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_1545807
_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, C8 H14 N2'
_chemical_formula_sum            'C8 H14 Br4 N2 Pb'
_chemical_formula_weight         665.04
_chemical_name_systematic
'3-(2-ammonioethyl)-anilinium 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             2015-12-16
_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                 95.197(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.7688(3)
_cell_length_b                   8.5108(4)
_cell_length_c                   24.6314(11)
_cell_measurement_reflns_used    9887
_cell_measurement_temperature    298
_cell_measurement_theta_max      31.52
_cell_measurement_theta_min      2.76
_cell_volume                     1621.90(12)
_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      298
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_wavelength     0.7749
_diffrn_reflns_av_R_equivalents  0.0889
_diffrn_reflns_av_unetI/netI     0.0436
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            32430
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        27.706
_diffrn_reflns_theta_max         27.833
_diffrn_reflns_theta_min         2.609
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    24.973
_exptl_absorpt_correction_T_max  0.2999
_exptl_absorpt_correction_T_min  0.0924
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/2 (Bruker,2014/2) was used for absorption correction.
wR2(int) was 0.1698 before and 0.1064 after correction.
The Ratio of minimum to maximum transmission is 0.3081.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.724
_exptl_crystal_description       plate
_exptl_crystal_F_000             1192
_exptl_crystal_preparation       ', Luminescent'
_exptl_crystal_recrystallization_method 'Slow-cooled from concentrated HBr'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.01
_refine_diff_density_max         4.194
_refine_diff_density_min         -2.671
_refine_diff_density_rms         0.432
_refine_ls_extinction_coef       0.0019(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     140
_refine_ls_number_reflns         3017
_refine_ls_number_restraints     83
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0780
_refine_ls_R_factor_gt           0.0710
_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^)+(0.0960P)^2^+64.7434P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2031
_refine_ls_wR_factor_ref         0.2092
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2659
_reflns_number_total             3017
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7sc01590a2.cif
_cod_data_source_block           g1_p21c_0p83_a
_cod_database_code               1545807
_shelxl_version_number           2014-3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.9664(13) 0.0336(13)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H,H) groups
3. Restrained distances
 C2-C1
 1.54 with sigma of 0.02
4. Rigid bond restraints
 N2, N1, C5, C6, C4, C7, C3, C8, C1, C2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
N2 \\sim N1 \\sim C5 \\sim C6 \\sim C4 \\sim C7 \\sim C3 \\sim C8 \\sim C1
\\sim C2: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
6.a Secondary CH2 refined with riding coordinates:
 C1(H1D,H1E), C2(H2D,H2E)
6.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C4(H4), C7(H7), C8(H8)
6.c Idealised Me refined as rotating group:
 N2(H2A,H2B,H2C), N1(H1A,H1B,H1C)
;
_shelx_res_checksum              17559
_olex2_submission_special_instructions 'No special instructions were received'