#------------------------------------------------------------------------------
#$Date: 2021-02-04 05:31:20 +0200 (Thu, 04 Feb 2021) $
#$Revision: 261502 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/55/4135512.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_4135512
loop_
_publ_author_name
'Zhang, Han-Yue'
'Zhang, Zhi-Xu'
'Chen, Xiao-Gang'
'Song, Xian-Jiang'
'Zhang, Yi'
'Xiong, Ren-Gen'
_publ_section_title
;
 Large Electrostrictive Coefficient in a Two-Dimensional Hybrid Perovskite
 Ferroelectric.
;
_journal_issue                   3
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1664
_journal_page_last               1672
_journal_paper_doi               10.1021/jacs.0c12907
_journal_volume                  143
_journal_year                    2021
_chemical_formula_moiety         'Br4 Pb, C5 H16 N2'
_chemical_formula_sum            'C5 H16 Br4 N Pb'
_chemical_formula_weight         631.00
_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                   11.9047(6)
_cell_length_b                   6.0106(4)
_cell_length_c                   9.7130(6)
_cell_measurement_reflns_used    2114
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      31.1750
_cell_measurement_theta_min      2.6850
_cell_volume                     695.01(7)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.847
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0863
_diffrn_reflns_av_unetI/netI     0.0668
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.847
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            3863
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.847
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.028
_diffrn_reflns_theta_min         2.706
_diffrn_source                   'Rotating-anode X-ray tube'
_exptl_absorpt_coefficient_mu    23.593
_exptl_absorpt_correction_T_max  0.003
_exptl_absorpt_correction_T_min  0.001
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.14e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.948
_exptl_crystal_description       sheet
_exptl_crystal_F_000             550
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.260
_exptl_crystal_size_min          0.250
_refine_diff_density_max         3.956
_refine_diff_density_min         -5.222
_refine_diff_density_rms         0.951
_refine_ls_extinction_coef       0.022(3)
_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   1.126
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     44
_refine_ls_number_reflns         1072
_refine_ls_number_restraints     88
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0996
_refine_ls_R_factor_gt           0.0820
_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)+(0.1486P)²+0.6366P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2151
_refine_ls_wR_factor_ref         0.2286
_reflns_Friedel_coverage         0.000
_reflns_number_gt                799
_reflns_number_total             1072
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja0c12907_si_002.cif
_cod_data_source_block           PMMA
_cod_depositor_comments
'Adding full bibliography for 4135512--4135514.cif.'
_cod_database_code               4135512
_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   0.053
_shelx_estimated_absorpt_t_max   0.067
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
C2 C 0.2500 0.269(13) 0.416(10) 0.149(10) Uani 0.5 2 d DS TU P . .
H2A H 0.1855 0.3223 0.4482 0.224 Uiso 0.25 1 d R U P . .
H2B H 0.3069 0.3241 0.4642 0.224 Uiso 0.25 1 d R U P . .
H2C H 0.2500 0.3086 0.3278 0.224 Uiso 0.5 2 d R U P . .
C3 C 0.323(4) 0.0000 0.542(4) 0.130(11) Uani 0.5 2 d DS TU P . .
H3A H 0.3515 -0.1366 0.5328 0.156 Uiso 0.25 1 d R U P . .
H3B H 0.3807 0.0921 0.5529 0.156 Uiso 0.25 1 d R U P . .
C4 C 0.2500 0.0000 0.668(4) 0.117(10) Uani 1 4 d DS TU P . .
H4A H 0.2055 -0.1173 0.6534 0.140 Uiso 0.25 1 d R U P . .
H4B H 0.2055 0.1173 0.6534 0.140 Uiso 0.25 1 d R U P . .
N2 N 0.2500 0.0000 0.820(4) 0.102(7) Uani 1 4 d DS TU P . .
H1D H 0.1839 0.0000 0.8490 0.152 Uiso 0.5 2 d R U P . .
H1E H 0.2830 -0.1140 0.8490 0.152 Uiso 0.25 1 d R U P . .
H1F H 0.2830 0.1140 0.8490 0.152 Uiso 0.25 1 d R U P . .
N1 N 0.2500 0.018(13) 0.417(4) 0.102(7) Uani 0.5 2 d DS TU P . .
Pb1 Pb 0.5000 0.5000 0.0000 0.0312(5) Uani 1 4 d S TU P . .
Br2 Br 0.5507(2) 0.5000 0.2984(2) 0.0704(8) Uani 1 2 d S TU P . .
Br3 Br 0.2500 0.5000 0.0457(4) 0.0737(11) Uani 1 4 d S TU P . .
Br4 Br 0.5000 0.0000 0.0000 0.0683(12) Uani 1 4 d S TU P . .
C1 C 0.364(2) 0.0000 0.355(4) 0.149(10) Uani 1 2 d DS TU P . .
H1A H 0.3739 -0.1476 0.3558 0.224 Uiso 0.5 1 d R U P . .
H1B H 0.3679 0.0496 0.2687 0.224 Uiso 0.5 1 d R U P . .
H1C H 0.4172 0.0652 0.4051 0.224 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'
Br Br -0.2901 2.4595 '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
N1 C3 N1 8(6) 2 . ?
N1 C3 C4 109(4) 2 . ?
N1 C3 C4 109(4) . . ?
N1 C3 C1 50.8(13) 2 . ?
N1 C3 C1 50.8(13) . . ?
C4 C3 C1 160(4) . . ?
N1 C3 C3 55(2) 2 2 ?
N1 C3 C3 55(2) . 2 ?
C4 C3 C3 54.8(19) . 2 ?
C1 C3 C3 105.2(19) . 2 ?
N2 C4 C3 144.8(19) . . ?
N2 C4 C3 144.8(19) . 2 ?
C3 C4 C3 70(4) . 2 ?
N1 N1 C1 86(3) 2 . ?
N1 N1 C1 86(3) 2 2 ?
C1 N1 C1 131(5) . 2 ?
N1 N1 C3 86(3) 2 2 ?
C1 N1 C3 148(4) . 2 ?
C1 N1 C3 78(2) 2 2 ?
N1 N1 C3 86(3) 2 . ?
C1 N1 C3 78(2) . . ?
C1 N1 C3 148(4) 2 . ?
C3 N1 C3 71(4) 2 . ?
N1 N1 C2 179(4) 2 . ?
C1 N1 C2 94(4) . . ?
C1 N1 C2 94(4) 2 . ?
C3 N1 C2 95(5) 2 . ?
C3 N1 C2 95(5) . . ?
Br2 Pb1 Br2 180.0 5_665 . ?
Br2 Pb1 Br4 90.0 5_665 1_565 ?
Br2 Pb1 Br4 90.0 . 1_565 ?
Br2 Pb1 Br4 90.0 5_665 . ?
Br2 Pb1 Br4 90.0 . . ?
Br4 Pb1 Br4 180.0 1_565 . ?
Br2 Pb1 Br3 93.28(10) 5_665 5_665 ?
Br2 Pb1 Br3 86.72(10) . 5_665 ?
Br4 Pb1 Br3 90.0 1_565 5_665 ?
Br4 Pb1 Br3 90.0 . 5_665 ?
Br2 Pb1 Br3 86.72(10) 5_665 . ?
Br2 Pb1 Br3 93.28(10) . . ?
Br4 Pb1 Br3 90.0 1_565 . ?
Br4 Pb1 Br3 90.0 . . ?
Br3 Pb1 Br3 180.0 5_665 . ?
Pb1 Br3 Pb1 163.03(16) 2_565 . ?
Pb1 Br4 Pb1 180.0 1_545 . ?
N1 C1 N1 8(6) 2 . ?
N1 C1 C3 51.0(15) 2 . ?
N1 C1 C3 51.0(15) . . ?
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
C2 N1 1.51(2) . ?
C3 N1 1.49(2) 2 ?
C3 N1 1.49(2) . ?
C3 C4 1.50(2) . ?
C3 C1 1.88(5) . ?
C3 C3 1.73(9) 2 ?
C4 N2 1.482(19) . ?
C4 C3 1.50(2) 2 ?
N1 N1 0.22(16) 2 ?
N1 C1 1.489(19) . ?
N1 C1 1.489(19) 2 ?
N1 C3 1.49(2) 2 ?
Pb1 Br2 2.960(2) 5_665 ?
Pb1 Br2 2.960(2) . ?
Pb1 Br4 3.0053(2) 1_565 ?
Pb1 Br4 3.0053(2) . ?
Pb1 Br3 3.0091(6) 5_665 ?
Pb1 Br3 3.0091(6) . ?
Br3 Pb1 3.0091(6) 2_565 ?
Br4 Pb1 3.0053(2) 1_545 ?
C1 N1 1.489(19) 2 ?
