Deciphering the electronic and structural origin of chiroptical activity of chiral 2D perovskites.
Zhang, Zixuan; Wu, Jin; Lu, Haipeng; Chemical science 15 (2024) 20440–20447; doi:10.1039/d4sc04915b

data_1572983
_publ_section_title
;
 Deciphering the electronic and structural origin of chiroptical activity
 of chiral 2D perovskites.
;
_journal_issue                   48
_journal_name_full               'Chemical science'
_journal_page_first              20440
_journal_page_last               20447
_journal_paper_doi               10.1039/d4sc04915b
_journal_volume                  15
_journal_year                    2024
_chemical_absolute_configuration ad
_chemical_formula_moiety         'I4 Pb, 2(C8 H11 Br N)'
_chemical_formula_sum            'C16 H22 Br2 I4 N2 Pb'
_chemical_formula_weight         1116.96
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2023-12-07
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2023.11.24 svn.r209d9fb2 for OlexSys, GUI svn.r6869)
;
_audit_update_record
;
2024-04-16 deposited with the CCDC.	2024-10-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.883(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.1768(2)
_cell_length_b                   8.2407(2)
_cell_length_c                   17.8463(5)
_cell_measurement_reflns_used    4917
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      74.0610
_cell_measurement_theta_min      4.8740
_cell_volume                     1333.41(6)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5-alpha (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3577
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.972
_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     13.00 116.00   1.00    4.00    --   39.70  37.00   0.00  103
  2  \w     12.00 106.00   1.00    4.00    --   39.70  57.00-120.00   94
  3  \w    -21.00  71.00   1.00    4.00    --   39.70 -77.00  90.00   92
  4  \w     80.00 127.00   1.00   11.00    --  107.44  45.00 120.00   47
  5  \w     77.00 158.00   1.00   11.00    --  107.44  61.00   0.00   81
  6  \w     32.00 103.00   1.00   11.00    --  107.44 -94.00 -30.00   71
  7  \w    104.00 178.00   1.00   11.00    --  107.44 111.00  30.00   74
  8  \w     80.00 116.00   1.00   11.00    --  107.44  45.00  90.00   36
  9  \w    127.00 170.00   1.00   11.00    --  107.44  45.00  90.00   43
 10  \w     39.00 108.00   1.00   11.00    --  107.44-111.00-120.00   69
 11  \w    139.00 178.00   1.00   11.00    --  107.44  45.00 120.00   39
 12  \w     29.00 141.00   1.00   11.00    --  107.44 -77.00  30.00  112
 13  \w     33.00  99.00   1.00   11.00    --  107.44 -30.00  90.00   66
 14  \w    113.00 138.00   1.00   11.00    --  107.44 -30.00  90.00   25
 15  \w    108.00 133.00   1.00   11.00    --  107.44 111.00-180.00   25
;
_diffrn_measurement_device       'kappa diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1512581000
_diffrn_orient_matrix_UB_12      0.0023984000
_diffrn_orient_matrix_UB_13      0.0273098000
_diffrn_orient_matrix_UB_21      0.0753700000
_diffrn_orient_matrix_UB_22      0.0480140000
_diffrn_orient_matrix_UB_23      0.0801174000
_diffrn_orient_matrix_UB_31      -0.0181100000
_diffrn_orient_matrix_UB_32      0.1806027000
_diffrn_orient_matrix_UB_33      -0.0216886000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0302
_diffrn_reflns_av_unetI/netI     0.0437
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            7755
_diffrn_reflns_point_group_measured_fraction_full 0.853
_diffrn_reflns_point_group_measured_fraction_max 0.817
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.263
_diffrn_reflns_theta_min         4.878
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           0.80
_diffrn_source_power             0.040
_diffrn_source_target            Cu
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    52.197
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66664
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.782
_exptl_crystal_description       plate
_exptl_crystal_F_000             992
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.043
_refine_diff_density_min         -0.830
_refine_diff_density_rms         0.148
_refine_ls_abs_structure_details
;
 Flack x determined using 1421 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.004(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     230
_refine_ls_number_reflns         4452
_refine_ls_number_restraints     55
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.0280
_refine_ls_R_factor_gt           0.0251
_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^)+(0.0207P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0548
_refine_ls_wR_factor_ref         0.0559
_reflns_Friedel_coverage         0.565
_reflns_Friedel_fraction_full    0.685
_reflns_Friedel_fraction_max     0.636
_reflns_number_gt                4199
_reflns_number_total             4452
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc04915b2.cif
_cod_data_source_block           zixuan49a_173k_auto
_cod_depositor_comments
'Adding full bibliography for 1572979--1572983.cif.'
_cod_original_cell_volume        1333.40(6)
_cod_database_code               1572983
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.422
_shelx_estimated_absorpt_t_min   0.303
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C15) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C12)
\\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C17) \\sim Ueq,
Uanis(C18) \\sim Ueq, Uanis(N2) \\sim Ueq: with sigma of 0.003 and sigma for
terminal atoms of 0.01
3.a Ternary CH refined with riding coordinates:
 C17(H17), C7(H7)
3.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C14(H14), C15(H15), C16(H16), C2(H2), C4(H4), C5(H5), C6(H6)
3.c Idealised Me refined as rotating group:
 N2(H2A,H2B,H2C), C18(H18A,H18B,H18C), N1(H1A,H1B,H1C), C8(H8A,H8B,H8C)
;
_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 1.699
_oxdiff_exptl_absorpt_empirical_full_min 0.703