#------------------------------------------------------------------------------
#$Date: 2018-12-04 05:50:51 +0200 (Tue, 04 Dec 2018) $
#$Revision: 212311 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/24/27/2242762.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2242762
loop_
_publ_author_name
'Granifo, Juan'
'Suárez, Sebastián'
'Baggio, Ricardo'
_publ_section_title
;
 The enrichment ratio of atomic contacts in the crystal structure of
 isomeric, triply protonated, 4'-functionalized terpyridine cations with
 [ZnCl₄]^2{-^} as counter-ion
;
_journal_coeditor_code           EB2014
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1881
_journal_page_last               1886
_journal_paper_doi               10.1107/S2056989018016250
_journal_volume                  74
_journal_year                    2018
_chemical_formula_iupac          '(C24 H19 N4)2 [Zn Cl4]3'
_chemical_formula_moiety         '2(C24 H19 N4 3+), 3(Cl4 Zn 2-)'
_chemical_formula_sum            'C48 H38 Cl12 N8 Zn3'
_chemical_formula_weight         1348.37
_chemical_name_systematic
;
Bis[4'-(isoquinolin-2-ium-4-yl)-4,2':6',4''-terpyridine-1,1''-diium]
tris(tetrachloridozincate)
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/1
_cell_angle_alpha                90
_cell_angle_beta                 114.316(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   30.642(2)
_cell_length_b                   8.0866(4)
_cell_length_c                   23.413(2)
_cell_measurement_reflns_used    4699
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      27.4920
_cell_measurement_theta_min      3.7020
_cell_volume                     5286.8(7)
_computing_cell_refinement
;
CrysAlisPro (Rigaku OD, 2015)
;
_computing_data_collection
;
CrysAlisPro (Rigaku OD, 2015)
;
_computing_data_reduction
;
CrysAlisPro  (Rigaku OD, 2015)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
SHELXL2014  (Sheldrick, 2015), PLATON (Spek, 2009)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      295(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.881
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0653
_diffrn_reflns_av_unetI/netI     0.0679
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            23819
_diffrn_reflns_theta_full        25.250
_diffrn_reflns_theta_max         29.384
_diffrn_reflns_theta_min         3.711
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    2.001
_exptl_absorpt_correction_T_max  0.82
_exptl_absorpt_correction_T_min  0.58
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2015)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.694
_exptl_crystal_description       blocks
_exptl_crystal_F_000             2704
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.623
_refine_diff_density_min         -0.602
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     330
_refine_ls_number_reflns         6416
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0802
_refine_ls_R_factor_gt           0.0454
_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)+(0.0313P)²+4.8559P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0862
_refine_ls_wR_factor_ref         0.1060
_reflns_number_gt                4482
_reflns_number_total             6416
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            eb2014sup1.cif
_cod_data_source_block           I
_cod_database_code               2242762
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x, -y, z+1/2'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z+1/2'
'-x, -y, -z'
'-x, y, -z-1/2'
'-x+1/2, -y+1/2, -z'
'-x+1/2, 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_occupancy
Zn Zn1 0.65199(2) 0.59124(5) 0.12147(2) 0.02480(12) Uani d 1
Cl Cl11 0.68969(3) 0.80880(11) 0.18160(5) 0.0407(3) Uani d 1
Cl Cl12 0.58917(3) 0.50894(12) 0.14395(5) 0.0419(3) Uani d 1
Cl Cl13 0.62471(4) 0.63226(13) 0.01753(4) 0.0418(2) Uani d 1
Cl Cl14 0.70191(3) 0.37027(10) 0.15801(4) 0.0325(2) Uani d 1
Zn Zn2 0.500000 0.40642(7) 0.750000 0.02449(14) Uani d 1
Cl Cl21 0.56071(3) 0.22938(11) 0.76067(5) 0.0384(2) Uani d 1
Cl Cl22 0.47311(3) 0.57574(10) 0.66606(4) 0.0342(2) Uani d 1
N N1 0.84733(11) 0.9147(4) 0.65467(16) 0.0383(8) Uani d 1
H H1N 0.8754(6) 0.887(4) 0.6794(16) 0.046 Uiso d 1
N N2 0.70304(9) 1.0267(3) 0.46155(13) 0.0257(6) Uani d 1
N N3 0.65260(11) 1.2242(4) 0.24416(14) 0.0327(7) Uani d 1
H H3N 0.6521(13) 1.273(4) 0.2119(11) 0.039 Uiso d 1
N N4 0.51052(10) 0.6700(3) 0.43396(14) 0.0281(7) Uani d 1
H H4N 0.4922(11) 0.609(3) 0.4043(12) 0.034 Uiso d 1
C C1 0.79534(11) 0.9775(4) 0.55141(17) 0.0328(9) Uani d 1
H H1 0.790536 1.005648 0.510738 0.039 Uiso calc 1
C C2 0.84084(12) 0.9559(5) 0.59660(19) 0.0380(9) Uani d 1
H H2 0.867084 0.969995 0.586770 0.046 Uiso calc 1
C C3 0.81105(13) 0.9004(4) 0.67238(18) 0.0377(10) Uani d 1
H H3 0.816987 0.874321 0.713614 0.045 Uiso calc 1
C C4 0.76494(12) 0.9249(4) 0.62865(17) 0.0334(9) Uani d 1
H H4 0.739506 0.919950 0.640532 0.040 Uiso calc 1
C C5 0.75647(11) 0.9572(4) 0.56675(16) 0.0257(8) Uani d 1
C C6 0.70667(11) 0.9661(4) 0.51656(15) 0.0233(7) Uani d 1
C C7 0.66782(11) 0.9041(4) 0.52621(15) 0.0228(7) Uani d 1
H H7 0.672074 0.860642 0.564933 0.027 Uiso calc 1
C C8 0.62267(11) 0.9081(4) 0.47714(16) 0.0221(7) Uani d 1
C C9 0.61866(11) 0.9763(4) 0.42063(16) 0.0251(7) Uani d 1
H H9 0.588853 0.984287 0.387052 0.030 Uiso calc 1
C C10 0.65932(11) 1.0322(4) 0.41467(15) 0.0230(7) Uani d 1
C C11 0.65678(11) 1.0990(4) 0.35449(15) 0.0232(7) Uani d 1
C C12 0.61460(12) 1.1688(4) 0.31040(16) 0.0285(8) Uani d 1
H H12 0.587272 1.172068 0.318353 0.034 Uiso calc 1
C C13 0.61339(13) 1.2323(4) 0.25572(17) 0.0313(8) Uani d 1
H H13 0.585546 1.280842 0.226775 0.038 Uiso calc 1
C C14 0.69363(13) 1.1557(5) 0.28393(18) 0.0366(9) Uani d 1
H H14 0.719948 1.150150 0.273842 0.044 Uiso calc 1
C C15 0.69625(13) 1.0939(4) 0.33971(17) 0.0321(8) Uani d 1
H H15 0.724803 1.048051 0.368031 0.039 Uiso calc 1
C C16 0.57945(11) 0.8377(4) 0.48229(15) 0.0225(7) Uani d 1
C C17 0.55171(11) 0.7358(4) 0.43484(16) 0.0270(8) Uani d 1
H H17 0.561020 0.710850 0.402698 0.032 Uiso calc 1
C C18 0.49493(11) 0.7020(4) 0.47743(16) 0.0253(8) Uani d 1
H H18 0.466264 0.655910 0.474464 0.030 Uiso calc 1
C C19 0.52111(11) 0.8044(4) 0.52799(16) 0.0236(7) Uani d 1
C C20 0.50381(11) 0.8408(4) 0.57389(16) 0.0262(8) Uani d 1
H H20 0.475249 0.794643 0.571249 0.031 Uiso calc 1
C C21 0.52914(12) 0.9435(4) 0.62180(16) 0.0301(8) Uani d 1
H H21 0.518261 0.966419 0.652638 0.036 Uiso calc 1
C C22 0.57181(12) 1.0155(4) 0.62503(16) 0.0283(8) Uani d 1
H H22 0.588456 1.087141 0.657908 0.034 Uiso calc 1
C C23 0.58967(11) 0.9837(4) 0.58143(15) 0.0243(7) Uani d 1
H H23 0.617993 1.033407 0.584754 0.029 Uiso calc 1
C C24 0.56479(11) 0.8747(4) 0.53117(15) 0.0218(7) Uani d 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'
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
Cl13 Zn1 Cl11 . . 115.32(4)
Cl13 Zn1 Cl14 . . 114.53(4)
Cl11 Zn1 Cl14 . . 106.61(4)
Cl13 Zn1 Cl12 . . 108.54(4)
Cl11 Zn1 Cl12 . . 110.25(4)
Cl14 Zn1 Cl12 . . 100.58(4)
Cl22 Zn2 Cl22 . 6_657 105.21(5)
Cl22 Zn2 Cl21 . . 117.78(4)
Cl22 Zn2 Cl21 6_657 . 107.29(3)
Cl22 Zn2 Cl21 . 6_657 107.30(3)
Cl22 Zn2 Cl21 6_657 6_657 117.77(4)
Cl21 Zn2 Cl21 . 6_657 102.14(5)
C2 N1 C3 . . 122.8(3)
C2 N1 H1N . . 117(3)
C3 N1 H1N . . 120(3)
C10 N2 C6 . . 117.4(3)
C13 N3 C14 . . 123.0(3)
C13 N3 H3N . . 118(3)
C14 N3 H3N . . 119(3)
C18 N4 C17 . . 122.8(3)
C18 N4 H4N . . 115(3)
C17 N4 H4N . . 122(3)
C2 C1 C5 . . 119.6(4)
C2 C1 H1 . . 120.2
C5 C1 H1 . . 120.2
N1 C2 C1 . . 119.7(4)
N1 C2 H2 . . 120.1
C1 C2 H2 . . 120.1
N1 C3 C4 . . 119.0(4)
N1 C3 H3 . . 120.5
C4 C3 H3 . . 120.5
C3 C4 C5 . . 119.8(4)
C3 C4 H4 . . 120.1
C5 C4 H4 . . 120.1
C1 C5 C4 . . 118.8(3)
C1 C5 C6 . . 119.8(3)
C4 C5 C6 . . 121.4(3)
N2 C6 C7 . . 123.3(3)
N2 C6 C5 . . 115.3(3)
C7 C6 C5 . . 121.2(3)
C8 C7 C6 . . 119.0(3)
C8 C7 H7 . . 120.5
C6 C7 H7 . . 120.5
C7 C8 C9 . . 117.7(3)
C7 C8 C16 . . 122.7(3)
C9 C8 C16 . . 119.6(3)
C10 C9 C8 . . 119.6(3)
C10 C9 H9 . . 120.2
C8 C9 H9 . . 120.2
N2 C10 C9 . . 123.0(3)
N2 C10 C11 . . 115.8(3)
C9 C10 C11 . . 121.2(3)
C15 C11 C12 . . 117.6(3)
C15 C11 C10 . . 121.1(3)
C12 C11 C10 . . 121.3(3)
C13 C12 C11 . . 120.3(3)
C13 C12 H12 . . 119.9
C11 C12 H12 . . 119.9
N3 C13 C12 . . 119.4(3)
N3 C13 H13 . . 120.3
C12 C13 H13 . . 120.3
N3 C14 C15 . . 118.9(4)
N3 C14 H14 . . 120.5
C15 C14 H14 . . 120.5
C14 C15 C11 . . 120.8(3)
C14 C15 H15 . . 119.6
C11 C15 H15 . . 119.6
C17 C16 C24 . . 119.0(3)
C17 C16 C8 . . 116.2(3)
C24 C16 C8 . . 124.7(3)
N4 C17 C16 . . 120.7(3)
N4 C17 H17 . . 119.6
C16 C17 H17 . . 119.6
N4 C18 C19 . . 120.5(3)
N4 C18 H18 . . 119.8
C19 C18 H18 . . 119.8
C18 C19 C20 . . 120.3(3)
C18 C19 C24 . . 118.6(3)
C20 C19 C24 . . 121.0(3)
C21 C20 C19 . . 119.5(3)
C21 C20 H20 . . 120.3
C19 C20 H20 . . 120.3
C20 C21 C22 . . 120.1(3)
C20 C21 H21 . . 119.9
C22 C21 H21 . . 119.9
C23 C22 C21 . . 122.1(3)
C23 C22 H22 . . 118.9
C21 C22 H22 . . 118.9
C22 C23 C24 . . 119.6(3)
C22 C23 H23 . . 120.2
C24 C23 H23 . . 120.2
C23 C24 C16 . . 124.0(3)
C23 C24 C19 . . 117.6(3)
C16 C24 C19 . . 118.3(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Zn1 Cl13 . 2.2485(10)
Zn1 Cl11 . 2.2521(10)
Zn1 Cl14 . 2.2775(9)
Zn1 Cl12 . 2.2935(10)
Zn2 Cl22 . 2.2545(9)
Zn2 Cl22 6_657 2.2545(9)
Zn2 Cl21 . 2.2782(9)
Zn2 Cl21 6_657 2.2783(9)
N1 C2 . 1.333(5)
N1 C3 . 1.342(5)
N1 H1N . 0.846(10)
N2 C10 . 1.338(4)
N2 C6 . 1.339(4)
N3 C13 . 1.337(5)
N3 C14 . 1.338(5)
N3 H3N . 0.847(10)
N4 C18 . 1.316(4)
N4 C17 . 1.362(4)
N4 H4N . 0.850(10)
C1 C2 . 1.371(5)
C1 C5 . 1.388(5)
C1 H1 . 0.9300
C2 H2 . 0.9300
C3 C4 . 1.376(5)
C3 H3 . 0.9300
C4 C5 . 1.388(5)
C4 H4 . 0.9300
C5 C6 . 1.496(4)
C6 C7 . 1.393(4)
C7 C8 . 1.388(4)
C7 H7 . 0.9300
C8 C9 . 1.391(5)
C8 C16 . 1.491(4)
C9 C10 . 1.385(4)
C9 H9 . 0.9300
C10 C11 . 1.481(5)
C11 C15 . 1.389(5)
C11 C12 . 1.399(4)
C12 C13 . 1.366(5)
C12 H12 . 0.9300
C13 H13 . 0.9300
C14 C15 . 1.369(5)
C14 H14 . 0.9300
C15 H15 . 0.9300
C16 C17 . 1.363(4)
C16 C24 . 1.423(5)
C17 H17 . 0.9300
C18 C19 . 1.396(5)
C18 H18 . 0.9300
C19 C20 . 1.411(5)
C19 C24 . 1.427(4)
C20 C21 . 1.354(5)
C20 H20 . 0.9300
C21 C22 . 1.405(5)
C21 H21 . 0.9300
C22 C23 . 1.367(5)
C22 H22 . 0.9300
C23 C24 . 1.416(4)
C23 H23 . 0.9300
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
N1 H1N Cl21 8_657 0.846(10) 2.272(16) 3.084(3) 161(3) no
N3 H3N Cl12 1_565 0.847(10) 2.71(3) 3.291(3) 127(3) no
N3 H3N Cl14 1_565 0.847(10) 2.47(2) 3.203(3) 144(3) no
N4 H4N Cl12 6_656 0.850(10) 2.41(2) 3.125(3) 142(3) no
N4 H4N Cl22 5_666 0.850(10) 2.74(3) 3.264(3) 121(3) no
C2 H2 Cl13 8_656 0.93 2.87 3.551(4) 130.8 no
C3 H3 Cl11 7_666 0.93 2.94 3.823(4) 158.1 no
C4 H4 Cl14 2_565 0.93 2.72 3.316(4) 122.8 no
C7 H7 Cl14 2_565 0.93 2.73 3.589(3) 154.7 no
C12 H12 Cl22 5_676 0.93 2.88 3.607(4) 136.4 no
C13 H13 Cl12 1_565 0.93 2.71 3.287(4) 120.8 no
C14 H14 Cl11 8_656 0.93 2.83 3.548(4) 134.7 no
C15 H15 Cl14 8_656 0.93 2.93 3.588(4) 128.5 no
C17 H17 Cl22 5_666 0.93 2.77 3.320(4) 118.9 no
C18 H18 Cl12 6_656 0.93 2.85 3.335(3) 114.0 no
C18 H18 Cl13 6_656 0.93 2.88 3.759(3) 158.9 no

_cod_database_fobs_code 2242762
