Three-Dimensional Perovskite Methylhydrazinium Lead Chloride with Two Polar Phases and Unusual Second-Harmonic Generation Bistability above Room Temperature
Ma̧czka, Mirosław; Gagor, Anna; Zarȩba, Jan K.; Stefanska, Dagmara; Drozd, Marek; Balciunas, Sergejus; Šimėnas, Mantas; Banys, Juras; Sieradzki, Adam; Chemistry of Materials  (2020) –; doi:10.1021/acs.chemmater.0c00973

data_4003536
_publ_section_title
;
 Three-Dimensional Perovskite Methylhydrazinium Lead Chloride with Two
 Polar Phases and Unusual Second-Harmonic Generation Bistability above
 Room Temperature
;
_journal_name_full               'Chemistry of Materials'
_journal_paper_doi               10.1021/acs.chemmater.0c00973
_journal_year                    2020
_chemical_formula_sum            'C H7 Cl3 N2 Pb'
_chemical_formula_weight         360.63
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 92.332(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.72660(10)
_cell_length_b                   11.3396(2)
_cell_length_c                   11.3926(2)
_cell_measurement_reflns_used    13945
_cell_measurement_temperature    300(1)
_cell_measurement_theta_max      32.2630
_cell_measurement_theta_min      3.4130
_cell_volume                     739.19(2)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      300(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6249
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.939
_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  0.0485
_diffrn_reflns_av_unetI/netI     0.0403
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.939
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            16004
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.910
_diffrn_reflns_theta_full        28.000
_diffrn_reflns_theta_max         29.272
_diffrn_reflns_theta_min         2.535
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    23.804
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.15262
_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_density_diffrn    3.240
_exptl_crystal_description       plate
_exptl_crystal_F_000             640
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.143
_refine_diff_density_min         -1.609
_refine_diff_density_rms         0.235
_refine_ls_abs_structure_details
;
 Flack x determined using 1579 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.032(5)
_refine_ls_extinction_coef       0.0117(4)
_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   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     132
_refine_ls_number_reflns         3671
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0283
_refine_ls_R_factor_gt           0.0272
_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^)+(0.0318P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0606
_refine_ls_wR_factor_ref         0.0615
_reflns_Friedel_coverage         0.850
_reflns_Friedel_fraction_full    0.967
_reflns_Friedel_fraction_max     0.878
_reflns_number_gt                3581
_reflns_number_total             3671
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm0c00973_si_002.cif
_cod_data_source_block           PhaseII
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4003536
_shelx_shelxl_version_number     2018/3
_oxdiff_exptl_absorpt_empirical_full_min 0.441
_oxdiff_exptl_absorpt_empirical_full_max 3.316
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              28953
_shelx_hkl_checksum              52694