#------------------------------------------------------------------------------
#$Date: 2016-03-26 22:26:07 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180505 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/74/7217421.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_7217421
loop_
_publ_author_name
'Fernando, Isurika R.'
'Mo, Yirong'
'Mezei, Gellert'
_publ_section_title
;
 Metal-binding studies of linear rigid-axle [2]pseudorotaxanes with in
 situ generated anionic metal halide complexes
;
_journal_issue                   31
_journal_name_full               CrystEngComm
_journal_page_first              7320
_journal_paper_doi               10.1039/C4CE00789A
_journal_volume                  16
_journal_year                    2014
_chemical_formula_sum            'C52 H52 Cl6 N4 O8 Zn2'
_chemical_formula_weight         1204.46
_chemical_name_common            Zn
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_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
_cell_angle_alpha                90
_cell_angle_beta                 97.588(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.5117(3)
_cell_length_b                   15.9674(5)
_cell_length_c                   20.4293(6)
_cell_measurement_reflns_used    9919
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      24.6493
_cell_measurement_theta_min      2.3818
_cell_volume                     2752.23(15)
_computing_cell_refinement       'SAINT V7.68A (Bruker AXS, 2009)'
_computing_data_collection       'Bruker Instrument Service v2010.7.0.0'
_computing_data_reduction        'SAINT V7.68A (Bruker AXS, 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0619
_diffrn_reflns_av_sigmaI/netI    0.0380
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            90784
_diffrn_reflns_theta_full        30.03
_diffrn_reflns_theta_max         30.03
_diffrn_reflns_theta_min         1.62
_exptl_absorpt_coefficient_mu    1.224
_exptl_absorpt_correction_T_max  0.82
_exptl_absorpt_correction_T_min  0.74
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'
_exptl_crystal_colour            'lustrous intense blue-green'
_exptl_crystal_density_diffrn    1.453
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       trapezoidal
_exptl_crystal_F_000             1308
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.260
_exptl_crystal_size_min          0.170
_refine_diff_density_max         1.036
_refine_diff_density_min         -1.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         8046
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0763
_refine_ls_R_factor_gt           0.0518
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1000P)²+0.3993P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1497
_refine_ls_wR_factor_ref         0.1617
_reflns_number_gt                5921
_reflns_number_total             8046
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             7216357
_cod_data_source_file            c4ce00789a2.cif
_cod_data_source_block           1(ZnCl3)2
_cod_database_code               7217421
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
C C1 0.3850(4) 0.3739(2) 1.01644(15) 0.0400(7) Uani d . 1
H H1 0.4689 0.3861 1.0506 0.048 Uiso calc R 1
C C2 0.3595(3) 0.42525(19) 0.96211(14) 0.0352(6) Uani d . 1
H H2 0.4217 0.4743 0.9599 0.042 Uiso calc R 1
C C3 0.2405(3) 0.40494(17) 0.90950(14) 0.0310(6) Uani d . 1
C C4 0.1477(3) 0.33139(17) 0.91276(13) 0.0325(6) Uani d . 1
C C5 0.1708(3) 0.28351(18) 0.97232(14) 0.0340(6) Uani d . 1
C C6 0.2893(4) 0.3041(2) 1.02212(15) 0.0409(7) Uani d . 1
H H6 0.3061 0.2705 1.0608 0.049 Uiso calc R 1
C C7 0.0373(4) 0.30732(19) 0.85792(14) 0.0366(6) Uani d . 1
H H7 -0.0229 0.2574 0.8593 0.044 Uiso calc R 1
C C8 0.0186(4) 0.3575(2) 0.80247(14) 0.0375(6) Uani d . 1
H H8 -0.0539 0.341 0.7653 0.045 Uiso calc R 1
C C9 0.1034(4) 0.43196(19) 0.79947(14) 0.0363(6) Uani d . 1
H H9 0.0865 0.4659 0.761 0.044 Uiso calc R 1
C C10 0.2120(3) 0.45647(18) 0.85239(14) 0.0323(6) Uani d . 1
C C11 0.7587(3) 0.42855(16) 0.88939(13) 0.0280(5) Uani d . 1
H H11 0.7137 0.4373 0.8448 0.034 Uiso calc R 1
C C12 0.8664(3) 0.48483(15) 0.91983(12) 0.0241(5) Uani d . 1
H H12 0.8922 0.5336 0.8968 0.029 Uiso calc R 1
C C13 0.9380(3) 0.47090(14) 0.98422(11) 0.0194(4) Uani d . 1
C C14 0.8888(3) 0.40124(14) 1.01758(12) 0.0231(5) Uani d . 1
H H14 0.9318 0.3914 1.0622 0.028 Uiso calc R 1
C C15 0.7787(3) 0.34702(15) 0.98613(12) 0.0254(5) Uani d . 1
H H15 0.7463 0.2997 1.0092 0.03 Uiso calc R 1
C C23 0.2698(4) 0.5843(2) 0.80012(15) 0.0373(6) Uani d . 1
H H23A 0.1552 0.5972 0.7916 0.045 Uiso calc R 1
H H23B 0.3015 0.5583 0.7599 0.045 Uiso calc R 1
C C24 0.3619(4) 0.6631(2) 0.81583(16) 0.0425(7) Uani d . 1
H H24A 0.4741 0.6491 0.8311 0.051 Uiso calc R 1
H H24B 0.3582 0.6978 0.7755 0.051 Uiso calc R 1
C C25 0.3350(4) 0.7959(2) 0.86742(19) 0.0490(8) Uani d . 1
H H25A 0.3595 0.8134 0.8234 0.059 Uiso calc R 1
H H25B 0.4304 0.8058 0.8998 0.059 Uiso calc R 1
C C26 0.2027(4) 0.8469(2) 0.88550(16) 0.0446(8) Uani d . 1
H H26A 0.2189 0.9063 0.874 0.054 Uiso calc R 1
H H26B 0.102 0.8278 0.8601 0.054 Uiso calc R 1
C C27 0.0839(5) 0.1646(2) 1.02973(18) 0.0506(9) Uani d . 1
H H27A 0.101 0.1959 1.0719 0.061 Uiso calc R 1
H H27B 0.1773 0.1285 1.0269 0.061 Uiso calc R 1
C C28 -0.0604(5) 0.1134(2) 1.02650(19) 0.0522(9) Uani d . 1
H H28A -0.0888 0.0926 0.9808 0.063 Uiso calc R 1
H H28B -0.039 0.0642 1.0558 0.063 Uiso calc R 1
Cl Cl1 0.14610(8) 0.16512(4) 0.68249(3) 0.03174(16) Uani d . 1
Cl Cl2 0.38701(9) -0.01242(4) 0.77079(3) 0.03638(17) Uani d . 1
Cl Cl3 0.04779(11) 0.07443(5) 0.84572(4) 0.0470(2) Uani d . 1
N N2 0.7159(2) 0.36022(12) 0.92272(10) 0.0234(4) Uani d . 1
O O1 0.0624(3) 0.22200(13) 0.97488(10) 0.0407(5) Uani d . 1
O O2 0.2999(2) 0.52718(13) 0.85475(10) 0.0361(5) Uani d . 1
O O3 0.2975(3) 0.70918(13) 0.86607(11) 0.0430(5) Uani d . 1
O O4 -0.1931(3) 0.15982(13) 1.04594(11) 0.0413(5) Uani d . 1
Zn Zn1 0.23128(4) 0.100943(19) 0.778549(15) 0.03194(12) Uani d . 1
N N1 0.3938(3) 0.18705(14) 0.82442(11) 0.0377(6) Uani d . 1
C C16 0.3995(3) 0.26447(16) 0.80377(13) 0.0266(5) Uani d . 1
H H16 0.3289 0.2808 0.766 0.032 Uiso calc R 1
C C17 0.5035(3) 0.32391(16) 0.83438(13) 0.0271(5) Uani d . 1
H H17 0.5034 0.3797 0.8181 0.033 Uiso calc R 1
C C18 0.6060(3) 0.30020(16) 0.88843(13) 0.0290(5) Uani d . 1
C C19 0.6082(7) 0.2191(2) 0.9086(2) 0.106(2) Uani d . 1
H H19 0.6821 0.2003 0.9445 0.128 Uiso calc R 1
C C20 0.4983(8) 0.1643(3) 0.8749(3) 0.118(3) Uani d . 1
H H20 0.4986 0.1076 0.889 0.142 Uiso calc R 1
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'
Zn Zn 0.2839 1.4301 '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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
C2 C1 C6 . . 120.8(3)
C1 C2 C3 . . 119.9(3)
C2 C3 C4 . . 120.0(3)
C2 C3 C10 . . 121.2(3)
C4 C3 C10 . . 118.7(3)
C7 C4 C3 . . 120.1(3)
C7 C4 C5 . . 122.1(3)
C3 C4 C5 . . 117.8(3)
O1 C5 C6 . . 125.6(3)
O1 C5 C4 . . 113.8(3)
C6 C5 C4 . . 120.5(3)
C5 C6 C1 . . 120.6(3)
C8 C7 C4 . . 119.0(3)
C7 C8 C9 . . 121.8(3)
C10 C9 C8 . . 120.2(3)
O2 C10 C9 . . 125.0(3)
O2 C10 C3 . . 114.9(3)
C9 C10 C3 . . 120.1(3)
N2 C11 C12 . . 120.3(2)
C11 C12 C13 . . 120.4(2)
C12 C13 C14 . . 117.7(2)
C12 C13 C13 . 3_767 120.5(3)
C14 C13 C13 . 3_767 121.8(3)
C15 C14 C13 . . 120.3(2)
N2 C15 C14 . . 120.7(2)
O2 C23 C24 . . 109.4(3)
O3 C24 C23 . . 110.3(3)
O3 C25 C26 . . 111.5(3)
O4 C26 C25 3_567 . 110.5(3)
O1 C27 C28 . . 107.4(3)
O4 C28 C27 . . 112.3(3)
C15 N2 C11 . . 120.4(2)
C15 N2 C18 . . 120.5(2)
C11 N2 C18 . . 119.0(2)
C5 O1 C27 . . 118.3(3)
C10 O2 C23 . . 117.5(2)
C25 O3 C24 . . 114.2(2)
C26 O4 C28 3_567 . 112.4(3)
N1 Zn1 Cl1 . . 102.14(7)
N1 Zn1 Cl3 . . 108.83(8)
Cl1 Zn1 Cl3 . . 116.63(3)
N1 Zn1 Cl2 . . 101.50(8)
Cl1 Zn1 Cl2 . . 115.36(3)
Cl3 Zn1 Cl2 . . 110.64(3)
C16 N1 C20 . . 117.5(3)
C16 N1 Zn1 . . 121.93(19)
C20 N1 Zn1 . . 120.6(2)
N1 C16 C17 . . 123.3(2)
C18 C17 C16 . . 118.4(2)
C19 C18 C17 . . 119.4(3)
C19 C18 N2 . . 120.0(3)
C17 C18 N2 . . 120.5(2)
C18 C19 C20 . . 117.8(3)
N1 C20 C19 . . 123.5(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
C1 C2 . 1.374(4)
C1 C6 . 1.394(5)
C2 C3 . 1.414(4)
C3 C4 . 1.422(4)
C3 C10 . 1.422(4)
C4 C7 . 1.417(4)
C4 C5 . 1.428(4)
C5 O1 . 1.354(4)
C5 C6 . 1.374(4)
C7 C8 . 1.380(4)
C8 C9 . 1.396(5)
C9 C10 . 1.383(4)
C10 O2 . 1.352(4)
C11 N2 . 1.361(3)
C11 C12 . 1.373(3)
C12 C13 . 1.393(3)
C13 C14 . 1.397(3)
C13 C13 3_767 1.487(4)
C14 C15 . 1.372(3)
C15 N2 . 1.351(3)
C23 O2 . 1.438(3)
C23 C24 . 1.494(5)
C24 O3 . 1.430(4)
C25 O3 . 1.421(4)
C25 C26 . 1.476(5)
C26 O4 3_567 1.418(4)
C27 O1 . 1.440(4)
C27 C28 . 1.470(5)
C28 O4 . 1.449(4)
Cl1 Zn1 . 2.2475(7)
Cl2 Zn1 . 2.2615(8)
Cl3 Zn1 . 2.2512(9)
N2 C18 . 1.453(3)
O4 C26 3_567 1.418(4)
Zn1 N1 . 2.083(2)
N1 C16 . 1.309(3)
N1 C20 . 1.320(4)
C16 C17 . 1.389(3)
C17 C18 . 1.367(4)
C18 C19 . 1.359(4)
C19 C20 . 1.395(5)
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
_geom_torsion
C6 C1 C2 C3 . . -3.5(4)
C1 C2 C3 C4 . . -0.2(4)
C1 C2 C3 C10 . . -179.5(3)
C2 C3 C4 C7 . . -174.9(3)
C10 C3 C4 C7 . . 4.5(4)
C2 C3 C4 C5 . . 4.7(4)
C10 C3 C4 C5 . . -175.9(2)
C7 C4 C5 O1 . . -9.6(4)
C3 C4 C5 O1 . . 170.8(2)
C7 C4 C5 C6 . . 173.8(3)
C3 C4 C5 C6 . . -5.8(4)
O1 C5 C6 C1 . . -173.8(3)
C4 C5 C6 C1 . . 2.4(4)
C2 C1 C6 C5 . . 2.4(5)
C3 C4 C7 C8 . . -1.8(4)
C5 C4 C7 C8 . . 178.6(3)
C4 C7 C8 C9 . . -1.1(4)
C7 C8 C9 C10 . . 1.3(5)
C8 C9 C10 O2 . . -179.8(3)
C8 C9 C10 C3 . . 1.5(4)
C2 C3 C10 O2 . . -3.8(4)
C4 C3 C10 O2 . . 176.9(2)
C2 C3 C10 C9 . . 175.0(3)
C4 C3 C10 C9 . . -4.4(4)
N2 C11 C12 C13 . . 2.7(4)
C11 C12 C13 C14 . . -4.1(4)
C11 C12 C13 C13 . 3_767 176.2(3)
C12 C13 C14 C15 . . 2.9(4)
C13 C13 C14 C15 3_767 . -177.5(3)
C13 C14 C15 N2 . . -0.2(4)
O2 C23 C24 O3 . . -70.2(3)
O3 C25 C26 O4 . 3_567 75.0(4)
O1 C27 C28 O4 . . -73.6(4)
C14 C15 N2 C11 . . -1.3(4)
C14 C15 N2 C18 . . 176.5(2)
C12 C11 N2 C15 . . 0.1(4)
C12 C11 N2 C18 . . -177.8(2)
C6 C5 O1 C27 . . -9.7(4)
C4 C5 O1 C27 . . 173.9(2)
C28 C27 O1 C5 . . 171.2(3)
C9 C10 O2 C23 . . 4.8(4)
C3 C10 O2 C23 . . -176.4(2)
C24 C23 O2 C10 . . 172.4(2)
C26 C25 O3 C24 . . 144.5(3)
C23 C24 O3 C25 . . -157.9(3)
C27 C28 O4 C26 . 3_567 -90.7(3)
Cl1 Zn1 N1 C16 . . 14.9(2)
Cl3 Zn1 N1 C16 . . -109.0(2)
Cl2 Zn1 N1 C16 . . 134.3(2)
Cl1 Zn1 N1 C20 . . -163.3(5)
Cl3 Zn1 N1 C20 . . 72.7(5)
Cl2 Zn1 N1 C20 . . -44.0(5)
C20 N1 C16 C17 . . -3.5(6)
Zn1 N1 C16 C17 . . 178.2(2)
N1 C16 C17 C18 . . 0.6(4)
C16 C17 C18 C19 . . 3.0(5)
C16 C17 C18 N2 . . -179.2(2)
C15 N2 C18 C19 . . -24.0(5)
C11 N2 C18 C19 . . 153.9(4)
C15 N2 C18 C17 . . 158.2(3)
C11 N2 C18 C17 . . -23.9(4)
C17 C18 C19 C20 . . -3.4(8)
N2 C18 C19 C20 . . 178.8(5)
C16 N1 C20 C19 . . 3.0(10)
Zn1 N1 C20 C19 . . -178.7(6)
C18 C19 C20 N1 . . 0.5(11)
