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_1571900
_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 H16 N4)'
_chemical_formula_sum            'C7 H8 I6 N2 Pb2'
_chemical_formula_weight         1295.93
_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                   12.9279(4)
_cell_length_b                   18.7521(6)
_cell_length_c                   17.6600(5)
_cell_measurement_reflns_used    7853
_cell_measurement_temperature    239.97(10)
_cell_measurement_theta_max      30.2530
_cell_measurement_theta_min      2.2780
_cell_volume                     4281.2(2)
_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 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      239.97(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 0.832
_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     -9.00  67.00   0.50    1.50    --    5.69  38.00 -30.00  152
  2  \w     -9.00  28.00   0.50    1.50    --   -6.24 -99.00-150.00   74
  3  \w    -22.00  10.00   0.50    1.50    --   -6.24 -94.00  39.00   64
  4  \w    -74.00  -4.00   0.50    1.50    --   -6.24 -42.00 149.00  140
;
_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      -0.0147940000
_diffrn_orient_matrix_UB_12      -0.0508550000
_diffrn_orient_matrix_UB_13      -0.0029482000
_diffrn_orient_matrix_UB_21      -0.0152481000
_diffrn_orient_matrix_UB_22      0.0039783000
_diffrn_orient_matrix_UB_23      0.0348684000
_diffrn_orient_matrix_UB_31      -0.0340868000
_diffrn_orient_matrix_UB_32      0.0202628000
_diffrn_orient_matrix_UB_33      -0.0143184000
_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  0.0828
_diffrn_reflns_av_unetI/netI     0.0556
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.832
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            15242
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.832
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.618
_diffrn_reflns_theta_min         2.172
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    24.349
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.07620
_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    4.021
_exptl_crystal_description       block
_exptl_crystal_F_000             4368
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         3.238
_refine_diff_density_min         -2.918
_refine_diff_density_rms         0.471
_refine_ls_extinction_coef       0.000063(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     90
_refine_ls_number_reflns         2864
_refine_ls_number_restraints     74
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0667
_refine_ls_R_factor_gt           0.0561
_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^)+(0.0848P)^2^+77.6044P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1520
_refine_ls_wR_factor_ref         0.1619
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2333
_reflns_number_total             2864
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc00954a2.cif
_cod_data_source_block           3Rac-240K
_cod_depositor_comments
'Adding full bibliography for 1571897--1571906.cif.'
_cod_original_sg_symbol_Hall     '-C 2bc 2'
_cod_database_code               1571900
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N I Pb'
_shelx_estimated_absorpt_t_max   0.085
_shelx_estimated_absorpt_t_min   0.085
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Shared sites
{N1, C1}
2. Restrained distances
 C4-C6 = C4-C7
 2.38 with sigma of 0.01
 C3-C6
 2.74 with sigma of 0.01
 C5-C7
 2.72 with sigma of 0.01
 C6-N2
 1.34 with sigma of 0.01
 C7-N2
 1.34 with sigma of 0.01
 C3-C4 = C5-C4 = C3-C7 = C5-C6
 1.37 with sigma of 0.01
 C2-C3
 1.49 with sigma of 0.01
 C4-N2
 2.74 with sigma of 0.01
 C6-C7
 2.33 with sigma of 0.01
 C3-C5
 2.36 with sigma of 0.01
 N2-C3 = N2-C5
 2.34 with sigma of 0.01
 C2-C6
 4.25 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uiso(N1) = Uiso(C1)
4. Rigid body (RIGU) restrains
 C5, C6, C7, N2, C3, C4, C2, N1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: N1(0.5) H1A(0.5) H1B(0.5) H1C(0.5) C1(0.5)
6.a Riding coordinates:
 N1(H1A,H1B,H1C)
6.b Aromatic/amide H refined with riding coordinates:
 N2(H2), C4(H4), C5(H5), C6(H6), C7(H7)
;
_shelx_res_checksum              71730
_shelx_hkl_checksum              85680
_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 3.921
_oxdiff_exptl_absorpt_empirical_full_min 0.394