#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:55:43 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179084 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/46/4304694.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4304694
loop_
_publ_author_name
'Javier Arias'
'Manuel Bardají'
'Pablo Espinet'
_publ_contact_author_address
;
 IU CINQUIMA/Quimica Inorganica, Facultad de Ciencias, 
Universidad de Valladolid. E-47071 Valladolid, Spain
;
_publ_contact_author_email       espinet@qi.uva.es
_publ_contact_author_fax         '+34 983 423013'
_publ_contact_author_name        'Pablo Espinet'
_publ_contact_author_phone       '+34 983 423231'
_publ_section_title
;
Mononuclear, Dinuclear, and Hexanuclear Gold(I) Complexes with
(aza-15-crown-5)Dithiocarbamate
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1597
_journal_page_last               1606
_journal_paper_doi               10.1021/ic702252j
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C11 H20 Au N O4 S2'
_chemical_formula_weight         491.37
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_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                120.00
_cell_formula_units_Z            18
_cell_length_a                   21.6188(14)
_cell_length_b                   21.6188(14)
_cell_length_c                   17.116(2)
_cell_measurement_temperature    298(2)
_cell_volume                     6927.8(10)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0673
_diffrn_reflns_av_sigmaI/netI    0.0767
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            9418
_diffrn_reflns_theta_full        23.26
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         1.61
_exptl_absorpt_coefficient_mu    9.835
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.651
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
SADABS; a Program for Absorption Correction with the
Siemens SMART system (1996).
;
_exptl_crystal_colour            YELLOW
_exptl_crystal_density_diffrn    2.120
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       PRISM
_exptl_crystal_F_000             4248
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.899
_refine_diff_density_min         -0.628
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.872
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     202
_refine_ls_number_reflns         2177
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.872
_refine_ls_R_factor_all          0.0636
_refine_ls_R_factor_gt           0.0330
_refine_ls_shift/su_max          0.036
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0266P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0650
_refine_ls_wR_factor_ref         0.0721
_reflns_number_gt                1438
_reflns_number_total             2177
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic702252j-file002_2.cif
_cod_data_source_block           ajmb9m1
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal' according
to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        6927.9(12)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4304694
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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 0.26217(2) 0.74940(2) 1.15175(2) 0.05101(16) Uani 1 1 d . . .
S1 S 0.26713(14) 0.72339(14) 1.02292(15) 0.0586(8) Uani 1 1 d . . .
S2 S 0.12983(14) 0.58364(15) 1.06066(16) 0.0594(8) Uani 1 1 d . . .
C1 C 0.1905(5) 0.6456(5) 0.9967(6) 0.045(2) Uani 1 1 d . . .
N1 N 0.1779(4) 0.6313(4) 0.9215(5) 0.058(2) Uani 1 1 d . . .
C2 C 0.1179(6) 0.5634(6) 0.8921(6) 0.068(3) Uani 1 1 d . . .
H2A H 0.1126 0.5245 0.9248 0.082 Uiso 1 1 calc R . .
H2B H 0.1286 0.5550 0.8395 0.082 Uiso 1 1 calc R . .
C3 C 0.0494(7) 0.5642(7) 0.8914(7) 0.084(4) Uani 1 1 d . . .
H3A H 0.0103 0.5161 0.8822 0.101 Uiso 1 1 calc R . .
H3B H 0.0421 0.5793 0.9422 0.101 Uiso 1 1 calc R . .
O1 O 0.0480(5) 0.6091(5) 0.8348(5) 0.092(3) Uani 1 1 d . . .
C4 C -0.0102(8) 0.6162(9) 0.8267(10) 0.114(5) Uani 1 1 d . A .
H4A H -0.0199 0.6302 0.8770 0.137 Uiso 1 1 calc R . .
H4B H -0.0504 0.5694 0.8147 0.137 Uiso 1 1 calc R . .
C5 C -0.0094(10) 0.6656(10) 0.7690(19) 0.132(8) Uani 1 1 d . . .
O2A O 0.050(5) 0.736(4) 0.759(5) 0.22(5) Uani 0.33(7) 1 d P A 1
O2B O 0.0459(15) 0.705(2) 0.732(2) 0.142(18) Uani 0.67(7) 1 d P A 2
C6 C 0.0610(15) 0.7597(13) 0.6859(14) 0.146(9) Uani 1 1 d . . .
C7 C 0.1375(19) 0.8037(16) 0.671(2) 0.178(13) Uani 1 1 d . A .
O3A O 0.182(5) 0.816(4) 0.724(4) 0.19(4) Uani 0.32(5) 1 d P A 1
O3B O 0.1828(9) 0.7771(10) 0.6743(13) 0.105(10) Uani 0.68(5) 1 d P A 2
C8 C 0.2533(15) 0.8216(13) 0.6827(15) 0.164(8) Uani 1 1 d . . .
C9A C 0.2831(12) 0.8379(15) 0.7504(16) 0.098(13) Uani 0.65(4) 1 d P A 1
C9B C 0.288(2) 0.771(3) 0.706(2) 0.10(3) Uani 0.35(4) 1 d P A 2
O4 O 0.2851(5) 0.7737(6) 0.7822(7) 0.137(4) Uani 1 1 d . . .
C10 C 0.2192(7) 0.7295(7) 0.8351(8) 0.092(4) Uani 1 1 d . A .
H10A H 0.2180 0.7567 0.8796 0.110 Uiso 1 1 calc R . .
H10B H 0.1747 0.7098 0.8065 0.110 Uiso 1 1 calc R . .
C11 C 0.2354(7) 0.6784(7) 0.8562(8) 0.093(4) Uani 1 1 d . . .
H11A H 0.2835 0.7001 0.8773 0.112 Uiso 1 1 calc R A .
H11B H 0.2320 0.6492 0.8116 0.112 Uiso 1 1 calc R . .
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'
O O 0.0106 0.0060 '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
_geom_angle_publ_flag
S2 Au1 S1 170.53(10) 14_457 . ?
S2 Au1 Au1 87.44(7) 14_457 14_457 ?
S1 Au1 Au1 96.69(7) . 14_457 ?
S2 Au1 Au1 97.69(8) 14_457 15_557 ?
S1 Au1 Au1 88.05(7) . 15_557 ?
Au1 Au1 Au1 117.028(9) 14_457 15_557 ?
C1 S1 Au1 110.4(3) . . ?
C1 S2 Au1 110.9(3) . 15_557 ?
N1 C1 S2 116.8(7) . . ?
N1 C1 S1 117.9(7) . . ?
S2 C1 S1 125.4(6) . . ?
C1 N1 C2 122.8(8) . . ?
C1 N1 C11 121.8(8) . . ?
C2 N1 C11 114.3(8) . . ?
N1 C2 C3 112.1(9) . . ?
O1 C3 C2 112.6(11) . . ?
C4 O1 C3 120.1(11) . . ?
O1 C4 C5 119.1(14) . . ?
O2B C5 O2A 33(2) . . ?
O2B C5 C4 120.3(17) . . ?
O2A C5 C4 122(4) . . ?
C6 O2A C5 114(4) . . ?
C5 O2B C6 130(2) . . ?
O2B C6 O2A 34.2(19) . . ?
O2B C6 C7 112(2) . . ?
O2A C6 C7 109(4) . . ?
O3A C7 O3B 55(4) . . ?
O3A C7 C6 121(5) . . ?
O3B C7 C6 123(2) . . ?
C7 O3A C8 107(5) . . ?
C8 O3B C7 120(2) . . ?
C9A C8 O3B 122(2) . . ?
C9A C8 O3A 87(3) . . ?
O3B C8 O3A 46(3) . . ?
C9A C8 C9B 69(2) . . ?
O3B C8 C9B 106(2) . . ?
O3A C8 C9B 124(3) . . ?
C8 C9A O4 108(3) . . ?
O4 C9B C8 100(4) . . ?
C9B O4 C9A 73(2) . . ?
C9B O4 C10 127(2) . . ?
C9A O4 C10 109.7(13) . . ?
C11 C10 O4 97.2(11) . . ?
C10 C11 N1 105.5(12) . . ?
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 S2 2.286(3) 14_457 ?
Au1 S1 2.291(3) . ?
Au1 Au1 2.9289(5) 14_457 ?
Au1 Au1 2.9289(5) 15_557 ?
S1 C1 1.729(9) . ?
S2 C1 1.720(10) . ?
S2 Au1 2.286(3) 15_557 ?
C1 N1 1.320(11) . ?
N1 C2 1.478(12) . ?
N1 C11 1.602(15) . ?
C2 C3 1.488(14) . ?
C3 O1 1.382(13) . ?
O1 C4 1.349(14) . ?
C4 C5 1.45(2) . ?
C5 O2B 1.24(2) . ?
C5 O2A 1.43(9) . ?
O2A C6 1.33(9) . ?
O2B C6 1.33(3) . ?
C6 C7 1.46(4) . ?
C7 O3A 1.26(7) . ?
C7 O3B 1.36(3) . ?
O3A C8 1.64(8) . ?
O3B C8 1.34(3) . ?
C8 C9A 1.29(3) . ?
C8 C9B 1.65(6) . ?
C9A O4 1.51(3) . ?
C9B O4 1.31(4) . ?
O4 C10 1.550(15) . ?
C10 C11 1.365(15) . ?
