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_1571904
_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_absolute_configuration ad
_chemical_formula_moiety         'C7 H12 N2, I6 Pb2'
_chemical_formula_sum            'C7 H12 I6 N2 Pb2'
_chemical_formula_weight         1299.97
_space_group_crystal_system      orthorhombic
_space_group_IT_number           20
_space_group_name_Hall           'C 2c 2'
_space_group_name_H-M_alt        'C 2 2 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_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                   12.9335(6)
_cell_length_b                   18.7349(8)
_cell_length_c                   17.6358(8)
_cell_measurement_reflns_used    6768
_cell_measurement_temperature    245.03(10)
_cell_measurement_theta_max      30.6550
_cell_measurement_theta_min      2.1820
_cell_volume                     4273.3(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 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      245.03(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 0.839
_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  35.00   0.50    1.10    --   -6.24  57.00   0.00   52
  2  \w     50.00  76.00   0.50    1.10    --    5.69  38.00 -60.00   52
  3  \w    -69.00  21.00   0.50    1.10    --    5.69 -17.00 -53.00  180
  4  \w    -14.00  24.00   0.50    1.10    --    5.69 -99.00 -90.00   76
  5  \w    -17.00  28.00   0.50    1.10    --   -6.24 -99.00  60.00   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      -0.0511923000
_diffrn_orient_matrix_UB_12      0.0114719000
_diffrn_orient_matrix_UB_13      -0.0076432000
_diffrn_orient_matrix_UB_21      -0.0156857000
_diffrn_orient_matrix_UB_22      -0.0360305000
_diffrn_orient_matrix_UB_23      -0.0046000000
_diffrn_orient_matrix_UB_31      -0.0118750000
_diffrn_orient_matrix_UB_32      -0.0019960000
_diffrn_orient_matrix_UB_33      0.0392004000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0663
_diffrn_reflns_av_unetI/netI     0.0612
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.839
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            15592
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.794
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.780
_diffrn_reflns_theta_min         1.913
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    24.395
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.19883
_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    4.041
_exptl_crystal_description       plate
_exptl_crystal_F_000             4400
_refine_diff_density_max         4.880
_refine_diff_density_min         -4.819
_refine_diff_density_rms         0.649
_refine_ls_abs_structure_details
;
 Flack x determined using 1214 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.00(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     159
_refine_ls_number_reflns         5320
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0900
_refine_ls_R_factor_gt           0.0684
_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^)+(0.1106P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1748
_refine_ls_wR_factor_ref         0.1865
_reflns_Friedel_coverage         0.727
_reflns_Friedel_fraction_full    0.992
_reflns_Friedel_fraction_max     0.740
_reflns_number_gt                3776
_reflns_number_total             5320
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc00954a2.cif
_cod_data_source_block           3S-245K
_cod_depositor_comments
'Adding full bibliography for 1571897--1571906.cif.'
_cod_database_code               1571904
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N I Pb'
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Restrained distances
 C2-C6
 4.25 with sigma of 0.02
 N2-C3 = N2-C5
 2.34 with sigma of 0.01
 C3-C5
 2.36 with sigma of 0.01
 C6-C7
 2.33 with sigma of 0.01
 C4-N2
 2.74 with sigma of 0.01
 C1-C2
 1.53 with sigma of 0.01
 C2-N1
 1.48 with sigma of 0.01
 C2-C3
 1.49 with sigma of 0.01
 C3-C4 = C5-C4 = C3-C7 = C5-C6
 1.37 with sigma of 0.01
 C7-N2
 1.34 with sigma of 0.01
 C6-N2
 1.34 with sigma of 0.01
 C5-C7
 2.72 with sigma of 0.01
 C3-C6
 2.74 with sigma of 0.01
 C4-C6 = C4-C7
 2.38 with sigma of 0.01
2. Uiso/Uaniso restraints and constraints
Uanis(C5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3.a Ternary CH refined with riding coordinates:
 C2(H2)
3.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), N2(H2A)
3.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), N1(H1D,H1E,H1F)
;
_shelx_res_checksum              62748
_shelx_hkl_checksum              37129
_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 2.741
_oxdiff_exptl_absorpt_empirical_full_min 0.545