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#$Date: 2020-03-07 01:43:11 +0200 (Sat, 07 Mar 2020) $
#$Revision: 249141 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/43/4134350.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_4134350
loop_
_publ_author_name
'Schmitt, Tanja'
'Bourelle, Sean'
'Tye, Nathaniel'
'Soavi, Giancarlo'
'Bond, Andrew D.'
'Feldmann, Sascha'
'Traore, Boubacar'
'Katan, Claudine'
'Even, Jacky'
'Dutton, Siân E'
'Deschler, Felix'
_publ_section_title
;
 Control of crystal symmetry breaking with halogen substituted
 benzylammonium in layered hybrid metal-halide perovskites.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.9b11809
_journal_year                    2020
_chemical_formula_moiety         '2(C7 H10 N +), I4 Pb 2-'
_chemical_formula_sum            'C14 H20 I4 N2 Pb'
_chemical_formula_weight         931.11
_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
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/1
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.1437(2)
_cell_length_b                   8.6684(2)
_cell_length_c                   28.5984(5)
_cell_measurement_reflns_used    12409
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.00
_cell_volume                     2266.74(8)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'Mercury (Macrae et al., 2008)'
_computing_publication_material  SHELXL
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'ω and φ-scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0578
_diffrn_reflns_av_unetI/netI     0.0432
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            12744
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.479
_diffrn_reflns_theta_min         3.538
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    12.888
_exptl_absorpt_correction_T_max  0.527
_exptl_absorpt_correction_T_min  0.423
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SORTAV (Blessing, 1995)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.728
_exptl_crystal_description       block
_exptl_crystal_F_000             1648
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.055
_refine_diff_density_min         -1.404
_refine_diff_density_rms         0.211
_refine_ls_extinction_coef       0.00124(5)
_refine_ls_extinction_method     'SHELXL-2018/1 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     99
_refine_ls_number_reflns         2571
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0435
_refine_ls_R_factor_gt           0.0290
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0133P)²+5.1779P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0523
_refine_ls_wR_factor_ref         0.0561
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2094
_reflns_number_total             2571
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja9b11809_si_002.cif
_cod_data_source_block           benzylammonium_180K
_cod_original_cell_volume        2266.75(8)
_cod_database_code               4134350
_cambridge_user_name             'Tanja Schmitt'
_cambridge_user_crsid            trs49
_cambridge_supervisor_name       'Sian Dutton'
_cambridge_supervisor_crsid      sed33
_cambridge_crystallographer_name 'Andrew Bond'
_cambridge_crystallographer_crsid adb29
_cambridge_data_id               AB_K3_0012
_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   0.359
_shelx_estimated_absorpt_t_max   0.565
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 1.000000 0.500000 0.500000 0.02150(9) Uani 1 2 d S . P . .
I2 I 0.79434(4) 0.79788(4) 0.49256(2) 0.02891(12) Uani 1 1 d . . . . .
I1 I 0.95570(5) 0.47834(4) 0.61075(2) 0.03193(12) Uani 1 1 d . . . . .
N1 N 0.5825(5) 0.5660(5) 0.58680(15) 0.0333(11) Uani 1 1 d . . . . .
H1A H 0.550733 0.662566 0.594069 0.050 Uiso 1 1 calc R U . . .
H1B H 0.586460 0.555353 0.555165 0.050 Uiso 1 1 calc R U . . .
H1C H 0.673167 0.551057 0.599095 0.050 Uiso 1 1 calc R U . . .
C1 C 0.4427(7) 0.4863(6) 0.65658(19) 0.0301(13) Uani 1 1 d . . . . .
C2 C 0.5172(7) 0.4179(7) 0.6931(2) 0.0428(16) Uani 1 1 d . . . . .
H2A H 0.595078 0.348472 0.686634 0.051 Uiso 1 1 calc R U . . .
C3 C 0.4798(8) 0.4494(9) 0.7389(2) 0.053(2) Uani 1 1 d . . . . .
H3A H 0.530192 0.400353 0.763844 0.064 Uiso 1 1 calc R U . . .
C4 C 0.3702(9) 0.5512(8) 0.7481(2) 0.0491(17) Uani 1 1 d . . . . .
H4A H 0.344599 0.572846 0.779618 0.059 Uiso 1 1 calc R U . . .
C5 C 0.2970(8) 0.6222(9) 0.7130(3) 0.059(2) Uani 1 1 d . . . . .
H5A H 0.221010 0.693347 0.719898 0.071 Uiso 1 1 calc R U . . .
C6 C 0.3334(7) 0.5909(8) 0.6670(2) 0.0434(16) Uani 1 1 d . . . . .
H6A H 0.282856 0.641704 0.642377 0.052 Uiso 1 1 calc R U . . .
C7 C 0.4790(8) 0.4493(7) 0.6066(2) 0.0418(16) Uani 1 1 d . . . . .
H7A H 0.523846 0.345514 0.604897 0.050 Uiso 1 1 calc R U . . .
H7B H 0.388065 0.447935 0.587838 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 0.0061 0.0033 '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
I1 Pb1 I1 179.999(15) 5_766 . ?
I1 Pb1 I2 87.777(9) 5_766 . ?
I1 Pb1 I2 92.222(9) . . ?
I1 Pb1 I2 92.222(9) 5_766 5_766 ?
I1 Pb1 I2 87.779(9) . 5_766 ?
I2 Pb1 I2 180.0 . 5_766 ?
I1 Pb1 I2 85.848(9) 5_766 4_566 ?
I1 Pb1 I2 94.152(9) . 4_566 ?
I2 Pb1 I2 93.240(3) . 4_566 ?
I2 Pb1 I2 86.760(3) 5_766 4_566 ?
I1 Pb1 I2 94.152(9) 5_766 8_755 ?
I1 Pb1 I2 85.848(9) . 8_755 ?
I2 Pb1 I2 86.760(3) . 8_755 ?
I2 Pb1 I2 93.240(3) 5_766 8_755 ?
I2 Pb1 I2 180.0 4_566 8_755 ?
Pb1 I2 Pb1 157.801(13) . 4_466 ?
C7 N1 H1A 109.5 . . ?
C7 N1 H1B 109.5 . . ?
H1A N1 H1B 109.5 . . ?
C7 N1 H1C 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C2 C1 C6 118.4(6) . . ?
C2 C1 C7 121.2(6) . . ?
C6 C1 C7 120.3(5) . . ?
C1 C2 C3 120.6(6) . . ?
C1 C2 H2A 119.7 . . ?
C3 C2 H2A 119.7 . . ?
C4 C3 C2 119.6(6) . . ?
C4 C3 H3A 120.2 . . ?
C2 C3 H3A 120.2 . . ?
C5 C4 C3 121.0(7) . . ?
C5 C4 H4A 119.5 . . ?
C3 C4 H4A 119.5 . . ?
C4 C5 C6 119.8(7) . . ?
C4 C5 H5A 120.1 . . ?
C6 C5 H5A 120.1 . . ?
C1 C6 C5 120.5(6) . . ?
C1 C6 H6A 119.8 . . ?
C5 C6 H6A 119.8 . . ?
N1 C7 C1 110.9(5) . . ?
N1 C7 H7A 109.5 . . ?
C1 C7 H7A 109.5 . . ?
N1 C7 H7B 109.5 . . ?
C1 C7 H7B 109.5 . . ?
H7A C7 H7B 108.1 . . ?
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 3.1985(4) 5_766 ?
Pb1 I1 3.1986(4) . ?
Pb1 I2 3.2014(3) . ?
Pb1 I2 3.2014(3) 5_766 ?
Pb1 I2 3.2184(3) 4_566 ?
Pb1 I2 3.2184(3) 8_755 ?
N1 C7 1.497(8) . ?
N1 H1A 0.9100 . ?
N1 H1B 0.9100 . ?
N1 H1C 0.9100 . ?
C1 C2 1.381(8) . ?
C1 C6 1.382(8) . ?
C1 C7 1.501(8) . ?
C2 C3 1.382(9) . ?
C2 H2A 0.9500 . ?
C3 C4 1.361(10) . ?
C3 H3A 0.9500 . ?
C4 C5 1.355(10) . ?
C4 H4A 0.9500 . ?
C5 C6 1.383(9) . ?
C5 H5A 0.9500 . ?
C6 H6A 0.9500 . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
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
C6 C1 C2 C3 2.3(9) . . . . ?
C7 C1 C2 C3 -178.0(6) . . . . ?
C1 C2 C3 C4 -1.3(10) . . . . ?
C2 C3 C4 C5 0.0(11) . . . . ?
C3 C4 C5 C6 0.2(11) . . . . ?
C2 C1 C6 C5 -2.0(9) . . . . ?
C7 C1 C6 C5 178.3(6) . . . . ?
C4 C5 C6 C1 0.8(11) . . . . ?
C2 C1 C7 N1 -95.7(7) . . . . ?
C6 C1 C7 N1 84.0(7) . . . . ?
