Circularly polarized luminescence enlargement from crystals to oriented films of enantiopure 2D hybrid perovskites.
Zhao, Xuan-Hui; Li, Na-Na; Peng, Jing; Xu, Jun; Luo, Peng; Dong, Xi-Yan; Hu, Xiaozong; Chemical communications (Cambridge, England) 59 (2023) 6881–6884; doi:10.1039/d3cc01739g

data_7131660
_publ_section_title
;
 Circularly polarized luminescence enlargement from crystals to oriented
 films of enantiopure 2D hybrid perovskites.
;
_journal_issue                   45
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              6881
_journal_page_last               6884
_journal_paper_doi               10.1039/d3cc01739g
_journal_volume                  59
_journal_year                    2023
_chemical_absolute_configuration syn
_chemical_formula_moiety         'Br4 Pb, 2(C8 H11 F N)'
_chemical_formula_sum            'C16 H22 Br4 F2 N2 Pb'
_chemical_formula_weight         807.18
_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     iterative
_audit_creation_date             2023-03-30
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-03-30 deposited with the CCDC.	2023-05-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.84030(10)
_cell_length_b                   8.79580(10)
_cell_length_c                   33.4329(4)
_cell_measurement_reflns_used    5326
_cell_measurement_temperature    200.00(10)
_cell_measurement_theta_max      72.7410
_cell_measurement_theta_min      5.1950
_cell_volume                     2305.59(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      200
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.972
_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    -29.00  44.00   0.50    0.50    --    0.00  57.00-120.00  146
  2  \w     43.00  84.00   0.50    0.50    --    0.00  57.00 -90.00   82
  3  \w      9.00  44.00   0.50    0.50    --   97.60 -61.00-120.00   70
  4  \w     16.00  42.00   0.50    0.50    --   97.60 -61.00 150.00   52
  5  \w     57.00 106.00   0.50    0.50    --   97.60 -61.00 150.00   98
  6  \w     59.00 115.00   0.50    0.50    --   97.60 -61.00-120.00  112
  7  \w     12.00 110.00   0.50    0.50    --   97.60 -45.00  60.00  196
  8  \w     31.00 116.00   0.50    0.50    --   97.60 -45.00 -60.00  170
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0563453000
_diffrn_orient_matrix_UB_12      -0.0189060000
_diffrn_orient_matrix_UB_13      0.0438271000
_diffrn_orient_matrix_UB_21      -0.0783512000
_diffrn_orient_matrix_UB_22      -0.1558933000
_diffrn_orient_matrix_UB_23      -0.0101939000
_diffrn_orient_matrix_UB_31      0.1712047000
_diffrn_orient_matrix_UB_32      -0.0777140000
_diffrn_orient_matrix_UB_33      0.0098047000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0424
_diffrn_reflns_av_unetI/netI     0.0534
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            6740
_diffrn_reflns_point_group_measured_fraction_full 0.896
_diffrn_reflns_point_group_measured_fraction_max 0.922
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         66.492
_diffrn_reflns_theta_min         5.200
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    22.518
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.08318
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.27b (Rigaku Oxford Diffraction, 2015)
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    2.325
_exptl_crystal_description       plank
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.907
_refine_diff_density_min         -1.504
_refine_diff_density_rms         0.244
_refine_ls_abs_structure_details
;
 Flack x determined using 1320 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.013(10)
_refine_ls_extinction_coef       0.00040(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     231
_refine_ls_number_reflns         3744
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0380
_refine_ls_R_factor_gt           0.0373
_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^+2.9522P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1019
_refine_ls_wR_factor_ref         0.1025
_reflns_Friedel_coverage         0.585
_reflns_Friedel_fraction_full    0.791
_reflns_Friedel_fraction_max     0.814
_reflns_number_gt                3653
_reflns_number_total             3744
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc01739g2.cif
_cod_data_source_block           hy-s-1
_cod_depositor_comments
'Adding full bibliography for 7131659--7131661.cif.'
_cod_database_code               7131660
_shelxl_version_number           2013-2
_chemical_oxdiff_usercomment     ' '
_shelx_estimated_absorpt_t_max   0.212
_shelx_estimated_absorpt_t_min   0.133
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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.a Ternary CH refined with riding coordinates:
 C10(H10), C2(H2)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C8(H8), C16(H16), C5(H5), C12(H12), C15(H15), C7(H7), C13(H13)
2.c Idealised Me refined as rotating group:
 N2(H2A,H2B,H2C), N1(H1A,H1B,H1C), C1(H1D,H1E,H1F), C9(H9A,H9B,H9C)
;
_shelx_res_checksum              49785
_shelx_hkl_checksum              50986
_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 5.700
_oxdiff_exptl_absorpt_empirical_full_min 0.362