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_1571899
_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, C7 H11 N2'
_chemical_formula_sum            'C7 H11 I6 N2 Pb2'
_chemical_formula_weight         1298.96
_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   mixed
_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                   12.9621(7)
_cell_length_b                   18.7875(13)
_cell_length_c                   17.6666(9)
_cell_measurement_reflns_used    3248
_cell_measurement_temperature    298.53(10)
_cell_measurement_theta_max      30.6130
_cell_measurement_theta_min      3.9010
_cell_volume                     4302.3(4)
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      298.53(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 0.808
_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    -23.00  53.00   0.50    2.00    --   -7.05  38.00   0.00  152
  2  \w    -35.00  -3.00   0.50    2.00    --   -7.05  87.00 134.00   64
  3  \w    -18.00  14.00   0.50    2.00    --   -7.05 -99.00-120.00   64
  4  \w     -9.00  18.00   0.50    2.00    --   -7.05 -99.00-150.00   54
;
_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      -0.0116812000
_diffrn_orient_matrix_UB_12      -0.0368952000
_diffrn_orient_matrix_UB_13      0.0005537000
_diffrn_orient_matrix_UB_21      -0.0476403000
_diffrn_orient_matrix_UB_22      0.0069374000
_diffrn_orient_matrix_UB_23      -0.0183189000
_diffrn_orient_matrix_UB_31      0.0242479000
_diffrn_orient_matrix_UB_32      -0.0041222000
_diffrn_orient_matrix_UB_33      -0.0357085000
_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  0.0252
_diffrn_reflns_av_unetI/netI     0.0380
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.808
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            11819
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.759
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.652
_diffrn_reflns_theta_min         1.909
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    24.230
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71819
_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    4.011
_exptl_crystal_description       block
_exptl_crystal_F_000             4392
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.955
_refine_diff_density_min         -2.707
_refine_diff_density_rms         0.293
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.41(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     176
_refine_ls_number_reflns         5064
_refine_ls_number_restraints     374
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0791
_refine_ls_R_factor_gt           0.0424
_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^)+(0.0414P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0952
_refine_ls_wR_factor_ref         0.1058
_reflns_Friedel_coverage         0.716
_reflns_Friedel_fraction_full    0.958
_reflns_Friedel_fraction_max     0.700
_reflns_number_gt                3198
_reflns_number_total             5064
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc00954a2.cif
_cod_data_source_block           3S-298K
_cod_depositor_comments
'Adding full bibliography for 1571897--1571906.cif.'
_cod_database_code               1571899
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C1 H1 N1 I1 Pb1'
_shelx_estimated_absorpt_t_max   0.643
_shelx_estimated_absorpt_t_min   0.530
_reflns_odcompleteness_completeness 99.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.58546
 0.41454
2. Restrained distances
 N1B-C2 = N1A-C2
 1.47 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
N2 \\sim H2 \\sim C2 \\sim H2A \\sim C3 \\sim C4 \\sim H4 \\sim C5 \\sim H5
\\sim C6 \\sim H6 \\sim C7 \\sim H7 \\sim N1A \\sim H1AA \\sim H1AB \\sim H1AC
\\sim C1A \\sim H1AD \\sim H1AE \\sim H1AF \\sim N1B \\sim H1BA \\sim H1BB
\\sim C1B \\sim H1BC \\sim H1BD \\sim H1BE: within 1.7A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 1.7A
Uanis(N1A) \\sim Ueq, Uanis(C1B) \\sim Ueq, Uanis(N1B) \\sim Ueq, Uanis(C1A)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 N2, H2, C2, C3, C4, H4, C5, H5, C6, H6, C7, H7, N1A, C1A, N1B, C1B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C7, C3, C4, C5, C6, N2, C2, N1B, C1A, N1A, C1B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: H2A(0.5) N1A(0.5) H1AA(0.5) H1AB(0.5) H1AC(0.5) C1A(0.5) H1AD(0.5)
 H1AE(0.5) H1AF(0.5) N1B(0.5) H1BA(0.5) H1BB(0.5) C1B(0.5) H1BC(0.5) H1BD(0.5)
 H1BE(0.5)
6.a Riding coordinates:
 N1A(H1AA,H1AB,H1AC), C1A(H1AD,H1AE,H1AF), C1B(H1BC,H1BD,H1BE)
6.b Ternary CH refined with riding coordinates:
 C2(H2A)
6.c Aromatic/amide H refined with riding coordinates:
 N2(H2), C4(H4), C5(H5), C6(H6), C7(H7)
6.d X=CH2 refined with riding coordinates:
 N1B(H1BA,H1BB)
;
_shelx_res_checksum              17689
_shelx_hkl_checksum              75365
_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 1.378
_oxdiff_exptl_absorpt_empirical_full_min 0.732