#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:23:34 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179841 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/37/7013711.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_7013711
loop_
_publ_author_name
'Santos, Isabel Garcia'
'Hagenbach, Adelheid'
'Abram, Ulrich'
_publ_section_title
;
 Stable gold(III) complexes with thiosemicarbazone derivatives.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              677
_journal_page_last               682
_journal_paper_doi               10.1039/b312978k
_journal_year                    2004
_chemical_formula_moiety         '[AuCl(hm4dh)]Cl'
_chemical_formula_sum            'C9 H16 Au Cl2 N5 O2 S'
_chemical_formula_weight         526.19
_chemical_name_common
;Chloro(2-pyridineformamide thiosemicarbazonato)gold(iii)
chloride
;
_chemical_name_systematic
'Chloro(2-pyridineformamide thiosemicarbazonato)gold(III) chloride'
_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                 90.70(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   36.752(6)
_cell_length_b                   12.413(2)
_cell_length_c                   13.958(2)
_cell_measurement_temperature    173(2)
_cell_volume                     6367.2(17)
_computing_cell_refinement       'Bruker CCD'
_computing_data_collection       'Bruker CCD'
_computing_data_reduction        SAINT
_computing_molecular_graphics    ORTEP
_computing_publication_material  WINGX
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SHELXS-98
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker areal 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  0.0255
_diffrn_reflns_av_sigmaI/netI    0.0227
_diffrn_reflns_limit_h_max       52
_diffrn_reflns_limit_h_min       -52
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            39108
_diffrn_reflns_theta_full        30.56
_diffrn_reflns_theta_max         30.56
_diffrn_reflns_theta_min         1.11
_diffrn_standards_decay_%        1
_exptl_absorpt_coefficient_mu    9.716
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5654
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    2.196
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             4000
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.726
_refine_diff_density_min         -1.255
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.979
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     369
_refine_ls_number_reflns         9721
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.979
_refine_ls_R_factor_all          0.0287
_refine_ls_R_factor_gt           0.0207
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0240P)²+20.9728P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0474
_refine_ls_wR_factor_ref         0.0502
_reflns_number_gt                8385
_reflns_number_total             9721
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b312978k.txt
_cod_data_source_block           auhm4dh
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7013711
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Au1 Au 0.497419(3) -0.182707(9) 0.122554(8) 0.02026(3) Uani 1 1 d . . .
Cl1 Cl 0.51056(2) -0.36153(6) 0.10896(7) 0.03593(19) Uani 1 1 d . . .
N1 N 0.54746(6) -0.1207(2) 0.08496(18) 0.0218(5) Uani 1 1 d . . .
C1 C 0.57699(9) -0.1761(3) 0.0585(3) 0.0287(7) Uani 1 1 d . . .
H1 H 0.5760 -0.2525 0.0555 0.034 Uiso 1 1 calc R . .
C2 C 0.60875(9) -0.1236(3) 0.0357(3) 0.0322(7) Uani 1 1 d . . .
H2 H 0.6296 -0.1634 0.0170 0.039 Uiso 1 1 calc R . .
C3 C 0.60999(8) -0.0140(3) 0.0402(2) 0.0298(7) Uani 1 1 d . . .
H3 H 0.6320 0.0227 0.0260 0.036 Uiso 1 1 calc R . .
C4 C 0.57936(8) 0.0444(2) 0.0653(2) 0.0242(6) Uani 1 1 d . . .
H4 H 0.5799 0.1209 0.0668 0.029 Uiso 1 1 calc R . .
C5 C 0.54812(7) -0.0113(2) 0.0880(2) 0.0198(5) Uani 1 1 d . . .
C6 C 0.51337(8) 0.0405(2) 0.1161(2) 0.0198(5) Uani 1 1 d . . .
N5 N 0.50950(7) 0.1454(2) 0.1194(2) 0.0250(5) Uani 1 1 d . . .
H5A H 0.4883 0.1736 0.1342 0.030 Uiso 1 1 calc R . .
H5B H 0.5281 0.1876 0.1067 0.030 Uiso 1 1 calc R . .
N2 N 0.48664(6) -0.02766(19) 0.13430(17) 0.0193(5) Uani 1 1 d . . .
N3 N 0.45314(6) 0.0108(2) 0.16297(18) 0.0216(5) Uani 1 1 d . . .
C7 C 0.42964(7) -0.0657(2) 0.1783(2) 0.0209(5) Uani 1 1 d . . .
S1 S 0.43895(2) -0.20646(6) 0.16562(6) 0.02587(15) Uani 1 1 d . . .
N4 N 0.39587(7) -0.0424(2) 0.2071(2) 0.0277(6) Uani 1 1 d . . .
H4A H 0.3894 0.0251 0.2158 0.033 Uiso 1 1 calc R . .
H4B H 0.3802 -0.0946 0.2173 0.033 Uiso 1 1 calc R . .
Au2 Au 0.706450(3) -0.152092(9) 0.398992(8) 0.01857(3) Uani 1 1 d . . .
Cl2 Cl 0.652328(19) -0.22149(6) 0.45071(6) 0.02906(16) Uani 1 1 d . . .
N11 N 0.73442(6) -0.2963(2) 0.38672(18) 0.0205(5) Uani 1 1 d . . .
C11 C 0.72133(9) -0.3952(2) 0.4020(2) 0.0260(6) Uani 1 1 d . . .
H11 H 0.6969 -0.4039 0.4221 0.031 Uiso 1 1 calc R . .
C12 C 0.74293(9) -0.4848(3) 0.3889(2) 0.0291(7) Uani 1 1 d . . .
H12 H 0.7336 -0.5549 0.4007 0.035 Uiso 1 1 calc R . .
C13 C 0.77807(9) -0.4715(2) 0.3588(2) 0.0278(6) Uani 1 1 d . . .
H13 H 0.7931 -0.5327 0.3490 0.033 Uiso 1 1 calc R . .
C14 C 0.79167(8) -0.3686(2) 0.3423(2) 0.0240(6) Uani 1 1 d . . .
H14 H 0.8160 -0.3586 0.3216 0.029 Uiso 1 1 calc R . .
C15 C 0.76910(8) -0.2814(2) 0.3568(2) 0.0202(5) Uani 1 1 d . . .
C16 C 0.77992(8) -0.1680(2) 0.3432(2) 0.0204(5) Uani 1 1 d . . .
N15 N 0.81284(7) -0.1405(2) 0.3157(2) 0.0299(6) Uani 1 1 d . . .
H15A H 0.8186 -0.0721 0.3096 0.036 Uiso 1 1 calc R . .
H15B H 0.8291 -0.1906 0.3034 0.036 Uiso 1 1 calc R . .
N12 N 0.75437(6) -0.09604(19) 0.36267(18) 0.0195(5) Uani 1 1 d . . .
N13 N 0.76264(7) 0.01252(19) 0.35944(19) 0.0225(5) Uani 1 1 d . . .
C17 C 0.73486(8) 0.0735(2) 0.3796(2) 0.0220(6) Uani 1 1 d . . .
S2 S 0.690115(19) 0.02367(6) 0.40317(6) 0.02476(15) Uani 1 1 d . . .
N14 N 0.73792(8) 0.1805(2) 0.3810(2) 0.0302(6) Uani 1 1 d . . .
H14A H 0.7589 0.2111 0.3683 0.036 Uiso 1 1 calc R . .
H14B H 0.7189 0.2206 0.3947 0.036 Uiso 1 1 calc R . .
Cl3 Cl 0.68127(2) -0.21808(6) 0.18742(6) 0.03357(17) Uani 1 1 d . . .
Cl4 Cl 0.87869(2) -0.28595(7) 0.24430(7) 0.03316(17) Uani 1 1 d . . .
O20 O 0.44957(7) 0.2768(2) 0.1341(2) 0.0439(7) Uani 1 1 d . . .
H20 H 0.4299 0.2630 0.1616 0.066 Uiso 1 1 calc R . .
C21 C 0.45904(13) 0.3857(3) 0.1504(4) 0.0524(11) Uani 1 1 d . . .
H21A H 0.4592 0.4003 0.2194 0.079 Uiso 1 1 calc R . .
H21B H 0.4412 0.4326 0.1184 0.079 Uiso 1 1 calc R . .
H21C H 0.4833 0.3997 0.1246 0.079 Uiso 1 1 calc R . .
O30 O 0.56567(8) 0.3033(2) 0.1075(2) 0.0435(7) Uani 1 1 d . . .
H30 H 0.5840 0.2830 0.1390 0.065 Uiso 1 1 calc R . .
C31 C 0.57465(12) 0.3942(3) 0.0525(3) 0.0460(9) Uani 1 1 d . . .
H31A H 0.5727 0.4591 0.0921 0.069 Uiso 1 1 calc R . .
H31B H 0.5579 0.3998 -0.0023 0.069 Uiso 1 1 calc R . .
H31C H 0.5996 0.3871 0.0295 0.069 Uiso 1 1 calc R . .
O40 O 0.68321(9) 0.3094(3) 0.4726(3) 0.0625(9) Uani 1 1 d . . .
H40 H 0.6801 0.2721 0.5221 0.094 Uiso 1 1 calc R . .
C41 C 0.65649(11) 0.3869(3) 0.4664(3) 0.0462(10) Uani 1 1 d . . .
H41A H 0.6330 0.3548 0.4823 0.069 Uiso 1 1 calc R . .
H41B H 0.6554 0.4156 0.4011 0.069 Uiso 1 1 calc R . .
H41C H 0.6621 0.4453 0.5115 0.069 Uiso 1 1 calc R . .
O50 O 0.84230(7) 0.0531(2) 0.2571(2) 0.0476(7) Uani 1 1 d . . .
H50 H 0.8346 0.1138 0.2739 0.071 Uiso 1 1 calc R . .
C51 C 0.87965(10) 0.0592(4) 0.2402(3) 0.0480(10) Uani 1 1 d . . .
H51A H 0.8916 0.0989 0.2925 0.072 Uiso 1 1 calc R . .
H51B H 0.8837 0.0968 0.1795 0.072 Uiso 1 1 calc R . .
H51C H 0.8898 -0.0136 0.2367 0.072 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'
Cl Cl 0.1484 0.1585 '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'
O O 0.0106 0.0060 '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
N2 Au1 N1 80.69(10) . . ?
N2 Au1 S1 84.98(7) . . ?
N1 Au1 S1 165.65(7) . . ?
N2 Au1 Cl1 179.36(7) . . ?
N1 Au1 Cl1 98.70(7) . . ?
S1 Au1 Cl1 95.64(3) . . ?
C1 N1 C5 120.5(3) . . ?
C1 N1 Au1 127.2(2) . . ?
C5 N1 Au1 112.31(18) . . ?
N1 C1 C2 120.8(3) . . ?
C3 C2 C1 119.3(3) . . ?
C2 C3 C4 120.4(3) . . ?
C5 C4 C3 118.4(3) . . ?
N1 C5 C4 120.5(3) . . ?
N1 C5 C6 115.2(2) . . ?
C4 C5 C6 124.3(3) . . ?
N5 C6 N2 123.2(3) . . ?
N5 C6 C5 122.2(3) . . ?
N2 C6 C5 114.6(3) . . ?
C6 N2 N3 120.0(2) . . ?
C6 N2 Au1 117.22(19) . . ?
N3 N2 Au1 122.76(18) . . ?
C7 N3 N2 112.9(2) . . ?
N3 C7 N4 120.6(3) . . ?
N3 C7 S1 124.6(2) . . ?
N4 C7 S1 114.8(2) . . ?
C7 S1 Au1 94.74(10) . . ?
N12 Au2 N11 80.66(10) . . ?
N12 Au2 S2 84.51(7) . . ?
N11 Au2 S2 165.16(7) . . ?
N12 Au2 Cl2 176.16(8) . . ?
N11 Au2 Cl2 97.73(7) . . ?
S2 Au2 Cl2 97.04(3) . . ?
C11 N11 C15 121.0(3) . . ?
C11 N11 Au2 126.9(2) . . ?
C15 N11 Au2 112.05(19) . . ?
N11 C11 C12 120.7(3) . . ?
C13 C12 C11 119.2(3) . . ?
C12 C13 C14 120.1(3) . . ?
C15 C14 C13 118.5(3) . . ?
N11 C15 C14 120.4(3) . . ?
N11 C15 C16 115.1(2) . . ?
C14 C15 C16 124.5(3) . . ?
N15 C16 N12 122.7(3) . . ?
N15 C16 C15 122.2(3) . . ?
N12 C16 C15 115.1(2) . . ?
C16 N12 N13 119.6(2) . . ?
C16 N12 Au2 116.94(19) . . ?
N13 N12 Au2 123.46(18) . . ?
C17 N13 N12 112.7(2) . . ?
N13 C17 N14 121.0(3) . . ?
N13 C17 S2 124.2(2) . . ?
N14 C17 S2 114.7(2) . . ?
C17 S2 Au2 94.78(10) . . ?
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 N2 1.972(2) . ?
Au1 N1 2.067(2) . ?
Au1 S1 2.2579(8) . ?
Au1 Cl1 2.2801(9) . ?
N1 C1 1.340(4) . ?
N1 C5 1.359(4) . ?
C1 C2 1.378(5) . ?
C2 C3 1.363(5) . ?
C3 C4 1.387(4) . ?
C4 C5 1.381(4) . ?
C5 C6 1.487(4) . ?
C6 N5 1.311(4) . ?
C6 N2 1.323(4) . ?
N2 N3 1.384(3) . ?
N3 C7 1.304(4) . ?
C7 N4 1.341(4) . ?
C7 S1 1.789(3) . ?
Au2 N12 1.966(2) . ?
Au2 N11 2.073(2) . ?
Au2 S2 2.2637(8) . ?
Au2 Cl2 2.2923(8) . ?
N11 C11 1.336(4) . ?
N11 C15 1.359(4) . ?
C11 C12 1.380(4) . ?
C12 C13 1.373(5) . ?
C13 C14 1.392(4) . ?
C14 C15 1.380(4) . ?
C15 C16 1.476(4) . ?
C16 N15 1.319(4) . ?
C16 N12 1.326(4) . ?
N12 N13 1.382(3) . ?
N13 C17 1.304(4) . ?
C17 N14 1.334(4) . ?
C17 S2 1.791(3) . ?
O20 C21 1.413(5) . ?
O30 C31 1.406(5) . ?
O40 C41 1.377(5) . ?
O50 C51 1.398(4) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N5 H5A O20 0.88 1.92 2.751(4) 157.7 .
N5 H5B O30 0.88 1.99 2.853(4) 165.3 .
N15 H15A O50 0.88 1.93 2.764(4) 157.5 .
N14 H14B O40 0.88 2.04 2.880(4) 159.9 .
