Structural Origins of Broadband Emission from Layered Pb‒Br Hybrid Perovskites
Smith, Matthew D.; Jaffe, Adam; Dohner, Emma R.; Lindenberg, Aaron; Karunadasa, Hemamala I.; Chem. Sci.  (2017) –; doi:10.1039/C7SC01590A

data_1545803
_publ_section_title
;
 Structural Origins of Broadband Emission from Layered Pb--Br Hybrid
 Perovskites
;
_journal_name_full               'Chem. Sci.'
_journal_paper_doi               10.1039/C7SC01590A
_journal_year                    2017
_chemical_formula_moiety         'Br4 Pb, C5 H11 N3'
_chemical_formula_sum            'C5 H11 Br4 N3 Pb'
_chemical_formula_weight         640.00
_chemical_name_systematic        'histammonium tetrabromoplumbate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-11-18
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2016-12-06 deposited with the CCDC.
2017-04-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.061(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.6055(13)
_cell_length_b                   11.6091(14)
_cell_length_c                   11.9312(14)
_cell_measurement_reflns_used    9997
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      32.760
_cell_measurement_theta_min      2.526
_cell_volume                     1379.8(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0413
_diffrn_reflns_av_unetI/netI     0.0236
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            31826
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.510
_diffrn_reflns_theta_min         2.526
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    23.777
_exptl_absorpt_correction_T_max  0.3404
_exptl_absorpt_correction_T_min  0.1374
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/2 (Bruker,2014/2) was used for absorption correction.
wR2(int) was 0.1360 before and 0.0569 after correction.
The Ratio of minimum to maximum transmission is 0.4036.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    3.081
_exptl_crystal_description       plate
_exptl_crystal_F_000             1136
_exptl_crystal_preparation       ', Luminescent'
_exptl_crystal_recrystallization_method 'Slowly cooled from conc. HBr'
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.390
_refine_diff_density_min         -1.561
_refine_diff_density_rms         0.193
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     119
_refine_ls_number_reflns         4219
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0292
_refine_ls_R_factor_gt           0.0230
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0307P)^2^+0.5211P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0540
_refine_ls_wR_factor_ref         0.0562
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3697
_reflns_number_total             4219
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7sc01590a2.cif
_cod_data_source_block           g1_mono_p_0p70_a
_cod_database_code               1545803
_shelxl_version_number           2014-3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All N(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C1(H1D,H1E)
2.b Aromatic/amide H refined with riding coordinates:
 N2(H2), N3(H3), C5(H5), C4(H4)
2.c Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C)
;
_shelx_res_checksum              80782
_olex2_exptl_crystal_mounting_method
'Mounted on a Mitegen loop using a trace of paratone'
_olex2_submission_special_instructions 'No special instructions were received'