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_1572979
_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         'Br4 Pb, 2(C8 H11 Br N)'
_chemical_formula_sum            'C16 H22 Br6 N2 Pb'
_chemical_formula_weight         929.00
_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     dual
_audit_creation_date             2023-10-06
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-04-16 deposited with the CCDC.	2024-10-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.8460(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.73840(10)
_cell_length_b                   7.84410(10)
_cell_length_c                   17.9204(2)
_cell_measurement_reflns_used    8231
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      74.4160
_cell_measurement_theta_min      4.9670
_cell_volume                     1216.85(3)
_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 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_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 1.000
_diffrn_measured_fraction_theta_max 0.984
_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    -93.00 -17.00   1.00    1.50    --  -41.26 -37.00   0.00   76
  2  \w   -119.00  -3.00   1.00    1.50    --  -41.26 -19.00  90.00  116
  3  \w    -48.00  -7.00   1.00    1.50    --  -41.26 125.00-180.00   41
  4  \w     28.00  95.00   1.00    1.50    --   41.26-125.00 -30.00   67
  5  \w     31.00  58.00   1.00    1.50    --   41.26-125.00-180.00   27
  6  \w     16.00  59.00   1.00    1.50    --   41.26  57.00  30.00   43
  7  \w     78.00 105.00   1.00    3.00    --  107.01  61.00  30.00   27
  8  \w     79.00 106.00   1.00    3.00    --  107.01  60.00 -14.72   27
  9  \w    112.00 177.00   1.00    3.00    --  107.01  69.00 -49.34   65
 10  \w     31.00 127.00   1.00    3.00    --  107.01 -77.00-120.00   96
 11  \w     82.00 107.00   1.00    3.00    --  107.01  45.00   0.00   25
 12  \w     34.00 121.00   1.00    3.00    --  107.01 -45.00 -90.00   87
 13  \w     78.00 177.00   1.00    3.00    --  107.01  61.00  60.00   99
 14  \w     58.00 177.00   1.00    3.00    --  107.01  15.00-180.00  119
 15  \w     78.00 109.00   1.00    3.00    --  107.01  61.00 -30.00   31
 16  \w    146.00 172.00   1.00    3.00    --  107.01  61.00   0.00   26
 17  \w     79.00 104.00   1.00    3.00    --  107.01  61.00 -60.00   25
 18  \w     82.00 138.00   1.00    3.00    --  107.01  45.00  60.00   56
 19  \w     81.00 115.00   1.00    3.00    --  107.01  45.00  30.00   34
 20  \w    107.00 156.00   1.00    3.00    --  107.01 111.00 -30.00   49
 21  \w     81.00 108.00   1.00    3.00    --  107.01  45.00 -30.00   27
 22  \w     78.00 104.00   1.00    3.00    --  107.01  61.00   0.00   26
 23  \w     77.00 104.00   1.00    3.00    --  107.01  69.00 -49.34   27
 24  \w     82.00 157.00   1.00    3.00    --  107.01  44.00  43.01   75
;
_diffrn_measurement_device       'kappa diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0944320000
_diffrn_orient_matrix_UB_12      0.0945593000
_diffrn_orient_matrix_UB_13      -0.0537672000
_diffrn_orient_matrix_UB_21      -0.1452170000
_diffrn_orient_matrix_UB_22      0.0135909000
_diffrn_orient_matrix_UB_23      -0.0589361000
_diffrn_orient_matrix_UB_31      -0.0402632000
_diffrn_orient_matrix_UB_32      0.1717138000
_diffrn_orient_matrix_UB_33      0.0341892000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0418
_diffrn_reflns_av_unetI/netI     0.0392
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            9475
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.950
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.513
_diffrn_reflns_theta_min         2.489
_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    25.048
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.09491
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.535
_exptl_crystal_description       plate
_exptl_crystal_F_000             848
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.918
_refine_diff_density_min         -2.067
_refine_diff_density_rms         0.332
_refine_ls_abs_structure_details
;
 Flack x determined using 1975 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.029(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     230
_refine_ls_number_reflns         4738
_refine_ls_number_restraints     100
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0482
_refine_ls_R_factor_gt           0.0476
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1102P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1329
_refine_ls_wR_factor_ref         0.1340
_reflns_Friedel_coverage         0.795
_reflns_Friedel_fraction_full    0.960
_reflns_Friedel_fraction_max     0.911
_reflns_number_gt                4621
_reflns_number_total             4738
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc04915b2.cif
_cod_data_source_block           zixuan46
_cod_depositor_comments
'Adding full bibliography for 1572979--1572983.cif.'
_cod_database_code               1572979
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'Pb Br5 N2 C20 H28'
_shelx_estimated_absorpt_t_max   0.520
_shelx_estimated_absorpt_t_min   0.082
_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. Rigid body (RIGU) restrains
 C17, C11, C16, C15, C14, C13, C12, Br12
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 Br11, C5, C4, C3, C2, C1, C6
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3.a Ternary CH refined with riding coordinates:
 C7(H7), C17(H17)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C6(H6), C12(H12), C14(H14), C15(H15), C16(H16)
3.c Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), C8(H8A,H8B,H8C), N2(H2A,H2B,H2C), C18(H18A,H18B,H18C)
;
_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 5.470
_oxdiff_exptl_absorpt_empirical_full_min 0.527