#------------------------------------------------------------------------------
#$Date: 2020-02-29 01:44:47 +0200 (Sat, 29 Feb 2020) $
#$Revision: 248542 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/42/4134275.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_4134275
loop_
_publ_author_name
'Zhang, Han-Yue'
'Song, Xian-Jiang'
'Chen, Xiao-Gang'
'Zhang, Zhi-Xu'
'You, Yu-Meng'
'Tang, Yuan-Yuan'
'Xiong, Ren-Gen'
_publ_section_title
;
 Observation of vortex domains in a two-dimensional lead iodide perovskite
 ferroelectric.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.0c00371
_journal_year                    2020
_chemical_formula_moiety         'I3 Pb, C5 H9 N, F'
_chemical_formula_sum            'C5 H9 F I3 N Pb'
_chemical_formula_weight         690.03
_space_group_crystal_system      orthorhombic
_space_group_IT_number           63
_space_group_name_Hall           '-C 2c 2'
_space_group_name_H-M_alt        'C m c m'
_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            4
_cell_length_a                   8.7441(14)
_cell_length_b                   19.056(3)
_cell_length_c                   8.0199(9)
_cell_measurement_reflns_used    1248
_cell_measurement_temperature    403(2)
_cell_measurement_theta_max      29.8270
_cell_measurement_theta_min      3.3160
_cell_volume                     1336.3(3)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      403(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.1677
_diffrn_reflns_av_unetI/netI     0.0818
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            3245
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        24.998
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         2.563
_diffrn_source                   'Rotating-anode X-ray tube'
_exptl_absorpt_coefficient_mu    19.524
_exptl_absorpt_correction_T_max  0.014
_exptl_absorpt_correction_T_min  0.004
_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    3.430
_exptl_crystal_description       prism
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.22
_refine_diff_density_max         2.885
_refine_diff_density_min         -3.185
_refine_diff_density_rms         0.637
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     39
_refine_ls_number_reflns         685
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.1304
_refine_ls_R_factor_gt           0.1049
_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)+(0.1840P)²+0.3798P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2548
_refine_ls_wR_factor_ref         0.2796
_reflns_Friedel_coverage         0.000
_reflns_number_gt                483
_reflns_number_total             686
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja0c00371_si_007.cif
_cod_data_source_block           CMCM
_cod_original_formula_sum        '	C5 H9 F I3 N Pb'
_cod_database_code               4134275
_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, z+1/2'
'-x, y, -z+1/2'
'x, -y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x, y, -z-1/2'
'x, -y, z-1/2'
'-x, y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, y+1/2, -z-1/2'
'x+1/2, -y+1/2, z-1/2'
'-x+1/2, 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
F1 F 0.693(3) 0.7437(9) 0.2500 0.1787(4) Uani 0.5 2 d S TU P . .
C2 C 0.5000 0.81648(4) 0.06208(16) 0.1783(2) Uani 1 2 d DS TU P . .
H2A H 0.4121 0.8147 -0.0095 0.214 Uiso 0.5 1 d R U P . .
H2B H 0.5879 0.8147 -0.0095 0.214 Uiso 0.5 1 d R U P . .
C3 C 0.5000 0.7572(9) 0.165(2) 0.1786(3) Uani 1 2 d S TU P . .
H3A H 0.4544 0.7172 0.1114 0.214 Uiso 0.75 1 d R U P . .
C1 C 0.5000 0.88004(4) 0.14460(16) 0.1782(2) Uani 0.5 2 d DS TU P . .
N1 N 0.5000 0.88004(4) 0.14460(16) 0.1782(2) Uani 0.5 2 d S TU P . .
H1A H 0.4170 0.9032 0.1016 0.214 Uiso 0.25 1 d R U P . .
H1B H 0.5830 0.9032 0.1016 0.214 Uiso 0.25 1 d R U P . .
Pb1 Pb 0.0000 1.0000 0.0000 0.07106(16) Uani 1 4 d S T P . .
I1 I 0.25596(9) 1.06063(4) 0.2500 0.0946(3) Uani 1 2 d S T P . .
I2 I 0.0000 0.86680(5) 0.2500 0.1016(4) Uani 1 4 d S T 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'
F F 0.0171 0.0103 '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
_geom_angle_publ_flag
C3 F1 C3 43.7(12) 10_556 . ?
C1 C2 C3 115.3(7) . . ?
C3 C3 C2 126.1(7) 10_556 . ?
C3 C3 F1 68.1(6) 10_556 . ?
C2 C3 F1 109.4(7) . . ?
C3 C3 F1 68.1(6) 10_556 3_655 ?
C2 C3 F1 109.4(7) . 3_655 ?
F1 C3 F1 133.1(12) . 3_655 ?
C2 C1 N1 118.65(7) . 10_556 ?
C2 C1 C1 118.65(7) . 10_556 ?
N1 C1 C1 0.0 10_556 10_556 ?
I1 Pb1 I1 88.09(2) 9_575 11_575 ?
I1 Pb1 I1 91.91(2) 9_575 3 ?
I1 Pb1 I1 180.0 11_575 3 ?
I1 Pb1 I1 180.0 9_575 . ?
I1 Pb1 I1 91.91(2) 11_575 . ?
I1 Pb1 I1 88.09(2) 3 . ?
I1 Pb1 I2 84.007(15) 9_575 9_575 ?
I1 Pb1 I2 84.007(15) 11_575 9_575 ?
I1 Pb1 I2 95.993(15) 3 9_575 ?
I1 Pb1 I2 95.993(15) . 9_575 ?
I1 Pb1 I2 95.993(15) 9_575 . ?
I1 Pb1 I2 95.993(15) 11_575 . ?
I1 Pb1 I2 84.007(15) 3 . ?
I1 Pb1 I2 84.008(15) . . ?
I2 Pb1 I2 180.0 9_575 . ?
Pb1 I1 Pb1 77.040(19) . 2_575 ?
Pb1 I2 Pb1 76.61(2) 2_575 . ?
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
F1 C3 1.84(2) 10_556 ?
F1 C3 1.84(2) . ?
C2 C1 1.3801(11) . ?
C2 C3 1.397(17) . ?
C3 C3 1.37(4) 10_556 ?
C3 F1 1.84(2) 3_655 ?
C1 N1 1.691(3) 10_556 ?
C1 C1 1.691(3) 10_556 ?
Pb1 I1 3.2193(7) 9_575 ?
Pb1 I1 3.2193(7) 11_575 ?
Pb1 I1 3.2193(7) 3 ?
Pb1 I1 3.2194(7) . ?
Pb1 I2 3.2346(8) 9_575 ?
Pb1 I2 3.2347(8) . ?
I1 Pb1 3.2194(7) 2_575 ?
I2 Pb1 3.2347(8) 2_575 ?
