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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/7/70/32/7703295.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_7703295
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            'C5 H12 I3 N Pb'
_chemical_formula_weight         674.05
_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
_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                 116.121(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.3160(19)
_cell_length_b                   8.2729(8)
_cell_length_c                   17.4841(17)
_cell_measurement_reflns_used    9850
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      38.75
_cell_measurement_theta_min      2.59
_cell_volume                     2508.6(4)
_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-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0969
_diffrn_reflns_av_unetI/netI     0.0777
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            17269
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.100
_diffrn_reflns_theta_max         25.681
_diffrn_reflns_theta_min         2.098
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    20.784
_exptl_absorpt_correction_T_max  0.7477
_exptl_absorpt_correction_T_min  0.1748
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.569
_exptl_crystal_description       block
_exptl_crystal_F_000             2320
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.210
_refine_diff_density_max         7.555
_refine_diff_density_min         -7.979
_refine_diff_density_rms         0.754
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     182
_refine_ls_number_reflns         4674
_refine_ls_number_restraints     144
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.1159
_refine_ls_R_factor_gt           0.1071
_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)+(0.3110P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3232
_refine_ls_wR_factor_ref         0.3496
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4083
_reflns_number_total             4674
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9dt04270a2.cif
_cod_data_source_block           pppppp
_cod_depositor_comments
'Adding full bibliography for 7703293--7703296.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7703295
_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   0.068
_shelx_estimated_absorpt_t_max   0.097
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
Pb1 Pb 1.00081(6) 0.45608(16) 0.75258(7) 0.0236(5) Uani 1 1 d . .
Pb2 Pb 0.49966(6) 0.4774(2) 0.75059(7) 0.0250(5) Uani 1 1 d . .
I1 I 0.85706(12) 0.6935(3) 0.66872(15) 0.0264(6) Uani 1 1 d . .
I2 I 0.55524(12) 0.6839(2) 0.64156(16) 0.0258(6) Uani 1 1 d . .
I3 I 1.08394(12) 0.6724(3) 0.67422(16) 0.0287(6) Uani 1 1 d . .
I4 I 0.94457(12) 0.2558(3) 0.58881(15) 0.0268(6) Uani 1 1 d . .
I5 I 0.41535(12) 0.2414(3) 0.59495(15) 0.0269(6) Uani 1 1 d . .
I6 I 0.64421(11) 0.2374(3) 0.80640(15) 0.0272(6) Uani 1 1 d . .
C10 C 0.3935(17) 0.718(4) 0.421(2) 0.020(5) Uani 1 1 d . U
H10A H 0.376494 0.693023 0.360014 0.024 Uiso 1 1 calc R U
H10B H 0.447146 0.678820 0.452768 0.024 Uiso 1 1 calc R U
C2 C 0.8062(19) 0.898(4) 0.925(2) 0.033(5) Uani 1 1 d . U
H2A H 0.807185 1.016966 0.920451 0.040 Uiso 1 1 calc R U
H2B H 0.777657 0.869579 0.958503 0.040 Uiso 1 1 calc R U
C1 C 0.7711(18) 0.641(4) 0.842(2) 0.030(5) Uani 1 1 d . U
H1C H 0.739059 0.603660 0.869981 0.036 Uiso 1 1 calc R U
H1D H 0.748829 0.596644 0.783777 0.036 Uiso 1 1 calc R U
N2 N 0.8485(15) 0.580(4) 0.8892(17) 0.030(4) Uani 1 1 d . U
H2C H 0.876230 0.602575 0.859663 0.036 Uiso 1 1 calc R U
H2D H 0.846819 0.471145 0.893963 0.036 Uiso 1 1 calc R U
C3 C 0.8889(19) 0.654(5) 0.977(2) 0.032(5) Uani 1 1 d . U
H3A H 0.862787 0.620939 1.012483 0.039 Uiso 1 1 calc R U
H3B H 0.943185 0.617189 1.005910 0.039 Uiso 1 1 calc R U
C4 C 0.8856(19) 0.832(4) 0.967(2) 0.032(5) Uani 1 1 d . U
H4A H 0.913328 0.883350 1.023397 0.038 Uiso 1 1 calc R U
H4B H 0.912780 0.862740 0.932222 0.038 Uiso 1 1 calc R U
C5 C 0.3119(16) 0.971(4) 0.389(2) 0.024(5) Uani 1 1 d . U
H5A H 0.291809 0.958285 0.326204 0.029 Uiso 1 1 calc R U
H5B H 0.315190 1.088542 0.401057 0.029 Uiso 1 1 calc R U
C6 C 0.3923(17) 0.899(4) 0.4318(19) 0.024(5) Uani 1 1 d . U
H6A H 0.424907 0.950202 0.407952 0.028 Uiso 1 1 calc R U
H6B H 0.415085 0.924770 0.493314 0.028 Uiso 1 1 calc R U
C7 C 0.3429(16) 0.629(4) 0.452(2) 0.023(5) Uani 1 1 d . U
H7A H 0.364637 0.636784 0.514583 0.027 Uiso 1 1 calc R U
H7B H 0.340537 0.512882 0.436441 0.027 Uiso 1 1 calc R U
C8 C 0.2546(19) 0.893(4) 0.418(2) 0.031(5) Uani 1 1 d . U
H8A H 0.201617 0.932014 0.381530 0.038 Uiso 1 1 calc R U
H8B H 0.268447 0.922317 0.477426 0.038 Uiso 1 1 calc R U
C9 C 0.7685(19) 0.821(4) 0.838(2) 0.027(5) Uani 1 1 d . U
H9A H 0.714125 0.856689 0.808078 0.032 Uiso 1 1 calc R U
H9B H 0.795198 0.858204 0.803734 0.032 Uiso 1 1 calc R U
N1 N 0.2583(16) 0.705(3) 0.409(2) 0.031(5) Uani 1 1 d . U
H1A H 0.235743 0.678794 0.352723 0.037 Uiso 1 1 calc R U
H1B H 0.229908 0.657947 0.433041 0.037 Uiso 1 1 calc R U
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'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 '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
I4 Pb1 I3 86.48(7) . .
I4 Pb1 I1 91.41(7) . .
I3 Pb1 I1 87.52(7) . .
I4 Pb1 I1 85.47(6) . 2_746
I3 Pb1 I1 93.84(6) . 2_746
I1 Pb1 I1 176.51(6) . 2_746
I4 Pb1 I3 86.98(7) . 2_746
I3 Pb1 I3 171.82(7) . 2_746
I1 Pb1 I3 97.57(6) . 2_746
I1 Pb1 I3 80.73(6) 2_746 2_746
I2 Pb2 I5 89.86(7) . .
I2 Pb2 I6 92.16(7) . .
I5 Pb2 I6 85.93(7) . .
I2 Pb2 I5 87.47(7) . 2_656
I5 Pb2 I5 176.64(8) . 2_656
I6 Pb2 I5 96.20(6) . 2_656
I2 Pb2 I6 85.88(7) . 2_656
I5 Pb2 I6 95.54(6) . 2_656
I6 Pb2 I6 177.54(8) . 2_656
I5 Pb2 I6 82.23(6) 2_656 2_656
Pb1 I1 Pb1 79.44(5) . 2_756
Pb1 I3 Pb1 78.70(5) . 2_756
Pb2 I5 Pb2 79.73(5) . 2_646
Pb2 I6 Pb2 78.89(5) . 2_646
C7 C10 C6 113(3) . .
C7 C10 H10A 108.9 . .
C6 C10 H10A 108.9 . .
C7 C10 H10B 108.9 . .
C6 C10 H10B 108.9 . .
H10A C10 H10B 107.7 . .
C4 C2 C9 106(3) . .
C4 C2 H2A 110.5 . .
C9 C2 H2A 110.5 . .
C4 C2 H2B 110.5 . .
C9 C2 H2B 110.5 . .
H2A C2 H2B 108.7 . .
N2 C1 C9 112(3) . .
N2 C1 H1C 109.1 . .
C9 C1 H1C 109.1 . .
N2 C1 H1D 109.1 . .
C9 C1 H1D 109.1 . .
H1C C1 H1D 107.9 . .
C1 N2 C3 112(3) . .
C1 N2 H2C 109.2 . .
C3 N2 H2C 109.2 . .
C1 N2 H2D 109.2 . .
C3 N2 H2D 109.2 . .
H2C N2 H2D 107.9 . .
C4 C3 N2 107(3) . .
C4 C3 H3A 110.3 . .
N2 C3 H3A 110.3 . .
C4 C3 H3B 110.3 . .
N2 C3 H3B 110.3 . .
H3A C3 H3B 108.5 . .
C2 C4 C3 114(3) . .
C2 C4 H4A 108.8 . .
C3 C4 H4A 108.8 . .
C2 C4 H4B 108.8 . .
C3 C4 H4B 108.8 . .
H4A C4 H4B 107.7 . .
C6 C5 C8 113(3) . .
C6 C5 H5A 108.9 . .
C8 C5 H5A 108.9 . .
C6 C5 H5B 108.9 . .
C8 C5 H5B 108.9 . .
H5A C5 H5B 107.7 . .
C10 C6 C5 113(2) . .
C10 C6 H6A 108.9 . .
C5 C6 H6A 108.9 . .
C10 C6 H6B 108.9 . .
C5 C6 H6B 108.9 . .
H6A C6 H6B 107.7 . .
C10 C7 N1 109(3) . .
C10 C7 H7A 109.8 . .
N1 C7 H7A 109.8 . .
C10 C7 H7B 109.8 . .
N1 C7 H7B 109.8 . .
H7A C7 H7B 108.2 . .
C5 C8 N1 108(3) . .
C5 C8 H8A 110.0 . .
N1 C8 H8A 110.0 . .
C5 C8 H8B 110.0 . .
N1 C8 H8B 110.0 . .
H8A C8 H8B 108.4 . .
C1 C9 C2 112(3) . .
C1 C9 H9A 109.2 . .
C2 C9 H9A 109.2 . .
C1 C9 H9B 109.2 . .
C2 C9 H9B 109.2 . .
H9A C9 H9B 107.9 . .
C8 N1 C7 115(2) . .
C8 N1 H1A 108.5 . .
C7 N1 H1A 108.5 . .
C8 N1 H1B 108.5 . .
C7 N1 H1B 108.5 . .
H1A N1 H1B 107.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb1 I4 3.063(3) .
Pb1 I3 3.098(3) .
Pb1 I1 3.183(2) .
Pb1 I1 3.290(2) 2_746
Pb1 I3 3.416(3) 2_746
Pb2 I2 3.084(3) .
Pb2 I5 3.157(3) .
Pb2 I6 3.208(2) .
Pb2 I5 3.295(3) 2_656
Pb2 I6 3.302(2) 2_656
C10 C7 1.50(4) .
C10 C6 1.51(4) .
C10 H10A 0.9900 .
C10 H10B 0.9900 .
C2 C4 1.48(4) .
C2 C9 1.52(5) .
C2 H2A 0.9900 .
C2 H2B 0.9900 .
C1 N2 1.44(4) .
C1 C9 1.49(4) .
C1 H1C 0.9900 .
C1 H1D 0.9900 .
N2 C3 1.52(4) .
N2 H2C 0.9100 .
N2 H2D 0.9100 .
C3 C4 1.49(5) .
C3 H3A 0.9900 .
C3 H3B 0.9900 .
C4 H4A 0.9900 .
C4 H4B 0.9900 .
C5 C6 1.52(4) .
C5 C8 1.55(4) .
C5 H5A 0.9900 .
C5 H5B 0.9900 .
C6 H6A 0.9900 .
C6 H6B 0.9900 .
C7 N1 1.60(4) .
C7 H7A 0.9900 .
C7 H7B 0.9900 .
C8 N1 1.57(4) .
C8 H8A 0.9900 .
C8 H8B 0.9900 .
C9 H9A 0.9900 .
C9 H9B 0.9900 .
N1 H1A 0.9100 .
N1 H1B 0.9100 .
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
C10 H10A I6 0.99 2.82 3.73(3) 154.1 3_666 yes
C10 H10B I2 0.99 3.03 3.75(3) 130.9 . yes
C10 H10B I5 0.99 3.18 3.84(3) 125.0 3_666 yes
N2 H2C I1 0.91 3.28 4.04(3) 142.3 . yes
N2 H2D I3 0.91 3.27 3.95(3) 132.7 2_746 yes
C3 H3A I1 0.99 3.18 3.87(4) 128.4 4_576 yes
C4 H4A I1 0.99 3.24 3.81(4) 118.8 4_576 yes
C4 H4A I3 0.99 3.22 3.95(3) 131.8 4_576 yes
C4 H4A I4 0.99 3.16 3.91(4) 134.2 4_576 yes
C4 H4B I3 0.99 3.18 3.95(4) 135.4 2_756 yes
C4 H4B I4 0.99 3.07 3.86(4) 138.2 2_756 yes
C5 H5B I5 0.99 3.33 3.96(3) 123.3 1_565 yes
C7 H7A I6 0.99 3.31 4.22(3) 153.0 2_656 yes
C7 H7B I2 0.99 3.31 4.01(3) 128.5 3_666 yes
C8 H8A I1 0.99 3.28 3.97(3) 128.1 3_676 yes
N1 H1B I4 0.91 3.30 3.95(3) 130.3 3_666 yes
