Reliably obtaining white light from layered halide perovskites at room temperature
Crace, Ethan; Su, Alexander; Karunadasa, Hemamala I.; Chemical Science  (2022) –; doi:10.1039/D2SC02381D

data_1567407
_publ_section_title
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 Reliably obtaining white light from layered halide perovskites at room
 temperature
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_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D2SC02381D
_journal_year                    2022
_chemical_formula_moiety         'Br4 Pb, C9 H13 N3'
_chemical_formula_sum            'C9 H13 Br4 N3 Pb'
_chemical_formula_weight         690.05
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-03-31
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
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2022-04-27 deposited with the CCDC.	2022-08-01 downloaded from the CCDC.
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_cell_angle_alpha                90
_cell_angle_beta                 94.0590(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.0291(2)
_cell_length_b                   31.1120(7)
_cell_length_c                   8.7353(2)
_cell_measurement_reflns_used    9623
_cell_measurement_temperature    300
_cell_measurement_theta_max      27.58
_cell_measurement_theta_min      2.62
_cell_volume                     3260.98(12)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      300.15
_diffrn_detector_area_resol_mean 7.3910
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'D8 Venture'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0588
_diffrn_reflns_av_unetI/netI     0.0270
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            38217
_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         26.372
_diffrn_reflns_theta_min         1.819
_exptl_absorpt_coefficient_mu    20.134
_exptl_absorpt_correction_T_max  0.4306
_exptl_absorpt_correction_T_min  0.2524
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. 
  wR2(int) was 0.1344 before and 0.0717 after correction. 
  The Ratio of minimum to maximum transmission is 0.5862. 
  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    2.811
_exptl_crystal_description       plate
_exptl_crystal_F_000             2480
_exptl_crystal_preparation
;
 'Crystals were prepared by dissolving the precursors in concentrated HBr
  at 100C and cooling the solution to room temperature at 2C/hr.'
;
_exptl_crystal_recrystallization_method
"'Large colorless rectangular plates appear after cooling.   Small needles also appear after a few days.   These needles are not always observed and are a non-perovskite phase.'"
_exptl_crystal_size_max          0.165
_exptl_crystal_size_mid          0.065
_exptl_crystal_size_min          0.015
_refine_diff_density_max         1.463
_refine_diff_density_min         -1.474
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     204
_refine_ls_number_reflns         3331
_refine_ls_number_restraints     218
_refine_ls_restrained_S_all      0.995
_refine_ls_R_factor_all          0.0380
_refine_ls_R_factor_gt           0.0296
_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^)+(0.0273P)^2^+26.6161P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0684
_refine_ls_wR_factor_ref         0.0730
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2823
_reflns_number_total             3331
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc02381d2.cif
_cod_data_source_block           sad_a
_cod_database_code               1567407
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
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1. Restrained distances
 C8-C9 \\sim C8-C10
 with sigma of 0.02
 C8-C10 \\sim C8-C11
 with sigma of 0.02
 C8-C11 \\sim C8-C9
 with sigma of 0.02
 N3-C9 \\sim N4-C10
 with sigma of 0.02
 N3-C9 \\sim N5-C11
 with sigma of 0.02
 N5-C11 \\sim N4-C10
 with sigma of 0.02
2. Rigid bond restraints
 N1, N2, C7, C3, C6, C2, C5, C4, C1, C8, N3, C9, N4, C10, N5, C11
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
N1 \\sim N2 \\sim C7 \\sim C3 \\sim C6 \\sim C2 \\sim C5 \\sim C4 \\sim C1
\\sim C8 \\sim N3 \\sim C9 \\sim N4 \\sim C10 \\sim N5 \\sim C11: within 2A
with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
4. Others
 Sof(Br2)=1-FVAR(1)
 Sof(Br3)=FVAR(1)
 Fixed Sof: H8AA(0.3333) H8AB(0.3333) H8BC(0.3333) H8BD(0.3333) H8CE(0.3333)
 H8CF(0.3333) N3(0.3333) H3A(0.3333) H3B(0.3333) H3C(0.3333) C9(0.3333)
 H9A(0.3333) H9B(0.3333) N4(0.3333) H4A(0.3333) H4B(0.3333) H4C(0.3333)
 C10(0.3333) H10A(0.3333) H10B(0.3333) N5(0.3333) H5A(0.3333) H5B(0.3333)
 H5C(0.3333) C11(0.3333) H11A(0.3333) H11B(0.3333)
5.a Secondary CH2 refined with riding coordinates:
 C8(H8AA,H8AB), C8(H8BC,H8BD), C8(H8CE,H8CF), C9(H9A,H9B), C10(H10A,H10B),
 C11(H11A,H11B)
5.b Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), C3(H3), C2(H2A), C5(H5), C4(H4)
5.c Idealised Me refined as rotating group:
 N3(H3A,H3B,H3C), N4(H4A,H4B,H4C), N5(H5A,H5B,H5C)
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_shelx_res_checksum              62133
_olex2_submission_special_instructions 'No special instructions were received'