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#$Date: 2016-03-22 11:39:11 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178909 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/38/4113895.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_4113895
loop_
_publ_author_name
'Cheng-Yong Su'
'Yue-Peng Cai'
'Chun-Long Chen'
'Mark D. Smith'
'Wolfgang Kaim'
'Hans-Conrad zur Loye'
_publ_section_title
;
 Ligand-Directed Molecular Architectures: Self-Assembly of Two-Dimensional
 Rectangular Metallacycles and Three-Dimensional Trigonal or Tetragonal
 Prisms
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8595
_journal_page_last               8613
_journal_paper_doi               10.1021/ja034267k
_journal_volume                  125
_journal_year                    2003
_chemical_formula_sum            'C80 H78 Ag2 F6 N12 O6 S2'
_chemical_formula_weight         1697.40
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           176
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-P 6c'
_symmetry_space_group_name_H-M   'P 63/m'
_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            2
_cell_length_a                   14.0129(13)
_cell_length_b                   14.0129(13)
_cell_length_c                   23.119(3)
_cell_measurement_temperature    293(2)
_cell_volume                     3931.5(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.947
_diffrn_measured_fraction_theta_max 0.947
_diffrn_measurement_device_type  'Bruker CCD'
_diffrn_measurement_method       'Phi and 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  0.0534
_diffrn_reflns_av_sigmaI/netI    0.0602
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            11234
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         7.88
_exptl_absorpt_coefficient_mu    0.625
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.821
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.434
_exptl_crystal_description       Flakelet
_exptl_crystal_F_000             1740
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.376
_refine_diff_density_min         -1.226
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    geom
_refine_ls_matrix_type           full
_refine_ls_number_parameters     175
_refine_ls_number_reflns         2247
_refine_ls_number_restraints     53
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.1245
_refine_ls_R_factor_gt           0.0716
_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)+(0.1251P)²+6.6217P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1935
_refine_ls_wR_factor_ref         0.2409
_reflns_number_gt                1329
_reflns_number_total             2247
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja034267ksi20030121_054932_04.cif
_cod_data_source_block           4
_cod_database_code               4113895
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z-1/2'
'-y, x-y, -z-1/2'
'-x+y, -x, -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 0.3333 0.6667 0.08831(2) 0.06531(14) Uani 1 3 d S
N2 N 0.0332(2) 0.6960(2) 0.09574(12) 0.0653(9) Uani 1 1 d .
N1 N 0.1740(2) 0.6695(2) 0.07878(13) 0.0648(9) Uani 1 1 d .
C2 C 0.1180(3) 0.6559(3) 0.02716(15) 0.0627(11) Uani 1 1 d .
C9 C -0.0348(2) 0.7238(3) 0.18933(17) 0.0677(11) Uani 1 1 d .
C12 C 0.0378(3) 0.8195(3) 0.21947(19) 0.0754(12) Uani 1 1 d .
C1 C 0.1206(3) 0.6931(3) 0.11734(17) 0.0650(11) Uani 1 1 d .
H1 H 0.1412 0.7066 0.1560 0.078 Uiso 1 1 calc R
C7 C 0.0306(3) 0.6726(3) 0.03732(16) 0.0696(12) Uani 1 1 d .
C10 C -0.1066(3) 0.6265(3) 0.21982(19) 0.0778(13) Uani 1 1 d .
C11 C -0.1813(4) 0.5220(4) 0.1863(3) 0.112(2) Uani 1 1 d .
H11A H -0.1706 0.5369 0.1456 0.168 Uiso 1 1 calc R
H11B H -0.2567 0.4971 0.1961 0.168 Uiso 1 1 calc R
H11C H -0.1637 0.4660 0.1961 0.168 Uiso 1 1 calc R
C3 C 0.1370(3) 0.6280(3) -0.02762(18) 0.0774(14) Uani 1 1 d .
H3 H 0.1952 0.6156 -0.0349 0.093 Uiso 1 1 calc R
C6 C -0.0434(4) 0.6629(4) -0.00695(19) 0.0877(14) Uani 1 1 d .
H6 H -0.1025 0.6742 -0.0005 0.105 Uiso 1 1 calc R
C8 C -0.0414(3) 0.7264(3) 0.1236(2) 0.0899(14) Uani 1 1 d .
H8A H -0.1163 0.6759 0.1114 0.108 Uiso 1 1 calc R
H8B H -0.0228 0.7999 0.1114 0.108 Uiso 1 1 calc R
C4 C 0.0652(4) 0.6197(4) -0.0706(2) 0.0940(18) Uani 1 1 d .
H4 H 0.0764 0.6027 -0.1080 0.113 Uiso 1 1 calc R
C5 C -0.0210(4) 0.6352(4) -0.0605(2) 0.1030(18) Uani 1 1 d .
H5 H -0.0676 0.6269 -0.0912 0.124 Uiso 1 1 calc R
C13 C 0.1178(4) 0.9241(4) 0.1869(2) 0.0977(17) Uani 1 1 d .
H13A H 0.1608 0.9816 0.2141 0.147 Uiso 1 1 calc R
H13B H 0.0770 0.9468 0.1626 0.147 Uiso 1 1 calc R
H13C H 0.1658 0.9098 0.1634 0.147 Uiso 1 1 calc R
S1 S 0.0000 1.0000 0.03905(11) 0.190(3) Uani 0.50 3 d SPU
C1W C 0.0000 1.0000 0.03905(11) 0.190(3) Uani 0.50 3 d SPD
O1 O 0.0105(4) 1.1037(3) 0.0532(2) 0.1876(18) Uani 0.50 1 d PU
F1 F 0.0105(4) 1.1037(3) 0.0532(2) 0.1876(18) Uani 0.50 1 d P
S2 S 0.3724(3) 0.7318(3) 0.2500 0.300 Uiso 0.33 2 d SPD
O2 O 0.3333 0.6667 0.19829(14) 0.209(4) Uani 1 3 d SDU
O3 O 0.4921(4) 0.7903(8) 0.2500 0.145(7) Uani 0.33 2 d SPDU
C2W C 0.3302(3) 0.8333(3) 0.2500 0.300 Uiso 0.33 2 d SPD
F2 F 0.3671(4) 0.8998(4) 0.29599(9) 0.230(6) Uani 0.33 1 d PDU
F3 F 0.2212(3) 0.7894(7) 0.2500 0.300 Uiso 0.33 2 d SPD
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'
Ag Ag -0.8971 1.1015 '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'
F F 0.0171 0.0103 '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 119.07(3) . 3_565
N1 Ag1 N1 119.07(3) . 2_665
N1 Ag1 N1 119.07(3) 3_565 2_665
N1 Ag1 O2 95.58(7) . .
N1 Ag1 O2 95.58(7) 3_565 .
N1 Ag1 O2 95.58(7) 2_665 .
C1 N2 C7 105.8(3) . .
C1 N2 C8 129.9(3) . .
C7 N2 C8 124.1(3) . .
C1 N1 C2 105.3(3) . .
C1 N1 Ag1 129.2(2) . .
C2 N1 Ag1 125.2(3) . .
C7 C2 N1 108.7(3) . .
C7 C2 C3 121.0(4) . .
N1 C2 C3 130.3(4) . .
C12 C9 C10 120.2(4) . .
C12 C9 C8 119.9(3) . .
C10 C9 C8 119.9(3) . .
C9 C12 C12 119.9(2) . 10_556
C9 C12 C13 120.5(4) . .
C12 C12 C13 119.6(3) 10_556 .
N1 C1 N2 113.6(3) . .
N1 C1 H1 123.2 . .
N2 C1 H1 123.2 . .
C2 C7 N2 106.6(3) . .
C2 C7 C6 122.1(4) . .
N2 C7 C6 131.3(4) . .
C10 C10 C9 119.9(2) 10_556 .
C10 C10 C11 120.7(3) 10_556 .
C9 C10 C11 119.4(4) . .
C10 C11 H11A 109.5 . .
C10 C11 H11B 109.5 . .
H11A C11 H11B 109.5 . .
C10 C11 H11C 109.5 . .
H11A C11 H11C 109.5 . .
H11B C11 H11C 109.5 . .
C4 C3 C2 116.5(5) . .
C4 C3 H3 121.8 . .
C2 C3 H3 121.8 . .
C5 C6 C7 114.7(5) . .
C5 C6 H6 122.7 . .
C7 C6 H6 122.7 . .
N2 C8 C9 111.9(4) . .
N2 C8 H8A 109.2 . .
C9 C8 H8A 109.2 . .
N2 C8 H8B 109.2 . .
C9 C8 H8B 109.2 . .
H8A C8 H8B 107.9 . .
C5 C4 C3 122.4(5) . .
C5 C4 H4 118.8 . .
C3 C4 H4 118.8 . .
C4 C5 C6 123.2(5) . .
C4 C5 H5 118.4 . .
C6 C5 H5 118.4 . .
C12 C13 H13A 109.5 . .
C12 C13 H13B 109.5 . .
H13A C13 H13B 109.5 . .
C12 C13 H13C 109.5 . .
H13A C13 H13C 109.5 . .
H13B C13 H13C 109.5 . .
O1 S1 F1 114.90(16) . 2_675
O1 S1 O1 114.90(16) . 2_675
F1 S1 O1 0.0(4) 2_675 2_675
O1 S1 F1 114.90(16) . 3_465
F1 S1 F1 114.90(16) 2_675 3_465
O1 S1 F1 114.90(16) 2_675 3_465
O1 S1 O1 114.90(16) . 3_465
F1 S1 O1 114.90(16) 2_675 3_465
O1 S1 O1 114.90(16) 2_675 3_465
F1 S1 O1 0.0(5) 3_465 3_465
O1 S1 C1W 103.3(2) . 7_575
F1 S1 C1W 103.3(2) 2_675 7_575
O1 S1 C1W 103.3(2) 2_675 7_575
F1 S1 C1W 103.3(2) 3_465 7_575
O1 S1 C1W 103.3(2) 3_465 7_575
O1 S1 S1 103.3(2) . 7_575
F1 S1 S1 103.3(2) 2_675 7_575
O1 S1 S1 103.3(2) 2_675 7_575
F1 S1 S1 103.3(2) 3_465 7_575
O1 S1 S1 103.3(2) 3_465 7_575
C1W S1 S1 0.0 7_575 7_575
S2 S2 S2 60.000(1) 3_565 2_665
S2 S2 O2 61.31(12) 3_565 .
S2 S2 O2 61.31(13) 2_665 .
S2 S2 O2 61.31(12) 3_565 10_556
S2 S2 O2 61.31(13) 2_665 10_556
O2 S2 O2 112.7(3) . 10_556
S2 S2 O3 95.8(7) 3_565 .
S2 S2 O3 155.8(7) 2_665 .
O2 S2 O3 108.9(3) . .
O2 S2 O3 108.9(3) 10_556 .
S2 S2 C2W 156.8(5) 3_565 .
S2 S2 C2W 96.8(5) 2_665 .
O2 S2 C2W 109.4(2) . .
O2 S2 C2W 109.4(2) 10_556 .
O3 S2 C2W 107.4(5) . .
S2 S2 O3 103.4(4) 3_565 2_665
S2 S2 O3 43.4(4) 2_665 2_665
O2 S2 O3 80.9(2) . 2_665
O2 S2 O3 80.9(2) 10_556 2_665
O3 S2 O3 160.7(4) . 2_665
C2W S2 O3 53.4(3) . 2_665
S2 O2 S2 57.4(3) . 2_665
S2 O2 S2 57.4(3) . 3_565
S2 O2 S2 57.4(3) 2_665 3_565
S2 O2 Ag1 146.34(15) . .
S2 O2 Ag1 146.34(15) 2_665 .
S2 O2 Ag1 146.34(15) 3_565 .
F3 O3 S2 143.8(10) 3_565 .
F3 O3 C2W 48.7(5) 3_565 3_565
S2 O3 C2W 95.1(6) . 3_565
F3 O3 S2 103.0(7) 3_565 3_565
S2 O3 S2 40.7(4) . 3_565
C2W O3 S2 54.3(3) 3_565 3_565
F3 C2W F2 106.1(4) . .
F3 C2W F2 106.1(4) . 10_556
F2 C2W F2 105.5(4) . 10_556
F3 C2W O3 40.7(5) . 2_665
F2 C2W O3 124.1(2) . 2_665
F2 C2W O3 124.1(2) 10_556 2_665
F3 C2W S2 113.0(5) . .
F2 C2W S2 112.8(4) . .
F2 C2W S2 112.8(4) 10_556 .
O3 C2W S2 72.3(3) 2_665 .
O3 F3 C2W 90.6(7) 2_665 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ag1 N1 2.263(3) .
Ag1 N1 2.263(3) 3_565
Ag1 N1 2.263(3) 2_665
Ag1 O2 2.543(3) .
N2 C1 1.341(5) .
N2 C7 1.386(5) .
N2 C8 1.462(6) .
N1 C1 1.308(5) .
N1 C2 1.389(5) .
C2 C7 1.376(6) .
C2 C3 1.390(6) .
C9 C12 1.398(5) .
C9 C10 1.413(5) .
C9 C8 1.523(6) .
C12 C12 1.412(9) 10_556
C12 C13 1.527(6) .
C1 H1 0.9300 .
C7 C6 1.414(6) .
C10 C10 1.395(9) 10_556
C10 C11 1.519(6) .
C11 H11A 0.9600 .
C11 H11B 0.9600 .
C11 H11C 0.9600 .
C3 C4 1.378(7) .
C3 H3 0.9300 .
C6 C5 1.380(7) .
C6 H6 0.9300 .
C8 H8A 0.9700 .
C8 H8B 0.9700 .
C4 C5 1.351(8) .
C4 H4 0.9300 .
C5 H5 0.9300 .
C13 H13A 0.9600 .
C13 H13B 0.9600 .
C13 H13C 0.9600 .
S1 O1 1.423(4) .
S1 F1 1.423(4) 2_675
S1 O1 1.423(4) 2_675
S1 F1 1.423(4) 3_465
S1 O1 1.423(4) 3_465
S1 C1W 1.806(5) 7_575
S1 S1 1.806(5) 7_575
S2 S2 1.379(7) 3_565
S2 S2 1.379(7) 2_665
S2 O2 1.436(3) .
S2 O2 1.436(3) 10_556
S2 O3 1.453(5) .
S2 C2W 1.792(7) .
S2 O3 2.102(9) 2_665
O2 S2 1.436(3) 2_665
O2 S2 1.436(3) 3_565
O3 F3 1.156(13) 3_565
O3 C2W 1.771(12) 3_565
O3 S2 2.102(9) 3_565
C2W F3 1.331(5) .
C2W F2 1.336(4) .
C2W F2 1.336(4) 10_556
C2W O3 1.771(12) 2_665
F3 O3 1.156(13) 2_665
