#------------------------------------------------------------------------------
#$Date: 2021-02-04 05:31:20 +0200 (Thu, 04 Feb 2021) $
#$Revision: 261502 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/55/4135513.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_4135513
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 N P '
_chemical_formula_sum            'C5 H16 Br4 N P Pb'
_chemical_formula_weight         647.96
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90.145(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.0177(3)
_cell_length_b                   12.0789(5)
_cell_length_c                   9.9796(4)
_cell_measurement_reflns_used    4860
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      31.5720
_cell_measurement_theta_min      2.0300
_cell_volume                     725.39(6)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0569
_diffrn_reflns_av_unetI/netI     0.0522
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            4964
_diffrn_reflns_point_group_measured_fraction_full 0.922
_diffrn_reflns_point_group_measured_fraction_max 0.922
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.041
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    22.718
_exptl_absorpt_correction_T_max  0.003
_exptl_absorpt_correction_T_min  0.002
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.39a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.967
_exptl_crystal_description       sheet
_exptl_crystal_F_000             580
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.26
_refine_diff_density_max         3.918
_refine_diff_density_min         -2.336
_refine_diff_density_rms         0.429
_refine_ls_abs_structure_details
;
 Flack x determined using 888 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.03(2)
_refine_ls_extinction_coef       0.0350(5)
_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   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     86
_refine_ls_number_reflns         2341
_refine_ls_number_restraints     74
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0694
_refine_ls_R_factor_gt           0.0679
_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)+(0.0905P)²+39.1359P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1764
_refine_ls_wR_factor_ref         0.1774
_reflns_Friedel_coverage         0.771
_reflns_Friedel_fraction_full    0.847
_reflns_Friedel_fraction_max     0.847
_reflns_number_gt                2265
_reflns_number_total             2341
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja0c12907_si_003.cif
_cod_data_source_block           P21
_cod_depositor_comments
'Adding full bibliography for 4135512--4135514.cif.'
_cod_original_sg_symbol_H-M      'P 21'
_cod_original_formula_sum        'C5 H16 Br4 N P Pb '
_cod_database_code               4135513
_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.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -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 0.49638(6) 0.37217(3) 0.51089(3) 0.02154(8) Uani 1 1 d . U . . .
Br1 Br 0.4974(2) 0.43890(12) 0.22295(12) 0.0368(3) Uani 1 1 d . U . . .
Br2 Br 0.4928(2) 0.62562(11) 0.54423(13) 0.0431(4) Uani 1 1 d . U . . .
Br3 Br 0.4727(3) 0.33934(12) 0.80380(15) 0.0564(5) Uani 1 1 d . U . . .
Br4 Br -0.0017(2) 0.35492(14) 0.49205(13) 0.0435(4) Uani 1 1 d . U . . .
P1 P 0.0918(7) 0.6434(4) -0.0728(4) 0.0518(12) Uani 1 1 d . U . . .
C5 C 0.046(2) 0.6602(10) 0.1985(9) 0.0415(16) Uani 1 1 d D U . . .
H5A H -0.0689 0.7156 0.1874 0.050 Uiso 1 1 calc R U . . .
H5B H 0.1880 0.6983 0.2011 0.050 Uiso 1 1 calc R U . . .
N1 N 0.013(3) 0.6039(9) 0.3266(8) 0.071(5) Uani 1 1 d D U . . .
H1A H 0.0168 0.6533 0.3928 0.106 Uiso 1 1 calc R U . . .
H1B H -0.1187 0.5701 0.3262 0.106 Uiso 1 1 calc R U . . .
H1F H 0.1198 0.5540 0.3389 0.106 Uiso 1 1 calc R U . . .
C3 C 0.422(2) 0.6500(12) -0.1037(15) 0.0415(16) Uani 1 1 d . U . . .
H3A H 0.4913 0.6909 -0.0324 0.062 Uiso 1 1 calc R U . . .
H3B H 0.4815 0.5763 -0.1059 0.062 Uiso 1 1 calc R U . . .
H3C H 0.4512 0.6861 -0.1876 0.062 Uiso 1 1 calc R U . . .
C1 C 0.012(2) 0.7899(12) -0.0867(15) 0.0415(16) Uani 1 1 d . U . . .
H1C H 0.0577 0.8287 -0.0073 0.062 Uiso 1 1 calc R U . . .
H1D H 0.0832 0.8221 -0.1634 0.062 Uiso 1 1 calc R U . . .
H1E H -0.1462 0.7955 -0.0967 0.062 Uiso 1 1 calc R U . . .
C4 C 0.043(2) 0.5879(11) 0.0841(14) 0.0415(16) Uani 1 1 d . U . . .
H4A H -0.1016 0.5522 0.0814 0.050 Uiso 1 1 calc R U . . .
H4B H 0.1522 0.5303 0.0993 0.050 Uiso 1 1 calc R U . . .
C2 C 0.018(2) 0.5703(12) -0.2070(14) 0.0415(16) Uani 1 1 d . U . . .
H2A H 0.0552 0.6109 -0.2865 0.062 Uiso 1 1 calc R U . . .
H2B H 0.0962 0.5009 -0.2068 0.062 Uiso 1 1 calc R U . . .
H2C H -0.1389 0.5569 -0.2050 0.062 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'
P P 0.1023 0.0942 '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
Br3 Pb1 Br1 171.63(4) . . ?
Br3 Pb1 Br4 90.12(5) . . ?
Br1 Pb1 Br4 87.88(4) . . ?
Br3 Pb1 Br2 92.80(4) . 2_646 ?
Br1 Pb1 Br2 95.20(4) . 2_646 ?
Br4 Pb1 Br2 86.70(4) . 2_646 ?
Br3 Pb1 Br4 95.89(5) . 1_655 ?
Br1 Pb1 Br4 87.39(4) . 1_655 ?
Br4 Pb1 Br4 169.34(6) . 1_655 ?
Br2 Pb1 Br4 84.23(4) 2_646 1_655 ?
Br3 Pb1 Br2 91.50(4) . . ?
Br1 Pb1 Br2 80.53(4) . . ?
Br4 Pb1 Br2 93.92(4) . . ?
Br2 Pb1 Br2 175.658(15) 2_646 . ?
Br4 Pb1 Br2 94.71(4) 1_655 . ?
Pb1 Br2 Pb1 163.25(5) 2_656 . ?
Pb1 Br4 Pb1 169.34(6) . 1_455 ?
C2 P1 C4 118.5(7) . . ?
C2 P1 C1 112.4(7) . . ?
C4 P1 C1 113.3(7) . . ?
C2 P1 C3 99.1(7) . . ?
C4 P1 C3 109.0(7) . . ?
C1 P1 C3 102.0(7) . . ?
C4 C5 N1 114.2(10) . . ?
C5 C4 P1 118.8(10) . . ?
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 Br3 2.9537(15) . ?
Pb1 Br1 2.9844(12) . ?
Pb1 Br4 3.0101(13) . ?
Pb1 Br2 3.0292(14) 2_646 ?
Pb1 Br4 3.0337(13) 1_655 ?
Pb1 Br2 3.0795(14) . ?
Br2 Pb1 3.0292(14) 2_656 ?
Br4 Pb1 3.0337(13) 1_455 ?
P1 C2 1.663(15) . ?
P1 C4 1.729(15) . ?
P1 C1 1.839(15) . ?
P1 C3 2.014(14) . ?
C5 C4 1.437(17) . ?
C5 N1 1.463(12) . ?
