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_4134349
_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_absolute_configuration ad
_chemical_formula_moiety         '2(C7 H9 Cl N +), I4 Pb 2-'
_chemical_formula_sum            'C14 H18 Cl2 I4 N2 Pb'
_chemical_formula_weight         999.99
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 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                 95.723(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.6180(3)
_cell_length_b                   8.9275(3)
_cell_length_c                   15.8350(5)
_cell_measurement_reflns_used    7969
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      66.73
_cell_measurement_theta_min      2.80
_cell_volume                     1212.23(7)
_computing_cell_refinement       'SAINT (Bruker, 2016)'
_computing_data_collection       'APEX3 (Bruker, 2016)'
_computing_data_reduction        SAINT
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8-QUEST PHOTON-100'
_diffrn_measurement_method       '\w and \f-scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0689
_diffrn_reflns_av_unetI/netI     0.0675
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            13967
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        66.906
_diffrn_reflns_theta_max         66.906
_diffrn_reflns_theta_min         2.804
_diffrn_source                   'Incoatec I\mS Cu microsource'
_exptl_absorpt_coefficient_mu    55.550
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.3383
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2014)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.740
_exptl_crystal_description       lath
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.010
_refine_diff_density_max         5.382
_refine_diff_density_min         -2.521
_refine_diff_density_rms         0.444
_refine_ls_abs_structure_details
;
Flack x determined using 1543 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.02(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     186
_refine_ls_number_reflns         4305
_refine_ls_number_restraints     97
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0781
_refine_ls_R_factor_gt           0.0698
_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^)+(0.1655P)^2^+0.2545P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2005
_refine_ls_wR_factor_ref         0.2107
_reflns_Friedel_coverage         0.861
_reflns_Friedel_fraction_full    0.991
_reflns_Friedel_fraction_max     0.991
_reflns_number_gt                3791
_reflns_number_total             4305
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b11809_si_004.cif
_cod_data_source_block           chlorobenzylammonium_180K
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4134349
_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_B1_0021
_shelx_estimated_absorpt_t_min   0.036
_shelx_estimated_absorpt_t_max   0.607
_shelx_res_checksum              46014
_shelx_hkl_checksum              99003