# Copyright The Royal Society of Chemistry, 1999
# CCDC Number: 182/1293

# Cif file for the manuscript "Deprotonated ethylenethiourea ... "

#

# submitted to Chem. Comm.

#

# Authors: P.G. Jones(*), S. Friedrichs

#

# This cif file contains ONE structure only

#

data_nichda



_audit_creation_method            SHELXL-97

_chemical_name_systematic

;

 ?

;

_chemical_name_common             ?

_chemical_melting_point           ?

_chemical_formula_moiety          ?

_chemical_formula_sum

 'C12 H20 Au4 N8 S4'

_chemical_formula_weight          1192.47



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'



_symmetry_cell_setting            orthorhombic

_symmetry_space_group_name_H-M    'I b a 2'



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'



_cell_length_a                    16.1973(9)

_cell_length_b                    10.3143(6)

_cell_length_c                    13.2818(7)

_cell_angle_alpha                 90.00

_cell_angle_beta                  90.00

_cell_angle_gamma                 90.00

_cell_volume                      2218.9(2)

_cell_formula_units_Z             4

_cell_measurement_temperature     143(2)

_cell_measurement_reflns_used     4174

_cell_measurement_theta_min       2

_cell_measurement_theta_max       28



_exptl_crystal_description        needle

_exptl_crystal_colour             colourless

_exptl_crystal_size_max           0.10

_exptl_crystal_size_mid           0.02

_exptl_crystal_size_min           0.01

_exptl_crystal_density_meas       ?

_exptl_crystal_density_diffrn     3.570

_exptl_crystal_density_method     'not measured'

_exptl_crystal_F_000              2112

_exptl_absorpt_coefficient_mu     26.758

_exptl_absorpt_correction_type    'multiple scans (SADABS)'

_exptl_absorpt_correction_T_min   0.453

_exptl_absorpt_correction_T_max   0.962

_exptl_absorpt_process_details    ?



_exptl_special_details

;

 ?

;



_diffrn_ambient_temperature       143(2)

_diffrn_radiation_wavelength      0.71073

_diffrn_radiation_type            MoK\a

_diffrn_radiation_source          'fine-focus sealed tube'

_diffrn_radiation_monochromator   graphite

_diffrn_measurement_device_type   'Bruker SMART 1000 CCD'

_diffrn_measurement_method        \w-scans

_diffrn_detector_area_resol_mean  8.192

_diffrn_standards_number          ?

_diffrn_standards_interval_count  ?

_diffrn_standards_interval_time   ?

_diffrn_standards_decay_%         ?

_diffrn_reflns_number             11368

_diffrn_reflns_av_R_equivalents   0.0555

_diffrn_reflns_av_sigmaI/netI     0.0437

_diffrn_reflns_limit_h_min        -21

_diffrn_reflns_limit_h_max        21

_diffrn_reflns_limit_k_min        -13

_diffrn_reflns_limit_k_max        13

_diffrn_reflns_limit_l_min        -17

_diffrn_reflns_limit_l_max        17

_diffrn_reflns_theta_min          2.34

_diffrn_reflns_theta_max          28.28

_reflns_number_total              2759

_reflns_number_gt                 2208

_reflns_threshold_expression      >2sigma(I)



_computing_data_collection        'Bruker SMART'

_computing_cell_refinement        'Bruker SAINT'

_computing_data_reduction         'Bruker SAINT'

_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)'

_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)'

_computing_molecular_graphics     'Siemens XP'

_computing_publication_material   SHELXL-97



_refine_special_details

;

 Refinement of F^2^ against ALL reflections.  The weighted R-factor wR and

 goodness of fit S are based on F^2^, conventional R-factors R are based

 on F, with F set to zero for negative F^2^. The threshold expression of

 F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is

 not relevant to the choice of reflections for refinement.  R-factors based

 on F^2^ are statistically about twice as large as those based on F, and R-

 factors based on ALL data will be even larger.

;



_refine_ls_structure_factor_coef  Fsqd

_refine_ls_matrix_type            full

_refine_ls_weighting_scheme       calc

_refine_ls_weighting_details

 'calc w=1/[\s^2^(Fo^2^)+(0.0402P)^2^+10.6284P] where P=(Fo^2^+2Fc^2^)/3'

_atom_sites_solution_primary      direct

_atom_sites_solution_secondary    difmap

_atom_sites_solution_hydrogens    riding

_refine_ls_hydrogen_treatment     mixed

_refine_ls_extinction_method      none

_refine_ls_extinction_coef        ?

_refine_ls_abs_structure_details

 'Flack H D (1983), Acta Cryst. A39, 876-881'

_refine_ls_abs_structure_Flack    0.46(2)

_refine_ls_number_reflns          2759

_refine_ls_number_parameters      119

_refine_ls_number_restraints      154

_refine_ls_R_factor_all           0.0463

_refine_ls_R_factor_gt            0.0323

_refine_ls_wR_factor_ref          0.0807

_refine_ls_wR_factor_gt           0.0753

_refine_ls_goodness_of_fit_ref    1.032

_refine_ls_restrained_S_all       1.016

_refine_ls_shift/su_max           0.001

_refine_ls_shift/su_mean          0.000



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

 _atom_site_disorder_assembly

 _atom_site_disorder_group

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_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 0.02538(19) 0.02109(17) 0.03208(19) 0.0022(5) 0.0014(6) 0.00560(16)

C11 0.030(5) 0.033(5) 0.030(5) 0.002(5) -0.003(4) -0.001(5)

N11 0.039(6) 0.050(6) 0.042(6) 0.005(5) -0.004(5) -0.019(5)

C12 0.052(8) 0.041(7) 0.054(8) -0.007(6) -0.003(6) -0.022(6)

C13 0.051(6) 0.028(6) 0.063(7) -0.013(5) 0.004(6) -0.003(5)

N12 0.032(5) 0.036(6) 0.020(5) -0.008(4) -0.008(4) -0.022(5)

Au2 0.0197(7) 0.0182(8) 0.0221(7) 0.000 0.000 0.0000(6)

C21 0.048(6) 0.022(5) 0.033(6) -0.002(5) -0.001(5) -0.005(5)

N21 0.059(7) 0.020(4) 0.046(6) -0.001(4) -0.009(5) -0.010(4)

C22 0.045(7) 0.035(6) 0.043(7) 0.003(6) -0.004(6) -0.014(6)

C23 0.037(6) 0.029(5) 0.034(6) 0.001(5) -0.001(5) -0.010(5)

N22 0.033(6) 0.031(5) 0.037(6) 0.000(5) 0.013(5) -0.011(5)

Au3 0.0262(8) 0.0140(7) 0.0203(7) 0.000 0.000 -0.0038(6)



_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 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_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

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_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

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 ?



_diffrn_measured_fraction_theta_max    0.999

_diffrn_reflns_theta_full              28.00

_diffrn_measured_fraction_theta_full   0.999

_refine_diff_density_max    2.260

_refine_diff_density_min   -2.200

_refine_diff_density_rms    0.282

#

# end of cif file