C11 N11 110.9(11) . .
N12 C11 S1 126.6(9) . .
N11 C11 S1 118.2(9) . .
C12 N11 C11 113.3(13) . .
N11 C12 C13 107.3(13) . .
N12 C13 C12 97.4(11) . .
C11 N12 C13 107.7(10) . .
C11 N12 Au2 129.6(9) . .
C13 N12 Au2 120.3(9) . .
N12 Au2 N12 178.3(7) . 2_665
N12 Au2 Au1 83.8(3) . .
N12 Au2 Au1 97.2(4) . 2_665
Au1 Au2 Au1 108.79(7) . 2_665
N12 Au2 Au3 89.2(3) . 7_454
Au1 Au2 Au3 125.61(4) . 7_454
C21 S2 Au1 92.6(4) . .
N22 C21 N21 113.6(11) . .
N22 C21 S2 128.3(9) . .
N21 C21 S2 115.8(9) . .
C22 N21 C21 112.7(12) . .
N21 C22 C23 108.2(12) . .
N22 C23 C22 99.9(11) . .
C21 N22 C23 105.1(10) . .
C21 N22 Au3 131.5(10) . .
C23 N22 Au3 122.5(9) . .
N22 Au3 N22 179.5(8) 2_665 .
N22 Au3 Au1 84.1(4) . .
N22 Au3 Au1 96.2(4) . 2_665
Au1 Au3 Au1 108.65(7) . 2_665
N22 Au3 Au2 89.7(4) . 7_455
Au1 Au3 Au2 125.68(4) . 7_455
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Au1 S1 2.284(4) .
Au1 S2 2.304(4) .
Au1 Au2 2.9717(13) .
Au1 Au3 2.9744(13) .
S1 C11 2.190(12) .
C11 N12 1.317(15) .
C11 N11 1.382(15) .
N11 C12 1.21(2) .
C12 C13 1.605(19) .
C13 N12 1.505(15) .
N12 Au2 2.038(10) .
Au2 Au3 3.1761(6) 7_454
S2 C21 2.154(13) .
C21 N22 1.320(15) .
C21 N21 1.378(15) .
N21 C22 1.20(2) .
C22 C23 1.591(18) .
C23 N22 1.505(15) .
N22 Au3 1.974(11) .
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_4
S2 Au1 S1 C11 128.3(8) .
Au2 Au1 S1 C11 -16.7(4) .
Au3 Au1 S1 C11 -87.7(4) .
Au1 S1 C11 N12 32.6(13) .
Au1 S1 C11 N11 -172.8(10) .
N12 C11 N11 C12 5(2) .
S1 C11 N11 C12 -153.8(15) .
C11 N11 C12 C13 -15(2) .
N11 C12 C13 N12 18(2) .
N11 C11 N12 C13 8.7(17) .
S1 C11 N12 C13 164.8(11) .
N11 C11 N12 Au2 171.2(10) .
S1 C11 N12 Au2 -32.7(19) .
C12 C13 N12 C11 -14.9(18) .
C12 C13 N12 Au2 -179.3(12) .
C11 N12 Au2 N12 -114.7(13) 2_665
C13 N12 Au2 N12 45.9(12) 2_665
C11 N12 Au2 Au1 11.2(13) .
C13 N12 Au2 Au1 171.8(13) .
C11 N12 Au2 Au1 119.5(13) 2_665
C13 N12 Au2 Au1 -79.9(12) 2_665
C11 N12 Au2 Au3 -114.7(13) 7_454
C13 N12 Au2 Au3 45.9(12) 7_454
S1 Au1 Au2 N12 9.1(4) .
S2 Au1 Au2 N12 -165.1(4) .
Au3 Au1 Au2 N12 95.5(4) .
S1 Au1 Au2 N12 -172.3(3) 2_665
S2 Au1 Au2 N12 13.5(3) 2_665
Au3 Au1 Au2 N12 -85.9(3) 2_665
S1 Au1 Au2 Au1 -86.45(9) 2_665
S2 Au1 Au2 Au1 99.39(9) 2_665
Au3 Au1 Au2 Au1 0.0 2_665
S1 Au1 Au2 Au3 93.55(9) 7_454
S2 Au1 Au2 Au3 -80.61(9) 7_454
Au3 Au1 Au2 Au3 180.0 7_454
S1 Au1 S2 C21 129.4(8) .
Au2 Au1 S2 C21 -85.0(4) .
Au3 Au1 S2 C21 -14.1(4) .
Au1 S2 C21 N22 25.9(14) .
Au1 S2 C21 N21 -173.0(11) .
N22 C21 N21 C22 0(2) .
S2 C21 N21 C22 -163.9(15) .
C21 N21 C22 C23 -5(2) .
N21 C22 C23 N22 7(2) .
N21 C21 N22 C23 4.7(17) .
S2 C21 N22 C23 166.1(11) .
N21 C21 N22 Au3 174.3(11) .
S2 C21 N22 Au3 -24(2) .
C22 C23 N22 C21 -6.4(17) .
C22 C23 N22 Au3 -177.2(12) .
C21 N22 Au3 N22 -119.3(14) 2_665
C23 N22 Au3 N22 48.8(12) 2_665
C21 N22 Au3 Au1 6.6(14) .
C23 N22 Au3 Au1 174.7(12) .
C21 N22 Au3 Au1 114.8(14) 2_665
C23 N22 Au3 Au1 -77.1(12) 2_665
C21 N22 Au3 Au2 -119.3(14) 7_455
C23 N22 Au3 Au2 48.8(11) 7_455
S1 Au1 Au3 N22 14.3(4) 2_665
S2 Au1 Au3 N22 -171.7(4) 2_665
Au2 Au1 Au3 N22 -85.9(4) 2_665
S1 Au1 Au3 N22 -165.3(4) .
S2 Au1 Au3 N22 8.7(4) .
Au2 Au1 Au3 N22 94.5(4) .
S1 Au1 Au3 Au1 100.19(9) 2_665
S2 Au1 Au3 Au1 -85.85(9) 2_665
Au2 Au1 Au3 Au1 0.0 2_665
S1 Au1 Au3 Au2 -79.81(9) 7_455
S2 Au1 Au3 Au2 94.15(9) 7_455
Au2 Au1 Au3 Au2 180.0 7_455
