Structural diversity in proline-based lead bromide chiral perovskites
Sirenko, Valerii Y.; Kucheriv, Olesia I.; Fritsky, Igor O.; Gumienna-Kontecka, Elzbieta; Dascalu, Andrei; Shova, Sergiu; Gural'skiy, Il'ya A.; Dalton Transactions  (2023) –; doi:10.1039/D3DT02056H

data_7713367
_publ_section_title
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 Structural diversity in proline-based lead bromide chiral perovskites
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT02056H
_journal_year                    2023
_chemical_absolute_configuration syn
_chemical_formula_moiety         'Br10 Pb3, 4(C5 H10 N O2), 4(H2 O)'
_chemical_formula_sum            'C20 H48 Br10 N4 O12 Pb3'
_chemical_formula_weight         1957.29
_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             2022-09-09
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-03-23 deposited with the CCDC.	2023-07-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.508(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   22.2582(5)
_cell_length_b                   9.3625(3)
_cell_length_c                   11.5564(4)
_cell_measurement_reflns_used    5073
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.2910
_cell_measurement_theta_min      1.8550
_cell_volume                     2405.96(13)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (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      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1593
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.886
_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    -45.00   9.00   1.00   30.00    --  -15.29  99.00  62.00   54
  2  \w     -6.00  19.00   1.00   30.00    --   17.87 -99.00 -43.00   25
  3  \w    -39.00  11.00   1.00   30.00    --  -15.29 -77.00 -30.00   50
  4  \w    -87.00 -41.00   1.00   30.00    --  -15.29-178.00  90.00   46
  5  \w    -87.00 -46.00   1.00   30.00    --  -15.29-178.00 150.00   41
  6  \w      8.00  83.00   1.00   30.00    --   17.87  38.00   0.00   75
  7  \w      0.00  25.00   1.00   30.00    --   17.87  77.00  90.00   25
  8  \w      2.00  73.00   1.00   30.00    --   17.87  57.00 150.00   71
  9  \w    -41.00 -16.00   1.00   30.00    --  -15.29  99.00  62.00   25
 10  \w    -78.00 -40.00   1.00   30.00    --  -15.29-178.00  60.00   38
 11  \w     12.00  38.00   1.00   30.00    --   17.71  57.00 -90.00   26
 12  \w     19.00  55.00   1.00   30.00    --   17.71  57.00  30.00   36
 13  \w      7.00   9.00   1.00   30.00    --   17.71  57.00 -60.00    2
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0112472000
_diffrn_orient_matrix_UB_12      -0.0701640000
_diffrn_orient_matrix_UB_13      -0.0092151000
_diffrn_orient_matrix_UB_21      0.0005722000
_diffrn_orient_matrix_UB_22      -0.0115396000
_diffrn_orient_matrix_UB_23      0.0606584000
_diffrn_orient_matrix_UB_31      -0.0298596000
_diffrn_orient_matrix_UB_32      0.0262051000
_diffrn_orient_matrix_UB_33      0.0017977000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0439
_diffrn_reflns_av_unetI/netI     0.0722
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.886
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            13778
_diffrn_reflns_point_group_measured_fraction_full 0.962
_diffrn_reflns_point_group_measured_fraction_max 0.815
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.396
_diffrn_reflns_theta_min         2.360
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    18.822
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.15485
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (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    2.702
_exptl_crystal_description       plate
_exptl_crystal_F_000             1776
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.226
_refine_diff_density_min         -1.380
_refine_diff_density_rms         0.187
_refine_ls_abs_structure_details
;
 Flack x determined using 1324 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.017(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     222
_refine_ls_number_reflns         5424
_refine_ls_number_restraints     158
_refine_ls_restrained_S_all      0.989
_refine_ls_R_factor_all          0.0698
_refine_ls_R_factor_gt           0.0427
_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^)+(0.0173P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0588
_refine_ls_wR_factor_ref         0.0675
_reflns_Friedel_coverage         0.738
_reflns_Friedel_fraction_full    0.920
_reflns_Friedel_fraction_max     0.734
_reflns_number_gt                4032
_reflns_number_total             5424
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02056h2.cif
_cod_data_source_block           shi_6078_ilgu_autored
_cod_database_code               7713367
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C5H5N2O4Pb1IBr3
_chemical_oxdiff_usercomment     SV_507
_shelx_estimated_absorpt_t_max   0.453
_shelx_estimated_absorpt_t_min   0.165
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3.a Riding coordinates:
 O1(H1), O5(H5C,H5D), O3(H3), O6(H6A,H6B)
3.b Ternary CH refined with riding coordinates:
 C2(H2), C7(H7)
3.c Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C5(H5A,H5B), N1(H1A,H1B), C8(H8A,H8B), C10(H10A,H10B), N2(H2A,
 H2B), C4(H4A,H4B), C9(H9A,H9B)
;
_shelx_res_checksum              69527
_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 4.145
_oxdiff_exptl_absorpt_empirical_full_min 0.525