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#$Date: 2016-03-21 18:20:39 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178809 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/63/4106351.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_4106351
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            'C20 H14 I2 N4 Zn'
_chemical_formula_weight         629.52
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 103.29(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.7312(19)
_cell_length_b                   11.277(2)
_cell_length_c                   18.980(4)
_cell_measurement_reflns_used    4008
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.28
_cell_measurement_theta_min      2.15
_cell_volume                     2027.1(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_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  0.2170
_diffrn_reflns_av_sigmaI/netI    0.2480
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            12160
_diffrn_reflns_theta_full        26.80
_diffrn_reflns_theta_max         26.80
_diffrn_reflns_theta_min         2.15
_exptl_absorpt_coefficient_mu    4.270
_exptl_absorpt_correction_T_max  0.69839
_exptl_absorpt_correction_T_min  0.34355
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   'A.L.Spek (2003) J. Appl. Cryst. 36, 7-13'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.063
_exptl_crystal_description       plate
_exptl_crystal_F_000             1192
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.150
_refine_diff_density_min         -1.201
_refine_diff_density_rms         0.212
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.839
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         4284
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.839
_refine_ls_R_factor_all          0.1717
_refine_ls_R_factor_gt           0.0726
_refine_ls_shift/su_max          0.029
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0300P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1471
_refine_ls_wR_factor_ref         0.1710
_reflns_number_gt                1650
_reflns_number_total             4284
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            ja2030273_si_004.cif
_cod_data_source_block           compound3
_cod_original_cell_volume        2027.0(7)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4106351
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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
I1 I 0.25524(13) 0.63149(10) 0.21271(6) 0.0562(3) Uani 1 1 d .
I2 I -0.07358(11) 0.90544(10) 0.15229(6) 0.0546(3) Uani 1 1 d .
Zn1 Zn 0.18527(19) 0.84697(16) 0.19347(9) 0.0474(5) Uani 1 1 d .
N2 N 0.2742(13) 0.9406(10) 0.2856(7) 0.050(3) Uani 1 1 d .
N1 N 0.2921(13) 0.9295(10) 0.1248(6) 0.045(3) Uani 1 1 d .
N3 N 0.4528(14) 1.2411(11) 0.4810(7) 0.047(3) Uani 1 1 d .
N4 N 1.1900(15) 1.1601(15) 0.5961(8) 0.065(4) Uani 1 1 d .
C8 C 0.4391(15) 1.0776(13) 0.4005(8) 0.040(3) Uani 1 1 d .
C9 C 0.3027(17) 1.1125(13) 0.3634(8) 0.052(4) Uani 1 1 d .
H9 H 0.2649 1.1835 0.3752 0.063 Uiso 1 1 calc R
C4 C 0.5192(17) 1.0060(15) 0.1155(9) 0.054(5) Uani 1 1 d .
H4 H 0.6170 1.0029 0.1312 0.065 Uiso 1 1 calc R
C5 C 0.4383(18) 0.9356(17) 0.1391(9) 0.062(5) Uani 1 1 d .
H5 H 0.4848 0.8786 0.1713 0.075 Uiso 1 1 calc R
C6 C 0.4065(18) 0.8997(15) 0.3285(10) 0.061(5) Uani 1 1 d .
H6 H 0.4364 0.8227 0.3230 0.074 Uiso 1 1 calc R
C1 C 0.2305(15) 1.0107(12) 0.0782(8) 0.042(4) Uani 1 1 d .
H1 H 0.1325 1.0162 0.0677 0.050 Uiso 1 1 calc R
C7 C 0.4874(17) 0.9730(15) 0.3767(7) 0.045(4) Uani 1 1 d .
H7 H 0.5813 0.9522 0.3952 0.054 Uiso 1 1 calc R
C11 C 0.5204(17) 1.1575(15) 0.4531(8) 0.052(4) Uani 1 1 d .
C12 C 0.6631(15) 1.1396(15) 0.4744(8) 0.053(4) Uani 1 1 d .
H12 H 0.7065 1.0790 0.4542 0.064 Uiso 1 1 calc R
C3 C 0.4498(14) 1.0901(13) 0.0633(7) 0.037(3) Uani 1 1 d .
C14 C 0.6754(14) 1.3015(12) 0.5566(7) 0.034(3) Uani 1 1 d .
H14 H 0.7253 1.3538 0.5910 0.041 Uiso 1 1 calc R
C2 C 0.3054(15) 1.0890(14) 0.0439(8) 0.046(4) Uani 1 1 d .
H2 H 0.2574 1.1400 0.0081 0.055 Uiso 1 1 calc R
C20 C 0.9729(16) 1.2170(16) 0.6248(10) 0.060(5) Uani 1 1 d .
H20 H 0.9285 1.2434 0.6603 0.072 Uiso 1 1 calc R
C13 C 0.7440(15) 1.2169(11) 0.5287(7) 0.036(3) Uani 1 1 d .
C16 C 0.8980(18) 1.1950(14) 0.5516(8) 0.052(4) Uani 1 1 d .
C19 C 1.118(2) 1.1956(16) 0.6382(10) 0.065(5) Uani 1 1 d .
H19 H 1.1683 1.2099 0.6854 0.078 Uiso 1 1 calc R
C17 C 0.9780(16) 1.1628(15) 0.5011(7) 0.044(4) Uani 1 1 d .
H17 H 0.9353 1.1568 0.4521 0.053 Uiso 1 1 calc R
C10 C 0.2220(17) 1.0387(16) 0.3074(11) 0.068(5) Uani 1 1 d .
H10 H 0.1298 1.0605 0.2857 0.082 Uiso 1 1 calc R
C18 C 1.1203(19) 1.1405(17) 0.5257(11) 0.073(6) Uani 1 1 d .
H18 H 1.1707 1.1111 0.4934 0.088 Uiso 1 1 calc R
C15 C 0.5305(16) 1.3107(13) 0.5341(8) 0.045(4) 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'
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'
I I -0.4742 1.8119 '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_3
N2 Zn1 N1 97.5(5) .
N2 Zn1 I1 108.9(3) .
N1 Zn1 I1 111.5(3) .
N2 Zn1 I2 108.8(3) .
N1 Zn1 I2 107.2(3) .
I1 Zn1 I2 120.52(8) .
C10 N2 C6 116.8(13) .
C10 N2 Zn1 125.4(11) .
C6 N2 Zn1 117.8(9) .
C1 N1 C5 112.6(14) .
C1 N1 Zn1 121.3(10) .
C5 N1 Zn1 122.8(10) .
C11 N3 C15 117.6(14) .
C19 N4 C18 117.1(15) .
C7 C8 C9 115.3(13) .
C7 C8 C11 125.9(14) .
C9 C8 C11 118.5(14) .
C10 C9 C8 120.1(14) .
C5 C4 C3 115.4(15) .
C4 C5 N1 130.7(17) .
C7 C6 N2 119.9(15) .
N1 C1 C2 123.1(13) .
C6 C7 C8 123.8(15) .
N3 C11 C12 123.3(15) .
N3 C11 C8 118.5(15) .
C12 C11 C8 118.1(15) .
C11 C12 C13 118.2(15) .
C2 C3 C4 118.3(14) .
C2 C3 C15 119.1(13) 4_585
C4 C3 C15 122.3(12) 4_585
C13 C14 C15 119.8(13) .
C3 C2 C1 119.6(14) .
C19 C20 C16 114.4(16) .
C14 C13 C12 118.3(14) .
C14 C13 C16 124.3(12) .
C12 C13 C16 117.4(13) .
C17 C16 C20 117.7(15) .
C17 C16 C13 121.4(14) .
C20 C16 C13 120.6(14) .
N4 C19 C20 129.2(18) .
C18 C17 C16 119.0(14) .
N2 C10 C9 122.2(15) .
N4 C18 C17 122.2(14) .
N3 C15 C14 122.7(13) .
N3 C15 C3 116.3(13) 4_586
C14 C15 C3 120.8(12) 4_586
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
I1 Zn1 2.527(2) .
I2 Zn1 2.547(2) .
Zn1 N2 2.055(13) .
Zn1 N1 2.066(13) .
N2 C10 1.32(2) .
N2 C6 1.43(2) .
N1 C1 1.317(17) .
N1 C5 1.39(2) .
N3 C11 1.327(19) .
N3 C15 1.362(18) .
N4 C19 1.24(2) .
N4 C18 1.37(2) .
C8 C7 1.38(2) .
C8 C9 1.41(2) .
C8 C11 1.44(2) .
C9 C10 1.43(2) .
C4 C5 1.27(2) .
C4 C3 1.42(2) .
C6 C7 1.35(2) .
C1 C2 1.40(2) .
C11 C12 1.37(2) .
C12 C13 1.44(2) .
C3 C2 1.369(19) .
C3 C15 1.542(19) 4_585
C14 C13 1.342(19) .
C14 C15 1.38(2) .
C20 C19 1.40(2) .
C20 C16 1.43(2) .
C13 C16 1.48(2) .
C16 C17 1.41(2) .
C17 C18 1.38(2) .
C15 C3 1.542(19) 4_586
