Control of crystal symmetry breaking with halogen substituted benzylammonium in layered hybrid metal-halide perovskites.
Schmitt, Tanja; Bourelle, Sean; Tye, Nathaniel; Soavi, Giancarlo; Bond, Andrew D.; Feldmann, Sascha; Traore, Boubacar; Katan, Claudine; Even, Jacky; Dutton, Siân E; Deschler, Felix; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.9b11809

data_4134350
_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       '\w and \f-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/[\s^2^(Fo^2^)+(0.0133P)^2^+5.1779P] where P=(Fo^2^+2Fc^2^)/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 > 2\s(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_estimated_absorpt_t_min   0.359
_shelx_estimated_absorpt_t_max   0.565
_shelx_res_checksum              68881
_shelx_hkl_checksum              74453