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_1567409
_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, C5 H11 N3'
_chemical_formula_sum            'C5 H11 Cl4 N3 Pb'
_chemical_formula_weight         462.16
_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'
_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
;
2022-04-27 deposited with the CCDC.	2022-08-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.608(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.7314(4)
_cell_length_b                   11.3143(4)
_cell_length_c                   11.5207(5)
_cell_measurement_reflns_used    6251
_cell_measurement_temperature    300
_cell_measurement_theta_max      28.24
_cell_measurement_theta_min      2.83
_cell_volume                     1215.56(9)
_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  (Sheldrick, 2015)'
_diffrn_ambient_temperature      300.15
_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 0.998
_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_unetI/netI     0.0300
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4837
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.319
_diffrn_reflns_theta_min         2.578
_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    14.721
_exptl_absorpt_correction_T_max  0.431128
_exptl_absorpt_correction_T_min  0.228460
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.

Final HKLF 4 output contains 46179 reflections, Rint = 0.0634
 (25055 with I > 3sig(I), Rint = 0.0504)
;
_exptl_crystal_colour            'clear light brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    2.525
_exptl_crystal_description       plate
_exptl_crystal_F_000             848
_exptl_crystal_preparation
;
 'Crystals were prepared by dissolving precursors in 6M HCl 
  at 100C and cooling the solution to room temperature 
  at a rate of 2C/hr.'
;
_exptl_crystal_recrystallization_method
"'Large crystals are light brown plates. Smaller crystals   or fragments of larger crystals appear colorless under   the microscope.'"
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.993
_refine_diff_density_min         -1.928
_refine_diff_density_rms         0.276
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.163
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     120
_refine_ls_number_reflns         4837
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.163
_refine_ls_R_factor_all          0.0479
_refine_ls_R_factor_gt           0.0380
_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^)+(0.0601P)^2^+9.5365P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1186
_refine_ls_wR_factor_ref         0.1267
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4225
_reflns_number_total             4837
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc02381d2.cif
_cod_data_source_block           twin4_a_CCDC1
_cod_database_code               1567409
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.7776
 0.2224
2.a Secondary CH2 refined with riding coordinates:
 C00A(H00D,H00E), C00C(H00G,H00H)
2.b Aromatic/amide H refined with riding coordinates:
 N007(H007), N008(H008), C00B(H00F), C00D(H00I)
2.c Idealised Me refined as rotating group:
 N006(H00A,H00B,H00C)
;
_shelx_res_checksum              79229
_olex2_exptl_crystal_mounting_method
;
 'Crystals were seperated from the mother liquor in paratone oil and placed
  on a kapton loop using the paratone to adhere the crystal to the loop.'
;
_olex2_submission_special_instructions 'No special instructions were received'