Effect of Pd(II) uptake on high-temperature phase transitions in a hybrid organic-inorganic perovskite semiconductor.
Xu, Yan; Xu, Ke; He, Lei; Mu, Jie; Yin, Ti-Jian; Men, Jin-Tao; Ye, Qiong; Dalton transactions (Cambridge, England : 2003) 52 (2023) 3815–3820; doi:10.1039/d2dt03526j

data_7712524
_publ_section_title
;
 Effect of Pd(II) uptake on high-temperature phase transitions in a hybrid
 organic-inorganic perovskite semiconductor.
;
_journal_issue                   12
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3815
_journal_page_last               3820
_journal_paper_doi               10.1039/d2dt03526j
_journal_volume                  52
_journal_year                    2023
_chemical_formula_moiety         'I3 Pb, C3 H7 N2 S'
_chemical_formula_sum            'C3 H7 I3 N2 Pb S'
_chemical_formula_weight         691.06
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2023-02-14
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2023-02-16 deposited with the CCDC.	2023-02-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.0602(7)
_cell_length_b                   8.3101(3)
_cell_length_c                   19.5118(8)
_cell_measurement_reflns_used    6390
_cell_measurement_temperature    299.99(10)
_cell_measurement_theta_max      31.0530
_cell_measurement_theta_min      2.1200
_cell_volume                     2441.94(18)
_computing_cell_refinement       'CrysAlisPro 1.171.42.63a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.63a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.63a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      300.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.832
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -36.00 -11.00   0.50    0.64    --   -5.49  97.00 -56.00   50
  2  \w     13.00  68.00   0.50    0.64    --    4.71  38.00 -90.00  110
  3  \w     40.00  79.00   0.50    0.64    --    4.71  26.00 152.00   78
  4  \w    -15.00  37.00   0.50    0.64    --    4.71 -99.00 150.00  104
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1328
_diffrn_reflns_av_unetI/netI     0.0825
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.832
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            13545
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.832
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.716
_diffrn_reflns_theta_min         2.087
_exptl_absorpt_coefficient_mu    21.524
_exptl_absorpt_correction_T_max  0.898
_exptl_absorpt_correction_T_min  0.813
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.63a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    3.759
_exptl_crystal_description       block
_exptl_crystal_F_000             2368
_exptl_crystal_size_max          0.01
_exptl_crystal_size_mid          0.008
_exptl_crystal_size_min          0.005
_refine_diff_density_max         2.247
_refine_diff_density_min         -3.619
_refine_diff_density_rms         0.532
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.977
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     91
_refine_ls_number_reflns         3156
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      0.979
_refine_ls_R_factor_all          0.0828
_refine_ls_R_factor_gt           0.0664
_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^)+(0.1209P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1718
_refine_ls_wR_factor_ref         0.1830
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2336
_reflns_number_total             3156
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03526j2.cif
_cod_data_source_block           xy_2_14_300k_auto
_cod_depositor_comments
'Adding full bibliography for 7712524--7712526.cif.'
_cod_database_code               7712524
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H) groups, All N(H,H) groups
2. Restrained distances
 N1-C1
 1.375 with sigma of 0.02
3. Restrained planarity
 N2, C1, S1, N1
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(N1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C2(H2A,H2B)
5.b Aromatic/amide H refined with riding coordinates:
 N2(H2)
5.c X=CH2 refined with riding coordinates:
 N1(H1A,H1B)
;
_shelx_res_checksum              21895
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;