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_7712526
_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, 0.5(C6 H14 N4 S2)'
_chemical_formula_sum            'C3 H7 I3 N2 Pb S'
_chemical_formula_weight         691.099
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2n 2a'
_space_group_name_H-M_alt        'P m c n'
_symmetry_Int_Tables_number      62
_audit_creation_date             2023-02-10
_audit_creation_method
;
Olex2 1.5-dev
(compiled 2023.02.06 svn.rdd5efbe3 for OlexSys, GUI svn.r6444)
;
_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            4
_cell_length_a                   8.7522(15)
_cell_length_b                   17.620(2)
_cell_length_c                   8.2301(11)
_cell_measurement_reflns_used    2327
_cell_measurement_temperature    377(2)
_cell_measurement_theta_max      21.91
_cell_measurement_theta_min      2.60
_cell_volume                     1269.2(3)
_computing_data_collection       'CrysAlisPro 1.171.42.63a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5-dev (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      377.15
_diffrn_measured_fraction_theta_full 0.9983
_diffrn_measured_fraction_theta_max 0.9983
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1858
_diffrn_reflns_av_unetI/netI     0.0936
_diffrn_reflns_Laue_measured_fraction_full 0.9983
_diffrn_reflns_Laue_measured_fraction_max 0.9983
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            21198
_diffrn_reflns_point_group_measured_fraction_full 0.9983
_diffrn_reflns_point_group_measured_fraction_max 0.9983
_diffrn_reflns_theta_full        24.9888
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.60
_exptl_absorpt_coefficient_mu    20.709
_exptl_absorpt_correction_T_max  0.902
_exptl_absorpt_correction_T_min  0.820
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    3.617
_exptl_crystal_description       block
_exptl_crystal_F_000             1169.805
_exptl_crystal_size_max          0.01
_exptl_crystal_size_mid          0.008
_exptl_crystal_size_min          0.005
_refine_diff_density_max         1.7798
_refine_diff_density_min         -2.4596
_refine_diff_density_rms         0.3488
_refine_ls_d_res_high            0.8412
_refine_ls_d_res_low             7.8385
_refine_ls_extinction_coef       0.0026
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_goodness_of_fit_ref   1.0120
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    11
_refine_ls_number_parameters     59
_refine_ls_number_reflns         1193
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.0010
_refine_ls_R_factor_all          0.0803
_refine_ls_R_factor_gt           0.0558
_refine_ls_shift/su_max          -0.0007
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1083P)^2^+1.1440P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1548
_refine_ls_wR_factor_ref         0.1844
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              10
_reflns_limit_h_min              0
_reflns_limit_k_max              20
_reflns_limit_k_min              0
_reflns_limit_l_max              9
_reflns_limit_l_min              0
_reflns_number_gt                786
_reflns_number_total             1193
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d2dt03526j2.cif
_cod_data_source_block           2-14-377k-split
_cod_depositor_comments
'Adding full bibliography for 7712524--7712526.cif.'
_cod_original_sg_symbol_Hall     '-P 2ac 2n (y,z,x)'
_cod_database_code               7712526
_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 planarity
 S1, C1, N2, N1
 with sigma of 0.001
3. Uiso/Uaniso restraints and constraints
Uanis(N1) \\sim Ueq: with sigma of 0.06 and sigma for terminal atoms of 0.01
4. Rigid body (RIGU) restrains
 S1, C1, N2, N1
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Fixed Sof: H3a(0.5) H3b(0.5) H2a(0.5) H2b(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C3(H3a,H3b), C2(H2a,H2b)
6.b Aromatic/amide H refined with riding coordinates:
 N2(H2)
6.c X=CH2 refined with riding coordinates:
 N1(H1a,H1b)
;
_olex2_submission_special_instructions 'No special instructions were received'