#------------------------------------------------------------------------------
#$Date: 2020-02-27 01:45:26 +0200 (Thu, 27 Feb 2020) $
#$Revision: 248461 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/42/4134255.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_4134255
loop_
_publ_author_name
'Zhang, Han-Yue'
'Song, Xian-Jiang'
'Cheng, Hao'
'Zeng, Yu-Ling'
'Zhang, Yi'
'Li, Peng-Fei'
'Liao, Wei-Qiang'
'Xiong, Ren-Gen'
_publ_section_title
;
 A Three-Dimensional Lead Halide Perovskite-Related Ferroelectric.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.0c00375
_journal_year                    2020
_chemical_formula_moiety         '2(Cl3 Pb), C5 H16 N2'
_chemical_formula_sum            'C5 H16 Cl6 N2 Pb2'
_chemical_formula_weight         731.30
_space_group_crystal_system      orthorhombic
_space_group_IT_number           51
_space_group_name_Hall           '-P 2a 2a'
_space_group_name_H-M_alt        'P m m a'
_atom_sites_solution_hydrogens   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.9183(9)
_cell_length_b                   5.8648(3)
_cell_length_c                   9.4829(5)
_cell_measurement_reflns_used    2951
_cell_measurement_temperature    423(2)
_cell_measurement_theta_max      30.5420
_cell_measurement_theta_min      2.5590
_cell_volume                     829.69(8)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Putz, 2005)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      423(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       'four-circle diffractometer'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0843
_diffrn_reflns_av_unetI/netI     0.0546
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            4345
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.500
_diffrn_reflns_theta_min         2.545
_diffrn_source                   'Rotating-anode X-ray tube'
_exptl_absorpt_coefficient_mu    21.207
_exptl_absorpt_correction_T_max  0.020
_exptl_absorpt_correction_T_min  0.018
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    2.927
_exptl_crystal_description       Block
_exptl_crystal_F_000             652
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.190
_refine_diff_density_max         2.799
_refine_diff_density_min         -1.850
_refine_diff_density_rms         0.350
_refine_ls_extinction_coef       0.0042(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     68
_refine_ls_number_reflns         975
_refine_ls_number_restraints     68
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.0539
_refine_ls_R_factor_gt           0.0494
_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)+(0.1177P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1422
_refine_ls_wR_factor_ref         0.1472
_reflns_Friedel_coverage         0.000
_reflns_number_gt                864
_reflns_number_total             975
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja0c00375_si_004.cif
_cod_data_source_block           Pmma
_cod_database_code               4134255
_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_min   0.101
_shelx_estimated_absorpt_t_max   0.107
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z'
'-x, y, -z'
'x+1/2, -y, -z'
'-x, -y, -z'
'x-1/2, y, -z'
'x, -y, z'
'-x-1/2, y, 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
Pb1 Pb 0.44110(3) 0.5000 0.78812(5) 0.0369(3) Uani 1 2 d S T P . .
Cl1 Cl 0.4359(4) 1.0000 0.7950(6) 0.076(2) Uani 1 2 d S T P . .
Cl2 Cl 0.5000 0.5000 0.5000 0.085(2) Uani 1 4 d S T P . .
Cl3 Cl 0.2500 0.5000 0.7479(9) 0.080(2) Uani 1 4 d S T P . .
Cl4 Cl 0.6126(2) 0.5000 0.9189(4) 0.0642(10) Uani 1 2 d S T P . .
N1 N 0.7500 1.060(4) 1.019(2) 0.057(8) Uani 0.5 2 d DS TU P . .
H1A H 0.7030 1.0000 1.0592 0.085 Uiso 1 2 d R U P . .
H1C H 0.7500 1.2125 1.0270 0.085 Uiso 0.5 2 d R U P . .
N2 N 0.7500 1.0000 0.616(2) 0.079(5) Uani 1 4 d DS TU P . .
C1 C 0.719(2) 1.0000 0.875(2) 0.061(8) Uani 0.5 2 d DS TU P . .
H1D H 0.6607 1.0669 0.8603 0.074 Uiso 0.25 1 d R U P . .
H1E H 0.7116 0.8375 0.8699 0.074 Uiso 0.25 1 d R U P . .
C2 C 0.778(2) 1.074(6) 0.758(3) 0.078(9) Uani 0.25 1 d D U P . .
H2A H 0.7825 1.2376 0.7587 0.094 Uiso 0.25 1 d R U P . .
H2B H 0.8370 1.0000 0.7744 0.094 Uiso 0.5 2 d R U P . .
C3 C 0.660(2) 1.083(6) 0.574(5) 0.089(9) Uani 0.25 1 d D U P . .
H3A H 0.6585 1.2462 0.5780 0.134 Uiso 0.25 1 d R U P . .
H3B H 0.6456 1.0333 0.4801 0.134 Uiso 0.25 1 d R U P . .
H3C H 0.6179 1.0205 0.6394 0.134 Uiso 0.25 1 d R U P . .
C4 C 0.7500 0.739(3) 0.612(4) 0.131(7) Uani 1 2 d DS TU P . .
H4A H 0.8152 0.6903 0.6098 0.197 Uiso 0.5 1 d R U P . .
H4B H 0.7243 0.6737 0.6920 0.197 Uiso 0.5 1 d R U P . .
H4C H 0.7242 0.6897 0.5270 0.197 Uiso 0.5 1 d R U P . .
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'
Cl Cl 0.1484 0.1585 '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
_geom_angle_publ_flag
Cl4 Pb1 Cl2 98.03(8) . . ?
Cl4 Pb1 Cl3 161.76(19) . . ?
Cl2 Pb1 Cl3 100.21(17) . . ?
Cl4 Pb1 Cl4 80.21(11) . 5_667 ?
Cl2 Pb1 Cl4 178.24(8) . 5_667 ?
Cl3 Pb1 Cl4 81.54(18) . 5_667 ?
Cl4 Pb1 Cl1 90.81(11) . 1_545 ?
Cl2 Pb1 Cl1 91.67(11) . 1_545 ?
Cl3 Pb1 Cl1 88.67(11) . 1_545 ?
Cl4 Pb1 Cl1 88.37(11) 5_667 1_545 ?
Cl4 Pb1 Cl1 90.81(11) . . ?
Cl2 Pb1 Cl1 91.67(11) . . ?
Cl3 Pb1 Cl1 88.67(11) . . ?
Cl4 Pb1 Cl1 88.37(11) 5_667 . ?
Cl1 Pb1 Cl1 176.1(2) 1_545 . ?
Pb1 Cl1 Pb1 176.1(2) 1_565 . ?
Pb1 Cl2 Pb1 180.0 . 5_666 ?
Pb1 Cl3 Pb1 164.8(3) . 2_565 ?
Pb1 Cl4 Pb1 99.78(11) . 5_667 ?
N1 N1 C1 76.3(9) 2_675 . ?
N1 N1 C1 76.3(9) 2_675 2_675 ?
C1 N1 C1 37(2) . 2_675 ?
C2 N2 C2 33(3) . 8_755 ?
C2 N2 C2 34(3) . 7_575 ?
C2 N2 C2 49(2) 8_755 7_575 ?
C2 N2 C2 49(2) . 2_675 ?
C2 N2 C2 34(3) 8_755 2_675 ?
C2 N2 C2 33(3) 7_575 2_675 ?
C2 N2 C3 114.2(17) . . ?
C2 N2 C3 84(3) 8_755 . ?
C2 N2 C3 127(2) 7_575 . ?
C2 N2 C3 95(3) 2_675 . ?
C2 N2 C3 127(2) . 7_575 ?
C2 N2 C3 95(3) 8_755 7_575 ?
C2 N2 C3 114.2(17) 7_575 7_575 ?
C2 N2 C3 84(3) 2_675 7_575 ?
C3 N2 C3 38(3) . 7_575 ?
C2 N2 C3 84(3) . 8_755 ?
C2 N2 C3 114.2(17) 8_755 8_755 ?
C2 N2 C3 95(3) 7_575 8_755 ?
C2 N2 C3 127(2) 2_675 8_755 ?
C3 N2 C3 129(4) . 8_755 ?
C3 N2 C3 148(4) 7_575 8_755 ?
C2 N2 C3 95(3) . 2_675 ?
C2 N2 C3 127(2) 8_755 2_675 ?
C2 N2 C3 84(3) 7_575 2_675 ?
C2 N2 C3 114.2(17) 2_675 2_675 ?
C3 N2 C3 148(4) . 2_675 ?
C3 N2 C3 129(4) 7_575 2_675 ?
C3 N2 C3 38(3) 8_755 2_675 ?
C2 N2 C4 108.8(15) . . ?
C2 N2 C4 108.8(15) 8_755 . ?
C2 N2 C4 74(2) 7_575 . ?
C2 N2 C4 74(2) 2_675 . ?
C3 N2 C4 108.7(14) . . ?
C3 N2 C4 70.4(16) 7_575 . ?
C3 N2 C4 108.7(14) 8_755 . ?
C3 N2 C4 70.4(16) 2_675 . ?
C2 N2 C4 74(2) . 2_675 ?
C2 N2 C4 74(2) 8_755 2_675 ?
C2 N2 C4 108.8(15) 7_575 2_675 ?
C2 N2 C4 108.8(15) 2_675 2_675 ?
C3 N2 C4 70.4(16) . 2_675 ?
C3 N2 C4 108.7(14) 7_575 2_675 ?
C3 N2 C4 70.4(16) 8_755 2_675 ?
C3 N2 C4 108.7(14) 2_675 2_675 ?
C4 N2 C4 177(3) . 2_675 ?
C1 C1 C2 88(3) 2_675 2_675 ?
C1 C1 C2 88(3) 2_675 8_755 ?
C2 C1 C2 43(3) 2_675 8_755 ?
C1 C1 N1 71.6(12) 2_675 2_675 ?
C2 C1 N1 139(2) 2_675 2_675 ?
C2 C1 N1 158(4) 8_755 2_675 ?
C1 C1 N1 71.6(12) 2_675 . ?
C2 C1 N1 158(4) 2_675 . ?
C2 C1 N1 139(2) 8_755 . ?
N1 C1 N1 27.5(18) 2_675 . ?
C1 C1 C2 53.4(16) 2_675 . ?
C2 C1 C2 52(2) 2_675 . ?
C2 C1 C2 34(3) 8_755 . ?
N1 C1 C2 125(2) 2_675 . ?
N1 C1 C2 115.5(18) . . ?
C1 C1 C2 53.4(16) 2_675 7_575 ?
C2 C1 C2 34(3) 2_675 7_575 ?
C2 C1 C2 52(2) 8_755 7_575 ?
N1 C1 C2 115.5(18) 2_675 7_575 ?
N1 C1 C2 125(2) . 7_575 ?
C2 C1 C2 34(3) . 7_575 ?
C2 C2 C2 90.00(2) 8_755 7_575 ?
C2 C2 C1 92(3) 8_755 2_675 ?
C2 C2 C1 68.7(14) 7_575 2_675 ?
C2 C2 C2 46(4) 8_755 2_675 ?
C2 C2 C2 44(4) 7_575 2_675 ?
C1 C2 C2 76(2) 2_675 2_675 ?
C2 C2 N2 73.4(14) 8_755 . ?
C2 C2 N2 72.8(14) 7_575 . ?
C1 C2 N2 139(3) 2_675 . ?
C2 C2 N2 65.7(12) 2_675 . ?
C2 C2 C1 53.4(16) 8_755 . ?
C2 C2 C1 73.0(13) 7_575 . ?
C1 C2 C1 39(3) 2_675 . ?
C2 C2 C1 51.4(14) 2_675 . ?
N2 C2 C1 115.2(19) . . ?
C2 C2 C4 76.6(11) 8_755 2_675 ?
C2 C2 C4 127.1(9) 7_575 2_675 ?
C1 C2 C4 160(3) 2_675 2_675 ?
C2 C2 C4 106(3) 2_675 2_675 ?
N2 C2 C4 54.3(13) . 2_675 ?
C1 C2 C4 128(2) . 2_675 ?
C2 C2 C3 117.7(14) 8_755 8_755 ?
C2 C2 C3 91.4(15) 7_575 8_755 ?
C1 C2 C3 144(3) 2_675 8_755 ?
C2 C2 C3 110(2) 2_675 8_755 ?
N2 C2 C3 48.2(14) . 8_755 ?
C1 C2 C3 161.2(18) . 8_755 ?
C4 C2 C3 54.3(18) 2_675 8_755 ?
C3 C3 N2 70.8(14) 7_575 . ?
C3 C3 C4 127.1(9) 7_575 2_675 ?
N2 C3 C4 56.2(11) . 2_675 ?
C3 C3 C2 88.6(15) 7_575 8_755 ?
N2 C3 C2 47.9(15) . 8_755 ?
C4 C3 C2 58(3) 2_675 8_755 ?
N2 C4 C3 53.4(10) . 2_675 ?
N2 C4 C3 53.4(10) . 7_575 ?
C3 C4 C3 101(3) 2_675 7_575 ?
N2 C4 C2 51.3(14) . 7_575 ?
C3 C4 C2 67(2) 2_675 7_575 ?
C3 C4 C2 88.4(17) 7_575 7_575 ?
N2 C4 C2 51.3(14) . 2_675 ?
C3 C4 C2 88.4(17) 2_675 2_675 ?
C3 C4 C2 67(2) 7_575 2_675 ?
C2 C4 C2 27(2) 7_575 2_675 ?
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
Pb1 Cl4 2.843(4) . ?
Pb1 Cl2 2.8700(5) . ?
Pb1 Cl3 2.8763(13) . ?
Pb1 Cl4 2.892(4) 5_667 ?
Pb1 Cl1 2.9341(3) 1_545 ?
Pb1 Cl1 2.9341(3) . ?
Cl1 Pb1 2.9341(2) 1_565 ?
Cl2 Pb1 2.8701(5) 5_666 ?
Cl3 Pb1 2.8763(13) 2_565 ?
Cl4 Pb1 2.892(4) 5_667 ?
N1 N1 0.71(4) 2_675 ?
N1 C1 1.485(19) . ?
N1 C1 1.485(19) 2_675 ?
N2 C2 1.471(18) . ?
N2 C2 1.472(18) 8_755 ?
N2 C2 1.472(18) 7_575 ?
N2 C2 1.472(18) 2_675 ?
N2 C3 1.479(17) . ?
N2 C3 1.479(17) 7_575 ?
N2 C3 1.479(17) 8_755 ?
N2 C3 1.479(17) 2_675 ?
N2 C4 1.531(15) . ?
N2 C4 1.531(15) 2_675 ?
C1 C1 0.94(6) 2_675 ?
C1 C2 1.20(3) 2_675 ?
C1 C2 1.20(3) 8_755 ?
C1 N1 1.485(19) 2_675 ?
C1 C2 1.489(19) . ?
C1 C2 1.489(19) 7_575 ?
C2 C2 0.84(7) 8_755 ?
C2 C2 0.87(7) 7_575 ?
C2 C1 1.20(3) 2_675 ?
C2 C2 1.21(6) 2_675 ?
C2 C4 1.82(5) 2_675 ?
C2 C3 1.97(5) 8_755 ?
C3 C3 0.97(7) 7_575 ?
C3 C4 1.73(4) 2_675 ?
C3 C2 1.97(5) 8_755 ?
C4 C3 1.73(4) 2_675 ?
C4 C3 1.73(4) 7_575 ?
C4 C2 1.82(5) 7_575 ?
C4 C2 1.82(5) 2_675 ?
