#------------------------------------------------------------------------------
#$Date: 2023-07-26 01:54:54 +0300 (Wed, 26 Jul 2023) $
#$Revision: 285340 $
#$URL: svn://www.crystallography.net/cod/cif/7/71/35/7713571.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_7713571
loop_
_publ_author_name
'Han, Ding-Chong'
'Tan, Yu-Hui'
'Tang, Yun Zhi'
'Wen, Jia Hui'
'Shi, Huijuan'
'Fan, Xiao-Wei'
'Li, QiaoLING'
'Wang, Meng Na'
_publ_section_title
;
 Halogen Regulating Induced Reversible High-T-Dielectric-Thermal
 Transitions in Novel Layered Organic-Inorganic Hybrid Semiconducting
 Crystals
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT01499A
_journal_year                    2023
_chemical_formula_moiety         '0.5(Cd2 Cl8), 2(C8 H11 Cl N)'
_chemical_formula_sum            'C16 H22 Cd Cl6 N2'
_chemical_formula_weight         567.45
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2023-01-31
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-05-15 deposited with the CCDC.	2023-07-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.102(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   18.8581(14)
_cell_length_b                   7.6030(6)
_cell_length_c                   7.6418(6)
_cell_measurement_reflns_used    9913
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.567
_cell_measurement_theta_min      2.894
_cell_volume                     1081.87(14)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0478
_diffrn_reflns_av_unetI/netI     0.0289
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            15000
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.593
_diffrn_reflns_theta_min         2.894
_exptl_absorpt_coefficient_mu    1.753
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5866
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'metallic light colourless'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.742
_exptl_crystal_description       plate
_exptl_crystal_F_000             564
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.934
_refine_diff_density_min         -0.589
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.153
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     116
_refine_ls_number_reflns         2470
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.153
_refine_ls_R_factor_all          0.0447
_refine_ls_R_factor_gt           0.0403
_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)+(0.0452P)²+3.2626P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1078
_refine_ls_wR_factor_ref         0.1125
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2230
_reflns_number_total             2470
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3dt01499a2.cif
_cod_data_source_block           cd
_cod_database_code               7713571
_shelx_shelxl_version_number     2014/7
_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_max   0.844
_shelx_estimated_absorpt_t_min   0.743
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C3(H3), C2(H2), C4(H4)
2.c Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'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
Cd1 Cd 0.5000 0.0000 0.5000 0.02352(14) Uani 1 2 d S T P . .
Cl3 Cl 0.48304(6) -0.24706(12) 0.74585(12) 0.0348(2) Uani 1 1 d . . . . .
Cl2 Cl 0.36784(5) 0.05189(15) 0.44739(16) 0.0399(2) Uani 1 1 d . . . . .
Cl1 Cl 0.15889(14) 0.2856(2) 0.2842(4) 0.1025(7) Uani 1 1 d . . . . .
N1 N 0.3881(2) 0.4693(5) 0.4542(6) 0.0435(9) Uani 1 1 d . . . . .
H1A H 0.3846 0.3719 0.3887 0.052 Uiso 1 1 calc GR . . . .
H1B H 0.4146 0.4477 0.5590 0.052 Uiso 1 1 calc GR . . . .
H1C H 0.4087 0.5538 0.3991 0.052 Uiso 1 1 calc GR . . . .
C1 C 0.1417(3) 0.5019(7) 0.3382(9) 0.0558(14) Uani 1 1 d . . . . .
C6 C 0.1953(3) 0.6274(7) 0.3415(7) 0.0476(11) Uani 1 1 d . . . . .
C7 C 0.2708(3) 0.5830(9) 0.3127(7) 0.0544(13) Uani 1 1 d . . . . .
H7A H 0.2689 0.4896 0.2256 0.065 Uiso 1 1 calc R . . . .
H7B H 0.2922 0.6854 0.2663 0.065 Uiso 1 1 calc R . . . .
C5 C 0.1773(3) 0.7993(7) 0.3729(7) 0.0510(12) Uani 1 1 d . . . . .
H5 H 0.2121 0.8864 0.3765 0.061 Uiso 1 1 calc R . . . .
C3 C 0.0578(3) 0.7175(10) 0.3965(10) 0.0741(19) Uani 1 1 d . . . . .
H3 H 0.0123 0.7470 0.4193 0.089 Uiso 1 1 calc R . . . .
C2 C 0.0733(3) 0.5464(10) 0.3604(10) 0.0696(17) Uani 1 1 d . . . . .
H2 H 0.0376 0.4611 0.3510 0.083 Uiso 1 1 calc R . . . .
C8 C 0.3163(3) 0.5260(8) 0.4800(8) 0.0551(13) Uani 1 1 d . . . . .
H8A H 0.3209 0.6227 0.5638 0.066 Uiso 1 1 calc R . . . .
H8B H 0.2927 0.4297 0.5309 0.066 Uiso 1 1 calc R . . . .
C4 C 0.1093(4) 0.8450(9) 0.3989(9) 0.0684(16) Uani 1 1 d . . . . .
H4 H 0.0983 0.9619 0.4181 0.082 Uiso 1 1 calc R . . . .
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'
Cd Cd -0.8075 1.2024 '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'
N N 0.0061 0.0033 '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
_geom_angle_publ_flag
Cl3 Cd1 Cl3 180.0 . 3_656 ?
Cl3 Cd1 Cl3 180.0 2_656 4 ?
Cl3 Cd1 Cl3 90.487(8) 3_656 4 ?
Cl3 Cd1 Cl3 90.487(8) . 2_656 ?
Cl3 Cd1 Cl3 89.513(8) 3_656 2_656 ?
Cl3 Cd1 Cl3 89.513(8) . 4 ?
Cl2 Cd1 Cl3 89.72(3) 3_656 2_656 ?
Cl2 Cd1 Cl3 89.72(3) . 4 ?
Cl2 Cd1 Cl3 90.18(4) . 3_656 ?
Cl2 Cd1 Cl3 90.28(3) . 2_656 ?
Cl2 Cd1 Cl3 89.82(4) 3_656 3_656 ?
Cl2 Cd1 Cl3 90.18(4) 3_656 . ?
Cl2 Cd1 Cl3 89.82(4) . . ?
Cl2 Cd1 Cl3 90.28(3) 3_656 4 ?
Cl2 Cd1 Cl2 180.0 3_656 . ?
Cd1 Cl3 Cd1 166.58(5) . 2_646 ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C8 N1 H1A 109.5 . . ?
C8 N1 H1B 109.5 . . ?
C8 N1 H1C 109.5 . . ?
C6 C1 Cl1 119.5(5) . . ?
C2 C1 Cl1 118.5(5) . . ?
C2 C1 C6 121.7(5) . . ?
C1 C6 C7 122.9(5) . . ?
C5 C6 C1 117.0(5) . . ?
C5 C6 C7 120.0(5) . . ?
C6 C7 H7A 109.3 . . ?
C6 C7 H7B 109.3 . . ?
H7A C7 H7B 108.0 . . ?
C8 C7 C6 111.7(4) . . ?
C8 C7 H7A 109.3 . . ?
C8 C7 H7B 109.3 . . ?
C6 C5 H5 119.1 . . ?
C4 C5 C6 121.8(5) . . ?
C4 C5 H5 119.1 . . ?
C2 C3 H3 120.0 . . ?
C4 C3 H3 120.0 . . ?
C4 C3 C2 120.0(6) . . ?
C1 C2 C3 119.6(6) . . ?
C1 C2 H2 120.2 . . ?
C3 C2 H2 120.2 . . ?
N1 C8 C7 113.0(5) . . ?
N1 C8 H8A 109.0 . . ?
N1 C8 H8B 109.0 . . ?
C7 C8 H8A 109.0 . . ?
C7 C8 H8B 109.0 . . ?
H8A C8 H8B 107.8 . . ?
C5 C4 H4 120.2 . . ?
C3 C4 C5 119.7(6) . . ?
C3 C4 H4 120.2 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cd1 Cl3 2.7111(9) . ?
Cd1 Cl3 2.7159(9) 2_656 ?
Cd1 Cl3 2.7111(9) 3_656 ?
Cd1 Cl3 2.7159(9) 4 ?
Cd1 Cl2 2.4922(10) 3_656 ?
Cd1 Cl2 2.4923(10) . ?
Cl3 Cd1 2.7159(9) 2_646 ?
Cl1 C1 1.738(6) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
N1 C8 1.463(7) . ?
C1 C6 1.387(7) . ?
C1 C2 1.370(9) . ?
C6 C7 1.512(7) . ?
C6 C5 1.381(8) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 C8 1.487(7) . ?
C5 H5 0.9300 . ?
C5 C4 1.372(8) . ?
C3 H3 0.9300 . ?
C3 C2 1.370(10) . ?
C3 C4 1.370(10) . ?
C2 H2 0.9300 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C4 H4 0.9300 . ?
