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_1567406
_publ_section_title
;
 Reliably obtaining white light from layered halide perovskites at room
 temperature
;
_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             2022-04-27
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-04-27 deposited with the CCDC.	2022-08-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.1860(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.9594(5)
_cell_length_b                   30.9963(17)
_cell_length_c                   8.6387(5)
_cell_measurement_reflns_used    9994
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.26
_cell_measurement_theta_min      2.63
_cell_volume                     3193.8(3)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_detector                 'Bruker Photon II'
_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_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0544
_diffrn_reflns_av_unetI/netI     0.0257
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            42973
_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         27.485
_diffrn_reflns_theta_min         2.608
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    20.557
_exptl_absorpt_correction_T_max  0.4311
_exptl_absorpt_correction_T_min  0.2491
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. 
  wR2(int) was 0.1144 before and 0.0648 after correction. 
  The Ratio of minimum to maximum transmission is 0.5778. 
  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    2.870
_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         2.854
_refine_diff_density_min         -4.020
_refine_diff_density_rms         0.328
_refine_ls_extinction_coef       0.00010(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.247
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     191
_refine_ls_number_reflns         3677
_refine_ls_number_restraints     218
_refine_ls_restrained_S_all      1.213
_refine_ls_R_factor_all          0.0681
_refine_ls_R_factor_gt           0.0634
_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^)+312.8122P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1433
_refine_ls_wR_factor_ref         0.1454
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3389
_reflns_number_total             3677
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc02381d2.cif
_cod_data_source_block           sad1_a
_cod_database_code               1567406
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Restrained distances
 C9-C8 \\sim C10-C8
 with sigma of 0.02
 C10-C8 \\sim C11-C8
 with sigma of 0.02
 C9-C8 \\sim C11-C8
 with sigma of 0.02
 N3-C9 \\sim N5-C10
 with sigma of 0.02
 N4-C11 \\sim N3-C9
 with sigma of 0.02
 N5-C10 \\sim N4-C11
 with sigma of 0.02
 N5-C10 \\sim N3-C9
 with sigma of 0.02
2. Rigid bond restraints
 N2, N1, C2, C3, C6, C4, C7, C1, C8, C5, N5, C10, N3, C9, N4, 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
N2 \\sim N1 \\sim C2 \\sim C3 \\sim C6 \\sim C4 \\sim C7 \\sim C1 \\sim C8
\\sim C5 \\sim N5 \\sim C10 \\sim N3 \\sim C9 \\sim N4 \\sim C11: within 2A
with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(N4) = Uanis(N5) = Uanis(N3)
Uanis(C10) = Uanis(C9) = Uanis(C11)
4. Others
 Sof(Br3)=1-FVAR(1)
 Sof(Br2)=FVAR(1)
 Sof(Br6)=1-FVAR(2)
 Sof(Br5)=FVAR(2)
 Fixed Sof: H8AB(0.3333) H8AA(0.3333) H8BD(0.3333) H8BC(0.3333) H8CF(0.3333)
 H8CE(0.3333) N5(0.3333) H5B(0.3333) H5C(0.3333) H5A(0.3333) C10(0.3333)
 H10B(0.3333) H10A(0.3333) N3(0.3333) H3B(0.3333) H3C(0.3333) H3A(0.3333)
 C9(0.3333) H9A(0.3333) H9B(0.3333) N4(0.3333) H4C(0.3333) H4A(0.3333)
 H4B(0.3333) C11(0.3333) H11B(0.3333) H11A(0.3333)
5.a Secondary CH2 refined with riding coordinates:
 C8(H8AB,H8AA), C8(H8BD,H8BC), C8(H8CF,H8CE), C10(H10B,H10A), C9(H9A,H9B),
 C11(H11B,H11A)
5.b Aromatic/amide H refined with riding coordinates:
 N2(H2), N1(H1), C2(H2A), C3(H3), C4(H4), C5(H5)
5.c Idealised Me refined as rotating group:
 N5(H5B,H5C,H5A), N3(H3B,H3C,H3A), N4(H4C,H4A,H4B)
;
_shelx_res_checksum              75736
_olex2_exptl_crystal_mounting_method
;
 'Crystals were seperated from the mother liquor using paratone oil. 
  The crystal used for diffaction was placed on a kapton loop using 
  paratone to adhere it to the loop.'
;
_olex2_submission_special_instructions 'No special instructions were received'