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_1567410
_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         'Cl4 Pb, C9 H13 N3'
_chemical_formula_sum            'C9 H13 Cl4 N3 Pb'
_chemical_formula_weight         512.21
_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             2021-04-01
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2022-04-27 deposited with the CCDC.	2022-08-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.590(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.4666(6)
_cell_length_b                   30.4225(18)
_cell_length_c                   8.3667(4)
_cell_measurement_reflns_used    8241
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.16
_cell_measurement_theta_min      2.68
_cell_volume                     2912.9(3)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_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      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 1.000
_diffrn_measured_fraction_theta_max 0.998
_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  0.0730
_diffrn_reflns_av_unetI/netI     0.0336
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            26789
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.406
_diffrn_reflns_theta_min         1.901
_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    12.299
_exptl_absorpt_correction_T_max  0.4288
_exptl_absorpt_correction_T_min  0.3384
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. 
  wR2(int) was 0.0885 before and 0.0753 after correction. 
  The Ratio of minimum to maximum transmission is 0.7892. 
  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    2.336
_exptl_crystal_description       plate
_exptl_crystal_F_000             1904
_exptl_crystal_preparation       'See crystallisation.'
_exptl_crystal_recrystallization_method
"'Precursors were dissolved in 6M HCl and heated to 100C to dissolve.   Solution was then cooled to room temperature at 2C/hr.'"
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_refine_diff_density_max         2.142
_refine_diff_density_min         -3.600
_refine_diff_density_rms         0.224
_refine_ls_extinction_coef       0.00016(3)
_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   1.271
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     203
_refine_ls_number_reflns         2686
_refine_ls_number_restraints     152
_refine_ls_restrained_S_all      1.237
_refine_ls_R_factor_all          0.0569
_refine_ls_R_factor_gt           0.0487
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+107.2131P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0935
_refine_ls_wR_factor_ref         0.0967
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2395
_reflns_number_total             2686
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc02381d2.cif
_cod_data_source_block           sad_a_CCDC1
_cod_database_code               1567410
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Restrained distances
 N3-C9 \\sim N4-C11
 with sigma of 0.02
 C9-C8 \\sim C11-C8
 with sigma of 0.02
 N5-C11 \\sim N4-C10 \\sim N3-C9
 with sigma of 0.02
 C9-C8 \\sim C10-C8 \\sim C11-C8
 with sigma of 0.02
2. Rigid bond restraints
 C9, N1, C7, C1, N2, C8, C2, C6, C11, C3, C5, N4, N3, C4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C11 \\sim N1 \\sim C7 \\sim C1 \\sim N2 \\sim C8 \\sim C2 \\sim C6 \\sim C9
\\sim C3 \\sim C5 \\sim N4 \\sim N3 \\sim C4: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
Uanis(C10) = Uanis(C11) = Uanis(C9)
4. Others
 Sof(Cl2)=1-FVAR(1)
 Sof(Cl3)=FVAR(1)
 Sof(Cl6)=1-FVAR(2)
 Sof(Cl5)=FVAR(2)
 Fixed Sof: H8CE(0.3333) H8CF(0.3333) H8AA(0.3333) H8AB(0.3333) H8BC(0.3333)
 H8BD(0.3333) C11(0.3333) H11A(0.3333) H11B(0.3333) N4(0.3333) H4A(0.3333)
 H4B(0.3333) H4C(0.3333) N3(0.3333) H3A(0.3333) H3B(0.3333) H3C(0.3333)
 C9(0.3333) H9A(0.3333) H9B(0.3333) N5(0.3333) H5A(0.3333) H5B(0.3333)
 H5C(0.3333) C10(0.3333) H10A(0.3333) H10B(0.3333)
5.a Secondary CH2 refined with riding coordinates:
 C8(H8CE,H8CF), C8(H8AA,H8AB), C8(H8BC,H8BD), C11(H11A,H11B), C9(H9A,H9B),
 C10(H10A,H10B)
5.b Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), C2(H2A), C3(H3), C5(H5), C4(H4)
5.c Idealised Me refined as rotating group:
 N4(H4A,H4B,H4C), N3(H3A,H3B,H3C), N5(H5A,H5B,H5C)
;
_shelx_res_checksum              36369
_olex2_exptl_crystal_mounting_method
'Crystals were isolated in paratone and placed on a kapton loop. '
_olex2_submission_special_instructions 'No special instructions were received'