#------------------------------------------------------------------------------
#$Date: 2025-07-06 16:12:52 +0200 (Sun 06 de Jul de 2025) $
#$Revision: 300596 $
#$URL: svn://www.crystallography.net/cod/cif/1/57/42/1574282.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1574282
loop_
_publ_author_name
'Yin, Jinlin'
'He, Yani'
'Sun, Chen'
'Jiang, Yilin'
'Fei, Honghan'
_publ_section_title
;
 Coordination-driven assembly of a ferrocene-functionalized lead iodide
 framework with enhanced stability and charge transfer for photocatalytic
 CO2-to-CH3OH conversion
;
_journal_issue                   19
_journal_name_full               'Chemical Science'
_journal_page_first              8327
_journal_page_last               8337
_journal_paper_doi               10.1039/D4SC08216H
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety         '0.5(C24 H16 Fe2 I4 O10 Pb6)'
_chemical_formula_sum            'C12 H8 Fe I2 O5 Pb3'
_chemical_formula_weight         1163.40
_space_group_crystal_system      orthorhombic
_space_group_IT_number           64
_space_group_name_Hall           '-C 2ac 2'
_space_group_name_H-M_alt        'C m c e'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-11-04
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2022-11-11 deposited with the CCDC.	2025-03-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.3688(7)
_cell_length_b                   10.6562(7)
_cell_length_c                   21.9752(8)
_cell_measurement_reflns_used    9902
_cell_measurement_temperature    297.0
_cell_measurement_theta_max      21.22
_cell_measurement_theta_min      2.88
_cell_volume                     4301.5(4)
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      297.0
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1154
_diffrn_reflns_av_unetI/netI     0.0369
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            26419
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        21.276
_diffrn_reflns_theta_max         21.276
_diffrn_reflns_theta_min         2.885
_exptl_absorpt_coefficient_mu    26.959
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear blackish black'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   blackish
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    3.593
_exptl_crystal_description       block
_exptl_crystal_F_000             3984
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.11
_refine_diff_density_max         2.916
_refine_diff_density_min         -2.990
_refine_diff_density_rms         0.614
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     124
_refine_ls_number_reflns         1226
_refine_ls_number_restraints     137
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.1418
_refine_ls_R_factor_gt           0.1395
_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/[σ²(Fo²)+5561.5684P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3051
_refine_ls_wR_factor_ref         0.3058
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1169
_reflns_number_total             1226
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4sc08216h2.cif
_cod_data_source_block           111_a
_cod_depositor_comments          'Adding full bibliography for 1574282.cif.'
_cod_original_sg_symbol_Hall     '-C 2bc 2'
_cod_database_code               1574282
_shelx_shelxl_version_number     2018/3
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.155
_shelx_estimated_absorpt_t_min   0.140
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C6-C1
 1.4 with sigma of 0.01
 C006-C009
 1.4 with sigma of 0.001
 Fe04-C18 \\sim Fe04-C18_$1 \\sim Fe04-C2_$1 \\sim Fe04-C1 \\sim Fe04-C2
 with sigma of 0.02
 Fe04-C00B \\sim Fe04-C7 \\sim Fe04-C7_$1 \\sim Fe04-C00B_$1 \\sim Fe04-C009
 with sigma of 0.02
 C00B-C009 \\sim C7-C00B
 with sigma of 0.02
 C2-C1 \\sim C2-C18
 with sigma of 0.02
 Pb02-I1A \\sim Pb02-I1B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C6 \\sim O2 \\sim O2: within 2A with sigma of 0.01 and sigma for terminal atoms
of 0.02 within 2A
O00D \\sim O00D \\sim C006: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
I1B \\sim I1A: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
Uanis(C006) \\sim Ueq, Uanis(O00D) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(C6)
\\sim Ueq, Uanis(O2) \\sim Ueq: with sigma of 0.001 and sigma for terminal
atoms of 0.002
Uanis(C006) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4. Rigid body (RIGU) restrains
 O2, C6, O2, C1
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 Fe04, C009, C00B, C00B, C7, C7, C2, C2, C18, C18, C1
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C1
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 I1A, Pb02
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 I1B, Pb02
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
5. Others
 Sof(I1B)=1-FVAR(1)
 Sof(I1A)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C00B(H00B), C7(H7), C2(H2), C18(H18)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y+1/2, z+1/2'
'-x, y+1/2, -z+1/2'
'x, -y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1, z+1/2'
'-x+1/2, y+1, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x, y-1/2, -z-1/2'
'x, -y-1/2, z-1/2'
'-x, y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, y, -z-1/2'
'x+1/2, -y, z-1/2'
'-x+1/2, y+1/2, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb01 Pb 0.500000 0.6083(3) 0.56347(16) 0.0446(12) Uani 1 2 d S T P . .
Pb02 Pb 0.34681(19) 0.3635(3) 0.55164(16) 0.0677(12) Uani 1 1 d D . . . .
Fe04 Fe 0.500000 0.0804(12) 0.6678(6) 0.052(4) Uani 1 2 d DS T P . .
O005 O 0.420(4) 0.500000 0.500000 0.045(16) Uani 1 2 d S T P A .
C006 C 0.500000 0.165(4) 0.536(2) 0.063(12) Uani 1 2 d DS TU P . .
C009 C 0.500000 0.062(4) 0.5758(16) 0.063(11) Uani 1 2 d DS T P . .
C00B C 0.442(4) 0.006(5) 0.5982(17) 0.062(11) Uani 1 1 d D . . . .
H00B H 0.391672 0.031551 0.588411 0.075 Uiso 1 1 calc R U . . .
O00D O 0.441(3) 0.221(5) 0.520(2) 0.065(11) Uani 1 1 d . U . . .
C7 C 0.457(4) -0.084(4) 0.638(3) 0.065(12) Uani 1 1 d D . . . .
H7 H 0.423546 -0.141220 0.658973 0.078 Uiso 1 1 calc R U . . .
I1B I 0.254(5) 0.408(8) 0.427(3) 0.121(8) Uani 0.15(3) 1 d D U P A 2
C2 C 0.442(4) 0.205(5) 0.718(3) 0.069(11) Uani 1 1 d D . . . .
H2 H 0.391340 0.224917 0.709937 0.083 Uiso 1 1 calc R U . . .
C1 C 0.500000 0.267(5) 0.688(5) 0.080(10) Uani 1 2 d DS T P . .
C18 C 0.463(4) 0.102(7) 0.754(2) 0.078(12) Uani 1 1 d D . . . .
H18 H 0.431205 0.045274 0.776823 0.093 Uiso 1 1 calc R U . . .
O2 O 0.427(3) 0.404(6) 0.627(3) 0.086(10) Uani 1 1 d . U . . .
C6 C 0.500000 0.371(10) 0.650(5) 0.085(10) Uani 1 2 d DS TU P . .
I1A I 0.2956(8) 0.3508(12) 0.4088(5) 0.116(5) Uani 0.85(3) 1 d D U P A 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O005 Pb01 Pb01 38.9(13) 9_666 9_666 ?
O005 Pb01 Pb01 38.9(13) . 9_666 ?
O005 Pb01 O005 78(3) 9_666 . ?
O005 Pb02 Pb02 36.2(14) . 4_566 ?
O005 Pb02 O00D 80.1(16) . . ?
O005 Pb02 I1B 78.5(16) . . ?
O005 Pb02 I1B 84.1(16) . 4_566 ?
O005 Pb02 I1A 73.3(8) . 4_566 ?
O005 Pb02 I1A 73.8(8) . . ?
O00D Pb02 Pb02 108.5(12) . 4_566 ?
O00D Pb02 I1B 164.3(16) . 4_566 ?
O00D Pb02 I1B 103(2) . . ?
O00D Pb02 I1A 84.5(12) . . ?
O00D Pb02 I1A 149.4(12) . 4_566 ?
I1B Pb02 I1B 73(4) 4_566 . ?
I1B Pb02 I1A 86(2) . 4_566 ?
I1B Pb02 I1A 19(2) 4_566 4_566 ?
O2 Pb02 Pb02 107.4(15) . 4_566 ?
O2 Pb02 O005 81.7(18) . . ?
O2 Pb02 O00D 82.0(19) . . ?
O2 Pb02 I1B 96(3) . 4_566 ?
O2 Pb02 I1B 158.3(19) . . ?
O2 Pb02 I1A 79.4(16) . 4_566 ?
O2 Pb02 I1A 153.7(15) . . ?
I1A Pb02 Pb02 55.60(17) 4_566 4_566 ?
I1A Pb02 Pb02 56.2(2) . 4_566 ?
I1A Pb02 I1A 102.0(5) . 4_566 ?
C009 Fe04 C00B 38.1(14) . . ?
C009 Fe04 C00B 38.1(14) . 12_655 ?
C009 Fe04 C7 66(2) . 12_655 ?
C009 Fe04 C7 66(2) . . ?
C009 Fe04 C2 127(2) . 12_655 ?
C009 Fe04 C2 127(2) . . ?
C009 Fe04 C1 108(3) . . ?
C00B Fe04 C00B 64(4) . 12_655 ?
C00B Fe04 C7 68(3) . 12_655 ?
C00B Fe04 C7 38.0(15) 12_655 12_655 ?
C00B Fe04 C7 68(3) 12_655 . ?
C00B Fe04 C7 38.0(15) . . ?
C00B Fe04 C1 123(3) . . ?
C00B Fe04 C1 123(3) 12_655 . ?
C7 Fe04 C7 46(4) . 12_655 ?
C7 Fe04 C1 156(2) . . ?
C7 Fe04 C1 156(2) 12_655 . ?
C2 Fe04 C00B 161(2) . 12_655 ?
C2 Fe04 C00B 113(3) . . ?
C2 Fe04 C00B 113(3) 12_655 12_655 ?
C2 Fe04 C00B 161(2) 12_655 . ?
C2 Fe04 C7 161(2) . 12_655 ?
C2 Fe04 C7 161(2) 12_655 . ?
C2 Fe04 C7 123(3) 12_655 12_655 ?
C2 Fe04 C7 123(3) . . ?
C2 Fe04 C2 63(4) 12_655 . ?
C2 Fe04 C1 40.4(17) 12_655 . ?
C2 Fe04 C1 40.4(17) . . ?
C18 Fe04 C009 161(2) 12_655 . ?
C18 Fe04 C009 161(2) . . ?
C18 Fe04 C00B 125(3) . . ?
C18 Fe04 C00B 158(2) 12_655 . ?
C18 Fe04 C00B 125(3) 12_655 12_655 ?
C18 Fe04 C00B 158(2) . 12_655 ?
C18 Fe04 C7 106(3) 12_655 12_655 ?
C18 Fe04 C7 106(3) . . ?
C18 Fe04 C7 122(3) 12_655 . ?
C18 Fe04 C7 122(3) . 12_655 ?
C18 Fe04 C2 65(3) . 12_655 ?
C18 Fe04 C2 65(3) 12_655 . ?
C18 Fe04 C2 40.5(17) . . ?
C18 Fe04 C2 40.5(17) 12_655 12_655 ?
C18 Fe04 C1 71(4) 12_655 . ?
C18 Fe04 C1 71(4) . . ?
C18 Fe04 C18 39(4) 12_655 . ?
Pb01 O005 Pb01 102(3) 9_666 . ?
Pb02 O005 Pb01 110.69(15) 4_566 . ?
Pb02 O005 Pb01 112.92(16) . . ?
Pb02 O005 Pb01 112.92(16) 4_566 9_666 ?
Pb02 O005 Pb01 110.69(15) . 9_666 ?
Pb02 O005 Pb02 108(3) . 4_566 ?
O00D C006 C009 123(3) 12_655 . ?
O00D C006 C009 123(3) . . ?
O00D C006 O00D 114(5) 12_655 . ?
C006 C009 Fe04 123(3) . . ?
C00B C009 Fe04 71.0(10) . . ?
C00B C009 Fe04 71.0(10) 12_655 . ?
C00B C009 C006 126(3) . . ?
C00B C009 C006 126(3) 12_655 . ?
C00B C009 C00B 108(6) . 12_655 ?
Fe04 C00B H00B 123.2 . . ?
C009 C00B Fe04 70.9(11) . . ?
C009 C00B H00B 123.2 . . ?
C7 C00B Fe04 71.0(10) . . ?
C7 C00B C009 113(6) . . ?
C7 C00B H00B 123.2 . . ?
C006 O00D Pb02 145(4) . . ?
Fe04 C7 H7 128.7 . . ?
C00B C7 Fe04 70.9(9) . . ?
C00B C7 C7 102(4) . 12_655 ?
C00B C7 H7 128.7 . . ?
C7 C7 Fe04 67(2) 12_655 . ?
C7 C7 H7 128.7 12_655 . ?
Pb02 I1B Pb02 72.1(8) 4_566 . ?
Fe04 C2 H2 122.2 . . ?
C1 C2 Fe04 69.9(11) . . ?
C1 C2 H2 122.2 . . ?
C1 C2 C18 115(6) . . ?
C18 C2 Fe04 69.7(10) . . ?
C18 C2 H2 122.2 . . ?
C2 C1 Fe04 69.7(11) 12_655 . ?
C2 C1 Fe04 69.7(11) . . ?
C2 C1 C2 98(7) 12_655 . ?
C6 C1 Fe04 130(8) . . ?
C6 C1 C2 131(3) . 12_655 ?
C6 C1 C2 131(3) . . ?
Fe04 C18 H18 127.0 . . ?
C2 C18 Fe04 69.8(10) . . ?
C2 C18 H18 127.0 . . ?
C18 C18 Fe04 71(2) 12_655 . ?
C18 C18 C2 106(4) 12_655 . ?
C18 C18 H18 127.0 12_655 . ?
C6 O2 Pb02 143(7) . . ?
C1 C6 O2 113(4) . . ?
C1 C6 O2 113(4) . 12_655 ?
O2 C6 O2 131(8) . 12_655 ?
Pb02 I1A Pb02 68.2(2) . 4_566 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb01 Pb01 3.621(7) 9_666 ?
Pb01 O005 2.33(4) 9_666 ?
Pb01 O005 2.33(4) . ?
Pb02 Pb02 3.690(6) 4_566 ?
Pb02 O005 2.29(4) . ?
Pb02 O00D 2.41(5) . ?
Pb02 I1B 3.01(6) 4_566 ?
Pb02 I1B 3.26(2) . ?
Pb02 O2 2.25(6) . ?
Pb02 I1A 3.280(10) . ?
Pb02 I1A 3.304(12) 4_566 ?
Fe04 C009 2.03(4) . ?
Fe04 C00B 2.03(4) . ?
Fe04 C00B 2.03(4) 12_655 ?
Fe04 C7 2.03(4) 12_655 ?
Fe04 C7 2.03(4) . ?
Fe04 C2 2.03(5) 12_655 ?
Fe04 C2 2.03(5) . ?
Fe04 C1 2.03(5) . ?
Fe04 C18 2.03(5) 12_655 ?
Fe04 C18 2.03(5) . ?
C006 C009 1.4000(11) . ?
C006 O00D 1.28(5) 12_655 ?
C006 O00D 1.28(5) . ?
C009 C00B 1.33(5) 12_655 ?
C009 C00B 1.33(5) . ?
C00B H00B 0.9800 . ?
C00B C7 1.33(5) . ?
C7 C7 1.58(15) 12_655 ?
C7 H7 0.9800 . ?
C2 H2 0.9800 . ?
C2 C1 1.41(7) . ?
C2 C18 1.41(7) . ?
C1 C6 1.400(11) . ?
C18 C18 1.35(15) 12_655 ?
C18 H18 0.9800 . ?
O2 C6 1.48(7) . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Pb02 O2 C6 C1 -88(10) . . . . ?
Pb02 O2 C6 O2 73(16) . . . 12_655 ?
Fe04 C009 C00B C7 -58(3) . . . . ?
Fe04 C00B C7 C7 -60.2(17) . . . 12_655 ?
Fe04 C2 C1 C2 -65(3) . . . 12_655 ?
Fe04 C2 C1 C6 125(11) . . . . ?
Fe04 C2 C18 C18 61.9(18) . . . 12_655 ?
Fe04 C1 C6 O2 82(9) . . . . ?
Fe04 C1 C6 O2 -82(9) . . . 12_655 ?
C006 C009 C00B Fe04 -118(4) . . . . ?
C006 C009 C00B C7 -176(4) . . . . ?
C009 C006 O00D Pb02 74(8) . . . . ?
C009 C00B C7 Fe04 58(3) . . . . ?
C009 C00B C7 C7 -2(4) . . . 12_655 ?
C00B C009 C00B Fe04 62(4) 12_655 . . . ?
C00B C009 C00B C7 3(7) 12_655 . . . ?
O00D C006 C009 Fe04 85(5) 12_655 . . . ?
O00D C006 C009 Fe04 -85(5) . . . . ?
O00D C006 C009 C00B -174(5) . . . 12_655 ?
O00D C006 C009 C00B 174(5) 12_655 . . . ?
O00D C006 C009 C00B 5(8) . . . . ?
O00D C006 C009 C00B -5(8) 12_655 . . 12_655 ?
O00D C006 O00D Pb02 -96(7) 12_655 . . . ?
C2 C1 C6 O2 -179(7) . . . 12_655 ?
C2 C1 C6 O2 15(16) 12_655 . . 12_655 ?
C2 C1 C6 O2 -15(16) . . . . ?
C2 C1 C6 O2 179(7) 12_655 . . . ?
C1 C2 C18 Fe04 -55(4) . . . . ?
C1 C2 C18 C18 7(5) . . . 12_655 ?
C18 C2 C1 Fe04 55(4) . . . . ?
C18 C2 C1 C2 -10(7) . . . 12_655 ?
C18 C2 C1 C6 -180(9) . . . . ?
