Layered Lead Iodide of [Methylhydrazinium]2PbI4 with a Reduced Band Gap: Thermochromic Luminescence and Switchable Dielectric Properties Triggered by Structural Phase Transitions
Mączka, Mirosław; Ptak, Maciej; Gągor, Anna; Stefańska, Dagmara; Sieradzki, Adam; Chemistry of Materials 31 (2019) 8563–; doi:10.1021/acs.chemmater.9b03775

data_4003007
_publ_section_title
;
 Layered Lead Iodide of [Methylhydrazinium]2PbI4 with a Reduced Band Gap:
 Thermochromic Luminescence and Switchable Dielectric Properties Triggered
 by Structural Phase Transitions
;
_journal_issue                   20
_journal_name_full               'Chemistry of Materials'
_journal_page_first              8563
_journal_paper_doi               10.1021/acs.chemmater.9b03775
_journal_volume                  31
_journal_year                    2019
_chemical_formula_sum            'C2 H14 I4 N4 Pb'
_chemical_formula_weight         808.96
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                89.996(4)
_cell_angle_beta                 90.032(5)
_cell_angle_gamma                90.004(5)
_cell_formula_units_Z            12
_cell_length_a                   18.4660(7)
_cell_length_b                   19.0768(11)
_cell_length_c                   12.6380(10)
_cell_measurement_reflns_used    4156
_cell_measurement_temperature    99.98(13)
_cell_measurement_theta_max      29.2960
_cell_measurement_theta_min      3.2540
_cell_volume                     4452.0(5)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.98(13)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6249
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.892
_diffrn_measured_fraction_theta_max 0.892
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0682
_diffrn_reflns_av_unetI/netI     0.1081
_diffrn_reflns_Laue_measured_fraction_full 0.892
_diffrn_reflns_Laue_measured_fraction_max 0.892
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            27845
_diffrn_reflns_point_group_measured_fraction_full 0.892
_diffrn_reflns_point_group_measured_fraction_max 0.892
_diffrn_reflns_theta_full        25.681
_diffrn_reflns_theta_max         25.681
_diffrn_reflns_theta_min         2.403
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    19.498
_exptl_absorpt_correction_T_max  0.75186
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_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    3.621
_exptl_crystal_description       plate
_exptl_crystal_F_000             4176
_exptl_crystal_size_max          0.293
_exptl_crystal_size_mid          0.129
_exptl_crystal_size_min          0.052
_refine_diff_density_max         3.311
_refine_diff_density_min         -3.975
_refine_diff_density_rms         0.589
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.983
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     439
_refine_ls_number_reflns         15114
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.983
_refine_ls_R_factor_all          0.1249
_refine_ls_R_factor_gt           0.0679
_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^)+(0.0775P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1649
_refine_ls_wR_factor_ref         0.2072
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8403
_reflns_number_total             15114
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm9b03775_si_004.cif
_cod_data_source_block           Phase_IV
_cod_original_cell_volume        4452.0(4)
_cod_database_code               4003007
_shelx_shelxl_version_number     2018/3
_oxdiff_exptl_absorpt_empirical_full_min 0.539
_oxdiff_exptl_absorpt_empirical_full_max 7.357
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              90361
_shelx_hkl_checksum              27135