#------------------------------------------------------------------------------
#$Date: 2020-02-29 01:44:59 +0200 (Sat, 29 Feb 2020) $
#$Revision: 248543 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/42/4134276.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_4134276
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 F N'
_chemical_formula_sum            'C5 H9 F I3 N Pb'
_chemical_formula_weight         690.03
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n 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            4
_cell_length_a                   8.0887(10)
_cell_length_b                   10.4653(14)
_cell_length_c                   14.9244(19)
_cell_measurement_reflns_used    2079
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      30.4590
_cell_measurement_theta_min      2.8720
_cell_volume                     1263.4(3)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      223(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  0.2900
_diffrn_reflns_av_unetI/netI     0.1313
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            5194
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.377
_diffrn_source                   'Rotating-anode X-ray tube'
_exptl_absorpt_coefficient_mu    20.651
_exptl_absorpt_correction_T_max  0.009
_exptl_absorpt_correction_T_min  0.003
_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    3.628
_exptl_crystal_description       block
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.23
_refine_diff_density_max         9.993
_refine_diff_density_min         -8.778
_refine_diff_density_rms         1.638
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     58
_refine_ls_number_reflns         1175
_refine_ls_number_restraints     110
_refine_ls_restrained_S_all      1.928
_refine_ls_R_factor_all          0.2227
_refine_ls_R_factor_gt           0.2091
_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)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.5026
_refine_ls_wR_factor_ref         0.5216
_reflns_Friedel_coverage         0.000
_reflns_number_gt                937
_reflns_number_total             1179
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja0c00371_si_003.cif
_cod_data_source_block           Pnma
_cod_database_code               4134276
_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+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'
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 0.47096(18) 0.2500 0.24889(8) 0.0320(4) Uani 1 2 d S TU P . .
I1 I 0.7085(2) 0.04474(17) 0.33999(14) 0.0415(5) Uani 1 1 d . U . . .
I2 I 0.2328(3) 0.2500 0.4173(2) 0.0446(7) Uani 1 2 d S TU P . .
C1 C 0.88237(17) 0.1291(17) 0.6008(4) 0.034(3) Uani 1 1 d D U . . .
H1A H 0.9312 0.0609 0.6347 0.041 Uiso 1 1 d R U . . .
H1B H 0.8991 0.1120 0.5382 0.041 Uiso 1 1 d R U . . .
C2 C 0.960(4) 0.2500 0.625(2) 0.032(4) Uani 1 2 d S TU P . .
H2A H 1.0724 0.2500 0.6044 0.038 Uiso 1 2 d R U P . .
C3 C 0.614(4) 0.2500 0.576(3) 0.038(4) Uani 1 2 d S TU P . .
H3A H 0.4966 0.2500 0.5837 0.045 Uiso 1 2 d R U P . .
H3B H 0.6407 0.2500 0.5131 0.045 Uiso 1 2 d R U P . .
C4 C 0.69828(17) 0.1367(17) 0.6205(5) 0.036(3) Uani 0.5 1 d D U P . .
F1 F 0.955(3) 0.2500 0.7260(15) 0.053(6) Uani 1 2 d S TU P . .
N1 N 0.69828(17) 0.1367(17) 0.6205(5) 0.036(3) Uani 0.5 1 d . U P . .
H1C H 0.6825 0.1484 0.6802 0.043 Uiso 0.5 1 d R U P . .
H1D H 0.6480 0.0633 0.6055 0.043 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'
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
I2 Pb1 I1 91.61(6) . 7_565 ?
I2 Pb1 I1 91.61(6) . . ?
I1 Pb1 I1 84.76(7) 7_565 . ?
I2 Pb1 I2 176.97(8) . 6_656 ?
I1 Pb1 I2 86.16(6) 7_565 6_656 ?
I1 Pb1 I2 86.16(6) . 6_656 ?
I2 Pb1 I1 85.86(6) . 6_556 ?
I1 Pb1 I1 176.99(6) 7_565 6_556 ?
I1 Pb1 I1 96.93(5) . 6_556 ?
I2 Pb1 I1 96.43(6) 6_656 6_556 ?
I2 Pb1 I1 85.86(6) . 4_455 ?
I1 Pb1 I1 96.93(5) 7_565 4_455 ?
I1 Pb1 I1 176.99(6) . 4_455 ?
I2 Pb1 I1 96.43(6) 6_656 4_455 ?
I1 Pb1 I1 81.27(7) 6_556 4_455 ?
Pb1 I1 Pb1 77.14(4) . 6_656 ?
Pb1 I2 Pb1 77.95(7) . 6_556 ?
C2 C1 C4 109.1(15) . . ?
C1 C2 C1 121(2) 7_565 . ?
C1 C2 F1 103.6(16) 7_565 . ?
C1 C2 F1 103.6(16) . . ?
N1 C3 C4 0.0 7_565 7_565 ?
N1 C3 C4 102.5 7_565 . ?
C4 C3 C4 102(2) 7_565 . ?
C3 C4 C1 113.2(16) . . ?
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 I2 3.167(3) . ?
Pb1 I1 3.187(2) 7_565 ?
Pb1 I1 3.187(2) . ?
Pb1 I2 3.262(3) 6_656 ?
Pb1 I1 3.298(2) 6_556 ?
Pb1 I1 3.298(2) 4_455 ?
I1 Pb1 3.298(2) 6_656 ?
I2 Pb1 3.262(3) 6_556 ?
C1 C2 1.46(2) . ?
C1 C4 1.5200(17) . ?
C2 C1 1.46(2) 7_565 ?
C2 F1 1.51(4) . ?
C3 N1 1.52(3) 7_565 ?
C3 C4 1.52(3) 7_565 ?
C3 C4 1.52(3) . ?
