#------------------------------------------------------------------------------
#$Date: 2020-10-04 06:25:37 +0300 (Sun, 04 Oct 2020) $
#$Revision: 257111 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/49/4134992.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_4134992
loop_
_publ_author_name
'Chen, Xiao-Gang'
'Song, Xian-Jiang'
'Zhang, Zhi-Xu'
'Zhang, Han-Yue'
'Pan, Qiang'
'Yao, Jie'
'You, Yu-Meng'
'Xiong, Ren-Gen'
_publ_section_title
;
 Confinement-Driven Ferroelectricity in a Two-Dimensional Hybrid Lead
 Iodide Perovskite.
;
_journal_issue                   22
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10212
_journal_page_last               10218
_journal_paper_doi               10.1021/jacs.0c03710
_journal_volume                  142
_journal_year                    2020
_chemical_formula_moiety         'I4 Pb, 2(C6 H12 F2 N) '
_chemical_formula_sum            'C12 H24 F4 I4 N2 Pb'
_chemical_formula_weight         987.13
_space_group_crystal_system      orthorhombic
_space_group_IT_number           36
_space_group_name_Hall           'C 2c -2'
_space_group_name_H-M_alt        'C m c 21'
_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                   8.5418(6)
_cell_length_b                   26.836(2)
_cell_length_c                   10.0432(6)
_cell_measurement_reflns_used    3198
_cell_measurement_temperature    343(2)
_cell_measurement_theta_max      29.5520
_cell_measurement_theta_min      2.5500
_cell_volume                     2302.2(3)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      343(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.816
_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  0.0996
_diffrn_reflns_av_unetI/netI     0.0598
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.816
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5458
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.814
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.646
_diffrn_reflns_theta_min         2.502
_diffrn_source                   'Rotating-anode X-ray tube'
_exptl_absorpt_coefficient_mu    12.721
_exptl_absorpt_correction_T_max  0.101
_exptl_absorpt_correction_T_min  0.076
_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            red
_exptl_crystal_density_diffrn    2.848
_exptl_crystal_description       sheet
_exptl_crystal_F_000             1760
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         2.263
_refine_diff_density_min         -2.140
_refine_diff_density_rms         0.314
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.232(9)
_refine_ls_extinction_coef       0.00048(7)
_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   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     150
_refine_ls_number_reflns         3529
_refine_ls_number_restraints     149
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0842
_refine_ls_R_factor_gt           0.0706
_refine_ls_shift/su_max          0.021
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1326P)²+34.6830P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2083
_refine_ls_wR_factor_ref         0.2233
_reflns_Friedel_coverage         0.896
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.812
_reflns_number_gt                1895
_reflns_number_total             3529
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja0c03710_si_008.cif
_cod_data_source_block           CMC21
_cod_depositor_comments
;Adding full bibliography for 4134988--4134996.cif.

 Adding full bibliography for 4134988--4134996.cif.
;
_cod_database_code               4134992
_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'
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
C1 C 1.0000 0.6315(4) 0.312(2) 0.100(5) Uani 1 2 d DS TU P . .
H1C H 1.1073 0.6305 0.2841 0.120 Uiso 0.5 1 d R U P . .
H1D H 0.9484 0.6556 0.2569 0.120 Uiso 0.5 1 d R U P . .
C2 C 0.9249(16) 0.5832(3) 0.2795(15) 0.073(5) Uani 0.5 1 d D U P . .
H2C H 0.9393 0.5770 0.1862 0.088 Uiso 0.5 1 d R U P . .
H2D H 0.8144 0.5844 0.2963 0.088 Uiso 0.5 1 d R U P . .
C3 C 1.0000 0.5387(4) 0.3442(9) 0.137(5) Uani 1 2 d DS TU P . .
C4 C 1.0000 0.5399(5) 0.4924(9) 0.115(6) Uani 1 2 d DS TU P . .
H4A H 1.0988 0.5531 0.5213 0.138 Uiso 0.5 1 d R U P . .
H4B H 1.0000 0.5068 0.5276 0.138 Uiso 1 2 d R U P . .
C5 C 0.8916(16) 0.5720(3) 0.5688(17) 0.093(6) Uani 0.5 1 d D U P . .
H5A H 0.8662 0.5605 0.6567 0.112 Uiso 0.5 1 d R U P . .
H5B H 0.7996 0.5691 0.5145 0.112 Uiso 0.5 1 d R U P . .
N1 N 0.9231(18) 0.6271(3) 0.5698(12) 0.102(6) Uani 0.5 1 d D U P . .
H1A H 0.8319 0.6462 0.5926 0.122 Uiso 0.5 1 d R U P . .
H1B H 1.0000 0.6299 0.6437 0.122 Uiso 1 2 d R U P . .
C7 C 1.0000 0.8705(4) 0.582(2) 0.096(5) Uani 1 2 d DS TU P . .
H7A H 1.1060 0.8810 0.5970 0.116 Uiso 0.5 1 d R U P . .
H7B H 0.9748 0.8478 0.6529 0.116 Uiso 0.5 1 d R U P . .
C8 C 0.9105(14) 0.9173(3) 0.6107(15) 0.071(5) Uani 0.5 1 d D U P . .
H8A H 0.8137 0.9144 0.5629 0.085 Uiso 0.5 1 d R U P . .
H8B H 0.8886 0.9228 0.7033 0.085 Uiso 0.5 1 d R U P . .
C9 C 1.0000 0.9581(4) 0.5391(8) 0.080(4) Uani 1 2 d DS TU P . .
C10 C 1.0000 0.9601(4) 0.3911(8) 0.096(4) Uani 1 2 d DS TU P . .
H10A H 1.1073 0.9639 0.3646 0.115 Uiso 0.5 1 d R U P . .
H10B H 0.9485 0.9909 0.3704 0.115 Uiso 0.5 1 d R U P . .
C11 C 0.9308(19) 0.9212(2) 0.3055(14) 0.084(4) Uani 0.5 1 d D U P . .
H11A H 0.8191 0.9249 0.3100 0.101 Uiso 0.5 1 d R U P . .
H11B H 0.9613 0.9295 0.2162 0.101 Uiso 0.5 1 d R U P . .
N2 N 0.9618(19) 0.8672(2) 0.3376(10) 0.079(5) Uani 0.5 1 d D U P . .
H2A H 0.8756 0.8499 0.2973 0.095 Uiso 0.5 1 d R U P . .
H2B H 1.0506 0.8608 0.2816 0.095 Uiso 0.5 1 d R U P . .
F1 F 0.8758(13) 0.5141(4) 0.3219(15) 0.163(4) Uani 1 1 d . U . . .
F2 F 0.8795(13) 0.9872(4) 0.5871(15) 0.160(5) Uani 1 1 d . U . . .
I2 I 0.5000 0.63391(4) 0.47766(12) 0.0683(3) Uani 1 2 d S TU P . .
I3 I 0.5000 0.86992(4) 0.41886(13) 0.0737(3) Uani 1 2 d S TU P . .
I4 I 0.75050(11) 0.75132(2) 0.21049(9) 0.0760(3) Uani 1 1 d . U . . .
C6 C 1.0000 0.6527(5) 0.4537(10) 0.073(5) Uani 1 2 d DS TU P . .
H6A H 0.9559 0.6831 0.4486 0.087 Uiso 0.5 1 d R U P . .
H6B H 1.1008 0.6575 0.4764 0.087 Uiso 0.5 1 d R U P . .
C12 C 1.0000 0.8398(5) 0.4640(10) 0.094(5) Uani 1 2 d DS TU P . .
H12A H 1.0941 0.8250 0.4558 0.113 Uiso 0.5 1 d R U P . .
H12B H 0.9281 0.8154 0.4718 0.113 Uiso 0.5 1 d R U P . .
Pb1 Pb 0.5000 0.75140(2) 0.43357(7) 0.05300(12) Uani 1 2 d S TU 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
C2 C1 C2 51.2(11) 4_755 . ?
C2 C1 C6 122.1(14) 4_755 . ?
C2 C1 C6 122.1(14) . . ?
C2 C2 C1 64.4(5) 4_755 . ?
C2 C2 C3 64.8(5) 4_755 . ?
C1 C2 C3 114.4(11) . . ?
F1 C3 F1 113.3(14) 4_755 . ?
F1 C3 C4 100.8(9) 4_755 . ?
F1 C3 C4 100.8(9) . . ?
F1 C3 C2 133.9(11) 4_755 . ?
F1 C3 C2 88.9(8) . . ?
C4 C3 C2 114.5(10) . . ?
F1 C3 C2 88.9(8) 4_755 4_755 ?
F1 C3 C2 133.9(11) . 4_755 ?
C4 C3 C2 114.5(10) . 4_755 ?
C2 C3 C2 50.5(11) . 4_755 ?
C5 C4 C5 77.5(12) 4_755 . ?
C5 C4 C3 122.1(10) 4_755 . ?
C5 C4 C3 122.1(10) . . ?
C4 C5 N1 117.7(11) . . ?
C4 C5 C5 51.3(6) . 4_755 ?
N1 C5 C5 79.7(8) . 4_755 ?
N1 N1 C5 100.3(8) 4_755 . ?
N1 N1 C6 64.1(6) 4_755 . ?
C5 N1 C6 121.5(11) . . ?
C12 C7 C8 129.4(14) . . ?
C12 C7 C8 129.4(14) . 4_755 ?
C8 C7 C8 61.4(10) . 4_755 ?
C7 C8 C9 104.9(10) . . ?
C7 C8 C8 59.3(5) . 4_755 ?
C9 C8 C8 59.7(5) . 4_755 ?
F2 C9 F2 96.6(12) 4_755 . ?
F2 C9 C10 109.2(8) 4_755 . ?
F2 C9 C10 109.2(8) . . ?
F2 C9 C8 82.3(7) 4_755 4_755 ?
F2 C9 C8 128.2(10) . 4_755 ?
C10 C9 C8 120.0(9) . 4_755 ?
F2 C9 C8 128.2(10) 4_755 . ?
F2 C9 C8 82.3(7) . . ?
C10 C9 C8 120.0(9) . . ?
C8 C9 C8 60.5(10) 4_755 . ?
C11 C10 C11 47.2(13) 4_755 . ?
C11 C10 C9 123.8(9) 4_755 . ?
C11 C10 C9 123.8(9) . . ?
C11 C11 C10 66.4(6) 4_755 . ?
C11 C11 N2 79.9(9) 4_755 . ?
C10 C11 N2 119.0(11) . . ?
C11 C11 N2 58.3(7) 4_755 4_755 ?
C10 C11 N2 105.6(10) . 4_755 ?
N2 C11 N2 21.6(11) . 4_755 ?
N2 N2 C12 77.5(6) 4_755 . ?
N2 N2 C11 100.1(9) 4_755 . ?
C12 N2 C11 133.5(10) . . ?
N2 N2 C11 58.3(7) 4_755 4_755 ?
C12 N2 C11 116.7(10) . 4_755 ?
C11 N2 C11 41.8(11) . 4_755 ?
N1 C6 N1 51.8(12) 4_755 . ?
N1 C6 C1 123.4(10) 4_755 . ?
N1 C6 C1 123.4(10) . . ?
C7 C12 N2 114.5(11) . 4_755 ?
C7 C12 N2 114.5(11) . . ?
N2 C12 N2 25.1(12) 4_755 . ?
I4 Pb1 I4 87.37(4) 4_655 . ?
I4 Pb1 I2 95.73(2) 4_655 . ?
I4 Pb1 I2 95.73(2) . . ?
I4 Pb1 I3 88.12(3) 4_655 . ?
I4 Pb1 I3 88.12(3) . . ?
I2 Pb1 I3 174.67(4) . . ?
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
C1 C2 1.484(13) 4_755 ?
C1 C2 1.484(13) . ?
C1 C6 1.53(2) . ?
C2 C2 1.28(3) 4_755 ?
C2 C3 1.504(13) . ?
C3 F1 1.271(13) 4_755 ?
C3 F1 1.271(13) . ?
C3 C4 1.488(12) . ?
C3 C2 1.504(13) 4_755 ?
C4 C5 1.479(14) 4_755 ?
C4 C5 1.480(14) . ?
C5 N1 1.503(9) . ?
C5 C5 1.85(3) 4_755 ?
N1 N1 1.31(3) 4_755 ?
N1 C6 1.504(14) . ?
C7 C12 1.45(2) . ?
C7 C8 1.498(13) . ?
C7 C8 1.498(13) 4_755 ?
C8 C9 1.516(13) . ?
C8 C8 1.53(2) 4_755 ?
C9 F2 1.378(14) 4_755 ?
C9 F2 1.378(13) . ?
C9 C10 1.487(11) . ?
C9 C8 1.516(13) 4_755 ?
C10 C11 1.476(13) 4_755 ?
C10 C11 1.476(13) . ?
C11 C11 1.18(3) 4_755 ?
C11 N2 1.509(9) . ?
C11 N2 1.746(14) 4_755 ?
N2 N2 0.65(3) 4_755 ?
N2 C12 1.503(13) . ?
N2 C11 1.746(14) 4_755 ?
I2 Pb1 3.1838(12) . ?
I3 Pb1 3.1840(12) . ?
I4 Pb1 3.0981(10) . ?
C6 N1 1.504(14) 4_755 ?
C12 N2 1.503(13) 4_755 ?
Pb1 I4 3.0981(10) 4_655 ?
