#------------------------------------------------------------------------------
#$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $
#$Revision: 25271 $
#$URL: svn://www.crystallography.net/cod/cif/2/2008594.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# 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_2008594
loop_
_publ_author_name
'Lang, E. S.'
'Dahmer, M.'
'Abram, U.'
_publ_section_title
;
 Tetraphenylphosphonium
 tetrakis(1-methyl-1,2,3,4-tetrazole-5-thiolato-<i>S</i>)aurate(III)
 hemihydate
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              854
_journal_page_last               856
_journal_volume                  55
_journal_year                    1999
_chemical_formula_iupac          '(C24 H20 P) [Au (C2 H3 N4 S)4], 0.5H2 O1'
_chemical_formula_moiety         'C24 H20 P 1+, C8 H12 N16 Au S4 1-, 0.5H2 O1'
_chemical_formula_sum            'C32 H33 Au N16 O0.5 P S4'
_chemical_formula_weight         1005.91
_chemical_name_systematic
'tetraphenylphosphonium tetra(1-methyl-1,2,3,4-tetrazol-5-thiolato)aurate(III)'
_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'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 103.340(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.460(4)
_cell_length_b                   6.5520(5)
_cell_length_c                   32.603(7)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    208(2)
_cell_measurement_theta_max      13.34
_cell_measurement_theta_min      9.45
_cell_volume                     3836.9(12)
_computing_cell_refinement       'SET4 in CAD-4 Software'
_computing_data_collection       'CAD-4 Software (Enraf Nonius, 1989)'
_computing_data_reduction        'HELENA (Spek, 1998)'
_computing_molecular_graphics    'ZORTEP (Zsolnai, 1997)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997b)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997a)'
_diffrn_ambient_temperature      208(2)
_diffrn_measured_fraction_theta_full 0.459
_diffrn_measured_fraction_theta_max 0.459
_diffrn_measurement_device_type  'Enraf-Nonius CAD-4'
_diffrn_measurement_method       \w
_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  0.023
_diffrn_reflns_av_sigmaI/netI    0.032
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            5168
_diffrn_reflns_theta_full        26.97
_diffrn_reflns_theta_max         26.97
_diffrn_reflns_theta_min         3.01
_diffrn_standards_decay_%        10
_diffrn_standards_interval_count 300
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.145
_exptl_absorpt_correction_T_max  0.661
_exptl_absorpt_correction_T_min  0.425
_exptl_absorpt_correction_type   '\y scans'
_exptl_absorpt_process_details   '(PLATON; Spek, 1998)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.740
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1992
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.565
_refine_diff_density_min         -0.649
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         4177
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.043
_refine_ls_R_factor_gt           0.024
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
'calc w = 1/[\s^2^(Fo^2^)+(0.0281P)^2^+6.6510P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_wR_factor_ref         0.060
_reflns_number_gt                3214
_reflns_number_total             4177
_reflns_threshold_expression     I>2\s(I)
_[local]_cod_data_source_file    na1415.cif
_[local]_cod_data_source_block   autetp
_[local]_cod_cif_authors_sg_H-M  'C 2/c'
_[local]_cod_chemical_formula_sum_orig 'C32 H33 Au N16 O0.50 P S4'
_cod_original_cell_volume        3836.0(10)
_cod_database_code               2008594
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_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_type_symbol
Au 0.25 0.25 0 0.02104(6) Uani d S 1 Au
S1 0.14528(5) 0.10052(17) 0.01778(3) 0.0319(2) Uani d . 1 S
C2 0.17037(18) 0.0547(5) 0.07164(11) 0.0232(7) Uani d . 1 C
N3 0.16390(18) 0.1813(5) 0.10187(11) 0.0346(7) Uani d . 1 N
N4 0.1846(2) 0.0757(6) 0.13813(10) 0.0423(9) Uani d . 1 N
N5 0.20326(19) -0.1097(6) 0.13099(10) 0.0388(8) Uani d . 1 N
N6 0.19482(16) -0.1255(5) 0.08905(9) 0.0246(6) Uani d . 1 N
C7 0.2136(3) -0.3119(8) 0.06992(18) 0.0398(10) Uani d . 1 C
S11 0.32005(5) 0.18336(18) 0.06859(3) 0.0334(2) Uani d . 1 S
C12 0.41246(17) 0.2336(6) 0.06891(10) 0.0251(7) Uani d . 1 C
N13 0.44938(18) 0.4002(6) 0.08441(11) 0.0384(8) Uani d . 1 N
N14 0.51941(18) 0.3705(6) 0.07906(12) 0.0424(9) Uani d . 1 N
N15 0.52584(17) 0.1970(6) 0.06217(11) 0.0387(9) Uani d . 1 N
N16 0.45865(16) 0.1073(5) 0.05529(9) 0.0274(6) Uani d . 1 N
C17 0.4444(3) -0.0914(8) 0.03542(16) 0.0434(11) Uani d . 1 C
P 0.5000 0.2420(2) 0.2500 0.0222(2) Uani d S 1 P
C21 0.50677(19) 0.0821(6) 0.20634(10) 0.0248(7) Uani d . 1 C
C22 0.4511(2) -0.0627(6) 0.19215(12) 0.0325(8) Uani d . 1 C
C23 0.4551(3) -0.1890(7) 0.15855(13) 0.0378(10) Uani d . 1 C
C24 0.5148(3) -0.1748(7) 0.14019(12) 0.0368(9) Uani d . 1 C
C25 0.5697(3) -0.0325(7) 0.15392(12) 0.0378(10) Uani d . 1 C
C26 0.5653(2) 0.0976(7) 0.18669(12) 0.0301(8) Uani d . 1 C
C31 0.41811(18) 0.3980(6) 0.23600(11) 0.0245(7) Uani d . 1 C
C32 0.4028(2) 0.5343(6) 0.26565(12) 0.0305(8) Uani d . 1 C
C33 0.3380(2) 0.6470(7) 0.25713(14) 0.0363(9) Uani d . 1 C
C34 0.2886(2) 0.6279(7) 0.21851(15) 0.0412(11) Uani d . 1 C
C35 0.3030(2) 0.4939(8) 0.18872(14) 0.0441(11) Uani d . 1 C
C36 0.3678(2) 0.3785(7) 0.19749(12) 0.0329(9) Uani d . 1 C
O40 0 0 0 0.075(3) Uani d SP 0.50 O
H7A 0.185(2) -0.423(7) 0.0730(13) 0.040(13) Uiso d . 1 H
H7B 0.252(3) -0.339(10) 0.0783(18) 0.07(2) Uiso d . 1 H
H7C 0.206(3) -0.293(9) 0.0420(19) 0.070(18) Uiso d . 1 H
H17A 0.483(3) -0.144(9) 0.0374(15) 0.048(15) Uiso d . 1 H
H17B 0.425(3) -0.069(8) 0.0059(16) 0.051(14) Uiso d . 1 H
H17C 0.414(3) -0.166(9) 0.0492(16) 0.061(16) Uiso d . 1 H
H22 0.410(2) -0.076(6) 0.2034(12) 0.027(10) Uiso d . 1 H
H23 0.422(2) -0.284(6) 0.1474(14) 0.036(12) Uiso d . 1 H
H24 0.517(2) -0.270(7) 0.1201(15) 0.045(13) Uiso d . 1 H
H25 0.608(3) -0.017(8) 0.1442(15) 0.052(14) Uiso d . 1 H
H26 0.599(2) 0.184(7) 0.1943(14) 0.037(12) Uiso d . 1 H
H32 0.433(2) 0.553(6) 0.2895(12) 0.029(11) Uiso d . 1 H
H33 0.331(2) 0.728(7) 0.2773(14) 0.041(12) Uiso d . 1 H
H34 0.251(3) 0.701(8) 0.2130(16) 0.059(16) Uiso d . 1 H
H35 0.272(2) 0.490(7) 0.1632(14) 0.038(12) Uiso d . 1 H
H36 0.376(2) 0.295(6) 0.1795(13) 0.028(11) Uiso d . 1 H
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Au 0.02098(8) 0.02060(9) 0.02163(9) -0.00064(10) 0.00512(6) 0.00163(11)
S1 0.0247(4) 0.0423(6) 0.0274(4) -0.0056(4) 0.0036(3) 0.0123(4)
C2 0.0254(16) 0.0201(18) 0.0254(17) -0.0028(14) 0.0087(13) 0.0031(14)
N3 0.0414(18) 0.0273(16) 0.0395(18) -0.0043(14) 0.0182(15) -0.0045(15)
N4 0.054(2) 0.047(2) 0.0287(17) -0.0085(19) 0.0142(15) -0.0080(17)
N5 0.0454(19) 0.045(2) 0.0249(16) -0.0035(17) 0.0066(14) 0.0077(16)
N6 0.0281(14) 0.0231(17) 0.0216(14) -0.0002(12) 0.0039(11) 0.0029(13)
C7 0.045(3) 0.026(2) 0.048(3) 0.0037(19) 0.010(2) -0.0015(19)
S11 0.0243(4) 0.0500(6) 0.0248(4) -0.0044(4) 0.0034(3) 0.0082(4)
C12 0.0237(14) 0.0263(19) 0.0239(14) -0.0019(17) 0.0030(11) 0.0016(18)
N13 0.0373(17) 0.034(2) 0.043(2) -0.0066(15) 0.0060(15) -0.0044(17)
N14 0.0316(17) 0.047(2) 0.047(2) -0.0150(17) 0.0065(15) -0.0037(19)
N15 0.0269(15) 0.055(3) 0.0334(17) -0.0055(14) 0.0058(13) 0.0036(16)
N16 0.0274(14) 0.0300(17) 0.0227(14) -0.0009(13) 0.0015(11) 0.0009(13)
C17 0.057(3) 0.034(3) 0.039(3) 0.000(2) 0.011(2) -0.009(2)
P 0.0252(5) 0.0224(6) 0.0181(5) 0.000 0.0030(4) 0.000
C21 0.0324(17) 0.0220(18) 0.0182(16) -0.0005(15) 0.0023(13) 0.0008(14)
C22 0.042(2) 0.029(2) 0.0269(18) -0.0096(18) 0.0094(16) -0.0007(17)
C23 0.055(3) 0.024(2) 0.0283(19) -0.0086(18) -0.0017(18) -0.0022(16)
C24 0.061(3) 0.0271(19) 0.0218(18) 0.007(2) 0.0078(18) 0.0006(17)
C25 0.049(2) 0.040(2) 0.0271(19) 0.006(2) 0.0138(18) -0.0031(18)
C26 0.0326(19) 0.031(2) 0.0265(18) 0.0013(17) 0.0066(15) -0.0030(17)
C31 0.0236(15) 0.0228(18) 0.0261(17) -0.0012(14) 0.0039(13) 0.0040(15)
C32 0.0336(19) 0.027(2) 0.0282(19) -0.0024(16) 0.0021(16) -0.0032(16)
C33 0.036(2) 0.029(2) 0.044(2) 0.0053(18) 0.0109(18) -0.001(2)
C34 0.0291(19) 0.038(3) 0.055(3) 0.0093(18) 0.0057(18) 0.008(2)
C35 0.035(2) 0.054(3) 0.035(2) 0.004(2) -0.0082(17) 0.006(2)
C36 0.040(2) 0.033(2) 0.0238(18) 0.0045(18) 0.0029(15) 0.0005(17)
O40 0.056(6) 0.063(7) 0.103(9) -0.017(5) 0.015(6) 0.038(7)
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'
P P 0.1023 0.0942 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
S11 Au S11 7 . 180.0 ?
S11 Au S1 7 . 90.50(3) ?
S11 Au S1 . . 89.50(3) y
S11 Au S1 7 7 89.50(3) ?
S11 Au S1 . 7 90.50(3) ?
S1 Au S1 . 7 180.0 ?
C2 S1 Au . . 106.20(10) y
N3 C2 N6 . . 108.5(3) ?
N3 C2 S1 . . 126.9(3) y
N6 C2 S1 . . 124.4(3) y
C2 N3 N4 . . 106.1(3) ?
N5 N4 N3 . . 110.9(3) ?
N4 N5 N6 . . 106.3(3) ?
C2 N6 N5 . . 108.1(3) ?
C2 N6 C7 . . 130.5(3) ?
N5 N6 C7 . . 121.3(4) ?
C12 S11 Au . . 107.10(10) y
N13 C12 N16 . . 109.0(3) ?
N13 C12 S11 . . 125.3(3) y
N16 C12 S11 . . 125.6(3) y
C12 N13 N14 . . 104.7(3) ?
N15 N14 N13 . . 111.6(3) ?
N14 N15 N16 . . 106.7(3) ?
C12 N16 N15 . . 108.0(3) ?
C12 N16 C17 . . 129.8(4) ?
N15 N16 C17 . . 122.2(4) ?
C31 P C31 . 2_655 110.5(2) ?
C31 P C21 . . 109.85(16) ?
C31 P C21 2_655 . 108.99(15) ?
C31 P C21 . 2_655 108.99(15) ?
C31 P C21 2_655 2_655 109.85(16) ?
C21 P C21 . 2_655 108.6(2) ?
C26 C21 C22 . . 119.4(3) ?
C26 C21 P . . 122.0(3) ?
C22 C21 P . . 118.6(3) ?
C23 C22 C21 . . 119.8(4) ?
C24 C23 C22 . . 119.9(4) ?
C23 C24 C25 . . 120.7(4) ?
C24 C25 C26 . . 119.9(4) ?
C21 C26 C25 . . 120.3(4) ?
C36 C31 C32 . . 119.2(3) ?
C36 C31 P . . 121.8(3) ?
C32 C31 P . . 118.9(3) ?
C33 C32 C31 . . 120.6(4) ?
C32 C33 C34 . . 119.7(4) ?
C33 C34 C35 . . 120.4(4) ?
C34 C35 C36 . . 119.9(4) ?
C31 C36 C35 . . 120.2(4) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Au S11 7 2.3520(10) ?
Au S11 . 2.3520(10) y
Au S1 . 2.3560(10) y
Au S1 7 2.3560(10) ?
S1 C2 . 1.736(3) y
C2 N3 . 1.315(5) y
C2 N6 . 1.342(4) y
N3 N4 . 1.347(5) ?
N4 N5 . 1.298(5) ?
N5 N6 . 1.344(4) ?
N6 C7 . 1.449(6) ?
S11 C12 . 1.735(3) y
C12 N13 . 1.324(5) y
C12 N16 . 1.336(5) y
N13 N14 . 1.358(5) ?
N14 N15 . 1.280(5) ?
N15 N16 . 1.344(4) ?
N16 C17 . 1.451(6) ?
P C31 . 1.795(4) ?
P C31 2_655 1.795(4) ?
P C21 . 1.795(4) ?
P C21 2_655 1.795(4) ?
C21 C26 . 1.380(5) ?
C21 C22 . 1.397(5) ?
C22 C23 . 1.389(6) ?
C23 C24 . 1.373(6) ?
C24 C25 . 1.374(6) ?
C25 C26 . 1.384(5) ?
C31 C36 . 1.385(5) ?
C31 C32 . 1.392(5) ?
C32 C33 . 1.378(5) ?
C33 C34 . 1.380(6) ?
C34 C35 . 1.380(7) ?
C35 C36 . 1.387(6) ?