#------------------------------------------------------------------------------
#$Date: 2021-05-19 00:52:09 +0300 (Wed, 19 May 2021) $
#$Revision: 265311 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/51/87/4518729.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_4518729
loop_
_publ_author_name
'Menahem, Matan'
'Dai, Zhenbang'
'Aharon, Sigalit'
'Sharma, Rituraj'
'Asher, Maor'
'Diskin-Posner, Yael'
'Korobko, Roman'
'Rappe, Andrew M.'
'Yaffe, Omer'
_publ_section_title
;
 Strongly Anharmonic Octahedral Tilting in Two-Dimensional Hybrid Halide
 Perovskites
;
_journal_name_full               'ACS Nano'
_journal_paper_doi               10.1021/acsnano.1c02022
_journal_year                    2021
_chemical_formula_moiety         'I4 Pb, 2(C4 H12 N)'
_chemical_formula_sum            'C8 H24 I4 N2 Pb'
_chemical_formula_weight         863.08
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_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                   8.8763(3)
_cell_length_b                   8.6936(3)
_cell_length_c                   27.6162(13)
_cell_measurement_reflns_used    6783
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.8390
_cell_measurement_theta_min      2.7060
_cell_volume                     2131.06(14)
_computing_cell_refinement       'CrysAlisPro 1.171.40.60a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.60a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.60a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'ShelXS (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, Pilatus 300K'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0314
_diffrn_reflns_av_unetI/netI     0.0199
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            16631
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.367
_diffrn_reflns_theta_min         1.475
_exptl_absorpt_coefficient_mu    13.696
_exptl_absorpt_correction_T_max  0.532
_exptl_absorpt_correction_T_min  0.378
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.60a (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.690
_exptl_crystal_description       block
_exptl_crystal_F_000             1520
_exptl_crystal_size_max          0.115
_exptl_crystal_size_mid          0.085
_exptl_crystal_size_min          0.059
_refine_diff_density_max         0.600
_refine_diff_density_min         -0.577
_refine_diff_density_rms         0.097
_refine_ls_extinction_coef       0.00081(4)
_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   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     73
_refine_ls_number_reflns         2184
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0352
_refine_ls_R_factor_gt           0.0256
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0210P)²+4.2410P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0586
_refine_ls_wR_factor_ref         0.0616
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1733
_reflns_number_total             2184
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            nn1c02022_si_004.cif
_cod_data_source_block           oy8_mt2_1_293_10
_cod_database_code               4518729
_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.
;
_shelx_estimated_absorpt_t_min   0.302
_shelx_estimated_absorpt_t_max   0.499
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -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
Pb1 Pb 0.5000 1.0000 0.5000 0.04998(11) Uani 1 2 d S . P . .
I1 I 0.69628(4) 0.69450(5) 0.50418(2) 0.07294(16) Uani 1 1 d . . . . .
I2 I 0.46666(6) 0.98578(5) 0.61548(2) 0.08005(16) Uani 1 1 d . . . . .
N1 N 0.5751(7) 0.4284(7) 0.4061(2) 0.0945(18) Uani 1 1 d . . . . .
H1A H 0.5611 0.3294 0.3992 0.113 Uiso 1 1 calc R U . . .
H1B H 0.5591 0.4440 0.4375 0.113 Uiso 1 1 calc R U . . .
H1C H 0.6691 0.4550 0.3987 0.113 Uiso 1 1 calc R U . . .
C1 C 0.4678(14) 0.5234(12) 0.3774(6) 0.155(5) Uani 1 1 d . . . . .
H1D H 0.3659 0.4931 0.3857 0.186 Uiso 1 1 calc R U . . .
H1E H 0.4800 0.6303 0.3867 0.186 Uiso 1 1 calc R U . . .
C2 C 0.4844(15) 0.5124(15) 0.3285(5) 0.180(7) Uani 1 1 d . . . . .
H2A H 0.4679 0.4072 0.3181 0.216 Uiso 1 1 calc R U . . .
H2B H 0.5857 0.5423 0.3193 0.216 Uiso 1 1 calc R U . . .
C3 C 0.3689(16) 0.620(2) 0.3043(6) 0.223(7) Uani 1 1 d D . . . .
H3A H 0.2674 0.5910 0.3138 0.268 Uiso 1 1 calc R U . . .
H3B H 0.3866 0.7253 0.3139 0.268 Uiso 1 1 calc R U . . .
C4 C 0.387(2) 0.603(3) 0.2540(5) 0.339(13) Uani 1 1 d D . . . .
H4A H 0.3159 0.6672 0.2374 0.508 Uiso 1 1 calc R U . . .
H4B H 0.3709 0.4976 0.2450 0.508 Uiso 1 1 calc R U . . .
H4C H 0.4877 0.6328 0.2450 0.508 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'
I I -0.4742 1.8119 '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'
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
I1 Pb1 I1 179.999(15) . 5_676 ?
I1 Pb1 I1 88.758(4) . 8_765 ?
I1 Pb1 I1 91.242(4) 5_676 8_765 ?
I1 Pb1 I1 91.242(4) . 4_466 ?
I1 Pb1 I1 88.758(4) 5_676 4_466 ?
I1 Pb1 I1 180.00(2) 8_765 4_466 ?
I1 Pb1 I2 91.017(11) . 5_676 ?
I1 Pb1 I2 88.983(11) 5_676 5_676 ?
I1 Pb1 I2 86.412(12) 8_765 5_676 ?
I1 Pb1 I2 93.588(12) 4_466 5_676 ?
I1 Pb1 I2 88.983(11) . . ?
I1 Pb1 I2 91.017(11) 5_676 . ?
I1 Pb1 I2 93.588(12) 8_765 . ?
I1 Pb1 I2 86.412(12) 4_466 . ?
I2 Pb1 I2 180.0 5_676 . ?
Pb1 I1 Pb1 155.020(15) . 4_566 ?
C1 N1 H1A 109.5 . . ?
C1 N1 H1B 109.5 . . ?
H1A N1 H1B 109.5 . . ?
C1 N1 H1C 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C2 C1 N1 114.8(11) . . ?
C2 C1 H1D 108.6 . . ?
N1 C1 H1D 108.6 . . ?
C2 C1 H1E 108.6 . . ?
N1 C1 H1E 108.6 . . ?
H1D C1 H1E 107.5 . . ?
C1 C2 C3 108.4(13) . . ?
C1 C2 H2A 110.0 . . ?
C3 C2 H2A 110.0 . . ?
C1 C2 H2B 110.0 . . ?
C3 C2 H2B 110.0 . . ?
H2A C2 H2B 108.4 . . ?
C4 C3 C2 106.8(16) . . ?
C4 C3 H3A 110.3 . . ?
C2 C3 H3A 110.4 . . ?
C4 C3 H3B 110.4 . . ?
C2 C3 H3B 110.4 . . ?
H3A C3 H3B 108.6 . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
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 3.1784(4) . ?
Pb1 I1 3.1785(4) 5_676 ?
Pb1 I1 3.1844(4) 8_765 ?
Pb1 I1 3.1844(4) 4_466 ?
Pb1 I2 3.2052(5) 5_676 ?
Pb1 I2 3.2053(5) . ?
I1 Pb1 3.1844(4) 4_566 ?
N1 C1 1.490(12) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
C1 C2 1.361(19) . ?
C1 H1D 0.9700 . ?
C1 H1E 0.9700 . ?
C2 C3 1.537(16) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.408(9) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C2 C3 -178.6(10) . . . . ?
C1 C2 C3 C4 -178.9(16) . . . . ?
