#------------------------------------------------------------------------------
#$Date: 2016-03-25 16:10:25 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179955 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/50/7025083.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_7025083
loop_
_publ_author_name
'Khanye, Setshaba D.'
'Báthori, Nikoletta B'
'Smith, Gregory S.'
'Chibale, Kelly'
_publ_section_title
;
 Gold(I) derived thiosemicarbazone complexes with rare halogen-halogen
 interaction-reduction of [Au(damp-C1,N)Cl2].
;
_journal_issue                   10
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2697
_journal_page_last               2700
_journal_paper_doi               10.1039/b925037a
_journal_volume                  39
_journal_year                    2010
_chemical_formula_sum            'C22 H24 Au Cl5 N8 S2'
_chemical_formula_weight         838.83
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 96.79(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.776(2)
_cell_length_b                   10.658(2)
_cell_length_c                   24.515(5)
_cell_measurement_reflns_used    9300
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.66
_cell_measurement_theta_min      2.59
_cell_volume                     3055.3(10)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2000)'
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    'X-Seed (Barbour, 2001), Platon (Spek, 2003)'
_computing_publication_material  'Platon (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Nonius Kappa CCD diffractometer'
_diffrn_measurement_method       '1.2° φ scans and 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  0.0395
_diffrn_reflns_av_sigmaI/netI    0.0489
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            9300
_diffrn_reflns_theta_full        25.66
_diffrn_reflns_theta_max         25.66
_diffrn_reflns_theta_min         2.59
_exptl_absorpt_coefficient_mu    5.417
_exptl_absorpt_correction_T_max  0.770
_exptl_absorpt_correction_T_min  0.763
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Sheldrick'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.824
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cubic
_exptl_crystal_F_000             1632
_exptl_crystal_recrystallization_method 'slow evaporation of acetonitrile'
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.737
_refine_diff_density_min         -1.183
_refine_diff_density_rms         0.127
_refine_ls_extinction_coef       0.00039(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     176
_refine_ls_number_reflns         2889
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0506
_refine_ls_R_factor_gt           0.0330
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0290P)²+4.3230P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0645
_refine_ls_wR_factor_ref         0.0708
_reflns_number_gt                2377
_reflns_number_total             2899
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b925037a.txt
_cod_data_source_block           d:
_cod_original_cell_volume        3055.3(11)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7025083
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, 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 0.5000 0.62628(3) 0.2500 0.03158(12) Uani 1 2 d S
Cl1 Cl 0.5000 0.94239(15) 0.2500 0.0295(4) Uani 1 2 d S
S1 S 0.30983(10) 0.60699(12) 0.25830(5) 0.0358(3) Uani 1 1 d .
N1 N 0.1222(3) 0.6843(4) 0.20078(17) 0.0364(10) Uani 1 1 d .
H1A H 0.0803 0.7319 0.1770 0.044 Uiso 1 1 calc R
H1B H 0.0904 0.6221 0.2170 0.044 Uiso 1 1 calc R
C1 C 0.2323(4) 0.7062(4) 0.21208(18) 0.0283(11) Uani 1 1 d .
Cl2 Cl -0.15645(11) 1.12731(13) 0.08305(6) 0.0474(3) Uani 1 1 d .
N2 N 0.2807(3) 0.8002(4) 0.18761(15) 0.0291(9) Uani 1 1 d .
H2 H 0.3546 0.8153 0.1939 0.035 Uiso 1 1 calc R
C2 C 0.2532(4) 0.9475(4) 0.11872(18) 0.0283(11) Uani 1 1 d .
Cl3 Cl -0.08445(14) 1.26839(14) -0.02139(6) 0.0542(4) Uani 1 1 d .
N3 N 0.2087(3) 0.8730(3) 0.15154(15) 0.0262(8) Uani 1 1 d .
C3 C 0.3783(4) 0.9602(5) 0.1133(2) 0.0370(12) Uani 1 1 d .
H2A H 0.4038 1.0451 0.1241 0.056 Uiso 1 1 calc R
H2B H 0.3911 0.9449 0.0751 0.056 Uiso 1 1 calc R
H2C H 0.4215 0.8989 0.1373 0.056 Uiso 1 1 calc R
N4 N -0.1020(4) 0.7956(5) 0.1480(2) 0.0542(13) Uani 1 1 d .
C4 C 0.1700(4) 1.0253(4) 0.08364(18) 0.0292(11) Uani 1 1 d .
C5 C 0.0591(4) 1.0408(4) 0.09667(19) 0.0306(11) Uani 1 1 d .
H5 H 0.0371 1.0002 0.1283 0.037 Uiso 1 1 calc R
C6 C -0.0194(4) 1.1133(4) 0.0650(2) 0.0330(11) Uani 1 1 d .
C7 C 0.0114(4) 1.1733(5) 0.0190(2) 0.0371(12) Uani 1 1 d .
C8 C 0.1202(5) 1.1578(5) 0.0045(2) 0.0392(13) Uani 1 1 d .
H8 H 0.1408 1.1970 -0.0277 0.047 Uiso 1 1 calc R
C9 C 0.1999(4) 1.0849(5) 0.0369(2) 0.0355(12) Uani 1 1 d .
H9 H 0.2751 1.0757 0.0270 0.043 Uiso 1 1 calc R
C10 C -0.1946(5) 0.8275(5) 0.1457(2) 0.0416(13) Uani 1 1 d .
C11 C -0.3127(4) 0.8690(5) 0.1410(3) 0.0489(14) Uani 1 1 d .
H11A H -0.3625 0.8024 0.1242 0.073 Uiso 1 1 calc R
H11B H -0.3217 0.9444 0.1181 0.073 Uiso 1 1 calc R
H11C H -0.3335 0.8881 0.1777 0.073 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'
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'
Cl Cl 0.1484 0.1585 '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_3
S1 Au1 S1 169.66(7) 2_655
C1 S1 Au1 109.53(16) .
N1 C1 N2 120.2(4) .
N1 C1 S1 117.5(4) .
N2 C1 S1 122.3(3) .
C1 N2 N3 116.4(4) .
N3 C2 C4 114.8(4) .
N3 C2 C3 126.0(4) .
C4 C2 C3 119.2(4) .
C2 N3 N2 118.7(4) .
C5 C4 C9 118.1(4) .
C5 C4 C2 120.6(4) .
C9 C4 C2 121.4(4) .
C6 C5 C4 121.7(5) .
C5 C6 C7 119.9(5) .
C5 C6 Cl2 119.4(4) .
C7 C6 Cl2 120.8(4) .
C8 C7 C6 119.7(5) .
C8 C7 Cl3 119.0(4) .
C6 C7 Cl3 121.3(4) .
C7 C8 C9 120.2(5) .
C4 C9 C8 120.4(5) .
N4 C10 C11 178.4(6) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Au1 S1 2.2819(13) .
Au1 S1 2.2819(13) 2_655
S1 C1 1.730(5) .
N1 C1 1.314(6) .
C1 N2 1.330(6) .
Cl2 C6 1.730(5) .
N2 N3 1.388(5) .
C2 N3 1.286(6) .
C2 C4 1.479(6) .
C2 C3 1.500(6) .
Cl3 C7 1.736(5) .
N4 C10 1.137(7) .
C4 C5 1.391(6) .
C4 C9 1.391(7) .
C5 C6 1.373(7) .
C6 C7 1.383(7) .
C7 C8 1.379(7) .
C8 C9 1.394(7) .
C10 C11 1.450(7) .
