#------------------------------------------------------------------------------
#$Date: 2015-08-06 13:27:16 +0300 (Thu, 06 Aug 2015) $
#$Revision: 152971 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/75/7117574.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_7117574
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            'C32 H28 Cl4 N4 Zn'
_chemical_formula_weight         675.75
_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                   14.7255(9)
_cell_length_b                   22.4827(15)
_cell_length_c                   10.2852(7)
_cell_measurement_reflns_used    4396
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      129.546
_cell_measurement_theta_min      9.456
_cell_volume                     3405.1(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 0.919
_diffrn_measured_fraction_theta_max 0.966
_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  0.1844
_diffrn_reflns_av_unetI/netI     0.0879
_diffrn_reflns_laue_measured_fraction_full 0.919
_diffrn_reflns_laue_measured_fraction_max 0.966
_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       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            11111
_diffrn_reflns_point_group_measured_fraction_full 0.919
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         65.608
_diffrn_reflns_theta_min         4.728
_diffrn_source                   'Microfocus source Incoatec'
_exptl_absorpt_coefficient_mu    4.092
_exptl_absorpt_correction_T_max  0.7527
_exptl_absorpt_correction_T_min  0.5772
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.318
_exptl_crystal_description       prism
_exptl_crystal_F_000             1384
_exptl_crystal_size_max          0.265
_exptl_crystal_size_mid          0.095
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.944
_refine_diff_density_min         -0.456
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     225
_refine_ls_number_reflns         2844
_refine_ls_number_restraints     70
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0862
_refine_ls_R_factor_gt           0.0765
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1540P)²+0.9490P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2036
_refine_ls_wR_factor_ref         0.2187
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2288
_reflns_number_total             2844
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c5cc02372f2.cif
_cod_data_source_block           1_dce
_cod_database_code               7117574
_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   0.410
_shelx_estimated_absorpt_t_max   0.791
_shelxl_version_number           2014-3
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z'
'-x+1/2, y+1/2, -z+1/2'
'x, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z'
'x-1/2, -y-1/2, z-1/2'
'-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_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
Zn1 Zn 0.18045(4) 0.2500 1.2500 0.0526(3) Uani 1 2 d S T P . .
Cl2 Cl 0.10575(7) 0.33080(5) 1.19130(14) 0.0765(4) Uani 1 1 d . . . . .
N1 N 0.27250(18) 0.22654(13) 1.1065(3) 0.0508(8) Uani 1 1 d . . . . .
C6 C 0.3686(2) 0.08517(17) 0.9773(4) 0.0520(9) Uani 1 1 d . . . . .
C5 C 0.2902(2) 0.16923(15) 1.0850(4) 0.0487(8) Uani 1 1 d . . . . .
H5 H 0.2573 0.1403 1.1330 0.058 Uiso 1 1 calc R U . . .
C3 C 0.4027(2) 0.19292(19) 0.9281(4) 0.0577(10) Uani 1 1 d . . . . .
H3 H 0.4475 0.1818 0.8663 0.069 Uiso 1 1 calc R U . . .
C1 C 0.3197(2) 0.26740(19) 1.0401(5) 0.0580(10) Uani 1 1 d . . . . .
H1 H 0.3074 0.3083 1.0552 0.070 Uiso 1 1 calc R U . . .
C9 C 0.3895(2) -0.03763(17) 0.9427(4) 0.0550(10) Uani 1 1 d . . . . .
C8 C 0.3809(3) -0.01423(18) 1.0650(4) 0.0569(10) Uani 1 1 d . . . . .
H8 H 0.3823 -0.0398 1.1386 0.068 Uiso 1 1 calc R U . . .
C4 C 0.3550(2) 0.14959(16) 0.9950(4) 0.0490(9) Uani 1 1 d . . . . .
C7 C 0.3702(3) 0.04708(17) 1.0822(4) 0.0571(10) Uani 1 1 d . . . . .
H7 H 0.3639 0.0627 1.1675 0.069 Uiso 1 1 calc R U . . .
C11 C 0.3782(3) 0.0617(2) 0.8530(5) 0.0690(11) Uani 1 1 d . . . . .
H11 H 0.3786 0.0874 0.7796 0.083 Uiso 1 1 calc R U . . .
C10 C 0.3874(4) 0.0002(2) 0.8361(5) 0.0741(13) Uani 1 1 d . . . . .
H10 H 0.3923 -0.0158 0.7509 0.089 Uiso 1 1 calc R U . . .
C2 C 0.3851(3) 0.25226(18) 0.9510(5) 0.0606(10) Uani 1 1 d . . . . .
H2 H 0.4178 0.2822 0.9058 0.073 Uiso 1 1 calc R U . . .
C12 C 0.3980(2) -0.10228(18) 0.9274(5) 0.0577(10) Uani 1 1 d . . . . .
H12 H 0.4005 -0.1261 1.0036 0.069 Uiso 1 1 calc R U . . .
N2 N 0.4021(2) -0.12783(16) 0.8186(4) 0.0639(10) Uani 1 1 d . . . . .
C13 C 0.4046(3) -0.19287(19) 0.8195(5) 0.0605(11) Uani 1 1 d . . . . .
H13 H 0.4047 -0.2074 0.9114 0.073 Uiso 1 1 calc R U . . .
C14 C 0.4887(2) -0.2161(2) 0.7500(4) 0.0593(11) Uani 1 1 d . . . . .
H14A H 0.5439 -0.2012 0.7943 0.071 Uiso 1 1 calc R U . . .
H14B H 0.4895 -0.2013 0.6593 0.071 Uiso 1 1 calc R U . . .
C15 C 0.3206(3) -0.2156(2) 0.7508(5) 0.0756(17) Uani 1 1 d . . . . .
H15A H 0.3193 -0.2004 0.6606 0.091 Uiso 1 1 calc R U . . .
H15B H 0.2656 -0.2011 0.7963 0.091 Uiso 1 1 calc R U . . .
C3S C 0.7469(14) 0.5332(5) 0.983(5) 0.318(14) Uani 0.398(5) 1 d D U P A 1
Cl3 Cl 0.6277(5) 0.5633(2) 0.9728(5) 0.248(3) Uani 0.795(9) 1 d D U P A 1
C3T C 0.732(2) 0.5320(8) 0.910(4) 0.313(14) Uani 0.398(5) 1 d D U P A 1
C4S C 0.7269(17) 0.4703(8) 1.013(15) 0.326(16) Uani 0.102(5) 1 d D U P A 2
Cl4 Cl 0.613(3) 0.4745(15) 0.956(3) 0.340(16) Uani 0.205(9) 1 d D U P A 2
C4T C 0.703(7) 0.488(12) 0.844(8) 0.328(16) Uani 0.102(5) 1 d D U P A 2
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 Zn1 N1 98.29(16) 4_557 .
N1 Zn1 Cl2 108.13(9) 4_557 .
N1 Zn1 Cl2 109.91(10) . .
N1 Zn1 Cl2 109.91(10) 4_557 4_557
N1 Zn1 Cl2 108.13(9) . 4_557
Cl2 Zn1 Cl2 120.24(7) . 4_557
C5 N1 C1 118.5(3) . .
C5 N1 Zn1 119.5(3) . .
C1 N1 Zn1 121.9(3) . .
C7 C6 C11 118.8(4) . .
C7 C6 C4 121.1(4) . .
C11 C6 C4 120.0(4) . .
N1 C5 C4 123.2(4) . .
C2 C3 C4 120.0(4) . .
N1 C1 C2 122.3(4) . .
C8 C9 C10 119.2(4) . .
C8 C9 C12 119.1(4) . .
C10 C9 C12 121.6(4) . .
C9 C8 C7 120.3(4) . .
C3 C4 C5 116.9(3) . .
C3 C4 C6 124.2(3) . .
C5 C4 C6 119.0(3) . .
C6 C7 C8 121.1(4) . .
C6 C11 C10 119.9(5) . .
C9 C10 C11 120.6(4) . .
C1 C2 C3 119.1(4) . .
N2 C12 C9 123.4(5) . .
C12 N2 C13 116.9(4) . .
N2 C13 C15 108.3(4) . .
N2 C13 C14 111.1(4) . .
C15 C13 C14 109.3(3) . .
C13 C14 C14 110.0(3) . 4_546
C13 C15 C15 110.1(4) . 4_546
C3T C3S C3S 89.1(15) . 2_665
C3T C3S C3T 66(2) . 2_665
C3S C3S C3T 28(2) 2_665 2_665
C3T C3S Cl3 73(2) . .
C3S C3S Cl3 114.5(19) 2_665 .
C3T C3S Cl3 117(2) 2_665 .
C3T Cl3 C3S 24(2) . .
C3S C3T C3T 86.4(11) . 2_665
C3S C3T C3S 63(2) . 2_665
C3T C3T C3S 28(2) 2_665 2_665
C3S C3T Cl3 83(2) . .
C3T C3T Cl3 131(3) 2_665 .
C3S C3T Cl3 109.7(19) 2_665 .
C4S C4S C4T 84(6) 2_665 .
C4S C4S Cl4 112(2) 2_665 .
C4T C4S Cl4 59(4) . .
C4S Cl4 C4T 61(8) . .
C4T C4T C4S 84(6) 2_665 .
C4T C4T Cl4 139(5) 2_665 .
C4S C4T Cl4 59(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 N1 2.072(3) 4_557
Zn1 N1 2.072(3) .
Zn1 Cl2 2.2079(12) .
Zn1 Cl2 2.2079(12) 4_557
N1 C5 1.333(5) .
N1 C1 1.339(5) .
C6 C7 1.378(6) .
C6 C11 1.390(6) .
C6 C4 1.473(5) .
C5 C4 1.400(5) .
C3 C2 1.379(6) .
C3 C4 1.384(6) .
C1 C2 1.372(6) .
C9 C8 1.369(6) .
C9 C10 1.388(7) .
C9 C12 1.467(5) .
C8 C7 1.399(6) .
C11 C10 1.400(7) .
C12 N2 1.259(5) .
N2 C13 1.463(6) .
C13 C15 1.514(6) .
C13 C14 1.522(5) .
C14 C14 1.526(9) 4_546
C15 C15 1.545(11) 4_546
C3S C3T 0.78(6) .
C3S C3S 1.49(2) 2_665
C3S C3T 1.67(3) 2_665
C3S Cl3 1.885(18) .
Cl3 C3T 1.81(2) .
C3T C3T 1.53(2) 2_665
C3T C3S 1.67(3) 2_665
C4S C4S 1.50(2) 2_665
C4S C4T 1.8(2) .
C4S Cl4 1.78(2) .
Cl4 C4T 1.78(2) .
C4T C4T 1.49(2) 2_665
