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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/4/11/38/4113894.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_4113894
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            'C54 H52 Ag2 F6 N8 O6 S2'
_chemical_formula_weight         1302.90
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                73.5910(10)
_cell_angle_beta                 75.0770(10)
_cell_angle_gamma                74.3250(10)
_cell_formula_units_Z            1
_cell_length_a                   9.1423(6)
_cell_length_b                   11.4306(8)
_cell_length_c                   15.1363(10)
_cell_measurement_temperature    293(2)
_cell_volume                     1432.53(17)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.937
_diffrn_measured_fraction_theta_max 0.937
_diffrn_measurement_device_type  CCD
_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  0.0144
_diffrn_reflns_av_sigmaI/netI    0.0342
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            10217
_diffrn_reflns_theta_full        30.04
_diffrn_reflns_theta_max         30.04
_diffrn_reflns_theta_min         4.03
_exptl_absorpt_coefficient_mu    0.831
_exptl_absorpt_correction_T_max  0.100
_exptl_absorpt_correction_T_min  0.635
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            Block
_exptl_crystal_density_diffrn    1.510
_exptl_crystal_description       Colorless
_exptl_crystal_F_000             660
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.944
_refine_diff_density_min         -0.868
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     365
_refine_ls_number_reflns         7860
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0760
_refine_ls_R_factor_gt           0.0544
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1140P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1644
_refine_ls_wR_factor_ref         0.1776
_reflns_number_gt                5317
_reflns_number_total             7860
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja034267ksi20030121_054932_03.cif
_cod_data_source_block           3
_cod_database_code               4113894
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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 0.86119(3) -0.23588(3) 0.579554(18) 0.06121(15) Uani 1 1 d . . .
N1 N 0.8000(4) -0.2037(3) 0.7159(2) 0.0550(8) Uani 1 1 d . . .
N2 N 0.6677(3) -0.1416(3) 0.8453(2) 0.0482(7) Uani 1 1 d . . .
N3 N 0.9634(3) -0.2901(3) 0.4519(2) 0.0505(7) Uani 1 1 d . . .
N4 N 0.9819(3) -0.3234(3) 0.31160(19) 0.0451(6) Uani 1 1 d . . .
C1 C 0.6722(4) -0.1354(4) 0.7546(2) 0.0558(9) Uani 1 1 d . . .
H1 H 0.5945 -0.0866 0.7223 0.067 Uiso 1 1 d R . .
C2 C 0.8853(4) -0.2591(3) 0.7866(2) 0.0442(7) Uani 1 1 d . . .
C3 C 1.0313(4) -0.3388(4) 0.7851(3) 0.0555(9) Uani 1 1 d . . .
H3 H 1.0874 -0.3659 0.7313 0.067 Uiso 1 1 d R . .
C4 C 1.0869(4) -0.3792(4) 0.8680(3) 0.0596(10) Uani 1 1 d . . .
H4 H 1.1842 -0.4318 0.8689 0.071 Uiso 1 1 d R . .
C5 C 1.0002(5) -0.3408(4) 0.9500(3) 0.0582(9) Uani 1 1 d . . .
H5 H 1.0414 -0.3697 1.0043 0.070 Uiso 1 1 d R . .
C6 C 0.8576(4) -0.2612(3) 0.9517(2) 0.0484(7) Uani 1 1 d . . .
H6 H 0.8010 -0.2350 1.0058 0.058 Uiso 1 1 d R . .
C7 C 0.8028(3) -0.2218(3) 0.8683(2) 0.0395(6) Uani 1 1 d . . .
C8 C 0.5487(5) -0.0786(5) 0.9109(3) 0.0682(12) Uani 1 1 d . . .
H8A H 0.5026 -0.1393 0.9619 0.082 Uiso 1 1 d R . .
H8B H 0.5993 -0.0364 0.9378 0.082 Uiso 1 1 d R . .
C9 C 0.9006(4) -0.2587(3) 0.3769(2) 0.0502(8) Uani 1 1 d . . .
H9 H 0.8093 -0.1995 0.3701 0.060 Uiso 1 1 d R . .
C10 C 1.0967(4) -0.3807(3) 0.4347(2) 0.0432(7) Uani 1 1 d . . .
C11 C 1.2078(4) -0.4454(4) 0.4879(3) 0.0557(9) Uani 1 1 d . . .
H11 H 1.2017 -0.4322 0.5468 0.067 Uiso 1 1 d R . .
C12 C 1.3273(5) -0.5320(4) 0.4512(3) 0.0633(10) Uani 1 1 d . . .
H12 H 1.4033 -0.5775 0.4858 0.076 Uiso 1 1 d R . .
C13 C 1.3387(4) -0.5534(4) 0.3646(3) 0.0574(9) Uani 1 1 d . . .
H13 H 1.4220 -0.6122 0.3423 0.069 Uiso 1 1 d R . .
C14 C 1.2295(4) -0.4909(3) 0.3088(3) 0.0483(8) Uani 1 1 d . . .
H14 H 1.2359 -0.5061 0.2505 0.058 Uiso 1 1 d R . .
C15 C 1.1094(4) -0.4035(3) 0.3467(2) 0.0397(6) Uani 1 1 d . . .
C16 C 0.9514(4) -0.3112(4) 0.2184(2) 0.0536(9) Uani 1 1 d . . .
H16A H 1.0431 -0.2964 0.1712 0.064 Uiso 1 1 d R . .
H16B H 0.9310 -0.3892 0.2163 0.064 Uiso 1 1 d R . .
C17 C 0.8162(4) -0.2073(3) 0.1948(2) 0.0420(7) Uani 1 1 d . . .
C18 C 0.6692(4) -0.2332(3) 0.2109(2) 0.0457(7) Uani 1 1 d . . .
C19 C 0.5494(4) -0.1391(4) 0.1791(3) 0.0519(9) Uani 1 1 d . . .
C20 C 0.4250(4) 0.0198(3) 0.8665(2) 0.0480(8) Uani 1 1 d . . .
C21 C 0.2822(4) -0.0093(3) 0.8741(3) 0.0545(8) Uani 1 1 d . . .
C22 C 0.8398(4) -0.0861(3) 0.1554(3) 0.0495(8) Uani 1 1 d . . .
C23 C 0.6418(6) -0.3632(4) 0.2648(4) 0.0726(12) Uani 1 1 d . . .
H23A H 0.7356 -0.4171 0.2822 0.109 Uiso 1 1 d R . .
H23B H 0.5637 -0.3559 0.3204 0.109 Uiso 1 1 d R . .
H23C H 0.6068 -0.3977 0.2251 0.109 Uiso 1 1 d R . .
C24 C 0.3889(5) -0.1662(6) 0.1949(5) 0.0904(18) Uani 1 1 d . . .
H24A H 0.3167 -0.0939 0.1696 0.136 Uiso 1 1 d R . .
H24B H 0.3982 -0.2321 0.1648 0.136 Uiso 1 1 d R . .
H24C H 0.3525 -0.1929 0.2612 0.136 Uiso 1 1 d R . .
C25 C 0.2630(8) -0.1407(5) 0.9146(5) 0.105(2) Uani 1 1 d . . .
H25A H 0.3575 -0.1933 0.9316 0.158 Uiso 1 1 d R . .
H25B H 0.2358 -0.1700 0.8687 0.158 Uiso 1 1 d R . .
H25C H 0.1816 -0.1428 0.9693 0.158 Uiso 1 1 d R . .
C26 C 0.9934(5) -0.0560(6) 0.1495(4) 0.0854(15) Uani 1 1 d . . .
H26A H 0.9871 0.0312 0.1209 0.128 Uiso 1 1 d R . .
H26B H 1.0168 -0.0739 0.2108 0.128 Uiso 1 1 d R . .
H26C H 1.0735 -0.1045 0.1113 0.128 Uiso 1 1 d R . .
S1 S -0.46040(19) 0.47637(17) 0.93837(12) 0.0715(4) Uani 0.60 1 d P . .
C27 C -0.46040(19) 0.47637(17) 0.93837(12) 0.0715(4) Uani 0.40 1 d P . .
O3 O -0.4963(5) 0.5849(3) 0.8765(2) 0.1035(13) Uani 0.60 1 d P . .
F1 F -0.4963(5) 0.5849(3) 0.8765(2) 0.1035(13) Uani 0.40 1 d P . .
O2 O -0.3093(4) 0.4310(4) 0.9369(2) 0.1011(12) Uani 0.60 1 d P . .
F2 F -0.3093(4) 0.4310(4) 0.9369(2) 0.1011(12) Uani 0.40 1 d P . .
O1 O -0.5446(6) 0.3919(4) 0.9462(3) 0.1153(14) Uani 0.60 1 d P . .
F3 F -0.5446(6) 0.3919(4) 0.9462(3) 0.1153(14) Uani 0.40 1 d P . .
S2 S 0.4446(3) -0.0428(3) 0.5159(3) 0.1043(12) Uani 0.50 1 d PD . .
C28 C 0.2939(12) -0.1263(9) 0.5469(8) 0.168(8) Uiso 0.50 1 d PD . .
O4 O 0.4153(11) 0.0744(8) 0.4499(7) 0.106(3) Uiso 0.50 1 d PD . .
O5 O 0.429(2) 0.0137(18) 0.6007(10) 0.280(11) Uiso 0.50 1 d PD . .
O6 O 0.5987(9) -0.1030(10) 0.5115(9) 0.123(4) Uiso 0.50 1 d PD . .
F6 F 0.3261(17) -0.2475(9) 0.5692(11) 0.097(4) Uiso 0.25 1 d PD A 1
F5 F 0.221(2) -0.0856(18) 0.6258(11) 0.159(7) Uiso 0.25 1 d PD A 1
F4 F 0.1922(17) -0.0849(14) 0.4904(11) 0.114(5) Uiso 0.25 1 d PD A 1
F6' F 0.316(2) -0.2321(12) 0.6109(12) 0.125(6) Uiso 0.25 1 d PD A 2
F5' F 0.1515(13) -0.0663(12) 0.5699(11) 0.104(4) Uiso 0.25 1 d PD A 2
F4' F 0.308(3) -0.154(2) 0.4646(12) 0.175(8) Uiso 0.25 1 d PD A 2
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'
F F 0.0171 0.0103 '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
N3 Ag1 N1 168.51(11) . .
C1 N1 C2 105.5(3) . .
C1 N1 Ag1 128.5(2) . .
C2 N1 Ag1 125.9(2) . .
C1 N2 C7 107.2(3) . .
C1 N2 C8 129.2(3) . .
C7 N2 C8 123.6(3) . .
C9 N3 C10 106.1(3) . .
C9 N3 Ag1 126.2(2) . .
C10 N3 Ag1 127.0(2) . .
C9 N4 C15 107.0(3) . .
C9 N4 C16 128.2(3) . .
C15 N4 C16 124.6(3) . .
N1 C1 N2 112.6(3) . .
C7 C2 N1 109.1(3) . .
C7 C2 C3 120.3(3) . .
N1 C2 C3 130.6(3) . .
C4 C3 C2 117.3(3) . .
C3 C4 C5 121.2(3) . .
C6 C5 C4 121.8(3) . .
C5 C6 C7 116.4(3) . .
N2 C7 C2 105.6(3) . .
N2 C7 C6 131.5(3) . .
C2 C7 C6 123.0(3) . .
N2 C8 C20 114.2(3) . .
N3 C9 N4 112.6(3) . .
C11 C10 N3 131.4(3) . .
C11 C10 C15 119.9(3) . .
N3 C10 C15 108.7(3) . .
C12 C11 C10 117.5(3) . .
C13 C12 C11 122.1(3) . .
C12 C13 C14 122.5(3) . .
C13 C14 C15 114.8(3) . .
C14 C15 N4 131.2(3) . .
C14 C15 C10 123.3(3) . .
N4 C15 C10 105.5(3) . .
N4 C16 C17 113.1(3) . .
C22 C17 C18 120.8(3) . .
C22 C17 C16 119.4(3) . .
C18 C17 C16 119.9(3) . .
C19 C18 C17 119.1(3) . .
C19 C18 C23 121.1(3) . .
C17 C18 C23 119.8(3) . .
C18 C19 C20 120.3(3) . 2_656
C18 C19 C24 119.8(4) . .
C20 C19 C24 119.9(4) 2_656 .
C19 C20 C21 120.5(3) 2_656 .
C19 C20 C8 120.6(4) 2_656 .
C21 C20 C8 118.9(4) . .
C22 C21 C20 119.1(3) 2_656 .
C22 C21 C25 121.5(4) 2_656 .
C20 C21 C25 119.4(4) . .
C17 C22 C21 119.8(3) . 2_656
C17 C22 C26 120.4(3) . .
C21 C22 C26 119.8(4) 2_656 .
O2 S1 O3 115.4(3) . .
O2 S1 O1 115.7(3) . .
O3 S1 O1 114.6(3) . .
O2 S1 C27 103.7(2) . 2_467
O3 S1 C27 103.0(2) . 2_467
O1 S1 C27 101.8(2) . 2_467
O2 S1 S1 103.7(2) . 2_467
O3 S1 S1 103.0(2) . 2_467
O1 S1 S1 101.8(2) . 2_467
C27 S1 S1 0.00(10) 2_467 2_467
O6 S2 O4 29.5(6) . 2_656
O6 S2 O4 115.7(7) . .
O4 S2 O4 116.9(4) 2_656 .
O6 S2 S2 65.6(5) . 2_656
O4 S2 S2 58.7(3) 2_656 2_656
O4 S2 S2 58.1(4) . 2_656
O6 S2 O5 96.6(7) . .
O4 S2 O5 67.1(7) 2_656 .
O4 S2 O5 95.9(7) . .
S2 S2 O5 74.2(8) 2_656 .
O6 S2 O6 119.4(4) . 2_656
O4 S2 O6 105.9(5) 2_656 2_656
O4 S2 O6 27.2(5) . 2_656
S2 S2 O6 53.8(3) 2_656 2_656
O5 S2 O6 68.7(7) . 2_656
O6 S2 C28 122.0(6) . .
O4 S2 C28 129.0(5) 2_656 .
O4 S2 C28 114.1(5) . .
S2 S2 C28 172.0(4) 2_656 .
O5 S2 C28 106.0(8) . .
O6 S2 C28 118.5(4) 2_656 .
O6 S2 O5 64.4(7) . 2_656
O4 S2 O5 84.6(6) 2_656 2_656
O4 S2 O5 59.0(6) . 2_656
S2 S2 O5 54.3(4) 2_656 2_656
O5 S2 O5 128.5(5) . 2_656
O6 S2 O5 80.0(6) 2_656 2_656
C28 S2 O5 124.9(6) . 2_656
F6 C28 F5' 119.4(12) . .
F6 C28 F6' 30.0(10) . .
F5' C28 F6' 107.8(10) . .
F6 C28 F4 110.3(10) . .
F5' C28 F4 55.5(9) . .
F6' C28 F4 129.3(13) . .
F6 C28 F4' 78.0(12) . .
F5' C28 F4' 107.5(11) . .
F6' C28 F4' 108.0(11) . .
F4 C28 F4' 52.9(10) . .
F6 C28 F5 108.0(11) . .
F5' C28 F5 50.1(9) . .
F6' C28 F5 79.7(11) . .
F4 C28 F5 105.4(10) . .
F4' C28 F5 157.3(14) . .
F6 C28 S2 120.1(10) . .
F5' C28 S2 118.3(9) . .
F6' C28 S2 115.0(11) . .
F4 C28 S2 114.4(9) . .
F4' C28 S2 99.3(12) . .
F5 C28 S2 96.4(11) . .
O6 O4 S2 72.3(10) 2_656 2_656
O6 O4 S2 86.6(12) 2_656 .
S2 O4 S2 63.1(4) 2_656 .
O6 O4 O5 132.5(14) 2_656 2_656
S2 O4 O5 60.2(6) 2_656 2_656
S2 O4 O5 72.9(7) . 2_656
S2 O5 O4 52.7(5) . 2_656
S2 O5 O6 55.9(5) . 2_656
O4 O5 O6 88.8(8) 2_656 2_656
S2 O5 S2 51.5(5) . 2_656
O4 O5 S2 48.1(5) 2_656 2_656
O6 O5 S2 45.2(5) 2_656 2_656
O4 O6 S2 78.2(11) 2_656 .
O4 O6 S2 66.2(11) 2_656 2_656
S2 O6 S2 60.6(4) . 2_656
O4 O6 O5 121.3(15) 2_656 2_656
S2 O6 O5 70.4(7) . 2_656
S2 O6 O5 55.3(5) 2_656 2_656
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ag1 N3 2.103(3) .
Ag1 N1 2.105(3) .
N1 C1 1.316(4) .
N1 C2 1.390(4) .
N2 C1 1.345(4) .
N2 C7 1.384(4) .
N2 C8 1.454(4) .
N3 C9 1.320(4) .
N3 C10 1.390(4) .
N4 C9 1.347(4) .
N4 C15 1.396(4) .
N4 C16 1.468(4) .
C2 C7 1.387(4) .
C2 C3 1.397(5) .
C3 C4 1.386(5) .
C4 C5 1.405(6) .
C5 C6 1.372(5) .
C6 C7 1.389(4) .
C8 C20 1.508(5) .
C10 C11 1.381(5) .
C10 C15 1.399(4) .
C11 C12 1.377(6) .
C12 C13 1.373(6) .
C13 C14 1.389(5) .
C14 C15 1.393(4) .
C16 C17 1.504(4) .
C17 C22 1.396(5) .
C17 C18 1.400(5) .
C18 C19 1.389(5) .
C18 C23 1.533(6) .
C19 C20 1.395(6) 2_656
C19 C24 1.526(5) .
C20 C19 1.395(6) 2_656
C20 C21 1.401(5) .
C21 C22 1.398(5) 2_656
C21 C25 1.493(7) .
C22 C21 1.398(5) 2_656
C22 C26 1.509(6) .
S1 O2 1.335(4) .
S1 O3 1.343(3) .
S1 O1 1.353(4) .
S1 C27 1.990(3) 2_467
S1 S1 1.990(3) 2_467
S2 O6 1.385(8) .
S2 O4 1.423(9) 2_656
S2 O4 1.433(7) .
S2 S2 1.495(6) 2_656
S2 O5 1.552(9) .
S2 O6 1.564(11) 2_656
S2 C28 1.776(9) .
S2 O5 1.838(17) 2_656
C28 F6 1.298(9) .
C28 F5' 1.306(9) .
C28 F6' 1.321(10) .
C28 F4 1.329(9) .
C28 F4' 1.339(10) .
C28 F5 1.349(10) .
O4 O6 0.716(14) 2_656
O4 S2 1.423(9) 2_656
O4 O5 1.648(18) 2_656
O5 O4 1.648(18) 2_656
O5 O6 1.759(19) 2_656
O5 S2 1.838(17) 2_656
O6 O4 0.716(14) 2_656
O6 S2 1.564(11) 2_656
O6 O5 1.759(19) 2_656
