#------------------------------------------------------------------------------
#$Date: 2016-03-26 22:29:45 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180508 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/77/7217725.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_7217725
loop_
_publ_author_name
'Constable, Edwin C.'
'Housecroft, Catherine E.'
'Prescimone, Alessandro'
'Vujovic, Srboljub'
'Zampese, Jennifer A.'
_publ_section_title
;
 Environmental control in the assembly of metallomacrocycles and
 one-dimensional polymers with
 4,2′:6′:4′′-terpyridine linkers and zinc(ii)
 nodes
;
_journal_issue                   37
_journal_name_full               CrystEngComm
_journal_page_first              8691
_journal_paper_doi               10.1039/C4CE00783B
_journal_volume                  16
_journal_year                    2014
_chemical_formula_moiety
'C108 H56 Cl8 N12 Zn4, 5(C H4 O), 2(C6 H4 Cl2)'
_chemical_formula_sum            'C125 H84 Cl12 F20 N12 O5 Zn4'
_chemical_formula_weight         2901.04
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           114
_space_group_name_Hall           'P -4 2n'
_space_group_name_H-M_alt        'P -4 21 c'
_symmetry_space_group_name_Hall  'P -4 2n'
_symmetry_space_group_name_H-M   'P -4 21 c'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   23.6145(15)
_cell_length_b                   23.6145(15)
_cell_length_c                   16.4568(10)
_cell_measurement_reflns_used    3326
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      40.98
_cell_measurement_theta_min      3.27
_cell_volume                     9177.0(10)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.2237
_diffrn_reflns_av_unetI/netI     0.1946
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            75018
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        66.500
_diffrn_reflns_theta_max         68.860
_diffrn_reflns_theta_min         2.646
_exptl_absorpt_coefficient_mu    2.722
_exptl_absorpt_correction_T_max  0.979
_exptl_absorpt_correction_T_min  0.810
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.050
_exptl_crystal_description       plate
_exptl_crystal_F_000             2448
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.010
_platon_squeeze_details
; 
this equates to 2dichloro-benzene and 5MeOH molecules per formula
 unit
;
_refine_diff_density_max         0.269
_refine_diff_density_min         -0.464
_refine_diff_density_rms         0.056
_refine_ls_abs_structure_details
; 
 Refined as an inversion twin. 
;
_refine_ls_abs_structure_Flack   0.57(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.853
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         8428
_refine_ls_number_restraints     81
_refine_ls_restrained_S_all      0.920
_refine_ls_R_factor_all          0.1907
_refine_ls_R_factor_gt           0.0769
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; 
 w=1/[σ²(Fo²)+(0.0702P)²] 
 where P=(Fo²+2Fc²)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1590
_refine_ls_wR_factor_ref         0.1884
_reflns_Friedel_coverage         0.836
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                3283
_reflns_number_total             8428
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c4ce00783b2.cif
_cod_data_source_block           squeeze_(ZnCl2(2))4
_cod_depositor_comments
'Adding full bibliography for 7217724--7217729.cif.'
_cod_original_cell_volume        9177.0(13)
_cod_database_code               7217725
#BEGIN Tags that were not found in dictionaries:
_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   0.817
_shelx_estimated_absorpt_t_max   0.979
_shelxl_version_number           2013-2
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, x+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
Zn1 Zn 0.30420(3) 0.17312(3) 0.99925(5) 0.0661(2) Uani 1 1 d . .
Cl1 Cl 0.33455(10) 0.10817(8) 1.08651(9) 0.0934(7) Uani 1 1 d . .
Cl2 Cl 0.23253(8) 0.16016(10) 0.91402(9) 0.0938(7) Uani 1 1 d . .
N1 N 0.2894(2) 0.2420(2) 1.0706(3) 0.085(2) Uani 1 1 d . .
C1 C 0.3055(3) 0.2469(3) 1.1467(3) 0.076(2) Uani 1 1 d . .
H1A H 0.3247 0.2152 1.1691 0.091 Uiso 1 1 calc R U
C2 C 0.2986(3) 0.2897(2) 1.1950(4) 0.075(2) Uani 1 1 d . U
H2A H 0.3127 0.2883 1.2490 0.090 Uiso 1 1 calc R U
C3 C 0.2696(4) 0.3391(3) 1.1664(3) 0.094(3) Uani 1 1 d . .
C4 C 0.2477(4) 0.3341(4) 1.0878(4) 0.106(3) Uani 1 1 d . .
H4A H 0.2228 0.3626 1.0680 0.127 Uiso 1 1 calc R U
C5 C 0.2607(3) 0.2905(3) 1.0396(4) 0.075(2) Uani 1 1 d . .
H5A H 0.2506 0.2918 0.9837 0.090 Uiso 1 1 calc R U
C6 C 0.2585(4) 0.3886(3) 1.2154(4) 0.115(3) Uani 1 1 d . .
N2 N 0.2463(3) 0.4352(2) 1.1747(3) 0.102(3) Uani 1 1 d . .
C10 C 0.2366(4) 0.4856(3) 1.2139(4) 0.103(3) Uani 1 1 d . .
C9 C 0.2274(4) 0.4833(3) 1.3008(4) 0.136(4) Uani 1 1 d . U
H9A H 0.2144 0.5161 1.3288 0.163 Uiso 1 1 calc R U
C8 C 0.2374(5) 0.4330(3) 1.3440(4) 0.136(4) Uani 1 1 d . U
C7 C 0.2530(5) 0.3859(3) 1.3019(4) 0.151(5) Uani 1 1 d . .
H7A H 0.2602 0.3514 1.3297 0.181 Uiso 1 1 calc R U
C13 C 0.2208(4) 0.5373(4) 1.1691(3) 0.116(4) Uani 1 1 d . .
C12 C 0.1984(5) 0.5838(4) 1.1959(4) 0.152(5) Uani 1 1 d . .
H12A H 0.1912 0.5857 1.2526 0.182 Uiso 1 1 calc R U
C11 C 0.1843(4) 0.6301(3) 1.1513(3) 0.113(4) Uani 1 1 d . .
H11A H 0.1672 0.6621 1.1763 0.135 Uiso 1 1 calc R U
N3 N 0.1951(2) 0.6298(2) 1.0703(2) 0.0718(18) Uani 1 1 d . .
C15 C 0.2131(4) 0.5813(3) 1.0399(4) 0.120(4) Uani 1 1 d . .
H15A H 0.2138 0.5787 0.9823 0.144 Uiso 1 1 calc R U
C14 C 0.2307(4) 0.5347(3) 1.0807(4) 0.144(4) Uani 1 1 d . .
H14A H 0.2480 0.5032 1.0547 0.172 Uiso 1 1 calc R U
C16 C 0.2384(5) 0.4339(3) 1.4344(4) 0.165(5) Uani 1 1 d . .
C17 C 0.2090(7) 0.4765(4) 1.4761(4) 0.279(8) Uani 1 1 d . U
H17A H 0.1857 0.5022 1.4468 0.335 Uiso 1 1 calc R U
C18 C 0.2137(8) 0.4816(5) 1.5628(5) 0.284(8) Uani 1 1 d . U
H18A H 0.2043 0.5159 1.5899 0.340 Uiso 1 1 calc R U
C19 C 0.2318(4) 0.4361(4) 1.6040(4) 0.179(5) Uani 1 1 d . U
C20 C 0.2628(6) 0.3945(4) 1.5649(5) 0.224(7) Uani 1 1 d . U
H20A H 0.2860 0.3686 1.5937 0.268 Uiso 1 1 calc R U
C21 C 0.2578(7) 0.3930(4) 1.4792(5) 0.291(8) Uani 1 1 d . .
H21A H 0.2696 0.3593 1.4524 0.349 Uiso 1 1 calc R U
C22 C 0.2239(3) 0.4352(4) 1.6963(5) 0.203(6) Uani 1 1 d . U
C23 C 0.2250(4) 0.4828(5) 1.7391(5) 0.261(7) Uani 1 1 d . .
C24 C 0.2208(9) 0.4916(5) 1.8211(6) 0.305(9) Uani 1 1 d . U
C25 C 0.2164(7) 0.4419(6) 1.8598(5) 0.252(8) Uani 1 1 d . U
C26 C 0.2044(8) 0.3855(5) 1.8306(6) 0.276(8) Uani 1 1 d . U
C27 C 0.2085(8) 0.3896(5) 1.7392(5) 0.273(8) Uani 1 1 d . U
F1 F 0.2352(4) 0.5353(3) 1.6990(3) 0.283(5) Uani 1 1 d . .
F2 F 0.2269(5) 0.5353(3) 1.8610(3) 0.307(6) Uani 1 1 d . .
F3 F 0.2142(4) 0.4442(3) 1.9466(3) 0.306(5) Uani 1 1 d . .
F4 F 0.2027(5) 0.3412(3) 1.8647(3) 0.307(6) Uani 1 1 d . .
F5 F 0.2105(5) 0.3382(3) 1.7055(3) 0.356(7) 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 0.0181 0.0091 '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'
F F 0.0727 0.0534 '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'
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
N3 Zn1 N1 104.9(2) 4_657 .
N3 Zn1 Cl2 105.58(14) 4_657 .
N1 Zn1 Cl2 110.12(17) . .
N3 Zn1 Cl1 107.28(16) 4_657 .
N1 Zn1 Cl1 103.52(16) . .
Cl2 Zn1 Cl1 124.04(9) . .
C1 N1 C5 114.1(5) . .
C1 N1 Zn1 124.9(5) . .
C5 N1 Zn1 121.1(4) . .
C2 C1 N1 128.1(6) . .
C1 C2 C3 119.6(6) . .
C4 C3 C2 114.4(6) . .
C4 C3 C6 121.2(7) . .
C2 C3 C6 124.2(6) . .
C5 C4 C3 121.9(7) . .
C4 C5 N1 121.1(6) . .
N2 C6 C7 121.5(7) . .
N2 C6 C3 115.6(6) . .
C7 C6 C3 122.4(7) . .
C6 N2 C10 121.4(6) . .
N2 C10 C9 117.1(6) . .
N2 C10 C13 121.7(6) . .
C9 C10 C13 119.2(6) . .
C8 C9 C10 120.4(7) . .
C7 C8 C9 118.6(6) . .
C7 C8 C16 121.2(7) . .
C9 C8 C16 119.7(6) . .
C8 C7 C6 119.7(7) . .
C12 C13 C10 129.3(6) . .
C12 C13 C14 115.8(7) . .
C10 C13 C14 114.8(7) . .
C13 C12 C11 126.7(7) . .
N3 C11 C12 118.7(7) . .
C15 N3 C11 116.0(5) . .
C15 N3 Zn1 122.9(4) . 3_567
C11 N3 Zn1 120.5(5) . 3_567
N3 C15 C14 128.0(6) . .
C15 C14 C13 114.1(7) . .
C21 C16 C17 115.4(7) . .
C21 C16 C8 124.2(8) . .
C17 C16 C8 119.5(7) . .
C16 C17 C18 120.6(11) . .
C19 C18 C17 117.3(10) . .
C18 C19 C20 120.2(8) . .
C18 C19 C22 118.2(8) . .
C20 C19 C22 121.2(8) . .
C19 C20 C21 116.0(10) . .
C16 C21 C20 125.2(10) . .
C23 C22 C27 113.9(8) . .
C23 C22 C19 120.9(9) . .
C27 C22 C19 124.6(8) . .
C22 C23 C24 130.6(11) . .
C22 C23 F1 119.5(7) . .
C24 C23 F1 109.7(10) . .
F2 C24 C25 119.4(9) . .
F2 C24 C23 130.1(11) . .
C25 C24 C23 109.9(11) . .
C24 C25 F3 116.3(10) . .
C24 C25 C26 131.7(10) . .
F3 C25 C26 111.1(10) . .
F4 C26 C25 131.5(10) . .
F4 C26 C27 121.9(10) . .
C25 C26 C27 105.1(10) . .
F5 C27 C22 120.2(9) . .
F5 C27 C26 111.0(9) . .
C22 C27 C26 126.5(10) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 N3 2.003(5) 4_657
Zn1 N1 2.036(5) .
Zn1 Cl2 2.219(2) .
Zn1 Cl1 2.2200(19) .
N1 C1 1.314(7) .
N1 C5 1.426(8) .
C1 C2 1.294(8) .
C2 C3 1.432(9) .
C3 C4 1.398(9) .
C3 C6 1.445(10) .
C4 C5 1.336(9) .
C6 N2 1.319(9) .
C6 C7 1.430(9) .
N2 C10 1.374(8) .
C10 C9 1.448(9) .
C10 C13 1.473(10) .
C9 C8 1.406(10) .
C8 C7 1.361(10) .
C8 C16 1.487(9) .
C13 C12 1.298(11) .
C13 C14 1.474(9) .
C12 C11 1.358(10) .
C11 N3 1.358(7) .
N3 C15 1.320(8) .
N3 Zn1 2.003(5) 3_567
C15 C14 1.354(10) .
C16 C21 1.300(12) .
C16 C17 1.402(13) .
C17 C18 1.436(11) .
C18 C19 1.342(14) .
C19 C20 1.383(13) .
C19 C22 1.530(10) .
C20 C21 1.414(12) .
C22 C23 1.327(14) .
C22 C27 1.339(14) .
C23 C24 1.369(12) .
C23 F1 1.425(12) .
C24 F2 1.231(13) .
C24 C25 1.340(16) .
C25 F3 1.430(9) .
C25 C26 1.442(16) .
C26 F4 1.187(13) .
C26 C27 1.510(12) .
C27 F5 1.336(11) .
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 0.000 0.000 -0.013 1647.1 634.5
2 0.000 0.500 -0.025 852.5 311.4
3 0.500 0.500 -0.013 1647.0 633.5
4 0.500 1.000 -0.003 852.5 309.4
