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#$Date: 2020-03-05 02:14:33 +0200 (Thu, 05 Mar 2020) $
#$Revision: 248968 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/32/7703293.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_7703293
loop_
_publ_author_name
'Chai, Siqian'
'Xiong, Jianbo'
'Zheng, Yongshen'
'Shi, Rongchao'
'Xu, Jialiang'
_publ_section_title
;
 Dielectric phase transition of an A₂BX₄-type
 perovskite with a pentahedral to octahedral transformation.
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2218
_journal_page_last               2224
_journal_paper_doi               10.1039/c9dt04270a
_journal_volume                  49
_journal_year                    2020
_chemical_formula_sum            'C10 H24 Cl4 N2 Pb'
_chemical_formula_weight         521.30
_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'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2020-01-10 deposited with the CCDC.	2020-01-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.112(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.0243(15)
_cell_length_b                   6.0344(3)
_cell_length_c                   11.7615(6)
_cell_measurement_reflns_used    7294
_cell_measurement_temperature    373(2)
_cell_measurement_theta_max      72.2130
_cell_measurement_theta_min      3.6450
_cell_volume                     1722.46(16)
_computing_cell_refinement       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      373(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1733
_diffrn_reflns_av_unetI/netI     0.0935
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7651
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         73.030
_diffrn_reflns_theta_min         3.642
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    24.621
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.07150
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.33c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.010
_exptl_crystal_description       plate
_exptl_crystal_F_000             992
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.210
_refine_diff_density_max         5.332
_refine_diff_density_min         -3.450
_refine_diff_density_rms         0.383
_refine_ls_extinction_coef       0.0016(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     137
_refine_ls_number_reflns         1690
_refine_ls_number_restraints     276
_refine_ls_restrained_S_all      0.952
_refine_ls_R_factor_all          0.0959
_refine_ls_R_factor_gt           0.0954
_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)+(0.2200P)²+0.4599P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2400
_refine_ls_wR_factor_ref         0.2413
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1637
_reflns_number_total             1690
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9dt04270a2.cif
_cod_data_source_block           www
_cod_depositor_comments
'Adding full bibliography for 7703293--7703296.cif.'
_cod_original_cell_volume        1722.46(17)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7703293
_shelx_shelxl_version_number     2018/3
_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   0.055
_shelx_estimated_absorpt_t_max   0.079
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_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
Pb1 Pb 0.500000 0.55274(8) 0.250000 0.0575(5) Uani 1 2 d S T P . .
Cl1 Cl 0.500000 1.0051(16) 0.250000 0.105(2) Uani 1 2 d S T P . .
Cl2 Cl 0.500000 0.500000 0.000000 0.108(2) Uani 1 2 d S . P . .
Cl3 Cl 0.6170(3) 0.5961(13) 0.3092(7) 0.1090(16) Uani 1 1 d . . . . .
N1 N 0.623(3) 1.078(12) 0.473(7) 0.114(15) Uani 0.45(5) 1 d . U P A 1
H1A H 0.607936 1.212651 0.470331 0.137 Uiso 0.45(5) 1 d R U P A 1
H1B H 0.615986 1.027333 0.399684 0.137 Uiso 0.45(5) 1 d R U P A 1
C1 C 0.6843(18) 1.182(8) 0.553(5) 0.087(10) Uani 0.45(5) 1 d . U P A 1
H1C H 0.704497 1.264433 0.505592 0.104 Uiso 0.45(5) 1 calc R U P A 1
H1D H 0.681099 1.267965 0.620373 0.104 Uiso 0.45(5) 1 calc R U P A 1
C2 C 0.709(3) 0.919(11) 0.586(6) 0.093(12) Uani 0.45(5) 1 d . U P A 1
H2A H 0.697878 0.819384 0.519995 0.111 Uiso 0.45(5) 1 calc R U P A 1
H2B H 0.748430 0.916281 0.615820 0.111 Uiso 0.45(5) 1 calc R U P A 1
C3 C 0.680(3) 0.870(15) 0.679(7) 0.121(15) Uani 0.45(5) 1 d . U P A 1
H3A H 0.672764 1.000659 0.720850 0.145 Uiso 0.45(5) 1 calc R U P A 1
H3B H 0.697676 0.755963 0.732827 0.145 Uiso 0.45(5) 1 calc R U P A 1
C4 C 0.626(3) 0.783(11) 0.583(7) 0.111(13) Uani 0.45(5) 1 d . U P A 1
H4A H 0.607061 0.713110 0.636710 0.133 Uiso 0.45(5) 1 d R U P A 1
H4B H 0.623323 0.681758 0.517897 0.133 Uiso 0.45(5) 1 d R U P A 1
C5 C 0.596(2) 1.033(9) 0.568(6) 0.084(12) Uani 0.45(5) 1 d . U P A 1
H5A H 0.560598 0.989845 0.518859 0.101 Uiso 0.45(5) 1 d R U P A 1
H5B H 0.589347 1.116255 0.633638 0.101 Uiso 0.45(5) 1 d R U P A 1
N1' N 0.6209(17) 1.165(7) 0.510(5) 0.103(10) Uani 0.55(5) 1 d . U P A 2
H1'1 H 0.633980 1.177812 0.587555 0.124 Uiso 0.55(5) 1 d R U P A 2
H1'2 H 0.604183 1.287523 0.476996 0.124 Uiso 0.55(5) 1 d R U P A 2
C1' C 0.682(2) 1.094(12) 0.505(6) 0.113(13) Uani 0.55(5) 1 d . U P A 2
H1'3 H 0.678723 0.978113 0.446844 0.135 Uiso 0.55(5) 1 calc R U P A 2
H1'4 H 0.699359 1.220107 0.478882 0.135 Uiso 0.55(5) 1 calc R U P A 2
C2' C 0.712(2) 1.026(10) 0.599(7) 0.103(13) Uani 0.55(5) 1 d . U P A 2
H2'1 H 0.714502 1.137432 0.659864 0.123 Uiso 0.55(5) 1 calc R U P A 2
H2'2 H 0.748375 0.995234 0.589617 0.123 Uiso 0.55(5) 1 calc R U P A 2
C3' C 0.684(2) 0.799(9) 0.635(6) 0.113(12) Uani 0.55(5) 1 d . U P A 2
H3'1 H 0.684112 0.683101 0.578484 0.136 Uiso 0.55(5) 1 calc R U P A 2
H3'2 H 0.704107 0.747590 0.711788 0.136 Uiso 0.55(5) 1 calc R U P A 2
C4' C 0.6229(18) 0.854(8) 0.638(5) 0.098(10) Uani 0.55(5) 1 d . U P A 2
H4'1 H 0.603921 0.733434 0.666215 0.118 Uiso 0.55(5) 1 d R U P A 2
H4'2 H 0.628290 0.979287 0.691705 0.118 Uiso 0.55(5) 1 d R U P A 2
C5' C 0.598(3) 0.949(8) 0.525(7) 0.097(13) Uani 0.55(5) 1 d . U P A 2
H5'1 H 0.558402 0.953287 0.499988 0.117 Uiso 0.55(5) 1 d R U P A 2
H5'2 H 0.614489 0.869855 0.469784 0.117 Uiso 0.55(5) 1 d R 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'
Pb Pb -4.0753 8.5060 '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
Cl1 Pb1 Cl3 84.73(15) . .
Cl1 Pb1 Cl3 84.73(15) . 2_655
Cl3 Pb1 Cl3 169.5(3) . 2_655
Cl1 Pb1 Cl2 96.178(9) . .
Cl3 Pb1 Cl2 90.22(17) . .
Cl3 Pb1 Cl2 90.91(17) 2_655 .
Cl1 Pb1 Cl2 96.178(9) . 2_655
Cl3 Pb1 Cl2 90.91(17) . 2_655
Cl3 Pb1 Cl2 90.22(17) 2_655 2_655
Cl2 Pb1 Cl2 167.644(18) . 2_655
Pb1 Cl2 Pb1 180.0 . 5_665
C5 N1 C1 100(6) . .
C5 N1 H1A 86.3 . .
C1 N1 H1A 89.5 . .
C5 N1 H1B 131.7 . .
C1 N1 H1B 125.8 . .
H1A N1 H1B 107.6 . .
C2 C1 N1 90(4) . .
C2 C1 H1C 113.6 . .
N1 C1 H1C 113.6 . .
C2 C1 H1D 113.6 . .
N1 C1 H1D 113.6 . .
H1C C1 H1D 110.8 . .
C3 C2 C1 98(5) . .
C3 C2 H2A 112.1 . .
C1 C2 H2A 112.1 . .
C3 C2 H2B 112.1 . .
C1 C2 H2B 112.1 . .
H2A C2 H2B 109.7 . .
C2 C3 C4 92(6) . .
C2 C3 H3A 113.3 . .
C4 C3 H3A 113.3 . .
C2 C3 H3B 113.3 . .
C4 C3 H3B 113.3 . .
H3A C3 H3B 110.7 . .
C3 C4 C5 93(6) . .
C3 C4 H4A 98.5 . .
C5 C4 H4A 100.4 . .
C3 C4 H4B 129.9 . .
C5 C4 H4B 122.5 . .
H4A C4 H4B 107.0 . .
N1 C5 C4 89(5) . .
N1 C5 H5A 96.5 . .
C4 C5 H5A 98.3 . .
N1 C5 H5B 135.4 . .
C4 C5 H5B 123.0 . .
H5A C5 H5B 107.5 . .
C5' N1' C1' 99(5) . .
C5' N1' H1'1 90.7 . .
C1' N1' H1'1 86.8 . .
C5' N1' H1'2 130.1 . .
C1' N1' H1'2 123.8 . .
H1'1 N1' H1'2 113.4 . .
C2' C1' N1' 116(7) . .
C2' C1' H1'3 108.4 . .
N1' C1' H1'3 108.4 . .
C2' C1' H1'4 108.4 . .
N1' C1' H1'4 108.4 . .
H1'3 C1' H1'4 107.5 . .
C1' C2' C3' 107(5) . .
C1' C2' H2'1 110.2 . .
C3' C2' H2'1 110.2 . .
C1' C2' H2'2 110.2 . .
C3' C2' H2'2 110.2 . .
H2'1 C2' H2'2 108.5 . .
C4' C3' C2' 108(4) . .
C4' C3' H3'1 110.1 . .
C2' C3' H3'1 110.1 . .
C4' C3' H3'2 110.1 . .
C2' C3' H3'2 110.1 . .
H3'1 C3' H3'2 108.5 . .
C5' C4' C3' 105(5) . .
C5' C4' H4'1 118.3 . .
C3' C4' H4'1 114.0 . .
C5' C4' H4'2 104.5 . .
C3' C4' H4'2 101.4 . .
H4'1 C4' H4'2 111.6 . .
C4' C5' N1' 112(5) . .
C4' C5' H5'1 118.0 . .
N1' C5' H5'1 109.8 . .
C4' C5' H5'2 105.8 . .
N1' C5' H5'2 97.1 . .
H5'1 C5' H5'2 112.2 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb1 Cl1 2.730(10) .
Pb1 Cl3 2.851(7) .
Pb1 Cl3 2.851(7) 2_655
Pb1 Cl2 2.95754(16) .
Pb1 Cl2 2.95754(16) 2_655
N1 C5 1.46(10) .
N1 C1 1.72(9) .
N1 H1A 0.8900 .
N1 H1B 0.8900 .
C1 C2 1.71(9) .
C1 H1C 0.9700 .
C1 H1D 0.9700 .
C2 C3 1.47(11) .
C2 H2A 0.9700 .
C2 H2B 0.9700 .
C3 C4 1.62(10) .
C3 H3A 0.9700 .
C3 H3B 0.9700 .
C4 C5 1.67(8) .
C4 H4A 0.9700 .
C4 H4B 0.9700 .
C5 H5A 0.9700 .
C5 H5B 0.9700 .
N1' C5' 1.45(7) .
N1' C1' 1.59(8) .
N1' H1'1 0.8900 .
N1' H1'2 0.8900 .
C1' C2' 1.25(9) .
C1' H1'3 0.9700 .
C1' H1'4 0.9700 .
C2' C3' 1.64(7) .
C2' H2'1 0.9700 .
C2' H2'2 0.9700 .
C3' C4' 1.56(7) .
C3' H3'1 0.9700 .
C3' H3'2 0.9700 .
C4' C5' 1.44(8) .
C4' H4'1 0.9700 .
C4' H4'2 0.9700 .
C5' H5'1 0.9700 .
C5' H5'2 0.9700 .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C5'^b H5'2^b Cl3 0.97 2.52 3.43(8) 156.0 . yes
C5'^b H5'1^b Cl1 0.97 2.96 3.57(6) 121.8 . yes
C4'^b H4'2^b Cl3 0.97 2.96 3.90(6) 164.3 6_576 yes
C4'^b H4'1^b Cl3 0.97 2.57 3.40(4) 143.8 6_566 yes
N1'^b H1'2^b Cl3 0.89 2.79 3.50(4) 138.0 1_565 yes
N1'^b H1'2^b Cl2 0.89 2.98 3.61(4) 130.1 2_665 yes
C5^a H5B^a Cl3 0.97 2.66 3.55(7) 153.5 6_576 yes
C5^a H5B^a Cl1 0.97 2.98 3.59(6) 122.2 5_676 yes
C4^a H4B^a Cl3 0.97 2.48 3.37(9) 153.2 . yes
C4^a H4A^a Cl3 0.97 2.72 3.55(6) 143.9 6_566 yes
N1^a H1B^a Cl3 0.89 2.81 3.47(8) 131.8 . yes
