#------------------------------------------------------------------------------
#$Date: 2016-03-21 18:20:39 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178809 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/63/4106349.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_4106349
loop_
_publ_author_name
'Johanna Heine'
'Jörn Schmedt auf der Günne'
'Stefanie Dehnen'
_publ_section_title
;
 Formation of a Strandlike Polycatenane of Icosahedral Cages for
 Reversible One-Dimensional Encapsulation of Guests
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10018
_journal_page_last               10021
_journal_paper_doi               10.1021/ja2030273
_journal_volume                  133
_journal_year                    2011
_chemical_formula_sum            'C160 H112 Cl24 N32 Zn12'
_chemical_formula_weight         4118.06
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   37.841(5)
_cell_length_b                   37.841(5)
_cell_length_c                   15.799(3)
_cell_measurement_reflns_used    17318
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      41.56
_cell_measurement_theta_min      2.86
_cell_volume                     19592(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Stoe IPDS 2'
_diffrn_measurement_method       ω-scan
_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  0.1621
_diffrn_reflns_av_sigmaI/netI    0.1543
_diffrn_reflns_limit_h_max       47
_diffrn_reflns_limit_h_min       -47
_diffrn_reflns_limit_k_max       47
_diffrn_reflns_limit_k_min       -47
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            66080
_diffrn_reflns_theta_full        26.78
_diffrn_reflns_theta_max         26.78
_diffrn_reflns_theta_min         1.86
_exptl_absorpt_coefficient_mu    1.365
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.047
_exptl_crystal_description       block
_exptl_crystal_F_000             6192
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.596
_refine_diff_density_min         -0.421
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.854
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     187
_refine_ls_number_reflns         9195
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.854
_refine_ls_R_factor_all          0.2079
_refine_ls_R_factor_gt           0.0811
_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)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2041
_refine_ls_wR_factor_ref         0.2312
_reflns_number_gt                2970
_reflns_number_total             9195
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            ja2030273_si_002.cif
_cod_data_source_block           compound1
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4106349
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'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+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, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-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+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'
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 0.2592(3) 0.3540(3) 0.0246(6) 0.1024(11) Uani 1 1 d .
H1 H 0.2863 0.3639 0.0399 0.123 Uiso 1 1 calc R
C2 C 0.2320(3) 0.3422(3) 0.0878(6) 0.1024(11) Uani 1 1 d .
H2 H 0.2398 0.3423 0.1437 0.123 Uiso 1 1 calc R
C3 C 0.1917(3) 0.3298(3) 0.0675(6) 0.1024(11) Uani 1 1 d .
C4 C 0.1824(3) 0.3298(3) -0.0170(5) 0.1024(11) Uani 1 1 d .
H4 H 0.1558 0.3217 -0.0337 0.123 Uiso 1 1 calc R
C5 C 0.2133(3) 0.3421(3) -0.0768(6) 0.1024(11) Uani 1 1 d .
H5 H 0.2068 0.3425 -0.1334 0.123 Uiso 1 1 calc R
C6 C 0.1591(3) 0.3161(3) 0.1335(5) 0.1039(11) Uani 1 1 d .
C7 C 0.1232(3) 0.3171(3) 0.1243(6) 0.1039(11) Uani 1 1 d .
H7 H 0.1182 0.3270 0.0745 0.125 Uiso 1 1 calc R
C8 C 0.0958(3) 0.3039(3) 0.1862(6) 0.1039(11) Uani 1 1 d .
C9 C 0.1035(3) 0.2889(3) 0.2592(5) 0.1039(11) Uani 1 1 d .
H9 H 0.0843 0.2797 0.3025 0.125 Uiso 1 1 calc R
C10 C 0.1383(3) 0.2872(3) 0.2701(6) 0.1039(11) Uani 1 1 d .
C11 C 0.0555(3) 0.3030(3) 0.1782(6) 0.1044(11) Uani 1 1 d .
C12 C 0.0519(3) 0.3311(3) 0.1276(5) 0.1044(11) Uani 1 1 d .
H12 H 0.0743 0.3513 0.0984 0.125 Uiso 1 1 calc R
C13 C 0.0141(3) 0.3279(3) 0.1223(6) 0.1044(11) Uani 1 1 d .
H13 H 0.0112 0.3458 0.0867 0.125 Uiso 1 1 calc R
C14 C -0.0149(3) 0.2747(3) 0.2127(5) 0.1044(11) Uani 1 1 d .
H14 H -0.0378 0.2547 0.2409 0.125 Uiso 1 1 calc R
C15 C 0.0211(3) 0.2755(3) 0.2227(6) 0.1044(11) Uani 1 1 d .
H15 H 0.0228 0.2573 0.2600 0.125 Uiso 1 1 calc R
C16 C 0.1469(2) 0.2726(3) 0.3496(5) 0.1003(11) Uani 1 1 d .
C17 C 0.1198(2) 0.2560(3) 0.4152(5) 0.1003(11) Uani 1 1 d .
H17 H 0.0948 0.2551 0.4124 0.120 Uiso 1 1 calc R
C18 C 0.1290(2) 0.2410(3) 0.4843(5) 0.1003(11) Uani 1 1 d .
H18 H 0.1099 0.2304 0.5278 0.120 Uiso 1 1 calc R
C19 C 0.1917(2) 0.2599(3) 0.4312(5) 0.1003(11) Uani 1 1 d .
H19 H 0.2172 0.2621 0.4373 0.120 Uiso 1 1 calc R
C20 C 0.1844(2) 0.2764(3) 0.3604(5) 0.1003(11) Uani 1 1 d .
H20 H 0.2049 0.2899 0.3203 0.120 Uiso 1 1 calc R
C21 C 0.1363(2) 0.1302(2) 0.5716(5) 0.0942(10) Uani 1 1 d .
H21 H 0.1598 0.1361 0.5419 0.113 Uiso 1 1 calc R
C22 C 0.1053(2) 0.0910(2) 0.5758(5) 0.0942(10) Uani 1 1 d .
H22 H 0.1088 0.0704 0.5525 0.113 Uiso 1 1 calc R
C23 C 0.0676(2) 0.0809(2) 0.6152(5) 0.0942(10) Uani 1 1 d .
C24 C 0.0647(2) 0.1127(2) 0.6519(5) 0.0942(10) Uani 1 1 d .
H24 H 0.0407 0.1083 0.6775 0.113 Uiso 1 1 calc R
C25 C 0.0993(2) 0.1515(2) 0.6490(5) 0.0942(10) Uani 1 1 d .
H25 H 0.0981 0.1726 0.6768 0.113 Uiso 1 1 calc R
C26 C 0.0323(2) 0.0387(2) 0.6146(5) 0.0913(16) Uani 1 1 d .
C27 C -0.0063(2) 0.0325(2) 0.6151(5) 0.0913(16) Uani 0.66666 1 d P
H27 H -0.0107 0.0546 0.6157 0.110 Uiso 0.66666 1 calc PR
Cl1 Cl -0.11172(8) 0.26902(8) 0.26742(17) 0.1254(9) Uani 1 1 d .
Cl2 Cl -0.06174(11) 0.35451(8) 0.0971(3) 0.1838(16) Uani 1 1 d .
Cl3 Cl 0.23744(6) 0.22260(6) 0.56633(14) 0.0961(6) Uani 1 1 d .
Cl4 Cl 0.17350(7) 0.25512(6) 0.70586(14) 0.1016(7) Uani 1 1 d .
N1 N 0.2515(2) 0.3531(2) -0.0577(4) 0.1024(11) Uani 1 1 d .
N2 N 0.1667(2) 0.3014(2) 0.2087(4) 0.1039(11) Uani 1 1 d .
N3 N -0.0186(2) 0.3006(2) 0.1652(4) 0.1044(11) Uani 1 1 d .
N4 N 0.1629(2) 0.2402(2) 0.4940(4) 0.1003(11) Uani 1 1 d .
N5 N 0.13392(19) 0.16057(19) 0.6090(4) 0.0942(10) Uani 1 1 d .
N6 N -0.0063(2) 0.0325(2) 0.6151(5) 0.0913(16) Uani 0.33333 1 d P
Zn1 Zn -0.07501(4) 0.29503(3) 0.15018(8) 0.1138(4) Uani 1 1 d .
Zn2 Zn 0.17904(3) 0.22056(3) 0.59868(6) 0.0844(3) Uani 1 1 d .
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'
Cl Cl 0.1484 0.1585 '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'
Zn Zn 0.2839 1.4301 '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 C1 C2 126.6(9) . .
C1 C2 C3 118.1(9) . .
C4 C3 C2 117.5(9) . .
C4 C3 C6 120.5(8) . .
C2 C3 C6 122.0(8) . .
C3 C4 C5 118.9(8) . .
N1 C5 C4 123.6(8) . .
C7 C6 N2 119.9(8) . .
C7 C6 C3 124.6(8) . .
N2 C6 C3 115.6(8) . .
C8 C7 C6 120.2(8) . .
C7 C8 C9 119.1(9) . .
C7 C8 C11 122.3(8) . .
C9 C8 C11 118.6(8) . .
C10 C9 C8 122.2(9) . .
N2 C10 C9 119.3(8) . .
N2 C10 C16 119.0(8) . .
C9 C10 C16 121.7(8) . .
C15 C11 C12 117.1(8) . .
C15 C11 C8 122.0(7) . .
C12 C11 C8 120.8(8) . .
C13 C12 C11 117.5(8) . .
N3 C13 C12 124.0(8) . .
N3 C14 C15 122.5(8) . .
C14 C15 C11 120.8(8) . .
C20 C16 C17 117.0(7) . .
C20 C16 C10 118.7(8) . .
C17 C16 C10 124.3(7) . .
C18 C17 C16 120.7(7) . .
N4 C18 C17 124.5(8) . .
C20 C19 N4 123.0(7) . .
C16 C20 C19 119.3(8) . .
N5 C21 C22 121.9(8) . .
C21 C22 C23 121.1(8) . .
C24 C23 C22 116.9(8) . .
C24 C23 C26 121.0(7) . .
C22 C23 C26 122.0(7) . .
C23 C24 C25 117.3(8) . .
N5 C25 C24 124.6(8) . .
C27 C26 N6 120.6(8) . 3
C27 C26 C27 120.6(8) . 3
C27 C26 C23 119.8(7) . .
N6 C26 C23 119.6(7) 3 .
C27 C26 C23 119.6(7) 3 .
C26 C27 C26 119.4(8) . 2
C5 N1 C1 115.1(8) . .
C5 N1 Zn1 121.0(6) . 11
C1 N1 Zn1 123.8(6) . 11
C10 N2 C6 119.3(8) . .
C14 N3 C13 118.0(8) . .
C14 N3 Zn1 119.3(6) . .
C13 N3 Zn1 122.4(6) . .
C18 N4 C19 115.0(7) . .
C18 N4 Zn2 125.7(6) . .
C19 N4 Zn2 118.7(5) . .
C21 N5 C25 117.9(7) . .
C21 N5 Zn2 122.7(5) . .
C25 N5 Zn2 119.1(6) . .
N3 Zn1 N1 103.4(3) . 12
N3 Zn1 Cl2 104.1(2) . .
N1 Zn1 Cl2 108.5(2) 12 .
N3 Zn1 Cl1 109.6(2) . .
N1 Zn1 Cl1 106.9(2) 12 .
Cl2 Zn1 Cl1 122.61(14) . .
N4 Zn2 N5 103.5(3) . .
N4 Zn2 Cl4 105.8(2) . .
N5 Zn2 Cl4 108.7(2) . .
N4 Zn2 Cl3 105.97(19) . .
N5 Zn2 Cl3 108.55(19) . .
Cl4 Zn2 Cl3 122.66(9) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N1 1.328(10) .
C1 C2 1.343(11) .
C2 C3 1.388(11) .
C3 C4 1.381(11) .
C3 C6 1.497(12) .
C4 C5 1.391(11) .
C5 N1 1.324(10) .
C6 C7 1.387(11) .
C6 N2 1.402(10) .
C7 C8 1.327(11) .
C8 C9 1.380(11) .
C8 C11 1.515(12) .
C9 C10 1.362(11) .
C10 N2 1.343(10) .
C10 C16 1.470(11) .
C11 C15 1.384(11) .
C11 C12 1.389(11) .
C12 C13 1.378(11) .
C13 N3 1.334(10) .
C14 N3 1.298(9) .
C14 C15 1.359(11) .
C16 C20 1.368(10) .
C16 C17 1.371(10) .
C17 C18 1.357(10) .
C18 N4 1.305(9) .
C19 C20 1.374(10) .
C19 N4 1.385(9) .
C21 N5 1.332(9) .
C21 C22 1.357(10) .
C22 C23 1.421(10) .
C23 C24 1.390(10) .
C23 C26 1.485(10) .
C24 C25 1.397(10) .
C25 N5 1.336(9) .
C26 C27 1.360(9) .
C26 N6 1.366(9) 3
C26 C27 1.366(9) 3
C27 C26 1.366(9) 2
Cl1 Zn1 2.228(3) .
Cl2 Zn1 2.211(3) .
Cl3 Zn2 2.231(2) .
Cl4 Zn2 2.213(3) .
N1 Zn1 2.051(7) 11
N3 Zn1 2.051(7) .
N4 Zn2 2.028(6) .
N5 Zn2 2.054(6) .
Zn1 N1 2.051(7) 12
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 -0.215 2724 734 ' '
2 0.333 0.667 0.452 2718 735 ' '
3 0.667 0.333 0.118 2722 734 ' '
