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_7713368
_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         'Br3 Pb, C5 H10 N O2, H2 O'
_chemical_formula_sum            'C5 H12 Br3 N O3 Pb'
_chemical_formula_weight         581.08
_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             2022-09-12
_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                 107.668(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.7757(3)
_cell_length_b                   15.3050(5)
_cell_length_c                   11.4543(5)
_cell_measurement_reflns_used    3627
_cell_measurement_temperature    293
_cell_measurement_theta_max      24.6650
_cell_measurement_theta_min      2.2810
_cell_volume                     1298.84(9)
_computing_cell_refinement       'CrysAlisPro 1.171.41.115a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.115a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.115a (Rigaku OD, 2021)'
_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
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1593
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.884
_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    -58.00  55.00   1.00   30.00    --  -15.29  13.00  56.00  113
  2  \w    -53.00 -28.00   1.00   30.00    --  -15.29 -13.00-114.00   25
  3  \w      7.00  32.00   1.00   30.00    --   17.79  13.00  56.00   25
  4  \w    -34.00   4.00   1.00   30.00    --   17.79 -13.00-114.00   38
  5  \w    -85.00 -58.00   1.00   30.00    --  -15.29-178.00  60.00   27
  6  \w    -39.00   6.00   1.00   30.00    --  -15.29 -77.00   0.00   45
  7  \w    -44.00  35.00   1.00   30.00    --   17.79 -57.00-120.00   79
  8  \w    -18.00  56.00   1.00   30.00    --   17.79 -99.00-180.00   74
  9  \w     -9.00   4.00   1.00   30.00    --   17.79  77.00-180.00   13
;
_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      0.0114508000
_diffrn_orient_matrix_UB_12      -0.0073740000
_diffrn_orient_matrix_UB_13      -0.0583496000
_diffrn_orient_matrix_UB_21      -0.0944348000
_diffrn_orient_matrix_UB_22      0.0041703000
_diffrn_orient_matrix_UB_23      -0.0277859000
_diffrn_orient_matrix_UB_31      0.0105422000
_diffrn_orient_matrix_UB_32      0.0455612000
_diffrn_orient_matrix_UB_33      -0.0068987000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0462
_diffrn_reflns_av_unetI/netI     0.0826
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.884
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            12888
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.824
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.169
_diffrn_reflns_theta_min         1.866
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    22.199
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.42522
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.115a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.972
_exptl_crystal_description       block
_exptl_crystal_F_000             1040
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.866
_refine_diff_density_min         -0.891
_refine_diff_density_rms         0.183
_refine_ls_abs_structure_details
;
 Flack x determined using 1378 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.007(11)
_refine_ls_extinction_coef       0.00288(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   0.936
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     237
_refine_ls_number_reflns         5784
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.936
_refine_ls_R_factor_all          0.0770
_refine_ls_R_factor_gt           0.0432
_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^)] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0490
_refine_ls_wR_factor_ref         0.0585
_reflns_Friedel_coverage         0.799
_reflns_Friedel_fraction_full    0.938
_reflns_Friedel_fraction_max     0.759
_reflns_number_gt                4013
_reflns_number_total             5784
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02056h2.cif
_cod_data_source_block           shi_5137_ilgu_autored
_cod_database_code               7713368
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C10H10N2O4Pb1Br3
_chemical_oxdiff_usercomment     SV244
_shelx_estimated_absorpt_t_max   0.215
_shelx_estimated_absorpt_t_min   0.136
_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.a Riding coordinates:
 O2(H2E,H2F), O1(H1C,H1D), O4(H4)
2.b Ternary CH refined with riding coordinates:
 C6(H6A), C1(H1)
2.c Secondary CH2 refined with riding coordinates:
 N2(H2A,H2B), C9(H9B,H9A), C8(H8A,H8B), C7(H7A,H7B), N1(H1A,H1B), C2(H2C,H2D),
 C4(H4A,H4B), C3(H3A,H3B)
2.d Idealised tetrahedral OH refined as rotating group:
 O6(H6)
;
_shelx_res_checksum              96603
_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 1.827
_oxdiff_exptl_absorpt_empirical_full_min 0.671