#------------------------------------------------------------------------------
#$Date: 2016-03-22 11:50:55 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178919 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/48/4114870.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_4114870
loop_
_publ_author_name
'Ariane Adolf'
'Marcin Gonsior'
'Ingo Krossing'
_publ_contact_author             'Ingo Krossing'
_publ_contact_author_email       krossing@chemie.uni-karlsruhe.de
_publ_contact_author_fax         '0721 608 49 52'
_publ_contact_author_phone       '0721 608 29 51'
_publ_section_title
;
 Extending the Coordination Chemistry of Molecular P4S3: The Polymeric
 Ag(P4S3)+ and Ag(P4S3)2+ Cations
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7111
_journal_page_last               7116
_journal_paper_doi               10.1021/ja012760v
_journal_volume                  124
_journal_year                    2002
_chemical_formula_sum            'C12 H4 Ag Al F24 O4 P4 S3'
_chemical_formula_weight         1023.06
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 110.38(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.680(3)
_cell_length_b                   11.185(2)
_cell_length_c                   18.324(4)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    175(2)
_cell_measurement_theta_max      26
_cell_measurement_theta_min      2
_cell_volume                     3204.6(12)
_computing_cell_refinement       CELL
_computing_data_collection       EXPOSE
_computing_data_reduction        INTEGRATE
_computing_molecular_graphics    'RESVIEW and XP '
_computing_publication_material  SHELXL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      175(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'STOE IPDS '
_diffrn_measurement_method       'Image Plate Technique '
_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  0.0538
_diffrn_reflns_av_sigmaI/netI    0.0386
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            16899
_diffrn_reflns_theta_full        24.71
_diffrn_reflns_theta_max         24.71
_diffrn_reflns_theta_min         6.81
_exptl_absorpt_coefficient_mu    1.215
_exptl_absorpt_correction_T_max  0.6718
_exptl_absorpt_correction_T_min  0.5356
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   numerical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.120
_exptl_crystal_description       block
_exptl_crystal_F_000             1968
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.847
_refine_diff_density_min         -0.683
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     506
_refine_ls_number_reflns         5335
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0640
_refine_ls_R_factor_gt           0.0504
_refine_ls_shift/su_max          0.063
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0949P)²+1.2237P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1363
_refine_ls_wR_factor_ref         0.1444
_reflns_number_gt                4144
_reflns_number_total             5335
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja012760v_1.cif
_cod_data_source_block           Compound_1_in_the_manuscript
_cod_original_cell_volume        3204.6(11)
_cod_database_code               4114870
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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
Ag1 Ag 0.78270(2) 0.39507(3) 0.624515(18) 0.05875(11) Uani 1 1 d . . .
P1 P 0.93084(12) 0.6058(2) 0.76562(12) 0.0770(6) Uani 0.6860(19) 1 d P A 1
P2 P 0.76658(12) 0.54511(19) 0.81921(10) 0.0676(5) Uani 0.6860(19) 1 d P A 1
P3 P 0.7863(2) 0.7391(4) 0.8172(2) 0.0765(11) Uani 0.6860(19) 1 d P . 1
P4 P 0.71919(18) 0.6408(3) 0.70204(15) 0.0569(6) Uani 0.6860(19) 1 d P A 1
S1 S 0.82116(11) 0.61510(14) 0.66066(9) 0.0600(4) Uani 0.6860(19) 1 d P A 1
S2 S 0.8766(2) 0.4763(3) 0.82504(14) 0.0777(9) Uani 0.6860(19) 1 d P A 1
S3 S 0.9134(2) 0.7705(3) 0.81754(17) 0.0783(8) Uani 0.6860(19) 1 d P A 1
P1A P 0.8161(2) 0.5525(3) 0.70927(18) 0.0488(8) Uani 0.3140(19) 1 d P A 2
P2A P 0.7836(5) 0.7548(7) 0.8069(4) 0.0538(15) Uani 0.3140(19) 1 d P . 2
P3A P 0.9077(6) 0.7581(12) 0.8128(7) 0.147(4) Uani 0.3140(19) 1 d P A 2
P4A P 0.8878(3) 0.6329(4) 0.8910(2) 0.0732(12) Uani 0.3140(19) 1 d P A 2
S1A S 0.7161(5) 0.6525(9) 0.7212(4) 0.085(2) Uani 0.3140(19) 1 d P A 2
S2A S 0.8929(4) 0.4937(8) 0.8249(5) 0.089(3) Uani 0.3140(19) 1 d P A 2
S3A S 0.9091(3) 0.6754(5) 0.7129(3) 0.0851(13) Uani 0.3140(19) 1 d P A 2
Al1 Al 0.78503(7) 0.22235(10) 0.48455(7) 0.0469(3) Uani 1 1 d . . .
O1 O 0.86811(18) 0.2692(3) 0.56951(18) 0.0619(8) Uani 1 1 d . A .
O2 O 0.7504(2) 0.0817(3) 0.49759(19) 0.0690(8) Uani 1 1 d . A .
O3 O 0.8008(2) 0.2248(3) 0.3975(2) 0.0786(9) Uani 1 1 d . A .
O4 O 0.71198(16) 0.3313(2) 0.49030(15) 0.0497(6) Uani 1 1 d . A .
C1 C 0.9536(3) 0.2374(4) 0.6031(3) 0.0607(11) Uani 1 1 d . . .
H1A H 0.9666 0.1763 0.5705 0.073 Uiso 1 1 calc R A .
C2 C 1.0086(3) 0.3477(6) 0.6052(4) 0.0862(17) Uani 1 1 d . A .
C3 C 0.9703(3) 0.1851(6) 0.6841(3) 0.0789(15) Uani 1 1 d . A .
C4 C 0.7422(4) -0.0218(4) 0.4539(3) 0.0703(12) Uani 1 1 d . . .
H4A H 0.7428 0.0006 0.4024 0.084 Uiso 1 1 calc R A .
C5 C 0.6562(5) -0.0790(6) 0.4434(5) 0.110(2) Uani 1 1 d . A .
C6 C 0.8197(7) -0.1006(7) 0.4932(6) 0.133(3) Uani 1 1 d . A .
C7 C 0.8507(3) 0.2744(6) 0.3605(3) 0.0818(16) Uani 1 1 d D . .
H7A H 0.8824 0.3404 0.3931 0.098 Uiso 1 1 calc R A .
C8 C 0.9147(4) 0.1846(7) 0.3558(4) 0.167(4) Uani 1 1 d D A .
C9 C 0.7994(4) 0.3261(6) 0.2831(4) 0.132(3) Uani 1 1 d D A .
C10 C 0.6462(3) 0.3855(4) 0.4303(2) 0.0526(10) Uani 1 1 d . . .
H10A H 0.6460 0.3521 0.3808 0.063 Uiso 1 1 calc R A .
C11 C 0.5612(3) 0.3577(6) 0.4384(4) 0.0820(15) Uani 1 1 d . A .
C12 C 0.6633(4) 0.5193(5) 0.4301(3) 0.0860(17) Uani 1 1 d . A .
F1 F 1.0907(2) 0.3290(5) 0.6375(3) 0.1171(14) Uani 1 1 d . . .
F2 F 0.9947(3) 0.3836(5) 0.5323(3) 0.1440(19) Uani 1 1 d . . .
F3 F 0.9897(3) 0.4379(4) 0.6434(4) 0.1357(18) Uani 1 1 d . . .
F4 F 0.9481(3) 0.2593(4) 0.73013(18) 0.1155(14) Uani 1 1 d . . .
F5 F 0.9237(3) 0.0874(4) 0.6779(3) 0.1155(13) Uani 1 1 d . . .
F6 F 1.0505(2) 0.1537(4) 0.7203(2) 0.1101(12) Uani 1 1 d . . .
F7 F 0.6581(4) -0.1165(5) 0.5164(3) 0.174(2) Uani 1 1 d . . .
F8 F 0.6412(3) -0.1762(4) 0.4011(3) 0.1320(15) Uani 1 1 d . . .
F9 F 0.5956(3) -0.0087(6) 0.4166(6) 0.233(5) Uani 1 1 d . . .
F10 F 0.8105(5) -0.2044(4) 0.4528(4) 0.182(2) Uani 1 1 d . . .
F11 F 0.8901(4) -0.0418(7) 0.4951(5) 0.182(3) Uani 1 1 d . . .
F12 F 0.8323(6) -0.1290(5) 0.5626(4) 0.184(3) Uani 1 1 d . . .
F13 F 0.9631(4) 0.1597(8) 0.4286(4) 0.236(4) Uani 1 1 d D . .
F14 F 0.9626(4) 0.2275(9) 0.3181(4) 0.302(5) Uani 1 1 d D . .
F15 F 0.8788(6) 0.0842(7) 0.3220(5) 0.275(5) Uani 1 1 d D . .
F16 F 0.7364(3) 0.3955(6) 0.2857(3) 0.175(3) Uani 1 1 d D . .
F17 F 0.8448(3) 0.3898(5) 0.2509(3) 0.156(2) Uani 1 1 d D . .
F18 F 0.7598(4) 0.2400(8) 0.2329(3) 0.227(4) Uani 1 1 d D . .
F19 F 0.4964(2) 0.4170(5) 0.3852(2) 0.1201(14) Uani 1 1 d . . .
F20 F 0.5601(2) 0.3890(4) 0.5090(2) 0.1116(13) Uani 1 1 d . . .
F21 F 0.5438(3) 0.2448(4) 0.4264(4) 0.1392(18) Uani 1 1 d . . .
F22 F 0.6593(3) 0.5733(3) 0.4930(2) 0.1226(15) Uani 1 1 d . . .
F23 F 0.6087(4) 0.5750(3) 0.3683(2) 0.1316(17) Uani 1 1 d . . .
F24 F 0.7402(4) 0.5390(4) 0.4314(4) 0.1507(19) Uani 1 1 d . . .
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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Al Al 0.0645 0.0514 '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
P1A Ag1 O4 146.11(11) . .
P1A Ag1 O1 132.99(11) . .
O4 Ag1 O1 64.13(9) . .
P1A Ag1 P2A 100.8(2) . 2_646
O4 Ag1 P2A 100.41(19) . 2_646
O1 Ag1 P2A 105.6(2) . 2_646
P1A Ag1 P3 106.52(13) . 2_646
O4 Ag1 P3 95.34(11) . 2_646
O1 Ag1 P3 101.12(13) . 2_646
P2A Ag1 P3 5.7(3) 2_646 2_646
P1A Ag1 S1 26.79(9) . .
O4 Ag1 S1 122.03(7) . .
O1 Ag1 S1 121.74(9) . .
P2A Ag1 S1 125.91(19) 2_646 .
P3 Ag1 S1 131.49(10) 2_646 .
S3 P1 S1 98.71(13) . .
S3 P1 S2 101.83(14) . .
S1 P1 S2 96.13(11) . .
S2 P2 P3 104.27(17) . .
S2 P2 P4 104.30(13) . .
P3 P2 P4 61.66(13) . .
S3 P3 P2 108.4(2) . .
S3 P3 P4 104.2(2) . .
P2 P3 P4 60.95(13) . .
S3 P3 Ag1 118.76(19) . 2_656
P2 P3 Ag1 125.7(2) . 2_656
P4 P3 Ag1 124.91(17) . 2_656
S1 P4 P2 102.47(13) . .
S1 P4 P3 101.52(16) . .
P2 P4 P3 57.39(13) . .
P4 S1 P1 103.11(11) . .
P4 S1 Ag1 93.61(10) . .
P1 S1 Ag1 104.07(10) . .
P2 S2 P1 104.73(17) . .
P1 S3 P3 98.34(18) . .
S3A P1A S1A 105.1(3) . .
S3A P1A S2A 89.4(3) . .
S1A P1A S2A 106.5(3) . .
S3A P1A Ag1 122.7(2) . .
S1A P1A Ag1 118.1(3) . .
S2A P1A Ag1 110.7(3) . .
S1A P2A P3A 110.1(5) . .
S1A P2A P4A 106.2(4) . .
P3A P2A P4A 57.5(5) . .
S1A P2A Ag1 122.7(4) . 2_656
P3A P2A Ag1 125.6(4) . 2_656
P4A P2A Ag1 113.3(3) . 2_656
P2A P3A S3A 105.7(5) . .
P2A P3A P4A 68.1(5) . .
S3A P3A P4A 111.0(6) . .
S2A P4A P3A 93.2(4) . .
S2A P4A P2A 103.6(3) . .
P3A P4A P2A 54.4(4) . .
P2A S1A P1A 98.1(4) . .
P4A S2A P1A 102.8(4) . .
P1A S3A P3A 95.0(4) . .
O3 Al1 O2 108.27(18) . .
O3 Al1 O4 112.48(17) . .
O2 Al1 O4 110.69(17) . .
O3 Al1 O1 119.38(18) . .
O2 Al1 O1 110.33(17) . .
O4 Al1 O1 95.12(14) . .
C1 O1 Al1 133.2(3) . .
C1 O1 Ag1 128.2(3) . .
Al1 O1 Ag1 98.21(12) . .
C4 O2 Al1 130.8(3) . .
C7 O3 Al1 142.5(4) . .
C10 O4 Al1 128.9(2) . .
C10 O4 Ag1 129.9(2) . .
Al1 O4 Ag1 99.33(11) . .
O1 C1 C3 109.9(4) . .
O1 C1 C2 108.6(4) . .
C3 C1 C2 112.3(4) . .
F1 C2 F3 106.7(5) . .
F1 C2 F2 107.0(5) . .
F3 C2 F2 108.0(6) . .
F1 C2 C1 114.1(5) . .
F3 C2 C1 112.0(5) . .
F2 C2 C1 108.9(5) . .
F6 C3 F5 106.6(5) . .
F6 C3 F4 107.8(5) . .
F5 C3 F4 106.6(5) . .
F6 C3 C1 113.7(4) . .
F5 C3 C1 109.3(4) . .
F4 C3 C1 112.5(5) . .
O2 C4 C5 108.9(4) . .
O2 C4 C6 108.3(5) . .
C5 C4 C6 115.1(6) . .
F9 C5 F8 109.3(8) . .
F9 C5 F7 108.4(8) . .
F8 C5 F7 104.8(6) . .
F9 C5 C4 112.7(6) . .
F8 C5 C4 113.7(6) . .
F7 C5 C4 107.5(6) . .
F12 C6 F11 105.2(10) . .
F12 C6 F10 106.4(7) . .
F11 C6 F10 111.6(8) . .
F12 C6 C4 116.1(8) . .
F11 C6 C4 108.8(6) . .
F10 C6 C4 108.8(8) . .
O3 C7 C8 109.2(5) . .
O3 C7 C9 112.5(4) . .
C8 C7 C9 113.0(5) . .
F14 C8 F15 108.9(6) . .
F14 C8 F13 109.6(6) . .
F15 C8 F13 108.1(6) . .
F14 C8 C7 111.3(6) . .
F15 C8 C7 112.5(6) . .
F13 C8 C7 106.2(6) . .
F17 C9 F16 106.6(5) . .
F17 C9 F18 107.7(5) . .
F16 C9 F18 103.9(5) . .
F17 C9 C7 113.8(5) . .
F16 C9 C7 113.1(5) . .
F18 C9 C7 110.9(6) . .
O4 C10 C11 110.0(4) . .
O4 C10 C12 109.4(4) . .
C11 C10 C12 112.7(5) . .
F21 C11 F20 109.8(6) . .
F21 C11 F19 106.3(5) . .
F20 C11 F19 107.0(4) . .
F21 C11 C10 110.2(5) . .
F20 C11 C10 111.6(5) . .
F19 C11 C10 111.8(5) . .
F24 C12 F22 104.9(6) . .
F24 C12 F23 108.3(6) . .
F22 C12 F23 107.5(5) . .
F24 C12 C10 110.6(5) . .
F22 C12 C10 112.4(5) . .
F23 C12 C10 112.8(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ag1 P1A 2.285(3) .
Ag1 O4 2.435(3) .
Ag1 O1 2.455(3) .
Ag1 P2A 2.497(7) 2_646
Ag1 P3 2.523(4) 2_646
Ag1 S1 2.5712(17) .
P1 S3 2.139(4) .
P1 S1 2.146(3) .
P1 S2 2.189(4) .
P2 S2 1.959(4) .
P2 P3 2.197(5) .
P2 P4 2.280(3) .
P3 S3 2.146(5) .
P3 P4 2.295(5) .
P3 Ag1 2.523(4) 2_656
P4 S1 2.109(4) .
P1A S3A 2.056(6) .
P1A S1A 2.082(9) .
P1A S2A 2.162(8) .
P2A S1A 1.952(10) .
P2A P3A 2.035(13) .
P2A P4A 2.321(8) .
P2A Ag1 2.497(7) 2_656
P3A S3A 2.058(12) .
P3A P4A 2.111(16) .
P4A S2A 1.993(10) .
Al1 O3 1.705(3) .
Al1 O2 1.721(3) .
Al1 O4 1.752(3) .
Al1 O1 1.765(3) .
O1 C1 1.388(5) .
O2 C4 1.386(6) .
O3 C7 1.361(6) .
O4 C10 1.393(5) .
C1 C3 1.528(7) .
C1 C2 1.530(8) .
C2 F1 1.306(6) .
C2 F3 1.328(8) .
C2 F2 1.335(8) .
C3 F6 1.317(6) .
C3 F5 1.322(7) .
C3 F4 1.325(7) .
C4 C5 1.521(9) .
C4 C6 1.523(11) .
C5 F9 1.238(10) .
C5 F8 1.309(7) .
C5 F7 1.391(10) .
C6 F12 1.255(11) .
C6 F11 1.337(12) .
C6 F10 1.356(10) .
C7 C8 1.491(8) .
C7 C9 1.495(7) .
C8 F14 1.314(7) .
C8 F15 1.321(7) .
C8 F13 1.327(7) .
C9 F17 1.319(6) .
C9 F16 1.320(6) .
C9 F18 1.335(7) .
C10 C11 1.509(7) .
C10 C12 1.524(7) .
C11 F21 1.298(8) .
C11 F20 1.346(7) .
C11 F19 1.350(7) .
C12 F24 1.293(9) .
C12 F22 1.323(7) .
C12 F23 1.335(7) .
