Alternating chiral and achiral spacers for constructing two-dimensional chiral hybrid perovskites toward circular-polarization-sensitive photodetection.
You, Shihai; Yu, Panpan; Zhu, Tingting; Guan, Qianwen; Wu, Jianbo; Dai, Hongliang; Zhong, Haiqing; Zhu, Zeng-Kui; Luo, Junhua; Materials horizons 10 (2023) 5307–5312; doi:10.1039/d3mh00745f

data_1569863
_publ_section_title
;
 Alternating chiral and achiral spacers for constructing two-dimensional
 chiral hybrid perovskites toward circular-polarization-sensitive
 photodetection.
;
_journal_issue                   11
_journal_name_full               'Materials horizons'
_journal_page_first              5307
_journal_page_last               5312
_journal_paper_doi               10.1039/d3mh00745f
_journal_volume                  10
_journal_year                    2023
_chemical_absolute_configuration ad
_chemical_formula_moiety         'Br4 Pb, C9 H14 N, C5 H14 N'
_chemical_formula_sum            'C14 H28 Br4 N2 Pb'
_chemical_formula_weight         751.21
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-03-25
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2023-03-30 deposited with the CCDC.	2023-09-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.0160(3)
_cell_length_b                   8.4161(4)
_cell_length_c                   34.5711(19)
_cell_measurement_reflns_used    6099
_cell_measurement_temperature    300.47(10)
_cell_measurement_theta_max      29.4920
_cell_measurement_theta_min      2.3520
_cell_volume                     2332.29(19)
_computing_cell_refinement       'CrysAlisPro 1.171.42.73a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.73a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.73a (Rigaku OD, 2022)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      300.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_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    -19.00   9.00   0.50    1.05    --    6.70  92.00 133.00   56
  2  \w    -17.00  27.00   0.50    1.05    --   -5.06 -99.00 150.00   88
  3  \w    -18.00  33.00   0.50    1.05    --   -5.06  38.00 -62.00  102
  4  \w      3.00  57.00   0.50    1.05    --    6.70  38.00-150.00  108
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0551
_diffrn_reflns_av_unetI/netI     0.0530
_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       10
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            11584
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        24.997
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_min         2.491
_exptl_absorpt_coefficient_mu    14.084
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.16462
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.73a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.139
_exptl_crystal_description       plate
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.370
_refine_diff_density_min         -1.213
_refine_diff_density_rms         0.190
_refine_ls_abs_structure_details
;
 Flack x determined using 1161 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.024(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     158
_refine_ls_number_reflns         4020
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0606
_refine_ls_R_factor_gt           0.0458
_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^)+(0.0621P)^2^+1.0486P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1048
_refine_ls_wR_factor_ref         0.1099
_reflns_Friedel_coverage         0.684
_reflns_Friedel_fraction_full    0.951
_reflns_Friedel_fraction_max     0.951
_reflns_number_gt                3336
_reflns_number_total             4020
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3mh00745f2.cif
_cod_data_source_block           220728e14_r_auto
_cod_depositor_comments
'Adding full bibliography for 1569862--1569864.cif.'
_cod_database_code               1569863
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C13-C14 = C13-C12 = C11-C12 = C11-C10
 1.5 with sigma of 0.01
 C12-C11
 1.5 with sigma of 0.01
 C14-C13
 1.5 with sigma of 0.01
 C3-C2 = C2-C1
 1.5 with sigma of 0.01
 N2-C14
 1.5 with sigma of 0.01
 C11-C10
 1.5 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C7) \\sim Ueq, Uanis(C8) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C11) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C12) = Uanis(C11)
Uanis(C14) = Uanis(C13) = Uanis(C12) = Uanis(C11) = Uanis(C10)
4.a Ternary CH refined with riding coordinates:
 C3(H3)
4.b Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C2(H2A,H2B), C13(H13A,H13B), C12(H12A,H12B), C11(H11A,H11B)
4.c Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C5(H5), C6(H6), C7(H7)
4.d Fitted hexagon refined as free rotating group:
 C8(C9,C4,C5,C6,C7)
4.e Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), N2(H2C,H2D,H2E), C1(H1D,H1E,H1F), C10(H10A,H10B,H10C)
;
_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
;