Chiral 2D organic-inorganic hybrid perovskites based upon L-histidine
Sirenko, Valerii Y.; Kucheriv, Olesia I.; Gumienna-Kontecka, Elzbieta; Shova, Sergiu; Gural'skiy, Il'ya A.; Dalton Transactions  (2022) –; doi:10.1039/D2DT03025J

data_7711441
_publ_section_title
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 Chiral 2D organic-inorganic hybrid perovskites based upon L-histidine
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT03025J
_journal_year                    2022
_chemical_absolute_configuration syn
_chemical_formula_moiety         'Br4 Pb, 2(C6 H10 N3 O2)'
_chemical_formula_sum            'C12 H20 Br4 N6 O4 Pb'
_chemical_formula_weight         839.17
_space_group_crystal_system      orthorhombic
_space_group_IT_number           20
_space_group_name_Hall           'C 2c 2'
_space_group_name_H-M_alt        'C 2 2 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2022-02-16
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-09-16 deposited with the CCDC.	2022-10-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.2006(6)
_cell_length_b                   7.8434(6)
_cell_length_c                   29.935(2)
_cell_measurement_reflns_used    1303
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.0080
_cell_measurement_theta_min      2.7180
_cell_volume                     2160.2(3)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_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    'SHELXS  (Sheldrick, 2008)'
_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 0.998
_diffrn_measured_fraction_theta_max 0.853
_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    -32.00  47.50   0.75  175.00    --  -15.29  66.00 164.00  106
  2  \w      4.00  39.25   0.75  175.00    --   17.71-132.00 -29.00   47
  3  \w     -9.00  30.00   0.75  175.00    --   17.71  77.00  30.00   52
  4  \w      6.00  38.25   0.75  175.00    --   17.71  77.00-120.00   43
  5  \w     -9.00  31.50   0.75  175.00    --   17.71  77.00 150.00   54
  6  \w    -65.00 -61.25   0.75  175.00    --  -15.29 139.00-143.00    5
;
_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      -0.0075521590
_diffrn_orient_matrix_UB_12      -0.0015998729
_diffrn_orient_matrix_UB_13      0.0235774342
_diffrn_orient_matrix_UB_21      0.0581544505
_diffrn_orient_matrix_UB_22      0.0588330015
_diffrn_orient_matrix_UB_23      0.0020289137
_diffrn_orient_matrix_UB_31      -0.0500166064
_diffrn_orient_matrix_UB_32      0.0686882423
_diffrn_orient_matrix_UB_33      -0.0011950239
_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  0.0765
_diffrn_reflns_av_unetI/netI     0.1237
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.853
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            5265
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.834
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.330
_diffrn_reflns_theta_min         2.041
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    15.239
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86446
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
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    2.580
_exptl_crystal_description       plate
_exptl_crystal_F_000             1552
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         4.696
_refine_diff_density_min         -3.274
_refine_diff_density_rms         0.340
_refine_ls_abs_structure_details
;
 Flack x determined using 474 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.02(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.157
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     92
_refine_ls_number_reflns         2482
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.151
_refine_ls_R_factor_all          0.1264
_refine_ls_R_factor_gt           0.0875
_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^)+(0.0835P)^2^+2.6954P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1883
_refine_ls_wR_factor_ref         0.2121
_reflns_Friedel_coverage         0.715
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.810
_reflns_number_gt                1744
_reflns_number_total             2482
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03025j2.cif
_cod_data_source_block           shi_5670_ilgu
_cod_database_code               7711441
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C12H16Br4N6O4Pb
_chemical_oxdiff_usercomment     SV_405
_shelx_estimated_absorpt_t_max   0.750
_shelx_estimated_absorpt_t_min   0.311
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.969(4)
 0.031(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All O(H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(C5) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(O2) \\sim
Ueq, Uanis(O1) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(C6) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(N3) = Uanis(C5) = Uanis(N2) = Uanis(C4) = Uanis(C6)
4.a Riding coordinates:
 O1(H1)
4.b Ternary CH refined with riding coordinates:
 C2(H2)
4.c Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B)
4.d Aromatic/amide H refined with riding coordinates:
 C6(H6), N3(H3), C5(H5)
4.e Fitted pentagon refined as free rotating group:
 C4(C6,N3,C5,N2)
4.f Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C)
;
_shelx_res_checksum              14862
_shelx_hkl_checksum              14525
_olex2_date_sample_data_collection 2022-02-12
_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 1.488
_oxdiff_exptl_absorpt_empirical_full_min 0.844