#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/34/4313451.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_4313451
loop_
_publ_author_name
'Megumu Munakata'
'Liang Ping Wu'
'Takayoshi Kuroda-Sowa'
'Masahiko Maekawa'
'Yusaku Suenaga'
'Tetsuhiro Ohta'
'Hisashi Konaka'
_publ_section_title
;
 Construction of the Multidecker Anthracene-Silver(I) System by
 Intramolecular π-π Interactions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2553
_journal_page_last               2558
_journal_paper_doi               10.1021/ic020379l
_journal_volume                  42
_journal_year                    2003
_chemical_formula_moiety         'C32 H34 Ag2 Cl2 O8 '
_chemical_formula_sum            'C32 H34 Ag2 Cl2 O8'
_chemical_formula_weight         833.26
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_cell_angle_alpha                90
_cell_angle_beta                 97.32(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.885(2)
_cell_length_b                   12.345(2)
_cell_length_c                   17.059(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      11.2
_cell_volume                     1647.0(6)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan Ver. 1.11'
_computing_publication_material  'teXsan Ver. 1.11'
_computing_structure_refinement  SHELXL97
_computing_structure_solution    MITHRIL90
_diffrn_measured_fraction_theta_full 1.00
_diffrn_measured_fraction_theta_max 1.00
_diffrn_measurement_device_type  'Rigaku AFC7R'
_diffrn_measurement_method       ω-2θ
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.018
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            3130
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_standards_decay_%        14.85
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.396
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.680
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       brick
_exptl_crystal_F_000             836.0
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.78
_refine_diff_density_min         -0.87
_refine_ls_extinction_coef       0.0000
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     199
_refine_ls_number_reflns         1974
_refine_ls_R_factor_gt           0.0567
_refine_ls_shift/su_max          0.0010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²) + (0.1016P)²+5.6717P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.2047
_reflns_number_gt                1974
_reflns_number_total             2906
_reflns_threshold_expression     >2.0sigma(I)
_cod_data_source_file            ic020379l_1.cif
_cod_data_source_block           '[Ag(dman)0.5(ClO4)(p-xylen'
_cod_original_cell_volume        1646.9(6)
_cod_original_formula_sum        'C32 H34 Ag2 Cl2 O8 '
_cod_database_code               4313451
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
1/2-x,1/2+y,1/2-z
-x,-y,-z
1/2+x,1/2-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
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ag(1) Ag 0.42728(8) 0.15653(6) 1.00873(5) 0.0648(3) Uani 1.00 d . . .
Cl(1) Cl 0.5030(5) 0.0277(2) 0.8368(2) 0.0854(9) Uani 1.00 d . . .
O(1) O 0.451(2) 0.1304(7) 0.8113(6) 0.130(4) Uani 1.00 d . . .
O(2) O 0.498(2) 0.0115(7) 0.9163(5) 0.144(5) Uani 1.00 d . . .
O(3) O 0.456(4) -0.050(1) 0.791(1) 0.31(2) Uani 1.00 d . . .
O(4) O 0.672(3) 0.028(2) 0.838(2) 0.35(2) Uani 1.00 d . . .
C(1) C 0.639(1) 0.2919(8) 0.9760(6) 0.062(2) Uani 1.00 d . . .
C(2) C 0.712(1) 0.2324(8) 1.0373(7) 0.069(3) Uani 1.00 d . . .
C(3) C 0.721(1) 0.2756(10) 1.1142(7) 0.076(3) Uani 1.00 d . . .
C(4) C 0.662(1) 0.3730(9) 1.1262(6) 0.070(3) Uani 1.00 d . . .
C(5) C 0.578(1) 0.4396(7) 1.0644(5) 0.055(2) Uani 1.00 d . . .
C(6) C 0.565(1) 0.3972(7) 0.9855(5) 0.055(2) Uani 1.00 d . . .
C(7) C 0.514(1) 0.5425(8) 1.0793(5) 0.061(2) Uani 1.00 d . . .
C(8) C 0.523(2) 0.5881(10) 1.1619(6) 0.092(4) Uani 1.00 d . . .
C(9) C 0.147(1) 0.182(1) 1.0487(8) 0.083(4) Uani 1.00 d . . .
C(10) C 0.106(1) 0.158(1) 0.971(1) 0.093(4) Uani 1.00 d . . .
C(11) C 0.074(1) 0.236(2) 0.9130(7) 0.095(4) Uani 1.00 d . . .
C(12) C 0.127(2) 0.365(1) 1.014(1) 0.103(5) Uani 1.00 d . . .
C(13) C 0.087(2) 0.339(1) 0.942(1) 0.110(5) Uani 1.00 d . . .
C(14) C 0.156(1) 0.291(2) 1.0719(8) 0.101(5) Uani 1.00 d . . .
C(15) C 0.201(2) 0.321(2) 1.156(1) 0.20(1) Uani 1.00 d . . .
C(16) C 0.026(2) 0.201(3) 0.827(1) 0.20(1) Uani 1.00 d . . .
H(1) H 0.6351 0.2632 0.9241 0.0739 Uiso 1.00 calc . . .
H(2) H 0.7562 0.1624 1.0288 0.0833 Uiso 1.00 calc . . .
H(3) H 0.7709 0.2338 1.1579 0.0913 Uiso 1.00 calc . . .
H(4) H 0.6758 0.4006 1.1786 0.0842 Uiso 1.00 calc . . .
H(5) H 0.6390 0.5926 1.1848 0.1100 Uiso 1.00 calc . . .
H(6) H 0.4619 0.5421 1.1931 0.1100 Uiso 1.00 calc . . .
H(7) H 0.4734 0.6584 1.1596 0.1100 Uiso 1.00 calc . . .
H(8) H 0.1696 0.1263 1.0867 0.0999 Uiso 1.00 calc . . .
H(9) H 0.0983 0.0841 0.9553 0.1112 Uiso 1.00 calc . . .
H(10) H 0.1369 0.4397 1.0268 0.1236 Uiso 1.00 calc . . .
H(11) H 0.0632 0.3961 0.9050 0.1322 Uiso 1.00 calc . . .
H(12) H 0.2168 0.2574 1.1870 0.2432 Uiso 1.00 calc . . .
H(13) H 0.3045 0.3619 1.1616 0.2432 Uiso 1.00 calc . . .
H(14) H 0.1123 0.3636 1.1727 0.2432 Uiso 1.00 calc . . .
H(15) H 0.0090 0.2632 0.7944 0.2367 Uiso 1.00 calc . . .
H(16) H -0.0758 0.1594 0.8228 0.2367 Uiso 1.00 calc . . .
H(17) H 0.1163 0.1585 0.8113 0.2367 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 Tablesfor Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Cl Cl 0.148 0.159
;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_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O(2) Ag(1) O(2) 70.5(4) . . 3_657 yes
O(2) Ag(1) C(1) 97.6(4) . . . yes
O(2) Ag(1) C(2) 97.5(4) . . . yes
O(2) Ag(1) C(9) 123.9(4) . . . yes
O(2) Ag(1) C(10) 98.0(5) . . . yes
O(2) Ag(1) C(1) 124.1(4) 3_657 . . yes
O(2) Ag(1) C(2) 93.8(4) 3_657 . . yes
O(2) Ag(1) C(9) 97.6(5) 3_657 . . yes
O(2) Ag(1) C(10) 107.8(4) 3_657 . . yes
C(1) Ag(1) C(2) 31.9(3) . . . yes
C(1) Ag(1) C(9) 129.9(4) . . . yes
C(1) Ag(1) C(10) 128.1(4) . . . yes
C(2) Ag(1) C(9) 138.5(4) . . . yes
C(2) Ag(1) C(10) 156.7(4) . . . yes
C(9) Ag(1) C(10) 31.8(5) . . . yes
O(1) Cl(1) O(2) 113.4(6) . . . yes
O(1) Cl(1) O(3) 116(1) . . . yes
O(1) Cl(1) O(4) 104(1) . . . yes
O(2) Cl(1) O(3) 117.1(10) . . . yes
O(2) Cl(1) O(4) 98(1) . . . yes
O(3) Cl(1) O(4) 103(2) . . . yes
Ag(1) O(2) Ag(1) 109.5(4) . . 3_657 yes
Ag(1) O(2) Cl(1) 123.7(5) . . . yes
Ag(1) O(2) Cl(1) 126.6(6) 3_657 . . yes
Ag(1) C(1) C(2) 71.9(6) . . . yes
Ag(1) C(1) C(6) 107.1(6) . . . yes
Ag(1) C(1) H(1) 91.0 . . . no
C(2) C(1) C(6) 122.9(9) . . . yes
C(2) C(1) H(1) 118.6 . . . no
C(6) C(1) H(1) 118.6 . . . no
Ag(1) C(2) C(1) 76.2(6) . . . yes
Ag(1) C(2) C(3) 105.7(7) . . . yes
Ag(1) C(2) H(2) 88.2 . . . no
C(1) C(2) C(3) 118.9(10) . . . yes
C(1) C(2) H(2) 120.5 . . . no
C(3) C(2) H(2) 120.6 . . . no
C(2) C(3) C(4) 120(1) . . . yes
C(2) C(3) H(3) 119.6 . . . no
C(4) C(3) H(3) 119.5 . . . no
C(3) C(4) C(5) 123.4(10) . . . yes
C(3) C(4) H(4) 118.3 . . . no
C(5) C(4) H(4) 118.3 . . . no
C(4) C(5) C(6) 116.8(8) . . . yes
C(4) C(5) C(7) 122.0(8) . . . yes
C(6) C(5) C(7) 121.3(8) . . . yes
C(1) C(6) C(5) 117.1(8) . . . yes
C(1) C(6) C(7) 122.1(8) . . 3_667 yes
C(5) C(6) C(7) 120.7(8) . . 3_667 yes
C(5) C(7) C(6) 118.0(8) . . 3_667 yes
C(5) C(7) C(8) 122.3(8) . . . yes
C(6) C(7) C(8) 119.7(9) 3_667 . . yes
C(7) C(8) H(5) 109.4 . . . no
C(7) C(8) H(6) 109.5 . . . no
C(7) C(8) H(7) 109.5 . . . no
H(5) C(8) H(6) 109.5 . . . no
H(5) C(8) H(7) 109.5 . . . no
H(6) C(8) H(7) 109.5 . . . no
Ag(1) C(9) C(10) 79.0(7) . . . yes
Ag(1) C(9) C(14) 101.1(8) . . . yes
Ag(1) C(9) H(8) 89.9 . . . no
C(10) C(9) C(14) 118(1) . . . yes
C(10) C(9) H(8) 120.5 . . . no
C(14) C(9) H(8) 120.5 . . . no
Ag(1) C(10) C(9) 69.2(6) . . . yes
Ag(1) C(10) C(11) 105.9(8) . . . yes
Ag(1) C(10) H(9) 94.9 . . . no
C(9) C(10) C(11) 122(1) . . . yes
C(9) C(10) H(9) 118.6 . . . no
C(11) C(10) H(9) 118.6 . . . no
C(10) C(11) C(13) 113(1) . . . yes
C(10) C(11) C(16) 118(1) . . . yes
C(13) C(11) C(16) 127(1) . . . yes
C(13) C(12) C(14) 122(1) . . . yes
C(13) C(12) H(10) 118.7 . . . no
C(14) C(12) H(10) 118.7 . . . no
C(11) C(13) C(12) 126(1) . . . yes
C(11) C(13) H(11) 117.0 . . . no
C(12) C(13) H(11) 117.0 . . . no
C(9) C(14) C(12) 116(1) . . . yes
C(9) C(14) C(15) 120(1) . . . yes
C(12) C(14) C(15) 122(2) . . . yes
C(14) C(15) H(12) 109.5 . . . no
C(14) C(15) H(13) 109.4 . . . no
C(14) C(15) H(14) 109.4 . . . no
H(12) C(15) H(13) 109.6 . . . no
H(12) C(15) H(14) 109.5 . . . no
H(13) C(15) H(14) 109.4 . . . no
C(11) C(16) H(15) 109.4 . . . no
C(11) C(16) H(16) 109.4 . . . no
C(11) C(16) H(17) 109.5 . . . no
H(15) C(16) H(16) 109.5 . . . no
H(15) C(16) H(17) 109.5 . . . no
H(16) C(16) H(17) 109.6 . . . no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ag(1) O(2) 2.494(10) . . yes
Ag(1) O(2) 2.469(9) . 3_657 yes
Ag(1) C(1) 2.474(10) . . yes
Ag(1) C(2) 2.422(9) . . yes
Ag(1) C(9) 2.42(1) . . yes
Ag(1) C(10) 2.54(1) . . yes
Cl(1) O(1) 1.387(10) . . yes
Cl(1) O(2) 1.377(10) . . yes
Cl(1) O(3) 1.26(2) . . yes
Cl(1) O(4) 1.33(2) . . yes
C(1) C(2) 1.35(1) . . yes
C(1) C(6) 1.44(1) . . yes
C(1) H(1) 0.950 . . no
C(2) C(3) 1.41(2) . . yes
C(2) H(2) 0.950 . . no
C(3) C(4) 1.32(2) . . yes
C(3) H(3) 0.950 . . no
C(4) C(5) 1.43(1) . . yes
C(4) H(4) 0.950 . . no
C(5) C(6) 1.43(1) . . yes
C(5) C(7) 1.40(1) . . yes
C(6) C(7) 1.41(1) . 3_667 yes
C(7) C(8) 1.51(1) . . yes
C(8) H(5) 0.950 . . no
C(8) H(6) 0.950 . . no
C(8) H(7) 0.950 . . no
C(9) C(10) 1.36(2) . . yes
C(9) C(14) 1.40(3) . . yes
C(9) H(8) 0.950 . . no
C(10) C(11) 1.38(2) . . yes
C(10) H(9) 0.950 . . no
C(11) C(13) 1.35(3) . . yes
C(11) C(16) 1.53(2) . . yes
C(12) C(13) 1.27(3) . . yes
C(12) C(14) 1.35(3) . . yes
C(12) H(10) 0.950 . . no
C(13) H(11) 0.950 . . no
C(14) C(15) 1.48(3) . . yes
C(15) H(12) 0.949 . . no
C(15) H(13) 0.950 . . no
C(15) H(14) 0.951 . . no
C(16) H(15) 0.950 . . no
C(16) H(16) 0.950 . . no
C(16) H(17) 0.949 . . no
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
Ag(1) C(10) 2.54(1) . . ?
O(1) C(15) 3.55(2) . 4_554 ?
O(4) C(16) 3.54(4) . 1_655 ?
C(2) C(9) 3.47(1) . 1_655 ?
C(2) C(14) 3.55(1) . 1_655 ?
C(2) C(10) 3.56(2) . 1_655 ?
C(3) C(14) 3.60(2) . 1_655 ?
Ag(1) C(10) 2.54(1) . . ?
