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_1575387
_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.cc28v6v6
_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                 100.385(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.8475(3)
_cell_length_b                   14.3845(6)
_cell_length_c                   16.1929(6)
_cell_measurement_reflns_used    4090
_cell_measurement_temperature    297.98(10)
_cell_measurement_theta_max      30.8730
_cell_measurement_theta_min      1.9370
_cell_volume                     1797.95(12)
_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      air
_diffrn_ambient_temperature      297.98(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.796
_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    -68.00  18.00   0.50    1.00    --    5.05 -19.00  60.00  172
  2  \w    -14.00  27.00   0.50    1.00    --   -5.21 -99.00 150.00   82
  3  \w    -68.00  -3.00   0.50    1.00    --    5.05 -37.00-180.00  130
;
_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      0.0185202000
_diffrn_orient_matrix_UB_12      0.0283827000
_diffrn_orient_matrix_UB_13      -0.0331312000
_diffrn_orient_matrix_UB_21      -0.0044610000
_diffrn_orient_matrix_UB_22      -0.0395594000
_diffrn_orient_matrix_UB_23      -0.0264239000
_diffrn_orient_matrix_UB_31      -0.0898512000
_diffrn_orient_matrix_UB_32      0.0078156000
_diffrn_orient_matrix_UB_33      -0.0137482000
_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  0.0270
_diffrn_reflns_av_unetI/netI     0.0407
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.796
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            6055
_diffrn_reflns_point_group_measured_fraction_full 0.897
_diffrn_reflns_point_group_measured_fraction_max 0.653
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.830
_diffrn_reflns_theta_min         1.908
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    14.529
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.25550
_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    2.908
_exptl_crystal_description       block
_exptl_crystal_F_000             1384
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.614
_refine_diff_density_min         -1.699
_refine_diff_density_rms         0.271
_refine_ls_abs_structure_details
;
 Flack x determined using 1144 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.022(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     173
_refine_ls_number_reflns         3690
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0293
_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^)+(0.0346P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0729
_refine_ls_wR_factor_ref         0.0746
_reflns_Friedel_coverage         0.639
_reflns_Friedel_fraction_full    0.795
_reflns_Friedel_fraction_max     0.510
_reflns_number_gt                3127
_reflns_number_total             3690
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc03384e3.cif
_cod_data_source_block           hcr_210526_3_auto
_cod_depositor_comments
'Adding full bibliography for 1575387--1575389.cif.'
_cod_original_sg_symbol_H-M      Ia
_cod_database_code               1575387
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N O I Pb'
_shelx_estimated_absorpt_t_max   0.868
_shelx_estimated_absorpt_t_min   0.670
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C007(H007), C008(H008), C009(H009), C00A(H00A), C00D(H00D), C00E(H00E),
 C00F(H00F), C00G(H00G), C3(H3), C5(H5)
2.b Idealised tetrahedral OH refined as rotating group:
 O005(H005)
;
_shelx_res_checksum              45868
_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 2.448
_oxdiff_exptl_absorpt_empirical_full_min 0.640