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_1572982
_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         'Br8 Pb2, 4(C8 H11 Br N), 2(H2 O)'
_chemical_formula_sum            'C32 H48 Br12 N4 O2 Pb2'
_chemical_formula_weight         1894.04
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-03-01
_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                 90.903(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.8357(2)
_cell_length_b                   35.9831(11)
_cell_length_c                   8.8981(2)
_cell_measurement_reflns_used    9632
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      29.7120
_cell_measurement_theta_min      2.3550
_cell_volume                     2508.53(11)
_computing_cell_refinement       'CrysAlisPro 1.171.43.90 (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.43.90 (Rigaku OD, 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      99.99(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    -86.00   8.50   0.75   12.00    --  -15.46 -57.00  60.00  126
  2  \w     -9.00  88.50   0.75   12.00    --   15.85  57.00   0.00  130
  3  \w    -35.00  51.25   0.75   12.00    --   15.85 -77.00-150.00  115
;
_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      0.0007341000
_diffrn_orient_matrix_UB_12      -0.0182299000
_diffrn_orient_matrix_UB_13      0.0302791000
_diffrn_orient_matrix_UB_21      -0.0408061000
_diffrn_orient_matrix_UB_22      0.0066485000
_diffrn_orient_matrix_UB_23      0.0652803000
_diffrn_orient_matrix_UB_31      -0.0808279000
_diffrn_orient_matrix_UB_32      -0.0035097000
_diffrn_orient_matrix_UB_33      -0.0342211000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0402
_diffrn_reflns_av_unetI/netI     0.0623
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            14228
_diffrn_reflns_point_group_measured_fraction_full 0.867
_diffrn_reflns_point_group_measured_fraction_max 0.867
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.348
_diffrn_reflns_theta_min         2.289
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    16.292
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.21466
_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    2.508
_exptl_crystal_description       plate
_exptl_crystal_F_000             1736
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.03
_refine_diff_density_max         3.143
_refine_diff_density_min         -2.295
_refine_diff_density_rms         0.328
_refine_ls_abs_structure_details
;
 Flack x determined using 2733 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.023(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     483
_refine_ls_number_reflns         7980
_refine_ls_number_restraints     219
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0543
_refine_ls_R_factor_gt           0.0508
_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^)+(0.0583P)^2^+30.7291P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1222
_refine_ls_wR_factor_ref         0.1248
_reflns_Friedel_coverage         0.705
_reflns_Friedel_fraction_full    0.731
_reflns_Friedel_fraction_max     0.729
_reflns_number_gt                7556
_reflns_number_total             7980
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc04915b2.cif
_cod_data_source_block           pbbr-4-brmba
_cod_depositor_comments
'Adding full bibliography for 1572979--1572983.cif.'
_cod_database_code               1572982
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Pb Br C N'
_shelx_estimated_absorpt_t_max   0.641
_shelx_estimated_absorpt_t_min   0.168
_diffrn_oxdiff_digest_frames
;
01f82cf9bd4f5debbdca55ef6f06e4812d000276603
;
_diffrn_oxdiff_digest_hkl
;
0135eb38af3f0b071d0768ab3aae2cd1e9fa16
;
_reflns_odcompleteness_completeness 99.93
_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, All O(H,H) groups
2. Restrained distances
 H1B-H00R
 2.1 with sigma of 0.01
 H1A-H00B
 2.1 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C01E) \\sim Ueq, Uanis(C00I) \\sim Ueq, Uanis(C00L) \\sim Ueq,
Uanis(N00K) \\sim Ueq, Uanis(N00J) \\sim Ueq, Uanis(C00O) \\sim Ueq,
Uanis(N00M) \\sim Ueq, Uanis(C00U) \\sim Ueq, Uanis(C019) \\sim Ueq: with sigma
of 0.001 and sigma for terminal atoms of 0.002
Uanis(C00N) \\sim Ueq, Uanis(C017) \\sim Ueq, Uanis(C00V) \\sim Ueq,
Uanis(C00W) \\sim Ueq, Uanis(C012) \\sim Ueq, Uanis(C01A) \\sim Ueq,
Uanis(C01F) \\sim Ueq, Uanis(C00R) \\sim Ueq, Uanis(C00Q) \\sim Ueq,
Uanis(C00S) \\sim Ueq, Uanis(C00X) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C00Y)
\\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C01C) \\sim Ueq, Uanis(C019) \\sim Ueq,
Uanis(C018) \\sim Ueq, Uanis(C00U) \\sim Ueq, Uanis(C010) \\sim Ueq,
Uanis(N00M) \\sim Ueq, Uanis(C00O) \\sim Ueq, Uanis(C00P) \\sim Ueq,
Uanis(N00J) \\sim Ueq, Uanis(N00K) \\sim Ueq, Uanis(C00L) \\sim Ueq,
Uanis(C00I) \\sim Ueq, Uanis(N00H) \\sim Ueq, Uanis(C00T) \\sim Ueq,
Uanis(C015) \\sim Ueq, Uanis(C01E) \\sim Ueq, Uanis(C013) \\sim Ueq,
Uanis(C014) \\sim Ueq, Uanis(C01G) \\sim Ueq, Uanis(C011) \\sim Ueq,
Uanis(C016) \\sim Ueq, Uanis(C00Z) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
4.a Free rotating group:
 O1(H1A,H1B), O0AA(H0AA,H0AB)
4.b Ternary CH refined with riding coordinates:
 C00L(H00L), C00O(H00Q), C00T(H00T), C00U(H00U)
4.c Aromatic/amide H refined with riding coordinates:
 C00Q(H00Z), C00R(H00R), C00V(H00V), C00W(H00W), C00X(H00), C012(H012),
 C013(H013), C014(H014), C016(H016), C017(H017), C018(H018), C01C(H01D),
 C01F(H01I), C01G(H01H), C4(H4), C5(H5)
4.d Idealised Me refined as rotating group:
 N00H(H00J,H00K,H00M), C00I(H00D,H00E,H00F), N00J(H00N,H00O,H00P), N00K(H00G,
 H00H,H00I), N00M(H00A,H00B,H00C), C00P(H00S,H00X,H00Y), C010(H01A,H01B,H01C),
 C015(H01E,H01F,H01G)
;
_shelx_res_checksum              51936
_shelx_hkl_checksum              55249
_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 3.047
_oxdiff_exptl_absorpt_empirical_full_min 0.507