#------------------------------------------------------------------------------
#$Date: 2020-02-27 01:45:02 +0200 (Thu, 27 Feb 2020) $
#$Revision: 248459 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/42/4134253.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_4134253
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           28
_space_group_name_Hall           'P 2 -2a'
_space_group_name_H-M_alt        'P m a 2'
_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                   14.8771(9)
_cell_length_b                   9.4425(5)
_cell_length_c                   5.8322(4)
_cell_measurement_reflns_used    4468
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.8840
_cell_measurement_theta_min      2.5510
_cell_volume                     819.29(9)
_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      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0908
_diffrn_reflns_av_unetI/netI     0.0539
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            5551
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.991
_diffrn_reflns_theta_max         24.991
_diffrn_reflns_theta_min         2.555
_diffrn_source                   'Rotating-anode X-ray tube'
_exptl_absorpt_coefficient_mu    21.476
_exptl_absorpt_correction_T_max  0.019
_exptl_absorpt_correction_T_min  0.017
_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    2.964
_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         2.756
_refine_diff_density_min         -2.842
_refine_diff_density_rms         0.406
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.50(10)
_refine_ls_extinction_coef       0.0077(12)
_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   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     86
_refine_ls_number_reflns         1462
_refine_ls_number_restraints     61
_refine_ls_restrained_S_all      0.986
_refine_ls_R_factor_all          0.0585
_refine_ls_R_factor_gt           0.0545
_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)+(0.0751P)²+50.8163P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1520
_refine_ls_wR_factor_ref         0.1569
_reflns_Friedel_coverage         0.807
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                1330
_reflns_number_total             1462
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja0c00375_si_002.cif
_cod_data_source_block           PMA2
_cod_database_code               4134253
_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   0.099
_shelx_estimated_absorpt_t_max   0.106
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'x+1/2, -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 0.05869(6) 0.71145(10) 0.4837(19) 0.0302(6) Uani 1 1 d . . . . .
Cl1 Cl 0.0000 1.0000 0.464(8) 0.067(5) Uani 1 2 d S T P . .
Cl2 Cl 0.0639(6) 0.7054(11) 0.966(6) 0.052(4) Uani 1 1 d . . . . .
Cl3 Cl 0.1135(5) 0.4184(8) 0.472(5) 0.050(2) Uani 1 1 d . . . . .
Cl4 Cl 0.2500 0.7540(14) 0.496(7) 0.060(4) Uani 1 2 d S T P . .
N1 N 0.2500 0.523(4) -0.071(14) 0.06(2) Uani 1 2 d DS T P . .
H1A H 0.2133 0.5910 -0.0154 0.096 Uiso 0.5 1 d R U P . .
H1B H 0.3070 0.5422 -0.0290 0.096 Uiso 0.5 1 d R U P . .
H1C H 0.2500 0.5220 -0.2251 0.096 Uiso 1 2 d R U P . .
N2 N 0.2500 0.126(4) 0.009(7) 0.050(9) Uani 1 2 d DS TU P . .
C1 C 0.222(3) 0.384(4) 0.023(10) 0.027(16) Uani 0.5 1 d D U P . .
H1D H 0.1612 0.3647 -0.0196 0.033 Uiso 0.5 1 d R U P . .
H1E H 0.2254 0.3860 0.1877 0.033 Uiso 0.5 1 d R U P . .
C2 C 0.282(4) 0.269(4) -0.068(12) 0.047(13) Uani 0.5 1 d D U P . .
H2A H 0.2826 0.2721 -0.2325 0.056 Uiso 0.5 1 d R U P . .
H2B H 0.3417 0.2833 -0.0135 0.056 Uiso 0.5 1 d R U P . .
C3 C 0.2500 0.115(7) 0.266(6) 0.060(14) Uani 1 2 d DS TU P . .
H3A H 0.3027 0.1610 0.3258 0.090 Uiso 1 1 d R U . . .
H3C H 0.2500 0.0175 0.3120 0.090 Uiso 1 2 d R U P . .
C4 C 0.170(3) 0.051(7) -0.087(8) 0.096(17) Uani 1 1 d D U . . .
H4A H 0.1698 0.0569 -0.2515 0.144 Uiso 1 1 d R U . . .
H4B H 0.1695 -0.0463 -0.0411 0.144 Uiso 1 1 d R U . . .
H4C H 0.1180 0.0983 -0.0272 0.144 Uiso 1 1 d 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'
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
Cl2 Pb1 Cl3 92.4(6) . 2_565 ?
Cl2 Pb1 Cl1 93.9(10) . . ?
Cl3 Pb1 Cl1 97.74(15) 2_565 . ?
Cl2 Pb1 Cl4 87.2(9) . . ?
Cl3 Pb1 Cl4 162.5(3) 2_565 . ?
Cl1 Pb1 Cl4 99.8(3) . . ?
Cl2 Pb1 Cl3 89.9(6) . . ?
Cl3 Pb1 Cl3 80.8(2) 2_565 . ?
Cl1 Pb1 Cl3 176.0(11) . . ?
Cl4 Pb1 Cl3 81.6(3) . . ?
Cl2 Pb1 Cl2 176.2(4) . 1_554 ?
Cl3 Pb1 Cl2 89.4(6) 2_565 1_554 ?
Cl1 Pb1 Cl2 89.1(10) . 1_554 ?
Cl4 Pb1 Cl2 90.1(8) . 1_554 ?
Cl3 Pb1 Cl2 87.1(6) . 1_554 ?
Pb1 Cl1 Pb1 175.3(19) . 2_575 ?
Pb1 Cl2 Pb1 176.2(4) . 1_556 ?
Pb1 Cl3 Pb1 99.1(2) 2_565 . ?
Pb1 Cl4 Pb1 163.7(6) . 4 ?
C1 N1 C1 32(4) 4 . ?
C2 N2 C2 37(5) 4 . ?
C2 N2 C4 94(3) 4 . ?
C2 N2 C4 124(4) . . ?
C2 N2 C4 124(4) 4 4 ?
C2 N2 C4 94(3) . 4 ?
C4 N2 C4 105(6) . 4 ?
C2 N2 C3 111(4) 4 . ?
C2 N2 C3 111(4) . . ?
C4 N2 C3 110(2) . . ?
C4 N2 C3 110(2) 4 . ?
C1 C1 C2 93(4) 4 4 ?
C1 C1 N1 74(2) 4 . ?
C2 C1 N1 130(6) 4 . ?
C1 C1 C2 54(3) 4 . ?
C2 C1 C2 39(6) 4 . ?
N1 C1 C2 110(4) . . ?
C2 C2 C1 87(4) 4 4 ?
C2 C2 N2 72(3) 4 . ?
C1 C2 N2 131(5) 4 . ?
C2 C2 C1 54(3) 4 . ?
C1 C2 C1 33(5) 4 . ?
N2 C2 C1 111(3) . . ?
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 Cl2 2.81(4) . ?
Pb1 Cl3 2.841(8) 2_565 ?
Pb1 Cl1 2.863(2) . ?
Pb1 Cl4 2.875(2) . ?
Pb1 Cl3 2.886(7) . ?
Pb1 Cl2 3.02(4) 1_554 ?
Cl1 Pb1 2.864(2) 2_575 ?
Cl2 Pb1 3.02(4) 1_556 ?
Cl3 Pb1 2.841(8) 2_565 ?
Cl4 Pb1 2.875(2) 4 ?
N1 C1 1.49(3) 4 ?
N1 C1 1.49(3) . ?
N2 C2 1.49(3) 4 ?
N2 C2 1.49(3) . ?
N2 C4 1.49(2) . ?
N2 C4 1.49(2) 4 ?
N2 C3 1.51(3) . ?
C1 C1 0.83(10) 4 ?
C1 C2 1.21(5) 4 ?
C1 C2 1.50(3) . ?
C2 C2 0.94(13) 4 ?
C2 C1 1.21(5) 4 ?
