#------------------------------------------------------------------------------
#$Date: 2016-03-26 00:21:35 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180074 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/20/7052055.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_7052055
loop_
_publ_author_name
'Alberto, Roger'
'Angst, Daniela'
'Ortner, Kirstin'
'Abram, Ulrich'
'Schubiger, P. August'
'Kaden, Thomas A.'
_publ_section_title
;
 Syntheses of a series of S6 thioether cages and their coordination
 chemistry with Ag+
;
_journal_issue                   3
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              409
_journal_paper_doi               10.1039/b606510b
_journal_volume                  31
_journal_year                    2007
_chemical_formula_moiety         'C29 H49 Ag O4 S7'
_chemical_formula_sum            'C29 H49 Ag O4 S7'
_chemical_formula_weight         793.97
_chemical_name_systematic
;
[(S6-Cage-C4-OH-CH3)(tosylato)silver(I)] polymer
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 103.61(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.707(4)
_cell_length_b                   17.737(4)
_cell_length_c                   19.081(8)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    208(2)
_cell_measurement_theta_max      11.50
_cell_measurement_theta_min      3.45
_cell_volume                     3522(2)
_computing_cell_refinement       SET4
_computing_data_collection       CAD4
_computing_data_reduction        'PLATON,HELENA (Spek, 1995)'
_computing_molecular_graphics    ORTEP
_computing_publication_material  WINGX
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SHELXS86
_diffrn_ambient_temperature      208(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  CAD4
_diffrn_measurement_method       '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  0.1338
_diffrn_reflns_av_sigmaI/netI    0.4892
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            6398
_diffrn_reflns_theta_full        24.00
_diffrn_reflns_theta_max         24.00
_diffrn_reflns_theta_min         3.02
_diffrn_standards_decay_%        .5
_diffrn_standards_interval_count 300
_diffrn_standards_interval_time  3600
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.020
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.8721
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   DIFABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.497
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1656
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.534
_refine_diff_density_min         -0.970
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.956
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         5419
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.962
_refine_ls_R_factor_all          0.3303
_refine_ls_R_factor_gt           0.0776
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0755
_refine_ls_wR_factor_ref         0.1173
_reflns_number_gt                1717
_reflns_number_total             5419
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b606510b.txt
_cod_data_source_block           ag14
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7052055
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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 0.34702(13) 0.14419(6) 0.07720(6) 0.0407(4) Uani 1 1 d . . .
O1 O 0.4067(11) 0.1309(5) -0.1948(5) 0.071(4) Uani 1 1 d . . .
H1 H 0.4404 0.1389 -0.1516 0.107 Uiso 1 1 calc R . .
C2 C 0.2885(15) 0.0920(7) -0.2007(7) 0.050(5) Uani 1 1 d . . .
H2A H 0.2495 0.0826 -0.2518 0.060 Uiso 1 1 calc R . .
H2B H 0.2297 0.1242 -0.1818 0.060 Uiso 1 1 calc R . .
C3 C 0.3040(14) 0.0184(7) -0.1609(7) 0.025(4) Uani 1 1 d . . .
C11 C 0.3563(13) 0.0292(7) -0.0798(6) 0.040(4) Uani 1 1 d . . .
H11A H 0.4276 0.0652 -0.0724 0.047 Uiso 1 1 calc R . .
H11B H 0.3914 -0.0190 -0.0590 0.047 Uiso 1 1 calc R . .
S12 S 0.2427(4) 0.0620(2) -0.03128(18) 0.0398(11) Uani 1 1 d . . .
C13 C 0.1944(15) -0.0257(8) 0.0034(7) 0.086(7) Uani 1 1 d . . .
H13A H 0.1031 -0.0337 -0.0187 0.103 Uiso 1 1 calc R . .
H13B H 0.2420 -0.0668 -0.0128 0.103 Uiso 1 1 calc R . .
C14 C 0.2127(15) -0.0318(7) 0.0806(7) 0.060(6) Uani 1 1 d . . .
H14A H 0.1810 0.0146 0.0984 0.072 Uiso 1 1 calc R . .
H14B H 0.3052 -0.0349 0.1023 0.072 Uiso 1 1 calc R . .
C15 C 0.1474(15) -0.0984(7) 0.1070(7) 0.052(5) Uani 1 1 d . . .
H15A H 0.1553 -0.0931 0.1590 0.063 Uiso 1 1 calc R . .
H15B H 0.0557 -0.0975 0.0834 0.063 Uiso 1 1 calc R . .
C16 C 0.2023(13) -0.1737(7) 0.0929(7) 0.048(5) Uani 1 1 d . . .
H16A H 0.2905 -0.1773 0.1221 0.058 Uiso 1 1 calc R . .
H16B H 0.2060 -0.1758 0.0421 0.058 Uiso 1 1 calc R . .
S17 S 0.1136(5) -0.2536(2) 0.1120(2) 0.0535(14) Uani 1 1 d . . .
C18 C -0.0226(12) -0.2556(8) 0.0352(6) 0.048(4) Uani 1 1 d . . .
H18A H -0.0984 -0.2691 0.0530 0.057 Uiso 1 1 calc R . .
H18B H -0.0362 -0.2040 0.0165 0.057 Uiso 1 1 calc R . .
C21 C 0.1746(12) -0.0236(7) -0.1795(6) 0.035(4) Uani 1 1 d . . .
H21A H 0.1111 0.0063 -0.1620 0.042 Uiso 1 1 calc R . .
H21B H 0.1846 -0.0717 -0.1536 0.042 Uiso 1 1 calc R . .
S22 S 0.1121(4) -0.0422(3) -0.27530(19) 0.0590(14) Uani 1 1 d . . .
C23 C -0.0181(16) -0.1126(12) -0.2693(9) 0.103(9) Uani 1 1 d . . .
H23A H -0.0498 -0.1356 -0.3169 0.123 Uiso 1 1 calc R . .
H23B H 0.0203 -0.1528 -0.2359 0.123 Uiso 1 1 calc R . .
C24 C -0.1211(19) -0.0836(11) -0.2469(9) 0.101(8) Uani 1 1 d . . .
H24A H -0.1508 -0.0381 -0.2751 0.121 Uiso 1 1 calc R . .
H24B H -0.0921 -0.0684 -0.1963 0.121 Uiso 1 1 calc R . .
C25 C -0.2352(17) -0.1378(9) -0.2539(7) 0.099(7) Uani 1 1 d . . .
H25A H -0.3019 -0.1118 -0.2356 0.119 Uiso 1 1 calc R . .
H25B H -0.2706 -0.1472 -0.3054 0.119 Uiso 1 1 calc R . .
C26 C -0.2108(14) -0.2124(7) -0.2168(6) 0.045(5) Uani 1 1 d . . .
H26A H -0.1452 -0.2400 -0.2344 0.054 Uiso 1 1 calc R . .
H26B H -0.2899 -0.2424 -0.2271 0.054 Uiso 1 1 calc R . .
S27 S -0.1569(4) -0.19718(19) -0.12076(19) 0.0411(12) Uani 1 1 d . . .
C28 C -0.1414(12) -0.2983(6) -0.0857(7) 0.035(4) Uani 1 1 d . . .
H28A H -0.2156 -0.3109 -0.0661 0.042 Uiso 1 1 calc R . .
H28B H -0.1402 -0.3331 -0.1255 0.042 Uiso 1 1 calc R . .
C31 C 0.4047(13) -0.0290(7) -0.1911(6) 0.038(4) Uani 1 1 d . . .
H31A H 0.4869 -0.0021 -0.1813 0.045 Uiso 1 1 calc R . .
H31B H 0.3743 -0.0340 -0.2435 0.045 Uiso 1 1 calc R . .
S32 S 0.4286(4) -0.12200(19) -0.15066(18) 0.0440(12) Uani 1 1 d . . .
C33 C 0.4046(14) -0.1838(6) -0.2287(6) 0.051(5) Uani 1 1 d . . .
H33A H 0.3232 -0.1712 -0.2625 0.062 Uiso 1 1 calc R . .
H33B H 0.4741 -0.1761 -0.2535 0.062 Uiso 1 1 calc R . .
C34 C 0.4025(18) -0.2670(8) -0.2056(8) 0.080(6) Uiso 1 1 d D . .
H34A H 0.4047 -0.3008 -0.2460 0.096 Uiso 1 1 calc R . .
H34B H 0.4759 -0.2784 -0.1655 0.096 Uiso 1 1 calc R . .
C35 C 0.280(2) -0.2748(12) -0.1831(12) 0.157(11) Uiso 1 1 d D . .
H35A H 0.2734 -0.2309 -0.1529 0.188 Uiso 1 1 calc R . .
H35B H 0.2108 -0.2697 -0.2269 0.188 Uiso 1 1 calc R . .
C36 C 0.251(3) -0.3369(15) -0.1471(13) 0.262(16) Uani 1 1 d D . .
H36A H 0.3122 -0.3367 -0.1000 0.314 Uiso 1 1 calc R . .
H36B H 0.2724 -0.3808 -0.1732 0.314 Uiso 1 1 calc R . .
S37 S 0.1054(5) -0.3554(3) -0.1306(2) 0.0981(18) Uani 1 1 d . . .
C38 C 0.1019(13) -0.2940(7) -0.0564(7) 0.041(4) Uani 1 1 d . . .
H38A H 0.1782 -0.3029 -0.0175 0.049 Uiso 1 1 calc R . .
H38B H 0.1041 -0.2415 -0.0720 0.049 Uiso 1 1 calc R . .
C4 C -0.0199(15) -0.3069(8) -0.0280(7) 0.034(4) Uani 1 1 d . . .
C5 C -0.0227(13) -0.3906(7) -0.0003(6) 0.055(5) Uani 1 1 d . . .
H5A H 0.0541 -0.4002 0.0372 0.082 Uiso 1 1 calc R . .
H5B H -0.0260 -0.4252 -0.0400 0.082 Uiso 1 1 calc R . .
H5C H -0.0980 -0.3977 0.0190 0.082 Uiso 1 1 calc R . .
O40 O 0.4001(9) 0.2637(4) 0.0281(4) 0.051(3) Uani 1 1 d . . .
O41 O 0.5197(11) 0.2007(6) -0.0484(6) 0.077(4) Uani 1 1 d . . .
O42 O 0.3049(11) 0.2396(6) -0.0966(5) 0.081(4) Uani 1 1 d . . .
S43 S 0.4210(5) 0.2558(2) -0.0445(2) 0.0474(14) Uani 1 1 d . . .
C51 C 0.4745(15) 0.3431(7) -0.0657(6) 0.038(4) Uani 1 1 d . . .
C52 C 0.4006(16) 0.4046(9) -0.0656(7) 0.058(5) Uani 1 1 d . . .
H52 H 0.3222 0.3989 -0.0520 0.070 Uiso 1 1 calc R . .
C53 C 0.4341(15) 0.4752(8) -0.0843(7) 0.042(4) Uani 1 1 d . . .
H53 H 0.3773 0.5157 -0.0849 0.050 Uiso 1 1 calc R . .
C54 C 0.5533(16) 0.4878(8) -0.1028(7) 0.036(4) Uani 1 1 d . . .
C55 C 0.6239(16) 0.4256(9) -0.1027(7) 0.058(6) Uani 1 1 d . . .
H55 H 0.7020 0.4314 -0.1164 0.069 Uiso 1 1 calc R . .
C56 C 0.5936(13) 0.3544(9) -0.0845(6) 0.048(4) Uani 1 1 d . . .
H56 H 0.6505 0.3140 -0.0844 0.057 Uiso 1 1 calc R . .
C57 C 0.5916(14) 0.5635(7) -0.1259(6) 0.055(5) Uani 1 1 d . . .
H57A H 0.6783 0.5752 -0.0994 0.082 Uiso 1 1 calc R . .
H57B H 0.5330 0.6016 -0.1161 0.082 Uiso 1 1 calc R . .
H57C H 0.5881 0.5626 -0.1771 0.082 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'
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'
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
_geom_angle_publ_flag
O40 Ag1 S32 94.1(2) . 3_655 ?
O40 Ag1 S27 94.6(2) . 3 ?
S32 Ag1 S27 127.41(12) 3_655 3 ?
O40 Ag1 S12 106.3(2) . . ?
S32 Ag1 S12 122.64(13) 3_655 . ?
S27 Ag1 S12 104.07(13) 3 . ?
O1 C2 C3 113.1(13) . . ?
C2 C3 C11 111.9(10) . . ?
C2 C3 C21 108.5(12) . . ?
C11 C3 C21 113.0(11) . . ?
C2 C3 C31 106.3(11) . . ?
C11 C3 C31 108.5(11) . . ?
C21 C3 C31 108.3(10) . . ?
C3 C11 S12 115.6(10) . . ?
C11 S12 C13 101.4(7) . . ?
C11 S12 Ag1 112.5(5) . . ?
C13 S12 Ag1 107.5(5) . . ?
C14 C13 S12 117.1(11) . . ?
C13 C14 C15 115.7(12) . . ?
C16 C15 C14 113.6(12) . . ?
C15 C16 S17 114.6(10) . . ?
C16 S17 C18 102.4(6) . . ?
C4 C18 S17 119.5(10) . . ?
C3 C21 S22 114.7(9) . . ?
C21 S22 C23 99.2(7) . . ?
C24 C23 S22 115.3(16) . . ?
C23 C24 C25 114.8(18) . . ?
C26 C25 C24 117.8(15) . . ?
C25 C26 S27 109.1(9) . . ?
C26 S27 C28 101.3(6) . . ?
C26 S27 Ag1 107.2(5) . 3 ?
C28 S27 Ag1 104.0(4) . 3 ?
C4 C28 S27 110.0(9) . . ?
C3 C31 S32 111.6(9) . . ?
C31 S32 C33 102.7(5) . . ?
C31 S32 Ag1 113.6(5) . 3_655 ?
C33 S32 Ag1 107.2(5) . 3_655 ?
C34 C33 S32 110.6(9) . . ?
C35 C34 C33 104.2(15) . . ?
C36 C35 C34 123(2) . . ?
C35 C36 S37 125(2) . . ?
C36 S37 C38 102.8(10) . . ?
C4 C38 S37 111.4(10) . . ?
C28 C4 C18 110.3(12) . . ?
C28 C4 C38 112.6(11) . . ?
C18 C4 C38 111.5(12) . . ?
C28 C4 C5 105.0(12) . . ?
C18 C4 C5 107.0(10) . . ?
C38 C4 C5 110.0(12) . . ?
S43 O40 Ag1 112.5(4) . . ?
O42 S43 O41 110.6(7) . . ?
O42 S43 O40 112.2(6) . . ?
O41 S43 O40 112.9(6) . . ?
O42 S43 C51 107.4(7) . . ?
O41 S43 C51 107.7(7) . . ?
O40 S43 C51 105.6(6) . . ?
C52 C51 C56 116.7(14) . . ?
C52 C51 S43 119.8(13) . . ?
C56 C51 S43 123.6(12) . . ?
C51 C52 C53 123.3(16) . . ?
C52 C53 C54 120.9(15) . . ?
C55 C54 C53 114.3(14) . . ?
C55 C54 C57 123.1(16) . . ?
C53 C54 C57 122.5(14) . . ?
C54 C55 C56 126.5(17) . . ?
C55 C56 C51 118.4(15) . . ?
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
Ag1 O40 2.438(8) . ?
Ag1 S32 2.511(4) 3_655 ?
Ag1 S27 2.552(4) 3 ?
Ag1 S12 2.563(4) . ?
O1 C2 1.421(15) . ?
C2 C3 1.501(15) . ?
C3 C11 1.528(14) . ?
C3 C21 1.539(16) . ?
C3 C31 1.579(15) . ?
C11 S12 1.790(13) . ?
S12 C13 1.812(13) . ?
C13 C14 1.445(15) . ?
C14 C15 1.519(16) . ?
C15 C16 1.508(15) . ?
C16 S17 1.791(12) . ?
S17 C18 1.808(12) . ?
C18 C4 1.517(16) . ?
C21 S22 1.823(10) . ?
S22 C23 1.896(19) . ?
C23 C24 1.37(2) . ?
C24 C25 1.535(19) . ?
C25 C26 1.495(16) . ?
C26 S27 1.807(11) . ?
S27 C28 1.908(11) . ?
S27 Ag1 2.552(4) 3 ?
C28 C4 1.502(16) . ?
C31 S32 1.814(12) . ?
S32 C33 1.818(11) . ?
S32 Ag1 2.511(4) 3_655 ?
C33 C34 1.543(16) . ?
C34 C35 1.481(14) . ?
C35 C36 1.372(14) . ?
C36 S37 1.69(2) . ?
S37 C38 1.793(12) . ?
C38 C4 1.543(17) . ?
C4 C5 1.577(15) . ?
O40 S43 1.460(8) . ?
O41 S43 1.455(10) . ?
O42 S43 1.427(10) . ?
S43 C51 1.731(13) . ?
C51 C52 1.348(18) . ?
C51 C56 1.418(17) . ?
C52 C53 1.373(16) . ?
C53 C54 1.420(19) . ?
C54 C55 1.336(17) . ?
C54 C57 1.500(15) . ?
C55 C56 1.369(17) . ?
