#------------------------------------------------------------------------------
#$Date: 2016-03-26 14:05:55 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180247 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/33/7113390.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_7113390
loop_
_publ_author_name
'Mahmoudkhani, Amir H.'
'Côté, Adrien P'
'Shimizu, George K. H.'
_publ_section_title
;
 A neutral self-assembled coordination cage organized for inclusion of
 aromatic guests.
;
_journal_issue                   23
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              2678
_journal_page_last               2679
_journal_paper_doi               10.1039/b412325e
_journal_year                    2004
_chemical_formula_sum            'C113 H95 Cu3 N13 O18 S6'
_chemical_formula_weight         2306.00
_chemical_name_common
;Tetrakis(pyridine)copper(ii) 1,3,5-tris(4-sulfophenyl)benzene
pyridine solvate
;
_chemical_name_systematic
;
?
;
_space_group_IT_number           167
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 90.000(5)
_cell_angle_gamma                120.000(5)
_cell_formula_units_Z            6
_cell_length_a                   20.324(5)
_cell_length_b                   20.324(5)
_cell_length_c                   47.623(5)
_cell_measurement_temperature    293(2)
_cell_volume                     17036(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0164
_diffrn_reflns_av_sigmaI/netI    0.0324
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       57
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6602
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         1.44
_exptl_absorpt_coefficient_mu    0.737
_exptl_crystal_density_diffrn    1.349
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             7146
_refine_diff_density_max         1.489
_refine_diff_density_min         -1.109
_refine_diff_density_rms         0.218
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.170
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         3462
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.170
_refine_ls_R_factor_all          0.1239
_refine_ls_R_factor_gt           0.1096
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w==1/[σ²(Fo²)+(0.1468P)²+260.4449P] where P==(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3136
_refine_ls_wR_factor_ref         0.3288
_reflns_number_gt                3047
_reflns_number_total             3462
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b412325e.txt
_cod_data_source_block           n
_cod_original_sg_symbol_H-M      R-3c
_cod_database_code               7113390
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'y, x, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'y+2/3, x+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'y+1/3, x+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-y, -x, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-y+2/3, -x+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'
'-y+1/3, -x+2/3, z+1/6'
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
C1 C 0.7216(4) 0.0050(4) 0.16463(14) 0.0465(16) Uani 1 1 d .
C2 C 0.7894(5) 0.0693(5) 0.1575(2) 0.067(2) Uani 1 1 d .
H2 H 0.7896 0.1138 0.1528 0.081 Uiso 1 1 calc R
C3 C 0.8575(5) 0.0679(5) 0.1572(2) 0.063(2) Uani 1 1 d .
H3 H 0.9024 0.1114 0.1522 0.076 Uiso 1 1 calc R
C4 C 0.8588(4) 0.0030(4) 0.16425(15) 0.0454(16) Uani 1 1 d .
C5 C 0.7890(5) -0.0625(4) 0.17007(19) 0.057(2) Uani 1 1 d .
H5 H 0.7881 -0.1077 0.1742 0.069 Uiso 1 1 calc R
C6 C 0.7210(5) -0.0613(4) 0.16974(19) 0.057(2) Uani 1 1 d .
H6 H 0.6752 -0.1057 0.1730 0.068 Uiso 1 1 calc R
C7 C 0.9315(4) 0.0012(4) 0.16474(14) 0.0429(15) Uani 1 1 d .
C8 C 0.9302(4) -0.0678(4) 0.16489(14) 0.0436(15) Uani 1 1 d .
H8 H 0.8840 -0.1131 0.1651 0.052 Uiso 1 1 calc R
C9 C 0.0000 0.068(2) 0.2500 0.191(13) Uiso 1 2 d S
H9 H 0.0000 0.1133 0.2500 0.229 Uiso 1 2 calc SR
C10 C -0.067(3) 0.0000 0.2500 0.238(19) Uiso 1 2 d S
H10 H -0.1124 0.0000 0.2500 0.286 Uiso 1 2 calc SR
C11 C 0.7855(5) 0.0822(6) 0.2344(2) 0.066(2) Uani 1 1 d .
H11 H 0.7706 0.0432 0.2213 0.079 Uiso 1 1 calc R
C12 C 0.8614(7) 0.1400(8) 0.2358(3) 0.096(4) Uani 1 1 d .
H12 H 0.8968 0.1424 0.2228 0.115 Uiso 1 1 calc R
C13 C 0.8825(8) 0.1929(7) 0.2566(3) 0.100(4) Uani 1 1 d .
H13 H 0.9333 0.2304 0.2584 0.119 Uiso 1 1 calc R
C14 C 0.8301(9) 0.1913(7) 0.2749(3) 0.106(4) Uani 1 1 d .
H14 H 0.8442 0.2275 0.2890 0.127 Uiso 1 1 calc R
C15 C 0.7579(6) 0.1363(5) 0.2719(2) 0.075(3) Uani 1 1 d .
H15 H 0.7221 0.1350 0.2844 0.090 Uiso 1 1 calc R
C21 C 0.4709(6) -0.0721(7) 0.22553(19) 0.081(3) Uani 1 1 d .
H21 H 0.4940 -0.0298 0.2139 0.097 Uiso 1 1 calc R
C22 C 0.3964(6) -0.1244(9) 0.2214(3) 0.110(5) Uani 1 1 d .
H22 H 0.3695 -0.1184 0.2068 0.132 Uiso 1 1 calc R
C23 C 0.3602(7) -0.1883(9) 0.2394(3) 0.113(5) Uani 1 1 d .
H23 H 0.3096 -0.2253 0.2369 0.135 Uiso 1 1 calc R
C24 C 0.4022(6) -0.1934(7) 0.2606(2) 0.086(3) Uani 1 1 d .
H24 H 0.3797 -0.2332 0.2733 0.103 Uiso 1 1 calc R
C25 C 0.4780(5) -0.1395(6) 0.26316(18) 0.068(2) Uani 1 1 d .
H25 H 0.5062 -0.1451 0.2774 0.082 Uiso 1 1 calc R
N1 N 0.7342(4) 0.0829(4) 0.25195(14) 0.0574(17) Uani 1 1 d .
N2 N 0.5122(4) -0.0800(5) 0.24612(14) 0.0615(18) Uani 1 1 d .
O1 O 0.5756(3) -0.0619(4) 0.16186(13) 0.0670(16) Uani 1 1 d .
O2 O 0.6374(4) 0.0254(4) 0.19907(12) 0.0693(17) Uani 1 1 d .
O3 O 0.6479(4) 0.0728(4) 0.15171(14) 0.0711(17) Uani 1 1 d .
S S 0.63893(10) 0.01211(11) 0.16950(4) 0.0462(5) Uani 1 1 d .
Cu Cu 0.62378(7) 0.0000 0.2500 0.0555(5) Uani 1 2 d S
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'
Cu Cu 0.3201 1.2651 '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
C6 C1 C2 119.3(7) . .
C6 C1 S 121.1(6) . .
C2 C1 S 119.4(6) . .
C1 C2 C3 120.7(8) . .
C4 C3 C2 120.7(8) . .
C3 C4 C5 117.6(7) . .
C3 C4 C7 121.4(6) . .
C5 C4 C7 121.0(7) . .
C6 C5 C4 121.4(7) . .
C1 C6 C5 120.0(7) . .
C8 C7 C8 119.5(7) . 3_765
C8 C7 C4 120.3(6) . .
C8 C7 C4 120.1(6) 3_765 .
C7 C8 C7 120.5(7) . 2_645
C10 C9 C10 119(6) . 3
C9 C10 C9 121(6) 2 .
N1 C11 C12 119.9(10) . .
C13 C12 C11 118.5(12) . .
C14 C13 C12 120.8(12) . .
C15 C14 C13 117.9(12) . .
N1 C15 C14 123.8(13) . .
N2 C21 C22 121.8(10) . .
C21 C22 C23 119.5(11) . .
C24 C23 C22 117.4(11) . .
C23 C24 C25 120.2(10) . .
N2 C25 C24 122.4(9) . .
C15 N1 C11 118.9(8) . .
C15 N1 Cu 120.5(7) . .
C11 N1 Cu 120.4(6) . .
C25 N2 C21 118.5(8) . .
C25 N2 Cu 122.6(6) . .
C21 N2 Cu 118.8(6) . .
O3 S O2 115.1(4) . .
O3 S O1 114.1(4) . .
O2 S O1 110.4(4) . .
O3 S C1 106.0(4) . .
O2 S C1 104.7(3) . .
O1 S C1 105.6(4) . .
N1 Cu N1 92.5(4) 4 .
N1 Cu N2 89.6(3) 4 .
N1 Cu N2 176.7(3) . .
N1 Cu N2 176.7(3) 4 4
N1 Cu N2 89.6(3) . 4
N2 Cu N2 88.5(5) . 4
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C6 1.363(11) .
C1 C2 1.386(11) .
C1 S 1.773(7) .
C2 C3 1.398(12) .
C3 C4 1.374(11) .
C4 C5 1.405(10) .
C4 C7 1.497(10) .
C5 C6 1.395(11) .
C7 C8 1.391(9) .
C7 C8 1.413(10) 3_765
C8 C7 1.413(10) 2_645
C9 C10 1.36(2) .
C9 C10 1.36(2) 3
C10 C9 1.36(2) 2
C11 N1 1.343(12) .
C11 C12 1.398(16) .
C12 C13 1.365(19) .
C13 C14 1.364(19) .
C14 C15 1.336(16) .
C15 N1 1.336(12) .
C21 N2 1.351(12) .
C21 C22 1.360(15) .
C22 C23 1.418(17) .
C23 C24 1.356(15) .
C24 C25 1.378(14) .
C25 N2 1.329(12) .
N1 Cu 2.025(7) .
N2 Cu 2.033(7) .
O1 S 1.455(6) .
O2 S 1.437(6) .
O3 S 1.431(6) .
Cu N1 2.025(7) 4
Cu N2 2.033(7) 4
