#------------------------------------------------------------------------------
#$Date: 2016-03-25 16:39:18 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179982 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/76/7027600.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# 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_7027600
loop_
_publ_author_name
'Sampanthar, Jeyagowry T.'
'Vittal, Jagadese J.'
'Dean, Philip A. W.'
_publ_section_title
;
 Chemistry of thiocarboxylates: syntheses and characterization of silver
 and copper thiocarboxylate complexes, and the structures of
 [Ph4P][M(SC{O}Me)2] (M = Cu or Ag) and
 [Et3NH][Ag(SC{O}Ph)2]
;
_journal_issue                   18
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3153
_journal_paper_doi               10.1039/a904718b
_journal_year                    1999
_chemical_compound_source        'see text'
_chemical_formula_structural     '[Ph~4~P][Ag(SC{O}Me~2~]'
_chemical_formula_sum            'C28 H26 Ag O2 P S2'
_chemical_formula_weight         597.45
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           114
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P -4 2n'
_symmetry_space_group_name_H-M   'P -4 21 c'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.7596(1)
_cell_length_b                   11.7596(1)
_cell_length_c                   19.1859(3)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.47
_cell_measurement_theta_min      2.03
_cell_volume                     2653.18(5)
_computing_cell_refinement       'SAINT (Siemens, 1996)'
_computing_data_collection       'SMART (Siemens, 1996)'
_computing_data_reduction        'SAINT (Siemens, 1996)'
_computing_molecular_graphics    'SHELXTL (Siemens, 1996)'
_computing_publication_material  'SHELXTL (Siemens, 1996)'
_computing_structure_refinement  'SHELXTL (Siemens, 1996)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens SMART CCD System'
_diffrn_measurement_method       'frames 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  0.0224
_diffrn_reflns_av_sigmaI/netI    0.0178
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            16269
_diffrn_reflns_theta_max         29.47
_diffrn_reflns_theta_min         2.03
_exptl_absorpt_coefficient_mu    1.001
_exptl_absorpt_correction_T_max  0.7567
_exptl_absorpt_correction_T_min  0.6646
_exptl_absorpt_correction_type   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.496
_exptl_crystal_density_meas      ?
_exptl_crystal_description       'distorted octahedral shape'
_exptl_crystal_F_000             1216
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.38
_refine_diff_density_max         0.638
_refine_diff_density_min         -0.477
_refine_diff_density_rms         0.046
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.02(4)
_refine_ls_extinction_coef       0.0007(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.061
_refine_ls_goodness_of_fit_obs   1.110
_refine_ls_hydrogen_treatment
; 
riding models
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     156
_refine_ls_number_reflns         3420
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_restrained_S_obs      1.110
_refine_ls_R_factor_all          0.0455
_refine_ls_R_factor_obs          0.0332
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0388P)²+0.8383P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0851
_refine_ls_wR_factor_obs         0.0799
_reflns_number_observed          2780
_reflns_number_total             3420
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            904718Bsup1.cif
_cod_data_source_block           agta1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0388P)^2^+0.8383P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0388P)^2^+0.8383P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P-42(1)c
_cod_database_code               7027600
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, x+1/2, z+1/2'
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
Ag1 0.0503(2) 0.0778(2) 0.0723(2) 0.000 0.000 0.0006(2)
S1 0.0576(4) 0.0741(5) 0.0785(5) 0.0192(5) 0.0031(4) 0.0040(4)
O1 0.077(2) 0.126(3) 0.133(2) 0.074(2) 0.011(2) 0.021(2)
C1 0.050(2) 0.066(2) 0.077(2) 0.009(2) -0.0028(15) -0.0035(14)
C2 0.060(2) 0.078(2) 0.112(3) 0.005(2) 0.020(2) 0.005(2)
P1 0.0386(4) 0.0433(4) 0.0391(4) 0.000 0.000 -0.0016(5)
C3 0.0465(15) 0.0458(12) 0.0406(10) -0.0042(10) 0.0083(12) -0.0054(12)
C4 0.054(2) 0.062(2) 0.0505(15) -0.0031(13) -0.0012(13) -0.0070(13)
C5 0.066(2) 0.083(2) 0.056(2) -0.018(2) 0.0011(15) -0.021(2)
C6 0.087(2) 0.069(2) 0.075(2) -0.027(2) 0.017(2) -0.025(2)
C7 0.083(2) 0.056(2) 0.076(2) -0.015(2) 0.021(2) 0.004(2)
C8 0.057(2) 0.058(2) 0.056(2) -0.0046(14) 0.0082(14) 0.0023(14)
C9 0.0408(11) 0.0499(14) 0.0377(10) 0.0012(12) -0.0006(9) 0.0016(12)
C10 0.051(2) 0.068(2) 0.052(2) 0.0141(14) 0.0035(13) -0.0026(14)
C11 0.063(2) 0.082(2) 0.049(2) 0.021(2) 0.0014(14) 0.015(2)
C12 0.0465(15) 0.094(3) 0.0450(14) 0.0010(15) -0.0032(12) 0.011(2)
C13 0.0463(15) 0.070(2) 0.054(2) -0.0082(14) -0.0045(13) -0.0025(13)
C14 0.0500(15) 0.052(2) 0.0475(13) -0.0013(12) -0.0023(12) -0.0018(12)
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
Ag1 Ag 0.5000 0.0000 0.34674(2) 0.06681(12) Uani 1 d S
S1 S 0.32667(7) 0.10094(8) 0.34562(5) 0.0701(2) Uani 1 d .
O1 O 0.3059(2) -0.0332(3) 0.4527(2) 0.1121(12) Uani 1 d .
C1 C 0.2632(3) 0.0398(3) 0.4178(2) 0.0642(8) Uani 1 d .
C2 C 0.1473(3) 0.0851(3) 0.4349(2) 0.0836(11) Uani 1 d .
H2A H 0.1269(3) 0.1426(3) 0.4017(2) 0.125 Uiso 1 calc R
H2B H 0.1481(3) 0.1174(3) 0.4809(2) 0.125 Uiso 1 calc R
H2C H 0.0929(3) 0.0243(3) 0.4331(2) 0.125 Uiso 1 calc R
P1 P 0.5000 0.5000 0.32108(4) 0.0404(2) Uani 1 d S
C3 C 0.4867(2) 0.3782(2) 0.26497(12) 0.0443(5) Uani 1 d .
C4 C 0.3951(3) 0.3780(3) 0.21819(15) 0.0557(7) Uani 1 d .
H4 H 0.3439(3) 0.4383(3) 0.21765(15) 0.067 Uiso 1 calc R
C5 C 0.3814(3) 0.2880(3) 0.1730(2) 0.0683(9) Uani 1 d .
H5 H 0.3213(3) 0.2876(3) 0.1415(2) 0.082 Uiso 1 calc R
C6 C 0.4575(4) 0.1981(3) 0.1747(2) 0.0769(11) Uani 1 d .
H6 H 0.4470(4) 0.1365(3) 0.1450(2) 0.092 Uiso 1 calc R
C7 C 0.5471(3) 0.1988(3) 0.2192(2) 0.0716(9) Uani 1 d .
H7 H 0.5981(3) 0.1384(3) 0.2191(2) 0.086 Uiso 1 calc R
C8 C 0.5636(3) 0.2890(3) 0.2651(2) 0.0568(7) Uani 1 d .
H8 H 0.6253(3) 0.2894(3) 0.2954(2) 0.068 Uiso 1 calc R
C9 C 0.6232(2) 0.4887(3) 0.37616(11) 0.0428(5) Uani 1 d .
C10 C 0.6333(3) 0.3947(3) 0.42021(15) 0.0571(7) Uani 1 d .
H10 H 0.5786(3) 0.3376(3) 0.41960(15) 0.069 Uiso 1 calc R
C11 C 0.7256(3) 0.3871(3) 0.4648(2) 0.0648(9) Uani 1 d .
H11 H 0.7333(3) 0.3242(3) 0.4938(2) 0.078 Uiso 1 calc R
C12 C 0.8062(3) 0.4721(3) 0.46650(14) 0.0619(9) Uani 1 d .
H12 H 0.8682(3) 0.4661(3) 0.49639(14) 0.074 Uiso 1 calc R
C13 C 0.7953(3) 0.5650(3) 0.4245(2) 0.0567(7) Uani 1 d .
H13 H 0.8493(3) 0.6227(3) 0.4266(2) 0.068 Uiso 1 calc R
C14 C 0.7046(2) 0.5743(2) 0.3787(2) 0.0497(6) Uani 1 d .
H14 H 0.6983(2) 0.6375(2) 0.3498(2) 0.060 Uiso 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'
O O 0.0106 0.0060 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ag Ag -0.8971 1.1015 '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
S1 Ag1 S1 178.96(5) 2_655 .
C1 S1 Ag1 98.99(12) . .
O1 C1 C2 120.9(3) . .
O1 C1 S1 124.4(3) . .
C2 C1 S1 114.8(3) . .
C9 P1 C9 108.02(15) 2_665 .
C9 P1 C3 109.89(13) 2_665 .
C9 P1 C3 111.30(13) . .
C9 P1 C3 111.30(13) 2_665 2_665
C9 P1 C3 109.89(13) . 2_665
C3 P1 C3 106.5(2) . 2_665
C8 C3 C4 120.1(3) . .
C8 C3 P1 123.0(2) . .
C4 C3 P1 116.8(2) . .
C5 C4 C3 119.6(3) . .
C4 C5 C6 119.8(3) . .
C7 C6 C5 120.7(3) . .
C6 C7 C8 120.7(3) . .
C3 C8 C7 119.0(3) . .
C14 C9 C10 119.6(2) . .
C14 C9 P1 121.5(2) . .
C10 C9 P1 118.8(2) . .
C11 C10 C9 119.4(3) . .
C12 C11 C10 120.5(3) . .
C13 C12 C11 120.2(3) . .
C12 C13 C14 120.7(3) . .
C13 C14 C9 119.6(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ag1 S1 2.3588(9) 2_655
Ag1 S1 2.3588(9) .
S1 C1 1.730(4) .
O1 C1 1.199(4) .
C1 C2 1.499(5) .
P1 C9 1.798(2) 2_665
P1 C9 1.798(2) .
P1 C3 1.799(2) .
P1 C3 1.799(2) 2_665
C3 C8 1.384(4) .
C3 C4 1.402(4) .
C4 C5 1.377(4) .
C5 C6 1.386(6) .
C6 C7 1.356(5) .
C7 C8 1.392(4) .
C9 C14 1.390(4) .
C9 C10 1.397(4) .
C10 C11 1.384(4) .
C11 C12 1.378(5) .
C12 C13 1.363(4) .
C13 C14 1.387(4) .
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
S1 Ag1 S1 C1 144.32(13) 2_655
Ag1 S1 C1 O1 -0.7(4) .
Ag1 S1 C1 C2 179.3(3) .
