Chiral three-dimensional organic-inorganic lead iodide hybrid semiconductors.
Fan, Chang-Chun; Liu, Cheng-Dong; Liang, Bei-Dou; Ju, Tong-Yu; Wang, Wei; Jin, Ming-Liang; Chai, Chao-Yang; Zhang, Wen; Chemical science 15 (2024) 11374–11381; doi:10.1039/d4sc00954a

data_1571905
_publ_section_title
;
 Chiral three-dimensional organic-inorganic lead iodide hybrid
 semiconductors.
;
_journal_issue                   29
_journal_name_full               'Chemical science'
_journal_page_first              11374
_journal_page_last               11381
_journal_paper_doi               10.1039/d4sc00954a
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'I6 Pb2, 0.5(C14 H24 N4)'
_chemical_formula_sum            'C7 H12 I6 N2 Pb2'
_chemical_formula_weight         1299.97
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-01-05
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2024-01-05 deposited with the CCDC.	2024-06-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.9548(6)
_cell_length_b                   18.8648(9)
_cell_length_c                   17.6101(7)
_cell_measurement_reflns_used    4263
_cell_measurement_temperature    299.13(10)
_cell_measurement_theta_max      30.7780
_cell_measurement_theta_min      2.1960
_cell_volume                     4303.7(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_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 (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      299.13(10)
_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 0.819
_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    -26.00   6.00   0.50    1.50    --    5.69  94.00  61.00   64
  2  \w    -20.00  44.00   0.50    1.50    --   -6.24  38.00 -60.00  128
  3  \w    -18.00  31.00   0.50    1.50    --    5.69 -99.00-180.00   98
  4  \w    -13.00  32.00   0.50    1.50    --    5.69 -94.00 -49.00   90
;
_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      0.0153755000
_diffrn_orient_matrix_UB_12      -0.0505868000
_diffrn_orient_matrix_UB_13      0.0006706000
_diffrn_orient_matrix_UB_21      -0.0079125000
_diffrn_orient_matrix_UB_22      -0.0054840000
_diffrn_orient_matrix_UB_23      -0.0366875000
_diffrn_orient_matrix_UB_31      0.0363751000
_diffrn_orient_matrix_UB_32      0.0201836000
_diffrn_orient_matrix_UB_33      -0.0082485000
_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  0.0394
_diffrn_reflns_av_unetI/netI     0.0380
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.819
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            13562
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.819
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.555
_diffrn_reflns_theta_min         2.159
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    24.222
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.11415
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic reddish red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    4.013
_exptl_crystal_description       block
_exptl_crystal_F_000             4400
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.491
_refine_diff_density_min         -4.696
_refine_diff_density_rms         0.325
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     96
_refine_ls_number_reflns         2819
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0762
_refine_ls_R_factor_gt           0.0517
_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^)+(0.0321P)^2^+157.0801P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1058
_refine_ls_wR_factor_ref         0.1151
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2076
_reflns_number_total             2819
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc00954a2.cif
_cod_data_source_block           2Rac
_cod_depositor_comments
'Adding full bibliography for 1571897--1571906.cif.'
_cod_original_sg_symbol_Hall     '-C 2bc 2'
_cod_database_code               1571905
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C1 H1 N1 Pb1 I1'
_shelx_estimated_absorpt_t_max   0.085
_shelx_estimated_absorpt_t_min   0.085
_reflns_odcompleteness_completeness 99.63
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Shared sites
{C1, N1}
2. Restrained distances
 C2-N1
 1.51 with sigma of 0.01
 C1-C2
 1.51 with sigma of 0.01
 C2-C3
 1.51 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C1) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C1) = Uanis(N1)
4. Rigid body (RIGU) restrains
 C4, C5, C6, C7, N2, C3, C2, N1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: C1(0.5) H1A(0.5) H1B(0.5) H1C(0.5) N1(0.5) H1D(0.5) H1E(0.5)
 H1F(0.5)
6.a Riding coordinates:
 C1(H1A,H1B,H1C), N1(H1D,H1E,H1F)
6.b Aromatic/amide H refined with riding coordinates:
 N2(H2), C7(H7), C5(H5), C6(H6), C4(H4)
;
_shelx_res_checksum              31384
_shelx_hkl_checksum              95600
_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 3.736
_oxdiff_exptl_absorpt_empirical_full_min 0.443