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_7135190
_publ_section_title
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 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 Pb1, C4.998 Fe1, 0.714(C7)'
_chemical_formula_sum            'C9.99 Fe I3 Pb'
_chemical_formula_weight         763.78
_space_group_crystal_system      hexagonal
_space_group_IT_number           194
_space_group_name_Hall           '-P 6c 2c'
_space_group_name_H-M_alt        'P 63/m m c'
_atom_sites_solution_primary     dual
_audit_creation_date             2023-09-06
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2025-10-15 deposited with the CCDC.	2025-10-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   10.9271(6)
_cell_length_b                   10.9271(6)
_cell_length_c                   8.1291(3)
_cell_measurement_reflns_used    1855
_cell_measurement_temperature    372.98(16)
_cell_measurement_theta_max      27.4990
_cell_measurement_theta_min      3.2910
_cell_volume                     840.59(7)
_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 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      372.98(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 0.888
_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      1.00  28.00   0.50    2.00    --   -5.21 -99.00 -30.00   54
  2  \w    -17.00  24.00   0.50    2.00    --   -5.21 -99.00 -60.00   82
  3  \w    -33.00  41.00   0.50    2.00    --   -5.21  88.00-156.00  148
;
_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      0.0620594000
_diffrn_orient_matrix_UB_12      0.0062653000
_diffrn_orient_matrix_UB_13      -0.0358254000
_diffrn_orient_matrix_UB_21      0.0360381000
_diffrn_orient_matrix_UB_22      0.0738157000
_diffrn_orient_matrix_UB_23      0.0151493000
_diffrn_orient_matrix_UB_31      0.0214704000
_diffrn_orient_matrix_UB_32      -0.0114489000
_diffrn_orient_matrix_UB_33      0.0781077000
_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  0.0480
_diffrn_reflns_av_unetI/netI     0.0191
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.888
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            3929
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.888
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.686
_diffrn_reflns_theta_min         2.152
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    16.345
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.06594
_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            'dull dark green'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    3.018
_exptl_crystal_description       prism
_exptl_crystal_F_000             654
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.211
_refine_diff_density_min         -0.507
_refine_diff_density_rms         0.198
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     57
_refine_ls_number_reflns         474
_refine_ls_number_restraints     338
_refine_ls_restrained_S_all      0.790
_refine_ls_R_factor_all          0.0694
_refine_ls_R_factor_gt           0.0529
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0962P)^2^+1.4548P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1416
_refine_ls_wR_factor_ref         0.1525
_reflns_Friedel_coverage         0.000
_reflns_number_gt                352
_reflns_number_total             474
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc03384e3.cif
_cod_data_source_block           Fc_PbI3_373K
_cod_original_cell_volume        840.59(10)
_cod_database_code               7135190
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C H Fe I Pb'
_chemical_oxdiff_usercomment     \
_shelx_estimated_absorpt_t_max   0.292
_shelx_estimated_absorpt_t_min   0.292
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Restrained distances
 Fe1-C1 = Fe1-C8
 1.98 with sigma of 0.02
 C1-C2 = C1-C3 = C1-C4 = C1-C5 = C1-C6 = C1-C7
 1.9 with sigma of 0.02
 C2-C9 = C3-C10 = C4-C11 = C5-C12 = C6-C13 = C7-C14
 2.13 with sigma of 0.02
 Fe1-C2 = Fe1-C3 = Fe1-C4 = Fe1-C5 = Fe1-C6 = Fe1-C7 = Fe1-C9 = Fe1-C10 = Fe1-
 C11 = Fe1-C12 = Fe1-C13 = Fe1-C14
 1.95 with sigma of 0.02
 C8-C9 = C8-C10 = C8-C11 = C8-C12 = C8-C13 = C8-C14
 2 with sigma of 0.03
 C2-C3 = C3-C4 = C4-C5 = C5-C6 = C6-C7 = C7-C2
 1.6 with sigma of 0.15
 C9-C10 = C10-C11 = C11-C12 = C12-C13 = C13-C14 = C14-C9
 1.6 with sigma of 0.15
2. Uiso/Uaniso restraints and constraints
Uanis(C8) = Uanis(C10) = Uanis(C11) = Uanis(C9) = Uanis(C12) = Uanis(C14) =
Uanis(C13) = Uanis(C1) = Uanis(C4) = Uanis(C3) = Uanis(C5) = Uanis(C6) =
Uanis(C7) = Uanis(C2)
3. Rigid body (RIGU) restrains
 Fe1, C1, C6, C3, C4, C2, C5, C7, C10, C9, C14, C11, C13, C12, C8
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Others
 Fixed Sof: C1(0.0595) C6(0.0595) C3(0.0595) C4(0.0595) C2(0.0595) C5(0.0595)
 C7(0.0595) C10(0.0595) C9(0.0595) C14(0.0595) C11(0.0595) C13(0.0595)
 C12(0.0595) C8(0.0595)
;
_shelx_res_checksum              3088
_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 5.850
_oxdiff_exptl_absorpt_empirical_full_min 0.433