Chiral organic‒inorganic lead halide perovskites based on α-alanine
Sirenko, Valerii Y.; Kucheriv, Olesia I.; Naumova, Dina D.; Fesych, Igor V.; Linnik, Rostyslav P.; Dascălu, Ioan-Andrei; Shova, Sergiu; Fritsky, Igor O.; Gural'skiy, Il'ya A.; New Journal of Chemistry 45 (2021) 12606–12612; doi:10.1039/D1NJ01089A

data_7060733
_publ_section_title
;
 Chiral organic--inorganic lead halide perovskites based on \a-alanine
;
_journal_issue                   28
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              12606
_journal_page_last               12612
_journal_paper_doi               10.1039/D1NJ01089A
_journal_volume                  45
_journal_year                    2021
_chemical_absolute_configuration syn
_chemical_formula_moiety         'Br3 Pb, C3 H8 N O2, H2 O'
_chemical_formula_sum            'C3 H10 Br3 N O3 Pb'
_chemical_formula_weight         555.04
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-12-01
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6219)
;
_audit_update_record
;
2021-01-26 deposited with the CCDC.	2021-06-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.41(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.836(4)
_cell_length_b                   6.0904(11)
_cell_length_c                   8.790(3)
_cell_measurement_reflns_used    1212
_cell_measurement_temperature    296
_cell_measurement_theta_max      27.0030
_cell_measurement_theta_min      2.3180
_cell_volume                     1167.9(5)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      296.0
_diffrn_detector_area_resol_mean 8.0797
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_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    -34.00  50.00   1.00   12.50    --  -15.52  77.00  30.00   84
  2  \w     25.00  52.00   1.00   12.50    --  -15.52  77.00  60.00   27
  3  \w    -23.00  46.00   1.00   12.50    --  -15.52  77.00 -60.00   69
  4  \w     -5.00  81.00   1.00   12.50    --   17.94  77.00-180.00   86
  5  \w     -4.00  81.00   1.00   12.50    --   17.94  77.00 -60.00   85
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0293
_diffrn_reflns_av_unetI/netI     0.0539
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            4219
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.347
_diffrn_reflns_theta_min         1.867
_exptl_absorpt_coefficient_mu    24.679
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.25291
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (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    3.157
_exptl_crystal_description       prism
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.328
_refine_diff_density_min         -0.981
_refine_diff_density_rms         0.179
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.01(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     100
_refine_ls_number_reflns         2392
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0513
_refine_ls_R_factor_gt           0.0436
_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^)+(0.0437P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0981
_refine_ls_wR_factor_ref         0.1037
_reflns_Friedel_coverage         0.823
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                2081
_reflns_number_total             2392
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj01089a2.cif
_cod_data_source_block           shi_4456_ilgu
_cod_depositor_comments
'Adding full bibliography for 7060732--7060735.cif.'
_cod_database_code               7060733
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.192
_shelx_estimated_absorpt_t_min   0.051
_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) groups, All O(H,H) groups
2. Restrained distances
 O2B-C1 \\sim O2A-C1
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uiso(O2B) = Uiso(O2A)
4. Others
 Fixed Sof: O2B(0.5) H2B(0.5) O2A(0.5) H2A(0.5)
5.a Riding coordinates:
 O1W(H1WA,H1WB), O2B(H2B), O2A(H2A)
5.b Ternary CH refined with riding coordinates:
 C2(H2)
5.c Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), C3(H3A,H3B,H3C)
;
_shelx_res_checksum              23971
_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
;