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_7712525
_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         'C6 H14 I6 N4 Pb2 S2'
_chemical_formula_sum            'C6 H14 I6 N4 Pb2 S2'
_chemical_formula_weight         1382.13
_space_group_crystal_system      orthorhombic
_space_group_IT_number           63
_space_group_name_Hall           '-C 2c 2'
_space_group_name_H-M_alt        'C m c m'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2023-02-14
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_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            2
_cell_length_a                   8.9920(14)
_cell_length_b                   17.951(4)
_cell_length_c                   8.1262(11)
_cell_measurement_reflns_used    812
_cell_measurement_temperature    416.15
_cell_measurement_theta_max      30.0870
_cell_measurement_theta_min      2.5110
_cell_volume                     1311.7(4)
_computing_data_collection       'CrysAlisPro 1.171.42.63a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      416.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0902
_diffrn_reflns_av_unetI/netI     0.0564
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            2586
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        23.474
_diffrn_reflns_theta_max         23.474
_diffrn_reflns_theta_min         2.269
_exptl_absorpt_coefficient_mu    20.035
_exptl_absorpt_correction_T_max  0.905
_exptl_absorpt_correction_T_min  0.825
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    3.499
_exptl_crystal_description       block
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.01
_exptl_crystal_size_mid          0.008
_exptl_crystal_size_min          0.005
_refine_diff_density_max         1.269
_refine_diff_density_min         -1.255
_refine_diff_density_rms         0.309
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     54
_refine_ls_number_reflns         567
_refine_ls_number_restraints     99
_refine_ls_restrained_S_all      1.595
_refine_ls_R_factor_all          0.1056
_refine_ls_R_factor_gt           0.0872
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2707
_refine_ls_wR_factor_ref         0.2945
_reflns_Friedel_coverage         0.000
_reflns_number_gt                374
_reflns_number_total             567
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03526j2.cif
_cod_data_source_block           xy_2_14_416k_auto_pl
_cod_depositor_comments
'Adding full bibliography for 7712524--7712526.cif.'
_cod_database_code               7712525
_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
 S1-C1
 1.55 with sigma of 0.01
 N1-C1
 1.3 with sigma of 0.01
 S1-C3 = C3-C2 = C2-N2 = N2-C1 = C1-S1
 1.39 with sigma of 0.01
 S1-C3 = S1-C1
 1.58 with sigma of 0.001
 S1-S1_$1
 2.5 with sigma of 0.02
 N1-S1
 2.55 with sigma of 0.02
 S1-C2 \\sim C3-N2 \\sim C2-C1 \\sim N2-S1 \\sim C1-C3
 with sigma of 0.02
3. Restrained planarity
 C1, S1, C3, N2, N1, C2
 with sigma of 0.001
 S1, C3, C2, N2, C1
 with sigma of 0.1
 S1, C1, C3, C2, N2, N1
 with sigma of 0.001
4. Uiso/Uaniso restraints and constraints
Uanis(N2) \\sim Ueq, Uanis(S1) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C3) \\sim
Ueq, Uanis(N1) \\sim Ueq, Uanis(C2) \\sim Ueq: with sigma of 0.005 and sigma
for terminal atoms of 0.01
5. Rigid body (RIGU) restrains
 N2, S1, C1, C3, N1, C2
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
6. Others
 Fixed Sof: S1(0.25) N2(0.25) H2(0.25) C1(0.25) N1(0.25) H1A(0.25) H1B(0.25)
 C3(0.25) H3A(0.25) H3B(0.25) C2(0.25) H2A(0.25) H2B(0.25)
 Fixed U11: C1(0.68776) N1(0.68935)
 Fixed U12: C1(0.00001) N1(-0.00005)
 Fixed U13: C1(-0.00001) N1(0.00005)
 Fixed U22: C1(0.68749) N1(0.6872)
 Fixed U23: C1(-0.00003) N1(0.00015)
 Fixed U33: C1(0.68752) N1(0.68877)
 Fixed X: S1(0.49632)
 Fixed Y: S1(0.304509)
 Fixed Z: S1(0.09656)
7.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C2(H2A,H2B)
7.b Aromatic/amide H refined with riding coordinates:
 N2(H2)
7.c X=CH2 refined with riding coordinates:
 N1(H1A,H1B)
;
_shelx_res_checksum              93409
_olex2_submission_special_instructions 'No special instructions were received'