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_4134352
_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 H9 F N +), I4 Pb 2-'
_chemical_formula_sum            'C14 H18 F2 I4 N2 Pb'
_chemical_formula_weight         967.09
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_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                 97.7423(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.7325(2)
_cell_length_b                   9.2819(2)
_cell_length_c                   27.7240(6)
_cell_measurement_reflns_used    12214
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.00
_cell_volume                     2226.66(9)
_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 0.994
_diffrn_measured_fraction_theta_max 0.964
_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  0.0738
_diffrn_reflns_av_unetI/netI     0.0854
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            14729
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.469
_diffrn_reflns_theta_min         3.675
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    13.138
_exptl_absorpt_correction_T_max  0.374
_exptl_absorpt_correction_T_min  0.283
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SORTAV (Blessing, 1995)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.885
_exptl_crystal_description       block
_exptl_crystal_F_000             1712
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.312
_refine_diff_density_min         -2.030
_refine_diff_density_rms         0.339
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     210
_refine_ls_number_reflns         4911
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.0930
_refine_ls_R_factor_gt           0.0472
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0406P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0903
_refine_ls_wR_factor_ref         0.1044
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3062
_reflns_number_total             4911
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b11809_si_003.cif
_cod_data_source_block           fluorobenzylammonium_180K
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4134352
_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_0011
_shelx_estimated_absorpt_t_min   0.560
_shelx_estimated_absorpt_t_max   0.560
_shelx_res_checksum              62742
_shelx_hkl_checksum              21746