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_1545808
_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         '0.5(Br24 Pb6), 6(C4 H10 N O2)'
_chemical_formula_sum            'C24 H60 Br12 N6 O12 Pb3'
_chemical_formula_weight         2205.27
_chemical_name_systematic
'bis(4-ammoniobutanoic acid) 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             2015-11-04
_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                 97.137(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.7721(12)
_cell_length_b                   8.0709(4)
_cell_length_c                   56.964(3)
_cell_measurement_reflns_used    9300
_cell_measurement_temperature    298
_cell_measurement_theta_max      25.815
_cell_measurement_theta_min      2.409
_cell_volume                     11300.7(10)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.1030
_diffrn_reflns_av_unetI/netI     0.0694
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       70
_diffrn_reflns_limit_l_min       -70
_diffrn_reflns_number            205643
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.022
_diffrn_reflns_theta_min         2.057
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    17.452
_exptl_absorpt_correction_T_max  0.4296
_exptl_absorpt_correction_T_min  0.2782
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/2 (Bruker,2014/2) was used for absorption correction.
wR2(int) was 0.0964 before and 0.0608 after correction.
The Ratio of minimum to maximum transmission is 0.6476.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.592
_exptl_crystal_description       plate
_exptl_crystal_F_000             8064
_exptl_crystal_preparation       ', Luminescent'
_exptl_crystal_recrystallization_method 'from HBr'
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.907
_refine_diff_density_min         -1.615
_refine_diff_density_rms         0.194
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1053
_refine_ls_number_reflns         22216
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.1251
_refine_ls_R_factor_gt           0.0493
_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^)+(0.0257P)^2^+47.8012P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0757
_refine_ls_wR_factor_ref         0.0928
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12004
_reflns_number_total             22216
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7sc01590a2.cif
_cod_data_source_block           aj80_p21c_a
_cod_original_cell_volume        11300.6(10)
_cod_database_code               1545808
_shelxl_version_number           2014-3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All O(H) groups
2.a Secondary CH2 refined with riding coordinates:
 C33(H33A,H33B), C45(H45A,H45B), C34(H34A,H34B), C37(H37A,H37B), C6(H6D,H6E),
 C29(H29A,H29B), C1(H1D,H1E), C17(H17A,H17B), C26(H26A,H26B), C2(H2A,H2B),
 C41(H41A,H41B), C25(H25A,H25B), C46(H46A,H46B), C5(H5D,H5E), C31(H31A,H31),
 C18(H18A,H18B), C35(H35A,H35), C30(H30A,H30B), C3(H3A,H3B), C22(H22A,H22B),
 C27(H27A,H27B), C10(H10D,H10E), C47(H47A,H47B), C21(H21A,H21B), C7(H7D,H7E),
 C9(H9D,H9E), C11(H11D,H11E), C15(H15A,H15B), C19(H19A,H19B), C42(H42A,H42B),
 C39(H39A,H39B), C38(H38A,H38B), C43(H43A,H43B), C23(H23A,H23B), C14(H14A,H14B),
  C13(H13A,H13B)
2.b Tetrahedral OH refined with riding coordinates:
 O22(H22)
2.c Idealised Me refined as rotating group:
 N8(H8A,H8B,H8C), N7(H7A,H7B,H7C), N10(H10A,H10B,H10C), N9(H9A,H9B,H9C),
 N1(H1A,H1B,H1C), N5(H5A,H5B,H5C), N6(H6A,H6B,H6C), N11(H11A,H11B,H11C),
 N12(H12A,H12B,H12C), N4(H4A,H4B,H4C), N2(H2C,H2D,H2E), N3(H3C,H3D,H3E)
2.d Idealised tetrahedral OH refined as rotating group:
 O12(H12), O10(H10), O5(H5), O16(H16), O17(H17), O24(H24), O3(H3), O19(H19),
 O7(H7), O13(H13), O2(H2)
;
_shelx_res_checksum              79486
_olex2_submission_original_sample_id AJ80
_olex2_submission_special_instructions 'No special instructions were received'