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_1572980
_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 R
_chemical_formula_moiety         'Br4 Pb, 2(C8 H11 Cl N)'
_chemical_formula_sum            'C16 H22 Br4 Cl2 N2 Pb'
_chemical_formula_weight         840.08
_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             2024-03-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2024-04-16 deposited with the CCDC.	2024-10-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.984(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.7598(2)
_cell_length_b                   7.7798(2)
_cell_length_c                   17.5050(4)
_cell_measurement_reflns_used    5213
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      29.6200
_cell_measurement_theta_min      2.3390
_cell_volume                     1181.39(5)
_computing_cell_refinement       'CrysAlisPro 1.171.43.90 (Rigaku OD, 2023)'
_computing_data_collection
'CrysAlisPro system (CCD 43.90 (release 15-09-2023))'
_computing_data_reduction        'CrysAlisPro 1.171.43.90 (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3577
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -40.00  49.00   1.00    2.50    --   15.85 -77.00-120.00   89
  2  \w    -40.00  50.00   1.00    2.50    --   15.85 -77.00 120.00   90
  3  \w    -41.00  50.00   1.00    2.50    --   15.85 -77.00   0.00   91
;
_diffrn_measurement_device       'four-circle 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      -0.0112390000
_diffrn_orient_matrix_UB_12      -0.0078378000
_diffrn_orient_matrix_UB_13      0.0392060000
_diffrn_orient_matrix_UB_21      0.0255938000
_diffrn_orient_matrix_UB_22      0.0858594000
_diffrn_orient_matrix_UB_23      0.0068711000
_diffrn_orient_matrix_UB_31      -0.0768147000
_diffrn_orient_matrix_UB_32      0.0297264000
_diffrn_orient_matrix_UB_33      -0.0094563000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0255
_diffrn_reflns_av_unetI/netI     0.0469
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            7306
_diffrn_reflns_point_group_measured_fraction_full 0.934
_diffrn_reflns_point_group_measured_fraction_max 0.926
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.731
_diffrn_reflns_theta_min         2.348
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    14.135
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.36143
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.90 (Rigaku Oxford Diffraction, 2023)
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    2.362
_exptl_crystal_description       block
_exptl_crystal_F_000             776
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.942
_refine_diff_density_min         -1.389
_refine_diff_density_rms         0.182
_refine_ls_abs_structure_details
;
 Flack x determined using 1708 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.040(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     230
_refine_ls_number_reflns         4643
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0335
_refine_ls_R_factor_gt           0.0307
_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^)+(0.0325P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0673
_refine_ls_wR_factor_ref         0.0691
_reflns_Friedel_coverage         0.724
_reflns_Friedel_fraction_full    0.858
_reflns_Friedel_fraction_max     0.842
_reflns_number_gt                4383
_reflns_number_total             4643
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc04915b2.cif
_cod_data_source_block           3-cl-mba-pbbr
_cod_depositor_comments
'Adding full bibliography for 1572979--1572983.cif.'
_cod_database_code               1572980
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Pb I Cl C N'
_shelx_estimated_absorpt_t_max   0.438
_shelx_estimated_absorpt_t_min   0.305
_diffrn_oxdiff_digest_frames
;
01a077a30a747393495c3aa531c2a1f46e00284d2b5
;
_diffrn_oxdiff_digest_hkl
;
01ba0dc6263eeef0982004e0b2d5abaac0ed6e
;
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.04
_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(C00B) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
3.a Ternary CH refined with riding coordinates:
 C00G(H00S), C00H(H00H)
3.b Aromatic/amide H refined with riding coordinates:
 C00C(H00Q), C00D(H00R), C00F(H00F), C00J(H00T), C00L(H00U), C00O(H00O),
 C00P(H00P), C1(H1)
3.c Idealised Me refined as rotating group:
 N008(H00A,H00B,H00C), N009(H00I,H00J,H00K), C00B(H00L,H00M,H00N), C00K(H00D,
 H00E,H00G)
;
_shelx_res_checksum              54257
_shelx_hkl_checksum              75500
_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 1.727
_oxdiff_exptl_absorpt_empirical_full_min 0.734