#------------------------------------------------------------------------------
#$Date: 2015-08-06 13:27:16 +0300 (Thu, 06 Aug 2015) $
#$Revision: 152971 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/75/7117572.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_7117572
loop_
_publ_author_name
'Martí-Rujas, Javier'
'Bonafede, Simone'
'Tushi, Dorearta'
'Cametti, Massimo'
_publ_section_title
;
 Multiple single-crystal-to-single-crystal guest exchange in a dynamic 1D
 coordination polymer.
;
_journal_issue                   62
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              12357
_journal_page_last               12360
_journal_paper_doi               10.1039/c5cc02372f
_journal_volume                  51
_journal_year                    2015
_chemical_formula_sum            'C31 H28 Cl5 N4 Zn'
_chemical_formula_weight         699.19
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           52
_space_group_name_Hall           '-P 2a 2bc'
_space_group_name_H-M_alt        'P n n a'
_symmetry_space_group_name_Hall  '-P 2a 2bc'
_symmetry_space_group_name_H-M   'P n n a'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2015-05-28 deposited with the CCDC.
2015-06-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.6608(9)
_cell_length_b                   22.7977(16)
_cell_length_c                   9.9218(7)
_cell_measurement_reflns_used    5766
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      131.666
_cell_measurement_theta_min      7.753
_cell_volume                     3316.2(4)
_computing_cell_refinement       'Bruker APEX2 Software Suite'
_computing_data_collection       'Bruker APEX2 Software Suite'
_computing_data_reduction        'Bruker APEX2 Software Suite'
_computing_molecular_graphics    'Bruker APEX2 Software Suite'
_computing_publication_material  'Bruker APEX2 Software Suite'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-1997 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.955
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       'Omega and phi scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0369
_diffrn_reflns_av_unetI/netI     0.0351
_diffrn_reflns_laue_measured_fraction_full 0.955
_diffrn_reflns_laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            10389
_diffrn_reflns_point_group_measured_fraction_full 0.955
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         66.183
_diffrn_reflns_theta_min         4.861
_diffrn_source                   'Microfocus source Incoatec'
_exptl_absorpt_coefficient_mu    4.944
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.5996
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.400
_exptl_crystal_description       prism
_exptl_crystal_F_000             1428
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.060
_refine_diff_density_max         1.124
_refine_diff_density_min         -1.361
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     221
_refine_ls_number_reflns         2870
_refine_ls_number_restraints     68
_refine_ls_restrained_S_all      1.219
_refine_ls_R_factor_all          0.0793
_refine_ls_R_factor_gt           0.0760
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1383P)²+7.4385P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2231
_refine_ls_wR_factor_ref         0.2268
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2638
_reflns_number_total             2870
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c5cc02372f2.cif
_cod_data_source_block           1_CHCl3
_cod_database_code               7117572
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.349
_shelx_estimated_absorpt_t_max   0.756
_shelxl_version_number           2014-3
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x, -y+1/2, -z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'-x+1/2, -y, z'
'-x, -y, -z'
'-x, y-1/2, z-1/2'
'x-1/2, -y-1/2, z-1/2'
'x-1/2, y, -z'
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cl1 Cl 0.39633(8) 0.32889(5) 0.31499(12) 0.0436(4) Uani 1 1 d . . . . .
Zn2 Zn 0.31950(5) 0.2500 0.2500 0.0315(3) Uani 1 2 d S T P . .
N2 N 0.0941(3) -0.12873(17) 0.6838(4) 0.0381(9) Uani 1 1 d . . . . .
N1 N 0.2282(2) 0.22422(15) 0.3955(3) 0.0300(7) Uani 1 1 d . . . . .
C1 C 0.1798(3) 0.26420(19) 0.4653(5) 0.0321(9) Uani 1 1 d . . . . .
H1 H 0.1919 0.3047 0.4520 0.039 Uiso 1 1 calc R U . . .
C2 C 0.1129(3) 0.24770(19) 0.5559(5) 0.0356(10) Uani 1 1 d . . . . .
H11 H 0.0787 0.2766 0.6028 0.043 Uiso 1 1 calc R U . . .
C3 C 0.0961(3) 0.1888(2) 0.5779(4) 0.0333(9) Uani 1 1 d . . . . .
H2 H 0.0510 0.1769 0.6411 0.040 Uiso 1 1 calc R U . . .
C6S C 0.1459(3) 0.14673(18) 0.5066(4) 0.0298(9) Uani 1 1 d . . . . .
C6 C 0.1313(3) 0.08282(19) 0.5246(4) 0.0332(9) Uani 1 1 d . . . . .
C7 C 0.1184(4) 0.0588(2) 0.6526(5) 0.0460(12) Uani 1 1 d . . . . .
H9 H 0.1172 0.0838 0.7292 0.055 Uiso 1 1 calc R U . . .
C8 C 0.1073(4) -0.0008(2) 0.6690(5) 0.0472(12) Uani 1 1 d . . . . .
H8 H 0.0987 -0.0163 0.7569 0.057 Uiso 1 1 calc R U . . .
C9 C 0.1084(3) -0.0386(2) 0.5587(5) 0.0340(9) Uani 1 1 d . . . . .
C10 C 0.1209(3) -0.0146(2) 0.4306(5) 0.0356(10) Uani 1 1 d . . . . .
H4 H 0.1214 -0.0397 0.3541 0.043 Uiso 1 1 calc R U . . .
C11 C 0.1324(3) 0.04544(19) 0.4133(4) 0.0348(9) Uani 1 1 d . . . . .
H3 H 0.1411 0.0611 0.3255 0.042 Uiso 1 1 calc R U . . .
C12 C 0.0992(3) -0.10255(19) 0.5726(4) 0.0329(9) Uani 1 1 d . . . . .
H12 H 0.0969 -0.1254 0.4927 0.039 Uiso 1 1 calc R U . . .
C13 C 0.0918(3) -0.1926(2) 0.6798(4) 0.0334(9) Uani 1 1 d . . . . .
H13 H 0.0911 -0.2059 0.5837 0.040 Uiso 1 1 calc R U . . .
C14 C 0.0079(3) -0.2165(2) 0.7512(4) 0.0344(10) Uani 1 1 d . . . . .
H6 H -0.0477 -0.2016 0.7063 0.041 Uiso 1 1 calc R U . . .
H5 H 0.0074 -0.2026 0.8458 0.041 Uiso 1 1 calc R U . . .
C5 C 0.2110(3) 0.16675(18) 0.4162(4) 0.0300(9) Uani 1 1 d . . . . .
H10 H 0.2451 0.1387 0.3664 0.036 Uiso 1 1 calc R U . . .
C15 C 0.1768(3) -0.2167(2) 0.7491(5) 0.0394(12) Uani 1 1 d . . . . .
H15A H 0.2318 -0.2025 0.7010 0.047 Uiso 1 1 calc R U . . .
H15B H 0.1794 -0.2018 0.8427 0.047 Uiso 1 1 calc R U . . .
Cl11 Cl 0.0806(4) 0.0743(2) 0.0270(5) 0.1145(17) Uani 0.5 1 d D U P A .
Cl12 Cl 0.2686(11) 0.0861(6) -0.0965(14) 0.187(9) Uani 0.218(5) 1 d D U P A 1
Cl13 Cl 0.2500 0.0000 0.1290(16) 0.231(8) Uani 0.436(9) 2 d DS TU P A 1
Cl2X Cl 0.2795(8) 0.0753(5) 0.0613(13) 0.149(5) Uani 0.282(5) 1 d D U P A 2
Cl3X Cl 0.1751(9) -0.0381(4) 0.0485(10) 0.122(4) Uani 0.282(5) 1 d D U P A 2
C51S C 0.1858(13) 0.0376(8) -0.001(2) 0.150(8) Uani 0.5 1 d D U P . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn -1.5491 0.6778 '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 Zn2 N1 98.67(18) 2 .
N1 Zn2 Cl1 111.02(10) 2 2
N1 Zn2 Cl1 107.65(10) . 2
N1 Zn2 Cl1 107.65(10) 2 .
N1 Zn2 Cl1 111.02(10) . .
Cl1 Zn2 Cl1 118.95(7) 2 .
C12 N2 C13 116.9(4) . .
C1 N1 C5 118.7(4) . .
C1 N1 Zn2 120.8(3) . .
C5 N1 Zn2 120.4(3) . .
N1 C1 C2 121.6(4) . .
N1 C1 H1 119.2 . .
C2 C1 H1 119.2 . .
C1 C2 C3 119.6(4) . .
C1 C2 H11 120.2 . .
C3 C2 H11 120.2 . .
C2 C3 C6S 119.5(4) . .
C2 C3 H2 120.2 . .
C6S C3 H2 120.2 . .
C5 C6S C3 117.5(4) . .
C5 C6S C6 120.1(4) . .
C3 C6S C6 122.5(4) . .
C11 C6 C7 118.8(4) . .
C11 C6 C6S 120.2(4) . .
C7 C6 C6S 121.0(4) . .
C8 C7 C6 120.7(5) . .
C8 C7 H9 119.7 . .
C6 C7 H9 119.7 . .
C7 C8 C9 121.1(4) . .
C7 C8 H8 119.5 . .
C9 C8 H8 119.5 . .
C8 C9 C10 118.3(4) . .
C8 C9 C12 122.6(4) . .
C10 C9 C12 119.0(4) . .
C11 C10 C9 120.9(4) . .
C11 C10 H4 119.5 . .
C9 C10 H4 119.5 . .
C10 C11 C6 120.2(4) . .
C10 C11 H3 119.9 . .
C6 C11 H3 119.9 . .
N2 C12 C9 124.0(4) . .
N2 C12 H12 118.0 . .
C9 C12 H12 118.0 . .
N2 C13 C14 111.3(4) . .
N2 C13 C15 109.1(4) . .
C14 C13 C15 108.8(3) . .
N2 C13 H13 109.2 . .
C14 C13 H13 109.2 . .
C15 C13 H13 109.2 . .
C13 C14 C14 110.5(3) . 2_546
C13 C14 H6 109.6 . .
C14 C14 H6 109.6 2_546 .
C13 C14 H5 109.6 . .
C14 C14 H5 109.6 2_546 .
H6 C14 H5 108.1 . .
N1 C5 C6S 123.1(4) . .
N1 C5 H10 118.4 . .
C6S C5 H10 118.4 . .
C15 C15 C13 111.4(4) 2_546 .
C15 C15 H15A 109.3 2_546 .
C13 C15 H15A 109.3 . .
C15 C15 H15B 109.3 2_546 .
C13 C15 H15B 109.3 . .
H15A C15 H15B 108.0 . .
C51S Cl13 C51S 89.1(17) . 4
Cl3X Cl2X C51S 93.3(12) 4 .
Cl2X Cl3X C51S 136.6(13) 4 .
Cl2X Cl3X C51S 55.6(11) 4 4
C51S Cl3X C51S 81.1(11) . 4
Cl2X C51S Cl11 113.4(13) . .
Cl2X C51S Cl3X 116.4(10) . .
Cl11 C51S Cl3X 109.3(11) . .
Cl11 C51S Cl13 124.0(14) . .
Cl11 C51S Cl12 111.1(10) . .
Cl13 C51S Cl12 107.4(11) . .
Cl2X C51S Cl3X 31.1(5) . 4
Cl11 C51S Cl3X 143.5(14) . 4
Cl3X C51S Cl3X 91.5(9) . 4
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cl1 Zn2 2.2179(12) .
Zn2 N1 2.054(3) 2
Zn2 N1 2.054(3) .
Zn2 Cl1 2.2179(12) 2
N2 C12 1.256(6) .
N2 C13 1.458(6) .
N1 C1 1.347(6) .
N1 C5 1.350(5) .
C1 C2 1.382(7) .
C1 H1 0.9500 .
C2 C3 1.384(6) .
C2 H11 0.9500 .
C3 C6S 1.398(6) .
C3 H2 0.9500 .
C6S C5 1.387(6) .
C6S C6 1.483(6) .
C6 C11 1.395(7) .
C6 C7 1.396(6) .
C7 C8 1.377(7) .
C7 H9 0.9500 .
C8 C9 1.393(7) .
C8 H8 0.9500 .
C9 C10 1.396(6) .
C9 C12 1.471(6) .
C10 C11 1.390(6) .
C10 H4 0.9500 .
C11 H3 0.9500 .
C12 H12 0.9500 .
C13 C14 1.520(6) .
C13 C15 1.525(6) .
C13 H13 1.0000 .
C14 C14 1.529(9) 2_546
C14 H6 0.9900 .
C14 H5 0.9900 .
C5 H10 0.9500 .
C15 C15 1.520(11) 2_546
C15 H15A 0.9900 .
C15 H15B 0.9900 .
Cl11 C51S 1.78(2) .
Cl12 C51S 1.89(2) .
Cl13 C51S 1.815(18) .
Cl13 C51S 1.815(18) 4
Cl2X Cl3X 1.085(15) 4
Cl2X C51S 1.74(2) .
Cl3X Cl2X 1.085(15) 4
Cl3X C51S 1.802(17) .
Cl3X C51S 2.10(2) 4
C51S Cl3X 2.10(2) 4
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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
C5 N1 C1 C2 -0.6(6) . .
Zn2 N1 C1 C2 174.8(3) . .
N1 C1 C2 C3 1.3(7) . .
C1 C2 C3 C6S -1.0(7) . .
C2 C3 C6S C5 0.2(6) . .
C2 C3 C6S C6 -179.8(4) . .
C5 C6S C6 C11 -40.3(6) . .
C3 C6S C6 C11 139.7(4) . .
C5 C6S C6 C7 138.2(5) . .
C3 C6S C6 C7 -41.8(6) . .
C11 C6 C7 C8 0.3(8) . .
C6S C6 C7 C8 -178.3(5) . .
C6 C7 C8 C9 -0.1(9) . .
C7 C8 C9 C10 -0.2(8) . .
C7 C8 C9 C12 178.4(5) . .
C8 C9 C10 C11 0.4(7) . .
C12 C9 C10 C11 -178.2(4) . .
C9 C10 C11 C6 -0.3(7) . .
C7 C6 C11 C10 0.0(7) . .
C6S C6 C11 C10 178.5(4) . .
C13 N2 C12 C9 -175.7(4) . .
C8 C9 C12 N2 -3.7(7) . .
C10 C9 C12 N2 174.9(4) . .
C12 N2 C13 C14 -123.9(4) . .
C12 N2 C13 C15 116.0(4) . .
N2 C13 C14 C14 -178.7(4) . 2_546
C15 C13 C14 C14 -58.4(5) . 2_546
C1 N1 C5 C6S -0.3(6) . .
Zn2 N1 C5 C6S -175.7(3) . .
C3 C6S C5 N1 0.5(6) . .
C6 C6S C5 N1 -179.6(4) . .
N2 C13 C15 C15 178.6(4) . 2_546
C14 C13 C15 C15 56.9(6) . 2_546
Cl3X Cl2X C51S Cl11 167.9(12) 4 .
Cl3X Cl2X C51S Cl3X 39.8(17) 4 .
Cl3X Cl2X C51S Cl13 50.0(10) 4 .
Cl3X Cl2X C51S Cl12 -92.9(12) 4 .
Cl2X Cl3X C51S Cl2X -41(3) 4 .
C51S Cl3X C51S Cl2X -45.6(19) 4 .
Cl2X Cl3X C51S Cl11 -171.2(15) 4 .
C51S Cl3X C51S Cl11 -175.8(8) 4 .
Cl2X Cl3X C51S Cl13 -52.6(19) 4 .
C51S Cl3X C51S Cl13 -57.2(9) 4 .
Cl2X Cl3X C51S Cl12 20(3) 4 .
C51S Cl3X C51S Cl12 16(2) 4 .
Cl2X Cl3X C51S Cl3X -22(2) 4 4
C51S Cl3X C51S Cl3X -26.4(13) 4 4
C51S Cl13 C51S Cl2X -94.6(9) 4 .
C51S Cl13 C51S Cl11 163.4(18) 4 .
C51S Cl13 C51S Cl3X 73.9(9) 4 .
C51S Cl13 C51S Cl12 -64.8(11) 4 .
C51S Cl13 C51S Cl3X -62.4(7) 4 4
