#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:23:56 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179375 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/72/4327243.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_4327243
loop_
_publ_author_name
'Zhi-Min Liu'
'Yu Liu'
'Sheng-Run Zheng'
'Zhi-Quan Yu'
'Mei Pan'
'Cheng-Yong Su'
_publ_section_title
;
 Assembly of Trigonal and Tetragonal Prismatic Cages from Octahedral Metal
 Ions and a Flexible Molecular Clip
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5814
_journal_page_last               5816
_journal_paper_doi               10.1021/ic062270+
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C154 H146 Cl6 F24 N24 O60 S8 Zn4'
_chemical_formula_weight         4479.61
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           176
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-P 6c'
_symmetry_space_group_name_H-M   'P 63/m'
_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            1
_cell_length_a                   16.5876(7)
_cell_length_b                   16.5876(7)
_cell_length_c                   19.0040(7)
_cell_measurement_reflns_used    4385
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.3578
_cell_measurement_theta_min      2.6724
_cell_volume                     4528.4(3)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET)
(compiled Aug 28 2006,13:05:05)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET)
(compiled Aug 28 2006,13:05:05)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET)
(compiled Aug 28 2006,13:05:05)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.0855
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Gemini S Untra'
_diffrn_measurement_method       'ω scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0313
_diffrn_reflns_av_sigmaI/netI    0.0382
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            11147
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         2.68
_exptl_absorpt_coefficient_mu    0.823
_exptl_absorpt_correction_T_max  0.8526
_exptl_absorpt_correction_T_min  0.7615
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET)
(compiled Aug 28 2006,13:05:05)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.643
_exptl_crystal_description       Block
_exptl_crystal_F_000             2284
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.252
_refine_diff_density_min         -1.012
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     241
_refine_ls_number_reflns         3522
_refine_ls_number_restraints     49
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0809
_refine_ls_R_factor_gt           0.0569
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0623P)²+6.6385P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1345
_refine_ls_wR_factor_ref         0.1480
_reflns_number_gt                2573
_reflns_number_total             3522
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0622702Bsi20061129_111444_4.cif
_cod_data_source_block           Compd1
_cod_database_code               4327243
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z-1/2'
'-y, x-y, -z-1/2'
'-x+y, -x, -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
_atom_site_disorder_group
Zn1 Zn 0.3333 0.6667 0.44221(3) 0.0336(2) Uani 1 3 d S .
S1 S -0.11537(8) 0.50579(9) 0.7500 0.0390(3) Uani 1 2 d S .
N1 N 0.2065(2) 0.5759(2) 0.49783(15) 0.0391(7) Uani 1 1 d . .
N2 N 0.0351(2) 0.2739(2) 0.58155(15) 0.0391(7) Uani 1 1 d . .
O1 O -0.12247(19) 0.1999(2) 0.59832(15) 0.0667(9) Uani 1 1 d . .
O2 O 0.1924(2) 0.3402(3) 0.59671(16) 0.0639(9) Uani 1 1 d . .
C1 C 0.1628(2) 0.4832(3) 0.48970(17) 0.0365(8) Uani 1 1 d . .
H1A H 0.1884 0.4585 0.4589 0.044 Uiso 1 1 calc R .
C2 C 0.0818(2) 0.4226(3) 0.52472(17) 0.0381(8) Uani 1 1 d . .
C3 C 0.0451(3) 0.4605(3) 0.5707(2) 0.0507(10) Uani 1 1 d . .
H3A H -0.0085 0.4219 0.5961 0.061 Uiso 1 1 calc R .
C4 C 0.0880(3) 0.5552(3) 0.5787(2) 0.0572(11) Uani 1 1 d . .
H4A H 0.0631 0.5815 0.6086 0.069 Uiso 1 1 calc R .
C5 C 0.1678(3) 0.6103(3) 0.5420(2) 0.0509(10) Uani 1 1 d . .
H5A H 0.1968 0.6745 0.5478 0.061 Uiso 1 1 calc R .
C6 C 0.0396(3) 0.3195(3) 0.51479(18) 0.0434(9) Uani 1 1 d . .
H6A H -0.0226 0.2939 0.4955 0.052 Uiso 1 1 calc R .
H6B H 0.0767 0.3075 0.4815 0.052 Uiso 1 1 calc R .
C7 C -0.0462(3) 0.2174(3) 0.61766(18) 0.0435(9) Uani 1 1 d . .
C8 C -0.0225(3) 0.1842(3) 0.68467(19) 0.0460(9) Uani 1 1 d . .
H8A H -0.0487 0.1166 0.6836 0.055 Uiso 1 1 calc R .
C9 C -0.0571(4) 0.2132(4) 0.7500 0.0429(12) Uani 1 2 d S .
H9A H -0.1251 0.1843 0.7500 0.052 Uiso 1 2 calc SR .
C10 C -0.0110(4) 0.3167(4) 0.7500 0.0436(12) Uani 1 2 d S .
H10A H -0.0443 0.3481 0.7500 0.052 Uiso 1 2 calc SR .
C11 C 0.1217(4) 0.2985(4) 0.7500 0.0443(12) Uani 1 2 d S .
H11A H 0.1898 0.3350 0.7500 0.053 Uiso 1 2 calc SR .
C12 C 0.0844(3) 0.2345(3) 0.68515(19) 0.0446(9) Uani 1 1 d . .
H12A H 0.1055 0.1889 0.6861 0.053 Uiso 1 1 calc R .
C13 C 0.1137(3) 0.2887(3) 0.6172(2) 0.0448(9) Uani 1 1 d . .
C15 C -0.0289(4) 0.6282(4) 0.7500 0.0551(15) Uani 1 2 d S .
C14 C 0.0796(4) 0.3599(4) 0.7500 0.0454(13) Uani 1 2 d S .
H20A H 0.1157 0.4245 0.7500 0.055 Uiso 1 2 calc SR .
F1 F -0.0369(2) 0.6697(2) 0.6943(2) 0.1032(12) Uani 1 1 d . .
F2 F 0.0549(2) 0.6385(2) 0.7500 0.0738(12) Uani 1 2 d SD .
O3 O -0.0960(2) 0.4718(2) 0.68666(16) 0.0649(9) Uani 1 1 d . .
O4 O -0.2030(3) 0.5038(3) 0.7500 0.0552(11) Uani 1 2 d S .
O5 O 0.24232(18) 0.68802(18) 0.37371(13) 0.0405(6) Uani 1 1 d D .
H12 H 0.187(2) 0.6327(19) 0.370(2) 0.061 Uiso 1 1 d D .
H11 H 0.267(3) 0.730(2) 0.3363(17) 0.061 Uiso 1 1 d D .
C16 C 0.3333 0.6667 0.729(2) 0.151(12) Uani 0.50 3 d SPU 1
Cl1 Cl 0.2461(9) 0.6693(12) 0.7500 0.225(6) Uani 0.40 2 d SPDU 1
Cl1' Cl 0.2702(10) 0.6777(15) 0.6898(6) 0.253(7) Uani 0.30 1 d PU 2
C17 C 0.0000 0.0000 0.5497(3) 0.336(9) Uani 0.50 3 d SPDU .
S2 S 0.0000 0.0000 0.5497(3) 0.336(9) Uani 0.50 3 d SPDU .
O6 O 0.0927(8) -0.0018(10) 0.4549(6) 0.302(5) Uani 0.50 1 d PU .
F3 F 0.0927(8) -0.0018(10) 0.4549(6) 0.302(5) Uani 0.50 1 d PDU .
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'
F F 0.0171 0.0103 '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'
Cl Cl 0.1484 0.1585 '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
O5 Zn1 O5 87.22(10) . 2_665
O5 Zn1 O5 87.22(10) . 3_565
O5 Zn1 O5 87.22(10) 2_665 3_565
O5 Zn1 N1 90.65(10) . 3_565
O5 Zn1 N1 170.84(11) 2_665 3_565
O5 Zn1 N1 83.78(11) 3_565 3_565
O5 Zn1 N1 83.78(11) . .
O5 Zn1 N1 90.65(11) 2_665 .
O5 Zn1 N1 170.84(11) 3_565 .
N1 Zn1 N1 97.98(10) 3_565 .
O5 Zn1 N1 170.84(11) . 2_665
O5 Zn1 N1 83.78(11) 2_665 2_665
O5 Zn1 N1 90.65(11) 3_565 2_665
N1 Zn1 N1 97.98(11) 3_565 2_665
N1 Zn1 N1 97.98(10) . 2_665
O3 S1 O3 114.3(3) . 10_557
O3 S1 O4 114.48(16) . .
O3 S1 O4 114.48(16) 10_557 .
O3 S1 C15 103.55(17) . .
O3 S1 C15 103.55(17) 10_557 .
O4 S1 C15 104.6(3) . .
C1 N1 C5 117.3(3) . .
C1 N1 Zn1 121.6(2) . .
C5 N1 Zn1 121.1(3) . .
C13 N2 C7 113.1(3) . .
C13 N2 C6 122.4(3) . .
C7 N2 C6 124.4(3) . .
N1 C1 C2 123.4(3) . .
N1 C1 H1A 118.3 . .
C2 C1 H1A 118.3 . .
C1 C2 C3 117.6(4) . .
C1 C2 C6 119.9(3) . .
C3 C2 C6 122.5(3) . .
C4 C3 C2 119.8(4) . .
C4 C3 H3A 120.1 . .
C2 C3 H3A 120.1 . .
C5 C4 C3 119.0(4) . .
C5 C4 H4A 120.5 . .
C3 C4 H4A 120.5 . .
N1 C5 C4 123.0(4) . .
N1 C5 H5A 118.5 . .
C4 C5 H5A 118.5 . .
N2 C6 C2 110.8(3) . .
N2 C6 H6A 109.5 . .
C2 C6 H6A 109.5 . .
N2 C6 H6B 109.5 . .
C2 C6 H6B 109.5 . .
H6A C6 H6B 108.1 . .
O1 C7 N2 124.3(4) . .
O1 C7 C8 126.9(3) . .
N2 C7 C8 108.8(3) . .
C7 C8 C12 104.3(3) . .
C7 C8 C9 111.1(4) . .
C12 C8 C9 109.5(3) . .
C7 C8 H8A 110.6 . .
C12 C8 H8A 110.6 . .
C9 C8 H8A 110.6 . .
C10 C9 C8 107.6(3) . .
C10 C9 C8 107.6(3) . 10_557
C8 C9 C8 107.3(5) . 10_557
C10 C9 H9A 111.4 . .
C8 C9 H9A 111.4 . .
C8 C9 H9A 111.4 10_557 .
C14 C10 C9 114.8(5) . .
C14 C10 H10A 122.6 . .
C9 C10 H10A 122.6 . .
C14 C11 C12 107.9(3) . .
C14 C11 C12 107.9(3) . 10_557
C12 C11 C12 106.3(5) . 10_557
C14 C11 H11A 111.5 . .
C12 C11 H11A 111.5 . .
C12 C11 H11A 111.5 10_557 .
C13 C12 C8 105.0(3) . .
C13 C12 C11 112.0(3) . .
C8 C12 C11 109.6(3) . .
C13 C12 H12A 110.0 . .
C8 C12 H12A 110.0 . .
C11 C12 H12A 110.0 . .
O2 C13 N2 123.8(4) . .
O2 C13 C12 127.5(4) . .
N2 C13 C12 108.7(3) . .
F1 C15 F1 108.3(6) . 10_557
F1 C15 F2 108.1(3) . .
F1 C15 F2 108.1(3) 10_557 .
F1 C15 S1 111.1(3) . .
F1 C15 S1 111.1(3) 10_557 .
F2 C15 S1 109.9(4) . .
C10 C14 C11 115.4(5) . .
C10 C14 H20A 122.3 . .
C11 C14 H20A 122.3 . .
Zn1 O5 H12 109(3) . .
Zn1 O5 H11 120(3) . .
H12 O5 H11 122(3) . .
C16 C16 Cl1 74.8(14) 10_557 .
C16 C16 Cl1 74.8(14) 10_557 3_565
Cl1 C16 Cl1 113.4(12) . 3_565
C16 C16 Cl1 74.8(14) 10_557 2_665
Cl1 C16 Cl1 113.4(12) . 2_665
Cl1 C16 Cl1 113.4(12) 3_565 2_665
C16 Cl1 C16 30(3) . 10_557
Cl1' Cl1' Cl1' 60.000(2) 3_565 2_665
Cl1' Cl1' Cl1' 90.000(3) 3_565 10_557
Cl1' Cl1' Cl1' 90.000(1) 2_665 10_557
F3 C17 O6 0.000(1) 8_556 8_556
F3 C17 F3 119.69(10) 8_556 9_556
O6 C17 F3 119.69(10) 8_556 9_556
F3 C17 O6 119.69(10) 8_556 9_556
O6 C17 O6 119.69(10) 8_556 9_556
F3 C17 O6 0.0(18) 9_556 9_556
F3 C17 O6 119.69(10) 8_556 7_556
O6 C17 O6 119.69(10) 8_556 7_556
F3 C17 O6 119.69(10) 9_556 7_556
O6 C17 O6 119.69(10) 9_556 7_556
F3 C17 F3 119.69(10) 8_556 7_556
O6 C17 F3 119.69(10) 8_556 7_556
F3 C17 F3 119.69(10) 9_556 7_556
O6 C17 F3 119.69(10) 9_556 7_556
O6 C17 F3 0.00(6) 7_556 7_556
F3 C17 S2 86.8(5) 8_556 7_556
O6 C17 S2 86.8(5) 8_556 7_556
F3 C17 S2 86.8(5) 9_556 7_556
O6 C17 S2 86.8(5) 9_556 7_556
O6 C17 S2 86.8(5) 7_556 7_556
F3 C17 S2 86.8(5) 7_556 7_556
F3 C17 C17 86.8(5) 8_556 7_556
O6 C17 C17 86.8(5) 8_556 7_556
F3 C17 C17 86.8(5) 9_556 7_556
O6 C17 C17 86.8(5) 9_556 7_556
O6 C17 C17 86.8(5) 7_556 7_556
F3 C17 C17 86.8(5) 7_556 7_556
S2 C17 C17 0.0 7_556 7_556
C17 O6 S2 0.0 7_556 7_556
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 O5 2.153(2) .
Zn1 O5 2.153(2) 2_665
Zn1 O5 2.153(2) 3_565
Zn1 N1 2.154(3) 3_565
Zn1 N1 2.154(3) .
Zn1 N1 2.154(3) 2_665
S1 O3 1.433(3) .
S1 O3 1.433(3) 10_557
S1 O4 1.437(4) .
S1 C15 1.807(6) .
N1 C1 1.341(5) .
N1 C5 1.344(5) .
N2 C13 1.379(5) .
N2 C7 1.379(5) .
N2 C6 1.459(5) .
O1 C7 1.205(5) .
O2 C13 1.212(5) .
C1 C2 1.382(5) .
C1 H1A 0.9300 .
C2 C3 1.382(5) .
C2 C6 1.502(5) .
C3 C4 1.371(6) .
C3 H3A 0.9300 .
C4 C5 1.366(6) .
C4 H4A 0.9300 .
C5 H5A 0.9300 .
C6 H6A 0.9700 .
C6 H6B 0.9700 .
C7 C8 1.515(5) .
C8 C12 1.537(5) .
C8 C9 1.541(5) .
C8 H8A 0.9800 .
C9 C10 1.491(8) .
C9 C8 1.541(5) 10_557
C9 H9A 0.9800 .
C10 C14 1.302(8) .
C10 H10A 0.9300 .
C11 C14 1.493(8) .
C11 C12 1.540(5) .
C11 C12 1.540(5) 10_557
C11 H11A 0.9800 .
C12 C13 1.508(5) .
C12 H12A 0.9800 .
C15 F1 1.305(4) .
C15 F1 1.305(4) 10_557
C15 F2 1.313(7) .
C14 H20A 0.9300 .
O5 H12 0.924(19) .
O5 H11 0.930(19) .
C16 C16 0.80(8) 10_557
C16 Cl1 1.523(13) .
C16 Cl1 1.523(13) 3_565
C16 Cl1 1.523(13) 2_665
Cl1 C16 1.523(13) 10_557
Cl1' Cl1' 1.99(3) 3_565
Cl1' Cl1' 1.99(3) 2_665
Cl1' Cl1' 2.29(2) 10_557
C17 F3 1.555(10) 8_556
C17 O6 1.555(10) 8_556
C17 F3 1.555(10) 9_556
C17 O6 1.555(10) 9_556
C17 O6 1.555(10) 7_556
C17 F3 1.555(10) 7_556
C17 S2 1.889(11) 7_556
O6 C17 1.555(10) 7_556
O6 S2 1.555(10) 7_556
