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#$Date: 2021-02-03 12:18:46 +0200 (Wed, 03 Feb 2021) $
#$Revision: 261392 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/02/1560257.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_1560257
loop_
_publ_author_name
'Najla Mahbouli Rhouma'
'Ali Rayes'
'Francesco Mezzadri'
'Davide Delmonte'
'Riccardi Cabassi'
'Gianluca Calestani'
'Mohamed Loukil'
_publ_section_title
;
 Structural and electrical phase transitions in the
 [(C2H5)4N]2ZnI3.86Cl0.14 system
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              60
_journal_page_last               66
_journal_paper_doi               10.1016/j.jssc.2017.08.029
_journal_volume                  256
_journal_year                    2017
_chemical_formula_moiety         '2(C8 H20 N), Cl0.15 I3.85 Zn'
_chemical_formula_sum            'C16 H40 Cl0.15 I3.85 N2 Zn'
_chemical_formula_weight         819.59
_chemical_name_common
;
2(C8 H20 N), Cl0.15 I3.85 Zn
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           113
_space_group_name_Hall           'P -4 2ab'
_space_group_name_H-M_alt        'P -4 21 m'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.6341(10)
_cell_length_b                   13.6341(10)
_cell_length_c                   14.6643(11)
_cell_measurement_reflns_used    284
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      20.30
_cell_measurement_theta_min      10.12
_cell_volume                     2725.9(3)
_computing_cell_refinement       'SAINT (Bruker, 2008)'
_computing_data_collection       'APEX2 (Bruker, 2008)'
_computing_data_reduction        'SAINT (Bruker, 2008)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2015b)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015a)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX2 CCD'
_diffrn_measurement_method       'ω scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0476
_diffrn_reflns_av_unetI/netI     0.0234
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            26007
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.498
_diffrn_reflns_theta_min         1.389
_exptl_absorpt_coefficient_mu    5.276
_exptl_absorpt_correction_T_max  0.248
_exptl_absorpt_correction_T_min  0.162
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.997
_exptl_crystal_description       block
_exptl_crystal_F_000             1546.1
_exptl_crystal_size_max          0.380
_exptl_crystal_size_mid          0.380
_exptl_crystal_size_min          0.280
_refine_diff_density_max         0.662
_refine_diff_density_min         -0.632
_refine_diff_density_rms         0.092
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.40(7)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     144
_refine_ls_number_reflns         2706
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0338
_refine_ls_R_factor_gt           0.0300
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0366P)²+3.4639P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0708
_refine_ls_wR_factor_ref         0.0729
_reflns_Friedel_coverage         0.774
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                2491
_reflns_number_total             2706
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            JSSC-2017-256-60-1.cif
_cod_data_source_block           O_130
_cod_original_cell_volume        2725.9(4)
_cod_database_code               1560257
_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   0.239
_shelx_estimated_absorpt_t_max   0.320
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'
'x+1/2, -y+1/2, -z'
'-y+1/2, -x+1/2, z'
'y+1/2, x+1/2, 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
Zn1 Zn 0.75279(8) 0.25279(8) 0.22761(8) 0.0444(5) Uani 1 2 d S T P . .
I1 I 0.62919(5) 0.12919(5) 0.29955(5) 0.0493(2) Uani 0.962(7) 2 d S T P . .
I2 I 0.74532(5) 0.24532(5) 0.05045(5) 0.0516(2) Uani 0.962(7) 2 d S T P . .
I3 I 0.70345(5) 0.42915(5) 0.27975(4) 0.0586(2) Uani 0.962(7) 1 d . . P . .
Cl1 Cl 0.62919(5) 0.12919(5) 0.29955(5) 0.0493(2) Uani 0.038(7) 2 d S T P . .
Cl2 Cl 0.74532(5) 0.24532(5) 0.05045(5) 0.0516(2) Uani 0.038(7) 2 d S T P . .
Cl3 Cl 0.70345(5) 0.42915(5) 0.27975(4) 0.0586(2) Uani 0.038(7) 1 d . . P . .
N1 N 0.7894(5) 0.2894(5) 0.5774(6) 0.040(2) Uani 1 2 d DS T P . .
N2 N 0.5000 0.5000 0.0000 0.042(3) Uani 1 4 d DS T P . .
N3 N 0.5000 0.0000 -0.0128(10) 0.059(5) Uani 1 4 d DS T P . .
C1 C 0.7151(7) 0.2151(7) 0.5465(12) 0.074(5) Uani 1 2 d DS T P . .
H1A H 0.6664 0.2491 0.5077 0.089 Uiso 0.5 1 calc R U P . .
H1B H 0.7491 0.1664 0.5077 0.089 Uiso 0.5 1 calc R U P . .
C2 C 0.6609(9) 0.1609(9) 0.6193(16) 0.104(7) Uani 1 2 d DS TU P . .
H2A H 0.6993 0.1619 0.6759 0.156 Uiso 0.5 1 calc R U P . .
H2B H 0.6506 0.0928 0.6001 0.156 Uiso 0.5 1 calc R U P . .
H2C H 0.5973 0.1924 0.6298 0.156 Uiso 0.5 1 calc R U P . .
C3 C 0.8326(7) 0.3326(7) 0.4931(8) 0.060(4) Uani 1 2 d DS TU P . .
H3A H 0.7789 0.3616 0.4566 0.072 Uiso 0.5 1 calc R U P . .
H3B H 0.8616 0.2789 0.4566 0.072 Uiso 0.5 1 calc R U P . .
C4 C 0.9098(8) 0.4098(8) 0.5076(11) 0.077(5) Uani 1 2 d DS TU P . .
H4A H 0.8782 0.4726 0.5215 0.115 Uiso 0.5 1 calc R U P . .
H4B H 0.9494 0.4165 0.4521 0.115 Uiso 0.5 1 calc R U P . .
H4C H 0.9522 0.3906 0.5585 0.115 Uiso 0.5 1 calc R U P . .
C5 C 0.8688(7) 0.2425(7) 0.6359(6) 0.051(2) Uani 1 1 d D U . . .
H5A H 0.9145 0.2943 0.6565 0.061 Uiso 1 1 calc R U . . .
H5B H 0.8377 0.2137 0.6907 0.061 Uiso 1 1 calc R U . . .
C6 C 0.9274(8) 0.1630(8) 0.5878(8) 0.066(3) Uani 1 1 d D U . . .
H6A H 0.8838 0.1085 0.5716 0.099 Uiso 1 1 calc R U . . .
H6B H 0.9792 0.1391 0.6285 0.099 Uiso 1 1 calc R U . . .
H6C H 0.9571 0.1900 0.5323 0.099 Uiso 1 1 calc R U . . .
C7 C 0.4611(8) 0.5826(8) -0.0580(7) 0.065(3) Uani 1 1 d D . . . .
H7A H 0.5166 0.6129 -0.0912 0.078 Uiso 1 1 calc R U . . .
H7B H 0.4327 0.6333 -0.0176 0.078 Uiso 1 1 calc R U . . .
C8 C 0.3829(7) 0.5512(10) -0.1276(6) 0.065(3) Uani 1 1 d D . . . .
H8A H 0.4142 0.5150 -0.1775 0.098 Uiso 1 1 calc R U . . .
H8B H 0.3501 0.6095 -0.1521 0.098 Uiso 1 1 calc R U . . .
H8C H 0.3344 0.5090 -0.0976 0.098 Uiso 1 1 calc R U . . .
C9 C 0.512(2) 0.0906(17) -0.0689(14) 0.102(10) Uani 0.5 1 d D . P A -1
H9A H 0.5246 0.1463 -0.0272 0.123 Uiso 0.5 1 calc R U P A -1
H9B H 0.4499 0.1037 -0.1010 0.123 Uiso 0.5 1 calc R U P A -1
C10 C 0.594(3) 0.088(4) -0.1391(14) 0.110(8) Uani 0.5 1 d D U P A -1
H10A H 0.5939 0.1495 -0.1739 0.165 Uiso 0.5 1 calc R U P A -1
H10B H 0.5838 0.0328 -0.1806 0.165 Uiso 0.5 1 calc R U P A -1
H10C H 0.6573 0.0806 -0.1081 0.165 Uiso 0.5 1 calc R U P A -1
C11 C 0.4096(12) 0.0131(16) 0.0445(12) 0.061(5) Uani 0.5 1 d D . P A -1
H11A H 0.3972 -0.0484 0.0785 0.073 Uiso 0.5 1 calc R U P A -1
H11B H 0.3529 0.0245 0.0038 0.073 Uiso 0.5 1 calc R U P A -1
C12 C 0.416(3) 0.097(3) 0.1117(11) 0.067(8) Uani 0.5 1 d D . P A -1
H12A H 0.4807 0.0959 0.1413 0.101 Uiso 0.5 1 calc R U P A -1
H12B H 0.3649 0.0896 0.1580 0.101 Uiso 0.5 1 calc R U P A -1
H12C H 0.4074 0.1591 0.0795 0.101 Uiso 0.5 1 calc R U P A -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'
I I -0.4742 1.8119 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
I2 Zn1 I1 110.70(6) . .
I2 Zn1 I3 108.56(4) . .
I1 Zn1 I3 108.08(4) . .
I2 Zn1 Cl3 108.57(4) . 8_545
I1 Zn1 Cl3 108.08(4) . 8_545
I3 Zn1 Cl3 112.9 . 8_545
I2 Zn1 I3 108.57(4) . 8_545
I1 Zn1 I3 108.08(4) . 8_545
I3 Zn1 I3 112.87(6) . 8_545
Cl3 Zn1 I3 0.0 8_545 8_545
C3 N1 C1 106.4(10) . .
C3 N1 C5 110.6(6) . 8_545
C1 N1 C5 111.5(7) . 8_545
C3 N1 C5 110.6(6) . .
C1 N1 C5 111.5(7) . .
C5 N1 C5 106.3(9) 8_545 .
C7 N2 C7 108.6(4) 3_565 2_665
C7 N2 C7 111.3(9) 3_565 4_655
C7 N2 C7 108.6(4) 2_665 4_655
C7 N2 C7 108.6(4) 3_565 .
C7 N2 C7 111.3(9) 2_665 .
C7 N2 C7 108.6(4) 4_655 .
C9 N3 C11 107.6(13) . .
C2 C1 N1 116.8(14) . .
C2 C1 H1A 108.1 . .
N1 C1 H1A 108.1 . .
C2 C1 H1B 108.1 . .
N1 C1 H1B 108.1 . .
H1A C1 H1B 107.3 . .
C1 C2 H2A 109.5 . .
C1 C2 H2B 109.5 . .
H2A C2 H2B 109.5 . .
C1 C2 H2C 109.5 . .
H2A C2 H2C 109.5 . .
H2B C2 H2C 109.5 . .
N1 C3 C4 115.9(11) . .
N1 C3 H3A 108.3 . .
C4 C3 H3A 108.3 . .
N1 C3 H3B 108.3 . .
C4 C3 H3B 108.3 . .
H3A C3 H3B 107.4 . .
C3 C4 H4A 109.5 . .
C3 C4 H4B 109.5 . .
H4A C4 H4B 109.5 . .
C3 C4 H4C 109.5 . .
H4A C4 H4C 109.5 . .
H4B C4 H4C 109.5 . .
C6 C5 N1 114.4(7) . .
C6 C5 H5A 108.7 . .
N1 C5 H5A 108.7 . .
C6 C5 H5B 108.7 . .
N1 C5 H5B 108.7 . .
H5A C5 H5B 107.6 . .
C5 C6 H6A 109.5 . .
C5 C6 H6B 109.5 . .
H6A C6 H6B 109.5 . .
C5 C6 H6C 109.5 . .
H6A C6 H6C 109.5 . .
H6B C6 H6C 109.5 . .
N2 C7 C8 114.2(9) . .
N2 C7 H7A 108.7 . .
C8 C7 H7A 108.7 . .
N2 C7 H7B 108.7 . .
C8 C7 H7B 108.7 . .
H7A C7 H7B 107.6 . .
C7 C8 H8A 109.5 . .
C7 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
C7 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
N3 C9 C10 116(2) . .
N3 C9 H9A 108.3 . .
C10 C9 H9A 108.3 . .
N3 C9 H9B 108.3 . .
C10 C9 H9B 108.3 . .
H9A C9 H9B 107.4 . .
C9 C10 H10A 109.5 . .
C9 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
C9 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
N3 C11 C12 114.0(19) . .
N3 C11 H11A 108.8 . .
C12 C11 H11A 108.8 . .
N3 C11 H11B 108.8 . .
C12 C11 H11B 108.8 . .
H11A C11 H11B 107.7 . .
C11 C12 H12A 109.5 . .
C11 C12 H12B 109.5 . .
H12A C12 H12B 109.5 . .
C11 C12 H12C 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 I2 2.6019(15) .
Zn1 I1 2.6063(17) .
Zn1 I3 2.6113(11) .
Zn1 Cl3 2.6113(11) 8_545
Zn1 I3 2.6113(11) 8_545
N1 C3 1.491(13) .
N1 C1 1.502(14) .
N1 C5 1.521(9) 8_545
N1 C5 1.521(9) .
N2 C7 1.508(9) 3_565
N2 C7 1.508(9) 2_665
N2 C7 1.508(9) 4_655
N2 C7 1.508(9) .
N3 C9 1.493(17) .
N3 C11 1.502(15) .
C1 C2 1.494(18) .
C1 H1A 0.9900 .
C1 H1B 0.9900 .
C2 H2A 0.9800 .
C2 H2B 0.9800 .
C2 H2C 0.9800 .
C3 C4 1.504(17) .
C3 H3A 0.9900 .
C3 H3B 0.9900 .
C4 H4A 0.9800 .
C4 H4B 0.9800 .
C4 H4C 0.9800 .
C5 C6 1.520(12) .
C5 H5A 0.9900 .
C5 H5B 0.9900 .
C6 H6A 0.9800 .
C6 H6B 0.9800 .
C6 H6C 0.9800 .
C7 C8 1.537(13) .
C7 H7A 0.9900 .
C7 H7B 0.9900 .
C8 H8A 0.9800 .
C8 H8B 0.9800 .
C8 H8C 0.9800 .
C9 C10 1.52(2) .
C9 H9A 0.9900 .
C9 H9B 0.9900 .
C10 H10A 0.9800 .
C10 H10B 0.9800 .
C10 H10C 0.9800 .
C11 C12 1.51(2) .
C11 H11A 0.9900 .
C11 H11B 0.9900 .
C12 H12A 0.9800 .
C12 H12B 0.9800 .
C12 H12C 0.9800 .
