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#$Date: 2016-03-26 02:12:40 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180128 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/26/7102680.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_7102680
loop_
_publ_author_name
'Turner, David R'
'Spencer, Elinor C'
'Howard, Judith A K'
'Tocher, Derek A'
'Steed, Jonathan W'
_publ_section_title
;
 A modular, self-assembled, separated ion pair binding system.
;
_journal_issue                   12
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              1352
_journal_page_last               1353
_journal_paper_doi               10.1039/b402882a
_journal_year                    2004
_chemical_formula_sum            'C52 H52 Ag2 N12 O8 S'
_chemical_formula_weight         1220.86
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   17.4146(6)
_cell_length_b                   17.4146(6)
_cell_length_c                   8.2655(6)
_cell_measurement_temperature    150(2)
_cell_volume                     2506.7(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker SMART APEX diffractometer'
_diffrn_measurement_method       'ω rotation with narrow frames'
_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  0.0299
_diffrn_reflns_av_sigmaI/netI    0.0210
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            21760
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.65
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.892
_exptl_absorpt_correction_T_max  0.9321
_exptl_absorpt_correction_T_min  0.7634
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.618
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1244
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.500
_refine_diff_density_min         -0.575
_refine_diff_density_rms         0.058
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.01(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     170
_refine_ls_number_reflns         3055
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0329
_refine_ls_R_factor_gt           0.0307
_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)+(0.0406P)²+0.9264P] where P==(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0749
_refine_ls_wR_factor_ref         0.0761
_reflns_number_gt                2908
_reflns_number_total             3055
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            b402882a.txt
_cod_data_source_block           str0192
_cod_original_sg_symbol_H-M      P-42(1)c
_cod_database_code               7102680
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_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
Ag1 Ag 1.0000 0.5000 0.18502(3) 0.04582(10) Uani 1 2 d S
O1 O 0.81794(9) 0.52835(11) 0.6562(2) 0.0334(4) Uani 1 1 d .
N1 N 0.88337(10) 0.47125(13) 0.1971(3) 0.0318(4) Uani 1 1 d .
N2 N 0.72157(9) 0.49781(13) 0.4782(2) 0.0247(3) Uani 1 1 d .
H2B H 0.6714 0.4961 0.4661 0.030 Uiso 1 1 calc R
N3 N 0.69118(10) 0.54412(11) 0.7265(2) 0.0242(4) Uani 1 1 d .
H3B H 0.6442 0.5385 0.6889 0.029 Uiso 1 1 calc R
C1 C 0.85025(15) 0.42663(18) 0.0860(3) 0.0401(6) Uani 1 1 d .
H1A H 0.8796 0.4096 -0.0039 0.048 Uiso 1 1 calc R
C2 C 0.77376(16) 0.40450(17) 0.0986(4) 0.0403(6) Uani 1 1 d .
H2A H 0.7506 0.3737 0.0173 0.048 Uiso 1 1 calc R
C3 C 0.73224(13) 0.42806(15) 0.2310(3) 0.0309(5) Uani 1 1 d .
H3A H 0.6802 0.4128 0.2425 0.037 Uiso 1 1 calc R
C4 C 0.76602(12) 0.47392(13) 0.3475(3) 0.0228(4) Uani 1 1 d .
C5 C 0.84240(11) 0.49548(15) 0.3251(3) 0.0265(4) Uani 1 1 d .
H5A H 0.8661 0.5282 0.4024 0.032 Uiso 1 1 calc R
C6 C 0.74901(12) 0.52397(13) 0.6249(3) 0.0240(4) Uani 1 1 d .
C7 C 0.69766(12) 0.57318(12) 0.8863(3) 0.0231(4) Uani 1 1 d .
C8 C 0.76460(13) 0.60378(14) 0.9522(3) 0.0275(5) Uani 1 1 d .
H8A H 0.8114 0.6020 0.8932 0.033 Uiso 1 1 calc R
C9 C 0.76241(14) 0.63684(14) 1.1047(3) 0.0300(5) Uani 1 1 d .
H9A H 0.8080 0.6587 1.1479 0.036 Uiso 1 1 calc R
C10 C 0.69525(13) 0.63898(13) 1.1969(3) 0.0267(5) Uani 1 1 d .
C11 C 0.63037(13) 0.60448(13) 1.1321(3) 0.0273(5) Uani 1 1 d .
H11A H 0.5845 0.6029 1.1941 0.033 Uiso 1 1 calc R
C12 C 0.63108(12) 0.57236(13) 0.9792(3) 0.0251(5) Uani 1 1 d .
H12A H 0.5857 0.5495 0.9372 0.030 Uiso 1 1 calc R
C13 C 0.69192(17) 0.67908(17) 1.3592(3) 0.0393(6) Uani 1 1 d .
H13A H 0.6401 0.6744 1.4042 0.059 Uiso 1 1 calc R
H13B H 0.7046 0.7335 1.3452 0.059 Uiso 1 1 calc R
H13C H 0.7289 0.6553 1.4332 0.059 Uiso 1 1 calc R
S1 S 0.0000 0.0000 0.0000 0.01705(17) Uani 1 4 d S
O2 O 0.05745(9) 0.03994(9) 0.1012(2) 0.0284(4) 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'
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'
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
N1 Ag1 N1 174.55(12) 2_765 .
C1 N1 C5 119.7(2) . .
C1 N1 Ag1 121.73(17) . .
C5 N1 Ag1 118.50(16) . .
C6 N2 C4 125.99(17) . .
C6 N3 C7 127.53(19) . .
N1 C1 C2 121.6(2) . .
C3 C2 C1 118.8(2) . .
C2 C3 C4 120.2(2) . .
C3 C4 N2 118.4(2) . .
C3 C4 C5 118.0(2) . .
N2 C4 C5 123.5(2) . .
N1 C5 C4 121.7(2) . .
O1 C6 N3 125.3(2) . .
O1 C6 N2 122.8(2) . .
N3 C6 N2 111.84(18) . .
C12 C7 C8 119.1(2) . .
C12 C7 N3 116.3(2) . .
C8 C7 N3 124.5(2) . .
C9 C8 C7 119.4(2) . .
C8 C9 C10 122.0(2) . .
C11 C10 C9 117.4(2) . .
C11 C10 C13 120.7(2) . .
C9 C10 C13 121.9(2) . .
C12 C11 C10 121.4(2) . .
C11 C12 C7 120.5(2) . .
O2 S1 O2 111.08(14) . 2
O2 S1 O2 108.67(7) . 3
O2 S1 O2 108.67(7) 2 3
O2 S1 O2 108.67(7) . 4
O2 S1 O2 108.67(7) 2 4
O2 S1 O2 111.08(14) 3 4
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ag1 N1 2.0941(19) 2_765
Ag1 N1 2.0941(19) .
O1 C6 1.230(3) .
N1 C1 1.334(4) .
N1 C5 1.344(3) .
N2 C6 1.381(3) .
N2 C4 1.393(3) .
N3 C6 1.357(3) .
N3 C7 1.419(3) .
C1 C2 1.391(4) .
C2 C3 1.374(4) .
C3 C4 1.382(3) .
C4 C5 1.394(3) .
C7 C12 1.390(3) .
C7 C8 1.393(3) .
C8 C9 1.386(4) .
C9 C10 1.396(3) .
C10 C11 1.387(3) .
C10 C13 1.514(4) .
C11 C12 1.382(3) .
S1 O2 1.4778(15) .
S1 O2 1.4778(15) 2
S1 O2 1.4778(15) 3
S1 O2 1.4778(15) 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
N1 Ag1 N1 C1 -147.1(2) 2_765
N1 Ag1 N1 C5 29.42(18) 2_765
C5 N1 C1 C2 0.3(4) .
Ag1 N1 C1 C2 176.7(2) .
N1 C1 C2 C3 -1.5(5) .
C1 C2 C3 C4 1.0(4) .
C2 C3 C4 N2 178.8(2) .
C2 C3 C4 C5 0.5(4) .
C6 N2 C4 C3 160.3(2) .
C6 N2 C4 C5 -21.6(4) .
C1 N1 C5 C4 1.4(4) .
Ag1 N1 C5 C4 -175.23(17) .
C3 C4 C5 N1 -1.7(3) .
N2 C4 C5 N1 -179.9(2) .
C7 N3 C6 O1 -0.5(4) .
C7 N3 C6 N2 180.0(2) .
C4 N2 C6 O1 -0.6(4) .
C4 N2 C6 N3 179.0(2) .
C6 N3 C7 C12 -165.2(2) .
C6 N3 C7 C8 16.8(3) .
C12 C7 C8 C9 -3.8(3) .
N3 C7 C8 C9 174.2(2) .
C7 C8 C9 C10 1.5(3) .
C8 C9 C10 C11 1.9(3) .
C8 C9 C10 C13 -176.5(2) .
C9 C10 C11 C12 -2.9(3) .
C13 C10 C11 C12 175.4(2) .
C10 C11 C12 C7 0.6(3) .
C8 C7 C12 C11 2.8(3) .
N3 C7 C12 C11 -175.4(2) .
