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_1571906
_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         'I6 Pb2, C7 H12 N2'
_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     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                   12.9629(3)
_cell_length_b                   18.7955(5)
_cell_length_c                   17.6714(5)
_cell_measurement_reflns_used    16647
_cell_measurement_temperature    297.98(10)
_cell_measurement_theta_max      30.4920
_cell_measurement_theta_min      2.4300
_cell_volume                     4305.53(19)
_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      297.98(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 0.925
_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    -68.00 -42.00   0.50    0.25    --    5.69 -38.00  30.00   52
  2  \w    -58.00  20.00   0.50    0.25    --    5.69 -38.00  90.00  156
  3  \w    -32.00  20.00   0.50    0.25    --    5.69 -38.00  30.00  104
  4  \w    -65.00  20.00   0.50    0.25    --    5.69 -29.00 -13.03  170
  5  \w    -68.00  20.00   0.50    0.25    --    5.69 -38.00-180.00  176
  6  \w     -6.00  79.00   0.50    0.25    --    5.69  77.00-180.00  170
  7  \w    -22.00  10.00   0.50    0.25    --   -6.24  30.00-144.33   64
  8  \w     -5.00  40.00   0.50    0.25    --    5.69 -99.00-180.00   90
  9  \w     28.00  69.00   0.50    0.25    --   -6.24  30.00-144.33   82
 10  \w    -22.00  69.00   0.50    0.25    --   -6.24  31.00 -73.99  182
 11  \w    -75.00   9.00   0.50    0.25    --   -6.24 -38.00-120.00  168
 12  \w    -18.00  26.00   0.50    0.25    --   -6.24 -99.00  30.00   88
 13  \w    -18.00  28.00   0.50    0.25    --   -6.24 -99.00 120.00   92
;
_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      0.0241828000
_diffrn_orient_matrix_UB_12      0.0143535000
_diffrn_orient_matrix_UB_13      -0.0326099000
_diffrn_orient_matrix_UB_21      0.0188808000
_diffrn_orient_matrix_UB_22      -0.0342734000
_diffrn_orient_matrix_UB_23      -0.0095203000
_diffrn_orient_matrix_UB_31      -0.0452985000
_diffrn_orient_matrix_UB_32      -0.0066250000
_diffrn_orient_matrix_UB_33      -0.0213720000
_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  0.0746
_diffrn_reflns_av_unetI/netI     0.0412
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.925
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            59812
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.897
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.914
_diffrn_reflns_theta_min         1.908
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    24.212
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.27583
_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 pinkish red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   pinkish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    4.011
_exptl_crystal_description       block
_exptl_crystal_F_000             4400
_refine_diff_density_max         3.013
_refine_diff_density_min         -5.375
_refine_diff_density_rms         0.501
_refine_ls_abs_structure_details
;
 Flack x determined using 1543 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.019(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.991
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     179
_refine_ls_number_reflns         6128
_refine_ls_number_restraints     100
_refine_ls_restrained_S_all      0.991
_refine_ls_R_factor_all          0.0767
_refine_ls_R_factor_gt           0.0488
_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^)+(0.0928P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1343
_refine_ls_wR_factor_ref         0.1492
_reflns_Friedel_coverage         0.772
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.863
_reflns_number_gt                4234
_reflns_number_total             6128
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc00954a2.cif
_cod_data_source_block           3R-298K
_cod_depositor_comments
'Adding full bibliography for 1571897--1571906.cif.'
_cod_database_code               1571906
_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-C1A = C2-C1B
 1.53 with sigma of 0.02
 N1A-C2 = N1B-C2
 1.47 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
N1B: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08 within
1.7A
Uanis(C2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N1A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C1A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C1B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N1B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Rigid body (RIGU) restrains
 N2, C3, C4, C5, C6, C7
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C7, N2, C5, C4, C6, C3, C2, C1B, N1A, N1B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: 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) H1BC(0.5) C1B(0.5) H1BD(0.5)
 H1BE(0.5) H1BF(0.5)
5.a Ternary CH refined with riding coordinates:
 C2(H2A)
5.b Aromatic/amide H refined with riding coordinates:
 N2(H2), C4(H4), C5(H5), C6(H6), C7(H7)
5.c Idealised Me refined as rotating group:
 N1A(H1AA,H1AB,H1AC), C1A(H1AD,H1AE,H1AF), N1B(H1BA,H1BB,H1BC), C1B(H1BD,H1BE,
 H1BF)
;
_shelx_res_checksum              48730
_shelx_hkl_checksum              13363
_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 2.286
_oxdiff_exptl_absorpt_empirical_full_min 0.569