#------------------------------------------------------------------------------
#$Date: 2016-03-22 12:28:27 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178951 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/80/4118039.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_4118039
loop_
_publ_author_name
'Irene Bassanetti'
'Francesco Mezzadri'
'Angiolina Comotti'
'Piero Sozzani'
'Marcello Gennari'
'Gianluca Calestani'
'Luciano Marchiò'
_publ_section_title
;
 Influence of Anions in Silver Supramolecular Frameworks: Structural
 Characteristics and Sorption Properties.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9142
_journal_page_last               9145
_journal_paper_doi               10.1021/ja303940d
_journal_volume                  134
_journal_year                    2012
_chemical_formula_moiety
'C138 H144 Ag6 N30 O18 S6, 12(C H2 Cl2), 2(C6 H14)'
_chemical_formula_sum            'C162 H196 Ag6 Cl24 N30 O18 S6'
_chemical_formula_weight         4541.87
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   29.821(5)
_cell_length_b                   29.821(5)
_cell_length_c                   20.416(3)
_cell_measurement_reflns_used    17006
_cell_measurement_temperature    190(2)
_cell_measurement_theta_max      27.07
_cell_measurement_theta_min      1.27
_cell_volume                     15723(4)
_computing_cell_refinement       Saint
_computing_data_collection       Smart
_computing_data_reduction        Saint
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    Sir2004
_diffrn_ambient_temperature      190(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker Smart 1000 CCD'
_diffrn_measurement_method       'theta & omega scan'
_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  0.0571
_diffrn_reflns_av_sigmaI/netI    0.0461
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            56680
_diffrn_reflns_theta_full        27.07
_diffrn_reflns_theta_max         27.07
_diffrn_reflns_theta_min         1.27
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    0.977
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.753
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.439
_exptl_crystal_description       prism
_exptl_crystal_F_000             6924
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.16
_platon_squeeze_details
;
;
_refine_diff_density_max         0.695
_refine_diff_density_min         -0.318
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     303
_refine_ls_number_reflns         7668
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0889
_refine_ls_R_factor_gt           0.0464
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0547P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1067
_refine_ls_wR_factor_ref         0.1165
_reflns_number_gt                4011
_reflns_number_total             7668
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja303940d_si_005.cif
_cod_data_source_block           ib131
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4118039
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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
Ag Ag 0.256822(11) 0.012300(10) 0.455503(15) 0.07327(13) Uani 1 1 d .
S13 S 0.24185(3) 0.17318(3) 0.56873(4) 0.0582(2) Uani 1 1 d .
N14 N 0.29847(15) -0.05789(15) 0.4969(2) 0.0906(11) Uani 1 1 d .
N21 N 0.26623(10) 0.07104(9) 0.53945(13) 0.0563(6) Uani 1 1 d .
N11 N 0.30252(10) 0.12056(10) 0.51924(13) 0.0561(6) Uani 1 1 d .
O14 O 0.26378(12) -0.05517(11) 0.52637(15) 0.0974(9) Uani 1 1 d .
C73 C 0.20874(13) 0.13529(12) 0.49835(16) 0.0561(8) Uani 1 1 d .
C23 C 0.23545(12) 0.12333(12) 0.45154(16) 0.0558(8) Uani 1 1 d .
C31 C 0.34029(12) 0.14519(13) 0.56483(17) 0.0599(9) Uani 1 1 d .
N12 N 0.31529(11) 0.13038(11) 0.40330(14) 0.0669(8) Uani 1 1 d .
N22 N 0.30765(10) 0.08163(11) 0.39302(14) 0.0665(7) Uani 1 1 d .
C13 C 0.29278(13) 0.14118(12) 0.46021(16) 0.0604(8) Uani 1 1 d .
H13 H 0.3108 0.1789 0.4653 0.073 Uiso 1 1 calc R
C83 C 0.19899(12) 0.13967(13) 0.63389(16) 0.0592(8) Uani 1 1 d .
C133 C 0.19244(13) 0.16785(15) 0.68285(18) 0.0682(9) Uani 1 1 d .
H133 H 0.2080 0.2037 0.6793 0.082 Uiso 1 1 calc R
C33 C 0.20881(14) 0.09680(13) 0.39649(17) 0.0666(9) Uani 1 1 d .
H33 H 0.2262 0.0898 0.3639 0.080 Uiso 1 1 calc R
C63 C 0.15694(14) 0.11927(14) 0.48918(18) 0.0676(9) Uani 1 1 d .
H63 H 0.1394 0.1274 0.5203 0.081 Uiso 1 1 calc R
C41 C 0.25210(14) 0.01705(13) 0.63601(19) 0.0740(10) Uani 1 1 d .
H41A H 0.2168 -0.0005 0.6211 0.111 Uiso 1 1 calc R
H41B H 0.2531 0.0251 0.6817 0.111 Uiso 1 1 calc R
H41C H 0.2667 -0.0049 0.6297 0.111 Uiso 1 1 calc R
C43 C 0.15730(15) 0.08049(14) 0.38838(19) 0.0760(10) Uani 1 1 d .
H43 H 0.1400 0.0618 0.3512 0.091 Uiso 1 1 calc R
C11 C 0.28268(13) 0.06608(13) 0.59787(17) 0.0613(9) Uani 1 1 d .
C51 C 0.38350(13) 0.19929(13) 0.55573(19) 0.0787(11) Uani 1 1 d .
H51A H 0.4013 0.2016 0.5156 0.118 Uiso 1 1 calc R
H51B H 0.4072 0.2087 0.5918 0.118 Uiso 1 1 calc R
H51C H 0.3698 0.2224 0.5539 0.118 Uiso 1 1 calc R
C12 C 0.32949(16) 0.08332(16) 0.3360(2) 0.0829(11) Uani 1 1 d .
C21 C 0.32858(14) 0.11104(14) 0.61493(18) 0.0687(9) Uani 1 1 d .
H21 H 0.3475 0.1165 0.6533 0.082 Uiso 1 1 calc R
C53 C 0.13131(15) 0.09152(15) 0.43468(19) 0.0755(10) Uani 1 1 d .
H53 H 0.0963 0.0802 0.4293 0.091 Uiso 1 1 calc R
C93 C 0.17600(14) 0.08633(14) 0.63950(19) 0.0742(10) Uani 1 1 d .
H93 H 0.1807 0.0673 0.6069 0.089 Uiso 1 1 calc R
O34 O 0.31242(13) -0.08742(13) 0.5164(2) 0.1341(14) Uani 1 1 d .
C52 C 0.3549(2) 0.21787(18) 0.3511(3) 0.137(2) Uani 1 1 d .
H52A H 0.3778 0.2362 0.3867 0.206 Uiso 1 1 calc R
H52B H 0.3239 0.2199 0.3551 0.206 Uiso 1 1 calc R
H52C H 0.3716 0.2331 0.3103 0.206 Uiso 1 1 calc R
C22 C 0.35108(18) 0.13289(19) 0.3098(2) 0.1047(15) Uani 1 1 d .
H22 H 0.3689 0.1442 0.2703 0.126 Uiso 1 1 calc R
O24 O 0.31709(16) -0.03000(18) 0.4485(2) 0.1577(17) Uani 1 1 d .
C123 C 0.16268(16) 0.14270(19) 0.7370(2) 0.0863(12) Uani 1 1 d .
H123 H 0.1587 0.1618 0.7703 0.104 Uiso 1 1 calc R
C103 C 0.14574(17) 0.06127(17) 0.6943(2) 0.0966(13) Uani 1 1 d .
H103 H 0.1302 0.0255 0.6986 0.116 Uiso 1 1 calc R
C113 C 0.13930(17) 0.0906(2) 0.7421(2) 0.0991(14) Uani 1 1 d .
H113 H 0.1185 0.0742 0.7782 0.119 Uiso 1 1 calc R
C32 C 0.34118(17) 0.16185(17) 0.3528(2) 0.0908(12) Uani 1 1 d .
C42 C 0.32996(19) 0.03696(18) 0.3095(2) 0.1147(16) Uani 1 1 d .
H42A H 0.3213 0.0119 0.3438 0.172 Uiso 1 1 calc R
H42B H 0.3638 0.0471 0.2930 0.172 Uiso 1 1 calc R
H42C H 0.3051 0.0221 0.2748 0.172 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'
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'
Cl Cl 0.1484 0.1585 '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
N22 Ag N21 87.38(10) . .
N22 Ag S13 131.47(8) . 11_556
N21 Ag S13 123.32(6) . 11_556
N22 Ag O14 139.25(10) . .
N21 Ag O14 98.38(10) . .
S13 Ag O14 77.75(7) 11_556 .
C83 S13 C73 103.46(15) . .
C83 S13 Ag 111.45(11) . 12_556
C73 S13 Ag 101.72(10) . 12_556
O34 N14 O24 123.4(5) . .
O34 N14 O14 119.4(5) . .
O24 N14 O14 117.2(4) . .
C11 N21 N11 104.5(3) . .
C11 N21 Ag 118.9(2) . .
N11 N21 Ag 108.27(18) . .
C31 N11 N21 111.5(3) . .
C31 N11 C13 129.0(3) . .
N21 N11 C13 119.0(2) . .
N14 O14 Ag 100.1(3) . .
C63 C73 C23 120.0(3) . .
C63 C73 S13 119.7(3) . .
C23 C73 S13 120.3(2) . .
C33 C23 C73 117.8(3) . .
C33 C23 C13 121.3(3) . .
C73 C23 C13 120.9(3) . .
N11 C31 C21 106.1(3) . .
N11 C31 C51 122.3(3) . .
C21 C31 C51 131.6(3) . .
C32 N12 N22 110.8(3) . .
C32 N12 C13 128.6(3) . .
N22 N12 C13 120.4(3) . .
C12 N22 N12 106.1(3) . .
C12 N22 Ag 128.8(3) . .
N12 N22 Ag 124.5(2) . .
N11 C13 N12 111.0(3) . .
N11 C13 C23 112.1(3) . .
N12 C13 C23 113.0(3) . .
N11 C13 H13 106.8 . .
N12 C13 H13 106.8 . .
C23 C13 H13 106.8 . .
C133 C83 C93 119.9(3) . .
C133 C83 S13 118.9(3) . .
C93 C83 S13 120.9(3) . .
C83 C133 C123 119.8(4) . .
C83 C133 H133 120.1 . .
C123 C133 H133 120.1 . .
C43 C33 C23 121.7(3) . .
C43 C33 H33 119.1 . .
C23 C33 H33 119.1 . .
C53 C63 C73 120.6(3) . .
C53 C63 H63 119.7 . .
C73 C63 H63 119.7 . .
C11 C41 H41A 109.5 . .
C11 C41 H41B 109.5 . .
H41A C41 H41B 109.5 . .
C11 C41 H41C 109.5 . .
H41A C41 H41C 109.5 . .
H41B C41 H41C 109.5 . .
C53 C43 C33 120.2(3) . .
C53 C43 H43 119.9 . .
C33 C43 H43 119.9 . .
N21 C11 C21 110.9(3) . .
N21 C11 C41 119.9(3) . .
C21 C11 C41 129.2(3) . .
C31 C51 H51A 109.5 . .
C31 C51 H51B 109.5 . .
H51A C51 H51B 109.5 . .
C31 C51 H51C 109.5 . .
H51A C51 H51C 109.5 . .
H51B C51 H51C 109.5 . .
N22 C12 C22 109.7(4) . .
N22 C12 C42 121.1(4) . .
C22 C12 C42 129.2(4) . .
C31 C21 C11 107.0(3) . .
C31 C21 H21 126.5 . .
C11 C21 H21 126.5 . .
C43 C53 C63 119.8(4) . .
C43 C53 H53 120.1 . .
C63 C53 H53 120.1 . .
C83 C93 C103 119.8(4) . .
C83 C93 H93 120.1 . .
C103 C93 H93 120.1 . .
C32 C52 H52A 109.5 . .
C32 C52 H52B 109.5 . .
H52A C52 H52B 109.5 . .
C32 C52 H52C 109.5 . .
H52A C52 H52C 109.5 . .
H52B C52 H52C 109.5 . .
C32 C22 C12 107.1(4) . .
C32 C22 H22 126.5 . .
C12 C22 H22 126.5 . .
C113 C123 C133 120.5(4) . .
C113 C123 H123 119.8 . .
C133 C123 H123 119.7 . .
C113 C103 C93 118.8(4) . .
C113 C103 H103 120.6 . .
C93 C103 H103 120.6 . .
C123 C113 C103 121.1(4) . .
C123 C113 H113 119.4 . .
C103 C113 H113 119.4 . .
N12 C32 C22 106.4(4) . .
N12 C32 C52 122.2(4) . .
C22 C32 C52 131.4(4) . .
C12 C42 H42A 109.5 . .
C12 C42 H42B 109.5 . .
H42A C42 H42B 109.5 . .
C12 C42 H42C 109.5 . .
H42A C42 H42C 109.5 . .
H42B C42 H42C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ag N22 2.251(3) .
Ag N21 2.365(3) .
Ag S13 2.5046(9) 11_556
Ag O14 2.569(3) .
S13 C83 1.768(3) .
S13 C73 1.789(3) .
S13 Ag 2.5046(9) 12_556
N14 O34 1.214(4) .
N14 O24 1.231(5) .
N14 O14 1.234(4) .
N21 C11 1.326(4) .
N21 N11 1.387(3) .
N11 C31 1.359(4) .
N11 C13 1.447(4) .
C73 C63 1.383(4) .
C73 C23 1.400(4) .
C23 C33 1.375(4) .
C23 C13 1.526(4) .
C31 C21 1.360(5) .
C31 C51 1.490(5) .
N12 C32 1.348(4) .
N12 N22 1.370(4) .
N12 C13 1.456(4) .
N22 C12 1.322(4) .
C13 H13 0.9800 .
C83 C133 1.381(4) .
C83 C93 1.387(5) .
C133 C123 1.382(5) .
C133 H133 0.9300 .
C33 C43 1.370(5) .
C33 H33 0.9300 .
C63 C53 1.369(5) .
C63 H63 0.9300 .
C41 C11 1.497(5) .
C41 H41A 0.9600 .
C41 H41B 0.9600 .
C41 H41C 0.9600 .
C43 C53 1.363(5) .
C43 H43 0.9300 .
C11 C21 1.399(5) .
C51 H51A 0.9600 .
C51 H51B 0.9600 .
C51 H51C 0.9600 .
C12 C22 1.391(6) .
C12 C42 1.491(5) .
C21 H21 0.9300 .
C53 H53 0.9300 .
C93 C103 1.396(5) .
C93 H93 0.9300 .
C52 C32 1.509(6) .
C52 H52A 0.9600 .
C52 H52B 0.9600 .
C52 H52C 0.9600 .
C22 C32 1.363(6) .
C22 H22 0.9300 .
C123 C113 1.351(6) .
C123 H123 0.9300 .
C103 C113 1.388(6) .
C103 H103 0.9300 .
C113 H113 0.9300 .
C42 H42A 0.9600 .
C42 H42B 0.9600 .
C42 H42C 0.9600 .
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 -0.022 -0.017 -0.001 6287.2 1824.7
