A low-dimensional ferrocenium lead-iodide perovskite ferroelastic with a narrow band gap.
Xu, Zhe-Kun; Wang, Zhong-Xia; Chemical communications (Cambridge, England) 61 (2025) 15810–15813; doi:10.1039/d5cc03384e

data_1575388
_publ_section_title
;
 A low-dimensional ferrocenium lead-iodide perovskite ferroelastic with a
 narrow band gap.
;
_journal_issue                   81
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              15810
_journal_page_last               15813
_journal_paper_doi               10.1039/d5cc03384e
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety         'I3 Pb, C12 H11 N2 O'
_chemical_formula_sum            'C12 H11 I3 N2 O Pb'
_chemical_formula_weight         787.12
_chemical_name_systematic        '[SAPD]PbI3'
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'I -2ya'
_space_group_name_H-M_alt        'I 1 a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc28v6w7
_audit_creation_date             2021-07-06
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2021-09-18 deposited with the CCDC.	2025-08-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.552(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.8102(2)
_cell_length_b                   14.2865(4)
_cell_length_c                   16.1155(4)
_cell_measurement_reflns_used    4869
_cell_measurement_temperature    172.91(16)
_cell_measurement_theta_max      31.1890
_cell_measurement_theta_min      2.7120
_cell_volume                     1767.77(8)
_computing_cell_refinement       'CrysAlisPro 1.171.41.108a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.108a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.108a (Rigaku OD, 2021)'
_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_environment      N~2~
_diffrn_ambient_temperature      172.91(16)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.792
_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    -57.00   9.00   0.50    1.00    --    5.05 -57.00 120.00  132
  2  \w    -12.00  73.00   0.50    1.00    --    5.05   0.00  90.00  170
  3  \w    -12.00  20.00   0.50    1.00    --   -5.21 -99.00-150.00   64
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0199794000
_diffrn_orient_matrix_UB_12      0.0282451000
_diffrn_orient_matrix_UB_13      -0.0331465000
_diffrn_orient_matrix_UB_21      -0.0031404000
_diffrn_orient_matrix_UB_22      -0.0401004000
_diffrn_orient_matrix_UB_23      -0.0261758000
_diffrn_orient_matrix_UB_31      -0.0901556000
_diffrn_orient_matrix_UB_32      0.0076678000
_diffrn_orient_matrix_UB_33      -0.0148338000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0265
_diffrn_reflns_av_unetI/netI     0.0273
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.792
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            5477
_diffrn_reflns_point_group_measured_fraction_full 0.906
_diffrn_reflns_point_group_measured_fraction_max 0.667
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.623
_diffrn_reflns_theta_min         1.919
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    14.777
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.13788
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.108a (Rigaku Oxford Diffraction, 2021)
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    2.957
_exptl_crystal_description       block
_exptl_crystal_F_000             1384
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.135
_refine_diff_density_min         -2.641
_refine_diff_density_rms         0.278
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.058(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     138
_refine_ls_number_reflns         3640
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0335
_refine_ls_R_factor_gt           0.0323
_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^)+(0.0601P)^2^+0.4110P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0861
_refine_ls_wR_factor_ref         0.0868
_reflns_Friedel_coverage         0.681
_reflns_Friedel_fraction_full    0.811
_reflns_Friedel_fraction_max     0.542
_reflns_number_gt                3460
_reflns_number_total             3640
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc03384e3.cif
_cod_data_source_block           hcr_210526_3_173k_auto
_cod_depositor_comments
'Adding full bibliography for 1575387--1575389.cif.'
_cod_original_sg_symbol_H-M      Ia
_cod_database_code               1575388
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N O I Pb'
_shelx_estimated_absorpt_t_max   0.757
_shelx_estimated_absorpt_t_min   0.589
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.942(10)
 0.058(10)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(C00F) = Uanis(C1) = Uanis(C4) = Uanis(C3)
Uanis(C3) = Uanis(C4)
Uanis(C5) = Uanis(C006) = Uanis(C00A)
Uanis(N005) = Uanis(N00C)
4.a Aromatic/amide H refined with riding coordinates:
 C006(H006), C007(H007), C008(H008), C00A(H00A), C00B(H00B), C00F(H00F),
 C2(H2), C4(H4), C3(H3), C5(H5)
4.b Idealised tetrahedral OH refined as rotating group:
 O009(H009)
;
_shelx_res_checksum              44147
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 3.457
_oxdiff_exptl_absorpt_empirical_full_min 0.601