#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/75/4327579.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_4327579
loop_
_publ_author_name
'Jian Chu Zhong'
'Megumu Munakata'
'Takayoshi Kuroda-Sowa'
'Masahiko Maekawa'
'Yusaku Suenaga'
'Hisashi Konaka'
_publ_section_title
;
 Spiral, Herringbone, and Triple-Decker Silver(I) Complexes of Benzopyrene
 Derivatives Assembled through η2-Coordination
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3191
_journal_page_last               3199
_journal_paper_doi               10.1021/ic001352+
_journal_volume                  40
_journal_year                    2001
_chemical_formula_moiety         'C42 H30 Ag4 F12 O12 S4 '
_chemical_formula_sum            'C42 H30 Ag4 F12 O12 S4'
_chemical_formula_weight         1514.38
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      13
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 1'
_cell_angle_alpha                90
_cell_angle_beta                 93.703(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   22.285(3)
_cell_length_b                   5.032(2)
_cell_length_c                   21.405(8)
_cell_measurement_reflns_used    6058
_cell_measurement_temperature    200.2
_cell_measurement_theta_max      27.6
_cell_measurement_theta_min      4.0
_cell_volume                     2395.3(13)
_computing_cell_refinement       D*TREK
_computing_data_collection       D*TREK
_computing_data_reduction        'teXsan Ver. 1.10'
_computing_publication_material  'teXsan Ver. 1.10'
_computing_structure_refinement  SHELXL97
_computing_structure_solution    SIR97
_diffrn_measurement_device_type  'Quantum CCD/Rigaku AFC7'
_diffrn_measurement_method       ω
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.000
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6058
_diffrn_reflns_theta_max         27.59
_exptl_absorpt_coefficient_mu    1.889
_exptl_absorpt_correction_T_max  0.954
_exptl_absorpt_correction_T_min  0.789
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Jacobson, 1998)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.099
_exptl_crystal_description       needle
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_refine_diff_density_max         2.50
_refine_diff_density_min         -1.42
_refine_ls_extinction_coef       0.0004
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.136
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     335
_refine_ls_number_reflns         4123
_refine_ls_R_factor_gt           0.0607
_refine_ls_shift/su_max          -0.0010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²) + (0.0154P)²+21.8685P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1205
_reflns_number_gt                4123
_reflns_number_total             5459
_reflns_threshold_expression     >2.0sigma(I)
_cod_data_source_file            ic0013522B_2.cif
_cod_data_source_block
'[Ag2(L2)(CF3SO3)2][Ag2(toluene)2(CF3SO3)2]}n(2)'
_cod_original_cell_volume        2395(1)
_cod_original_formula_sum        'C42 H30 Ag4 F12 O12 S4 '
_cod_database_code               4327579
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,y,1/2-z
-x,-y,-z
x,-y,1/2+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_calc_flag
Ag(1) Ag -0.00423(3) 0.4425(1) 0.67387(2) 0.0358(2) Uani 1.00 d
Ag(2) Ag 0.53730(3) 0.3686(1) 0.31958(3) 0.0540(2) Uani 1.00 d
S(1) S -0.08682(7) 0.9272(3) 0.75227(7) 0.0271(3) Uani 1.00 d
S(2) S 0.57006(8) 0.8511(4) 0.2014(1) 0.0427(4) Uani 1.00 d
F(1) F -0.1883(2) 1.058(1) 0.7974(3) 0.073(2) Uani 1.00 d
F(2) F -0.1870(2) 1.096(1) 0.6978(2) 0.066(1) Uani 1.00 d
F(3) F -0.1930(2) 0.710(1) 0.7390(3) 0.068(1) Uani 1.00 d
F(4) F 0.6367(3) 0.996(2) 0.1122(3) 0.105(2) Uani 1.00 d
F(5) F 0.6818(3) 0.994(2) 0.2033(4) 0.104(2) Uani 1.00 d
F(6) F 0.6623(3) 0.627(1) 0.1556(4) 0.126(3) Uani 1.00 d
O(1) O -0.0729(2) 0.7980(9) 0.6950(2) 0.035(1) Uani 1.00 d
O(2) O -0.0729(2) 0.7759(9) 0.8087(2) 0.036(1) Uani 1.00 d
O(3) O -0.0686(2) 1.2033(9) 0.7557(2) 0.039(1) Uani 1.00 d
O(4) O 0.5831(3) 0.709(1) 0.2589(3) 0.061(2) Uani 1.00 d
O(5) O 0.5317(3) 0.714(1) 0.1551(3) 0.057(1) Uani 1.00 d
O(6) O 0.5555(3) 1.127(1) 0.2098(3) 0.057(1) Uani 1.00 d
C(1) C -0.0627(3) 0.282(1) 0.5816(3) 0.033(1) Uani 1.00 d
C(2) C -0.0099(3) 0.151(1) 0.5848(3) 0.032(1) Uani 1.00 d
C(3) C 0.0390(3) 0.222(1) 0.5466(3) 0.029(1) Uani 1.00 d
C(4) C 0.0927(3) 0.086(1) 0.5509(3) 0.036(1) Uani 1.00 d
C(5) C 0.1372(3) 0.146(1) 0.5125(3) 0.036(2) Uani 1.00 d
C(6) C 0.1931(4) -0.007(1) 0.5154(3) 0.045(2) Uani 1.00 d
C(7) C 0.2359(3) 0.043(2) 0.4755(4) 0.047(2) Uani 1.00 d
C(8) C 0.2278(4) 0.245(2) 0.4301(4) 0.052(2) Uani 1.00 d
C(9) C 0.1766(3) 0.395(1) 0.4252(3) 0.042(2) Uani 1.00 d
C(10) C 0.1301(3) 0.349(1) 0.4664(3) 0.033(1) Uani 1.00 d
C(11) C 0.0740(3) 0.501(1) 0.4615(3) 0.027(1) Uani 1.00 d
C(12) C 0.0283(3) 0.433(1) 0.5017(2) 0.022(1) Uani 1.00 d
C(13) C 0.6605(6) 0.381(3) 0.3956(6) 0.094(4) Uani 1.00 d
C(14) C 0.6216(9) 0.164(3) 0.3786(7) 0.110(6) Uani 1.00 d
C(15) C 0.577(1) 0.109(3) 0.414(1) 0.15(1) Uani 1.00 d
C(16) C 0.5680(8) 0.255(5) 0.468(1) 0.145(8) Uani 1.00 d
C(17) C 0.6054(9) 0.447(3) 0.4835(6) 0.104(5) Uani 1.00 d
C(18) C 0.6507(6) 0.512(2) 0.4480(6) 0.075(3) Uani 1.00 d
C(19) C 0.7081(9) 0.441(6) 0.3564(10) 0.22(1) Uani 1.00 d
C(20) C -0.1689(3) 0.949(2) 0.7467(4) 0.044(2) Uani 1.00 d
C(21) C 0.6418(4) 0.868(2) 0.1654(6) 0.072(3) Uani 1.00 d
H(1) H -0.0931 0.2310 0.6083 0.0399 Uiso 1.00 calc
H(2) H -0.0045 0.0068 0.6132 0.0383 Uiso 1.00 calc
H(3) H 0.0988 -0.0514 0.5811 0.0431 Uiso 1.00 calc
H(5) H 0.2720 -0.0578 0.4780 0.0562 Uiso 1.00 calc
H(6) H 0.2585 0.2772 0.4023 0.0619 Uiso 1.00 calc
H(7) H 0.1721 0.5307 0.3943 0.0500 Uiso 1.00 calc
H(8) H 0.6276 0.0620 0.3422 0.1321 Uiso 1.00 calc
H(9) H 0.5512 -0.0354 0.4031 0.1860 Uiso 1.00 calc
H(10) H 0.5350 0.2164 0.4920 0.1737 Uiso 1.00 calc
H(11) H 0.6005 0.5426 0.5211 0.1248 Uiso 1.00 calc
H(12) H 0.6765 0.6553 0.4606 0.0898 Uiso 1.00 calc
H(13) H 0.7456 0.4212 0.3796 0.2686 Uiso 1.00 calc
H(14) H 0.7064 0.3221 0.3218 0.2686 Uiso 1.00 calc
H(15) H 0.7040 0.6182 0.3416 0.2686 Uiso 1.00 calc
H(16) H 0.1992 -0.1438 0.5458 0.0544 Uiso 1.00 calc
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Ag Ag -0.897 1.101
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
S S 0.125 0.123
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
F F 0.017 0.010
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
O O 0.011 0.006
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
C C 0.003 0.002
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.000 0.000
;International Tables for Crystallography
(1992, Vol. C, Table 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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O(1) Ag(1) O(2) 84.8(2) 1_555 2_556 yes
O(1) Ag(1) O(3) 80.5(1) 1_555 1_545 yes
O(1) Ag(1) O(3) 130.5(1) 1_555 2_546 yes
O(1) Ag(1) C(1) 94.8(2) 1_555 1_555 yes
O(1) Ag(1) C(2) 126.8(2) 1_555 1_555 yes
O(2) Ag(1) O(3) 129.0(1) 2_556 1_545 yes
O(2) Ag(1) O(3) 79.1(1) 2_556 2_546 yes
O(2) Ag(1) C(1) 134.0(2) 2_556 1_555 yes
O(2) Ag(1) C(2) 123.2(2) 2_556 1_555 yes
O(3) Ag(1) O(3) 74.6(2) 1_545 2_546 yes
O(3) Ag(1) C(1) 95.9(2) 1_545 1_555 yes
O(3) Ag(1) C(2) 104.3(2) 1_545 1_555 yes
O(3) Ag(1) C(1) 129.3(2) 2_546 1_555 yes
O(3) Ag(1) C(2) 100.7(2) 2_546 1_555 yes
C(1) Ag(1) C(2) 32.4(2) 1_555 1_555 yes
O(4) Ag(2) O(5) 84.7(2) 1_555 2_655 yes
O(4) Ag(2) O(6) 76.0(2) 1_555 1_545 yes
O(4) Ag(2) O(6) 126.4(2) 1_555 2_645 yes
O(4) Ag(2) C(14) 103.9(4) 1_555 1_555 yes
O(4) Ag(2) C(15) 131.2(5) 1_555 1_555 yes
O(5) Ag(2) O(6) 131.0(2) 2_655 1_545 yes
O(5) Ag(2) O(6) 82.8(2) 2_655 2_645 yes
O(5) Ag(2) C(14) 132.4(4) 2_655 1_555 yes
O(5) Ag(2) C(15) 113.1(6) 2_655 1_555 yes
O(6) Ag(2) O(6) 74.1(2) 1_545 2_645 yes
O(6) Ag(2) C(14) 96.2(4) 1_545 1_555 yes
O(6) Ag(2) C(15) 113.6(5) 1_545 1_555 yes
O(6) Ag(2) C(14) 122.6(4) 2_645 1_555 yes
O(6) Ag(2) C(15) 101.5(5) 2_645 1_555 yes
C(14) Ag(2) C(15) 30.7(7) 1_555 1_555 yes
O(1) S(1) O(2) 115.4(3) 1_555 1_555 yes
O(1) S(1) O(3) 113.7(3) 1_555 1_555 yes
O(1) S(1) C(20) 104.0(3) 1_555 1_555 yes
O(2) S(1) O(3) 114.8(3) 1_555 1_555 yes
O(2) S(1) C(20) 104.2(3) 1_555 1_555 yes
O(3) S(1) C(20) 102.7(3) 1_555 1_555 yes
O(4) S(2) O(5) 115.5(3) 1_555 1_555 yes
O(4) S(2) O(6) 114.0(4) 1_555 1_555 yes
O(4) S(2) C(21) 104.5(5) 1_555 1_555 yes
O(5) S(2) O(6) 114.7(3) 1_555 1_555 yes
O(5) S(2) C(21) 103.2(5) 1_555 1_555 yes
O(6) S(2) C(21) 102.6(4) 1_555 1_555 yes
Ag(1) O(1) S(1) 131.9(3) 1_555 1_555 yes
Ag(1) O(2) S(1) 127.4(3) 2_556 1_555 yes
Ag(1) O(3) Ag(1) 79.5(1) 1_565 2_566 yes
Ag(1) O(3) S(1) 124.7(3) 1_565 1_555 yes
Ag(1) O(3) S(1) 132.3(3) 2_566 1_555 yes
Ag(2) O(4) S(2) 138.0(4) 1_555 1_555 yes
Ag(2) O(5) S(2) 123.3(3) 2_655 1_555 yes
Ag(2) O(6) Ag(2) 80.1(2) 1_565 2_665 yes
Ag(2) O(6) S(2) 126.2(3) 1_565 1_555 yes
Ag(2) O(6) S(2) 129.7(3) 2_665 1_555 yes
Ag(1) C(1) C(2) 72.6(4) 1_555 1_555 yes
Ag(1) C(1) C(11) 109.4(4) 1_555 3_566 yes
C(2) C(1) C(11) 121.3(6) 1_555 3_566 yes
Ag(1) C(2) C(1) 75.1(4) 1_555 1_555 yes
Ag(1) C(2) C(3) 107.2(4) 1_555 1_555 yes
C(1) C(2) C(3) 122.5(5) 1_555 1_555 yes
C(2) C(3) C(4) 121.5(6) 1_555 1_555 yes
C(2) C(3) C(12) 117.3(5) 1_555 1_555 yes
C(4) C(3) C(12) 121.1(6) 1_555 1_555 yes
C(3) C(4) C(5) 120.9(6) 1_555 1_555 yes
C(4) C(5) C(6) 120.5(6) 1_555 1_555 yes
C(4) C(5) C(10) 121.7(6) 1_555 1_555 yes
C(6) C(5) C(10) 117.7(6) 1_555 1_555 yes
C(5) C(6) C(7) 120.7(7) 1_555 1_555 yes
C(6) C(7) C(8) 120.5(7) 1_555 1_555 yes
C(7) C(8) C(9) 121.5(8) 1_555 1_555 yes
C(8) C(9) C(10) 120.0(7) 1_555 1_555 yes
C(5) C(10) C(9) 119.6(6) 1_555 1_555 yes
C(5) C(10) C(11) 118.7(6) 1_555 1_555 yes
C(9) C(10) C(11) 121.7(6) 1_555 1_555 yes
C(1) C(11) C(10) 123.6(6) 3_566 1_555 yes
C(1) C(11) C(12) 118.0(6) 3_566 1_555 yes
C(10) C(11) C(12) 118.4(5) 1_555 1_555 yes
C(3) C(12) C(11) 119.2(5) 1_555 1_555 yes
C(3) C(12) C(12) 119.3(6) 1_555 3_566 yes
C(11) C(12) C(12) 121.5(6) 1_555 3_566 yes
C(14) C(13) C(18) 117(1) 1_555 1_555 yes
C(14) C(13) C(19) 118(1) 1_555 1_555 yes
C(18) C(13) C(19) 124(1) 1_555 1_555 yes
Ag(2) C(14) C(13) 104.2(10) 1_555 1_555 yes
Ag(2) C(14) C(15) 78(1) 1_555 1_555 yes
C(13) C(14) C(15) 118(1) 1_555 1_555 yes
Ag(2) C(15) C(14) 70(1) 1_555 1_555 yes
Ag(2) C(15) C(16) 108(1) 1_555 1_555 yes
C(14) C(15) C(16) 121(1) 1_555 1_555 yes
C(15) C(16) C(17) 118(1) 1_555 1_555 yes
C(16) C(17) C(18) 121(1) 1_555 1_555 yes
C(13) C(18) C(17) 121(1) 1_555 1_555 yes
S(1) C(20) F(1) 110.7(5) 1_555 1_555 yes
S(1) C(20) F(2) 109.8(5) 1_555 1_555 yes
S(1) C(20) F(3) 110.4(5) 1_555 1_555 yes
F(1) C(20) F(2) 108.8(6) 1_555 1_555 yes
F(1) C(20) F(3) 109.3(6) 1_555 1_555 yes
F(2) C(20) F(3) 107.9(6) 1_555 1_555 yes
S(2) C(21) F(4) 111.2(7) 1_555 1_555 yes
S(2) C(21) F(5) 109.6(8) 1_555 1_555 yes
S(2) C(21) F(6) 110.3(7) 1_555 1_555 yes
F(4) C(21) F(5) 108.3(9) 1_555 1_555 yes
F(4) C(21) F(6) 109(1) 1_555 1_555 yes
F(5) C(21) F(6) 108.1(8) 1_555 1_555 yes
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
Ag(1) O(1) 2.416(5) . yes
Ag(1) O(2) 2.414(5) 2_556 yes
Ag(1) O(3) 2.627(5) 1_545 yes
Ag(1) O(3) 2.458(5) 2_546 yes
Ag(1) C(1) 2.432(6) . yes
Ag(1) C(2) 2.402(6) . yes
Ag(2) O(4) 2.417(6) . yes
Ag(2) O(5) 2.407(6) 2_655 yes
Ag(2) O(6) 2.698(6) 1_545 yes
Ag(2) O(6) 2.446(6) 2_645 yes
Ag(2) C(14) 2.42(2) . yes
Ag(2) C(15) 2.53(3) . yes
S(1) O(1) 1.440(4) . yes
S(1) O(2) 1.445(4) . yes
S(1) O(3) 1.448(5) . yes
S(1) C(20) 1.829(8) . yes
S(2) O(4) 1.436(6) . yes
S(2) O(5) 1.441(6) . yes
S(2) O(6) 1.442(6) . yes
S(2) C(21) 1.82(1) . yes
F(1) C(20) 1.311(10) . yes
F(2) C(20) 1.323(9) . yes
F(3) C(20) 1.326(9) . yes
F(4) C(21) 1.31(1) . yes
F(5) C(21) 1.33(1) . yes
F(6) C(21) 1.32(1) . yes
C(1) C(2) 1.348(10) . yes
C(1) C(11) 1.439(8) 3_566 yes
C(2) C(3) 1.448(9) . yes
C(3) C(4) 1.375(10) . yes
C(3) C(12) 1.444(8) . yes
C(4) C(5) 1.36(1) . yes
C(5) C(6) 1.46(1) . yes
C(5) C(10) 1.424(9) . yes
C(6) C(7) 1.35(1) . yes
C(7) C(8) 1.41(1) . yes
C(8) C(9) 1.37(1) . yes
C(9) C(10) 1.42(1) . yes
C(10) C(11) 1.464(9) . yes
C(11) C(12) 1.416(8) . yes
C(12) C(12) 1.43(1) 3_566 yes
C(13) C(14) 1.43(2) . yes
C(13) C(18) 1.33(2) . yes
C(13) C(19) 1.43(3) . yes
C(14) C(15) 1.32(3) . yes
C(15) C(16) 1.39(4) . yes
C(16) C(17) 1.31(3) . yes
C(17) C(18) 1.34(2) . yes
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_2
Ag(1) O(3) 2.627(5) 1_545
Ag(2) O(6) 2.698(6) 1_545
Ag(2) C(15) 2.53(3) .
F(1) F(5) 3.427(8) 4_475
F(1) F(3) 3.511(8) 1_565
F(2) F(5) 2.967(7) 4_475
F(2) F(3) 3.216(8) 1_565
F(3) F(5) 3.211(8) 4_475
F(3) C(19) 3.53(2) 4_465
F(4) F(6) 3.35(1) 1_565
F(4) C(8) 3.45(1) 2_665
F(4) C(7) 3.51(1) 2_665
F(4) C(17) 3.58(2) 4_564
F(4) C(16) 3.59(2) 4_564
F(5) F(6) 3.36(1) 1_565
F(5) C(20) 3.407(9) 4_674
O(1) C(2) 3.335(8) 1_565
O(1) C(1) 3.457(8) 1_565
O(2) C(2) 3.408(7) 2_566
O(2) C(4) 3.438(8) 2_566
O(4) C(14) 3.50(2) 1_565
O(5) C(15) 3.40(2) 2_665
C(1) C(5) 3.320(9) 3_556
C(1) C(4) 3.418(9) 3_556
C(2) C(3) 3.408(8) 3_556
C(2) C(12) 3.484(8) 3_556
C(2) C(4) 3.547(9) 3_556
C(3) C(3) 3.40(1) 3_556
