#------------------------------------------------------------------------------
#$Date: 2023-10-29 01:49:08 +0300 (Sun, 29 Oct 2023) $
#$Revision: 287161 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/43/7714328.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_7714328
loop_
_publ_author_name
'Jung, Mi Hee'
_publ_section_title
;
 Diammonium Spacer-Induced Stable Zigzag Type 2D Dion-Jacobson
 Lead/Tin-Based Perovskite Solar Cells
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT02041J
_journal_year                    2023
_chemical_formula_sum            'C12 H20 I6 N4 Pb'
_chemical_formula_weight         1188.91
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2022-07-27 deposited with the CCDC.	2023-10-28 downloaded from the CCDC.
;
_cell_angle_alpha                91.10(3)
_cell_angle_beta                 108.87(3)
_cell_angle_gamma                112.65(3)
_cell_formula_units_Z            1
_cell_length_a                   8.6700(17)
_cell_length_b                   8.7800(18)
_cell_length_c                   10.557(2)
_cell_measurement_reflns_used    15298
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      33.749
_cell_measurement_theta_min      0.401
_cell_volume                     692.2(3)
_computing_cell_refinement       'HKL3000sm (Otwinowski & Minor, 1997)'
_computing_data_collection       'PAL BL2D-SMDC Program (Shin et. al, 2016)'
_computing_data_reduction        'HKL3000sm (Otwinowski & Minor, 1997)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.931
_diffrn_measured_fraction_theta_max 0.748
_diffrn_measurement_device_type  'Rayonix MX225HS CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.700
_diffrn_reflns_av_R_equivalents  0.0215
_diffrn_reflns_av_unetI/netI     0.0280
_diffrn_reflns_Laue_measured_fraction_full 0.931
_diffrn_reflns_Laue_measured_fraction_max 0.748
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8340
_diffrn_reflns_point_group_measured_fraction_full 0.931
_diffrn_reflns_point_group_measured_fraction_max 0.748
_diffrn_reflns_theta_full        24.835
_diffrn_reflns_theta_max         33.605
_diffrn_reflns_theta_min         2.036
_diffrn_source                   'PLSII 2D bending magnet'
_exptl_absorpt_coefficient_mu    12.164
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.951
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'HKL3000sm Scalepack(Otwinowski et.al,2003)'
_exptl_crystal_density_diffrn    2.852
_exptl_crystal_description       plate
_exptl_crystal_F_000             520
_refine_diff_density_max         5.408
_refine_diff_density_min         -1.639
_refine_diff_density_rms         0.322
_refine_ls_extinction_coef       0.0110(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.418
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     107
_refine_ls_number_reflns         4275
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.418
_refine_ls_R_factor_all          0.0424
_refine_ls_R_factor_gt           0.0422
_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)+(0.0691P)²+0.6199P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1288
_refine_ls_wR_factor_ref         0.1289
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4223
_reflns_number_total             4275
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3dt02041j2.cif
_cod_data_source_block           3APPbI3_1_a
_cod_database_code               7714328
_shelx_shelxl_version_number     2017/1
_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'
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 1.000000 0.500000 0.500000 0.03077(10) Uani 1 2 d S . P . .
N1 N 0.5135(9) 0.2640(8) 1.0044(5) 0.0494(14) Uani 1 1 d . . . . .
H1 H 0.467482 0.229729 1.064982 0.059 Uiso 1 1 calc R U . . .
C1 C 0.6592(9) 0.4047(9) 1.0389(6) 0.0480(14) Uani 1 1 d . . . . .
H1A H 0.708701 0.465968 1.125896 0.058 Uiso 1 1 calc R U . . .
I1 I 0.57241(4) 0.36265(5) 0.36817(4) 0.04105(12) Uani 1 1 d . . . . .
I3 I 1.01585(5) 0.74676(5) 0.73696(4) 0.04147(12) Uani 1 1 d . . . . .
C3 C 0.6577(8) 0.3680(8) 0.8134(6) 0.0432(12) Uani 1 1 d . . . . .
H3 H 0.706941 0.405316 0.747615 0.052 Uiso 1 1 calc R U . . .
I2 I 0.96402(5) 0.21082(4) 0.69033(4) 0.03891(12) Uani 1 1 d . . . . .
N2 N 0.2858(7) 0.1709(8) 0.5511(5) 0.0446(11) Uani 1 1 d . . . . .
H2A H 0.235645 0.107289 0.469769 0.067 Uiso 1 1 calc R U . . .
H2B H 0.201469 0.160982 0.585136 0.067 Uiso 1 1 calc R U . . .
H2C H 0.341060 0.277292 0.543384 0.067 Uiso 1 1 calc R U . . .
C2 C 0.7373(9) 0.4599(10) 0.9431(7) 0.0525(17) Uani 1 1 d . . . . .
H2 H 0.841705 0.557342 0.965647 0.063 Uiso 1 1 calc R U . . .
C5 C 0.4331(9) 0.1712(8) 0.8805(6) 0.0441(13) Uani 1 1 d . . . . .
H5 H 0.329132 0.073943 0.861206 0.053 Uiso 1 1 calc R U . . .
C4 C 0.5054(7) 0.2209(7) 0.7818(5) 0.0352(10) Uani 1 1 d . . . . .
C6 C 0.4193(9) 0.1156(8) 0.6443(6) 0.0419(12) Uani 1 1 d . . . . .
H6 H 0.359534 -0.000747 0.651830 0.050 Uiso 1 1 calc R U . . .
H00D H 0.510381 0.124942 0.606712 0.050 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 0.0064 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4611 1.7922 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.1439 9.9644 '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
I1 Pb1 I1 180.000(14) . 2_766 ?
I1 Pb1 I3 91.50(4) . . ?
I1 Pb1 I3 88.50(4) 2_766 . ?
I1 Pb1 I3 88.50(4) . 2_766 ?
I1 Pb1 I3 91.50(4) 2_766 2_766 ?
I3 Pb1 I3 180.0 . 2_766 ?
I1 Pb1 I2 89.45(3) . 2_766 ?
I1 Pb1 I2 90.55(3) 2_766 2_766 ?
I3 Pb1 I2 90.43(2) . 2_766 ?
I3 Pb1 I2 89.57(2) 2_766 2_766 ?
I1 Pb1 I2 90.55(3) . . ?
I1 Pb1 I2 89.45(3) 2_766 . ?
I3 Pb1 I2 89.57(2) . . ?
I3 Pb1 I2 90.43(2) 2_766 . ?
I2 Pb1 I2 180.0 2_766 . ?
C1 N1 C5 123.9(5) . . ?
N1 C1 C2 118.8(6) . . ?
C4 C3 C2 120.0(5) . . ?
C3 C2 C1 119.2(6) . . ?
N1 C5 C4 119.5(5) . . ?
C5 C4 C3 118.6(5) . . ?
C5 C4 C6 119.9(5) . . ?
C3 C4 C6 121.5(5) . . ?
C4 C6 N2 110.4(5) . . ?
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 I1 3.2077(13) . ?
Pb1 I1 3.2077(13) 2_766 ?
Pb1 I3 3.2109(11) . ?
Pb1 I3 3.2109(11) 2_766 ?
Pb1 I2 3.2516(10) 2_766 ?
Pb1 I2 3.2516(10) . ?
N1 C1 1.318(9) . ?
N1 C5 1.338(8) . ?
C1 C2 1.387(9) . ?
C3 C4 1.381(8) . ?
C3 C2 1.385(10) . ?
N2 C6 1.503(9) . ?
C5 C4 1.378(8) . ?
C4 C6 1.496(8) . ?
